CN103736994B - A kind of processing method of chemical nickel-plating solution - Google Patents

A kind of processing method of chemical nickel-plating solution Download PDF

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Publication number
CN103736994B
CN103736994B CN201410016076.3A CN201410016076A CN103736994B CN 103736994 B CN103736994 B CN 103736994B CN 201410016076 A CN201410016076 A CN 201410016076A CN 103736994 B CN103736994 B CN 103736994B
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Prior art keywords
powder
solution
nickel
chemical
processing method
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CN201410016076.3A
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Chinese (zh)
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CN103736994A (en
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吴浩
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NANJING DELEI SCIENCE AND TECHNOLOGY Co Ltd
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NANJING DELEI SCIENCE AND TECHNOLOGY Co Ltd
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Priority to CN201410016076.3A priority Critical patent/CN103736994B/en
Publication of CN103736994A publication Critical patent/CN103736994A/en
Priority to PCT/CN2015/070347 priority patent/WO2015106649A1/en
Priority to JP2016546849A priority patent/JP6154961B2/en
Priority to KR1020167022034A priority patent/KR101737292B1/en
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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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17—Metallic particles coated with metal
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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    • C01—INORGANIC CHEMISTRY
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    • C01F7/00—Compounds of aluminium
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    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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    • C23C18/1601—Process or apparatus
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Abstract

The invention provides a kind of processing method of chemical nickel-plating solution, comprise the following steps: utilize chemical nickeling ageing liquid to produce powder; In powder enrobing process, continue stir the chemical nickeling ageing liquid adding powder and heat the solution added containing sodium hypophosphite, stir again after making chemical nickeling ageing liquid become white clear solution by the blueness being rich in nickel and heat; Advanced oxidation, leaches the nickel hydroxide white precipitate of production in the chemical nickeling ageing liquid adding next batch and dissolves reuse; Solution through previous step process is continued to carry out advanced oxidation.After present invention process process, the nickel in aging waste liquid can be down to below 1mg/L, has both achieved and has recycled more than 99.9% of nickel, can produce again the functional powder material that added value is higher, and eliminate the pollution of nickel to environment.

Description

A kind of processing method of chemical nickel-plating solution
Technical field
The invention belongs to surface treatment and technical field of sewage, particularly a kind of processing method of chemical nickeling ageing liquid.
Background technology
Existing chemical nickeling ageing liquid waste disposal technique mostly is regeneration of aging liquid, and processing method is as follows:
1. the regenerating treater of chemical nickel-plating liquid mainly contains chemical pumping, calcium carbonate process bed, stillpot, filter pump, connected and composed successively by pipeline, ammoniacal liquor is added groove and is added ammoniacal liquor to stillpot, and the nickel-plating liquid in chemical nickel plating groove is extracted into calcium carbonate filtering bed by chemical pumping, and filter pump sends the chemical nickel-plating liquid after process back to chemical nickel plating groove.
2. will with nickelous sulfate for main salt, sodium hypophosphite is that the chemical nickel-plating liquid cooling of reducing agent leaves standstill, accessory substance sodium sulphate in chemical nickel-plating liquid and sodium phosphite are crystallized out from solution, obtain the chemical nickel-plating liquid regenerated, being that chemical nickel-plating liquid obtains auto purification process, recovering because being rich in the accessory substance such as sodium sulphate and sodium phosphite and the deposition velocity of aging chemical nickel-plating liquid.
3. first regulate chemical nickeling ageing liquid pH value, electrodialysis process 1 ~ 8 hour under uniform temperature, current density, the Ageing solution after being disposed supplements can directly use through composition.Concentrate after electrodialysis process of learning from else's experience carries out chemical precipitation process, and feed intake stirring in accordance with the appropriate ratio, ageing 1 ~ 8 hour.
It is more than the technical method of more existing process chemical nickeling ageing waste liquids, can by recycling after the recycling of aging chemical nickel-plating liquid in order to upper method, but the quality of chemical nickel-plating liquid to nickel plating coating adopting these methods to reclaim first has a certain impact, quality of coating can not ensure, can not adapt to require high production field to coating technology, second, new discarded object can be produced in these processes, still can not accomplish environment friendly and pollution-free.
Summary of the invention
The object of this invention is to provide a kind of processing method of chemical nickel-plating solution, to solve the unwarrantable problem of quality of coating of the chemical nickel plating existed in the method for existing process chemical nickeling ageing waste liquid.
