CN114751468A - Method for treating TOC in nickel, cobalt or manganese finished product solution - Google Patents
Method for treating TOC in nickel, cobalt or manganese finished product solution Download PDFInfo
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- CN114751468A CN114751468A CN202210417399.8A CN202210417399A CN114751468A CN 114751468 A CN114751468 A CN 114751468A CN 202210417399 A CN202210417399 A CN 202210417399A CN 114751468 A CN114751468 A CN 114751468A
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- solution
- toc
- cobalt
- nickel
- manganese
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 18
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 17
- 239000010941 cobalt Substances 0.000 title claims abstract description 17
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 17
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 16
- 239000011572 manganese Substances 0.000 title claims abstract description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000654 additive Substances 0.000 claims abstract description 23
- 230000000996 additive effect Effects 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 12
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical group [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000000725 suspension Substances 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 20
- 238000005070 sampling Methods 0.000 description 12
- 230000000087 stabilizing effect Effects 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 5
- 229940099596 manganese sulfate Drugs 0.000 description 4
- 235000007079 manganese sulphate Nutrition 0.000 description 4
- 239000011702 manganese sulphate Substances 0.000 description 4
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 4
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 2
- 229940044175 cobalt sulfate Drugs 0.000 description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical class C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- 101000713575 Homo sapiens Tubulin beta-3 chain Proteins 0.000 description 1
- 102100036790 Tubulin beta-3 chain Human genes 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/10—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/08—Halides
- C01G51/085—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/10—Sulfates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for removing TOC from a nickel, cobalt or manganese finished product solution, which comprises the following steps: adding a proper amount of sulfuric acid or hydrochloric acid to adjust the pH value to meet the requirement of oxidation reaction, and heating the solution to a proper temperature; reacting organic molecules in the solution with the additive to generate volatile gas to overflow; the insoluble suspension in the solution was filtered. The method has the advantages of simple operation, short flow, high accuracy of removing the TOC, low cost and capability of obtaining the high-purity solution with lower TOC content.
Description
Technical Field
The invention relates to the technical field of chemical impurity removal, in particular to a method for treating TOC in nickel, cobalt or manganese finished product solution.
Background
Currently, in the industry, a method for removing TOC (total organic carbon) from a nickel, cobalt and manganese finished product solution mostly adopts activated carbon or resin for adsorption, the TOC removal precision of the method is not high, the solution cannot meet the increasing quality requirement of a battery material, in addition, the adsorption capacity of the activated carbon is limited, the replacement is frequent, and the operation is complicated; the resin is not sufficiently resolved, and the service life is short; the generated waste activated carbon and the failure resin are dangerous waste, the treatment process is complex, and the cost is higher. In addition, patent application CN113929154A discloses a method for removing TOC from cobalt chloride, in which a cobalt chloride solution is sequentially fed into a belt skimmer, a microcrystalline oil remover, an activated carbon oil remover, etc. to obtain a cobalt chloride solution from which TOC is removed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for treating TOC in a nickel, cobalt or manganese finished product solution, which has the advantages of simple operation, short flow, high TOC removal precision and low cost.
The invention is realized by the following technical scheme.
A method for processing TOC in a finished nickel, cobalt or manganese solution, the method comprising:
(1) adding sulfuric acid or hydrochloric acid into the finished solution of nickel, cobalt or manganese to control the end point pH1-4, and heating the solution to 50-90 ℃;
(2) adding a liquid additive A, a gas additive B or a solid additive C into the solution, and carrying out heat preservation reaction for 30-90 min; the liquid additive A is one or more of sulfuric acid, nitric acid, perchloric acid and hydrogen peroxide, the gas additive B is ozone, and the solid additive C is ammonium persulfate or sodium persulfate;
(3) filtering the solution obtained in the step (2) to remove suspended matters.
Further, in the step (2), the adding amount of the liquid additive A is 5ml-50ml/L (namely, the adding amount of the liquid additive A is 5ml-50ml per liter of the finished nickel, cobalt or manganese solution), the adding amount of the gas additive B is 1L-10L/L (namely, the adding amount of the gas additive B is 1L-10L per liter of the finished nickel, cobalt or manganese solution), and the adding amount of the solid additive C is 5g-15g/L (namely, the adding amount of the solid additive C is 5g-15g per liter of the finished nickel, cobalt or manganese solution).
Further, in the step (3), a filter element with 0.3 micron micropores is adopted for filtering to remove suspended matters of the solution.
