CN110951977A - Method for leaching cobaltite by using biomass reducing agent - Google Patents
Method for leaching cobaltite by using biomass reducing agent Download PDFInfo
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- CN110951977A CN110951977A CN201911264683.0A CN201911264683A CN110951977A CN 110951977 A CN110951977 A CN 110951977A CN 201911264683 A CN201911264683 A CN 201911264683A CN 110951977 A CN110951977 A CN 110951977A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a method for leaching cobaltite by using a biomass reducing agent, which comprises the following steps: (1) drying and crushing the waste biomass raw material to obtain a solid A; (2) adding the solid A into water for reaction, wherein the reaction temperature is 250-350 ℃, the pressure is 1.4-2.7 MPa, and the time is 4-24 h; after the separation, drying to obtain solid B; (3) crushing the solid B, adding an acid solution, fully stirring, adding the heterogenite, stirring and leaching for 1-5 hours, wherein the mass ratio of the solid B to the heterogenite is (0.08-0.2): 1. according to the method, the biomass reducing agent and the cobaltite do not need to be calcined together, and toxic and harmful gases are not discharged; when the transformed biomass reduces the cobaltite, the leaching process is carried out at room temperature, high-temperature heating is not needed, and the effects of energy conservation and consumption reduction are obvious; the novel biomass reducing agent is adopted to leach the cobaltite, so that the requirements on the control of equipment and process conditions are not high, the investment is low, the method is simple and feasible, and the method has no pollution to the environment.
Description
Technical Field
The invention relates to a hydrometallurgical process for leaching cobaltite by using a reducing agent prepared from waste biomass, belonging to the technical field of cobalt hydrometallurgy.
Background
The world cobalt resource distribution is unbalanced, reserves are highly concentrated in Australia, Gouba, Russia, Africa and the like, the Africa continent has rich cobalt mineral resources, and is mainly distributed in famous Africa plus red copper ore zones, wherein Congo (gold) is the most abundant world cobalt resource reserve, reaches 340 million tons and accounts for 47.2 percent of the global total reserve. The cobalt resource in China is relatively poor, most of the cobalt resource is associated ore, the grade is low, the cobalt resource is mostly recovered as a byproduct, and more than 90 percent of cobalt production enterprises need to import the cobalt raw material from African countries mainly comprising Congo (gold). Congo (gold) has also become the first choice for cobalt in domestic capital. Cobalite is a major cobalt resource in Congo (gold) and mainly contains complex cobalt oxide and cobalt hydroxide, which may be a variation of monohydrate of two-valence and three-valence, with different impurity components and degrees of crystallinity, and unstable components, but Co in high valence state is mostly cobalt in the cobalt2O3The method has the advantages that a reducing agent is added in the leaching process to leach the cobalt in the cobalt.
At present, the mainstream process for treating the heterogenite is a reduction acid leaching method, namely reduction leaching is carried out in a sulfuric acid system, and reducing agents mainly comprise ferrous sulfate, iron powder, sodium sulfite, sodium metabisulfite, sulfur dioxide and the like. In the leaching process by adding ferrous salt or iron powder as a reducing agent, although the leaching effect of copper and cobalt is better, the content of iron ions in the leaching solution is increased, the workload of the subsequent purification process is increased, and a certain amount of cobalt loss is caused. The sodium sulfite, the sodium metabisulfite or the sulfur dioxide is adopted as a reducing agent, so that impurities are not brought in, the leaching effect of cobalt and copper is good, but a certain amount of sulfur dioxide overflows in the leaching process, the pollution is caused, and the working environment is deteriorated. The waste biomass is properly treated and activated and then used as a reducing agent for metallurgical leaching, which is a research hotspot in recent years, and is mostly reported in literature reports of reducing and leaching manganese oxide ores by using the biomass, and the related research results of corn stalks, bagasse, straws, wheat bran, rice chaff, cassava residue, wood chips, sawdust, waste molasses and the like prove that the leaching of manganese can be realized under certain conditions, and the biomass can be recycled and reused, so that the environment is not harmful. After biomass is properly treated, main components of the biomass can be hydrolyzed under an acidic condition to generate a reducing substance which can be subjected to oxidation reduction reaction with the main components in the cobaltite, so that trivalent cobalt in the cobaltite is reduced into acid-soluble divalent cobalt, high-temperature roasting is not needed in the leaching process, external heat supply is not needed, reaction equipment is simple, equipment investment cost is low, environmental pollution is small, and the method is a novel green reducing agent for wet-process reduction leaching of the cobaltite.