Another object of the present invention solves the new discarded object of the generation that exists in the method for existing process chemical nickeling ageing waste liquid, can not accomplish environment friendly and pollution-free problem.
For achieving the above object, the present invention is by the following technical solutions:
A processing method for chemical nickel-plating solution, comprises the following steps:
A, utilize chemical nickeling ageing liquid produce powder: chemical nickeling ageing liquid is pumped in the container that can stir with continuous heating, using chemical nickeling ageing liquid as raw material, utilize chemical nickeling ageing liquid to carry out coated to the powder surface that can carry out surface chemistry deposition, produce nickel bag powder;
B, in powder enrobing process, continue stir the chemical nickeling ageing liquid adding powder and heat holding temperature at 80 ~ 92 DEG C, adding alkaline solution regulates pH value to be stabilized between 4.5 ~ 7.5, add the solution containing sodium hypophosphite, stir again after making chemical nickeling ageing liquid become white clear solution by the blueness being rich in nickel and heat more than 2 hours, make nickel ion concentration in solution be reduced to below 20mg/L, coated powder after separation, rinsing, drying as product;
C, the advanced oxidation more than 1 hour being continued after the cooling of the solution of step b process, adding alkaline solution regulates between pH value to 8 ~ 9, leached in the chemical nickeling ageing liquid adding next batch by the nickel hydroxide white precipitate of production and dissolve reuse, in the solution of this step process, nickel ion content is down to below 1mg/L;
D, continued to carry out advanced oxidation by the solution through step c process, in time not adding alkaline solution, pH value is stabilized in till 6.5 ~ 7.5.
Preferably, the described powder that can carry out surface chemistry deposition be iron powder, the one of ferroalloy powder and the pretreated ceramic powders that metallizes through nonmetallic surface.
Preferably, in step a, before powder enrobing process, first nickel in chemical nickel-plating ageing liquid ion concentration is analyzed, and by determining that chemical nickeling ageing liquid volume calculates weight nickeliferous in solution, confirm with this weight needing to add powder, thus the powder of a certain setting ratio of nickeliferous 0.1% ~ 80% can be produced on demand.
Preferably, in step a, the particle diameter of powder is between 1 nanometer to 200 micron.
Preferably, in step a through nonmetallic surface metallize the treatment process of pretreated ceramic powders be alligatoring, sensitization, activation or alligatoring and sensitization and activation in one.
Preferably, the ceramic powders in step a is containing one or more ceramic powders in alundum (Al2O3), zirconium dioxide, titanium dioxide, silica composition.
Further, when the powder that can carry out surface chemistry deposition be iron or ferroalloy powder time, the nickel bag powder of generation is as the raw material in the fields such as powder metallurgy; When the powder that can carry out surface chemistry deposition is ceramic powders, the nickel bag powder of generation is as the raw material of the functional materials such as conduction, absorbing material.
Preferably, the advanced oxidation described in step c, d is H 2o 2+ UV system, O 3+ UV system, O 3one or more of the method for treating water of+catalyst.
Further, the alkaline solution in step b, c, d is potassium hydroxide or solution of potassium carbonate, and the Ageing solution after its process is as the raw material of liquid composite fertilizer; Or alkaline solution is NaOH or sodium carbonate liquor; Or alkaline solution is aqua calcis or lime powder, as the raw material of phosphate fertilizer after the precipitate and separate of formation, waste water then can be introduced Sewage Plant and continue process.
Further, the part drag-out of chemical nickel plating supplements as evaporation water after the secondary recovery of trough rim, and washings clear water after UF membrane realizes Treated sewage reusing, and dense water is mixed into Ageing solution process.
The invention has the beneficial effects as follows: after present invention process process, nickel in aging waste liquid can be down to below 1mg/L, both achieved and more than 99.9% of nickel had been recycled, and the functional powder material that added value is higher can have been produced again, and eliminate the pollution of nickel to environment.The hypophosphite contained in remaining aging waste liquid and phosphite form phosphate by advanced oxidation operation, can conveniently be used as the raw material of fertilizer.The present invention had both achieved the comprehensive utilization of resource, prevented environmental pollution again.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention will be further described.
