CN115652105B - Sectional leaching process for cobalt raw material - Google Patents

Sectional leaching process for cobalt raw material Download PDF

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CN115652105B
CN115652105B CN202211449621.9A CN202211449621A CN115652105B CN 115652105 B CN115652105 B CN 115652105B CN 202211449621 A CN202211449621 A CN 202211449621A CN 115652105 B CN115652105 B CN 115652105B
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leaching
stage
kettle
cobalt
solution
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CN115652105A (en
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李小鹏
胡伟
王国超
毛腾
岳志洲
寇占伟
王复龙
周林华
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Lanzhou Jinchuan Advangced Materials Technology Co ltd
Jinchuan Group Co Ltd
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Lanzhou Jinchuan Advangced Materials Technology Co ltd
Jinchuan Group Co Ltd
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Abstract

The invention discloses a cobalt raw material sectional leaching method, which comprises the following steps: (1) mixing cobalt raw material and acid wastewater according to a liquid-solid ratio of 3-5:1, and stirring for 30-120min; (2) Transferring the slurry into a primary kettle of a primary leaching kettle; (3) Continuously adjusting the PH value of the first-stage leaching kettle to 3.5-4.0 in a segmented manner; (4) adding the solution in the step (3) into an oxidant in a segmented manner; (5) Press-filtering the supernatant produced by the thickener in the step (4) and then extracting to prepare cobalt salt solution; (6) Pumping the underflow slag generated by the thickener in the step (4) into a two-stage leaching kettle, and adding sulfuric acid and a reducing agent in sections to carry out two-stage full leaching; (7) Carrying out solid-liquid separation on the second-stage leaching solution in the step (6) by using a filter press, wherein part of filtrate is used for adjusting the first-stage leaching process by using acid, and the rest part is used for chemically removing iron; (8) And (3) washing the filter residue obtained in the step (7) to remove residual cobalt metal in the filter residue.