The biomass energy conversion and utilization technology can be divided into five major categories from the conversion mode, namely a direct combustion technology, a physical-chemical conversion technology, a biological-chemical conversion technology, a liquefaction conversion technology and a solid waste conversion technology. But can be divided into three major categories from a technical perspective: the method is a direct combustion method for directly obtaining heat from biomass by a combustion technology; the second method is a biological conversion technology for preparing gas and liquid fuel by carrying out biological fermentation on biomass; the third method is a process of converting biomass into a novel functional material or fuel by utilizing a thermochemical technology, wherein the process comprises technologies such as gasification, pyrolysis liquefaction, hydrothermal and the like, and the process is one of the hotspots of the current research on novel functional materials and novel fuel technologies. According to different research target products, hydrothermal methods can be divided into three major categories, namely hydrothermal gasification, hydrothermal liquefaction and hydrothermal carbonization. As a novel waste biomass treatment mode, compared with pyrolysis, the biomass hydrothermal carbonization technology has the advantages that raw materials are not limited by water content, the preparation process is easy to master, the cost is low, the conversion rate is high, and the like, and has a good application prospect. The hydrothermal carbonization is a thermochemical conversion process for converting biomass into a series of high-energy value-added products mainly comprising biochar by using water as a reaction medium in a closed reactor, wherein the temperature is controlled at 300 ℃, the pressure is 1.4-2.7 MPa, the reaction time is 4-24 hours, and the hydrothermal carbonization is carried out. Compared with other hydrothermal technologies, the hydrothermal carbonization technology has the advantage that various reaction conditions are easy to achieve. In recent years, a great deal of research is carried out on the optimization of hydrothermal carbonization technology at home and abroad, the method is expanded from various simple pure carbon compounds to biomass raw materials and finally to the preparation of waste biomass into high-energy materials by using additives, the application range is continuously extended, and the method is widely applied to various fields such as medicine, fuel, electrode preparation, metallurgy, energy storage, environment restoration and the like.
The biomass itself has low sulfur, low ash and CO2Zero emission in total amount and the like, and the energy-saving agent accounts for 2/3 of all renewable energy sources in the world and has great potential utilization value. By utilizing the existing biomass conversion technology, the biomass resource recovery channel and the application field are continuously expanded, and the method has important meanings for relieving the problems of energy shortage, preventing environmental pollution, maintaining ecological balance and the like.
CN109338122A discloses a leaching method of heterogenite, which comprises calcining heterogenite and fuel particle reducing agent, cooling calcined material, adding water, adding acid, stirring and leaching, wherein the fuel particle is also prepared from plant material. However, the method has some problems, especially when the heterogenite and the fuel particles are calcined, some toxic and harmful gases are generated, and the environment is polluted.
Disclosure of Invention
Aiming at the current research situation of the leaching of the heterogenite, the invention introduces a novel biomass reducing agent, the leaching process does not need high-temperature roasting, does not need external heat supply, and has simple reaction equipment, small environmental pollution and environmental protection.
