",isbn:"978-1-83969-084-6",printIsbn:"978-1-83969-083-9",pdfIsbn:"978-1-83969-085-3",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"521fce75254e23855ed5c3ff4a4f1ea1",bookSignature:"Prof. Xianquan Zhan",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/10220.jpg",keywords:"Sample Preparation, Mass Spectrometry, Metabolite, Metabolome, Nuclear Magnetic Resonance, Lipid Metabolomics, Targeted Metabolomics, Untargeted Metabolomics, Cancer, Neurodegenerative Disease, Endocrine Diseases, Metabolic Disease",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"October 13th 2020",dateEndSecondStepPublish:"November 10th 2020",dateEndThirdStepPublish:"January 9th 2021",dateEndFourthStepPublish:"March 30th 2021",dateEndFifthStepPublish:"May 29th 2021",remainingDaysToSecondStep:"2 months",secondStepPassed:!0,currentStepOfPublishingProcess:4,editedByType:null,kuFlag:!1,biosketch:"A pioneering expert in the field of proteomics and proteofroms, multiomics, biomarkers, and 3P medicine in cancer, appointed as Fellow of Royal Society of Medicine, Fellow and National Representative of EPMA, and Associate Editor of EPMA Journal and BMC Medical Genomics.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"223233",title:"Prof.",name:"Xianquan",middleName:null,surname:"Zhan",slug:"xianquan-zhan",fullName:"Xianquan Zhan",profilePictureURL:"https://mts.intechopen.com/storage/users/223233/images/system/223233.jpg",biography:"Xianquan Zhan received his M.D. and Ph.D. training in preventive medicine at the West China University of Medical Sciences from 1989 to 1999. He received his post-doctoral training in oncology and cancer proteomics at the Central South University and University of Tennessee Health Science Center (UTHSC). He worked at UTHSC and Cleveland Clinic in USA from 2001 to 2012, and achieved the rank of Associate Professor at UTHSC. After that, he became a Full Professor at the Central South University and Shandong First Medical University, and an Advisor of MS/PhD graduate students and postdoctoral fellows. He is also a Fellow of the Royal Society of Medicine, Fellow of EPMA, European EPMA National Representative, full member of the American Society of Clinical Oncology (ASCO), member of the American Association for the Advancement of Sciences (AAAS), Editor-In-Chief of the International Journal of Chronic Diseases & Therapy, Associate Editor of the EPMA Journal and BMC Medical Genomics, and Guest Editor of Frontiers in Endocrinology and Mass Spectrometry Reviews. 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1. Introduction
Nanostructured materials exhibit novel properties, which notably differ from those of the corresponding bulk solid, due to the small size effect [1]. Transition metal-oxide nanoparticles have attracted considerable interest on account of their applications in various fields, including catalysis, electronics, coatings, gas sensing, electrochemical devices, solar energy conversion and biomedicine [2, 3]. Several methods have been employed for the synthesis of cobalt nanomaterials, including: (i) microemulsion, (ii) solvothermal method, (iii) thermal decomposition of cobalt precursors, (iv) spray pyrolysis, (v) sol-gel process, etc. [1, 4, 5]. Thermal decomposition is a commonly employed method for preparation of nanoscale cobalt or cobalt oxide, due to process simplicity, short reaction time, and, most importantly, low-cost and efficiency. Such nanoparticles are typically prepared via transformation of precursors under controlled conditions. There are many potential precursors, such as, inorganic and organic salts and metal-organic frameworks (MOFs). The decomposition pathway of the precursor depends on the type of the gaseous atmosphere prevailing during heating, on the heating schedule itself, as well as on the characteristics of the organic group. Co-addition of other metal cations toward a mixed metal-organic precursor provides a straightforward approach to the synthesis of mixed metal oxides. Additionally, supported cobalt-based nanomaterials (i.e. cobalt oxide/graphene composites) can be fabricated. The aim of the current work is to present a comprehensive review of the research focusing on synthesis of cobalt-based nanomaterials from activation of organic precursors.
2. Cobalt and cobalt oxide nanoparticles from carboxylates
A major group of organic precursors that have been employed for the synthesis of cobalt and cobalt oxide nanoparticles via a thermal decomposition route is cobalt-carboxylate salts. The “carboxylate” term includes several organic species that contain at least one carboxyl group, such as oxalate, citrate, etc. Methods for synthesis of cobalt-carboxylates include (i) sol-gel [2, 4], (ii) intimate mixing of cobalt ions [6–8], (iii) precipitation [9, 10], (iv) hot oxidation-redox reaction [11], (v) ball milling [12] and (vi) microemulsion [13]. Reaction of cobalt acetate with a carboxylic acid, for example, leads directly to the synthesis of cobalt-carboxylate, when the carboxylic acid in question is stronger than acetic acid: Co(Ac)2 + RCOOH → Co(RCOO)2 + 2 AcH (1). This cannot be the case when cobalt nitrate or cobalt chloride is employed, since nitrate and chloride anions are weak conjugate bases of the strong nitric and hydrochloric acids. Nevertheless, many research groups choose to utilize metal-inorganic salts to synthesize cobalt-carboxylate precursors. Thermal treatment of the synthesized carboxylate precursor leads to the removal of the organic species, thus cobalt or cobalt oxide nanoparticles are formed. In the following sections, a review of the synthetic protocols for synthesis of cobalt-based nanomaterials from cobalt-carboxylates is presented.
2.1. Cobalt oxide nanoparticles from oxalate precursors
There are several publications concerning the synthesis of cobalt or cobalt oxide nanoparticles from oxalate precursors. Abdelkader et al. synthesized Co3O4 nanoparticles by calcination of cobalt (II) oxalate dihydrate in static air at 500°C for 2 h [14]. Thota et al. employed a sol-gel process to synthesize oxalate precursors and their subsequent thermal treatment to produce Co3O4 nanocrystallites. More specifically, cobalt acetate tetrahydrate was dissolved in ethanol at 35–40°C under continuous stirring followed by oxalic acid addition to yield a thick gel. Thermal decomposition of the dried gel in air at 400–600°C for 2 h led to Co3O4 [4]. Luisetto et al. have also produced Co3O4 by thermal treatment of cobalt oxalate precipitate at 450°C for 2 h in air [2]. de Rivas et al. prepared Co3O4 nanoparticles via calcination of oxalate nanorods at 500°C in static air [15]. Cobalt oxalate precursors have been also prepared from cobalt nitrate, cobalt chloride or cobaltous hydroxide carbonate. Shen et al. obtained CoO nanoparticles from the decomposition of corresponding oxalates at 500°C for 4 h in air. Oxalates were prepared via precipitation from a solution of cobalt nitrate, oxalic acid and ethanol [16]. Manteghi et al. synthesized Co3O4 nanostructures by thermal decomposition of cobalt oxalate synthesized by precipitation from cobalt nitrate or cobalt chloride and ammonium oxalate in the presence or absence of surfactants [17]. Yuan et al. synthesized Co3O4 by annealing cobalt oxalate precursors prepared via hydrothermal and rheological phase reaction methods [18, 19].
2.2. Cobalt oxide nanoparticles from citrate precursors
Manouchehri et al. reported on the synthesis of Co3O4 and CoO nanoparticles via solid state ball milling of cobalt acetate and citric acid powders and subsequent calcination of the prepared carboxylate precursors [12]. de Rivas et al. also used ball milling for synthesis of cobalt citrate starting from cobalt carbonate and citric acid [20]. An aqueous sol-gel citrate procedure has been employed by many research groups initiating from cobalt nitrate and citric acid and the obtained precursors were thermally decomposed between 300 and 500°C in static air for 4 h [20–22]. Pudukudy et al. chose a simple solid-state mixing of cobalt nitrate with various modifiers such as citric acid, glucose, sucrose and urea. The components were mixed, pulverized and heated at 80°C for 1 h. The bimodal mesoporous spinel cobalt oxide nanomaterials were prepared by calcination at 300°C for 2 h [23].
2.3. Cobalt and cobalt oxide nanoparticles from malonate precursors
Mohamed et al. synthesized cobalt malonates by precipitation using cobalt chloride and disodium malonate or malonic acid. The precipitates were heated up to 500°C at heating rates between 2 and 20°C min−1 in a dynamic atmosphere of N2, H2 or air resulting in cobalt oxides and metallic cobalt [10]. Stefanescu et al. synthesized nanosized cobalt oxides unsupported [3] or dispersed in a SiO2 matrix [24] by thermal decomposition of compounds resulting from a redox reaction of cobalt nitrate and diols (1,2-ethanediol, 1,3-propanediol). The produced caboxylates were oxalate, glyoxylate and malonate. The redox reaction between the NO3− ions and -OH groups of each diol took place under controlled heating (90–120°C, 2 h) and the resulting powders were annealed at 350 and 1000°C for 3 h in ambient air.
2.4. Cobalt and cobalt oxide nanoparticles from succinate precursors
Ganguly et al. synthesized cobalt and cobalt oxide nanoparticles from cobalt succinate originated from a reverse micellar method using cobalt nitrate, 1-butanol and CTAB (as the surfactant). The collected product by centrifugation was thermally decomposed under N2 at 650°C and under air at 500°C for 6 h, yielding pure Co and Co3O4, respectively [13].
2.5. Cobalt oxide nanoparticles from tartrate precursors
Bhattacharjee et al. reported the synthesis of Co3O4 nanoparticles by thermal decomposition at 400–600°C of cobalt (II)-tartrate complex prepared by a modified sol-gel route employing cobalt nitrate and tartaric acid [25]. Palacios-Hernández et al. prepared CoO and Co3O4 nanoparticles by thermal treatment of cobalt tartrate synthesized by precipitation. Cobalt tartrate was obtained by mixing solutions of cobalt nitrate and the disodium salt of L-tartaric acid. The nanoparticles were prepared by thermal decomposition of the metal-organic complex under isothermal conditions at 500°C in the presence of air for 4 h [26].
2.6. Cobalt oxide nanoparticles from other carboxylate precursors
Chen et al. synthesized CoO nanoparticles using cobalt oleate as precursor. Cobalt chloride and sodium oleate were used as initial chemicals and the obtained dried precipitate was dissolved with oleic acid in 1-octadecene. The CoO nanoparticles were produced by heating the mixture up to 320°C and maintaining that temperature for 30 min [27]. Assim et al. presented the synthesis of a series of ethylene glycol-functionalized cobalt (II) carboxylates by an anion exchange reaction of cobalt (II) acetate tetrahydrate with the corresponding acids. Co3O4 nanoparticles were prepared by solid state thermal decomposition of Co(CO2CH2(OC2H4)2OMe)2 at 300°C, while different decomposition times of 10, 20 and 30 min were applied [28]. Semenov et al. prepared cobalt composites via thermal treatment under isothermal conditions (335°C for 9 h under Ar) of unsaturated cobalt dicarboxylates (hydrogen allylmalonate, acetylenedicarboxylate, itaconate, maleate, glutaconate, cis-muconate) using cobalt carbonate and an unsaturated dicarboxylic acid aqueous solution [9].
3. Mixed metal-oxide nanoparticles from carboxylate precursors
Mixed metal oxides contain two or more metallic ions in proportions that may either be defined by stoichiometry or variable. One way to classify mixed metal oxides is according to their crystalline structure (spinels, perovskites, etc.) [29].
3.1. Spinel mixed metal-oxide nanoparticles from carboxylate precursors
The preparation methods for CoFe2O4 nanoparticles require specialized techniques to prevent agglomeration. Diodati et al. synthesized various spinel ferrites (CoFe2O4, NiFe2O4, ZnFe2O4 and MgFe2O4) by a wet-synthesis coprecipitation route starting from iron(III) nitrate, cobalt(II) chloride and oxalic acid in order to prepare the oxalate precursors. The precipitate was centrifuged, dried and calcined at 873 or 1173 K for 5 h in air [30]. Many researchers used the redox method to synthesize the carboxylate precursors (oxalate, malonate, succinate, etc.) initiating from iron(III) nitrate, cobalt(II) nitrate and various diols (ethylene glycol, 1,2-propanediol, 1,3-propanediol and 1,4-butanediol). The obtained precursors were calcined at various temperatures in air to cobalt ferrites [11, 31, 32]. In some cases, the synthesized ferrites were dispersed in a SiO2 matrix using a modified sol-gel and redox reaction method [31, 33–35]. Amiri et al. synthesized CoFe2O4/SiO2 nanocomposites by a procedure described as sol-gel autocombustion method. Iron and cobalt nitrate were dissolved in water and acid solutions (maleic, malonic, trimesic and ascorbic acid) were added separately as well as tetraethoxysilane. The sols were transformed into gel at 40°C for 24 h [36]. Cobalt-zinc ferrite, Co1−xZnxFe2O4 (x varying from 0 to 1) was obtained by thermal decomposition of the carboxylate precursor, starting from a mixture of Fe(III), Co(II) and Zn(II) nitrates and 1,3-propanediol whereas a redox reaction took place. The precursor was decomposed at 300°C and further annealed in air for 3 h at various temperatures from 350 to 1000°C [37, 38].
Mixed cobalt-manganese oxide is another spinel synthesized by thermal decomposition of carboxylate salts. Papadopoulou et al. obtained Co-MnO catalysts from the pyrolytic decomposition of mixed cobalt-manganese fumarate and gluconate salts. The precursor compounds were prepared by mixing aqueous solution of cobalt and manganese acetate with an aqueous solution of D-gluconic acid or an ethanolic solution of fumaric acid. The corresponding mixed metal/metal-oxide nanoparticles were prepared by thermal decomposition of the organic precursors under inert gas flow in the temperature range of 500–700°C. Cobalt-manganese spinel oxide was also prepared via oxidative treatment of the same mixed carboxylates at 500°C for 2 h [6–8]. Faure et al. prepared CoxMn3−xO4 (0 ≤ x ≤ 3) by controlled decomposition of mixed oxalates, precipitated at room temperature using cobalt nitrate, manganese nitrate and ammonium oxalate. The thermal decomposition of oxalates was carried out near 200°C under O2/Ar flow and further calcination up to 300°C for 1 h [39].
