CN113215401B - High-efficiency impurity washing method for cobalt hydroxide salt - Google Patents
High-efficiency impurity washing method for cobalt hydroxide salt Download PDFInfo
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- CN113215401B CN113215401B CN202110347894.1A CN202110347894A CN113215401B CN 113215401 B CN113215401 B CN 113215401B CN 202110347894 A CN202110347894 A CN 202110347894A CN 113215401 B CN113215401 B CN 113215401B
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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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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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
Abstract
The invention discloses a cobalt hydroxide salt efficient impurity washing method. The technical scheme adopted by the invention is as follows: 1) Preparing cobalt hydroxide salt slurry; 2) Introducing carbon dioxide into the cobalt hydroxide salt slurry liquid at normal temperature and normal pressure, stirring for reaction, continuously adding sodium hydroxide, and controlling the pH value of the slurry liquid to be 8-14 stably; 3) Adding sodium carbonate into the reaction solution to carry out stirring reaction; 4) Carrying out liquid-solid separation on the reaction liquid to obtain primary filter residue and primary filtrate; 5) Heating the primary filtrate to obtain a reaction solution containing calcium carbonate and magnesium carbonate precipitates; 6) Carrying out liquid-solid separation on the reaction liquid to obtain secondary filter residue and secondary filtrate; 7) And returning the obtained secondary filtrate to a production system for size mixing. The method has the advantages of simple process, easy operation, stable quality and high purity of the obtained product, low cobalt loss of the product, high magnesium removal rate and high calcium removal rate which can reach more than 60 percent, greatly reduced production water and greatly reduced cost consumed by the subsequent treatment process.
Description
Technical Field
The invention belongs to the technical field of hydrometallurgy, and relates to a high-efficiency impurity washing method for cobalt hydroxide salt.
Background
At present, the production of the cobalt in China is mainly processed by cobalt hydroxide salt, and the advantage of using the cobalt hydroxide salt to produce the cobalt has wide application range, does not need to be provided with a special reaction kettle for treatment, can carry out reaction without heating, and can be used as a residual acid regulator in the production; the method has the disadvantages that other metal elements in the cobalt hydroxide salt react with acid during acid leaching, so that impurities in the leaching solution are more and more, the subsequent treatment is difficult, the treatment cost is overhigh, and the loss of cobalt is overhigh; the presence of impurity ions makes it difficult to separate cobalt ions from them during extraction, resulting in increased difficulty in controlling pH. Too high loss of cobalt can cause large economic loss of subsequent products, and high content of impurity ions can cause large amount of wastewater generated by subsequent treatment, high treatment cost and low recovery value. The method is necessary for reducing the treatment cost, improving the resource utilization rate and economic benefit, reducing the loss of cobalt and simultaneously reducing the impurity content in the cobalt hydroxide salt.
The existing cobalt hydroxide salt raw material is analyzed and detected, the grade of cobalt in the obtained raw material is more than 25%, the grade of magnesium is more than 4%, the grade of calcium is more than 0.4%, and the subsequent treatment process is influenced and the subsequent treatment cost is increased due to overhigh grade of calcium and magnesium.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a high-efficiency impurity washing method for cobalt hydroxide salt, which is used for reducing the content of calcium and magnesium impurities in the cobalt hydroxide salt, reducing the loss of cobalt during reaction, improving the product quality of the cobalt hydroxide salt and reducing the cost of the subsequent treatment process.
The invention adopts the following technical scheme: the efficient impurity washing method of cobalt hydroxide salt includes the following steps:
1) Preparing cobalt hydroxide salt into cobalt hydroxide salt slurry;
2) Introducing carbon dioxide into the cobalt hydroxide salt slurry liquid at normal temperature and normal pressure, stirring for reaction, continuously adding sodium hydroxide, and controlling the pH value of the slurry liquid to be stable within 8-14;
3) After the reaction is finished, adding sodium carbonate into the reaction solution to carry out stirring reaction;
4) After the reaction in the step 3) is finished, carrying out liquid-solid separation on the reaction liquid to obtain primary filter residue and primary filtrate;
5) Heating the primary filtrate to obtain a reaction solution containing calcium carbonate and magnesium carbonate precipitates;
6) Carrying out liquid-solid separation on the reaction liquid obtained in the step 5) to obtain secondary filter residue and secondary filtrate;
7) And returning the obtained secondary filtrate to a production system for size mixing.
