CN110172581A - A method of LITHIUM BATTERY manganese sulfate is prepared from anti-copper manganese liquid - Google Patents

A method of LITHIUM BATTERY manganese sulfate is prepared from anti-copper manganese liquid Download PDF

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Publication number
CN110172581A
CN110172581A CN201910359623.0A CN201910359623A CN110172581A CN 110172581 A CN110172581 A CN 110172581A CN 201910359623 A CN201910359623 A CN 201910359623A CN 110172581 A CN110172581 A CN 110172581A
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copper
solution
manganese
lithium battery
adjusted
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刘楠楠
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Wenzhou University
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Wenzhou University
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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
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0084—Treating solutions
    • 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
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • 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
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
    • 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
    • C22B47/00—Obtaining manganese
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a kind of methods from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate, include following steps: (1) anti-copper manganese liquid being carried out stratification, after grease is sufficiently separated, remove upper layer organic extractant；(2) pH value of remaining solution is adjusted to 2.0-2.5, and is filtered；(3) filtered solution will be adjusted and carry out copper extraction；(4) pH value of raffinate after copper extraction is adjusted to 1.8-2.2, and is concentrated；(5) extractant p204 is added in solution after concentration to be extracted；(6) H is passed through in solution after the extraction2S gas cleans, and filters；(7) pH value of solution after filtering is adjusted to 4.0-6.5, and is filtered again；(8) filtered solution will be adjusted and crystallization is dried, obtain LITHIUM BATTERY manganese sulfate product.This method has many advantages, such as that low production cost, Environmental Safety, economic value are high.

