CN115386737A - Method for recovering solution containing low-concentration cobalt and nickel - Google Patents
Method for recovering solution containing low-concentration cobalt and nickel Download PDFInfo
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- CN115386737A CN115386737A CN202210971851.5A CN202210971851A CN115386737A CN 115386737 A CN115386737 A CN 115386737A CN 202210971851 A CN202210971851 A CN 202210971851A CN 115386737 A CN115386737 A CN 115386737A
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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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- 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
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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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Abstract
The present disclosure provides a method for recovering a solution containing low-concentration cobalt and nickel, which comprises the following steps: step one, neutralizing and precipitating: adding sodium carbonate powder into a low-concentration cobalt-nickel solution, adjusting the pH value, stirring until the pH value is unchanged, and then carrying out the next step; step two, deep neutralization and precipitation: adding sodium hydroxide into the cobalt-nickel solution with the adjusted pH value to adjust the pH value, and stirring until the pH value is unchanged to perform the next step; step three, deeply removing impurities: adding sodium sulfide into the prepared strong alkali solution, and carrying out constant temperature reaction after heating; step four, filter pressing: pumping the solution neutralized in the third step into a filter press, pressing the filtrate into a sewage storage tank and discharging into a sewage workshop, and bagging the filter cake to be used for refining cobalt and nickel again. The method disclosed by the invention has the advantages that the neutralized slurry is extremely easy to filter, the filtering time is short, the efficiency is high, the energy consumption is low, the operation is easy, the sewage discharge after recovery can reach the industrial sewage discharge standard, and the production efficiency is improved.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy and sewage treatment, in particular to a method for recovering a solution containing low-concentration cobalt and nickel.
Background
Cobalt nickel metal has excellent properties of energy storage, corrosion resistance, wear resistance, high temperature resistance, high strength and the like, and is a key material for stainless steel, rechargeable batteries, electroplating, automobile parts and military devices. Therefore, it is called as an important strategic material for national economic development. In the process of cobalt-nickel hydrometallurgy, a large amount of waste water is generated, after most of cobalt-nickel metal is recovered, 2-5 g/L of cobalt and nickel in the waste liquid can be recovered and can not be directly discharged into a sewage process, cobalt and nickel sewage respectively belongs to two types of pollution and one type of pollution emission, and according to the emission standard of pollutants for copper, nickel and drilling industry (GB 25467-2010), the emission standard of the cobalt-nickel sewage in a workshop must reach
And Ni is less than or equal to 0.5mg/L. The conventional treatment methods are divided into two types: one is to directly add sodium carbonate to adjust the pH value, control the pH value at normal temperature, control the reaction time to neutralize and precipitate cobalt and nickel, then filter to form a filter cake and recover the cobalt and nickel; the other is directly adding sodium hydroxide (flake caustic soda or liquid caustic soda) to adjust the pH value, and recovering the cobalt and nickel at the same normal temperature. The first recovery mode has good filtering effect, but is difficult to rise when the pH value is adjusted to be about neutral, for example, a small amount of heavy metals such As Fe, cu, pb, cr, mn, as and the like are difficult to completely settle, and can not reach the discharge standard of a workshop; in the second recovery method, cobalt and nickel and a small amount of heavy metals such As Fe, cu, pb, cr, mn, and As can be completely precipitated, but the filtering effect is poor. The two treatment modes can not meet the requirements of industrial recovery and sewage treatment, so that the production efficiency is extremely low, the energy consumption is high, and the requirements of industrial sewage discharge standards can not be met.
Disclosure of Invention
In view of the problems in the prior art, the present disclosure aims to provide a method for recovering a solution containing low-concentration cobalt and nickel.
In order to achieve the above object, the present disclosure provides a method for recovering a solution containing low-concentration cobalt and nickel, comprising the steps of: step one, neutralizing and precipitating: adding sodium carbonate powder into a low-concentration cobalt-nickel solution, adjusting the pH value to 6-9, stirring until the pH value is unchanged, and then carrying out the next step; step two, deep neutralization and precipitation: adding sodium hydroxide into the cobalt-nickel solution with the adjusted pH value to adjust the pH value to 10-13, and stirring until the pH value is unchanged to carry out the next step; step three, deeply removing impurities: adding sodium sulfide into the prepared strong alkali solution, and carrying out constant temperature reaction after heating; step four, filter pressing: pumping the solution neutralized in the third step into a filter press, pressing the filtrate into a sewage storage tank, discharging the filtrate into a sewage workshop, and bagging the filter cake to be used for refining cobalt and nickel again.
In some embodiments, in step one, stirring is for 1-1.5h.
In some embodiments, in step two, the sodium hydroxide may be selected from liquid caustic or flake caustic.
In some embodiments, in step two, stirring is for 1-1.5h.