Description

Sectional leaching process for cobalt raw material
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a cobalt raw material sectional leaching method.
Background
In the hydrometallurgical process of outsourced cobalt feedstock, the outsourced cobalt feedstock is typically in the form of cobalt hydroxide, which contains some of the more difficult to leach trivalent cobalt and metal compounds. Cobalt hydroxide is susceptible to leaching at low acidity conditions, and other trivalent cobalt is not able to leach at low acidity conditions. Cobalt raw materials generally contain relatively large amounts of metal impurity ions, such as Cu, mn, fe, cd and the like. The method generally needs a chemical impurity removal method to chemically separate part of impurity elements in the leaching solution before the leaching solution of the cobalt raw material enters extraction separation, and the process can lead most of Fe, as, al and other impurities to enter slag in a precipitation mode, and then the chemical extraction method is utilized to separate main metal elements from impurity ions and prepare high-purity cobalt salt solution.
The hydrometallurgical process mainly comprises the processes of chemical leaching, chemical impurity removal, extraction impurity removal and the like. The leaching process is an essential step prior to achieving the separation of the cobalt feedstock impurities, common leaching methods include acid leaching, alkaline leaching and bioleaching. The cobalt system mainly comprises two purification processes, namely a wet process and a fire process, wherein the wet leaching process of the cobalt system usually adopts a section of acid full leaching and a subsequent chemical neutralization impurity removal process to realize the leaching and purification of raw materials, and finally, a chemical extraction method is utilized to separate main metal ions from impurity ions in the solution.
At present, for a common one-stage full leaching process, a large amount of acid and reducing agent are required to be added to adjust the pH value of the solution to 1.5, then the reaction is continued for a long time to realize the full leaching of the cobalt raw material, and a large amount of neutralizing agent is required to be added later for separating iron ions and aluminum ions from the solution, so that a large amount of chemical reagents are required to be consumed in the whole solution purification process, and the cost is high.
Disclosure of Invention
Aiming at the technical problems, the invention provides a cobalt raw material sectional leaching method.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a segmented leaching method for cobalt raw materials, comprising the following steps:
(1) Cobalt raw material and acid wastewater are mixed according to a liquid-solid ratio of 3-5:1, and stirring for 30-120min to obtain slurry;
(2) Transferring the slurry into a first-stage kettle of a first-stage leaching kettle, and continuously supplementing the slurry to enable the solution in the kettle to continuously flow into the next stages of kettles connected in series;
(3) Continuously adjusting the PH value of the first-stage leaching kettle to 3.5-4.0 in a segmented manner to realize continuous acid leaching;
(4) Adding an oxidant into the solution in the step (3) in sections, fully oxidizing ferrous iron generated in the leaching process to trivalent iron, hydrolyzing ferric iron ions, generating precipitate, entering slag, flowing the solution to a subsequent kettle under the stirring effect, and finally flowing into a thickener to realize solid-liquid separation;
(5) Press-filtering the supernatant produced by the thickener in the step (4) and then extracting to prepare cobalt salt solution;
(6) Pumping the underflow slag generated by the thickener in the step (4) into a two-stage leaching kettle, and adding sulfuric acid and a reducing agent in sections to carry out two-stage full leaching;
(7) Carrying out solid-liquid separation on the second-stage leaching solution in the step (6) by using a filter press, wherein part of filtrate is used for adjusting the first-stage leaching process by using acid, and the rest part is used for chemically removing iron;
(8) And (3) washing the filter residue in the step (7) to remove residual cobalt metal in the filter residue, and feeding the cobalt-containing washing water into the step (1) for pulping.
In the step (1), the theoretical cobalt ion concentration in the slurry is kept at 60-70g/L, the pH value of the slurry is 5.5-6, and the solution flow rate in one stage of leaching process is 10-25 m/h.
Wherein, in the stage leaching process in the step (3), the first stage leaching kettle is a stage series equipment, and the stage number of the first stage leaching kettle is 5-7.
In the step (4), the oxidant is sodium hypochlorite or hydrogen peroxide or high-energy oxygen.
Wherein in the step (5), the content of iron in the supernatant is lower than 0.005g/L.
In the step (6), a leaching kettle is adopted for a stage-two continuous leaching process, wherein the leaching kettle is 3-5 stages.
In the step (6), the reducing agent comprises sodium metabisulfite, sodium sulfite and sulfur dioxide.
The beneficial effects of the invention are as follows:
(1) The staged leaching process saves a significant amount of neutralizing agent over the traditional one-stage total leaching.
(2) The method adopts sectional multistage continuous leaching, so that a great deal of labor intensity can be reduced.
(3) The method uses the second-stage leaching supernatant to adjust the first-stage slurry, and saves a large amount of acid while maintaining the high cobalt ion concentration of the leaching solution.
(4) The scheme can realize iron removal during one-stage leaching, and greatly shortens the whole leaching process of the cobalt raw material.
Drawings
Fig. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described in detail with reference to the following embodiments, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the description is only illustrative and is not intended to limit the scope of the invention. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the present invention.
Example 1
A segmented leaching method for cobalt raw materials, comprising the following steps:
(1) Cobalt raw material and acid wastewater are mixed according to a liquid-solid ratio of 3:1, and stirring for 30min to obtain slurry;
(2) Transferring the slurry into a first-stage kettle of a first-stage leaching kettle, and continuously supplementing the slurry to enable the solution in the kettle to continuously flow into the next stages of kettles connected in series;
(3) Continuously adjusting the PH value of the first-stage leaching kettle to 3.5-4.0 in a segmented manner to realize continuous acid leaching;
(4) Adding an oxidant into the solution in the step (3) in sections, fully oxidizing ferrous iron generated in the leaching process to trivalent iron, hydrolyzing ferric iron ions, generating precipitate, entering slag, flowing the solution to a subsequent kettle under the stirring effect, and finally flowing into a thickener to realize solid-liquid separation;
(5) Press-filtering the supernatant produced by the thickener in the step (4) and then extracting to prepare cobalt salt solution;
(6) Pumping the underflow slag generated by the thickener in the step (4) into a two-stage leaching kettle, and adding sulfuric acid and a reducing agent in sections to carry out two-stage full leaching;
(7) Carrying out solid-liquid separation on the second-stage leaching solution in the step (6) by using a filter press, wherein part of filtrate is used for adjusting the first-stage leaching process by using acid, and the rest part is used for chemically removing iron;
(8) And (3) washing the filter residue in the step (7) to remove residual cobalt metal in the filter residue, and feeding the cobalt-containing washing water into the step (1) for pulping.
In the step (1), the theoretical cobalt ion concentration in the slurry is kept at 60g/L, the pH value of the slurry is 5.5-6, and the solution flow rate in the first leaching process is 10 m/h.
Wherein, in the stage leaching process in the step (3), the first stage leaching kettle is a stage series equipment, and the stage number of the first stage leaching kettle is 5-7.
In the step (4), the oxidant is sodium hypochlorite or hydrogen peroxide or high-energy oxygen.
Wherein in the step (5), the content of iron in the supernatant is lower than 0.005g/L.