Description

A method of LITHIUM BATTERY manganese sulfate is prepared from anti-copper manganese liquid
Technical field
The present invention relates to a kind of preparation methods of LITHIUM BATTERY manganese sulfate, and in particular to a kind of to prepare LITHIUM BATTERY from anti-copper manganese liquid The method of manganese sulfate.
Background technique
Anti- copper manganese liquid is that a kind of stripping section nonferrous metal ion containing there are many obtained is extracted in nickel cobalt hydrometallurgy Acid solution, because copper, manganese ion concentration are higher, therefore named anti-copper manganese liquid.Anti- copper manganese liquid is according to hydrometallurgy mineral aggregate tenor Its ingredient is slightly different, general 8-20g/L containing Cu, Mn 12-25g/L, remaining is the lower foreign metal of content: Ca 0.1- 0.5g/L, Zn 0.1-2g/L, Co 0.05-0.1 g/L, Fe0.001-0.01g/L, Ni 0.001-0.01g/L, Mg 0.001-0.01g/L, sulfuric acid 20-35g/L.
Anti- copper manganese liquid uses the modes such as iron replacement or extraction to extract copper metal, remaining manganese containing solution after generally adjusting pH value Since dopant species are more, processing is scrapped after being generally precipitated as manganese slag, this method does not make full use of the promoter manganese in solution, makes At the wasting of resources and environmental pollution.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides it is a kind of from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate method, This method has many advantages, such as that low production cost, Environmental Safety, economic value are high.
To achieve the above object, the present invention provides a kind of methods from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate, including There are following steps:
(1) anti-copper manganese liquid is subjected to stratification, after grease is sufficiently separated, removes upper layer organic extractant；
(2) pH value of remaining solution is adjusted to 2.0-2.5, and is filtered；
(3) filtered solution will be adjusted and carry out copper extraction；
(4) pH value of raffinate after copper extraction is adjusted to 1.8-2.2, and is concentrated；
(5) extractant p204 is added in solution after concentration to be extracted；
(6) H is passed through in solution after the extraction2S gas cleans, and filters；
(7) pH value of solution after filtering is adjusted to 4.0-6.5, and is filtered again；
(8) filtered solution will be adjusted and crystallization is dried, obtain LITHIUM BATTERY manganese sulfate product.
The present invention can be further arranged to stratification time >=2h of anti-copper manganese liquid in step (1).Can prevent in this way because The anti-remaining Microamounts of Cobalt And Nickel extractant of copper manganese liquid enters copper extraction workshop section and pollutes copper extractant.
It is electrolytic manganese powder that the present invention, which can be further arranged to adjust in step (2) substance used in solution ph, fineness >= 325 mesh, reaction time 2-4h.
The present invention can be further arranged to copper extraction in step (3) and be extracted using counter-current fractionation, and control raffinate containing Cu < 0.5g/L.
It is electrolytic manganese powder that the present invention, which can be further arranged to adjust in step (4) substance used in solution ph, fineness >= 325 mesh, reaction time 3-5h, 30~45g/L containing Mn after control solution concentration.
The present invention can be further arranged to p204 extraction in step (5) and use multistage cross flow extraction process, and control p204 Concentration 0.7-1.5mol/L, compares 4:1-8:1, time of contact 2.5-4min, 4~8 grades of series, controls by 40-55 DEG C of extraction temperature Raffinate Cu < 0.001g/L, Fe < 0.001g/L, Ca < 0.01g/L, Zn < 0.001g/L.
The present invention can be further arranged to H in step (6)2S dosage: m(H2S)=1.1~1.3 [m (Cu)+m (Ni)+m (Co)], in formula m indicate substance amount, 40-80 DEG C of reaction temperature, reaction time 3-5h.
It is electrolytic manganese powder that the present invention, which can be further arranged to adjust in step (7) substance used in solution ph, fineness >= 325 mesh, reaction time 3-5h.
The chemical reaction occurred in present invention process process are as follows:
(1) pH value of solution is adjusted:
Mn+H2SO4= MnSO4+ H2↑
(2) H2S removal of impurities:
Me2++H2S= MeS↓+2H+(Me Co, Cu, Ni etc.)
The beneficial effects of the present invention are: 1, production cost is low.Auxiliary material needed for this method is cheap and easy to get, and dosage is less；It is used to set Standby is industrial production commonly used equipment, and depreciable cost is lower；The energy-output ratios such as water, electricity, vapour are low in production process.2, environmental protection peace Entirely.For this method process conditions without rigors such as high temperature and pressure, production process is safer.After the resources such as copper, manganese are effectively extracted Gained waste water metal impurities total amount is lower, is easily handled, while reducing the stockpiling of a large amount of manganese slags.