The technical solution provided by the invention is as follows:
a method for leaching cobaltite by using a biomass reducing agent comprises the following steps:
(1) drying and crushing the waste biomass raw material to obtain a solid A;
(2) adding the solid A into water for reaction, wherein the reaction temperature is 250-350 ℃, the pressure is 1.4-2.7 MPa, and the time is 4-24 h; after the reaction is finished, separating and drying to obtain solid B;
(3) crushing the solid B, adding an acid liquor, fully stirring, adding the solid B and the acid liquor with the mass ratio of (8-13) to 1, adding the cobaltite, stirring and leaching for 1-5 hours, wherein the mass ratio of the solid B to the cobaltite is (0.08-0.2): 1.
preferably, the biomass raw material in step (1) includes, but is not limited to, one or more of corncob, peanut shell, rice hull, bagasse, straw, wheat bran, wheat straw and sorghum stalk.
Preferably, in the step (1), the drying temperature is 105-; further preferably, the drying temperature is 110 ℃.
Preferably, in the step (2), the mass ratio of the solid A to the water is 1: 2.
Preferably, the acid solution in the step (3) is dilute sulfuric acid.
Preferably, the mass concentration of the dilute sulfuric acid is 18-40 mg/ml.
Preferably, the number of the crushed meshes of the solid B in the step (3) is-100 meshes or less.
Preferably, the cobaltous ore in the step (3) is dried, crushed and ground to below-100 meshes.
A method for leaching cobaltite by using a biomass reducing agent comprises the following steps:
taking 300 parts of cornstalks, drying at 110 ℃ in advance, crushing, putting into a reaction kettle, controlling the temperature at 300 ℃, the pressure at 1.5MPa, reacting for 5 hours, adopting water as a reaction medium, performing liquid-solid separation after the reaction is finished, drying the obtained biomass reducing agent at 100 ℃, and continuously grinding to below-100 meshes. Taking 150 parts of dilute sulfuric acid with the mass concentration of 19.6mg/ml, then adding 5 parts of corn stalk reducing agent, and fully stirring for 20min to obtain a leaching solution for later use. Adding 50 parts of cobaltite into the leaching solution, mechanically stirring and leaching at room temperature for 1h, wherein the liquid-solid ratio (liquid volume to solid mass ratio) is 3: and 1, filtering after leaching is finished.
A method for leaching cobaltite by using a biomass reducing agent comprises the following steps:
300 parts of wheat straw is taken and dried at 110 ℃ in advance, the crushed wheat straw is put into a reaction kettle, the temperature is controlled at 350 ℃, the pressure is 2.0MPa, the reaction time is 10 hours, water is used as a reaction medium, liquid-solid separation is carried out after the reaction is finished, and the obtained biomass reducing agent is dried at 100 ℃ and then continuously ground to be below-80 meshes. Taking 100 parts of dilute sulfuric acid with the mass concentration of 38.46mg/ml, then adding 4 parts of wheat straw reducing agent, and fully stirring for 20min to obtain a leaching solution for later use. Adding 50 parts of cobaltite into the leaching solution, mechanically stirring and leaching at room temperature for 2 hours, wherein the liquid-solid ratio is 2: and 1, filtering after leaching is finished.
A method for leaching cobaltite by using a biomass reducing agent comprises the following steps:
taking 300 parts of straw stalks, drying at 110 ℃ in advance, crushing, putting into a reaction kettle, controlling the temperature at 250 ℃, the pressure at 2.5MPa, reacting for 15 hours, adopting water as a reaction medium, performing liquid-solid separation after the reaction is finished, drying the obtained biomass reducing agent at 100 ℃, and continuously grinding to below-60 meshes. Taking 200 parts of dilute sulfuric acid with the mass concentration of 29.13mg/ml, adding 6 parts of corn stalk reducing agent, fully stirring for 20min to obtain a leaching solution for later use, adding 50 parts of cobalt hydrate into the leaching solution, and mechanically stirring and leaching at room temperature for 1.5h, wherein the liquid-solid ratio is 4: and 1, filtering after leaching is finished.
