CN109852794A - A method of being used to prepare LITHIUM BATTERY nickel sulfate - Google Patents
A method of being used to prepare LITHIUM BATTERY nickel sulfate Download PDFInfo
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Abstract
A kind of method for being used to prepare LITHIUM BATTERY nickel sulfate of the present invention removes de-iron and arsenic first with the method for hydrogen peroxide oxidation.Recycle the calcium ions and magnesium ions in sodium fluoride precipitation system.Filtrate is passed sequentially through into the resin tower containing p204 resin and cyanex272 resin and removes copper, lead, zinc, manganese and cobalt respectively.It finally with the nickel in the p204 extractant extraction solution being saponified, is then stripped with sulfuric acid, and passes through twice evaporation condensing crystallizing.This method of purification can effectively utilize macroporous ion exchange resin, reduce the operating procedure in purification process, reduce the cost of purification.Most of foreign ion in nickel can be effectively removed, finished product is made to reach the purity requirement of LITHIUM BATTERY nickel sulfate.
Description
Technical field
The present invention relates to a kind of methods for being used to prepare LITHIUM BATTERY nickel sulfate, belong to chemical field.
Background technique
Metallic nickel is widely applied and manufacture alloy, catalyst, ceramic, chemical ware, electronic circuit, anode
Material etc..Lithium electricity industry high speed development now, the demand to high-purity LITHIUM BATTERY nickel sulfate increase year by year, and crude nickel sulfate contains
Some major impurities are cobalt, iron, arsenic, copper, lead, zinc, calcium, magnesium, manganese.Industrial nickel sulfate purity is far not achieved lithium battery and makes
It is required that LITHIUM BATTERY nickel sulfate is very high to purity requirement, it is desirable that nickel content is 22% or more in nickel sulfate hexahydrate.Therefore nickel
Purification have a vast market and prospect.
Summary of the invention
The present invention proposes a kind of method for being used to prepare LITHIUM BATTERY nickel sulfate.
The present invention is as follows using technical solution:
Step 1: nickel sulfate solution pH is adjusted to 7 or so.Add hydrogen peroxide and 30min is sufficiently stirred.
Step 2: into solution plus alkali adjusts pH to 3.5-4.0, reacts 1h, staticly settles, leaches, obtain 1 He of leachate
Filter residue 1.
Step 3: leachate 1 is added sodium fluoride and removes calcium and magnesium.It leaches, obtains leachate 2 and filter residue 2.
Step 4: leachate 2 flows through the resin tower equipped with p204 resin and carries out deep purifying, removes copper, lead, zinc, manganese.?
To efflux 1.
Step 5: efflux 1 flows through the resin tower equipped with cyanex272 resin and removes cobalt.Obtain efflux 2.
Step 6: efflux 2 flows through the P204 resin tower extraction of nickel that soda soap is crossed, and is stripped with sulfuric acid；Then through 85 DEG C or more
It is evaporated concentration, is cooled to 50 DEG C later, is kept for temperature 1 hour, feed liquid is centrifugated at 45-50 DEG C, obtained solid
That is LITHIUM BATTERY nickel sulfate.
A kind of method being used to prepare LITHIUM BATTERY nickel sulfate of the present invention, in step 2 nickel sulfate pH it is adjustable
Between 1-10.
A kind of method being used to prepare LITHIUM BATTERY nickel sulfate of the present invention, hydrogen peroxide concentration can be from step 2
5%-95% etc..
A kind of method being used to prepare LITHIUM BATTERY nickel sulfate of the present invention, leaching in step 2, step 3 can be often
Pressure leaches, and is also possible to high pressure leaching, leaching pressure can be between 0.1MPa-40MPa.
A kind of method being used to prepare LITHIUM BATTERY nickel sulfate of the present invention, step 2, step 3, middle extraction temperature can be with
Between 0 DEG C -100 DEG C.
A kind of method being used to prepare LITHIUM BATTERY nickel sulfate of the present invention, extraction time can be in step 2, step 3
Between 1h-10h.
A kind of method being used to prepare LITHIUM BATTERY nickel sulfate of the present invention, before leachate 2 enters resin tower in step 4
Adjust pH value between 1 and 3.