A processing method for chemical nickel-plating solution, comprises the following steps:
A, utilize chemical nickeling ageing liquid produce powder: first nickel in chemical nickel-plating ageing liquid ion concentration is analyzed, and by determining that chemical nickeling ageing liquid volume calculates weight nickeliferous in solution, confirm with this weight needing to add powder, thus the powder of a certain setting ratio of nickeliferous 0.1% ~ 80% can be produced on demand; Chemical nickeling ageing liquid is pumped in the container that can stir with continuous heating, using chemical nickeling ageing liquid as raw material, utilize chemical nickeling ageing liquid to carry out coated to the powder surface that can carry out surface chemistry deposition, produce nickel bag powder; The particle diameter of preferred powder is between 1 nanometer to 200 micron; Can carry out the preferred iron powder of powder of surface chemistry deposition, ferroalloy powder and metallize pretreated ceramic powders through nonmetallic surface, ceramic powders is containing one or more ceramic powders in alundum (Al2O3), zirconium dioxide, titanium dioxide, silica composition; Through nonmetallic surface metallize the treatment process of pretreated ceramic powders be alligatoring, sensitization, activation or alligatoring and sensitization and activation in one;
When the powder that can carry out surface chemistry deposition be iron or ferroalloy powder time, the nickel bag powder of generation is as the raw material in the fields such as powder metallurgy; When the powder that can carry out surface chemistry deposition is ceramic powders, the nickel bag powder of generation is as the raw material of the functional materials such as conduction, absorbing material;
B, in powder enrobing process, continue stir the chemical nickeling ageing liquid adding powder and heat holding temperature at 80 ~ 92 DEG C, adding alkaline solution regulates pH value to be stabilized between 4.5 ~ 7.5, add the solution containing sodium hypophosphite, stir again after making chemical nickeling ageing liquid become white clear solution by the blueness being rich in nickel and heat more than 2 hours, make nickel ion concentration in solution be reduced to below 20mg/L, coated powder after separation, rinsing, drying as product;
C, the advanced oxidation more than 1 hour being continued after the cooling of the solution of step b process, adding alkaline solution regulates between pH value to 8 ~ 9, leached in the chemical nickeling ageing liquid adding next batch by the nickel hydroxide white precipitate of production and dissolve reuse, in the solution of this step process, nickel ion content is down to below 1mg/L;
D, continued to carry out advanced oxidation by the solution through step c process, in time not adding alkaline solution, pH value is stabilized in till 6.5 ~ 7.5, and the solution through this process is sold as the raw material of liquid composite fertilizer.
Advanced oxidation in step c, d is H 2o 2+ UV system, O 3+ UV system, O 3one or more of the method for treating water of+catalyst, neither to other material introduced in solution except O, H, can produce again the hydroxyl radical free radical with Strong oxdiative ability and the phosphorus oxidation of lower valency is high-valence state and makes organic matter fast degradation in solution.
Alkaline solution in step b, c, d is potassium hydroxide or solution of potassium carbonate, and the Ageing solution after its process is as the raw material of liquid composite fertilizer; Or alkaline solution is NaOH or sodium carbonate liquor; Or alkaline solution is aqua calcis or lime powder, as the raw material of phosphate fertilizer after the precipitate and separate of formation, waste water then can be introduced Sewage Plant and continue process.
The part drag-out of chemical nickel plating supplements as evaporation water after the secondary recovery of trough rim, and washings clear water after UF membrane realizes Treated sewage reusing, and dense water is mixed into Ageing solution process.
Below in conjunction with specific embodiment, the present invention will be further described, and according to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, the content described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
embodiment 1:
The 500L acid chemical plating nickel solution of use 6 cycle periods is pumped into the container that is greater than 500L, it is 0.075M that chemical analysis goes out nickel ion concentration, calculate in solution altogether containing nickel=58.69*0.075*500=2200.875 gram, the nickel iron clad powder of planned production iron content about 75%, heating agitating solution, add 500 object iron powder 7kg, potassium hydroxide solution with 20% to regulate about pH value to 7 and continues to maintain, when there being a large amount of bubble to discharge in solution, altogether the sodium hypophosphite of 10kg is slowly added in solution, until after solution clarified solution water white transparency, maintain stir and insulation 85 ~ 90 DEG C more than two hours, cooled and filtered solution, by powder rinsing dry packing, to weigh to obtain 9.3kg nickel-phosphorus alloy iron clad powder, Powder Metallurgy Industry part can be sold to and substitute nickel powder use.
Solution after filtering is analyzed, nickel content is 13mg/L, with " moral space is clear " sewage treating machine persistent loop process that a bench-type number is NR150/4-240P12, it is the catalytic reactor of R150 that this machine have employed 4 models, ozone generator is 120g/ hour, and the circular flow of pump is 12 cubes ms/h; Potassium hydroxide solution with 20% regulates pH value 8 ~ 9, maintain the catalytic ozonation 2 ~ 3 hour of " moral space is clear " sewage treating machine to solution of NR150/4-120P10, add in the chemical nickeling ageing liquid of next batch after the white precipitate occurred in solution is separated, the stillness of night proceeds catalytic ozonation, until pH value no longer declines maintain about 7, in solution, P, K content is greater than 5%, can be supplied to the compound fertilizer producer and use as raw material after cooling.
