CN106430775A - Comprehensive treatment and resource treatment method of nickel-containing waste liquid - Google Patents
Comprehensive treatment and resource treatment method of nickel-containing waste liquid Download PDFInfo
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- CN106430775A CN106430775A CN201610884608.4A CN201610884608A CN106430775A CN 106430775 A CN106430775 A CN 106430775A CN 201610884608 A CN201610884608 A CN 201610884608A CN 106430775 A CN106430775 A CN 106430775A
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- nickel
- waste liquid
- nickeliferous
- solid
- high concentration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/06—Carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
Abstract
The invention discloses a comprehensive treatment and resource treatment method of nickel-containing waste liquid. The comprehensive treatment and resource treatment method comprises the following steps: 1), collecting four types of nickel-containing waste liquid, namely nickel-electroplating waste liquid, nickel-plating rinsing waste liquid, nickel-deplating waste liquid and chemical nickel-plating waste liquid; 2), performing distilling concentration on the nickel-containing waste liquid to obtain distillate distilled water and remaining concentrated liquid; 3), recycling the distillate distilled water as recycled water, cooling and crystallizing the remaining concentrated liquid to obtain coarse crystal and a filtrate, and returning the filtrate to the step 2); 4),dissolving the coarse crystal to obtain a high-concentration nickel-containing solution, adjusting the pH of the high-concentration nickel-containing solution, and then adding chemicals to prepare high-purity metal nickel salt or ultrafine nickel powder. With the comprehensive treatment and resource treatment method, different kinds of nickel-containing waste liquid are treated in a centralized way, and are not required to be collected or treated class by class, so that unified treatment is achieved and practical application is facilitated; in the process of treating the nickel-containing waste liquid, no secondary pollution is caused, and the whole process is clean and pollution-free.
Description
Technical field
The present invention relates at a kind of processing method of nickeliferous waste liquid, specially a kind of nickeliferous waste liquid comprehensive control and resource
The method of reason.
Background technology
Electroplating industry is the important component part of national economy, the every field such as is widely used in producing, lives, wherein plating
Nickel processing capacity occupies second in whole electroplating industry, and in Ni-Speed, plating piece washings and waste plating solution account for plant effluent row
More than 90% for putting.Nickel in nickeliferous waste liquid can enter human body by the enrichment of food chain, so as to shadow after water body is entered
Growth promoter is rung, serious possibility causes cranial nerve pathological changes, so must be acted upon to the nickel in nickeliferous waste liquid.
In nickel plating production process, different process step will produce different nickeliferous waste liquids, cause the physics and chemistry of nickeliferous waste liquid
Property and nickel content are different.Process nickeliferous waste liquid at present to produce in different process step generally by waste collection pond
Nickeliferous waste collection be mixed to form final waste liquid after be uniformly processed again, bring certain difficulty to the final process of nickeliferous waste liquid
Degree, also reduces the efficiency of resource recycling.Traditional nickeliferous liquid waste processing is typically using chemical precipitation, electrolysis or film
Isolation technics are processed.Wherein, chemical precipitation method add medicament in referring to toward nickeliferous waste liquid so that nickel therein formed hard to tolerate
Precipitate remove, but as nickel ion is present with complex state form in waste liquid, need a large amount of precipitation medicaments to carry out which
Process, heavy metals qualified discharge can be caused, but the method generates substantial amounts of sludge.Although electrolysis can will be nickeliferous
Nickel in nickeliferous waste liquid is reclaimed by the nickel in waste liquid with electro deposited nickel or nikel powder form, but electrolysis tail water is still needed to further
Do harmless treatment.Nickeliferous waste liquid can be concentrated by membrane separation technique, and the nickeliferous waste liquid of the low concentration for being is through membrane filtration
After be divided into the nickeliferous waste liquid of high concentration with can waste discharge, membrane separation process is only to have carried out minimizing process to nickeliferous waste liquid, high
The nickeliferous waste liquid of concentration still needs to process further.Chemical precipitation method and electrolysis all only carry out harmless treatment to nickeliferous waste liquid,
Maximum resource recycling is not carried out to nickeliferous waste liquid, waste ample resources and the energy.