A kind of method being used to prepare LITHIUM BATTERY nickel sulfate of the present invention, before efflux 1 enters resin tower in step 5
PH value is adjusted between 5-6.
A kind of method being used to prepare LITHIUM BATTERY nickel sulfate of the present invention, in step 4, step 5 p204 resin and
Cyanex272 resin partial size can be from 0.1mm-1mm etc..
A kind of method being used to prepare LITHIUM BATTERY nickel sulfate of the present invention, in step 4, step 5 p204 resin tower with
And flow velocity when cyanex272 resin tower feed liquor can be 1BV/h-20BV/h etc..
A kind of method being used to prepare LITHIUM BATTERY nickel sulfate of the present invention, in step 4, step 5 p204 resin and
Cyanex272 resin is containing two kinds of resins for being applicable in the acidic phosphorus-containing extractant for extracting cobalt from cobalt-nickel mixture, Ke Yitong
Prior art preparation or commercial sources purchase are crossed, can also be prepared by following methods:
Step 1, using suspension polymerization, it is added suitable monomer in a kettle, crosslinking agent, pore-foaming agent, initiator, point
Powder prepares matrix macroreticular resin；The monomer can be polystyrene, oleic series, acrylic, phenolic aldehyde system, epoxy
System, vinylpyridine system, ureaformaldehyde system, vinyl chloride etc. are one such；The crosslinking agent can be divinylbenzene, two isocyanides
Acid esters, N,N methylene bis acrylamide etc. are one such；Crosslinking agent accounts for the ratio of monomer (i.e. when described matrix resin polymerization
The degree of cross linking) it can be 1%-90% etc.；Pore-foaming agent can be toluene, isooctane, gasoline, aviation gasoline, normal heptane, hexamethylene
Alkane, atoleine, white oil etc. are one such；The initiator can be lauroyl peroxide, benzoyl peroxide, isopropylbenzene
Hydrogen peroxide, tert-butyl hydroperoxide, di-t-butyl peroxide, cumyl peroxide, potassium peroxydisulfate, sodium peroxydisulfate, over cure
Sour ammonium azodiisobutyronitrile, azobisisoheptonitrile etc. are one such；The dispersing agent can be polyvinyl alcohol, gelatin, fat
Acids, aliphatic amide type, paraffin class, cellulose family etc. are one such；Water-oil factor can be from 10:1- when the suspension polymerisation
1:1 etc., wherein water phase refers to that the water dissolved with dispersing agent, oil mutually refer to the mixture of monomer and crosslinking agent, perforating agent；Described suspend is gathered
Temperature can control when conjunction differs at 40 DEG C -110 DEG C.
Step 2, the perforating agent in resin is removed after the completion of polymerization, obtains matrix macroreticular resin.
Step 3, effective component extractant is adsorbed on matrix resin surface using infusion process；The extractant can be two
(2,4,4- tri-methyl-amyl) phosphinic acids (i.e. cyanex272) or di-(2-ethylhexyl)phosphoric acid (i.e. P204)；The extractant
It can use Aqueous phase when dipping, oily phase method, any one in the methods of diffusion method；The extractant dosage can be matrix tree
The 1%-100% of lipid amount；C3-C15 can be added in extractant alkane when impregnating makees auxiliary agent；Described matrix resin dipping
Before can be swollen with the organic solvent of small molecule.
The method of preparation LITHIUM BATTERY nickel sulfate provided by the invention has the advantage that
Provide a kind of process of crude nickle sulphate purification.The various impurity in crude nickle sulphate are successively removed by 6 steps,
The purity of nickel sulfate is set to reach requirement.A large amount of ion exchange resin has been used in process, obtains purification process in program
Simplify, reduces equipment operating cost, while reaching higher level on refining effect.Impurity-eliminating effect is more satisfactory, compares
With traditional purification process, the present invention is more time saving and energy saving, has more economic benefit using this method production LITHIUM BATTERY nickel sulfate.
Specific embodiment
In order to illustrate effect of the invention, enumerating embodiment, invention is further described in detail, but the present invention is not
It is only limitted to these embodiments.