In the step (6), a leaching kettle is adopted for a stage-two continuous leaching process, wherein the leaching kettle is 3-5 stages.
In the step (6), the reducing agent comprises sodium metabisulfite, sodium sulfite and sulfur dioxide.
Example 2
A segmented leaching method for cobalt raw materials, comprising the following steps:
(1) Cobalt raw material and acid wastewater are mixed according to a liquid-solid ratio of 5:1, and stirring for 120min to obtain slurry;
(2) Transferring the slurry into a first-stage kettle of a first-stage leaching kettle, and continuously supplementing the slurry to enable the solution in the kettle to continuously flow into the next stages of kettles connected in series;
(3) Continuously adjusting the PH value of the first-stage leaching kettle to 3.5-4.0 in a segmented manner to realize continuous acid leaching;
(4) Adding an oxidant into the solution in the step (3) in sections, fully oxidizing ferrous iron generated in the leaching process to trivalent iron, hydrolyzing ferric iron ions, generating precipitate, entering slag, flowing the solution to a subsequent kettle under the stirring effect, and finally flowing into a thickener to realize solid-liquid separation;
(5) Press-filtering the supernatant produced by the thickener in the step (4) and then extracting to prepare cobalt salt solution;
(6) Pumping the underflow slag generated by the thickener in the step (4) into a two-stage leaching kettle, and adding sulfuric acid and a reducing agent in sections to carry out two-stage full leaching;
(7) Carrying out solid-liquid separation on the second-stage leaching solution in the step (6) by using a filter press, wherein part of filtrate is used for adjusting the first-stage leaching process by using acid, and the rest part is used for chemically removing iron;
(8) And (3) washing the filter residue in the step (7) to remove residual cobalt metal in the filter residue, and feeding the cobalt-containing washing water into the step (1) for pulping.
In the step (1), the theoretical cobalt ion concentration in the slurry is kept at 70g/L, the pH value of the slurry is 5.5-6, and the solution flow rate in one stage of leaching process is 25 m/h.
Wherein, in the stage leaching process in the step (3), the first stage leaching kettle is a stage series equipment, and the stage number of the first stage leaching kettle is 5-7.
In the step (4), the oxidant is sodium hypochlorite or hydrogen peroxide or high-energy oxygen.
Wherein in the step (5), the content of iron in the supernatant is lower than 0.005g/L.
In the step (6), a leaching kettle is adopted for a stage-two continuous leaching process, wherein the leaching kettle is 3-5 stages.
In the step (6), the reducing agent comprises sodium metabisulfite, sodium sulfite and sulfur dioxide.
Example 3
1. Adding 3 bags of cobalt hydroxide raw materials such as warrior into a slurrying tank, adding wastewater, and keeping the liquid-solid ratio at 4:1, continuously stirring for 30min, and returning to a first-stage leaching serial kettle;
2. the first-stage leaching kettle is continuously stirred, and the solution in the tank continuously flows to the last several stages of the series kettles through continuously supplementing the slurry;
3. adding a proper amount of low second-stage leaching liquid (1.5) continuously into the first-stage front three stages of the first-stage serial kettles to adjust the leaching liquid to be first-stage 4.5, second-stage 4 and third-stage 3.5 in a grading manner so as to realize first-stage leaching;
4. adding a proper amount of sodium hypochlorite into the second to fourth stages of the first-stage serial kettles to oxidize all ferrous ions in the solution to trivalent, flowing the solution to a subsequent reaction kettle under the stirring effect, and finally flowing into a thickener to realize solid-liquid separation and iron removal in the process;
5. performing multistage solid-liquid separation on the supernatant produced by the thickener in the step 4, and taking the supernatant as a copper material required by P204 extraction;
6. pumping the underflow slag generated by the thickener in the step 4 into a second-stage leaching kettle, adding sulfuric acid and a reducing agent, and carrying out second-stage full leaching;
7. carrying out solid-liquid separation on the leached solution in the step 6 by using a filter press, and washing filter pressing residues by using water;
and 8, returning the washing water generated in the step 7 to raw material pulping, and using the filtrate generated in the step 7 for one-stage leaching adjustment solution.
Experimental results: the experimental results are shown in Table 1.
Table 1 example metal ion concentration conditions of a stage leaching output solution and slag
Experimental results show that the lower iron content of the first-stage leaching solution produced by the first-stage experimental process can meet the requirement of the subsequent extraction production on the concentration of iron ions, and the slag produced by the second-stage leaching is lower in cobalt content after water washing.
Example 4
1. Adding 3 bags of raw materials such as Wash and 1 bag of Jianeng cobalt hydroxide into a slurrying tank, adding two-stage acid waste water for slag washing, and keeping the liquid-solid ratio at 4:1, continuously stirring for 30min, and then returning the mixture into a first-stage leaching serial kettle, wherein the end point of the solution is 5.5-6;
2. the first-stage leaching kettle is continuously stirred, the solution in the kettle continuously flows to the rear several stages of the serial kettles through continuously supplementing the slurry, the flow rate of the solution is 20 m/h, and the temperature in the kettle is ensured to be 80 ℃;
3. adding a proper amount of low second-stage leaching liquid (1.5) continuously into the first-stage front three stages of the first-stage serial kettles to adjust the leaching liquid to be first-stage 4.5, second-stage 4 and third-stage 3.5 in a grading manner so as to realize first-stage leaching;
4. adding a proper amount of 30% hydrogen peroxide into the second to fourth stages of the first-stage serial kettles to oxidize all ferrous ions in the solution to trivalent, flowing the solution to a subsequent reaction kettle under the stirring effect, and finally flowing into a thickener to realize solid-liquid separation and iron removal in the process;
5. performing multistage solid-liquid separation on the supernatant produced by the thickener in the step 4, and taking the supernatant as a copper material required by P204 extraction;
6. pumping the underflow slag generated by the thickener in the step 4 into a second-stage leaching kettle, adding sulfuric acid and a reducing agent, and carrying out second-stage full leaching;
7. carrying out solid-liquid separation on the leached solution in the step 6 by using a filter press, and washing filter pressing residues by using water;
8. and (3) returning the washing water generated in the step (7) to raw material pulping, and using the filtrate generated in the step (7) in a first-stage leaching adjustment solution.
Experimental results: the experimental results are shown in Table 1.
Table 1 example metal ion concentration conditions of a stage leaching output solution and slag
Experimental results show that the lower iron content in the first-stage leaching solution produced in the second-stage experimental process can meet the requirement of the subsequent extraction production on the concentration of iron ions, and the slag produced in the second-stage leaching process has lower cobalt content after water washing.
As described above, the invention provides a sectional leaching process for cobalt raw materials, the whole leaching process adopts two-stage multistage continuous leaching, the labor intensity of the whole process is obviously reduced compared with that of the traditional leaching mode, and the one-stage leaching is controlled to be carried out at a higher level in the leaching process, so that all iron ions in the one-stage leaching liquid are removed without iron removal and purification processes in the whole one-stage leaching process. Meanwhile, the low leaching liquid generated in the two-stage leaching process can be used for adjusting the one-stage leaching process, and meanwhile, the concentration of main metal ions in the one-stage leaching process can be improved.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims (4)