Further, in the step 7), the obtained secondary filtrate contains cobalt ions, when the cobalt ions are enriched to a set concentration, sodium sulfide is added to recover the cobalt, and the solution is returned to the production system for use again.
Further, in the step 1), the solid ratio of water to the cobalt hydroxide slurry is 2 to 1.
Further, in step 2), the pH is adjusted to 11.5-12.5 with sodium hydroxide.
Further, in the step 2), the stirring speed is 150 to 800rpm.
Further, in the step 2), the reaction time is 0.5 to 8.0 hours.
Further, in the step 3), the adding amount of sodium carbonate is 8-20 g/L.
Further, in the step 3), the stirring speed is 150 to 600rpm.
Further, in the step 3), the reaction time is 0.2 to 8.0 hours.
Further, the addition amount of the sodium sulfide is 1.0 to 2.5 times of the theoretical addition amount.
In order to reduce the treatment cost of the cobalt hydroxide salt and improve the quality of the cobalt hydroxide salt product, the loss of cobalt needs to be reduced, and the grade of calcium and magnesium impurities in the cobalt hydroxide salt is reduced; the method comprises the steps of slurrying cobalt hydroxide salt and water according to a certain liquid-solid ratio, introducing carbon dioxide into slurried liquid at normal temperature and normal pressure, continuously adding sodium hydroxide to adjust the pH value to be stable within a certain range, continuously introducing carbon dioxide, reacting reaction liquid with the carbon dioxide to generate magnesium bicarbonate and calcium bicarbonate, introducing the magnesium bicarbonate and the calcium bicarbonate into the solution, adding sodium carbonate to carry out stirring reaction after the reaction is finished, and carrying out liquid-solid separation after the reaction is finished to obtain primary filter residue and primary filtrate. And heating the primary filtrate to obtain a reaction liquid containing calcium carbonate and magnesium carbonate precipitates, carrying out liquid-solid separation on the reaction liquid to obtain secondary filter residues and secondary filtrate, removing calcium and magnesium impurities in the form of calcium carbonate and magnesium carbonate, and returning the secondary filtrate to a production system for size mixing.
The invention has the following beneficial effects:
(1) The product prepared by the invention has high quality, stable components, less cobalt loss and low contents of calcium and magnesium impurities.
(2) The method has the advantages of short flow, simple operation, high magnesium removal efficiency, high magnesium removal rate and high calcium removal rate which can both reach more than 60 percent, reduces the treatment cost for the subsequent treatment process, and is suitable for industrial production.
(3) The invention can not bring other harmful impurities, further omits the subsequent treatment process and reduces the treatment consumption cost.
(4) The water used by the invention can be returned to the production system for use, and the problem of water expansion can be well relieved.
Drawings
FIG. 1 is a process flow diagram of an embodiment of the invention;
FIG. 2 is a schematic view of the structure of a reaction apparatus used in the present invention.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings. It will be appreciated by those skilled in the art that the examples are provided merely to assist in understanding the present disclosure and are not to be construed as limiting the invention.
Example 1
In an embodiment of the method for removing impurities from cobalt hydroxide salt according to the present invention, the method for removing impurities from cobalt hydroxide salt includes the following steps:
1) Taking 50g of cobalt hydroxide salt as a raw material and 600mL of water for slurrying, and controlling the stirring speed to be 150rpm;
2) Introducing carbon dioxide into the reaction solution, continuously adding sodium hydroxide to adjust and control the pH value to be 9 stably, and reacting for 1h;
3) After the reaction is finished, adding 8g of sodium carbonate into the reaction solution, and stirring for reaction;
4) After the stirring reaction is finished, carrying out solid-liquid separation on the reaction liquid to obtain primary filter residue and primary filtrate;
5) Heating the primary filtrate to obtain a reaction solution containing calcium carbonate and magnesium carbonate precipitates;
6) Carrying out liquid-solid separation on the reaction liquid to obtain secondary filter residue and secondary filtrate; returning the obtained secondary filtrate to a production system for size mixing;
7) And carrying out element analysis and detection on the slag sample, the liquid sample and the raw materials.