Embodiment 1: preparation LITHIUM BATTERY nickel sulfate
Crude nickel sulfate solution pH is adjusted to 7, is added and is used for precipitated iron and 1.2 times of arsenic theoretical amount of 60% dioxygen
Water stirs 30min, ammonium hydroxide and the concentration of 8mol/L is added then as 10% calcium hydroxide, reaction temperature is 85 DEG C.To solution
PH is maintained at 3.5 or so, normal pressure leaching.
The sodium fluoride for precipitating 1.2 times of calcium and magnesium theoretical amount, 60 DEG C of reaction 2h, normal pressure leaching is added in leachate.
Leachate flows successively through two sets of p204 resin towers, cyanex272 resin tower with the speed of 2BV/h.Two kinds of resin towers
It is all made of double-column in series, the mode of single column parsing.Material liquid pH is adjusted to 1.5 and 3 before two sets of p204 resin tower feed liquors simultaneously.p204
Resin and cyanex272 resin impregnate the macroreticular resin of extractant using styrene skeleton.Then use is flowed through with the speed of 2BV/h
The P204 resin tower extraction of nickel that soda soap is crossed, is stripped with sulfuric acid.Efflux uses the weak base tree for switching to hydrogen-oxygen type with sodium hydroxide
PH is adjusted to 5 by rouge, is then concentrated by evaporation in 85 DEG C, is cooled to 50 DEG C, is kept temperature 1h, is centrifugated at 45-50 DEG C, institute
Obtain solid, that is, LITHIUM BATTERY nickel sulfate.
Then six obtained water battery grade nickel sulfates are taken a certain amount of melt into 10mg/L's by the detection limit for demarcating ICP-OES
Solution, with nickel, the iron, copper, cobalt, lead, zinc, manganese content in ICP-OES measurement solution, nickel content 2.213mg/L is greater than
22%, cobalt content is less than 0.04%, and copper content is less than 0.0005%, and less than 0.0005%, lead content is less than iron content
0.001%, Zn content is less than 0.001%, and for calcium content less than 0.01%, content of magnesium meets LITHIUM BATTERY nickel sulfate less than 0.01%
Requirement.
Embodiment 2: preparation LITHIUM BATTERY nickel sulfate
Crude nickel sulfate solution pH is adjusted to 7, is added and is used for precipitated iron and 1.2 times of arsenic theoretical amount of 50% dioxygen
Water stirs 30min, ammonium hydroxide and the concentration of 8mol/L is added then as 10% calcium hydroxide, reaction temperature is 85 DEG C.To solution
PH is maintained at 3.5 or so, normal pressure leaching.
The sodium fluoride for precipitating 1.2 times of calcium and magnesium theoretical amount, 60 DEG C of reaction 2h, normal pressure leaching is added in leachate.
Leachate flows successively through two sets of p204 resin towers, cyanex272 resin tower with the speed of 2BV/h.Two kinds of resin towers
It is all made of double-column in series, the mode of single column parsing.Material liquid pH is adjusted to 1.5 and 3 before two sets of p204 resin tower feed liquors simultaneously.p204
Resin and cyanex272 resin impregnate the macroreticular resin of extractant using styrene skeleton.Then use is flowed through with the speed of 2BV/h
The P204 resin tower extraction of nickel that soda soap is crossed, is stripped with sulfuric acid.Efflux uses the weak base tree for switching to hydrogen-oxygen type with sodium hydroxide
PH is adjusted to 5 by rouge, is then concentrated by evaporation in 85 DEG C, is cooled to 50 DEG C, is kept temperature 1h, is centrifugated at 45-50 DEG C, institute
Obtain solid, that is, LITHIUM BATTERY nickel sulfate.
Obtained LITHIUM BATTERY nickel sulfate, is then taken the solution of a certain amount of melt into 10mg/L by the detection limit for demarcating ICP-OES,
With iron, the copper, cobalt, lead, zinc, manganese content in ICP-OES measurement solution, nickel content 2.245mg/L is greater than 22%, cobalt content
Less than 0.04%, copper content is less than 0.0005%, and iron content is less than 0.0005%, and less than 0.001%, Zn content is less than lead content
0.001%, for calcium content less than 0.01%, content of magnesium meets the requirement of LITHIUM BATTERY nickel sulfate less than 0.01%.