In some embodiments, the amount of sodium sulfide is 10-20 times the amount of metal impurities.
In some embodiments, in step three, the temperature is raised to 50-60 ℃.
In some embodiments, the reaction is carried out for 1-1.5h at constant temperature in step three.
The beneficial effects of this disclosure are as follows:
the method disclosed by the invention has the advantages that the neutralized slurry is extremely easy to filter, the filtering time is short, the efficiency is high, the energy consumption is low, the operation is easy, the sewage discharge after recovery can reach the industrial sewage discharge standard, the production efficiency is improved, the sewage can be discharged after being qualified through one-time treatment, the repeated treatment procedures are reduced, the labor intensity is reduced, and the environmental protection accident risk caused by heavy metal discharge is effectively avoided.
Detailed Description
The method for recovering a solution containing low concentration of cobalt and nickel according to the present disclosure is described in detail below.
The application discloses a method for recovering a solution containing low-concentration cobalt and nickel, which comprises the following steps: step one, neutralizing and precipitating: adding sodium carbonate powder into a low-concentration cobalt-nickel solution, adjusting the pH value to 6-9, stirring until the pH value is unchanged, and then carrying out the next step; step two, deep neutralization and precipitation: adding sodium hydroxide into the cobalt-nickel solution with the adjusted pH value to adjust the pH value to 10-13, and stirring until the pH value is unchanged to carry out the next step; step three, deeply removing impurities: adding sodium sulfide into the prepared strong alkali solution, and carrying out constant temperature reaction after heating; step four, filter pressing: pumping the solution neutralized in the third step into a filter press, pressing the filtrate into a sewage storage tank and discharging into a sewage workshop, and bagging the filter cake to be used for refining cobalt and nickel again.
The application aims at a method for recycling a solution containing low-concentration cobalt and nickel, the pH value is adjusted by adding sodium carbonate and sodium hydroxide at normal temperature, cobalt and nickel metal can be effectively neutralized and precipitated, the sodium carbonate is added firstly to adjust the solution to be neutral, so that the sodium carbonate is prevented from being added to be neutral and then the solution is saturated, the solution is sticky, the accurate pH value cannot be judged, auxiliary materials are wasted, the sodium hydroxide is added to be deep neutralized and precipitated, the pH value of the solution can be adjusted to meet the technological requirements, and the cobalt and nickel can be recycled to the maximum extent.
The sodium carbonate and the sodium hydroxide are added in a matching way, so that the filling power of byproducts can be improved, the viscosity can be reduced, the filter pressing is facilitated, the production efficiency is improved, after the pH value of the solution is adjusted in place, a small amount of heavy metals such as cobalt, nickel, chromium and copper can not reach the industrial sewage discharge standard, after a small amount of sodium sulfide is added for deep impurity removal, the discharge standard can be completely reached, the cobalt and nickel can be recovered to the maximum extent, and the industrial sewage discharge standard can also be reached.
In some embodiments, in step one, stirring is for 1-1.5h. The stirring time was too short to allow sufficient reaction.
In some embodiments, in step two, the sodium hydroxide may be selected from liquid caustic or flake caustic.
In some embodiments, in step two, stirring is for 1-1.5h. The stirring time was too short to allow sufficient reaction.
In some embodiments, the amount of sodium sulfide is 10-20 times the amount of metal impurities.
In some embodiments, in step three, the temperature is raised to 50-60 ℃. The solution is easy to crystallize at a too low temperature, the reaction effect is poor, the reaction is violent at a too high temperature, and the groove spraying accident is easy to happen.
In some embodiments, in step three, the reaction is carried out for 1-1.5h at constant temperature. The reaction time is short, the reaction is insufficient, and impurities cannot be removed completely.
[ test ]
Example 1
Step one, neutralizing and precipitating: adding sodium carbonate powder into a low-concentration cobalt-nickel solution, adjusting the pH value to 6, stirring for reacting for 30 minutes until the pH value is unchanged, and then carrying out the next step;
step two, deep neutralization and precipitation: adding sodium hydroxide liquid alkali into the cobalt-nickel solution with the adjusted pH value to adjust the pH value to 13, stirring and reacting for 1h until the pH value is unchanged, and carrying out the next step;
step three, deeply removing impurities: adding 10kg of sodium sulfide into the prepared strong alkali solution, heating to 50 ℃, and carrying out constant-temperature reaction for 1h;
step four, filter pressing: pumping the solution neutralized in the third step into a filter press, pressing the filtrate into a sewage storage tank, discharging the filtrate into a sewage workshop after the filtrate is detected to be qualified, and bagging the filter cake to be ready for refining cobalt and nickel again.