Compared with the prior art, the invention has the beneficial effects that:
(1) compared with patent CN109338122A, the biomass reducing agent and the cobaltite do not need to be calcined together, the reducing agent prepared by hydrothermal activation of the waste biomass can be used for industrial production and application in large scale, the carrying and the transportation are convenient, the process conditions are easier to control, and no toxic or harmful gas is discharged in the whole process.
(2) Compared with the traditional biomass direct reduction leaching ore technology, the leaching process is carried out at room temperature when the transformed biomass reduces the cobaltite, high-temperature heating is not needed, and the effects of energy conservation and consumption reduction are obvious.
(3) Compared with the mainstream process of the existing cobaltite reduction acid leaching method, the novel biomass reducing agent is adopted to leach the cobaltite, so that the requirements on the control of equipment and process conditions are not high, the investment is low, the method is simple and feasible, and the method has no pollution to the environment.
Detailed Description
The following will further illustrate the specific technical solutions of the present invention with reference to the following examples.
Example 1
Taking 300 parts of cornstalks, drying at 110 ℃ in advance, crushing, putting into a reaction kettle, controlling the temperature at 300 ℃, the pressure at 1.5MPa, reacting for 5 hours, adopting water as a reaction medium, performing liquid-solid separation after the reaction is finished, drying the obtained biomass reducing agent at 100 ℃, and continuously grinding to below-100 meshes. Adding 3g of concentrated sulfuric acid into 150ml of water, uniformly mixing, adding 5 parts of corn stalk reducing agent, and fully stirring for 20min to obtain a leaching solution for later use. Adding 50 parts of cobaltite into the leaching solution, mechanically stirring and leaching at room temperature for 1h, wherein the liquid-solid ratio is 3: 1, filtering after leaching, and analyzing and calculating that the leaching rate of cobalt is 99.21 percent according to slag.
Example 2
300 parts of wheat straw is taken and dried at 110 ℃ in advance, the crushed wheat straw is put into a reaction kettle, the temperature is controlled at 350 ℃, the pressure is 2.0MPa, the reaction time is 10 hours, water is used as a reaction medium, liquid-solid separation is carried out after the reaction is finished, and the obtained biomass reducing agent is dried at 100 ℃ and then continuously ground to be below-80 meshes. Adding 4g of concentrated sulfuric acid into 100ml of water, uniformly mixing, adding 4 parts of wheat straw reducing agent, and fully stirring for 20min to obtain a leaching solution for later use. Adding 50 parts of cobaltite into the leaching solution, mechanically stirring and leaching at room temperature for 2 hours, wherein the liquid-solid ratio is 2: 1, filtering after leaching is finished, and analyzing and calculating to obtain 99.18% of cobalt leaching rate according to slag.
Example 3
Taking 300 parts of straw stalks, drying at 110 ℃ in advance, crushing, putting into a reaction kettle, controlling the temperature at 250 ℃, the pressure at 2.5MPa, reacting for 15 hours, adopting water as a reaction medium, performing liquid-solid separation after the reaction is finished, drying the obtained biomass reducing agent at 100 ℃, and continuously grinding to below-60 meshes. Adding 6g of concentrated sulfuric acid into 200ml of water, uniformly mixing, adding 6 parts of corn stalk reducing agent, fully stirring for 20min to obtain a leaching solution for later use, adding 50 parts of cobalt hydrate into the leaching solution, mechanically stirring and leaching at room temperature for 1.5h, wherein the liquid-solid ratio is 4: 1, filtering after leaching, and calculating by analysis that the leaching rate of cobalt is 99.06 percent according to slag.
Comparative example 1
Crushing 6 parts of straw stalks, fully mixing with 50 parts of hydrocobaltite, calcining for 1h at 300 ℃, cooling, taking out, adding the calcined material into dilute sulfuric acid (200 ml of water is taken, 6g of concentrated sulfuric acid is added, and the mixture is uniformly mixed) to be mechanically stirred and leached, wherein the leaching temperature is room temperature, the leaching time is 1.5h, and the liquid-solid ratio is 4: 1, filtering after leaching, and analyzing and calculating to obtain the cobalt leaching rate of 98.17 percent according to slag.
