CN106395921A - Method used for producing nickel chloride products taking waste printing nickel screens as raw materials - Google Patents
Method used for producing nickel chloride products taking waste printing nickel screens as raw materials Download PDFInfo
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- CN106395921A CN106395921A CN201610738616.8A CN201610738616A CN106395921A CN 106395921 A CN106395921 A CN 106395921A CN 201610738616 A CN201610738616 A CN 201610738616A CN 106395921 A CN106395921 A CN 106395921A
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- nickel
- remover
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- waste printing
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/08—Halides
- C01G53/09—Chlorides
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- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method used for producing nickel chloride products taking waste printing nickel screens as raw materials, and belongs to the field of hydrometallurgy. According to the method, cyclic utilization of waste printing nickel screens is realized, and the waste printing nickel screens are taken as the raw materials to produce the nickel chloride products. The mehod comprises following steps: the waste printing nickel screens are processed with a release agent so as to remove photoresist on the surfaces of the waste printing nickel screens, and then are subjected to leaching treatment with industrial hydrochloric acid; an obtained leached solution is subjected to extraction with P507 extraction agent so as to remove impurities until the content of impurities in an obtained extraction raffinate is capable of satisfying requirements on the content in nickel chloride product production; and the extraction raffinate is subjected to evaporation, crystallization, centrifugalization, and drying so as to obtain the qualified nickel chloride products. The method is capable of realizing cyclic utilization of the waste printing nickel screens, and broadening the sources of raw materials used for producing the nickel chloride products.
Description
Technical field
The invention belongs to field of hydrometallurgy, it is related to a kind of side with waste and old printed nickel net for raw material production Nickel dichloride. product
Method.
Background technology
In Nickel dichloride. production, usually to first produce nickel chloride solution, then nickel chloride solution be evaporated, tie
Crystalline substance, finally obtains Nickel dichloride. product.The method producing nickel chloride solution is more, the method that can pass through dissolving with hydrochloric acid electrolytic nickel,
The method of chlorine leaching nickel ore concentrate can be passed through it is also possible to the method for dissolving with hydrochloric acid nickel hydroxide produces, various production methods
To be determined using the raw materials used physics of Main Basiss and chemical property.Use salt Ore Leaching to produce Nickel dichloride. after nickel screen demoulding to produce
Product, can make waste nickel net recycle, turn waste into wealth, meet the requirement of national recycling economy.And chemically react angle
See although nickel screen and hydrochloric acid Leach reaction, can be with output nickel chloride solution, but waste and old printed nickel net surface is stained with photoresists, nickel
Net and hydrochloric acid isolation, it is impossible to produce chemical reaction, therefore need waste and old nickel screen demoulding is processed.
Content of the invention
It is an object of the invention to provide a kind of method with waste and old printed nickel net for raw material production Nickel dichloride. product.
Technical scheme：A kind of with waste and old printed nickel net for the method for raw material production Nickel dichloride. product, use demoulding
Photoresists on waste and old printed nickel net are removed by agent, and the nickel screen after removing is leached with technical hydrochloric acid, and leachate extracts through P507
Remove miscellaneous, leached mud is unreacted nickel screen, add technical hydrochloric acid to proceed leaching process, P507 raffinate is through evaporation, knot
Brilliant, be centrifuged, output qualified Nickel dichloride. product be dried.
Specifically：A, configuration printing nickel net demoulding agent:Following reagent is proportionally added into a band mechanical agitation and heating
In the kettle of device, addition reagent and ratio are：Main remover is hydrogen peroxide, and hydrogen peroxide is 2-5 with the mass ratio of water:1, help stripping
In agent, the mass ratio of each component is：Dodecyl sodium sulfate：Fatty alcohol-polyoxyethylene ether：Ethanol=2-3:1-2:2-4, main stripping
Agent with the mass ratio helping remover is：3-5:2, the pH value of remover is：10-14；
B, printing nickel net demoulding:After the completion of remover configuration, nickel screen to be stripped is totally submerged in remover, temperature is even
Insulation after speed rises to 50-80 DEG C removes photoresists, reacts 1-5h, takes out nickel screen water under high pressure and be carried out after 1-5h；
C, nickel screen leach：By after degumming nickel screen add technical hydrochloric acid leach, during temperature control be 50-90 DEG C, to be leached
Liquid pH value, for stopping Leach reaction during 3.0-4.5, is filtered；
D, leachate extraction：With P507 extractant extracting and purifying nickel screen leachate, extraction phase compares O:A=3-5:1, raffinate impurity
Content is：Ni >=180g/L, Co, Cu, Fe, Zn, Pb, Mn≤0.004g/L, Ca≤0.1g/L, Mg≤0.5g/L, Na≤1g/L.