Wang et al. synthesized CoAl2O4 nanoparticles via thermal treatment of Co-Al-glycine precursors, initiating from cobalt and aluminum nitrate and glycine. The precursor was treated under air at 200–1000°C for 2 h [40]. Synthesis of CoCr2O4, a member of the chromite spinel family, was reported by Gingasu et al. via thermal decomposition of tartrate and gluconate precursors obtained by precipitation using cobalt (II) nitrate, chromium (III) nitrate and tartaric acid or δ-gluconolactone [41]. Finally, synthesis of metal cobaltite spinels (MgCo2O4, NiCo2O4) by thermal decomposition of coprecipitated mixed oxalate precursors has been reported [42, 43].
3.2. Perovskite mixed metal nanoparticles from carboxylate precursors
Seyfi et al. synthesized unsupported perovskite samples (i.e. LaCoO3) by thermal decomposition of citrate complexes using lanthanum(III) nitrate, cobalt(II) nitrate and citric acid as initial compounds. The obtained viscous gel was dried and calcined at 700°C for 5 h under air atmosphere [44].
3.3. Ilmenite mixed metal-oxide nanoparticles from carboxylate precursors
Gabal et al. prepared CoTiO3 via a coprecipitation method. The mixed oxalate precursor was thermally treated at various temperatures (230–950°C, 30 min and 1000°C, 2 h) and CoTiO3 nanoparticles were obtained [45].
4. Supported cobalt oxide from carboxylate salts
Transition metal oxides have been proposed as materials for lithium-ion batteries (LIBs) and it has been reported that the performance of cobalt oxides is further improved if cobalt oxide nanoparticles are supported on carbon (nanofibers, nanoflakes, etc.) [46]. From this point of view, Guo et al. synthesized Co3O4/graphite composites by precipitation of cobalt oxalate on the surface of graphite and pyrolysis of the precipitate [47].
5. Cobalt-based nanomaterials from metal-organic frameworks (MOFs)
A number of recent publications have reported on the synthesis of cobalt-based nanomaterials embedded in carbon, employing metal-organic framework compounds as precursors. Metal-organic frameworks (MOFs) are an emerging class of porous materials constructed from metal-containing nodes and organic linkers [46]. Wang et al. showed that the direct pyrolysis of cobalt nitrate accommodated by impregnation in the pores of ZIF-8 and ZIF-67 yields Co3O4 nanoparticles [48]. Ashouri et al. utilized the thermal decomposition of cobalt-terephthalate MOF precursor as a synthetic route for the fabrication of Co3O4 nanoparticles [49]. Pei et al. synthesized carbon-supported and Si-doped carbon-supported Co nanomaterials by the thermolysis of Co-MOF-71 at 600°C for 8 h under He flow [50]. Many researchers have utilized MOFs as precursors for the synthesis of cobalt-based nanoparticles embedded in carbon. Zhou et al. prepared nitrogen-doped carbon-embedded Co catalysts by one-step pyrolysis (600–900°C, for 8 h, under N2) of ZIF-67 with silica as the hard template [51] while, Khan et al. used direct carbonization of ZIF-12 at 950°C for 6 h under Ar atmosphere [52]. Lu et al. fabricated metallic Co nanoparticles embedded in N-doped porous carbon layers by thermal treatment of macroscale Co-MOFs obtained by using 1,3,5-benzenetricarboxylic acid, triethylamine and nonanoic acid, at various temperatures (800, 900, 1000°C) for 1 h under N2 atmosphere [53]. Qiu et al. obtained cobalt-based nanoparticles coated with a thin carbon shell from Co-MOF-74 via a two-step carbonization where at first the cobalt precursor was heated at 700°C for 2 h under Ar atmosphere to produce cobalt nanoparticles coated with carbon shell and in a second phase the as-synthesized material was calcined either at 500°C for 1 h under CO2 atmosphere to produce carbon-coated Co3O4 nanoparticles or for 30 min under the same conditions to produce Co/CoO nanomaterials. Pure Co3O4 nanocrystals were obtained by treating carbon-coated cobalt nanoparticles at 250°C for 2 h under air atmosphere [54].
6. Structure and characterization of cobalt-based nanoparticles
6.1. Structure and characterization of Co3O4 nanoparticles
The majority of publications for the synthesis of cobalt-based nanoparticles from thermal decomposition of organic precursors under air have reported on the formation of the spinel Co3O4 phase. The published X-Ray Diffraction (XRD) patterns have reflection peaks that can be perfectly indexed to the cubic phase of Co3O4 spinel with the cell parameter α in the range 8.07–8.15 Å and space group Fd3m (Figure 1). In most cases, there were no diffraction peaks related to CoO or metallic cobalt (Co0), except for thermal treatment above 900°C, where Co3O4 decomposes to CoO. The average crystallite size, estimated by the Debye-Scherrer equation, varied between 5 and 50 nm, depending on the preparation method and the type of cobalt precursor, the thermal treatment conditions, etc. Structural details of Co3O4 have been investigated by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). SEM results indicated the agglomeration of Co3O4 nanoparticles and various types of morphologies were observed, that is, matchstick type bars [4, 17], nanorods of bamboo stick type [4], truncated hexahedral shape [18], flocculent-like structures [48] and irregularly shaped aggregates (dense clusters) [21, 22, 26, 49]. TEM results were relatively consistent with XRD results concerning the crystallite size (5–50 nm). Palacios-Hernández et al. reported the synthesis of Co3O4 with average grain size of 300 nm and a scarce number of nanoparticles with a diameter of 100 nm and smaller, according to TEM. Most nanoparticles had faceted morphology and high crystalline quality as verified by Selected-Area Electron Diffraction (SAED) analysis and High-Resolution Transmission Electron Microscopy (HRTEM) [26]. Pseudo-hexagonal [15, 17, 18, 21], circular and occasionally rectangular [2] or uniform spherical [12] shaped nanoparticles were observed. In general, powders are homogeneously dispersed with dimensions ranging from 50 to 600 nm, in accordance with SEM results, mentioned above. TEM images further validated that the porous architectures—agglomerations—are constructed from the interconnection among the primary crystalline nanoparticles with size of a few nanometers. Furthermore, the regular diffraction spots displayed from SAED pattern, validated the cubic face-centered structure of Co3O4 [2, 4, 18, 25]. HRTEM analysis also indicated the single crystalline nature of Co3O4 [18, 25].
Figure 1.
Typical XRD pattern of pure Co3O4 [17].
The textural properties of cobalt oxides are typically determined by N2 adsorption-desorption at liquid N2 temperature. The reported Brunauer–Emmett–Teller (BET) specific surface area and Barrett-Joyner-Halenda (BJH) pore size distribution of Co3O4 nanoparticles differ significantly from sample to sample. Factors like the synthesis method of cobalt precursor, its nature, the treatment temperature and soak time affect their textural properties. The specific surface areas of Co3O4 nanoparticles vary from 7 [23] to 120 m2 g−1 [21], the pore volume ranges between 0.03 [23] and 0.24 cm3 g−1 [20] while average pore size is between 9 [20] and 68 nm [23]. Wang et al. found that all N2 sorption isotherms of Co3O4 and Co-Ce oxide nanoparticles can be assigned to a type IV isotherm, typical for mesoporous materials, showing a hysteresis loop at P/P0 = 0.45 [22]. The mesoporous structure of the nanomaterials was also noted by other researchers [15, 17, 20, 23]. Pudukudy et al. synthesized Co3O4 spinels possessing a bimodal mesopore distribution in the presence of modifiers [23]. Manteghi et al. also suggested the presence of a secondary porous structure formed by aggregation of primary nanostructures [17]. Another very useful technique for the characterization of cobalt oxide and its precursors is Fourier Transform Infrared spectroscopy (FTIR) spectroscopy. The appearance of characteristic infrared absorption bands of cobalt precursor and final product obtained from thermal decomposition of the precursor validates their formation. The IR spectrum of cobalt oxide exhibits two major bands at ~570 cm−1 (ν1) and ~670 cm−1 (ν2) (Figure 2a). The first band (ν1) is associated with the Co3+ vibration in the octahedral hole and the second band (ν2) is attributed to the Co2+ vibration in the tetrahedral hole, which confirms the formation of the Co3O4 spinel [12, 17, 23, 24, 48, 49]. Raman spectroscopy has also been utilized for the confirmation of Co3O4 formation. Typically, five Raman bands at 198, 484, 522, 622 and 694 cm−1 are visible in the range 100–800 cm−1, which correspond, respectively, to the F12g, Eg, F22g, F32g and A1g modes of crystalline Co3O4 (Figure 2b). F2g and Eg modes are associated with the vibration of tetrahedral and octahedral sites, whereas the high-frequency band, A1g mode, is linked to the occurrence of octahedral sites [14, 15, 20–22, 25].
Figure 2.
Typical (a) FTIR [17] and (b) Raman [22] spectra of Co3O4 nanostructures.
Τhe surface chemical status and composition of the nanomaterials can be investigated by means of X-ray photoelectron spectroscopy (XPS). According to XPS results, the Co2p spectrum is decomposed into two distinct peaks and two weak satellites (Figure 3a). The two spin orbit doublets assigned to cobalt oxides located at 780.8 and 795.9 eV can correspond to Co2p(3/2) and Co2p(1/2), respectively. The spin orbit doublet of Co2p(3/2) can be deconvoluted into two peaks at 780.8 and 782.3 eV, which are attributed to Co3+2p(3/2) and Co2+2p(3/2) configurations, respectively. The Co2p(1/2) spin orbit doublet can also be deconvoluted into two distinct peaks located at binding energies of 795.8 and 797.4 eV and are assigned to Co3+2p(1/2) and Co2+2p(1/2), respectively. The energy difference of 15.1 eV between Co2p(3/2) and Co2p(1/2) splitting is characteristic of the Co3O4 cubic phase. The presence of the two satellite peaks (Cosat.) in the vicinity of the two spin orbit doublets, at binding energies of 788.2 and 804.8 eV, further demonstrates the existence of cobalt oxides [22, 55]. The XPS spectrum of O1s presented in Figure 3b demonstrates a peak at 530.0 eV attributed to lattice oxygen of Co3O4 (Olatt., O2−) and another one at 531.0 eV associated with adsorbed oxygen onto surface oxygen vacancies and oxygen-containing groups such as hydroxyl species. The additional peak at 532.1 eV can be attributed to physical and chemical adsorption of water on the surface of defects (Oadsorbates) and apparently is not always present in O1s spectra [22, 55].
Figure 3.
XPS spectra of (a) Co2p region and (b) O1s region [55].
Reducibility and acidity-basicity are important properties affecting material behavior in a specific application. Temperature programmed reduction (TPR) of Co3O4 nanoparticles shows two main peaks. The first peak is located at 250–360°C and is assigned to reduction of Co3+ to Co2+ with the concomitant phase change to CoO and the second peak appears at 350–473°C corresponding to reduction of Co2+ to Co0. Peak temperature deviations in TPR might be due to structural variations of Co3O4 nanoparticles (particle size and faceting) and TPR protocols [2, 14, 20–22]. The acidic properties of Co3O4 nanoparticles have been studied by NH3-TPD. Abdelkader et al. performed NH3-TPD on Co3O4 pre-reduced at 400°C for 1 h and reported that the TPD profile contained two peaks, at 104 and 240°C, indicating the presence of two acidic sites [14]. de Rivas et al. carried out NH3-TPD experiments on Co3O4 nanomaterials pretreated in a O2/He stream at 500°C and observed two ammonia desorption peaks at 190–200°C and 300–305°C as well as a shoulder at 250°C. They concluded that the peak at low temperature could be associated with weak acidic sites and the peak at high temperature with strong acidic sites [20]. In addition to physicochemical characterization of cobalt nanoparticles, some researchers have studied the optical, electrical and magnetic characteristics of the synthesized nanomaterials by means of UV-Vis-NIR Spectrometry [4], SQUID [4], cyclic voltammetry (CV) [17, 18] and electrochemical impedance spectroscopy (EIS) [17].
6.2. Structure and characterization of CoO nanoparticles
As already mentioned above, there is scarce bibliography concerning the preparation of CoO nanoparticles by thermal decomposition of cobalt-organic precursors. XRD results reported by Bartůněk et al. [5] and Manouchehri et al. [12] showed the presence of a face-centered cubic phase with cell parameter α = 4.26 Å and space group F33m [12]. In the FTIR spectrum, the appearance of a broad band at 450 cm−1 verified the formation of cubic CoO. According to TEM the as-prepared CoO consisted of two types of structures, small nanoparticles and nanorods [12]. Shen et al. claimed that the CoO nanoparticles exhibited quasi-spherical shape and their measured—from TEM micrographs—average particle size was 18 nm [16]. Chen et al. reported on flower-like CoO nanoparticles with an average particle size of 50 nm [27]. In some cases, synthesis of Co3O4 nanoparticles was accompanied by the formation of CoO or metallic cobalt as impurities. Pursuant to XRD results face-centered cubic (space group: F33m) [23], monoclinic (space group: C2/m) [23] and tetragonal [9] crystal systems were reported.
6.3. Structure and characterization of metallic Co nanoparticles
Ganguly et al. produced pure metallic Co nanoparticles confirmed by XRD results with average size, as measured by TEM, between 10 and 40 nm [13]. Co composites were also synthesized by Semenov et al. containing, according to XRD data, metallic Co (hexagonal symmetry, unit cell parameters: а = 2.506 Å, с = 4.071 Å) and CoO as admixtures in the main phase of Co3O4 [9].