1. The sectional leaching method for the cobalt raw material is characterized by comprising the following steps of:
(1) Cobalt raw material and acid wastewater are mixed according to a liquid-solid ratio of 3-5:1, and stirring for 30-120min to obtain slurry;
(2) Transferring the slurry into a first-stage kettle of a first-stage leaching kettle, and continuously supplementing the slurry to enable the solution in the kettle to continuously flow into the next stages of kettles connected in series;
(3) Continuously adjusting the PH value of the first-stage leaching kettle to 3.5-4.0 in a segmented manner to realize continuous acid leaching;
(4) Adding an oxidant into the solution in the step (3) in sections, fully oxidizing ferrous iron generated in the leaching process to trivalent iron, hydrolyzing ferric iron ions, generating precipitate, entering slag, flowing the solution to a subsequent kettle under the stirring effect, and finally flowing into a thickener to realize solid-liquid separation;
(5) Press-filtering the supernatant produced by the thickener in the step (4) and then extracting to prepare cobalt salt solution;
(6) Pumping the underflow slag generated by the thickener in the step (4) into a two-stage leaching kettle, and adding sulfuric acid and a reducing agent in sections to carry out two-stage full leaching;
(7) Carrying out solid-liquid separation on the second-stage leaching solution in the step (6) by using a filter press, wherein part of filtrate is used for adjusting the first-stage leaching process by using acid, and the rest part is used for chemically removing iron;
(8) Washing the filter residue in the step (7) to remove residual cobalt metal in the filter residue, and allowing cobalt-containing washing water to enter the step (1) for pulping;
in the step (1), the theoretical cobalt ion concentration in the slurry is kept at 60-70g/L, the pH value of the slurry is 5.5-6, and the solution flow rate in one stage of leaching process is 10-25 m/h;
in the step (3), the first-stage leaching kettle is a hierarchical series device, and the number of stages of the first-stage leaching kettle is 5-7;
wherein in the step (5), the content of iron in the supernatant is lower than 0.005g/L.
2. The method for sectional leaching of cobalt raw material according to claim 1, wherein in the step (4), the oxidant is sodium hypochlorite or hydrogen peroxide or high-energy oxygen.
3. The method for sectional leaching of cobalt raw material according to claim 1, wherein in the step (6), a sectional two-stage continuous leaching process is adopted, and a leaching kettle is 3-5 stages.
4. The method according to claim 1, wherein in the step (6), the reducing agent comprises sodium metabisulfite, sodium sulfite, and sulfur dioxide.
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Citations (9)