Content of the invention
The technical problem to be solved in the present invention is to overcome the processing method of existing nickeliferous waste liquid to be required to enter one to tail water
Step does the defect of harmless treatment, a kind of method for providing nickeliferous waste liquid comprehensive control and recycling treatment.
In order to solve above-mentioned technical problem, the invention provides following technical scheme:
A kind of nickeliferous waste liquid comprehensive control and the method for recycling treatment, comprise the following steps:
1) electronickelling waste liquid, nickel-plating rinsing waste water, are collected, moves back nickel-plating waste liquid, the nickeliferous waste liquid of four class of chemical nickel plating waste solution;
2), above-mentioned nickeliferous waste liquid is carried out distillation and concentration, obtains fraction distilled water and remaining dope;
3), water in fraction distilled water work is recycled, remaining dope crystallisation by cooling obtains coarse crystal and filtrate, will
Filtrate return to step 2);
4), coarse crystal is dissolved, high concentration solution containing nickel is obtained, the pH of high concentration solution containing nickel is adjusted, is subsequently adding medicine
Agent, reclaims nickel resources.
Further, the process of high concentration solution containing nickel can be divided into two routes, route one:Prepare high purity metal
Nickel salt;Route two:Prepare extra-fine nickel powder.
Further, can be respectively adopted in route one high concentration solution containing nickel prepare nickel sulfamic acid, basic nickel carbonate,
Nickel nitrate and nickel sulfate.
Preferably, step 4) in using in ammonia, piece alkali and potassium hydroxide one or several adjustment high concentrations nickeliferous
PH value >=12 of solution, then still aging 1~2h at 40~90 DEG C, solid-liquid separation;Solid adds 10 in batches~
The sulfamic acid solution of 50wt.%, after solid is completely dissolved, nNi in solution2+:nNH2SO3H=1:2~2.2, it is concentrated to give ammonia
Base nickel sulphonic acid.
Preferably, step 4) in molten using one or several in sodium carbonate, sodium bicarbonate, ammonium carbonate and ammonium hydrogen carbonate
Yu Shuizhong, configures the carbonate solution that pH value is 9~10, then mixes high concentration solution containing nickel and carbonate solution in proportion
Close, the pH for controlling mixed liquor is that 7~9, temperature is 30~80 DEG C, filters, obtain basic nickel carbonate after 1~2h of ageing.
Preferably, step 4) in using in ammonia, piece alkali and potassium hydroxide one or several adjustment high concentrations nickeliferous
PH value >=12 of solution, then still aging 1~2h at 40~90 DEG C, solid-liquid separation;Solid adds 10 in batches~
The salpeter solution of 40wt.%, after solid is completely dissolved, nNi in solution2+:nHNO3=1:2~2.2, it is concentrated to give nickel nitrate.
Preferably, step 4) in using in ammonia, piece alkali and potassium hydroxide one or several adjustment high concentrations nickeliferous
PH value >=12 of solution, then still aging 1~2h at 40~90 DEG C, solid-liquid separation;Solid adds 10 in batches~
The sulfuric acid solution of 40wt.%, after solid is completely dissolved, nNi in solution2+:nH2SO4=1:1~1.2, it is concentrated to give nickel sulfate.
Further, route two prepares extra-fine nickel powder.In step 4) in using in ammonia, piece alkali and potassium hydroxide and sulphuric acid
PH value of one or several adjustment high concentration solution containing nickels be 4~12, then add 0.1~1wt.%'s at 40~80 DEG C
Exciting agent, the surfactant of 0.01wt.%, filter after insulation 2h, and filtrate nickel is remained less than 1ppm, is directly entered sewage disposal
System, filter mud is extra-fine nickel powder after clear water washing and drying.Preferably, described exciting agent is polynary secondary alcohol, hydrazine hydrate
With one or several in sodium hypophosphite.Exciting agent can promote nickel ion in solution to be reduced into nickel simple substance.Preferably, institute
One or more in the surfactant that states PEG, SDBS and K12 for the degree of polymerization more than 2000.Surfactant, can control
The particle diameter of reduced nickel powder processed.