6.4. Structure and characterization of mixed metal-oxide nanoparticles
Dippong et al. synthesized CoFe2O4 nanoparticles and concluded that single phase cubic spinel CoFe2O4 can be produced at all temperatures initiating from 1,3-propanediol whereas, when initiating from 1,2-ethanediol and 1,2-propanediol elevated temperatures are required. The degree of CoFe2O4 crystallization increased with the increase of calcination temperature. The appearance of the intense, symmetric band at 560–585 cm−1 in the FTIR spectra, characteristic of the CoFe2O4 phase, confirmed its formation, while, TEM results revealed—in accordance with XRD—the presence of CoFe2O4 as nearly spherical nanoparticles with dimensions varying with calcination temperature between 8 and 20 nm [11]. Another publication from the same group focused on the influence of Co/Fe ratio on the oxide phases in CoFe2O4 nanoparticles and proved the dependence of nanoparticle size on sample composition (Fe and Co content) and calcination temperature. The diameter of the as-synthesized nanoparticles ranged between 12 and 88 nm and according to TEM micrographs, the spherical nanocrystallites showed an agglomerated conformation [56]. Similar work has been conducted by Stefanescu et al., who concluded that the average particle size of the nanoparticles estimated from XRD varied in the range 10–19 nm [32]. Diodati et al. synthesized CoFe2O4 and carried out in-situ temperature-dependent XRD of the oxalate precursors and showed that the XRD patterns of the spinel phase began to be visible at 773–873 K whereas they became sharp and distinct at 1073–1173 K. The crystallite size calculated by means of XRD and TEM was 23 nm (calcination at 873 K) and 185 nm (calcination at 1173 K). Furthermore, TEM micrographs showed that cobalt ferrite nanoparticles retained their identity and size but they had a tendency to form agglomerates. According to XPS and Mössbauer results, the as-synthesized compounds contained surface iron in oxidation state (III) and not in (II). The TPR result showed that the reduction process took place at 700–1173 K and resulted in the reduction of Co(II) and Fe(III) cations to a metallic state [30]. In addition, some researchers have studied the synthesis of CoFe2O4 embedded in SiO2 and according to XRD results the formation of CoFe2O4 spinel phase is affected by various factors, that is, annealing temperature, percentage of silica matrix, the precursor type, etc. For instance, Dippong et al. have shown that the nanocrystallite size and crystallinity increased with increase of CoFe2O4 and decrease of SiO2 content [34], with the use of longer chain precursors [31] and the increase of the annealing temperature [36]. The diameter of CoFe2O4 nanoparticles, calculated by means of XRD and TEM, ranged between 8 and 32 nm depending on the parameters mentioned above and according to SEM images they were spherical and formed irregular agglomerations [31, 34, 35]. Amiri et al. synthesized CoFe2O4 nanoparticles dispersed in a SiO2 matrix by thermal decomposition of iron-cobalt-carboxylates (maleate, malonate, trimesate and ascorbate) and according to XRD patterns, the thermal decomposition of iron-cobalt trimesate precursor led to the formation of pure cubic spinel CoFe2O4 with a crystallite size of 7 nm. The formation of the CoFe2O4 phase was also confirmed by FTIR spectra due to the appearance of the characteristic bands at 469 and 694 cm−1. FE-SEM analysis showed irregularly shaped nanoparticles with an average size of 36 nm (Fe-Co-malonate), 38 nm (Fe-Co-ascorbate) and 27 nm spherical nanoparticles with (Fe-Co-trimesate) and 37 nm (Fe-Co-maleate). All nanoparticles formed agglomerations according to SEM images [36]. Another nanomaterial prepared using thermal decomposition of the corresponding carboxylate precursors was Co1-xZnxFe2O4. Muntean et al. concluded by means of XRD that the as-synthesized nanomaterials consisted of the cubic spinel phase Co1-xZnxFe2O4 and impurities (CoFe2O4, ZnFe2O4) except for the thermal decomposition at 1000°C, where Co0.5Zn0.5Fe2O4 ferrite was obtained as a single, well crystallized phase. The increase in annealing temperature increased the crystallinity and the crystallite size of the nanoparticles. The formation of mixed spinel structure was also confirmed by FTIR spectra due to the presence of characteristic bands at 400 and 600 cm−1 which indicate the anion-cation interaction in octahedral and tetrahedral voids. The average crystallite size varied between 11 and 81 nm depending on the annealing temperature [37]. Similar experiments performed by Stefanescu et al. led to particles with average crystallite size in the range 7–33 nm due to the lower annealing temperature (up to 600°C instead of 1000°C in Ref. [37]) [38].
Mixed cobalt-manganese oxides were investigated by Papadopoulou et al. [6–8]. They employed in-situ XRD to identify the evolving crystalline phases at various stages of pyrolysis of cobalt-manganese gluconate or fumarate precursors and concluded the formation of MnO and metallic Co phases at 550°C due to the thermal decomposition of the fumarate precursor, whereas the decomposition of gluconate precursor above 200°C did not lead to the formation of crystalline phases before 650°C. Same results were obtained by XRD measurements over passivated samples originated from fumarate salts. Thus, the thermal decomposition of both fumarate and gluconate precursors led to the formation of reduced Co-MnO phases in a single step, due to a carbothermal reaction that took place between residual carbon and Co2+ ions. Additionally, the specific surface area of all samples obtained from fumarate precursor ranged between 200 and 220 m2 g−1 regardless of the pyrolysis temperature, due to the presence of residual carbon in the materials which stabilized their porous structure and prevented extensive sintering of MnO and Co crystallites. Furthermore, the same research group synthesized Co-Mn spinel oxide via oxidative treatment of fumarate precursors and the calcined samples had considerably smaller surface area than pyrolyzed ones in the range of 21–35 m2 g−1 [6–8]. Faure et al. synthesized CoxMn3-xO4 (0 ≤ x ≤ 3) by thermal decomposition of oxalate precursor and concluded that the oxides with x < 0.9 are amorphous, while for x > 0.9 all the nanomaterials had a cubic spinel structure. According to TEM and XRD results, the crystallite size ranged between 6 (x = 1.6) and 16 (x = 3) nm. Regarding textural properties, the BET surface area and the pore volume were the highest for x = 2 (SBET = 270 m2 g−1, pore volume = 0.48 cm3 g−1) whereas further increase of cobalt content was associated with a decrease of surface area and pore volume [39].
The structure and physicochemical characteristics of cobalt aluminate (CoAl2O4) nanomaterials were investigated by means of XRD, FTIR, TEM and SEM. Wang et al. synthesized CoIICoIIIxAl2−xO4 (x = 0–2) and reported that nanomaterials had spinel cubic structure (Fd3m) and that their crystallite size ranged between 9 and 51 nm depending on Co/Al ratio and pyrolysis temperature. Their formation was further validated by FTIR spectroscopy from the appearance of the characteristic vibrational bands of CoAl2O4 (572 and 668 cm−1). According to SEM images the spinel samples were agglomerated in large particles with irregular shape. The BET surface area was 22–69 m2 g−1 depending on annealing temperature [40]. Gingasu et al. investigated the physicochemical properties of CoCr2O4 nanomaterials synthesized by thermal decomposition of tartrate and gluconate precursors. The reflections of XRD patterns could be indexed to the face-centered cubic cell with the Fd3m space group and the average crystallite size obtained from tartrate and gluconate precursors was 14–18 and 21 nm, respectively. According to SEM and TEM micrographs, the particle size of CoCr2O4 obtained from tartrate was in the range 13–35 nm (depending on annealing temperature), while CoCr2O4 obtained from gluconate was in the range 16–28 nm showing in each case well-faceted pyramidal or bipyramidal geometry. CoCr2O4 from gluconate precursor formed spherical aggregates with an average size 200–400 nm. The formation of cobalt chromite nanomaterials was confirmed by the presence of sharp and intense bands in the range 615–640 and 500–530 cm−1 in FTIR spectra, which are characteristic of Cr-O bonds. According to Raman spectra, the spinel type CoCr2O4 has a cubic symmetry where the Co2+ and Cr3+ ions occupy the tetrahedral and octahedral sites, respectively. Furthermore, the nitrogen adsorption isotherms were of IV type with a H3 hysteresis loop, characteristic for mesoporous materials. The BET surface area and pore parameters for tartrate-derived CoCr2O4 were SBET = 15–51 m2 g−1, pore volume = 0.11–0.24 cm3 g−1 and average pore diameter = 21–32 nm, whereas for gluconate-derived CoCr2O4 were 17–42 m2 g−1, 0.15–0.21 cm3 g−1 and 21–34 nm, respectively [41]. Darbar et al. synthesized MgCo2O4 by oxalate decomposition and XRD patterns were indexed to the standard cubic structure with Fd3m space group. The SEM images revealed the agglomeration of MgCo2O4 nanoparticles and the BET surface area was measured in the range 4–22 m2 g−1 depending on calcination temperature [42]. Kim et al. produced NiCo2O4 aggregates by oxalate decomposition and the XRD pattern confirmed the formation of cubic spinel NiCo2O4 phase with minor additional impurities (NiO). SEM micrographs showed the presence of various morphologies, such as micro flowers and rod shapes and according to TEM images each microstructure consisted of aggregates of spherical metal-oxide nanoparticles with diameter between 20 and 100 nm [43]. Seyfi et al. reported on the synthesis of LaCoO3 perovskite catalysts with specific surface area of 5 m2 g−1 [44]. On the other hand, Gabal et al. produced purely trigonal ilmenite CoTiO3 by thermal treatment of cobalt oxalate-TiO2 precursor. They concluded that at high temperature (1000°C), CoTiO3 with rhombohedral symmetry (space group R-3 (148)) was formed. According to TEM images, the nanomaterial showed weak agglomeration with heterogeneous morphology in both shape and dimensions and exhibited a larger grain size, 300 nm, compared to that estimated from Scherrer’s equation, 209 nm, due to the agglomeration nature of the nanoparticles as observed from the TEM micrograph. In addition, the specific surface area of the sample was 30 m2 g−1 and the adsorption isotherm was classified to type II, characteristic for macroporous adsorbents and had very small hysteresis loop [45].
6.5. Structure and characterization of supported cobalt oxide nanoparticles
The results from XRD analysis of cobalt compounds supported on carbonaceous carriers differ depending on the nature of the compound (Co3O4, CoO, Co) but in all cases reflections corresponding to the lattice planes of graphitic materials have been observed. The reflections due to cobalt/cobalt oxide nanoparticles were similar to those mentioned above for unsupported materials or in some cases they were not detected at all. It is obvious that an increase in the carbon content leads to an increase of the graphitic diffraction peaks and simultaneous decrease of cobalt/cobalt oxide peaks. Additionally, with increasing calcination temperature, the diffraction peaks for cobalt/cobalt oxide became sharper in contrast to those for carbon, indicating that the crystallinity of cobalt-based nanoparticles increased and graphite content decreased due to its partial oxidation [47]. According to SEM and TEM micrographs, cobalt-based nanoparticles were spherical, coated with carbon and dispersed in the carbon matrix [54], uniformly distributed on carbon layered structures with particle size of 5–30 nm [53], supported on carbon with random size distribution in the range from 1 to 32 nm [50], embedded in carbon with average particle size of 8–10 nm [51] and encapsulated within carbon nanotubes with an average particle size of 50 nm [52]. N2 adsorption-desorption isotherms of the as-synthesized nanocomposites exhibited the type IV isotherm with a H3-type hysteresis loop, demonstrating the mesoporous nature of the materials, while the textural properties of the materials varied widely (SBET = 76–365 m2 g−1, pore volume = 0.15–0.96 cm3 g−1, average pore size = 1.5–20 nm) [50, 52–54]. However, Zhou et al. observed a N2 adsorption isotherm of type V with a H3-type hysteresis loop, while the specific surface area ranged between 160 and 375 m2 g−1, the pore volume was 0.58–0.98 cm3 g−1 and the average pore size varied from 4.8 to 6.9 nm depending on the calcination temperature [51]. In many publications, electrical and magnetic properties have been investigated due to the potential use of the as-synthesized materials in Li-ion batteries and as electrocatalysts [47, 52–54].
7. Applications of cobalt-based nanoparticles
The structure and physicochemical characteristics of cobalt-based nanomaterials make them suitable candidates as catalysts for various processes, that is, alcohol reforming, Fischer-Tropsch, oxidation of organic compounds and CO, as oxygen electrocatalysts and as electrode materials in lithium-ion batteries.
There has been a significant effort to decrease the dependence on non-renewable fossil fuels and move toward sustainable energy carriers, such as hydrogen derived from renewable sources. H2 is considered to be the energy carrier of the future and the use of liquid bio-fuels, such as ethanol and methanol, as hydrogen carriers is an attractive option. Thus, H2 production from alcohol steam reforming has been of great interest and has been extensively investigated. Since alcohol reforming is a catalytic process, various catalytic systems have been tested aiming at optimization of their efficiency. Among them, cobalt-based catalysts are promising candidates. Papadopoulou et al. prepared Co-MnO catalysts by pyrolytic decomposition of the corresponding fumarate and gluconate salts and examined them in methanol and ethanol reforming. They concluded that catalysts with the highest cobalt loading were the most active both in methanol and ethanol reforming. The utilization of fumarate-derived Co-MnO catalysts led to complete methanol conversion at 375–400°C (high-temperature methanol reforming compared to copper-based catalysts), while complete ethanol conversion was achieved at 480°C (low-temperature ethanol reforming compared to noble-metal catalysts). Thus, reforming of both alcohols took place under comparable conditions at temperatures in the range of 400–450°C. The advantages of the proposed method of catalyst preparation were the formation of the reduced active state of the catalysts in a single step and the existence of residual carbon, which hindered sintering and excessive particle growth under synthesis and reaction conditions [6–8]. Abdelkader et al. studied the catalytic activity of Co3O4, Fe2O3 and corresponding mixed Co-Fe in the steam reforming of ethanol and concluded that the mixed Co-Fe sample exhibited higher H2 yield, greater selectivity to CO and CO2 and reduced by-product formation compared to pure Co3O4, Fe2O3 and physical Co-Fe mixture [14].
Rechargeable lithium-ion batteries (LIBs) are the most utilized energy storage devices for portable electronics and one of the most promising electrode materials are cobalt-based nanomaterials in place of carbon. Novel porous Co3O4 architectures [18, 19], MgCo2O4 nanomaterials [42], Co3O4/graphite composites [47], cobalt-based nanoparticles embedded in nitrogen-doped nanotubes [52] and carbon-coated Co3O4 nanoparticles [54] have been studied regarding their electrochemical performance. Briefly, Yuan et al. reported on the performance of Co3O4 polyhedral architectures and showed that they exhibited high discharge capacities for many discharge/charge cycles, due to their porous structure [18]. Yuan et al. synthesized nanosized Co3O4 and concluded that the advantage of this material over carbon was due to its higher capacity per unit volume (7.5 times in comparison to carbon) and that the particle size affected its electrochemical properties (the optimum average particle size was 37 nm) [19]. Guo et al. studied the electrochemical properties of Co3O4/graphite composites and showed that the reversible capacity increased with decrease in graphite content and increase in the calcination temperature, while cycling stability decreased dramatically with decrease in graphitic content [47]. Khan et al. reported on the excellent performance of cobalt oxide nanoparticles embedded in nitrogen-doped carbon nanotubes, which is attributed to the nitrogen doping of carbon nanotubes, the strong interaction between the encapsulated cobalt oxide nanoparticles with the carbon nanotubes, the porosity and the specific surface area of the nanomaterial [52]. In addition, Qiu et al. investigated the electrochemical performance of carbon-coated Co3O4 nanoparticles in comparison to bare Co3O4 electrode and concluded that the superior electrode performance of the first was attributed to better dispersion and to the thin carbon shell coating of the nanoparticles on the electrode surface [54].