In the present embodiment, iron powder can be replaced with ferroalloy powder, potassium hydroxide solution replaces with solution of potassium carbonate, can reach same effect.
Catalytic ozonation mode can also replace with H 2o 2+ UV system, O 3+ UV system, O 3one or more modes combined of the method for treating water of+catalyst.
embodiment 2:
The 300L acid chemical plating nickel solution of use 6 cycle periods is pumped into the container that is greater than 300L, it is 0.06M that chemical analysis goes out nickel ion concentration, calculate in solution altogether containing nickel=58.69*0.06*300=1056.42 gram, planned production is containing the nickel bag ceramic powder of nickel-phosphorus alloy about 35%, add 200 object alundum (Al2O3) powder 2.1kg, this powder first carries out steps of processing through the pretreatment process of nonmetallic surface plating: 50%H 2sO 4+ 5%HF solution alligatoring 20 minutes---washing---15g/LSnCL 2---washing---1g/LPdCL solution 2 minutes---washing that+50ml/LHCL solution soaks 10 minutes.
Heating agitating solution, sodium hydroxide solution with 20% regulates pH value to 6.5 and continues to maintain, add above-mentioned pretreated ceramic powders, when there being a large amount of bubble to discharge in solution, altogether the sodium hypophosphite of 5.5kg is slowly added in solution, until after solution clarified solution water white transparency, maintain stir and insulation 85-90 DEG C more than two hours, cooled and filtered solution, by powder rinsing dry packing, 3.2kg nickel-phosphorus alloy bag ceramic powders of weighing to obtain, to this powder measurement, its specific insulation is 0.015 Ω m, can add antistatic coating and substitute nickel powder use.
Solution after filtering is analyzed, nickel content is 11mg/L, with " moral space is clear " sewage treating machine persistent loop process that a bench-type number is NR150/2-60P5, it is the catalytic reactor of R150 that this machine have employed 2 models, ozone generator is 60g/ hour, and the flow of circulating pump is 5 cubes ms/h; Sodium hydroxide solution with 20% regulates pH value 8-9, maintain the catalytic ozonation 3 hour of " moral space is clear " sewage treating machine to solution of NR150/2-60P5, add in the chemical nickeling ageing liquid of next batch after being separated by the white precipitate occurred in solution, carrying out nickel content analysis to solution is 0.7mg/L; Proceed catalytic ozonation to the stillness of night, and be greater than 7 with aqua calcis maintenance pH value, until pH value no longer declines, produce a large amount of precipitation in solution, cleaner liquid is introduced blow-off line, and sediment presses fixed-end forces.
In the present embodiment, alundum (Al2O3) powder can also to replace with in alundum (Al2O3), zirconium dioxide, titanium dioxide, silica composition one or more ceramic powders, NaOH can replace with sodium carbonate, can reach the technique effect identical with the present embodiment.
Above-mentioned ceramic powders is obtained by a kind of pretreating process process in alligatoring, sensitization, activation or alligatoring and sensitization and activation.
embodiment 3:
Potassium hydroxide solution in embodiment 1 is replaced with aqua calcis or lime powder, and as the raw material of phosphate fertilizer after the precipitate and separate of formation, waste water then can be introduced Sewage Plant and continue process.
The part drag-out of chemical nickel plating supplements as evaporation water after the secondary recovery of trough rim, and washings clear water after UF membrane realizes Treated sewage reusing, and dense water is mixed into Ageing solution process.