Nickel-bearing Waste liquid of the same race is focused on by the present invention, resource secondary metal nickel salt and extra-fine nickel powder, is not required to
Categorised collection process is carried out to nickel-containing waste water not of the same race, it is achieved that unitized process, beneficial to practical application;Process nickeliferous waste liquid
During do not produce secondary " pollution ", whole technological process cleanliness without any pollution.
Specific embodiment
Hereinafter the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
A kind of nickeliferous waste liquid comprehensive control and the method for recycling treatment, comprise the following steps:
1) electronickelling waste liquid, nickel-plating rinsing waste water, are collected, moves back nickel-plating waste liquid, the nickeliferous waste liquid of four class of chemical nickel plating waste solution;
2), above-mentioned nickeliferous waste liquid is carried out distillation and concentration, obtains fraction distilled water and remaining dope;
3), water in fraction distilled water work is recycled, remaining dope crystallisation by cooling obtains coarse crystal and filtrate, will
Filtrate return to step 2);
4), coarse crystal is dissolved, obtains high concentration solution containing nickel, using the one kind in ammonia, piece alkali and potassium hydroxide or
PH value >=12 of several adjustment high concentration solution containing nickels of person, then still aging 1~2h at 40~90 DEG C, solid-liquid separation;Will be solid
Body adds the sulfamic acid solution of 10~50wt.% in batches, after solid is completely dissolved, nNi in solution2+:nNH2SO3H=1:2
~2.2, it is concentrated to give nickel sulfamic acid.
Embodiment 2
A kind of nickeliferous waste liquid comprehensive control and the method for recycling treatment, comprise the following steps:
1) electronickelling waste liquid, nickel-plating rinsing waste water, are collected, moves back nickel-plating waste liquid, the nickeliferous waste liquid of four class of chemical nickel plating waste solution;
2), above-mentioned nickeliferous waste liquid is carried out distillation and concentration, obtains fraction distilled water and remaining dope;
3), water in fraction distilled water work is recycled, remaining dope crystallisation by cooling obtains coarse crystal and filtrate, will
Filtrate return to step 2);
4), coarse crystal is dissolved, high concentration solution containing nickel is obtained, using sodium carbonate, sodium bicarbonate, ammonium carbonate and bicarbonate
One or several in ammonium are soluble in water, configure the carbonate solution that pH value is 9~10, then by high concentration solution containing nickel and
Carbonate solution is mixed in proportion, and the pH for controlling mixed liquor is that 7~9, temperature is 30~80 DEG C, filters, obtain after 1~2h of ageing
Basic nickel carbonate.
Embodiment 3
A kind of nickeliferous waste liquid comprehensive control and the method for recycling treatment, comprise the following steps:
1) electronickelling waste liquid, nickel-plating rinsing waste water, are collected, moves back nickel-plating waste liquid, the nickeliferous waste liquid of four class of chemical nickel plating waste solution;
2), above-mentioned nickeliferous waste liquid is carried out distillation and concentration, obtains fraction distilled water and remaining dope;
3), water in fraction distilled water work is recycled, remaining dope crystallisation by cooling obtains coarse crystal and filtrate, will
Filtrate return to step 2);
4), coarse crystal is dissolved, obtains high concentration solution containing nickel, using the one kind in ammonia, piece alkali and potassium hydroxide or
PH value >=12 of several adjustment high concentration solution containing nickels of person, then still aging 1~2h at 40~90 DEG C, solid-liquid separation;Will be solid
Body adds the salpeter solution of 10~40wt.% in batches, after solid is completely dissolved, nNi in solution2+:nHNO3=1:2~2.2,
It is concentrated to give nickel nitrate.
Embodiment 4
A kind of nickeliferous waste liquid comprehensive control and the method for recycling treatment, comprise the following steps:
1) electronickelling waste liquid, nickel-plating rinsing waste water, are collected, moves back nickel-plating waste liquid, the nickeliferous waste liquid of four class of chemical nickel plating waste solution;
2), above-mentioned nickeliferous waste liquid is carried out distillation and concentration, obtains fraction distilled water and remaining dope;
3), water in fraction distilled water work is recycled, remaining dope crystallisation by cooling obtains coarse crystal and filtrate, will
Filtrate return to step 2);
4), coarse crystal is dissolved, obtains high concentration solution containing nickel, using the one kind in ammonia, piece alkali and potassium hydroxide or
PH value >=12 of several adjustment high concentration solution containing nickels of person, then still aging 1~2h at 40~90 DEG C, solid-liquid separation;Will be solid
Body adds the sulfuric acid solution of 10~40wt.% in batches, after solid is completely dissolved, nNi in solution2+:nH2SO4=1:1~1.2,
It is concentrated to give nickel sulfate.