Lu et al. showed that the utilization of Co-MOFs for the fabrication of metallic Co nanoparticles embedded in nitrogen-doped porous carbon layers led to the production of an efficient electrocatalyst with bifunctional activities toward oxygen reduction and evolution reactions (ORR, OER) in alkaline media due to nitrogen doping and embedded cobalt nanoparticles in the carbon structure [53].
Concerning environmental catalysis, the strict environmental legislation for pollutant emissions and the high-cost of noble-metal catalysts has shifted interest toward the production of effective transition metal-oxide catalysts. Cobalt-based nanomaterials, such as nanocrystalline Co3O4, Co-Ce composite oxide, CoFe2O4 and Co-Mn oxide spinels have been synthesized by thermal decomposition of organic precursors and studied in various pollutant abatement processes. de Rivas et al. have examined nanocrystalline Co3O4 catalysts in the gas-phase oxidation of chlorinated short chain alkanes and reported on their enhanced catalytic behavior as they exhibited high conversion to deep oxidation products (CO2, HCl, Cl2) at low temperatures with excellent selectivity to CO2 and resistance to deactivation [15, 20]. Similar experiments have been conducted by Wang et al. using Co-Ce catalysts [22]. Liu et al. have demonstrated the excellent activity and stability of Co3O4-based catalysts for propane catalytic combustion [21]. Faure et al. synthesized Co-Mn-oxide spinel catalysts and concluded that their high activity for CO oxidation was correlated to both their surface area and cobalt concentration. Among the synthesized nanomaterials, Co2,3Mn0,7O4 exhibited higher activity than cobalt oxide catalysts [39]. Co3O4 nanoparticles [48] and LaCoO3 nano-perovskite [44] catalysts were also investigated for CO oxidation reaction and exhibited good structural and chemical stability and high activity. Additionally, Ashouri et al. employed MOF-derived Co3O4 for the catalytic oxidation and epoxidation of olefins and reported that the catalyst showed good catalytic stability and reusability [49]. Diodati et al. synthesized and used CoFe2O4 in the catalytic oxidation of methane and concluded that the catalytic reaction took place at lower temperature (by about 300 K) in comparison to the uncatalyzed reaction while the cobalt ferrite catalyst exhibited good stability [30]. Gingasu et al. synthesized cobalt chromite catalysts via thermal decomposition of tartrate and gluconate precursors and reported that gluconate-derived CoCr2O4 was the best catalyst for total oxidation of methane exhibiting high activity and CO2 selectivity [41]. Co nanoparticles embedded in mesoporous nitrogen-doped carbon were investigated by Zhou et al. for the reductive amination of carbonyl compounds with nitro compounds by transfer hydrogenation with formic acid and found them to be active and selective with excellent yields for secondary amines [51]. Another reported application of cobalt-based nanoparticles is in water treatment for the removal of dye pollutants. Advanced oxidation processes and especially Fenton reactions are considered to be among the most feasible pollutant degradation technologies [16, 55].
One of the most significant applications of cobalt nanomaterials in catalysis, is in Fischer-Tropsch synthesis. The Fischer-Tropsch process targets the production of synthetic liquid fuels using coal, natural gas and biomass and hydrogen derived from renewable electricity as feedstocks. Cobalt-based catalysts have been employed to a great extent since they have high selectivity for long chain hydrocarbons and low selectivity for the water-gas shift reaction and they are cost-effective. The reducibility, cobalt dispersion and loading and nanoparticle structure are some of the parameters that affect the catalytic activity and selectivity. Pei et al. synthesized fully reduced carbon-supported cobalt catalysts by pyrolysis of Co-MOF-71 precursor and showed that the as-prepared catalysts had extremely high Co site density, high activity and selectivity with diesel fuels being the main products and high C5+ space-time yields in comparison to conventional cobalt catalysts [50].
8. Conclusions
Nanostructured cobalt-based materials have attracted considerable interest due to their multiple applications in various fields, like catalysis, electronics, electrochemical devices, etc. Among the synthesized cobalt nanomaterials, Co3O4 is by far the main nanostructure been reported in the literature, whereas fewer studies have been made regarding CoO, metallic Co, mixed metal-oxide nanoparticles or other types of cobalt-based nanomaterials. A great number of methods have been employed for their synthesis with the thermal decomposition of organic precursors bearing noteworthy advantages as, for instance, simplicity, short processing time and cost-effectiveness. Carboxylate salts (e.g. oxalate, citrate, etc.) as well as metal-organic frameworks (MOFs) are utilized as organic precursors for the production of cobalt oxides, metallic cobalt, mixed cobalt oxides and supported cobalt-based nanomaterials. The nature of organic precursor, the precursor synthesis method, the cobalt content, the combination with other elements, the treatment schedule and temperature and the type of the gaseous atmosphere (oxidizing, inert, reducing) prevailing during heating are some of the factors that affect the physical and chemical properties of the final composite. The relevant nanomaterials have been extensively characterized and analyzed using various techniques (XRD, FTIR, SEM, TEM, XPS, Raman, etc.) and accounts have been reported on their novel properties in comparison to bulk solids. A non-exhaustive list of potential applications of such cobalt-based nanomaterials includes catalysts for Fischer-Tropsch process, alcohol reforming, oxidation of organic compounds and CO, oxygen electrocatalysts and anode materials for Li-ion batteries.
\n',keywords:"pyrolysis, carboxylates, thermal treatment, cobalt oxides, cobalt, Co3O4, nanoparticles, nanomaterials",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/57559.pdf",chapterXML:"https://mts.intechopen.com/source/xml/57559.xml",downloadPdfUrl:"/chapter/pdf-download/57559",previewPdfUrl:"/chapter/pdf-preview/57559",totalDownloads:1571,totalViews:658,totalCrossrefCites:0,totalDimensionsCites:2,hasAltmetrics:0,dateSubmitted:"April 12th 2017",dateReviewed:"September 12th 2017",datePrePublished:null,datePublished:"December 6th 2017",dateFinished:null,readingETA:"0",abstract:"Development of efficient and low-cost methods for the production of cobalt and cobalt oxide nanoparticles is of great interest. Such nanoparticles are typically prepared via transformation of precursors under controlled conditions. In the case of organic precursors, the production of said nanoparticles takes place through thermal decomposition of the organic moiety. The decomposition pathway of the precursor is greatly dependent on the type (i.e. inert, reducing or oxidizing) of the gaseous atmosphere prevailing during heating, as well as on the heating schedule itself. The characteristics of the organic group have also an important influence on the structure of the final material. The goal of the current work is to present a comprehensive review of the research work focusing on the synthesis of cobalt-based nanomaterials from activation of organic precursors.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/57559",risUrl:"/chapter/ris/57559",book:{slug:"cobalt"},signatures:"Maria Smyrnioti and Theophilos Ioannides",authors:[{id:"208984",title:"Dr.",name:"Theophilos",middleName:null,surname:"Ioannides",fullName:"Theophilos Ioannides",slug:"theophilos-ioannides",email:"theo@iceht.forth.gr",position:null,institution:{name:"Foundation for Research and Technology Hellas",institutionURL:null,country:{name:"Greece"}}},{id:"218366",title:"B.Sc.",name:"Maria",middleName:null,surname:"Smyrnioti",fullName:"Maria Smyrnioti",slug:"maria-smyrnioti",email:"mariasmyrnioti@gmail.com",position:null,institution:{name:"University of Patras",institutionURL:null,country:{name:"Greece"}}}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Cobalt and cobalt oxide nanoparticles from carboxylates",level:"1"},{id:"sec_2_2",title:"2.1. Cobalt oxide nanoparticles from oxalate precursors",level:"2"},{id:"sec_3_2",title:"2.2. Cobalt oxide nanoparticles from citrate precursors",level:"2"},{id:"sec_4_2",title:"2.3. Cobalt and cobalt oxide nanoparticles from malonate precursors",level:"2"},{id:"sec_5_2",title:"2.4. Cobalt and cobalt oxide nanoparticles from succinate precursors",level:"2"},{id:"sec_6_2",title:"2.5. Cobalt oxide nanoparticles from tartrate precursors",level:"2"},{id:"sec_7_2",title:"2.6. Cobalt oxide nanoparticles from other carboxylate precursors",level:"2"},{id:"sec_9",title:"3. Mixed metal-oxide nanoparticles from carboxylate precursors",level:"1"},{id:"sec_9_2",title:"3.1. Spinel mixed metal-oxide nanoparticles from carboxylate precursors",level:"2"},{id:"sec_10_2",title:"3.2. Perovskite mixed metal nanoparticles from carboxylate precursors",level:"2"},{id:"sec_11_2",title:"3.3. Ilmenite mixed metal-oxide nanoparticles from carboxylate precursors",level:"2"},{id:"sec_13",title:"4. Supported cobalt oxide from carboxylate salts",level:"1"},{id:"sec_14",title:"5. Cobalt-based nanomaterials from metal-organic frameworks (MOFs)",level:"1"},{id:"sec_15",title:"6. Structure and characterization of cobalt-based nanoparticles",level:"1"},{id:"sec_15_2",title:"6.1. Structure and characterization of Co3O4 nanoparticles",level:"2"},{id:"sec_16_2",title:"6.2. Structure and characterization of CoO nanoparticles",level:"2"},{id:"sec_17_2",title:"6.3. Structure and characterization of metallic Co nanoparticles",level:"2"},{id:"sec_18_2",title:"6.4. Structure and characterization of mixed metal-oxide nanoparticles",level:"2"},{id:"sec_19_2",title:"6.5. Structure and characterization of supported cobalt oxide nanoparticles",level:"2"},{id:"sec_21",title:"7. Applications of cobalt-based nanoparticles",level:"1"},{id:"sec_22",title:"8. Conclusions",level:"1"}],chapterReferences:[{id:"B1",body:'Thangavelu K, Parameswari K, Kuppusamy K, Haldorai Y. A simple and facile method to synthesize Co3O4 nanoparticles from metal benzoate dihydrazinate complex as a precursor. Materials Leters. 2011;65:1482-1484'},{id:"B2",body:'Luisetto I, Pepe F, Bemporad E. Preparation and characterization of nano cobalt oxide. Journal of Nanoparticle Research. 2008;10:59-67'},{id:"B3",body:'Stefanescu O, Davidescu C, Muntean C. Preparation and characterization of cobalt oxides nanoparticles starting from Co(II) carboxylate precursors. Journal of Optoelectronics and Advanced Materials. 2015;17:991-996'},{id:"B4",body:'Thota S, Kumar A, Kumar J. Optical, electrical and magnetic properties of Co3O4 nanocrystallites obtained by thermal decomposition of sol-gel derived oxalates. Materials Science and Engineering B. 2009;164:30-37'},{id:"B5",body:'Bartůněk V, Huber Š, Sedmidubský D, Sofer Z, Šimek P, Jankovský O. 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Highly Active and Selective Co-Based Fischer-Tropsch Catalysts Derived from Metal–Organic Frameworks. AICHE Journal. 2017;63(7):2935-2944'},{id:"B51",body:'Zhou P, Zhang Z, Jiang L, Yu C, Lv K, Sun J, Wang S. A versatile cobalt catalyst for the reductive amination of carbonyl compounds with nitro compounds by transfer hydrogenation. Applied Catalysis. B, Environmental. 2017;210:522-5329'},{id:"B52",body:'Khan IA, Nasim F, Choucair M, Ullah S, Badshah A, Nadeem MA. Cobalt oxide nanoparticles embedded N-CNTs: Lithium ion battery applications. RSC Advances. 2016;6(2):1129-1135'},{id:"B53",body:'Lu H, Zhang H, Liu R, Zhang X, Zhao H, Wang G. Macroscale cobalt-MOFs derived metallic Co nanoparticles embedded in N-doped porous carbon layers as efficient oxygen electrocatalysts. Applied Surface Science. 2017;392:402-409'},{id:"B54",body:'Qiu B, Guo W, Liang Z, Xia W, Gao S, Wang Q, Yu X, Zhao R, Zou R. Fabrication of Co3O4 nanoparticles in thin porous carbon shells from metal-organic frameworks for enhanced electrochemical performance. RSC Advances. 2017;7:13340-13346'},{id:"B55",body:'Huang Q, Zhang J, He Ζ, Shi P, Qin X, Yao W. Direct fabrication of lamellar self-supporting Co3O4/N/C peroxymonosulfate activation catalysts for effective aniline degradation. Chemical Engineering Journal. 2017;313:1088-1098'},{id:"B56",body:'Dippong T, Levei EA, Borodi G, Goga F, Tudoran LB. Influence of Co/Fe ratio on the oxide phases in nanoparticles of CoxFe3–xO4. Journal of Thermal Analysis and Calorimetry. 2015;119:1001-1009'}],footnotes:[],contributors:[{corresp:null,contributorFullName:"Maria Smyrnioti",address:null,affiliation:'
Foundation for Research & Technology – Hellas, Institute of Chemical Engineering Sciences (FORTH/ICE-HT), Patras, Greece
Department of Chemistry, University of Patras, Greece
Foundation for Research & Technology – Hellas, Institute of Chemical Engineering Sciences (FORTH/ICE-HT), Patras, Greece