Embodiment 3: preparation LITHIUM BATTERY nickel sulfate
Crude nickel sulfate solution pH is adjusted to 7, is added and is used for precipitated iron and 1.2 times of arsenic theoretical amount of 60% dioxygen
Water stirs 30min, ammonium hydroxide and the concentration of 8mol/L is added then as 10% calcium hydroxide, reaction temperature is 80 DEG C.To solution
PH is maintained at 3.5 or so, normal pressure leaching.
The sodium fluoride for precipitating 1.2 times of calcium and magnesium theoretical amount, 60 DEG C of reaction 2h, normal pressure leaching is added in leachate.
Leachate flows successively through two sets of p204 resin towers, cyanex272 resin tower with the speed of 2BV/h.Two kinds of resin towers
It is all made of double-column in series, the mode of single column parsing.Material liquid pH is adjusted to 1.5 and 3 before two sets of p204 resin tower feed liquors simultaneously.p204
Resin and cyanex272 resin impregnate the macroreticular resin of extractant using styrene skeleton.Then use is flowed through with the speed of 2BV/h
The P204 resin tower extraction of nickel that soda soap is crossed, is stripped with sulfuric acid.Efflux uses the weak base tree for switching to hydrogen-oxygen type with sodium hydroxide
PH is adjusted to 5 by rouge, is then concentrated by evaporation in 85 DEG C, is cooled to 50 DEG C, is kept temperature 1h, is centrifugated at 45-50 DEG C, institute
Obtain solid, that is, LITHIUM BATTERY nickel sulfate.
Obtained LITHIUM BATTERY nickel sulfate, is then taken the solution of a certain amount of melt into 10mg/L by the detection limit for demarcating ICP-OES,
With iron, the copper, cobalt, lead, zinc, manganese content in ICP-OES measurement solution, nickel content 2.251mg/L is greater than 22%, cobalt content
Less than 0.04%, copper content is less than 0.0005%, and iron content is less than 0.0005%, and less than 0.001%, Zn content is less than lead content
0.001%, for calcium content less than 0.01%, content of magnesium meets the requirement of LITHIUM BATTERY nickel sulfate less than 0.01%.
Embodiment 4: preparation LITHIUM BATTERY nickel sulfate
Crude nickel sulfate solution pH is adjusted to 7, is added and is used for precipitated iron and 1.2 times of arsenic theoretical amount of 60% dioxygen
Water stirs 30min, ammonium hydroxide and the concentration of 8mol/L is added then as 10% calcium hydroxide, reaction temperature is 85 DEG C.To solution
PH is maintained at 3.5 or so, normal pressure leaching.
The sodium fluoride for precipitating 1.2 times of calcium and magnesium theoretical amount, 50 DEG C of reaction 2h, normal pressure leaching is added in leachate.
Leachate flows successively through two sets of p204 resin towers, cyanex272 resin tower with the speed of 2BV/h.Two kinds of resin towers
It is all made of double-column in series, the mode of single column parsing.Material liquid pH is adjusted to 1.5 and 3 before two sets of p204 resin tower feed liquors simultaneously.p204
Resin and cyanex272 resin impregnate the macroreticular resin of extractant using styrene skeleton.Then use is flowed through with the speed of 2BV/h
The P204 resin tower extraction of nickel that soda soap is crossed, is stripped with sulfuric acid.Efflux uses the weak base tree for switching to hydrogen-oxygen type with sodium hydroxide
PH is adjusted to 5 by rouge, is then concentrated by evaporation in 85 DEG C, is cooled to 50 DEG C, is kept temperature 1h, is centrifugated at 45-50 DEG C, institute
Obtain solid, that is, LITHIUM BATTERY nickel sulfate.