And (3) detection results:
TABLE 1 results of the detection of the strong base solution in step III
| Kind of element | Co | Ni | As | Cr | Zn | Mg | Fe | Pb | Cu |
| Content (mg/L) | 20 | 15 | ＜0.2 | 5.8 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | 18 |
TABLE 2 results of wastewater detection in step four
| Kind of element | Co | Ni | As | Cr | Zn | Mg | Fe | Pb | Cu |
| Content (mg/L) | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 |
TABLE 3 analysis of the cake results in step four
| Species of | H 2 O | Co | Ni | Cu | Zn | Fe |
| Content (%) | 64.12 | 7.7 | 2.66 | 8.95 | 1.10 | 0.06 |
Example 2
Step one, neutralizing and precipitating: adding sodium carbonate powder into a low-concentration cobalt-nickel solution, adjusting the pH value to 7, stirring and reacting for 1h until the pH value is unchanged, and then carrying out the next step;
step two, deep neutralization and precipitation: adding sodium hydroxide liquid alkali into the cobalt-nickel solution with the adjusted pH value to adjust the pH value to 12, stirring and reacting for 1 hour until the pH value is unchanged, and carrying out the next step;
step three, deeply removing impurities: adding 15kg of sodium sulfide into the prepared strong alkali solution, heating to 55 ℃, and then carrying out constant-temperature reaction for 1.5h;
step four, filter pressing: pumping the solution neutralized in the third step into a filter press, pressing the filtrate into a sewage storage tank, discharging the filtrate into a sewage workshop after the filtrate is detected to be qualified, and bagging the filter cake to be ready for extracting cobalt and nickel again.
And (3) detection results:
TABLE 4 detection results of the strong base solution in step III
| Kind of element | Co | Ni | As | Cr | Zn | Mg | Fe | Pb | Cu |
| Content (mg/L) | 16 | 20 | ＜0.2 | 18 | 26 | ＜0.2 | ＜0.2 | ＜0.2 | 20 |
TABLE 5 results of wastewater detection in step four
TABLE 6 analysis of the cake results in step four
| Species of | H 2 O | Co | Ni | Cu | Zn | Fe |
| Content (%) | 65.50 | 8.1 | 3.55 | 9.6 | 2.15 | 0.10 |
Example 3
Step one, neutralizing and precipitating: adding sodium carbonate powder into a low-concentration cobalt-nickel solution, adjusting the pH value to 8, stirring for reacting for 1 hour until the pH value is unchanged, and then carrying out the next step;
step two, deep neutralization and precipitation: adding sodium hydroxide liquid alkali into the cobalt-nickel solution with the adjusted pH value to adjust the pH value to 11, stirring and reacting for 1h until the pH value is unchanged, and carrying out the next step;
step three, deeply removing impurities: adding 20kg of sodium sulfide into the prepared strong alkali solution, and carrying out constant temperature reaction for 1.5h after the temperature is raised to 55 ℃;
step four, filter pressing: pumping the solution neutralized in the third step into a filter press, pressing the filtrate into a sewage storage tank, discharging the filtrate into a sewage workshop after the filtrate is detected to be qualified, and bagging the filter cake to be ready for refining cobalt and nickel again.
And (3) detection results:
TABLE 7 results of the detection of the strongly basic solution in step three
| Kind of element | Co | Ni | As | Cr | Zn | Mg | Fe | Pb | Cu |
| Content (mg/L) | 30 | 25 | ＜0.2 | 16 | 35 | ＜0.2 | ＜0.2 | ＜0.2 | 26 |
TABLE 8 results of wastewater detection in step four
| Kind of element | Co | Ni | As | Cr | Zn | Mg | Fe | Pb | Cu |
| Content (mg/L) | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 |
TABLE 9 analysis of the cake results in step four
Example 4
Step one, neutralizing and precipitating: adding sodium carbonate powder into a low-concentration cobalt-nickel solution, adjusting the pH value to 9, stirring and reacting for 1h until the pH value is unchanged, and then carrying out the next step;
step two, deep neutralization and precipitation: adding sodium hydroxide liquid alkali into the cobalt-nickel solution with the adjusted pH value to adjust the pH value to 10, stirring and reacting for 1 hour until the pH value is unchanged, and carrying out the next step;
step three, deeply removing impurities: adding 25kg of sodium sulfide into the prepared strong alkali solution, and carrying out constant-temperature reaction for 1.5 hours after heating to 60 ℃;
step four, filter pressing: pumping the solution neutralized in the third step into a filter press, pressing the filtrate into a sewage storage tank, discharging the filtrate into a sewage workshop after the filtrate is detected to be qualified, and bagging the filter cake to be ready for extracting cobalt and nickel again.