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CN102126761A (en) * 2011-04-22 2011-07-20 桂金鸣 Method for preparing cobaltous sulfate
JP2013194269A (en) * 2012-03-17 2013-09-30 Mitsubishi Materials Corp Impurity removal method of cobalt content liquid
CN109234525A (en) * 2018-11-16 2019-01-18 温州大学 A kind of inexpensive leaching method of heterogenite
CN109518005A (en) * 2018-10-29 2019-03-26 安徽寒锐新材料有限公司 A kind of production method of battery grade cobalt sulfate crystal
CN111575480A (en) * 2020-05-12 2020-08-25 浙江中金格派锂电产业股份有限公司 Method for processing cobalt intermediate product
CN112359225A (en) * 2020-11-12 2021-02-12 格林美(江苏)钴业股份有限公司 Selective leaching process of rough cobalt hydroxide ore
CN113046573A (en) * 2021-03-11 2021-06-29 浙江中金格派锂电产业股份有限公司 Production process of cobalt sulfate
CN113502394A (en) * 2021-05-26 2021-10-15 广东佳纳能源科技有限公司 Method for recovering cobalt or nickel intermediate product

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101899571A (en) * 2009-11-05 2010-12-01 中国恩菲工程技术有限公司 Process for producing nickel and cobalt from nickel and cobalt ores
CN102126761A (en) * 2011-04-22 2011-07-20 桂金鸣 Method for preparing cobaltous sulfate
JP2013194269A (en) * 2012-03-17 2013-09-30 Mitsubishi Materials Corp Impurity removal method of cobalt content liquid
CN109518005A (en) * 2018-10-29 2019-03-26 安徽寒锐新材料有限公司 A kind of production method of battery grade cobalt sulfate crystal
CN109234525A (en) * 2018-11-16 2019-01-18 温州大学 A kind of inexpensive leaching method of heterogenite
CN111575480A (en) * 2020-05-12 2020-08-25 浙江中金格派锂电产业股份有限公司 Method for processing cobalt intermediate product
CN112359225A (en) * 2020-11-12 2021-02-12 格林美(江苏)钴业股份有限公司 Selective leaching process of rough cobalt hydroxide ore
CN113046573A (en) * 2021-03-11 2021-06-29 浙江中金格派锂电产业股份有限公司 Production process of cobalt sulfate
CN113502394A (en) * 2021-05-26 2021-10-15 广东佳纳能源科技有限公司 Method for recovering cobalt or nickel intermediate product

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