Obtained LITHIUM BATTERY nickel sulfate, is then taken the solution of a certain amount of melt into 10mg/L by the detection limit for demarcating ICP-OES,
With iron, the copper, cobalt, lead, zinc, manganese content in ICP-OES measurement solution, nickel content 2.209mg/L is greater than 22%, cobalt content
Less than 0.04%, copper content is less than 0.0005%, and iron content is less than 0.0005%, and less than 0.001%, Zn content is less than lead content
0.001%, for calcium content less than 0.01%, content of magnesium meets the requirement of LITHIUM BATTERY nickel sulfate less than 0.01%.
Embodiment 5: a method of preparing LITHIUM BATTERY nickel sulfate
Crude nickel sulfate solution pH is adjusted to 7, is added and is used for precipitated iron and 1.2 times of arsenic theoretical amount of 60% dioxygen
Water stirs 30min, ammonium hydroxide and the concentration of 8mol/L is added then as 10% calcium hydroxide, reaction temperature is 85 DEG C.To solution
PH is maintained at 3.5 or so, normal pressure leaching.
The sodium fluoride for precipitating 1.2 times of calcium and magnesium theoretical amount, 60 DEG C of reaction 2h, normal pressure leaching is added in leachate.
Leachate flows successively through two sets of p204 resin towers, cyanex272 resin tower with the speed of 2BV/h.Two kinds of resin towers
It is all made of double-column in series, the mode of single column parsing.Material liquid pH is adjusted to 1.5 and 3 before two sets of p204 resin tower feed liquors simultaneously.p204
Resin and cyanex272 resin impregnate the macroreticular resin of extractant using acrylic backbone.Then use is flowed through with the speed of 2BV/h
The P204 resin tower extraction of nickel that soda soap is crossed, is stripped with sulfuric acid.Efflux uses the weak base tree for switching to hydrogen-oxygen type with sodium hydroxide
PH is adjusted to 5 by rouge, is then concentrated by evaporation in 85 DEG C, is cooled to 50 DEG C, is kept temperature 1h, is centrifugated at 45-50 DEG C, institute
Obtain solid, that is, LITHIUM BATTERY nickel sulfate.
Obtained LITHIUM BATTERY nickel sulfate, is then taken the solution of a certain amount of melt into 10mg/L by the detection limit for demarcating ICP-OES,
With iron, the copper, cobalt, lead, zinc, manganese content in ICP-OES measurement solution, nickel content 2.242mg/L is greater than 22%, cobalt content
Less than 0.04%, copper content is less than 0.0005%, and iron content is less than 0.0005%, and less than 0.001%, Zn content is less than lead content
0.001%, for calcium content less than 0.01%, content of magnesium meets the requirement of LITHIUM BATTERY nickel sulfate less than 0.01%.
Embodiment 6: a method of preparing LITHIUM BATTERY nickel sulfate
Crude nickel sulfate solution pH is adjusted to 7, is added and is used for precipitated iron and 1.2 times of arsenic theoretical amount of 60% dioxygen
Water stirs 30min, ammonium hydroxide and the concentration of 8mol/L is added then as 10% calcium hydroxide, reaction temperature is 85 DEG C.To solution
PH is maintained at 3.5 or so, normal pressure leaching.
The sodium fluoride for precipitating 1.2 times of calcium and magnesium theoretical amount, 60 DEG C of reaction 2h, normal pressure leaching is added in leachate.
Leachate flows successively through two sets of p204 resin towers, cyanex272 resin tower with the speed of 2BV/h.Two kinds of resin towers
It is all made of double-column in series, the mode of single column parsing.Material liquid pH is adjusted to 1.5 and 3 before two sets of p204 resin tower feed liquors simultaneously.p204
Resin and cyanex272 resin impregnate the macroreticular resin of extractant using styrene skeleton.Then use is flowed through with the speed of 2BV/h
The P204 resin tower extraction of nickel that soda soap is crossed, is stripped with sulfuric acid.Efflux uses the weak base tree for switching to hydrogen-oxygen type with sodium hydroxide
PH is adjusted to 5 by rouge, is then concentrated by evaporation in 80 DEG C, is cooled to 50 DEG C, is kept temperature 1h, is centrifugated at 45-50 DEG C, institute
Obtain solid, that is, LITHIUM BATTERY nickel sulfate.
