CN114561556A - Method for reducing COD (chemical oxygen demand) of P507 raffinate in nickel cobalt hydrometallurgy process through reverse extraction - Google Patents
Method for reducing COD (chemical oxygen demand) of P507 raffinate in nickel cobalt hydrometallurgy process through reverse extraction Download PDFInfo
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- CN114561556A CN114561556A CN202210017842.2A CN202210017842A CN114561556A CN 114561556 A CN114561556 A CN 114561556A CN 202210017842 A CN202210017842 A CN 202210017842A CN 114561556 A CN114561556 A CN 114561556A
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- raffinate
- organic phase
- kerosene
- extraction
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- 238000000605 extraction Methods 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 43
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000009854 hydrometallurgy Methods 0.000 title claims abstract description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title description 2
- 229910052760 oxygen Inorganic materials 0.000 title description 2
- 239000001301 oxygen Substances 0.000 title description 2
- 239000000126 substance Substances 0.000 title description 2
- 239000012074 organic phase Substances 0.000 claims abstract description 46
- 239000003350 kerosene Substances 0.000 claims abstract description 38
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 11
- 239000010941 cobalt Substances 0.000 claims abstract description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 238000004064 recycling Methods 0.000 claims abstract description 8
- 238000003723 Smelting Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000004065 wastewater treatment Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 229910017709 Ni Co Inorganic materials 0.000 claims 1
- 229910003267 Ni-Co Inorganic materials 0.000 claims 1
- 229910003262 Ni‐Co Inorganic materials 0.000 claims 1
- 239000002351 wastewater Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- LRDDEBYPNRKRRK-UHFFFAOYSA-N [Mg].[Co].[Ni] Chemical compound [Mg].[Co].[Ni] LRDDEBYPNRKRRK-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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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
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for reducing COD of P507 raffinate in a nickel cobalt hydrometallurgy process by reverse extraction. The method comprises the following steps: step 1, preparing an acidified organic phase; step 2, carrying out reverse extraction of the P507 raffinate and the acidified organic phase in an extraction tank according to a certain ratio; and 3, performing subsequent wastewater treatment on the P507 subjected to reverse extraction, recycling the organic phase, and performing open-circuit to a nickel-cobalt wet smelting extraction process after sufficient recycling times. After the treatment of the steps, the COD of the P507 raffinate is reduced by more than 500 mg/L. Wherein the acidified organic phase is selected from one of kerosene, kerosene + P204 and kerosene + P507; the P507 raffinate is selected from one or a mixture of two of the P507 raffinate of the nickel extraction separation line and the P507 raffinate of the cobalt extraction separation line. The method for reducing P507 raffinate COD in the nickel cobalt hydrometallurgy process through reverse extraction provided by the invention has strong applicability and strong operability. The COD of the P507 raffinate is obviously reduced by a reverse extraction means, and the input organic phase can be recycled to the extraction process after being recycled for a certain number of times.
Description
Technical Field
The invention relates to the field of nickel and cobalt smelting, in particular to a method for reducing P507 raffinate COD in a nickel and cobalt hydrometallurgy process by utilizing reverse extraction.
Background
One important use of nickel cobalt is in the manufacture of 3C battery and ternary battery materials. With the rise and the continuous popularization of new energy materials, the demand of nickel and cobalt will be larger and larger. Nickel cobalt and compounds thereof are mainly obtained by wet smelting, the wet smelting process comprises an extraction process, the prior industry commonly uses a process of P204 impurity removal and P507 nickel cobalt magnesium separation, and the process generates a large amount of P507 raffinate with high COD.
The high COD content of the P507 raffinate is the largest part of the wastewater treatment cost of the nickel cobalt hydrometallurgy industry. According to statistics, an enterprise which produces 3000 tons of nickel and cobalt in total per year has the wastewater (more than 80% of P507 raffinate) yield of 20 ten thousand tons, the cost for COD treatment of the wastewater reaches 2000 ten thousand yuan per year, and the COD in the wastewater is reduced by 100mg/L, and the average cost for the treatment of the wastewater per ton is reduced by 3 yuan. Therefore, the COD of the P507 raffinate is reduced from the source, which has great significance.