E, raffinate evaporate, crystallize, are centrifuged, are dried：Qualified raffinate vaporizer is evaporated concentrating, evaporation and concentration
To after evaporate liquid nickeliferous for 300-340g/L when, stop evaporation, liquid will put and be passed through cooling water circulation fall to crystallizer after evaporation
Temperature, crystallization time be 18-24h, when built-in temperature to be crystallized is down to 20-30 DEG C, close cooling water, crystallizer intercrystalline is put to
In centrifuge, centrifugation, completes solid-liquid separation, and after being centrifuged, material is delivered to be dried in rotary kiln and is dried, and baking temperature is 20-40
DEG C, drying time 3-8min, be dried after material be qualified Nickel dichloride. product.
Beneficial effects of the present invention：Reclaim the nickel of waste residue, the qualified Nickel dichloride. product of output, so that waste and old nickel screen is circulated
Using, and widened the raw material type producing Nickel dichloride. product.
Brief description
Fig. 1 is the process chart of the present invention.
Specific embodiment
Embodiment 1
A kind of with waste and old printed nickel net for the method for raw material production Nickel dichloride. product, comprise the following steps：
A. configure printing nickel net demoulding agent
Add hydrogen peroxide 30kg, dodecyl sodium sulfate 8kg, fatty alcohol-polyoxyethylene ether in remover configuration kettle（Peregal
o-20）4kg, ethanol 8kg, water 12.5kg, open mechanical agitation mixing, and add nickel hydroxide adjust remover pH value be
12.5, to be mixed uniformly and pH value is that i.e. remover configuration completes after 12.5.
B, printing nickel net demoulding
The nickel screen taking 5kg to be stripped is totally submerged in remover, insulation removing photoresists 2h after temperature is at the uniform velocity risen to 70 DEG C,
Take out nickel screen water under high pressure after 2h to be carried out.
C, nickel screen leach
Nickel screen after degumming described in step b is added technical hydrochloric acid to leach, in leaching process, temperature control is 80 DEG C, to be leached
Liquid pH value is to stop Leach reaction when 3.5, is filtered, and filtrate is nickel screen leachate.
D, nickel screen leachate abstraction impurity removal
P507 extractant is pressed 1 with sulfonated kerosene:After 3 mixing, the NaOH solution that mass concentration is 30% is added to carry out saponification, to
Organic middle addition Ni ion concentration after saponification is that the nickel chloride solution of 90.7g/L produces nickel soap, the organic and sulphur removal after nickel soap
Liquid mixing before Nickel dichloride. extraction after acid group, through the extraction of extraction box 7 stage countercurrent, extraction phase compares O:A=1:1, obtain qualified Nickel dichloride.
Solution（Wherein Ni >=180g/L, Co, Cu, Fe, Zn, Pb, Mn≤0.004g/L, Ca≤0.1g/L, Mg≤0.5g/L, Na≤1g/
L）, the organic hydrochloric acid with 6mol/L of the load after extraction re-starts saponification after the regeneration of extraction box 6 stage countercurrent and reuses.
E, raffinate evaporate, crystallize, are centrifuged, are dried
By qualified raffinate vaporizer be evaporated concentrate, evaporation and concentration to evaporate after liquid nickeliferous for 315.9g/L when, stop
Evaporation, liquid after evaporation is put and is passed through cooling water circulation cooling to crystallizer, and crystallization time is 23h, built-in temperature fall to be crystallized
During to 22 DEG C, close cooling water, crystallizer intercrystalline is put to centrifuge with centrifugation, completes solid-liquid separation, material after being centrifuged
Be delivered to be dried in rotary kiln and be dried, baking temperature is 35 DEG C, drying time 6min, after being dried, material is qualified Nickel dichloride. and produces
Product.
After testing, gained Nickel dichloride. product can meet Nickel dichloride. HG/T 2771-2009 standard.
Embodiment 2
Embodiment 2 step process with embodiment 1, specifically：
Step a is with the difference of embodiment 1, and the pH value controlling remover is 12.3.
Step b is with the difference of embodiment 1, and in de-filming process, temperature control is 75 DEG C, and the time is 2.5h.
Step c is with the difference of embodiment 1, and leaching process temperature control is 80 DEG C, leachate PH=4.0.
Step d is with the difference of embodiment 1, is 85.5g/L to the organic middle addition Ni ion concentration after saponification
Nickel chloride solution produce nickel soap, organic after nickel soap is mixed with nickel screen leachate and is extracted, through extraction box 7 stage countercurrent extraction
Take, extraction phase compares O:A=2:1, loading after organic hydrochloric acid with 6.8mol/L regenerates through extraction box 6 stage countercurrent again after extraction
Carry out saponification reuse.