The reaction apparatus used in the present invention is shown in FIG. 2.
Table 1.1 shows the content (g/L) of major elements in cobalt hydroxide salt
Table 1.2 shows the content (g/L) of the essential element in the secondary filtrate
Table 1.3 shows the primary residue content (%)
Example 2
In an embodiment of the method for removing impurities from cobalt hydroxide salt according to the present invention, the method for removing impurities from cobalt hydroxide salt includes the following steps:
1) Taking 80g of cobalt hydroxide salt as a raw material and 400ml of water for slurrying, and controlling the stirring speed to be 350rpm;
2) Introducing carbon dioxide into the reaction solution, continuously adding sodium hydroxide to control the pH value to be stable at 11, and reacting for 6 hours;
3) After the reaction is finished, 10g of sodium carbonate is added into the reaction solution for stirring reaction;
4) After the stirring reaction is finished, carrying out solid-liquid separation on the reaction liquid to obtain primary filter residue and primary filtrate;
5) Heating the primary filtrate to obtain a reaction solution containing calcium carbonate and magnesium carbonate precipitates;
6) Carrying out liquid-solid separation on the reaction liquid to obtain secondary filter residue and secondary filtrate; returning the obtained secondary filtrate to a production system for size mixing;
7) And carrying out element analysis and detection on the slag sample, the liquid sample and the raw materials.
Table 2.1 shows the content (g/L) of major elements in cobalt hydroxide salt
Table 2.2 shows the content of major elements (g/L) in the secondary filtrate
Table 2.3 shows the primary residue content (%)
Example 3
In an embodiment of the method for removing impurities from cobalt hydroxide salt according to the present invention, the method for removing impurities from cobalt hydroxide salt includes the following steps:
1) Taking 100g of cobalt hydroxide salt as a raw material and 400ml of water for slurrying, and controlling the stirring speed to be 300 rpm;
2) Introducing carbon dioxide into the reaction solution, continuously adding sodium hydroxide to control the pH value to be stable at 12, and reacting for 6 hours;
3) After the reaction, 12g of sodium carbonate was added to the reaction solution to conduct a stirring reaction
4) After the stirring reaction is finished, carrying out solid-liquid separation on the reaction liquid to obtain primary filter residue and primary filtrate;
5) Heating the primary filtrate to obtain a reaction solution containing calcium carbonate and magnesium carbonate precipitates;
6) Carrying out liquid-solid separation on the reaction liquid to obtain secondary filter residue and secondary filtrate; returning the obtained secondary filtrate to a production system for size mixing;
7) And carrying out element analysis and detection on the slag sample, the liquid sample and the raw materials.
Table 3.1 shows the content (g/L) of major elements in cobalt hydroxide salt
Table 3.2 shows the content (g/L) of the essential elements in the secondary filtrate
Table 3.3 shows the primary residue content (%)
Example 4
In an embodiment of the method for removing impurities from cobalt hydroxide salt according to the present invention, the method for removing impurities from cobalt hydroxide salt includes the following steps:
1) Taking 200g of cobalt hydroxide salt as a raw material and 800ml of water for slurrying, and controlling the stirring speed to be 700rpm;
2) Introducing carbon dioxide into the reaction solution, continuously adding sodium hydroxide to control the pH value to be stable at 13, and reacting for 5 hours;
3) After the reaction is finished, adding 15g of sodium carbonate into the reaction solution, and stirring for reaction;
4) After the stirring reaction is finished, carrying out solid-liquid separation on the reaction liquid to obtain primary filter residue and primary filtrate;
5) Heating the primary filtrate to obtain a reaction solution containing calcium carbonate and magnesium carbonate precipitates;
6) Carrying out liquid-solid separation on the reaction liquid to obtain secondary filter residue and secondary filtrate; returning the obtained secondary filtrate to a production system for size mixing;
7) And carrying out element analysis and detection on the slag sample, the liquid sample and the raw materials.