Based on the reasons, the invention provides a method for reducing P507 raffinate COD in a nickel-cobalt hydrometallurgy process by reverse extraction, which can obviously reduce the P507 raffinate COD.
Disclosure of Invention
The invention mainly aims to provide a method for reducing P507 raffinate COD in a nickel cobalt hydrometallurgy process by reverse extraction so as to reduce the wastewater treatment cost of the nickel cobalt hydrometallurgy.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for reducing P507 raffinate COD in a nickel cobalt hydrometallurgical process by reverse extraction. The method comprises the following steps: step 1, preparing an acidified organic phase; step 2, carrying out reverse extraction of the P507 raffinate and the acidified organic phase in an extraction tank according to a certain ratio; and 3, performing subsequent wastewater treatment on the P507 subjected to reverse extraction, recycling the organic phase, and performing open-circuit to a nickel-cobalt wet smelting extraction process after sufficient recycling times. Wherein the acidified organic phase is selected from one of kerosene, kerosene + P204 and kerosene + P507; the P507 raffinate is one or two of the raffinate of the nickel extraction separation line P507 and the raffinate of the cobalt extraction separation line P507.
Preferably, the acidified organic phase is selected from kerosene + P507.
More preferably, the kerosene is selected from sulfonated kerosene.
More preferably, the volume fraction of P507 in the acidified organic phase is above 5%.
Further, the volume ratio of the acidified organic phase to the P507 raffinate in the reverse extraction is more than 1: 1.
Preferably, the acid for acidifying the organic phase to occur is sulfuric acid.
More preferably, the amount of sulfuric acid is such that the pH of the P507 raffinate after back extraction is in the range of 0.5-4.
Preferably, the back extraction temperature is in the range of 10-60 ℃.
More preferably, the back extraction temperature is in the range of 25-60 ℃.
Further, the number of the back extraction stages is 1 or more.
Preferably, the number of reverse extraction stages is 2-10 stages.
The method for reducing the COD of the P507 raffinate in the nickel cobalt hydrometallurgy process through reverse extraction has the advantages of environmental protection, simple and easy process, no consumption of other reagents and low cost.
Drawings
FIG. 1 is a schematic flow chart of the method for reducing COD in P507 raffinate in a nickel cobalt hydrometallurgy process by reverse extraction.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As described in the background section, in order to effectively reduce the treatment cost of a large amount of high COD wastewater (mainly P507 wastewater) generated in the nickel cobalt hydrometallurgy process, the present invention provides a method for reducing the COD of P507 raffinate in the nickel cobalt hydrometallurgy process by reverse extraction, as shown in fig. 1, the method comprises the following steps: step 1, preparing an acidified organic phase; step 2, carrying out reverse extraction of the P507 raffinate and the acidified organic phase in an extraction tank according to a certain ratio; and 3, performing subsequent wastewater treatment on the P507 subjected to reverse extraction, recycling the organic phase, and performing open-circuit to a nickel-cobalt wet smelting extraction process after sufficient recycling times.
Preferably, the acidified organic phase is one of sulfonated kerosene, sulfonated kerosene + P204, and sulfonated kerosene + P507.
Preferably, the acid for acidifying the organic phase to occur is one or more of sulfuric acid or hydrochloric acid.
Further, when the acidified organic phase is sulfonated kerosene + P204, the volume fraction of the P204 is not less than 15%, and the number of reverse extraction stages is not less than 2.
Further, when the acidified organic phase is sulfonated kerosene + P507, the volume fraction of the P507 is not less than 10%, and the number of reverse extraction stages is not less than 2.
Preferably, the back extraction temperature is 30-50 ℃.
Preferably, the P507 raffinate is one or more of nickel line and cobalt line P507 raffinate, and COD is 2000-3000 mg/L.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
The acidified organic phase was sulfonated kerosene, the acid used for the generation was 8 equivalents sulfuric acid, the P507 raffinate was from a cobalt line, and the COD was 2031.44 mg/L. The back extraction O/A is 2:1, the temperature is 42.7 ℃, and the extraction grade is 4 grades. After 4-stage back extraction, the COD of the P507 raffinate was 1428.09mg/L, and the pH was 1.36. The sulfonated kerosene is opened and replaced after circulating for 15 times.