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Lackner and Jerzy Morgiel",authors:[{id:"61319",title:"Dr.",name:"Juergen M.",middleName:null,surname:"Lackner",fullName:"Juergen M. Lackner",slug:"juergen-m.-lackner"},{id:"99492",title:"Dr.",name:"Lukasz",middleName:null,surname:"Major",fullName:"Lukasz Major",slug:"lukasz-major"},{id:"130138",title:"Prof.",name:"Jerzy",middleName:null,surname:"Morgiel",fullName:"Jerzy Morgiel",slug:"jerzy-morgiel"}]},{id:"34885",title:"Deposition and Characterization of Platinum and Palladium Nanoparticles on Highly Oriented Pyrolytic Graphite",slug:"deposition-and-characterization-of-platinum-and-palladium-nanoparticles-on-highly-oriented-pyrolytic",signatures:"Nora Elizondo, Donald H. Galvan, Lorena Alvarez-Contreras, Ran Tel-Vered, Arquímedes Cruz-Lopez, Ricardo Obregon, Sergio Belmares-Perales, Manuel Garcia-Mendez,\r\nOdilon Vazquez-Cuchillo and Antonio A. Zaldivar",authors:[{id:"72518",title:"Dr.",name:"Manuel",middleName:null,surname:"Garcia-Mendez",fullName:"Manuel Garcia-Mendez",slug:"manuel-garcia-mendez"},{id:"99818",title:"Prof.",name:"Nora",middleName:null,surname:"Elizondo-Villarreal",fullName:"Nora Elizondo-Villarreal",slug:"nora-elizondo-villarreal"},{id:"108058",title:"Dr.",name:"Ricardo",middleName:null,surname:"Obregon-Guerra",fullName:"Ricardo Obregon-Guerra",slug:"ricardo-obregon-guerra"},{id:"108059",title:"Dr.",name:"Sergio",middleName:null,surname:"Belmares-Perales",fullName:"Sergio Belmares-Perales",slug:"sergio-belmares-perales"},{id:"109435",title:"Dr.",name:"Arquimedes",middleName:null,surname:"Cruz-Lopez",fullName:"Arquimedes Cruz-Lopez",slug:"arquimedes-cruz-lopez"},{id:"109437",title:"Dr.",name:"Odilon",middleName:null,surname:"Vazquez-Cuchillo",fullName:"Odilon Vazquez-Cuchillo",slug:"odilon-vazquez-cuchillo"},{id:"109440",title:"Dr.",name:"Antonio A.",middleName:null,surname:"Zaldivar-Cadena",fullName:"Antonio A. Zaldivar-Cadena",slug:"antonio-a.-zaldivar-cadena"},{id:"109443",title:"Prof.",name:"Donald Homero",middleName:null,surname:"Galvan-Martinez",fullName:"Donald Homero Galvan-Martinez",slug:"donald-homero-galvan-martinez"},{id:"109447",title:"Dr.",name:"Lorena",middleName:null,surname:"Alvarez-Contreras",fullName:"Lorena Alvarez-Contreras",slug:"lorena-alvarez-contreras"},{id:"141548",title:"Dr.",name:"Ran",middleName:null,surname:"Tel-Vered",fullName:"Ran Tel-Vered",slug:"ran-tel-vered"}]},{id:"34886",title:"Ultrastructure and Cell Wall Thickness Modification and Its Detection After Chemical Treatments in Huanglongbing Infected Citrus Plants",slug:"ultrastructures-and-cell-wall-thickness-modification-after-chemical-treatments-in-huanglongbing-infe",signatures:"Hajivand Shokrollah,\r\nThohirah Lee Abdullah and Kamaruzaman Sijam",authors:[{id:"99851",title:"Dr.",name:"Shokrollah",middleName:null,surname:"Hajivand",fullName:"Shokrollah Hajivand",slug:"shokrollah-hajivand"}]},{id:"34887",title:"Ultrastructural Mechanisms of Aposporous Embryo Sac Initial Cell Appearance and Its Developmental Process in Gametophytic Apomicts of Guinea Grass (Panicum maximum)",slug:"ultrastructural-mechanism-of-aposporous-intial-cell-appearance-and-its-developmental-process-in-game",signatures:"Lanzhuang Chen and Liming Guan",authors:[{id:"102161",title:"Dr.",name:"Lanzhuang",middleName:null,surname:"Chen",fullName:"Lanzhuang Chen",slug:"lanzhuang-chen"},{id:"102182",title:"Dr.",name:"Liming",middleName:null,surname:"Guan",fullName:"Liming Guan",slug:"liming-guan"}]},{id:"34888",title:"Cathodoluminescence of Surface Plasmon Induced Light Emission",slug:"cathodoluminescence-of-surface-plasmon-induced-light-emission",signatures:"Naoki Yamamoto",authors:[{id:"125444",title:"Dr.",name:"Naoki",middleName:null,surname:"Yamamoto",fullName:"Naoki Yamamoto",slug:"naoki-yamamoto"}]},{id:"34889",title:"Ulinastatin and Septic Cardiac Dysfunction",slug:"ulinastatin-and-septic-cardiac-dysfunction",signatures:"Jian-Dong Lin and Ming-Rui Lin",authors:[{id:"102852",title:"Dr.",name:"Jiandong",middleName:null,surname:"Lin",fullName:"Jiandong Lin",slug:"jiandong-lin"},{id:"108246",title:"Mr.",name:"Mingrui",middleName:null,surname:"Lin",fullName:"Mingrui Lin",slug:"mingrui-lin"}]},{id:"34890",title:"Morphological Study of HDPE/Clay Hybrids Synthesized by an Alternative Compatibilization Path",slug:"morphological-study-of-hdpe-clay-hybrids-synthesized-by-an-alternative-compatibilization-path",signatures:"Fernanda Elena Monasterio",authors:[{id:"107914",title:"Dr.",name:"Fernanda",middleName:"Elena",surname:"Monasterio",fullName:"Fernanda Monasterio",slug:"fernanda-monasterio"}]},{id:"34891",title:"Ceramic-Metal Joining Using Active Filler Alloy-An In-Depth Electron Microscopic Study",slug:"ceramic-metal-joining-using-active-filler-alloy-an-in-depth-electron-microscopic-study",signatures:"Abhijit Kar and Ajoy Kumar Ray",authors:[{id:"111049",title:"Dr.",name:"Abhijit",middleName:null,surname:"Kar",fullName:"Abhijit Kar",slug:"abhijit-kar"},{id:"116525",title:"Dr.",name:"Ajoy Kumar",middleName:null,surname:"Ray",fullName:"Ajoy Kumar Ray",slug:"ajoy-kumar-ray"}]},{id:"34892",title:"Investigation on Structure and Behaviours of Proton Exchange Membrane Materials by TEM",slug:"investigation-on-structure-and-behaviors-of-proton-exchange-membrane-materials-by-tem",signatures:"Zhe Wang, Chengji Zhao, Hongzhe Ni, Mingyao Zhang and Huixuan Zhang",authors:[{id:"106250",title:"Prof.",name:"Zhe",middleName:null,surname:"Wang",fullName:"Zhe Wang",slug:"zhe-wang"},{id:"121073",title:"Dr.",name:"Chengji",middleName:null,surname:"Zhao",fullName:"Chengji Zhao",slug:"chengji-zhao"},{id:"121074",title:"Dr.",name:"Hongzhe",middleName:null,surname:"Ni",fullName:"Hongzhe Ni",slug:"hongzhe-ni"}]},{id:"34893",title:"In-Situ Mechanical Testing of Nano-Component in TEM",slug:"in-situ-mechanical-testing-of-nano-component-in-tem",signatures:"Takashi Sumigawa and Takayuki Kitamura",authors:[{id:"108983",title:"Dr.",name:"Takashi",middleName:null,surname:"Sumigawa",fullName:"Takashi Sumigawa",slug:"takashi-sumigawa"},{id:"111079",title:"Dr.",name:"Takayuki",middleName:null,surname:"Kitamura",fullName:"Takayuki Kitamura",slug:"takayuki-kitamura"}]}]}]},onlineFirst:{chapter:{type:"chapter",id:"66110",title:"Gold Recovery Process from Primary and Secondary Resources Using Bioadsorbents",doi:"10.5772/intechopen.84770",slug:"gold-recovery-process-from-primary-and-secondary-resources-using-bioadsorbents",body:'\n
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1. Introduction
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In recent years, accompanied by huge consumption of various metals, metal contents or grade of metal ores have become poor and complex. Under such situation, not only poor and complex natural resources but also secondary resources, i.e., various wastes containing valuable metals in low contents, have to be employed as feed materials to recover valuable metals. The typical wastes containing valuable metals are those of spent electric and electronic appliances, i.e., e-wastes.
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For the recovery of valuable metals from such poor and complex feed materials, hydrometallurgical processes are more suitable than pyrometallurgical processes. Hydrometallurgical processes consist of leaching of metals from solid feed materials into aqueous solutions, separation and concentration of the targeted metals from other metals, and final recovery as solid metals of high purity such as ingot metals. For the separation and concentration of the targeted metals, various processes such as precipitation, solvent extraction, ion-exchange including chelating ion-exchange and adsorption have been employed. Of these processes, precipitation and solvent extraction are suitable for the recovery from solutions of high concentration, while adsorption and ion-exchange are suitable from those of low or trace concentration.
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During long operation, solvent extraction reagents, adsorbents, and ion-exchangers gradually deteriorate and finally they are discarded. For example, in the cases of ion-exchange resins, they deteriorate through the formation of many cracks and clogging of micropores of the resins by fine particles present in actual solutions, both of which impede smooth operation using packed columns.
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For the effective separation and concentration in hydrometallurgical processes, high selectivity and high loading capacity for targeted metals are strongly required for solvent extraction reagents and adsorbents. However, the selectivity exhibited by a majority of commercially available ion-exchange resins including chelating resins has not been always satisfactory.
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Ion-exchange resins are plastic beads produced from petroleum. In recent years, environmental pollutions by microplastics have been deeply worried all over the world and big expectations are placed on biodegradable plastics. However, their high production costs prevent their actual employments in various fields.
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In our recent studies, we found that adsorption gels prepared from various kinds of biomass materials including various biomass wastes, i.e., bioadsorbents, exhibit high selectivity and high loading capacity for targeted metals such as hazardous heavy metals and valuable metals. These are prepared from waste wood [1, 2, 3, 4] and straws of rice and wheat [5], spent papers [6, 7, 8, 9, 10], cotton [11], waste seaweeds [12, 13], persimmon tannin [14, 15, 16] or wastes of persimmon [17, 18] and grape [19, 20] rich in tannin compounds, wastes of citrus such as orange [21] and lemon [22], and residue of microalgae after extracting biofuel [23, 24].
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In the present chapter, we introduce the adsorptive recovery of gold from printed circuit boards (PCBs) of spent mobile phones, a typical e-waste, and actual gold ore, a primary resource of gold, as well as that of trace concentration of gold from simulated spent cyanide solutions using some of these bioadsorbents.
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2. Preparation of bioadsorbents for gold recovery
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The bioadsorbents for gold recovery can be easily prepared in a simple manner as schematically shown in Figure 1. Pieces of feed materials of biomass are stirred in boiling concentrated sulfuric acid for about 24 h, where hydroxyl groups contained in the biomass undergo dehydration condensation reactions and polymer chains of the biomass are cross-linked via ether bonds. The solid materials are neutralized using dilute alkali solution and water-washed and then, they are dried in a convection oven and pulverized. Finally, they are sieved to uniform the particle size. The final products are black powder, the particle size of which are less than 0.1 mm.
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Figure 1.
Flow sheet of the preparation of bioadsorbents.
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3. Adsorption behaviors of bioadsorbents for metal ions
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All of the bioadsorbents prepared by the method mentioned above exhibited extraordinary high selectivity only to gold(III) in the adsorption from hydrochloric acid solutions. For example, Figure 2 shows the % adsorption of some metal ions onto bioadsorbent prepared from orange waste (orange juice residue) from various concentrations of hydrochloric acid solution [21], where the % adsorption denotes the percentage of metal ion adsorbed on the adsorbent from aqueous solution and defined by the following equation.
\n\n\n\n\n%\nAdsorption\n=\n\n\nMass of metal\n\nion\n\nadsorbed\n\non\n\nthe adsorbent\n/\nMass of metal\n\nion\n\ninitially present in the aqueous solution\n\n\n×\n100\n=\n\n\n\n\ninitial concentration of the metal\n\nion\n−\nconcentration of the metal\n\nion\n\nafter adsorption\n\n\n/\ninitial concentration of the metal\n\nion\n\n\n×\n100\n\n\n\n\nE1
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Figure 2.
Percentage adsorptions of some metal ions on bioadsorbent prepared from orange waste by treating in boiling concentrated sulfuric acid [21].
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As seen in this figure, only gold(III) is quantitatively adsorbed over the whole concentration range of hydrochloric acid tested, while other metal ions, not only precious metals such as palladium(II) and platinum(IV) but also base metals such as copper(II) and zinc(II), are not practically adsorbed. Similar phenomena were also observed also for all bioadsorbents prepared by the method using boiling concentrated sulfuric acid.
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Figure 3 shows the similar plots in the case of the adsorption on the bioadsorbent of orange waste prepared by means of carbonization at 800°C, for comparison. Although gold(III) is quantitatively adsorbed over the whole concentration range of hydrochloric acid also on this bioadsorbent, considerable amount of platinum(IV) and palladium(II) is also adsorbed at low concentration range in particular; i.e., the selectivity of the carbonized bioadsorbent to gold(III) is inferior to that prepared by using boiling concentrated sulfuric acid.
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Figure 3.
Percentage adsorptions of some metal ions on bioadsorbent prepared from orange waste by means of carbonization at 800°C.
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Figure 4 shows the adsorption isotherm of gold(III), i.e., the relationship between the amount of adsorption of gold(III) and its concentration present in the aqueous solution (0.1 mol/L hydrochloric acid solution) at equilibrium at 30°C, on the adsorbent prepared from orange waste. The amount of adsorption increases with increasing concentration of gold(III) at low concentration range, while it tends to approach a constant value at high concentration range, suggesting the typical Langmuir-type adsorption isotherm. From the constant value, the maximum adsorption capacity for gold(III) on this adsorbent was evaluated as 10.5 mol/kg ( = 2.07 kg gold(III)/kg adsorbent), which is an extraordinarily high value, greater than the weight of the adsorbent. Similarly, very high values of adsorption capacity for gold(III) were observed also for other adsorbent prepared from different kinds of biomass materials. Table 1 shows the maximum adsorption capacities for gold(III) on the adsorbent prepared from various biomass materials and those on other adsorbents reported in some literatures, for comparison.
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Figure 4.
Adsorption isotherm of gold(III) on bioadsorbent prepared from orange waste [21], where q and Ce denote the amount of adsorbed gold(III) and concentration gold(III) present in the aqueous solution at equilibrium, respectively.