Embodiment 5
A kind of nickeliferous waste liquid comprehensive control and the method for recycling treatment, comprise the following steps:
1) electronickelling waste liquid, nickel-plating rinsing waste water, are collected, moves back nickel-plating waste liquid, the nickeliferous waste liquid of four class of chemical nickel plating waste solution;
2), above-mentioned nickeliferous waste liquid is carried out distillation and concentration, obtains fraction distilled water and remaining dope;
3), water in fraction distilled water work is recycled, remaining dope crystallisation by cooling obtains coarse crystal and filtrate, will
Filtrate return to step 2);
4), coarse crystal is dissolved, high concentration solution containing nickel is obtained, using in ammonia, piece alkali and potassium hydroxide and sulphuric acid
PH value of one or several adjustment high concentration solution containing nickels are 4~12, then add swashing for 0.1~1wt.% at 40~80 DEG C
Agent, the surfactant of 0.01wt.% is sent out, is filtered after insulation 2h, filtrate nickel is remained less than 1ppm, is directly entered sewage disposal system
System, filter mud is extra-fine nickel powder after clear water washing and drying.Described exciting agent is polynary secondary alcohol, hydrazine hydrate and ortho phosphorous acid
The mixture of sodium, exciting agent can promote nickel ion in solution to be reduced into nickel simple substance.Surfactant is more than 2000 for the degree of polymerization
PEG, SDBS and K12 in mixture, the particle diameter of reduced nickel powder can be controlled.
Finally it should be noted that:The preferred embodiments of the present invention are the foregoing is only, the present invention are not limited to,
Although being described in detail to the present invention with reference to the foregoing embodiments, for a person skilled in the art, which still may be used
To modify to the technical scheme described in foregoing embodiments, or equivalent is carried out to which part technical characteristic.
All any modification, equivalent substitution and improvement that within the spirit and principles in the present invention, is made etc., should be included in the present invention's
Within protection domain.
Claims (8)
1. a kind of method of nickeliferous waste liquid comprehensive control and recycling treatment, it is characterised in that comprise the following steps:
1) electronickelling waste liquid, nickel-plating rinsing waste water, are collected, moves back nickel-plating waste liquid, the nickeliferous waste liquid of four class of chemical nickel plating waste solution;
2), above-mentioned nickeliferous waste liquid is carried out distillation and concentration, obtains fraction distilled water and remaining dope;
3), water in fraction distilled water work is recycled, remaining dope crystallisation by cooling obtains coarse crystal and filtrate, by filtrate
Return to step 2);
4), coarse crystal is dissolved, high concentration solution containing nickel is obtained, the pH of high concentration solution containing nickel is adjusted, medicament is subsequently adding, return
Receive nickel resources.
2. a kind of method of nickeliferous waste liquid comprehensive control and recycling treatment as claimed in claim 1, it is characterised in that described
Step 4) in using in ammonia, piece alkali and potassium hydroxide one or several adjustment high concentration solution containing nickels pH value >=12,
Then still aging 1~2h at 40~90 DEG C, solid-liquid separation;Solid is added in batches the sulfamic acid of 10~50wt.% molten
Liquid, after solid is completely dissolved, nNi in solution2+:nNH2SO3H=1:2~2.2, it is concentrated to give nickel sulfamic acid.
3. a kind of method of nickeliferous waste liquid comprehensive control and recycling treatment as claimed in claim 1, it is characterised in that described
Step 4) in soluble in water using one or several in sodium carbonate, sodium bicarbonate, ammonium carbonate and ammonium hydrogen carbonate, configure pH value
For 9~10 carbonate solution, then high concentration solution containing nickel and carbonate solution are mixed in proportion, control the pH of mixed liquor
It is 30~80 DEG C for 7~9, temperature, filters after 1~2h of ageing, obtain basic nickel carbonate.