Obtained LITHIUM BATTERY nickel sulfate, is then taken the solution of a certain amount of melt into 10mg/L by the detection limit for demarcating ICP-OES,
With iron, the copper, cobalt, lead, zinc, manganese content in ICP-OES measurement solution, nickel content 2.262mg/L is greater than 22%, cobalt content
Less than 0.04%, copper content is less than 0.0005%, and iron content is less than 0.0005%, and less than 0.001%, Zn content is less than lead content
0.001%, for calcium content less than 0.01%, content of magnesium meets the requirement of LITHIUM BATTERY nickel sulfate less than 0.01%.
Embodiment 7: a method of preparing LITHIUM BATTERY nickel sulfate
Crude nickel sulfate solution pH is adjusted to 7, is added and is used for precipitated iron and 1.2 times of arsenic theoretical amount of 60% dioxygen
Water stirs 30min, ammonium hydroxide and the concentration of 8mol/L is added then as 10% calcium hydroxide, reaction temperature is 85 DEG C.To solution
PH is maintained at 3.5 or so, normal pressure leaching.
The sodium fluoride for precipitating 1.2 times of calcium and magnesium theoretical amount, 60 DEG C of reaction 2h, normal pressure leaching is added in leachate.
Leachate flows successively through two sets of p204 resin towers, cyanex272 resin tower with the speed of 2BV/h.Two kinds of resin towers
It is all made of double-column in series, the mode of single column parsing.Material liquid pH is adjusted to 1.5 and 3 before two sets of p204 resin tower feed liquors simultaneously.p204
Resin and cyanex272 resin impregnate the macroreticular resin of extractant using styrene skeleton.Then use is flowed through with the speed of 2BV/h
The P204 resin tower extraction of nickel that soda soap is crossed, is stripped with sulfuric acid.Efflux uses the weak base tree for switching to hydrogen-oxygen type with sodium hydroxide
PH is adjusted to 5 by rouge, is then concentrated by evaporation in 85 DEG C, is cooled to 45 DEG C, is kept temperature 1h, is centrifugated at 45-50 DEG C, institute
Obtain solid, that is, LITHIUM BATTERY nickel sulfate.
Obtained LITHIUM BATTERY nickel sulfate, is then taken the solution of a certain amount of melt into 10mg/L by the detection limit for demarcating ICP-OES,
With iron, the copper, cobalt, lead, zinc, manganese content in ICP-OES measurement solution, nickel content 2.228mg/L is greater than 22%, cobalt content
Less than 0.04%, copper content is less than 0.0005%, and iron content is less than 0.0005%, and less than 0.001%, Zn content is less than lead content
0.001%, for calcium content less than 0.01%, content of magnesium meets the requirement of LITHIUM BATTERY nickel sulfate less than 0.01%.
Embodiment 8: a method of preparing LITHIUM BATTERY nickel sulfate
Crude nickel sulfate solution pH is adjusted to 7, is added and is used for precipitated iron and 1.2 times of arsenic theoretical amount of 60% dioxygen
Water stirs 30min, ammonium hydroxide and the concentration of 8mol/L is added then as 10% calcium hydroxide, reaction temperature is 85 DEG C.To solution
PH is maintained at 3.5 or so, normal pressure leaching.
The sodium fluoride for precipitating 1.2 times of calcium and magnesium theoretical amount, 60 DEG C of reaction 2h, normal pressure leaching is added in leachate.
Leachate flows successively through two sets of p204 resin towers, cyanex272 resin tower with the speed of 2BV/h.Two kinds of resin towers
It is all made of double-column in series, the mode of single column parsing.Material liquid pH is adjusted to 1.5 and 3 before two sets of p204 resin tower feed liquors simultaneously.p204
Resin and cyanex272 resin impregnate the macroreticular resin of extractant using styrene skeleton.Then use is flowed through with the speed of 2BV/h
The P204 resin tower extraction of nickel that soda soap is crossed, is stripped with sulfuric acid.Efflux uses the weak base tree for switching to hydrogen-oxygen type with sodium hydroxide
PH is adjusted to 5 by rouge, is then concentrated by evaporation in 85 DEG C, is cooled to 50 DEG C, is kept temperature 1h, is centrifugated at 55 DEG C, gained
Solid, that is, LITHIUM BATTERY nickel sulfate.