Table 4.1 shows the content (g/L) of the main element of cobalt hydroxide salt
Table 4.2 shows the content (g/L) of the essential elements in the secondary filtrate
Table 4.3 shows the primary residue content (%)
Example 5
In an embodiment of the method for removing impurities from cobalt hydroxide salt according to the present invention, the method for removing impurities from cobalt hydroxide salt includes the following steps:
1) Taking 200g of cobalt hydroxide salt as a raw material and 700ml of water for slurrying, and controlling the stirring speed to be 500rpm;
2) Introducing carbon dioxide into the reaction solution, continuously adding sodium hydroxide to control the pH value to be stable at 12, and reacting for 3 hours;
3) After the reaction is finished, 20g of sodium carbonate is added into the reaction solution to be stirred and reacted;
4) After the stirring reaction is finished, carrying out solid-liquid separation on the reaction liquid to obtain primary filter residue and primary filtrate;
5) Heating the primary filtrate to obtain a reaction solution containing calcium carbonate and magnesium carbonate precipitates;
6) Carrying out liquid-solid separation on the reaction liquid to obtain secondary filter residue and secondary filtrate; returning the obtained secondary filtrate to a production system for size mixing;
7) And carrying out element analysis and detection on the slag sample, the liquid sample and the raw materials.
Table 5.1 shows the content (g/L) of major elements in cobalt hydroxide salt
Table 5.2 shows the content (g/L) of the essential elements in the secondary filtrate
Table 5.3 shows the primary residue content (%)
The method has the advantages of simple process, easy operation, stable quality and high purity of the obtained product, over 60 percent of both the magnesium removal rate and the calcium removal rate, cobalt loss prevention by adding sodium sulfide for recovering cobalt, water return to a system in the production process, water expansion problem prevention and cost reduction of subsequent treatment process consumption.
The present invention is not limited to the above embodiments, and various modifications and changes can be made to the present invention. Any modifications, improvements, equivalents and the like of the above embodiments according to the technical spirit of the present invention are within the scope of the present invention.
Claims (4)
1. The efficient impurity washing method of cobalt hydroxide salt is characterized by comprising the following steps:
1) Preparing cobalt hydroxide salt into cobalt hydroxide salt slurry;
2) Introducing carbon dioxide into the cobalt hydroxide salt slurry liquid at normal temperature and normal pressure, stirring for reaction, continuously adding sodium hydroxide, and controlling the pH value of the slurry liquid to be stable within 8-14;
3) After the reaction is finished, adding sodium carbonate into the reaction solution to carry out stirring reaction;
4) After the reaction in the step 3) is finished, carrying out liquid-solid separation on the reaction liquid to obtain primary filter residue and primary filtrate;
5) Heating the primary filtrate to obtain a reaction solution containing calcium carbonate and magnesium carbonate precipitates;
6) Carrying out liquid-solid separation on the reaction liquid obtained in the step 5) to obtain secondary filter residue and secondary filtrate;
7) Returning the obtained secondary filtrate to a production system for size mixing;
during slurrying in the step 1), the solid ratio of water to the slurrying solution of the cobalt hydroxide salt is 2 to 1;
in the step 2), the stirring speed is 150 to 800rpm, and the reaction time is 0.5 to 8.0 hours;
in the step 3), the adding amount of sodium carbonate is 8-20g/L, the stirring speed is 150-600rpm, and the reaction time is 0.2-8.0 h.
2. The method for efficiently washing impurities with cobalt hydroxide salt according to claim 1, wherein in the step 7), the obtained secondary filtrate contains cobalt ions, when the cobalt ions are enriched to a set concentration, sodium sulfide is added to recover cobalt, and the solution is returned to the production system for use again.
3. The efficient impurity washing method for the cobalt hydroxide salt according to claim 2, wherein in the step 7), the addition amount of the sodium sulfide is 1.0 to 2.5 times of the theoretical addition amount.
4. The method for efficiently washing impurities with cobalt hydroxide salt according to claim 1 or 2, wherein in the step 2), the pH is adjusted to 11.5-12.5 with sodium hydroxide.
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| CN111218567A (en) * | 2020-01-10 | 2020-06-02 | 衢州华友钴新材料有限公司 | Method for reducing magnesium from cobalt (nickel) salt high-efficiency source |
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