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\n\n
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Adsorbent
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Maximum adsorption capacity (g/kg)
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Reference
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\n\n\n
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Cross-linked lignophenol prepared from sawdust of cedar
Maximum adsorption capacities for gold(III) on bioadsorbents we prepared and those reported in some literatures.
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As seen in this table, some of bioadsorbents exhibit much higher adsorption capacity for gold(III) than commercially available adsorbents such as activated carbon and chelating resins.
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Figure 5 shows the image of optical microscope of the bioadsorbent prepared from residue of microalgae after biofuel extraction after adsorption of gold(III). In this photograph, aggregates of elemental gold particles are observed as brilliant yellow lumps, while black particles are bioadsorbents of microalgae. The formation of elemental gold was confirmed also from the observation by X-ray diffraction (XRD) analysis. Similar phenomena were observed also for other bioadsorbents we prepared. From these results, it can be concluded that the adsorbed gold(III) was reduced into elemental gold on the surface of the bioadsorbent and that the extraordinary high adsorption capacity for gold(III) is attributable to the formation of elemental gold particles on these bioadsorbents. Furthermore, it can be concluded that the high selectivity for gold(III) over other metal ions is attributed to the higher oxidation-reduction potential (ORP) for gold(III) than other metal ions; e.g., those of some metal ions are as follows. Au(III): 1.52 V, Pd(II): 0.915 V, Cu(II): 0.340V, Ni(II): −0.257 V, Zn(II): −0.763 V.
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Figure 5.
Image of optical microscope of the bioadsorbent prepared from residue of microalgae after biofuel extraction after adsorption of gold(III).
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The mechanism of adsorptive reduction of gold(III) is shown in Figure 6. Gold(III) present in aqueous solution is adsorbed on the surface of the bioadsorbents and reduced into elemental gold as follows.
Interaction of positively charged gold(III) ion with oxygen atoms of hydroxyl groups and ether oxygen atoms of polysaccharide molecules or tannin compounds contained in bioadsorbents followed by adsorption forming stable five-membered chelate rings. Here, by the cross-linking reactions using boiling concentrated sulfuric acid, structures of polymer chains of polysaccharide and tannin molecules are transformed into those suitable for forming stable five-membered metal chelates.
Reduction of the adsorbed gold(III) ions into elemental or metallic gold particles by the aid of hydroxyl groups that take part in the interaction with the gold(III) ions, releasing hydrogen ions, where the hydroxyl groups are oxidized into carbonyl groups.
Protonation of the carbonyl groups followed by returning back to hydroxyl groups which function again as the adsorption sites.
Aggregation of elemental gold particles into bigger lumps followed by isolation from surface of the bioadsorbents.
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Figure 6.
Mechanism of the cross-linking between polymer chains of cellulose molecules by the aid of concentrated sulfuric acid and that of reductive adsorption of gold(III) on the cross-linked cellulose [25].
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The surface of polysaccharides and tannin compounds cross-linked by the aid of boiling concentrated sulfuric acid functions as catalysts for the reduction reaction of gold(III) ions into elemental gold(0) under acidic conditions.
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Figure 7 shows the effect of pH on the adsorption of gold(III) on the bioadsorbent prepared from orange waste by treating in boiling concentrated sulfuric acid. As seen from this figure, although gold(III) is quantitatively adsorbed at pH less than 6 (acidic condition), no adsorption of gold(III) takes place at pH higher than 8 (basic condition) in accordance with the mechanism mentioned above.
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Figure 7.
Effect of equilibrium pH (pHe) on the % adsorption of gold(III) on the bioadsorbent prepared from orange waste by treating in boiling concentrated sulfuric acid where chloride concentration was maintained constant at 0.1 mol/L.
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Figure 8 shows the effect of solid/liquid ratio, the ratio of dry weight of the added adsorbent to volume of aqueous solution, on the concentration of gold(III) remained in the aqueous solution after the adsorption from 0.25 mol/L hydrochloric acid solution containing 1.05 mg/L gold(IIII) on bioadsorbent prepared from orange waste by treating in boiling concentrated sulfuric acid. As seen in this figure, the concentration of gold(III) is lowered down to as low as 0.02 mg/L (20 ppb) by this bioadsorbent; i.e., about 98% recovery was achieved from such trace concentration of gold(III) solution.
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Figure 8.
Relationship between concentration of gold(III) remained in the aqueous solution after the adsorption on bioadsorbent prepared from orange waste by treating in boiling concentrated sulfuric acid and solid/liquid ratio, the ratio of dry weight of the added adsorbent to volume of aqueous solution.
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The elution or desorption of the adsorbed gold(III) is difficult or nearly impossible using usual elution agents. In such cases, as will be mentioned in the latter section, gold-loaded adsorbents are incinerated leaving solid gold particles in the incineration residues. The bioadsorbents prepared from biomass materials are easy to be incinerated at relatively low temperature compared with commercially available ion-exchange resins, plastic beads produced from petroleum, which is another advantage of bioadsorbents.
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Figure 9 shows the thermogravimetric curves (relationship between percentage decrease in the weight of materials and temperature) of bioadsorbent of microalgae residue after extracting biofuel before and after gold adsorption. As seen from this figure, both samples are completely decomposed at the temperature between 500 and 600°C. In this figure, the difference between red and blue lines at the temperature higher than 600°C corresponds the weight of gold loaded on this bioadsorbent sample.
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Figure 9.
Thermogravimetric curves of the bioadsorbents prepared from microalgae residue after biofuel extraction before (blue line) and after (red line) the adsorption of gold(III) [23].
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4. Recovery of gold from printed circuit boards of spent mobile phones
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As an example of the use of bioadsorbents we prepared, recovery of gold from printed circuit boards (PCBs) of spent mobile phones is introduced in this section.
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Spent home appliances such as mobile phones are dismantled by hand work into various parts to recover various valuables for their reuses as shown in Figure 10.
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Figure 10.
Flow sheet of the dismantling of spent mobile phones.
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Of these dismantled parts, gold and other precious metals such as palladium and platinum are contained in PCBs; i.e., PCBs of spent electronics are typical secondary resources of precious metals. According to the conventional recovery process of precious metals from complex feed materials such as anode slimes of copper and nickel generated in electrorefining processes of these metals which contain many kinds of metals such as gold, silver, palladium, platinum and base metals, they are recovered by repeating dissolution using aqua regia followed by precipitation for many times, which needs tedious long-time operations and high labor costs. In early 1970s, new recovery process was developed and commercialized by INCO [31]. In this process, the feed materials are totally dissolved in hydrochloric acid into that chlorine gas had been blown, abbreviated as chlorine-containing HCl, hereafter. Here, the chlorine gas dissolved in hydrochloric acid solution is converted into hypochlorous acid (HClO) according to the following reaction:
Thus, formed hypochlorous acid functions as a strong oxidation agent, converting solid metals into metal ions, dissolving into hydrochloric acid solution, where the metal ions give rise to stable chloro-complexes interacting with chloride ions; e.g., gold(III) is present as AuCl4−, anionic species. However, because the hypochlorous acid formed by the abovementioned reaction is unstable and is easily converted into hydrochloric acid, the metal recovery from such solutions is actually the same with that from hydrochloric acid solutions.
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In the present work, the sample of spent PCBs was treated in the similar manner using chlorine-containing HCl as schematically shown in Figure 11.
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Figure 11.
Flow sheet for the treatment of spent PCBs in the present work.
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They are incinerated at first at 750°C to extinguish epoxy resin boards on which various parts are placed. Then, the residues are leached using nitric acid solution to remove silver, which impedes the recovery of gold and other precious metals in the latter steps, together with some base metals. The residue of the nitric acid leaching was calcined at 750°C again and leached using chlorine-containing HCl to recover gold and other precious metals. In the present work, the sample of such metal-loaded leach liquor was kindly donated by Shonan Factory of TANAKA KIKINZOKU KOGYO Co. Ltd., Hiratsuka, Japan. The metal concentrations of this sample solution measured by ICP-AES were as follows (mg/L): Au(100), Pd(8), Pb(342), Fe(314), Cu(250), Ni(411), and Zn(41). The total acid concentration measured by acid-base titration was around 3.0 mol/L.
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Figures 12 and 13 show the effect of solid/liquid ratio, the ratio of amount (dry weight) of added bioadsorbent to unit volume of sample leach liquor, on % adsorption of each metal in the case of adsorptive recovery using bioadsorbents of orange waste and cotton prepared by treating in boiling concentrated sulfuric acid, respectively. As seen from these figures, although gold is nearly quantitatively adsorbed, other metals are not practically adsorbed on these bioadsorbents.
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Figure 12.
Effect of solid/liquid ratio on the % adsorption of various metals from leach liquor of chlorine-containing HCl using the bioadsorbent prepared from orange waste by treating in boiling concentrated sulfuric acid.
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Figure 13.
Effect of solid/liquid ratio on the % adsorption of various metals from leach liquor of chlorine-containing HCl using the bioadsorbent of cotton prepared by treating in boiling concentrated sulfuric acid.
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5. Recovery of gold from Mongolian gold ore
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At present, majority of gold has been recovered from gold and silver ores by means of cyanide process developed at the beginning of twentieth century as schematically shown in Figure 14. In this process, pulverized ores are leached using alkaline cyanide solution to extract gold as gold(I)-cyanide complexes according to the following reaction:
Flow sheet of conventional gold recovery process from gold ores using alkaline cyanide solutions.
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The extracted gold(I) as anionic species, AuCN2−, is adsorbed onto activated carbon or strongly basic anion exchange resins, which are termed as CIP and RIP processes, respectively. Because it is difficult to desorb the gold adsorbed onto these adsorbents, these are incinerated at high temperature to recover metallic gold.
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This cyanide process has suffered from some problems as follows:
Strong toxicity of cyanide, which causes serious environmental problems and, consequently, needs some costs for safe operation and environmental protection.
Interference by other coexisting metals or low selectivity over other metals.
Slow dissolution of gold as shown in Table 2 that shows the comparison of dissolution rate of gold by some lixiviants.
Comparison of dissolution rates of gold using some lixiviants [32].
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As alternatives to cyanide leaching, some noncyanide leaching processes such as those using hypochlorous acid, bromine, thiosulfate, and thiourea have been proposed. However, these new processes also suffer from their own drawbacks as follows. Thiourea is known as carcinogen and, additionally, it is expensive and chemically unstable compared to cyanide, while it has a big advantage of much faster dissolution rate of gold than cyanide; that is, it was reported that the dissolution rate of gold using the mixture of 1% thiourea in 0.5% sulfuric acid containing 0.1% ferric ion is over 10-folds faster than that using the mixture of 0.5% sodium cyanide and 0.05% calcium oxide [33].
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Following the recovery of gold from spent PCBs, a typical secondary resource, we attempted to apply the bioadsorbents we prepared to noncyanide leach liquor of actual gold ore (one example of typical primary resources). The sample of the ore was kindly donated by Western Mongolian Metals Co. Ltd., Ulaanbaatar, Mongolia. It was fine powder, the particle size of which was around 75–150 μm and the metal contents (mg/g) were as follows: gold 0.046, platinum 0.018, aluminum 0.694, iron 64.75, cobalt 0.008, nickel 0.040, copper 0.779, and zinc 0.069.
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In the present work, the recovery of gold from the abovementioned gold ore was investigated by means of leaching using acidothiourea solution consisting of 0.1 mol/L thiourea and 0.05 mol/L sulfuric acid followed by adsorption using bioadsorbent of cotton. Figure 15 shows the effect of liquid/solid ratio (ratio of volume of the leach liquor to unit dry weight of the sample of ore powder) on the leached amount of gold and platinum from the ore sample. From this result, 30 mL/g appears to be the most suitable liquid/solid ratio for extracting gold and platinum from the ore sample; i.e., addition of about 0.23 g of thiourea and 0.15 g of sulfuric acid is necessary for complete extraction of gold and platinum from unit gram of the ore sample.
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Figure 15.
Effect of liquid/solid ratio on the leaching amount of gold and platinum from the Mongolian gold ore sample using acidothiourea consisting of 0.1 mol/L thiourea and 0.05 mol/L sulfuric acid.
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Figure 16 shows effect of solid/liquid ratio (ratio of dry weight of the added adsorbent to unit volume of the leach liquor containing gold(III)) on the adsorption of gold using bioadsorbent of cotton prepared by treating in boiling concentrated sulfuric acid from the leach liquor of Mongolian gold ore. This figure indicates that addition of at least 3 g of bioadsorbent of cotton is necessary for quantitative adsorption of gold(III) from this leach liquor.
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Figure 16.
Effect of solid/liquid ratio on the adsorption of gold using cotton adsorbent from the leach liquor of the Mongolian gold ore.
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Figure 17 shows the XRD pattern of the bioadsorbent of cotton after adsorption of gold(III). Four sharp peaks in this figure obviously evidence the presence of solid elemental gold, suggesting that gold was recovered as elemental gold particles also in this system.
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Figure 17.
XRD pattern of the cotton adsorbent after adsorption of gold(III).
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6. Recovery of gold from simulated spent cyanide solutions using bioadsorbents
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As mentioned earlier, cyanide solution has been extensively employed for a long time in gold mining and also in plating applications because of its special complexing capabilities in aqueous solutions, creating the soluble Au(CN)2− complex. Also as mentioned in the preceding section, such Au(CN)2− complex is recovered by means of adsorption on activated carbon or strongly basic anion-exchange resin. However, such adsorptive recovery of gold is not always quantitative and trace concentrations of gold still remain in the cyanide solution. Spent cyanide solutions generated after the recovery of gold are treated for cyanide decomposition before discharging in environments according to the following processes [34]:
Oxidative decomposition using sulfur dioxide (INCO process)
\n
In this process, cyanide ion is decomposed by the aid of sulfur dioxide and oxygen gasses blown into the cyanide solution catalyzed by cupric sulfate according to the following reaction:
where OCN− ion is unstable and easily hydrolyzed into ammonium bicarbonate. The sulfur dioxide gas can be replaced by sulfurous acid or sodium pyrosulfite (Na2S2O5).
Oxidative decomposition using hydrogen peroxide
\n
Cyanide ion is decomposed by the aid of hydrogen peroxide also catalyzed by cupric sulfate according to the following reaction:
The recovery of trace concentrations of gold remaining in spent cyanide solutions has been difficult due to relatively high processing costs as well as other various technical problems. However, the recovery of such trace concentration of gold has become highly attractive from an economical point of view due to the high price of gold in recent years. Consequently, we attempted to recover such trace concentration of gold(I) from waste cyanide solutions.