Specific embodiment
Embodiment 1
Anti- copper manganese liquid 11.2g/L containing Cu, the Mn 19.3g/L of 1L, remaining foreign metal: Ca 0.12g/L, Zn 1.5g/L, Co 0.06 g/L, Fe0.003g/L, Ni 0.001g/L, Mg 0.002g/L, sulfuric acid 21.5g/L.Stratification 4h first, by upper layer Residual organic solvent removal.Anti- copper manganese liquid is added in the electrolytic manganese powder of appropriate >=325 mesh, and is stirred, 2h is reacted, controls final pH Value is 2.0, and counter-current fractionation extraction process extracting copper is used after filtering, and raffinate contains Cu0.2g/L.Continue to use the electricity of >=325 mesh It solves manganese powder and adjusts extract liquor pH value to 1.8, react 3h, 30~45g/L containing Mn after control solution concentration, using multistage after filtering The cross current solvent extraction solution controls P204 concentration 1.2mol/L, 48 DEG C of extraction temperature, compares 5:1, time of contact 3min, series 5 Grade.Raffinate contains Cu0.0003g/L, Fe0.0002g/L, Ca0.004g/L, Zn0.0002g/L, Mn34.6g/L after extraction.It will The H of 0.0012mol2S gas is passed through above-mentioned raffinate, controls 50 DEG C of reaction temperature, reaction time 3.5h, used after filtering >= The electrolytic manganese powders of 325 mesh adjusts pH value to 4.5, reaction time 3.5h, solution evaporating, concentrating and crystallizing, and carries out being centrifuged while hot Filter, obtain manganese sulfate solid≤105 DEG C of low temperature dryings to get LITHIUM BATTERY manganese sulfate product, the specific ingredient of the product and with electricity Pond grade manganese sulfate qualified product index is as shown in the table:
Embodiment 2
Anti- copper manganese liquid 18.8g/L containing Cu, the Mn 23.6g/L of 1L, remaining foreign metal: Ca 0.41g/L, Zn 1.8g/L, Co 0.08 g/L, Fe0.004g/L, Ni 0.002g/L, Mg 0.01g/L, sulfuric acid 18.5g/L.Stratification 6h first, by upper layer Residual organic solvent removal.Anti- copper manganese liquid is added in the electrolytic manganese powder of appropriate >=325 mesh, and is stirred, 3h is reacted, controls final pH Value is 2.3, and counter-current fractionation extraction process extracting copper is used after filtering, and raffinate contains Cu0.3g/L.Continue to use the electricity of >=325 mesh It solves manganese powder and adjusts extract liquor pH value to 2, react 4h, 30~45g/L containing Mn after control solution concentration, using multistage wrong after filtering Stream extracts the solution, controls P204 concentration 1.5mol/L, 40 DEG C of extraction temperature, compares 4:1, time of contact 2.5min, series 8 Grade.Raffinate contains Cu0.0003g/L, Fe0.0002g/L, Ca0.01g/L, Zn0.0002g/L, Mn41.9g/L after extraction.It will The H of 0.0013mol2S gas is passed through above-mentioned raffinate, controls 80 DEG C of reaction temperature, reaction time 5h, and >=325 are used after filtering Purpose electrolytic manganese powder adjusts pH to 6.5, reaction time 5h, solution evaporating, concentrating and crystallizing, and carries out centrifugal filtration while hot, obtains sulphur Sour manganese solid≤105 DEG C of low temperature dryings to get LITHIUM BATTERY manganese sulfate product, the specific ingredient of the product and with LITHIUM BATTERY manganese sulfate Qualified product index is as shown in the table:
Embodiment 3
Anti- copper manganese liquid 9.8g/L containing Cu, the Mn 12.4g/L of 1L, remaining foreign metal: Ca 0.11g/L, Zn 0.5g/L, Co 0.05 g/L, Fe0.003g/L, Ni 0.002g/L, Mg 0.01g/L, sulfuric acid 15.2g/L.Stratification 2h first, by upper layer Residual organic solvent removal.Anti- copper manganese liquid is added in the electrolytic manganese powder of appropriate >=325 mesh, and is stirred, 4h is reacted, controls final pH Value 2.5, uses counter-current fractionation extraction process extracting copper after filtering, raffinate contains Cu0.1g/L.Continue to use the electrolysis of >=325 mesh Manganese powder adjusts extract liquor pH value to 2.2, reacts 5h, 30~45g/L containing Mn after control solution concentration, using multistage wrong after filtering Stream extract the solution, control P204 concentration 0.7mol/L, 55 DEG C of extraction temperature, compare 8:1, time of contact 4min, 4 grades of series. Raffinate contains Cu0.0001g/L, Fe0.0002g/L, Ca0.008g/L, Zn0.0001g/L, Mn25.3g/L after extraction.It will The H of 0.0011mol2S gas is passed through above-mentioned raffinate, controls 40 DEG C of reaction temperature, reaction time 3h, and >=325 are used after filtering Purpose electrolytic manganese powder adjusts pH to 4, reaction time 3h, solution evaporating, concentrating and crystallizing, and carries out centrifugal filtration while hot, obtains sulfuric acid Manganese solid≤105 DEG C of low temperature dryings to get LITHIUM BATTERY manganese sulfate product, the specific ingredient of the product and with LITHIUM BATTERY manganese sulfate close Lattice product index is as shown in the table:

Claims (8)

1. a kind of method from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate, it is characterised in that: include following steps:
(1) anti-copper manganese liquid is subjected to stratification, after grease is sufficiently separated, removes upper layer organic extractant；
(2) pH value of remaining solution is adjusted to 2.0-2.5, and is filtered；
(3) filtered solution will be adjusted and carry out copper extraction；
(4) pH value of raffinate after copper extraction is adjusted to 1.8-2.2, and is concentrated；
(5) extractant p204 is added in solution after concentration to be extracted；
(6) H is passed through in solution after the extraction2S gas cleans, and filters；
(7) pH value of solution after filtering is adjusted to 4.0-6.5, and is filtered again；
(8) filtered solution will be adjusted and crystallization is dried, obtain LITHIUM BATTERY manganese sulfate product.
2. a kind of method from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate according to claim 1, it is characterised in that: step (1) stratification time >=2h of anti-copper manganese liquid in.
3. a kind of method from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate according to claim 1, it is characterised in that: step (2) it is electrolytic manganese powder, fineness >=325 mesh, reaction time 2-4h that substance used in solution ph is adjusted in.
4. a kind of method from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate according to claim 1, it is characterised in that: step (3) copper extraction is extracted using counter-current fractionation in, and controls raffinate < containing Cu 0.5g/L.
5. a kind of method from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate according to claim 1, it is characterised in that: step (4) it is electrolytic manganese powder, fineness >=325 mesh, reaction time 3-5h, control solution concentration that substance used in solution ph is adjusted in 30~45g/L containing Mn afterwards.
6. a kind of method from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate according to claim 1, it is characterised in that: step (5) p204 extraction uses multistage cross flow extraction process in, and controls p204 concentration 0.7-1.5mol/L, and 40-55 DEG C of extraction temperature, Compared to 4:1-8:1, time of contact 2.5-4min, 4~8 grades of series, raffinate Cu < 0.001g/L, Fe < 0.001g/L are controlled, Ca < 0.01g/L, Zn < 0.001g/L.
7. a kind of method from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate according to claim 1, it is characterised in that: step (6) H in2S dosage: m(H2S)=1.1~1.3 [m (Cu)+m (Ni)+m (Co)], m indicates the amount of substance, reaction temperature in formula 40-80 DEG C, reaction time 3-5h.
8. a kind of method from anti-copper manganese liquid preparation LITHIUM BATTERY manganese sulfate according to claim 1, it is characterised in that: step (7) it is electrolytic manganese powder, fineness >=325 mesh, reaction time 3-5h that substance used in solution ph is adjusted in.
CN201910359623.0A 2019-04-30 2019-04-30 A method of LITHIUM BATTERY manganese sulfate is prepared from anti-copper manganese liquid Pending CN110172581A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111187907A (en) * 2020-02-20 2020-05-22 中国恩菲工程技术有限公司 Method for purifying manganese sulfate solution
CN111620377A (en) * 2020-06-12 2020-09-04 福建常青新能源科技有限公司 Process and device for removing oil and impurities from manganese sulfate solution

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013165071A1 (en) * 2012-04-30 2013-11-07 전남대학교산학협력단 Method for producing high-purity manganese sulfate monohydrate and high-purity manganese sulfate monohydrate produced by the method
CN106517347A (en) * 2016-11-23 2017-03-22 吉林吉恩镍业股份有限公司 Preparation method of battery-grade manganese sulfate
CN107416908A (en) * 2017-05-27 2017-12-01 广东芳源环保股份有限公司 A kind of method that low cost prepares high-purity sulphuric acid manganese solution

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013165071A1 (en) * 2012-04-30 2013-11-07 전남대학교산학협력단 Method for producing high-purity manganese sulfate monohydrate and high-purity manganese sulfate monohydrate produced by the method
CN106517347A (en) * 2016-11-23 2017-03-22 吉林吉恩镍业股份有限公司 Preparation method of battery-grade manganese sulfate
CN107416908A (en) * 2017-05-27 2017-12-01 广东芳源环保股份有限公司 A kind of method that low cost prepares high-purity sulphuric acid manganese solution

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111187907A (en) * 2020-02-20 2020-05-22 中国恩菲工程技术有限公司 Method for purifying manganese sulfate solution
CN111620377A (en) * 2020-06-12 2020-09-04 福建常青新能源科技有限公司 Process and device for removing oil and impurities from manganese sulfate solution
CN111620377B (en) * 2020-06-12 2023-06-30 福建常青新能源科技有限公司 Oil removal and impurity removal process and device for manganese sulfate solution

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Application publication date: 20190827