The method for removing TOC from the nickel, cobalt or manganese finished product solution has the advantages of simple operation, short flow, high TOC removal precision and low cost, can obtain high-purity solution with lower TOC content, and can ensure that the minimum TOC content is lower than 1mg/l and the maximum TOC content is not more than 30 mg/l.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention provides a method for removing TOC from a nickel, cobalt or manganese finished product solution, which comprises the following steps: (1) adding a proper amount of sulfuric acid or hydrochloric acid to adjust the pH value to meet the requirement of oxidation reaction, and heating the solution to a proper temperature; (2) reacting organic molecules in the solution with the additive to generate volatile gas to overflow; (3) the insoluble suspension in the solution was filtered.
Example 1
Taking 1L of nickel sulfate finished product solution, adding sulfuric acid to adjust pH back to 1.0, stabilizing for 10min, heating the solution to 85 ℃, adding 15g of sodium persulfate, carrying out heat preservation reaction for 50min, filtering by adopting a filter element with 0.3 micron micropores, and sampling to detect the TOC of the solution before and after detection, 178mg/L of the TOC of the front solution, 0.3mg/L of the TOC of the rear solution and 4mg/L of SS.
Example 2
Taking 1L of nickel sulfate finished product solution, adding sulfuric acid to adjust pH back to 2.5, stabilizing for 10min, heating the solution to 80 ℃, adding 5g of ammonium persulfate, carrying out heat preservation reaction for 80min, filtering by adopting a 0.3 micron microporous filter element, and carrying out sampling detection on the front solution TOC, the front solution TOC 178mg/L, the rear solution TOC 3.6mg/L and SS 7mg/L of the solution.
Example 3
Taking 1L of cobalt sulfate finished product solution, adding sulfuric acid to adjust pH to 1.0, stabilizing for 10min, heating the solution to 60 ℃, adding 50ml of hydrogen peroxide, carrying out heat preservation reaction for 60min, filtering by adopting a 0.3 micron microporous filter element, and sampling to detect the TOC of the solution before and after detection, the TOC of the solution after detection, and the TOC of the solution after detection, 23mg/L of the solution after detection and SS of 5 mg/L.
Example 4
Taking 1L of cobalt sulfate finished product solution, adding sulfuric acid to adjust pH back to 2.0, stabilizing for 10min, heating the solution to 80 ℃, adding 13g of ammonium persulfate, carrying out heat preservation reaction for 70min, filtering by adopting a 0.3 micron microporous filter element, and carrying out sampling detection on the solution TOC before and after detection, 5.8mg/L of the solution TOC after detection, and SS 9 mg/L.
Example 5
Taking 1L of manganese sulfate finished product solution, adding sulfuric acid to adjust pH back to 3.0, stabilizing for 10min, heating the solution to 90 ℃, adding sodium persulfate 5g, carrying out heat preservation reaction for 30min, filtering by adopting a 0.3 micron microporous filter element, and sampling to detect the TOC of the solution before and after detection, the TOC of the solution after detection, and the TOC of the solution after detection, 17mg/L of the solution after detection and SS of 10 mg/L.
Example 6
Taking 1L of cobalt chloride finished product solution, adding hydrochloric acid to adjust pH to 1.0, stabilizing for 10min, heating the solution to 55 ℃, adding 10ml of perchloric acid, carrying out heat preservation reaction for 60min, filtering by adopting a 0.3 micron microporous filter element, and sampling to detect the TOC of the solution before and after detection, 121mg/L of the TOC of the solution before, 3.6mg/L of the TOC of the solution after detection and 3mg/L of SS.
Example 7
Taking 1L of cobalt chloride finished product solution, adding hydrochloric acid to adjust pH to 1.5, stabilizing for 10min, heating the solution to 85 ℃, adding 20ml of nitric acid, carrying out heat preservation reaction for 40min, filtering by adopting a filter element with 0.3 micron micropores, and sampling to detect the TOC of the solution before and after detection, 121mg/L of the TOC of the solution before, 1.5mg/L of the TOC of the solution after detection and 6mg/L of SS.
Example 8
Taking 1L of manganese sulfate finished product solution, adding sulfuric acid to adjust pH back to 3.0, stabilizing for 10min, heating the solution to 50 ℃, adding 3L of ozone, carrying out heat preservation reaction for 60min, filtering by adopting a 0.3 micron micropore filter element, and sampling and detecting a front solution TOC, a rear solution TOC and SS 4 mg/L.
Example 9
Taking 1L of manganese sulfate finished product solution, adding sulfuric acid to adjust pH back to 3.0, stabilizing for 10min, heating the solution to 55 ℃, adding 10ml of perchloric acid, carrying out heat preservation reaction for 60min, filtering by adopting a 0.3 micron microporous filter element, and sampling and detecting the TOC of the solution before and after detection, 58.7mg/L of the TOC of the solution before detection, 17.8mg/L of the TOC of the solution after detection and 1.6mg/L of SS.