Example 2
The acidified organic phase was sulfonated kerosene + P204 with a P204 volume fraction of 15%, the acid used for the generation was 8 equivalents of sulfuric acid, the P507 raffinate was from the cobalt line, and the COD was 2719.34 mg/L. The reverse extraction O/A is 2:1, the temperature is 35.1 ℃, and the extraction grade is 2 grades. After 2-stage back extraction, the COD of the P507 raffinate was 1500.38mg/L, and the pH was 0.97. The organic phase is circulated for 40 times and then replaced by new open circuit.
Example 3
The acidified organic phase was sulfonated kerosene + P204, the P204 volume fraction was 15%, the acid used for the generation was 10 equivalents of hydrochloric acid, the P507 raffinate was from the nickel wire, and the COD was 3010.48 mg/L. The reverse extraction O/A is 3:1, the temperature is 31.58 ℃, and the extraction grade is 3 grades. After 3-stage back extraction, the COD of the P507 raffinate was 1350.91mg/L, and the pH was 0.82. The organic phase was cycled 17 times before opening the circuit and renewing.
Example 4
The acidified organic phase is sulfonated kerosene + P507, the volume fraction of P507 is 10%, the acid used for generation is 8 equivalent sulfuric acid, the P507 raffinate is mixed liquor with the volume ratio of 1:1 from the P507 raffinate of the nickel cobalt line, and the COD is 2576.45 mg/L. The reverse extraction O/A is 1:1, the temperature is 29.5 ℃, and the extraction grade is 2 grades. After 2-stage back extraction, the COD of the P507 raffinate was 1833.33mg/L, and the pH was 1.56. The organic phase was cycled 32 times before opening the circuit and renewing.
Example 5
The acidified organic phase is sulfonated kerosene + P507, the volume fraction of P507 is 15%, the acid used for generation is 8 equivalent sulfuric acid, the P507 raffinate comes from a cobalt line, and the COD is 3012.94 mg/L. The reverse extraction O/A is 3:1, the temperature is 45.9 ℃, and the extraction grade is 4 grades. After 4-stage back extraction, the COD of the P507 raffinate was 1115.37mg/L, and the pH was 0.67. The organic phase is circulated for 20 times and then replaced by new open circuit.
Example 6
The acidified organic phase is sulfonated kerosene + P507, the volume fraction of P507 is 15%, the acid used for generation is 10 equivalent hydrochloric acid, the P507 raffinate nickel line has COD of 2736.57 mg/L. The reverse extraction O/A is 4:1, the temperature is 40.5 ℃, and the extraction grade is 3 grades. After 3-stage back extraction, the COD of the P507 raffinate was 1202.30mg/L, and the pH was 1.01. The organic phase is circulated for 20 times and then replaced by new open circuit.
Example 7
The only difference from example 5 is that the back extraction stage was 2 stages, the temperature was 41.4 ℃ and the P507 end point pH was 0.70. The COD of the P507 raffinate after back extraction was 1095.36 mg/L.
Example 8
The only difference from example 5 is that the back extraction stage number is 3, the temperature is 40.3 ℃ and the P507 end point pH is 0.66. The COD of the P507 raffinate after back extraction was 1262.40 mg/L.
Example 9
The only difference from example 6 is that the back extraction stage number is 2, the temperature is 40.3 ℃ and the P507 end point pH is 1.10. The COD of the P507 raffinate after back extraction was 1230.01 mg/L.