\n
However, since gold(I) cyanide solutions are very toxic and its use is prohibited in our laboratory, a sodium salt of gold(I) sulfite, i.e., sodium gold(I) sulfite, Na3[Au(I)(SO3)2], was employed for the adsorptive recovery test of gold(I) in the present work as a simulated solution of cyanide solutions to obtain the fundamental information for exploring the feasibility for the recovery of gold(I) [35]. The use of the gold(I) sulfite complex for gold plating had been known since 1842 [36] and has been currently employed in noncyanide gold plating. The trace amount of Au(I) is also exhausted from such gold sulfite-based plating baths.
\n
In the adsorption of gold(I) in the absence of hypochlorite, only negligible adsorption of gold(I) was observed regardless of pH values. However, by adding sodium hypochlorite to the gold(I) solution in hydrochloric acidic media, the adsorption was drastically improved as shown in Figure 18, suggesting that the addition of sodium hypochlorite provides suitable chemical changes for gold(I). Additionally, a high selectivity to gold(I) was also observed over other metals similar to the case of the adsorption of gold(III) from hydrochloric acid solution as shown in Figure 2, for example.
\n
Figure 18.
Effect of sodium hypochlorite concentration on the adsorption of some metal ions on bioadsorbent of pure cellulose prepared by treating in boiling concentrated sulfuric acid [35].
\n
It is considered that gold(I) was oxidized into gold(III) by the aid of sodium hypochlorite according to the following reaction and adsorbed onto the bioadsorbent of pure cellulose.
Here, the sample solution of sodium gold(I) sulfite, Na3[Au(SO3)2], was colorless. But, after the addition of excess amount of sodium hypochlorite in the presence of hydrochloric acid, the color was changed to pale yellow, the color of AuCl4−, i.e., Au(III) solution, which visually evidence the oxidation reaction.
\n
Figure 19 shows the effect of solid/liquid ratio, the ratio of added amount (dry weight) of bioadsorbent of cellulose prepared by treating in boiling concentrated sulfuric acid to unit volume of the test solution, on the concentration of gold(I) remained in the aqueous solution after the adsorption from the aqueous solution initially contained 60 mg/L gold(I). As seen from this figure, gold(I) can be quantitatively recovered from the solution at the solid/liquid ratio = around 1 g/dm3.
\n
Figure 19.
Effect of adsorbent dose on the concentration of gold(I) remained in the aqueous solution after the adsorption on bioadsorbent of cellulose at pH = 3 where the test aqueous solution initially contained 0.3 mmol/L gold(I) in 0.1 mol/L sodium hypochlorite [35].
\n
\n
\n
7. Prospects for the application of bioadsorbents to actual cyanide processes
\n
As mentioned in the preceding section, gold(I) can be quantitatively recovered by means of adsorption using bioadsorbents under acidic conditions similar to gold(III) after oxidizing gold(I) into gold(III) by the oxidation treatment using sodium hypochlorite, for example.
\n
Also as mentioned earlier, the main hydrometallurgical process for gold and silver ores is cyanide leaching followed by gold recovery by means of adsorption on strongly basic anion exchange resins and activated carbon or by means of cementation using zinc powder. In the adsorption process, the adsorbed gold is recovered by incinerating these loaded adsorbents because the elution of gold adsorbed on these adsorbents is difficult. On the other hand, the cementation using zinc powder also suffers from some problems, one of which is severe control of oxygen or air, except for which it would consume too much amount of zinc powder and cause redisolution of the resulted elemental gold powders. The major gold plating process is also that using cyanide plating solution, in which gold is recovered by the same processes. In these processes, after the recovery of gold, spent cyanide solutions are discharged into environment after the decomposition of cyanide using sodium hypochlorite, for example, as mentioned in the preceding section.
\n
However, by means of the adsorption using bioadsorbents as mentioned above, more economical and more environmental benign process can be proposed as schematically depicted in Figure 20.
\n
Figure 20.
New recovery process of gold from cyanide solutions using bioadsorbents.
\n
In the new process shown in Figure 20, trace concentration of gold(I) contained in cyanide solution will be able to be quantitatively recovered using bioadsorbents, which are easy to be incinerated at comparatively low temperature consuming less amount of energy leaving only gold powder as shown in Figure 9, for example.
\n
A number of processes for recovering cyanide from gold plant barren solutions or pulps also have been developed [32]. For example, the acidification, volatilization and reneutralization (AVR) process as schematically depicted in Figure 21 was practiced at Pachuca silver mine in Mexico and at Flin Flon mine in Canada more than 60 years ago and still now is under operation. Further, it has been recently installed at several other mines around the world.
\n
Figure 21.
Flow sheet of AVR process for the recovery of gold by cyanide leaching followed by recycling of cyanide.
\n
In this process, by adding acid to the barren solution after recovering gold, cyanide is converted into HCN gas, which is scrubbed using caustic solution, returning into cyanide for reuse again. For this process, more economical and more environmentally benign process using bioadsorbents can be proposed as shown in Figure 22 only by changing the order of the step of acidification.
\n
Figure 22.
Modification of AVR process using bioadsorbents.
\n
Further, a more recent advancement is the sulfidization, acidification, recycling, and thickening of precipitate (SART) process schematically shown in Figure 23 developed for ores containing high content of copper, which consumes large amount of cyanide, making worse of the economy of gold recovery. In this process, sulfides are added during the acidification by which pH is lowered from about 10 to 4.5. Under such conditions, the copper present as cyanide complex, Cu(CN)43−, is completely converted into the mineral chalcocite, Cu2S, releasing hydrogen cyanide, HCN gas. However, because selectivity of both strongly basic anion exchange resins and activated carbon to gold(I) cyanide are inferior, large amount of copper(I) cyanide are also adsorbed onto these adsorbents together with gold(I) cyanide, which results in tedious posttreatments.
\n
Figure 23.
Flow sheet for the recovery of gold by means of cyanide leaching followed by recycling of cyanide by means of SART process.
\n
Also for this process, more economical and more environmentally benign new process using biomass adsorbents can be proposed as schematically depicted in Figure 24. In this proposed process, cyanide leach liquor is acidified by adding hydrochloric acid, not after the recovery of gold but before the gold recovery step. During the acidification, gold(I) and copper(I) are spontaneously oxidized into gold(III) and copper(II) by oxygen in air. From such acidified liquor containing gold(III) and copper(II), gold(III) can be quantitatively and highly selectively recovered over copper(II) using the bioadsorbents as metallic gold in a simple manner, leaving copper(II) in the raffinate, which can be easily recovered by means of solvent extraction using hydroxime reagents or, more simply, by means of precipitation using sodium sulfide as the precipitates of copper sulfide.
\n
Figure 24.
Modification of SART process using bioadsorbents.
\n
\n
\n
8. Conclusion
\n
Bioadsorbents for gold recovery were prepared from various biomaterials including biomass wastes such as orange juice residue in a simple manner only by treating in boiling concentrated sulfuric acid. These bioadsorbents exhibited extraordinary high loading capacity and high selectivity for gold in the adsorption from acidic chloride media, which were elucidated to be attributable to the reduction reaction of gold(III) into gold(0), elemental gold, due to the highest oxidation-reduction potential of gold(III), catalyzed by the surface of the bioadsorbents prepared by condensation reaction using concentrated sulfuric acid.
\n
It was confirmed in the recovery tests of gold from printed circuit boards of spent mobile phones, Mongolian gold ore, and simulated spent cyanide solutions containing trace concentration of gold(I) that satisfactory gold recovery was achieved by using these bioadsorbents. Some new gold recovery processes using bioadsorbents were proposed for actual cyanide processes.
\n
By using other types of bioadsorbents, it is possible to recover other precious metals such as palladium and platinum and hazardous materials such as heavy metals.
\n
\n
Acknowledgments
\n
The authors are deeply indebted to Shonan Factory of Tanaka Kikinzoku Kogyo Co. Ltd. and Western Mongolian Metals Co. Ltd. for the kind donation of the samples of printed circuit boards of spent mobile phones and Mongolian gold ore, respectively. We also indebted to Miss Kumiko Kajiyama, Miss Miyuki Matsueda, Miss Sayaka Yamada, Mr. Minoru Abe, Jun-ichi Inoue for their assistance in adsorption and recovery tests.
\n
\n',keywords:"gold recovery, biomass materials",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/66110.pdf",chapterXML:"https://mts.intechopen.com/source/xml/66110.xml",downloadPdfUrl:"/chapter/pdf-download/66110",previewPdfUrl:"/chapter/pdf-preview/66110",totalDownloads:1107,totalViews:0,totalCrossrefCites:2,dateSubmitted:"December 13th 2018",dateReviewed:"January 28th 2019",datePrePublished:"March 12th 2019",datePublished:"October 23rd 2019",dateFinished:null,readingETA:"0",abstract:"Bioadsorbents were prepared in a simple manner only by treating in boiling concentrated sulfuric acid from various biomass materials such as various polysaccharides, persimmon tannin, cotton, paper and biomass wastes such as orange juice residue and microalgae residue after extracting biofuel. These bioadsorbents exhibited high selectivity only to gold over other metals and extraordinary high loading capacity for gold(III), which were elucidated to be attributable to the selective reduction of gold(III) ion to elemental gold due to its highest oxidation-reduction potential of gold(III) of metal ions, catalyzed by the surface of bioadsorbents prepared in boiling sulfuric acid. By using these biosorbents, recovery of gold from actual samples of printed circuit boards of spent mobile phones and Mongolian gold ore was investigated. Recovery of trace concentration of gold(I) from simulated spent alkaline cyanide solution was also investigated using the bioadsorbent. Application of bioadsorbents to some recovery processes of gold from cyanide solutions was proposed.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/66110",risUrl:"/chapter/ris/66110",signatures:"Katsutoshi Inoue, Durga Parajuli, Manju Gurung, Bimala Pangeni, Kanjana Khunathai, Keisuke Ohto and Hidetaka Kawakita",book:{id:"8150",title:"Elements of Bioeconomy",subtitle:null,fullTitle:"Elements of Bioeconomy",slug:"elements-of-bioeconomy",publishedDate:"October 23rd 2019",bookSignature:"Krzysztof Biernat",coverURL:"https://cdn.intechopen.com/books/images_new/8150.jpg",licenceType:"CC BY 3.0",editedByType:"Edited by",editors:[{id:"155009",title:"Prof.",name:"Krzysztof",middleName:null,surname:"Biernat",slug:"krzysztof-biernat",fullName:"Krzysztof Biernat"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}},authors:[{id:"198951",title:"Prof.",name:"Keisuke",middleName:null,surname:"Ohto",fullName:"Keisuke Ohto",slug:"keisuke-ohto",email:"ohtok@cc.saga-u.ac.jp",position:null,institution:{name:"Saga University",institutionURL:null,country:{name:"Japan"}}},{id:"259238",title:"Dr.",name:"Hidetaka",middleName:null,surname:"Kawakita",fullName:"Hidetaka Kawakita",slug:"hidetaka-kawakita",email:"kawakita@cc.saga-u.ac.jp",position:null,institution:null},{id:"289372",title:"Dr.",name:"Katsutoshi",middleName:null,surname:"Inoue",fullName:"Katsutoshi Inoue",slug:"katsutoshi-inoue",email:"inoueka@cc.saga-u.ac.jp",position:null,institution:null},{id:"298633",title:"Dr.",name:"Bimala",middleName:null,surname:"Pangeni",fullName:"Bimala Pangeni",slug:"bimala-pangeni",email:"bimalapangeni@yahoo.co.in",position:null,institution:null},{id:"298634",title:"Dr.",name:"Manju",middleName:null,surname:"Gurung",fullName:"Manju Gurung",slug:"manju-gurung",email:"grgmanju@gmail.com",position:null,institution:null},{id:"298635",title:"Dr.",name:"Kanjana",middleName:null,surname:"Khunathai",fullName:"Kanjana Khunathai",slug:"kanjana-khunathai",email:"kanjana416@yahoo.com",position:null,institution:null},{id:"298636",title:"Dr.",name:"Durga",middleName:null,surname:"Parajuli",fullName:"Durga Parajuli",slug:"durga-parajuli",email:"parajuli.durga@aist.go.jp",position:null,institution:null}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Preparation of bioadsorbents for gold recovery",level:"1"},{id:"sec_3",title:"3. Adsorption behaviors of bioadsorbents for metal ions",level:"1"},{id:"sec_4",title:"4. Recovery of gold from printed circuit boards of spent mobile phones",level:"1"},{id:"sec_5",title:"5. Recovery of gold from Mongolian gold ore",level:"1"},{id:"sec_6",title:"6. Recovery of gold from simulated spent cyanide solutions using bioadsorbents",level:"1"},{id:"sec_7",title:"7. Prospects for the application of bioadsorbents to actual cyanide processes",level:"1"},{id:"sec_8",title:"8. Conclusion",level:"1"},{id:"sec_9",title:"Acknowledgments",level:"1"}],chapterReferences:[{id:"B1",body:'Parajuli D, Inoue K, Ohto K, Oshima T, Murota A, Funaoka M, et al. Adsorption of heavy metals on crosslinked lignocatechol: A modified lignin gel. Reactive and Functional Polymers. 2005;62:129-139. DOI: 10.1016/j.reactfunctpolym.2004.11.003\n'},{id:"B2",body:'Parajuli D, Inoue K, Kuriyama M, Funaoka M, Makino M. Reductive adsorption of gold(III) by crosslinked lignophenol. Chemistry Letters. 