Step e with implement 1 difference be, evaporation and concentration to evaporate after liquid nickeliferous for 318.6g/L when, stop steam
Send out, liquid after evaporation is put and is passed through cooling water circulation cooling to crystallizer, crystallization time is 23.5h, built-in temperature fall to be crystallized
During to 23 DEG C, close cooling water, crystallizer intercrystalline is put to centrifuge with centrifugation, completes solid-liquid separation, material after being centrifuged
Be delivered to be dried in rotary kiln and be dried, baking temperature is 36 DEG C, drying time 7min, after being dried, material is qualified Nickel dichloride. and produces
Product.
After testing, gained Nickel dichloride. product can meet Nickel dichloride. HG/T 2771-2009 standard.
Embodiment 3
Embodiment 2 step process with embodiment 1, specifically：
Step a is with the difference of embodiment 1, and the pH value controlling remover is 13.
Step b is with the difference of embodiment 1, and in de-filming process, temperature control is 80 DEG C, and the time is 2.8h.
Step c is with the difference of embodiment 1, and leaching process temperature control is 78 DEG C, leachate PH=3.6.
Step d is with the difference of embodiment 1, is 88g/L's to the organic middle addition Ni ion concentration after saponification
Nickel chloride solution produces nickel soap, and organic after nickel soap is mixed with nickel screen leachate and extracted, through the extraction of extraction box 7 stage countercurrent,
Extraction phase compares O:A=1.5:1, the organic hydrochloric acid with 7mol/L that loads after extraction re-starts after the regeneration of extraction box 6 stage countercurrent
Saponification is reused.
Step e with implement 1 difference be, evaporation and concentration to evaporate after liquid nickeliferous for 320.5g/L when, stop steam
Send out, liquid after evaporation is put and is passed through cooling water circulation cooling to crystallizer, crystallization time is 24h, built-in temperature to be crystallized is down to
When 21 DEG C, close cooling water, crystallizer intercrystalline is put to centrifuge with centrifugation, completes solid-liquid separation, after being centrifuged, material is defeated
Deliver to be dried in rotary kiln and be dried, baking temperature is 39 DEG C, drying time 8min, after being dried, material is qualified Nickel dichloride. and produces
Product.
After testing, gained Nickel dichloride. product can meet Nickel dichloride. HG/T 2771-2009 standard.
Claims (2)
1. a kind of with waste and old printed nickel net for the method for raw material production Nickel dichloride. product it is characterised in that：Will be waste and old with remover
Photoresists on printed nickel net are removed, and the nickel screen after removing is leached with technical hydrochloric acid, and leachate, through P507 abstraction impurity removal, soaks
Slag tap for unreacted nickel screen, add technical hydrochloric acid to proceed leaching process, P507 raffinate is through evaporation, crystallization, centrifugation, dry
The qualified Nickel dichloride. product of dry output.
2. a kind of method with waste and old printed nickel net for raw material production Nickel dichloride. product according to claim 1, its feature
It is：A, configuration printing nickel net demoulding agent:Following reagent is proportionally added in a kettle with mechanical agitation with heater,
Addition reagent and ratio are：Main remover is hydrogen peroxide, and hydrogen peroxide is 2-5 with the mass ratio of water:1, help each component in remover
Mass ratio be：Dodecyl sodium sulfate：Fatty alcohol-polyoxyethylene ether：Ethanol=2-3:1-2:2-4, main remover with help stripping
The mass ratio of agent is：3-5:2, the pH value of remover is：10-14；
B, printing nickel net demoulding:After the completion of remover configuration, nickel screen to be stripped is totally submerged in remover, temperature is even
Insulation after speed rises to 50-80 DEG C removes photoresists, reacts 1-5h, takes out nickel screen water under high pressure and be carried out after 1-5h；
C, nickel screen leach：By after degumming nickel screen add technical hydrochloric acid leach, during temperature control be 50-90 DEG C, to be leached
Liquid pH value, for stopping Leach reaction during 3.0-4.5, is filtered；
D, leachate extraction：With P507 extractant extracting and purifying nickel screen leachate, extraction phase compares O:A=3-5:1, raffinate impurity
Content is：Ni >=180g/L, Co, Cu, Fe, Zn, Pb, Mn≤0.004g/L, Ca≤0.1g/L, Mg≤0.5g/L, Na≤1g/L；