Claims (9)

1. a processing method for chemical nickel-plating solution, is characterized in that: comprise the following steps:
A, utilize chemical nickeling ageing liquid produce powder: chemical nickeling ageing liquid is pumped in the container that can stir with continuous heating, using chemical nickeling ageing liquid as raw material, utilize chemical nickeling ageing liquid to carry out coated to the powder surface that can carry out surface chemistry deposition, produce nickel bag powder;
B, in powder enrobing process, continue stir the chemical nickeling ageing liquid adding powder and heat holding temperature at 80 ~ 92 DEG C, adding alkaline solution regulates pH value to be stabilized between 4.5 ~ 7.5, add the solution containing sodium hypophosphite, stir again after making chemical nickeling ageing liquid become white clear solution by the blueness being rich in nickel and heat more than 2 hours, make nickel ion concentration in solution be reduced to below 20mg/L, coated powder after separation, rinsing, drying as product;
C, the advanced oxidation more than 1 hour being continued after the cooling of the solution of step b process, adding alkaline solution regulates between pH value to 8 ~ 9, leached in the chemical nickeling ageing liquid adding next batch by the nickel hydroxide white precipitate of production and dissolve reuse, in the solution of this step process, nickel ion content is down to below 1mg/L;
D, continued to carry out advanced oxidation by the solution through step c process, in time not adding alkaline solution, pH value is stabilized in till 6.5 ~ 7.5.
2. the processing method of chemical nickel-plating solution as claimed in claim 1, is characterized in that: the described powder that can carry out surface chemistry deposition is iron powder, the one of ferroalloy powder and the pretreated ceramic powders that metallizes through nonmetallic surface.
3. the processing method of chemical nickel-plating solution as claimed in claim 1, it is characterized in that: in step a, before powder enrobing process, first nickel in chemical nickel-plating ageing liquid ion concentration is analyzed, and by determining that chemical nickeling ageing liquid volume calculates weight nickeliferous in solution, confirm with this weight needing to add powder, thus the powder of a certain setting ratio of nickeliferous 0.1% ~ 80% can be produced on demand.
4. the processing method of chemical nickel-plating solution as claimed in claim 1 or 2, is characterized in that: in step a, the particle diameter of powder is between 1 nanometer to 200 micron.
5. the processing method of chemical nickel-plating solution as claimed in claim 2, is characterized in that: the ceramic powders in step a is containing one or more ceramic powders in alundum (Al2O3), zirconium dioxide, titanium dioxide, silica composition.
6. the processing method of chemical nickel-plating solution as claimed in claim 1 or 2, is characterized in that: in step a, the powder that can carry out surface chemistry deposition be iron powder or ferroalloy powder time, the nickel bag powder of generation is as the raw material of field of powder metallurgy; When the powder that can carry out surface chemistry deposition is ceramic powders, the nickel bag powder of generation is as the raw material of conduction, absorbing material functional material.
7. the processing method of chemical nickel-plating solution as claimed in claim 1, is characterized in that: the advanced oxidation described in step c, d is H 2o 2+ UV system, O 3+ UV system, O 3one or more of the method for treating water of+catalyst.
8. the processing method of chemical nickel-plating solution as claimed in claim 1, is characterized in that: the alkaline solution in step b, c, d is potassium hydroxide or solution of potassium carbonate, and the Ageing solution after its process is as the raw material of liquid composite fertilizer; Or alkaline solution is NaOH or sodium carbonate liquor; Or alkaline solution is aqua calcis or calcium oxide solution, as the raw material of phosphate fertilizer after the precipitate and separate of formation, waste water then can be introduced Sewage Plant and continue process.
9. the processing method of chemical nickel-plating solution as claimed in claim 1, it is characterized in that: the part drag-out of chemical nickel plating supplements as evaporation water after the secondary recovery of trough rim, washings clear water after UF membrane realizes Treated sewage reusing, and dense water is mixed into Ageing solution process.
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CN103736994B (en) * 2014-01-15 2015-11-18 南京德磊科技有限公司 A kind of processing method of chemical nickel-plating solution
CN106045123B (en) * 2016-07-15 2019-03-08 苏州市东方环境工程有限公司 A kind of recycling and zero discharge recovery process method of chemical nickel waste liquid
CN107604346A (en) * 2017-09-06 2018-01-19 中航沈飞民用飞机有限责任公司 The processing method of a kind of aging method of chemical conversion solution and the chemical conversion solution newly prepared to sheet metal
CN109097807A (en) * 2018-07-27 2018-12-28 佛山市三水雄鹰铝表面技术创新中心有限公司 The method of single nickel salt coloring recycling hole sealing agent and Waste water utilization
CN111333152A (en) * 2019-04-11 2020-06-26 西南科技大学 Method for treating high-concentration nickel-phosphorus-containing organic waste liquid through electrolytic oxidation
CN112158978B (en) * 2020-09-14 2021-08-10 浙江海拓环境技术有限公司 Method for treating hypophosphite in chemical nickel plating waste liquid
CN112251741A (en) * 2020-11-13 2021-01-22 北京曙光航空电气有限责任公司 Preparation and repair method of nickel plating film repair liquid

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