Claims (8)
1. A method for leaching cobaltite by using a biomass reducing agent is characterized by comprising the following steps:
(1) drying and crushing the waste biomass raw material to obtain a solid A;
(2) adding the solid A into water for reaction, wherein the reaction temperature is 250-350 ℃, the pressure is 1.4-2.7 MPa, and the time is 4-24 h; after the reaction is finished, separating and drying to obtain solid B;
(3) crushing the solid B, adding an acid solution, fully stirring, adding the cobaltite, stirring and leaching for 1-5 hours, wherein the mass ratio of the solid B to the acid solution is (8-13): 1, and the mass ratio of the solid B to the cobaltite is (0.08-0.2): 1.
2. the method for leaching hydrocobalt ore with a biomass reducing agent according to claim 1, wherein the biomass raw material in the step (1) includes but is not limited to one or more of corncob, peanut shell, rice hull, bagasse, straw, wheat bran, wheat straw and sorghum stalk.
3. The method for leaching cobaltous ore by using biomass reducing agent as claimed in claim 1, wherein in the step (1), the drying temperature is 105-115 ℃; further preferably, the drying temperature is 110 ℃.
4. The method for leaching hydrocobaltite by using the biomass reducing agent according to claim 1, wherein in the step (2), the mass ratio of the solid A to the water is 1: 2.
5. The method for leaching cobaltite by using the biomass reducing agent according to claim 1, wherein the acid solution in the step (3) is dilute sulfuric acid.
6. The method for leaching cobaltous ore by using the biomass reducing agent according to claim 1, wherein the mass concentration of the dilute sulfuric acid is 18-40 mg/ml.
7. The method for leaching hydrocobaltite by using the biomass reducing agent according to claim 1, wherein the crushing mesh number in the step (3) is-100 meshes or less.
8. The method for leaching cobaltous oxide by using the biomass reducing agent according to claim 1, wherein the cobaltous oxide in the step (3) is dried, crushed and ground to below-100 meshes.
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| CN201911264683.0A CN110951977A (en) | 2019-12-11 | 2019-12-11 | Method for leaching cobaltite by using biomass reducing agent |
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| CN201911264683.0A CN110951977A (en) | 2019-12-11 | 2019-12-11 | Method for leaching cobaltite by using biomass reducing agent |
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| CN109338122A (en) * | 2018-11-06 | 2019-02-15 | 广东佳纳能源科技有限公司 | A kind of leaching method of heterogenite |
| CN110184455A (en) * | 2019-06-20 | 2019-08-30 | 东北大学 | A kind of leaching method of difficult leaching cobalt ore |
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2019
- 2019-12-11 CN CN201911264683.0A patent/CN110951977A/en active Pending
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| FR2948946A1 (en) * | 2009-08-07 | 2011-02-11 | Metaleach Ltd | PROCESS FOR LEACHING COBALT FROM COBALT OXIDE ORES |
| US20120244051A1 (en) * | 2009-08-07 | 2012-09-27 | Metaleach Limited | Method for leaching cobalt from oxidised cobalt ores |
| CN101831546A (en) * | 2010-06-10 | 2010-09-15 | 中南大学 | Method for preparing biomass reductant and application thereof |
| CN107739845A (en) * | 2017-08-31 | 2018-02-27 | 广东佳纳能源科技有限公司 | A kind of cleaning procedure of reducing leaching Africa heterogenite |
| CN109338122A (en) * | 2018-11-06 | 2019-02-15 | 广东佳纳能源科技有限公司 | A kind of leaching method of heterogenite |
| CN110184455A (en) * | 2019-06-20 | 2019-08-30 | 东北大学 | A kind of leaching method of difficult leaching cobalt ore |
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| 贾智慧: "废弃电池的生物质浸出及金属回收研究", 《中国优秀硕士论文全文数据库（电子期刊）》 * |
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