E, raffinate evaporate, crystallize, are centrifuged, are dried：Qualified raffinate vaporizer is evaporated concentrating, evaporation and concentration is to steaming
After sending out liquid nickeliferous for 300-340g/L when, stop evaporation, liquid will put and be passed through cooling water circulation cooling to crystallizer after evaporation, knot
The brilliant time is 18-24h, when built-in temperature to be crystallized is down to 20-30 DEG C, closes cooling water, crystallizer intercrystalline is put to centrifugation
In machine, centrifugation, completes solid-liquid separation, and after being centrifuged, material is delivered to be dried in rotary kiln and is dried, and baking temperature is 20-40 DEG C, does
Dry time 3-8min, after being dried, material is qualified Nickel dichloride. product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610738616.8A CN106395921A (en) | 2016-08-29 | 2016-08-29 | Method used for producing nickel chloride products taking waste printing nickel screens as raw materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610738616.8A CN106395921A (en) | 2016-08-29 | 2016-08-29 | Method used for producing nickel chloride products taking waste printing nickel screens as raw materials |
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| CN106395921A true CN106395921A (en) | 2017-02-15 |
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| CN201610738616.8A Pending CN106395921A (en) | 2016-08-29 | 2016-08-29 | Method used for producing nickel chloride products taking waste printing nickel screens as raw materials |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109626448A (en) * | 2018-11-09 | 2019-04-16 | 浙江科菲科技股份有限公司 | A method of high-purity sulphuric acid nickel is produced with useless printed nickel net |
| CN109850958A (en) * | 2018-12-19 | 2019-06-07 | 浙江科菲科技股份有限公司 | A kind of discarded printed nickel net recovery and treatment method |
| CN110804697A (en) * | 2019-10-23 | 2020-02-18 | 金川集团股份有限公司 | Waste printed nickel screen stripping method |
| CN114314699A (en) * | 2021-12-31 | 2022-04-12 | 金川集团镍盐有限公司 | Iron removal method for nickel pill dissolving solution in chlorination system |
| CN114835176A (en) * | 2022-05-30 | 2022-08-02 | 金川集团镍盐有限公司 | Preparation method of spherical anhydrous nickel chloride product |
| CN114934183A (en) * | 2022-05-30 | 2022-08-23 | 金川集团镍盐有限公司 | Method for producing nickel sulfate solution by using waste nickel net |
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| CN101481149A (en) * | 2009-02-11 | 2009-07-15 | 四川师范大学 | Preparation of nickel nitrate solution |
| CN102436153A (en) * | 2011-10-28 | 2012-05-02 | 绍兴文理学院 | Photosensitive rubber stripping agent for printing screen and stripping method |
| CN104073635A (en) * | 2014-06-12 | 2014-10-01 | 金川集团股份有限公司 | Method of removing impurities out of nickel chloride leachate |
| CN105200238A (en) * | 2015-09-29 | 2015-12-30 | 广西银亿再生资源有限公司 | Method of recovering copper and nickel from plastic plated parts |
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2016
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481149A (en) * | 2009-02-11 | 2009-07-15 | 四川师范大学 | Preparation of nickel nitrate solution |
| CN102436153A (en) * | 2011-10-28 | 2012-05-02 | 绍兴文理学院 | Photosensitive rubber stripping agent for printing screen and stripping method |
| CN104073635A (en) * | 2014-06-12 | 2014-10-01 | 金川集团股份有限公司 | Method of removing impurities out of nickel chloride leachate |
| CN105200238A (en) * | 2015-09-29 | 2015-12-30 | 广西银亿再生资源有限公司 | Method of recovering copper and nickel from plastic plated parts |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109626448A (en) * | 2018-11-09 | 2019-04-16 | 浙江科菲科技股份有限公司 | A method of high-purity sulphuric acid nickel is produced with useless printed nickel net |
| CN109626448B (en) * | 2018-11-09 | 2021-07-06 | 浙江科菲科技股份有限公司 | Method for producing high-purity nickel sulfate by using waste printed nickel screen |
| CN109850958A (en) * | 2018-12-19 | 2019-06-07 | 浙江科菲科技股份有限公司 | A kind of discarded printed nickel net recovery and treatment method |
| CN110804697A (en) * | 2019-10-23 | 2020-02-18 | 金川集团股份有限公司 | Waste printed nickel screen stripping method |
| CN114314699A (en) * | 2021-12-31 | 2022-04-12 | 金川集团镍盐有限公司 | Iron removal method for nickel pill dissolving solution in chlorination system |
| CN114835176A (en) * | 2022-05-30 | 2022-08-02 | 金川集团镍盐有限公司 | Preparation method of spherical anhydrous nickel chloride product |
| CN114934183A (en) * | 2022-05-30 | 2022-08-23 | 金川集团镍盐有限公司 | Method for producing nickel sulfate solution by using waste nickel net |
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Application publication date: 20170215 |
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