2005;34:34-35. DOI: 10.1246/cl.2005.34\n'},{id:"B3",body:'Parajuli D, Adhikari CR, Kuriyama M, Kawakita H, Ohto K, Inoue K, et al. Selective recovery of gold by novel lignin-based adsorption gels. Industrial & Engineering Chemistry Research. 2006;45:8-14. DOI: 10.1021/ie050532u CCC: $33.50\n'},{id:"B4",body:'Parajuli D, Kawakita H, Inoue K, Funaoka M. Recovery of gold(III), palladium(II), and platinum(IV) by aminated lignin derivatives. Industrial & Engineering Chemistry Research. 2006;45:6405-6412. DOI: 10.1021/ie0605318 CCC: $33.50\n'},{id:"B5",body:'Khunathai K, Matsueda M, Biswas BK, Kawakita H, Ohto K, Harada H, et al. Adsorption behavior of lignophenol compounds and their dimethylamine derivatives prepared from rice and wheat straw for precious metal ion. Journal of Chemical Engineering of Japan. 2011;44:781-787\n'},{id:"B6",body:'Kawakita H, Inoue K, Ohto K, Shimada S, Itayama K. Adsorption behavior of waste paper gel chemically modified with functional groups of primary amine and ethylenediamine for some metal ions. Solvent Extraction and Ion Exchange. 2007;25:845-855. DOI: 10.1080/07366290701634024\n'},{id:"B7",body:'Adhikari CR, Parajuli D, Kawakita H, Chand R, Inoue K, Ohto K. Recovery and separation of precious metals using waste paper. Chemistry Letters. 2007;36:1254-1255. DOI: 10.1246/cl.2007.1254\n'},{id:"B8",body:'Adhikari CR, Parajuli D, Kawakita H, Inoue K, Ohto K, Harada H. Dimethylamine-modified waste paper for the recovery of precious metals. Environmental Science & Technology. 2008;42:5486-5491. DOI: 10.1021/es800155xCCC: $40.75\n'},{id:"B9",body:'Adhikari CR, Parajuli D, Inoue K, Ohto K, Kawakita H, Harada H. Recovery of precious metals by using chemically modified waste paper. New Journal of Chemistry. 2008;32:1634-1641\n'},{id:"B10",body:'Pangeni B, Paudyal H, Inoue K, Kawakita H, Ohto K, Alam S. An assessment of gold recovery processes using cross-linked paper gel. Journal of Chemical & Engineering Data. 2012;57:796-804. DOI: 10.1021/je201018a\n'},{id:"B11",body:'Pangeni B, Paudyal H, Inoue K, Kawakita H, Ohto K, Alam S. Selective recovery of gold(III) using cotton cellulose treated with concentrated sulfuric acid. Cellulose. 2012;19:381-391. DOI: 10.1007/s10570-011-9628-6\n'},{id:"B12",body:'Ghimire KN, Inoue K, Ohto K, Hayashida T. Adsorptive separation of metallic pollutants onto waste seaweeds Porphyra Yezoensis and Ulva Japonica. Separation Science and Technology. 2007;42:2003-2018. DOI: 10.1080/15363830701313461\n'},{id:"B13",body:'Ghimire KN, Inoue K, Ohto K, Hayashida T. Adsorption study of metal ions onto crosslinked seaweed Laminaria japonica. Bioresource Technology. 2008;99:32-37. DOI: 10.1016/j.biortech.2006.11.057\n'},{id:"B14",body:'Gurung M, Adhikari BB, Kawakita H, Ohto K, Inoue K, Alam S. Recovery of Au(III) by using low cost adsorbent prepared from persimmon tannin extract. Chemical Engineering Journal. 2011;174:556-563. DOI: 10.1016/j.cej.2011.09.039\n'},{id:"B15",body:'Gurung M, Adhikari BB, Alam S, Kawakita H, Ohto K, Inoue K. Persimmon tannin-based new material for resource recycling and recovery of precious metals. Chemical Engineering Journal. 2013;228:405-414. DOI: 10.1016/j.cej.2013.05.011\n'},{id:"B16",body:'Gurung M, Adhikari BB, Kawakita H, Ohto K, Inoue K, Alam S. Selective recovery of precious metals from acidic leach liquor of circuit boards of spent mobile phones using chemically modified persimmon tannin gel. Industrial & Engineering Chemistry Research. 2012;51:11901-11913. DOI: 10.1021/ie30090231\n'},{id:"B17",body:'Parajuli D, Kawakita H, Inoue K, Ohto K, Kajiyama K. Persimmon peel gel for the recovery of gold. Hydrometallurgy. 2007;87:133-139. DOI: 10.1016/j.hydromet.2007.02.006\n'},{id:"B18",body:'Xiong Y, Adhikari CR, Kawakita H, Ohto K, Inoue K, Harada H. Selective recovery of precious metals by persimmon waste chemically modified with dimethylamine. Bioresource Technology. 2009;100:4083-4089. DOI: 10.1016/j.biortech.2009.03.014\n'},{id:"B19",body:'Parajuli D, Adhikari CR, Kawakita H, Kajiyama K, Ohto K, Inoue K. Reduction and accumulation of Au(III) by grape waste: A kinetic approach. Reactive and Functional Polymers. 2008;68:1194-1199. DOI: 10.1016/j.reactfunctpolym.2008.04.006\n'},{id:"B20",body:'Chand R, Narimura K, Kawakita H, Ohto K, Watari T, Inoue K. Grape waste as a biosorbent for removing Cr(VI) from aqueous solution. Journal of Hazardous Materials. 2009;163:245-250. DOI: 10.1016/j.jhazmat.2008.06.084\n'},{id:"B21",body:'Kawakita H, Abe M, Inoue J, Ohto K, Harada H, Inoue K. Selective gold recovery using orange waste. Separation Science and Technology. 2009;44:2797-2805. DOI: 10.1080/01496390903014615\n'},{id:"B22",body:'Parajuli D, Kawakita H, Kajiyama K, Ohto K, Harada H, Inoue K. Recovery of gold from hydrochloric acid by using lemon peel gel. Separation Science and Technology. 2008;43:2363-2374. DOI: 10.1080/01496390802148472\n'},{id:"B23",body:'Khunathai K, Xiong Y, Biswas BK, Adhikari BB, Kawakita H, Ohto K, et al. Selective recovery of gold by simultaneous adsorption-reduction using microalgal residues generated from biofuel conversion processes. Journal of Chemical Technology & Biotechnology. 2012;87:393-401. DOI: 10.1002/jctb.2733\n'},{id:"B24",body:'Khunathai K, Inoue K, Ohto K, Kawakita H, Kurata M, Atsumi K, et al. Adsorptive recovery of palladium(II) and platinum(IV) on the chemically modified-microalgal residue. Solvent Extraction and Ion Exchange. 2013;31:320-334. DOI: 10.1080/07366299.2012.757092\n'},{id:"B25",body:'Pangeni B, Paudyal H, Abe M, Inoue K, Kawakita H, Ohto K, et al. Selective recovery of gold using some cross-linked polysaccharide gels. Green Chemistry. 2012;14:1917-1927. DOI: 10.1039/c2gc35321k\n'},{id:"B26",body:'Parajuli D, Adhikari CR, Kawakita H, Yamada S, Ohto K, Inoue K. Chestnut pellicle for the recovery of gold. Bioresource Technology. 2009;100:1000-1002. DOI: 10.1016/j.biortech.2008.06.058\n'},{id:"B27",body:'Chand R, Watari T, Inoue K, Kawakita H, Luitel HN, Parajuli D, et al. Selective adsorption of precious metals from hydrochloric acid solutions using porous carbon prepared from barley straw and rice husk. Minerals Engineering. 2009;22:1277-1282. DOI: 10.1016/j.mineng.2009.07.007\n'},{id:"B28",body:'Ogata T, Nakano Y. Mechanism of gold recovery from aqueous solutions using a novel tannin gel adsorbent synthesized from condensed tannin. Water Research. 2005;39:4281-4286. DOI: 10.1016/j.watres.2005.06.036\n'},{id:"B29",body:'Arrascue ML, Garcia HM, Horna O, Guibal E. Gold sorption on chitosan derivatives. Hydrometallurgy. 2003;71:191-200. DOI: 10.1016/S0304-386X(03)00156-7\n'},{id:"B30",body:'Iglesias M, Antico E, Salvado V. Recovery of palladium(II) and gold(III) from diluted liquors using the resin Duolite GT-73. Analytica Chimica Acta. 1999;381:61-67. DOI: 10.1016/S0003-2670(98)00707-7\n'},{id:"B31",body:'Rimmer BF. Refining of gold from precious metal concentrates by liquid-liquid extraction. Chemistry & Industry. 1974;2:63-66\n'},{id:"B32",body:'Anon. Cyanide management in the gold industry. Mining Environmental Management. 2010:26-27\n'},{id:"B33",body:'Chen CK, Lung TN, Wan CC. A study of the leaching of gold and silver by acidothioureation. Hydrometallurgy. 1980;5:207-212\n'},{id:"B34",body:'Kuyucak N, Akcil A. Cyanide and removal options from effluents in gold mining and metallurgical processes. Minerals Engineering. 2013;50-51:13-29. DOI: 10.1016/j.mineng.2013.05.027\n'},{id:"B35",body:'Inoue K, Kawakita H, Ohto K, Alam S. Adsorptive recovery of gold(I) from sodium hypochlorite media. Journal of Chemical Engineering of Japan. 2017;50:94-101. DOI: 10.1252/jcej.16we087\n'},{id:"B36",body:'Dimitrijevic S, Rajcic-Vujasinovic M, Trujic V. Non-cyanide electrolytes for gold plating–A review. International Journal of Electrochemical Science. 2013;8:6620-6646\n'}],footnotes:[],contributors:[{corresp:"yes",contributorFullName:"Katsutoshi Inoue",address:"kanoko1921@gmail.com",affiliation:'
Department of Applied Chemistry, Saga University, Saga, Japan
Department of Applied Chemistry, Saga University, Saga, Japan
'}],corrections:null},book:{id:"8150",title:"Elements of Bioeconomy",subtitle:null,fullTitle:"Elements of Bioeconomy",slug:"elements-of-bioeconomy",publishedDate:"October 23rd 2019",bookSignature:"Krzysztof Biernat",coverURL:"https://cdn.intechopen.com/books/images_new/8150.jpg",licenceType:"CC BY 3.0",editedByType:"Edited by",editors:[{id:"155009",title:"Prof.",name:"Krzysztof",middleName:null,surname:"Biernat",slug:"krzysztof-biernat",fullName:"Krzysztof Biernat"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}}},profile:{item:{id:"255839",title:"Dr.",name:"Juan",middleName:"Carlos",surname:"Gutiérrez Franchi",email:"juangutierrezfranchi@gmail.com",fullName:"Juan Gutiérrez Franchi",slug:"juan-gutierrez-franchi",position:null,biography:null,institutionString:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",totalCites:0,totalChapterViews:"0",outsideEditionCount:0,totalAuthoredChapters:"1",totalEditedBooks:"0",personalWebsiteURL:null,twitterURL:null,linkedinURL:null,institution:{name:"Alfonso X el Sabio University",institutionURL:null,country:{name:"Spain"}}},booksEdited:[],chaptersAuthored:[{title:"Imaging Tests for Predicting the Presence of Difficult Airway in Head and Neck Cancer Patients Undergoing Otorhinolaryngological Surgery",slug:"imaging-tests-for-predicting-the-presence-of-difficult-airway-in-head-and-neck-cancer-patients-under",abstract:"Patients with head and neck cancers represent a challenge for the surgical team from many points of view, but, especially, the surgical moment where greater stress generated corresponds to the perioperative management of the airway, because in many occasions we can face unexpected situations, most of the time, incidental findings can hinder ventilation and endotracheal intubation. Gutierrez et al., in 2018, decided to study four tomography measures and their correlation in anesthesia records with airway management difficulties. Material and methods: A retrospective, observational study was carried out in 104 patients operated by head and neck cancers over a period of 36 months, only in those with access to tomographic records. Four tomographic measurements were considered and were statistically related to the extreme degrees of visualization of the glottis (Cormack III–IV) and the presence of the physical examination of Mallampati III–IV. Results: After performing a multivariate model in the group of extreme degrees of visualization of the glottis, the results were not statistically significant (p > 0.05; 95% CI: 0.030–2.31: EPI/PPW, 0.018–1.37 TB/PPW). In the Mallampati III–IV group, in the multivariate model only the VC/PPW showed clinically significant results (p < 0.05; 95% CI: 0.104–8.53). Conclusions: Tomographic measurements and the physical examination predictors could represent a useful guide in the prediction of the difficult airway in these patients.",signatures:"Juan Gutiérrez Franchi, S. Merino, P. de la Calle, C. Perrino, M. Represa\nand P. 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Her main research interest is in radiology and neuroscience applications. She had been trained and worked as a medical imaging scientist at several prestigious institutes including Columbia University, University of Pennsylvania, and the National Institutes of Health (NIH). Her research focuses on multimodal neuroimaging integration including MRI/PET and EEG/MEG instrumentation that makes the best use of multiple modalities to help interpret underlying disease mechanisms. She has authored six monograph books, and edited several books for well-known publishers including IntechOpen and Nova Science. She has published more than 100 papers and presentations in many reputed international journals and conferences, and served as reviewer and editor for several well-known associations.",institutionString:"University of Southern California",institution:{name:"University of Southern California",institutionURL:null,country:{name:"United States of America"}}},{id:"264444",title:"Dr.",name:"Mitsuo",surname:"Tonoike",slug:"mitsuo-tonoike",fullName:"Mitsuo Tonoike",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"264445",title:"Dr.",name:"Takuyo",surname:"Hayashi",slug:"takuyo-hayashi",fullName:"Takuyo Hayashi",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null}]},generic:{page:{slug:"open-access-funding-funders-list",title:"List of Funders by Country",intro:"
If your research is financed through any of the below-mentioned funders, please consult their Open Access policies or grant ‘terms and conditions’ to explore ways to cover your publication costs (also accessible by clicking on the link in their title).
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IMPORTANT: You must be a member or grantee of the listed funders in order to apply for their Open Access publication funds. Do not attempt to contact the funders if this is not the case.
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UK Research and Innovation (former Research Councils UK (RCUK) - including AHRC, BBSRC, ESRC, EPSRC, MRC, NERC, STFC.) Processing charges for books/book chapters can be covered through RCUK block grants which are allocated to most universities in the UK, which then handle the OA publication funding requests. It is at the discretion of the university whether it will approve the request.)
UK Research and Innovation (former Research Councils UK (RCUK) - including AHRC, BBSRC, ESRC, EPSRC, MRC, NERC, STFC.) Processing charges for books/book chapters can be covered through RCUK block grants which are allocated to most universities in the UK, which then handle the OA publication funding requests. It is at the discretion of the university whether it will approve the request.)
Wellcome Trust (Funding available only to Wellcome-funded researchers/grantees)
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