Example 10
The only difference from example 9 is that the O/A is 2:1, the temperature is 38.4 ℃ and the P507 end point pH is 1.03. The COD of the P507 raffinate after back extraction was 1357.05 mg/L.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: the invention provides a method for reducing P507 raffinate COD in a nickel cobalt hydrometallurgy process by reverse extraction, which effectively reduces the P507 raffinate COD generated in the nickel cobalt hydrometallurgy process, obviously lightens the treatment pressure of subsequent wastewater and obviously reduces the wastewater treatment cost.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for reducing COD of P507 raffinate in a nickel cobalt hydrometallurgy process by reverse extraction is characterized by comprising the following steps:
step 1, preparing an acidified organic phase; step 2, carrying out reverse extraction of the P507 raffinate and the acidified organic phase in an extraction tank according to a certain ratio; and 3, performing subsequent wastewater treatment on the P507 subjected to reverse extraction, recycling the organic phase, and performing open-circuit to a nickel-cobalt wet smelting extraction process after sufficient recycling times.
2. The method of claim 1 wherein the acidified organic phase is selected from one of kerosene, kerosene + P204, kerosene + P507.
3. The method of claim 1 wherein the P507 raffinate COD is selected from one or a mixture of a nickel extraction separation line P507 raffinate and a cobalt extraction separation line P507 raffinate.
4. The method of claim 1 wherein the acid used to acidify the organic phase is one or more of hydrochloric acid and sulfuric acid.
5. The method of claim 2 wherein the kerosene is one or more of industrial kerosene, aviation kerosene and sulfonated kerosene.
6. The method of claim 2 wherein when the acidified organic phase is kerosene, the volume ratio of acidified organic phase to P507 raffinate is 3: preferably more than 1; when the acidified organic phase is kerosene + P204, the volume ratio of the acidified organic phase to the P507 raffinate is 1: preferably more than 1; when the acidified organic phase is kerosene + P507, the volume ratio of the acidified organic phase to the P507 raffinate is 1: preferably 1 or more.
7. The method for reducing COD in P507 raffinate in a nickel cobalt hydrometallurgical process through back extraction according to claim 6, wherein when said acidified organic phase is one of said kerosene, kerosene + P204, kerosene + P507, kerosene is preferably sulfonated kerosene; when the acidified organic phase is the kerosene + P204, the volume fraction of the P204 is preferably more than 5%; when the acidified organic phase is the kerosene + P507, the volume fraction of P507 is preferably 5% or more.
8. The method of any of claims 1 to 7 wherein when the acid used to acidify the organic phase is one or more of hydrochloric acid or sulfuric acid, the amount of acid used is such that the corresponding consumption of P507 raffinate after back extraction is maintained between 0.5 and 4.0.
9. The method for reducing COD in P507 raffinate from Ni-Co hydrometallurgy according to any one of claims 1 to 7 wherein the number of back extraction stages is preferably 1 or more.
10. The method of any of claims 1 to 7 wherein the back extraction temperature is 10-60 ℃ for reducing COD in the P507 raffinate from the nickel cobalt hydrometallurgical process.
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|---|---|---|---|
| CN202210017842.2A CN114561556A (en) | 2022-01-08 | 2022-01-08 | Method for reducing COD (chemical oxygen demand) of P507 raffinate in nickel cobalt hydrometallurgy process through reverse extraction |
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| CN202210017842.2A CN114561556A (en) | 2022-01-08 | 2022-01-08 | Method for reducing COD (chemical oxygen demand) of P507 raffinate in nickel cobalt hydrometallurgy process through reverse extraction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115321706A (en) * | 2022-07-29 | 2022-11-11 | 格林美（江苏）钴业股份有限公司 | Method for reducing COD (chemical oxygen demand) and total phosphorus in nickel-cobalt raffinate |
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| CN113384917A (en) * | 2020-03-13 | 2021-09-14 | 杭州中冶有色科技有限公司 | Oil removing method for raffinate or strip liquor produced in countercurrent extraction process |
| CN111517407A (en) * | 2020-04-30 | 2020-08-11 | 中国科学院过程工程研究所 | Method and device for recovering acidic extracting agent from acidic extraction system saponification wastewater |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115321706A (en) * | 2022-07-29 | 2022-11-11 | 格林美（江苏）钴业股份有限公司 | Method for reducing COD (chemical oxygen demand) and total phosphorus in nickel-cobalt raffinate |
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