Example 10
Taking 1L of manganese sulfate finished product solution, adding hydrochloric acid to adjust the pH value back to 3.0, stabilizing for 10min, heating the solution to 85 ℃, adding 15ml of sulfuric acid and nitric acid in total, carrying out heat preservation reaction for 65min, filtering by using a 0.3 micron microporous filter element, and sampling to detect the TOC of the solution before and after sampling, 58.7mg/L of the TOC of the solution before, 28.6mg/L of the TOC of the solution after sampling and 1.8mg/L of SS.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (3)
1. A method for processing TOC in a finished solution of nickel, cobalt or manganese, the method comprising:
(1) adding sulfuric acid or hydrochloric acid into the finished solution of nickel, cobalt or manganese to control the end point pH1-4, and heating the solution to 50-90 ℃;
(2) adding a liquid additive A, a gas additive B or a solid additive C into the solution, and carrying out heat preservation reaction for 30-90 min; the liquid additive A is one or more of sulfuric acid, nitric acid, perchloric acid and hydrogen peroxide, the gas additive B is ozone, and the solid additive C is ammonium persulfate or sodium persulfate;
(3) filtering the solution obtained in the step (2) to remove suspended matters.
2. The method for treating TOC in finished nickel, cobalt or manganese solution according to claim 1, wherein the amount of liquid additive A added in step (2) is 5ml-50ml/L, the amount of gas additive B added is 1L-10L/L, and the amount of solid additive C added is 5g-15 g/L.
3. The method for treating TOC in finished nickel, cobalt or manganese solution according to claim 1, wherein step (3) is performed by filtering with a 0.3 micron microporous filter element to remove suspended substances in the solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210417399.8A CN114751468A (en) | 2022-04-20 | 2022-04-20 | Method for treating TOC in nickel, cobalt or manganese finished product solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210417399.8A CN114751468A (en) | 2022-04-20 | 2022-04-20 | Method for treating TOC in nickel, cobalt or manganese finished product solution |
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| CN114751468A true CN114751468A (en) | 2022-07-15 |
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| CN202210417399.8A Pending CN114751468A (en) | 2022-04-20 | 2022-04-20 | Method for treating TOC in nickel, cobalt or manganese finished product solution |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704554A (en) * | 2009-07-16 | 2010-05-12 | 贵州红星发展股份有限公司 | Method for preparing manganese sulfate |
| CN106186078A (en) * | 2016-07-27 | 2016-12-07 | 中信大锰矿业有限责任公司大新锰矿分公司 | A kind of method utilizing oil refining spent acid to prepare manganese sulfate |
| CN106542583A (en) * | 2015-09-18 | 2017-03-29 | 江原大学校产学协力团 | The method that high-purity manganese sulphate is prepared from manganese sulfate waste liquid |
| CN109574359A (en) * | 2018-12-30 | 2019-04-05 | 江门市崖门新财富环保工业有限公司 | A kind of process for reclaiming of nickel-containing waste water Treated sewage reusing and nickel |
| CN113528818A (en) * | 2021-06-22 | 2021-10-22 | 江门市长优实业有限公司 | Method for removing impurities from nickel sulfate solution |
| CN113755906A (en) * | 2021-06-06 | 2021-12-07 | 阿克陶科邦锰业制造有限公司 | Method for removing impurities by oxidizing manganese sulfate first-stage purification liquid by using electrolytic manganese self-produced anode mud |
-
2022
- 2022-04-20 CN CN202210417399.8A patent/CN114751468A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704554A (en) * | 2009-07-16 | 2010-05-12 | 贵州红星发展股份有限公司 | Method for preparing manganese sulfate |
| CN106542583A (en) * | 2015-09-18 | 2017-03-29 | 江原大学校产学协力团 | The method that high-purity manganese sulphate is prepared from manganese sulfate waste liquid |
| CN106186078A (en) * | 2016-07-27 | 2016-12-07 | 中信大锰矿业有限责任公司大新锰矿分公司 | A kind of method utilizing oil refining spent acid to prepare manganese sulfate |
| CN109574359A (en) * | 2018-12-30 | 2019-04-05 | 江门市崖门新财富环保工业有限公司 | A kind of process for reclaiming of nickel-containing waste water Treated sewage reusing and nickel |
| CN113755906A (en) * | 2021-06-06 | 2021-12-07 | 阿克陶科邦锰业制造有限公司 | Method for removing impurities by oxidizing manganese sulfate first-stage purification liquid by using electrolytic manganese self-produced anode mud |
| CN113528818A (en) * | 2021-06-22 | 2021-10-22 | 江门市长优实业有限公司 | Method for removing impurities from nickel sulfate solution |
Non-Patent Citations (1)
| Title |
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Application publication date: 20220715 |