And (3) detection results:
TABLE 10 results of the detection of the strongly basic solution in step three
| Kind of element | Co | Ni | As | Cr | Zn | Mg | Fe | Pb | Cu |
| Content (mg/L) | 35 | 30 | ＜0.2 | 20 | 45 | ＜0.2 | ＜0.2 | ＜0.2 | 30 |
TABLE 11 results of wastewater detection in step four
| Kind of element | Co | Ni | As | Cr | Zn | Mg | Fe | Pb | Cu |
| Content (mg/L) | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.2 |
TABLE 12 analysis of the cake results in step four
| Species of | H 2 O | Co | Ni | Cu | Zn | Fe |
| Content (%) | 66.80 | 7.6 | 4.01 | 7.99 | 1.28 | 0.07 |
The examples 1-4 show that the treatment method can effectively treat the content of other metals in the solution after the cobalt and nickel are recovered to be less than or equal to 0.2mg/L at one time, completely accords with the industrial discharge standard, and can recover the cobalt and nickel to the maximum extent.
The above-disclosed features are not intended to limit the scope of the present disclosure, and therefore, all equivalent variations that are described in the claims of the present disclosure are intended to be included within the scope of the claims of the present disclosure.
Claims (7)
1. A method for recovering a solution containing low-concentration cobalt and nickel comprises the following steps:
step one, neutralizing and precipitating: adding sodium carbonate powder into a low-concentration cobalt-nickel solution, adjusting the pH value to 6-9, stirring until the pH value is unchanged, and then carrying out the next step;
step two, deep neutralization and precipitation: adding sodium hydroxide into the cobalt-nickel solution with the adjusted pH value to adjust the pH value to 10-13, and stirring until the pH value is unchanged to carry out the next step;
step three, deeply removing impurities: adding sodium sulfide into the prepared strong alkali solution, and carrying out constant temperature reaction after heating;
step four, filter pressing: pumping the solution neutralized in the third step into a filter press, pressing the filtrate into a sewage storage tank and discharging into a sewage workshop, and bagging the filter cake to be used for refining cobalt and nickel again.
2. The method for recovering a solution containing low concentration of cobalt and nickel according to claim 1,
in the first step, stirring is carried out for 1-1.5h.
3. The method for recovering a solution containing low concentration of cobalt and nickel according to claim 1,
in step two, the sodium hydroxide may be selected from liquid caustic soda or flake caustic soda.
4. The method for recovering a solution containing low concentration of cobalt and nickel according to claim 1,
in the second step, stirring is carried out for 1-1.5h.
5. The method for recovering a solution containing low concentration of cobalt and nickel according to claim 1,
the amount of the sodium sulfide is 10-20 times of the amount of metal impurities.
6. The method for recovering a solution containing low concentration of cobalt and nickel according to claim 1,
in the third step, the temperature is raised to 50-60 ℃.
7. The method for recovering a solution containing low concentration of cobalt and nickel according to claim 1,
in the third step, the reaction is carried out for 1 to 1.5 hours at constant temperature.
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| CN202210971851.5A CN115386737A (en) | 2022-08-12 | 2022-08-12 | Method for recovering solution containing low-concentration cobalt and nickel |
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| CN202210971851.5A CN115386737A (en) | 2022-08-12 | 2022-08-12 | Method for recovering solution containing low-concentration cobalt and nickel |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628764A (en) * | 2009-07-30 | 2010-01-20 | 浙江华友钴业股份有限公司 | Processing method of industrial waste water generated in hydrometallurgical process of nickel, cobalt and copper |
| CN111092273A (en) * | 2019-09-14 | 2020-05-01 | 湖南金源新材料股份有限公司 | Novel method for comprehensively recovering cobalt, nickel, manganese and lithium elements from ternary battery waste |
| CN113105020A (en) * | 2021-04-09 | 2021-07-13 | 瀚蓝工业服务(嘉兴)有限公司 | Method for recycling nickel resources in waste acid system |
| CN113636672A (en) * | 2021-06-30 | 2021-11-12 | 深圳市祺鑫环保科技有限公司 | Method for recovering nickel-containing wastewater |
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- 2022-08-12 CN CN202210971851.5A patent/CN115386737A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628764A (en) * | 2009-07-30 | 2010-01-20 | 浙江华友钴业股份有限公司 | Processing method of industrial waste water generated in hydrometallurgical process of nickel, cobalt and copper |
| CN111092273A (en) * | 2019-09-14 | 2020-05-01 | 湖南金源新材料股份有限公司 | Novel method for comprehensively recovering cobalt, nickel, manganese and lithium elements from ternary battery waste |
| CN113105020A (en) * | 2021-04-09 | 2021-07-13 | 瀚蓝工业服务(嘉兴)有限公司 | Method for recycling nickel resources in waste acid system |
| CN113636672A (en) * | 2021-06-30 | 2021-11-12 | 深圳市祺鑫环保科技有限公司 | Method for recovering nickel-containing wastewater |
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