4. a kind of method of nickeliferous waste liquid comprehensive control and recycling treatment as claimed in claim 1, it is characterised in that described
Step 4) in using in ammonia, piece alkali and potassium hydroxide one or several adjustment high concentration solution containing nickels pH value >=12,
Then still aging 1~2h at 40~90 DEG C, solid-liquid separation;Solid is added the salpeter solution of 10~40wt.% in batches, Gu
After body is completely dissolved, nNi in solution2+:nHNO3=1:2~2.2, it is concentrated to give nickel nitrate.
5. a kind of method of nickeliferous waste liquid comprehensive control and recycling treatment as claimed in claim 1, it is characterised in that described
Step 4) in using in ammonia, piece alkali and potassium hydroxide one or several adjustment high concentration solution containing nickels pH value >=12,
Then still aging 1~2h at 40~90 DEG C, solid-liquid separation;Solid is added the sulfuric acid solution of 10~40wt.% in batches, Gu
After body is completely dissolved, nNi in solution2+:nH2SO4=1:1~1.2, it is concentrated to give nickel sulfate.
6. a kind of method of nickeliferous waste liquid comprehensive control and recycling treatment as claimed in claim 1, it is characterised in that described
Step 4) in using in ammonia, piece alkali and potassium hydroxide and sulphuric acid one or several adjustment high concentration solution containing nickels pH value
For 4~12, exciting agent, the surfactant of 0.01wt.% of 0.1~1wt.% are then added at 40~80 DEG C, after insulation 2h
Filter, filtrate nickel is remained less than 1ppm, is directly entered sewage disposal system, filter mud is ultra-fine nickel after clear water washing and drying
Powder.
7. a kind of method of nickeliferous waste liquid comprehensive control and recycling treatment as claimed in claim 6, it is characterised in that described
Exciting agent be one or several in polynary secondary alcohol, hydrazine hydrate and sodium hypophosphite.
8. a kind of nickeliferous waste liquid comprehensive control as claimed in claims 6 or 7 and the method for recycling treatment, it is characterised in that
One or more in described surfactant PEG, SDBS and K12 for the degree of polymerization more than 2000.
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Cited By (4)
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CN106830452A (en) * | 2017-02-27 | 2017-06-13 | 环境保护部华南环境科学研究所 | A kind of method that nickel, buffer salt and water are reclaimed in chemically nickel plating Ageing solution |
CN106894047A (en) * | 2017-03-10 | 2017-06-27 | 傅楚闽 | A kind of high-efficiency environment friendly recovery method of nickel in chemical nickel-plating ageing liquid |
CN108191107A (en) * | 2017-12-29 | 2018-06-22 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | The recovery system and method for single nickel salt coloring and medium temperature sealing of hole medicament in aluminium processing |
CN114162950A (en) * | 2021-12-02 | 2022-03-11 | 扬州市景杨表面工程有限公司 | Nickel-containing waste liquid treatment and comprehensive utilization process |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106830452A (en) * | 2017-02-27 | 2017-06-13 | 环境保护部华南环境科学研究所 | A kind of method that nickel, buffer salt and water are reclaimed in chemically nickel plating Ageing solution |
CN106830452B (en) * | 2017-02-27 | 2018-02-06 | 环境保护部华南环境科学研究所 | A kind of method that nickel, buffer salt and water are reclaimed in chemically nickel plating Ageing solution |
CN106894047A (en) * | 2017-03-10 | 2017-06-27 | 傅楚闽 | A kind of high-efficiency environment friendly recovery method of nickel in chemical nickel-plating ageing liquid |
CN108191107A (en) * | 2017-12-29 | 2018-06-22 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | The recovery system and method for single nickel salt coloring and medium temperature sealing of hole medicament in aluminium processing |
CN114162950A (en) * | 2021-12-02 | 2022-03-11 | 扬州市景杨表面工程有限公司 | Nickel-containing waste liquid treatment and comprehensive utilization process |
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