Obtained LITHIUM BATTERY nickel sulfate, is then taken the solution of a certain amount of melt into 10mg/L by the detection limit for demarcating ICP-OES,
With iron, the copper, cobalt, lead, zinc, manganese content in ICP-OES measurement solution, nickel content 2.277mg/L is greater than 22%, cobalt content
Less than 0.04%, copper content is less than 0.0005%, and iron content is less than 0.0005%, and less than 0.001%, Zn content is less than lead content
0.001%, for calcium content less than 0.01%, content of magnesium meets the requirement of LITHIUM BATTERY nickel sulfate less than 0.01%.
Above embodiments are only a part explanations of the invention, are not used in the limitation present invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of method for being used to prepare LITHIUM BATTERY nickel sulfate, which comprises the following steps:
Step 1, nickel sulfate solution pH is adjusted to 7 or so；Add hydrogen peroxide and 30min is sufficiently stirred；
Step 2, add alkali to adjust pH to 3.5-4.0 into solution, react 1 hour, staticly settle, leach, obtain 1 He of leachate
Filter residue 1；
Step 3, leachate 1 is added sodium fluoride and removes calcium and magnesium；It leaches, obtains leachate 2 and filter residue 2；
Step 4, leachate 2 flows through the resin tower equipped with p204 resin and carries out deep purifying, removes copper, lead, zinc, manganese flowed
Liquid 1 out；
Step 5, the resin tower that efflux 1 flows through dress cyanex272 resin removes cobalt, obtains efflux 2；
Step 6, efflux 2 flows through the P204 resin tower extraction of nickel that soda soap is crossed, and is stripped with sulfuric acid；Then it is carried out through 85 DEG C or more
It is concentrated by evaporation, is cooled to 50 DEG C later, kept for temperature 1 hour, feed liquid is centrifugated at 45-50 DEG C, obtained solid is electricity
Pond grade nickel sulfate.
2. the method according to claim 1, wherein nickel sulfate pH described in step 2 it is adjustable 1-10 it
Between.
3. the method according to claim 1, wherein hydrogen peroxide concentration described in step 1 is 5%-95%.
4. the method according to claim 1, wherein leaching described in step 2 or step 3 can be normal pressure leaching
Out, it is also possible to high pressure leaching, leaching pressure can be between 0.1MPa-40MPa.
5. the method according to claim 1, wherein extraction temperature described in step 2 or step 3 is 0 DEG C -100
℃。
6. the method according to claim 1, wherein extraction time described in step 2 or step 3 is that 1-10 is small
When.
7. the method according to claim 1, wherein leachate 2 described in step 4 adjusts pH before entering resin tower
Value is 1-3.
8. the method according to claim 1, wherein efflux 1 described in step 5 adjusts pH before entering resin tower
Value is 5-6.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403477A (en) * | 2021-06-18 | 2021-09-17 | 国家电投集团黄河上游水电开发有限责任公司 | Comprehensive utilization method of nickel sulfide concentrate |
| CN113416855A (en) * | 2021-06-18 | 2021-09-21 | 国家电投集团黄河上游水电开发有限责任公司 | Method for preparing nickel sulfate from nickel sulfide concentrate leaching solution |
| CN113416856A (en) * | 2021-06-18 | 2021-09-21 | 国家电投集团黄河上游水电开发有限责任公司 | Method for selectively extracting cobalt and nickel from nickel sulfide concentrate |
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| CN113416856A (en) * | 2021-06-18 | 2021-09-21 | 国家电投集团黄河上游水电开发有限责任公司 | Method for selectively extracting cobalt and nickel from nickel sulfide concentrate |
| CN113403477B (en) * | 2021-06-18 | 2023-02-28 | 国家电投集团黄河上游水电开发有限责任公司 | Comprehensive utilization method of nickel sulfide concentrate |
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