CN103726036B - Environment-friendly high-brightness medium-phosphorus chemical nickel-plating additive - Google Patents
Environment-friendly high-brightness medium-phosphorus chemical nickel-plating additive Download PDFInfo
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- CN103726036B CN103726036B CN201410031854.6A CN201410031854A CN103726036B CN 103726036 B CN103726036 B CN 103726036B CN 201410031854 A CN201410031854 A CN 201410031854A CN 103726036 B CN103726036 B CN 103726036B
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Abstract
The invention discloses an environment-friendly high-brightness medium-phosphorus chemical nickel-plating additive which is composed of components A and B, wherein the component A comprises the following raw materials: a 2-5mg/L mixture of nano copper and a soluble copper salt, 2-4mg/L rhenium sulfate, 1-4mg/L sodium allysulfonate (ALS), a complexing agent, a stabilizer, and 20-40g/L NaOH; the component B comprises the following raw materials: 1-4mg/L 1,4-bis(2-hydroxyethoxy)-2-butyne (BEO), 1-3mg/L N,N-diethylaminopropyne (DEP), 1-4mg/L dibenzenesulfonimide (BBI), and 2-4mg/L sodium hydroxymethanesulphonate (PN). The formula of the environment-friendly high-brightness medium-phosphorus chemical nickel-plating additive provided by the invention contains no heavy metal ions such as cadmium and lead, and is harmless to the environment; if applied to a chemical nickel-plating solution, the additive is capable of keeping the plating solution stable so that the obtained coating is even and compact, low in porosity, high in brightness and good in nitric acid resistance; more specifically, even though the nickel coating is soaked in concentrated nitric acid for 300 seconds, the nickel coating does not change color.
Description
Technical field
The present invention relates to phosphorus chemistry nickel plating additive and preparation method thereof in a kind of environment-friendly type height light.
Background technology
Chemical nickel plating can be described as electroless nickel plating again, is to rely on the chemical reaction of autocatalysis in the process for treating surface of metallic surface nickel deposited, nickel alloy plating layer in containing the solution of nickel salt, reductive agent and other ancillary component.The coating that above technique obtains has the advantages such as hardness is higher, solidity to corrosion good, wear-resisting, thickness of coating is even, is used widely at the numerous areas of the industrial aspect such as machinery, electronics, petrochemical complex, mining, medicine equipment, automobile, aviation.The coating obtained by middle phosphorus chemistry nickel plating technology has good solidity to corrosion, and containing heavy metal ion such as lead ions in traditional nickel chemical plating technology stablizer, brightening agent contains cadmium ion compound.These harmful heavy metals in traditional chemical nickel-plating waste water, although still the difficulty of wastewater treatment is very big less for addition, make it accumulate in the environment because dealing with improperly, severe contamination will be caused to local environment, the character of heavy metal itself makes this impact of polluting generation permanence, and the injury caused ecotope and human survival is catastrophic.
In chemical nickel-plating solution, additive adds, not only can stop or postpone the Auto-decomposition of chemical nickel-plating solution, play the effect of stable plating solution, sometimes can also add fast response, improve phosphorus content and the internal stress of chemical Ni-plating layer, thus, for a ripe electroless plating nickel product, additive is absolutely necessary important component part, but traditional additive is many containing heavy metals such as lead ions, is inevitably mingled with plumbous etc. to environment and the harmful heavy metal of human body in chemical nickel coating.Particularly in recent years, people require more and more higher to the bright property of chemical nickel, in order to obtain coating attractive in appearance, propose the method adding brightening agent in chemical nickel-plating solution, and the requirement, particularly product technology that can not meet people as the nickel chemical plating technology of stablizer and brightening agent using heavy metal lead, cadmium ion of traditional relative maturity require and environmental emission requirement.
Summary of the invention
The object of this invention is to provide phosphorus chemistry nickel plating additive in a kind of environment-friendly type height light.
The technical solution used in the present invention is: phosphorus chemistry nickel plating additive in a kind of environment-friendly type height light, it is made up of A and B two kinds of components, component A comprises the raw material of following concentration: the Nanometer Copper of 2-5mg/L and the mixture of soluble copper salt, the sulfuric acid rhenium of 2-4mg/L, 1-4mg/L sodium allyl sulfonate (ALS), complexing agent, stablizer, the NaOH of 20-40g/L; B component comprises the raw material of following concentration: the butynediol diethoxy ether (BEO) of 1-4mg/L, the N of 1-3mg/L, N-diethyl propargylamine (DEP), the BBI (BBI) of 1-4mg/L, the sodium hydroxymethane sulfonate (PN) of 2-4mg/L.
Described complexing agent is citric acid, lactic acid, propionic acid, DL-oxysuccinic acid, the mixture of succinic acid.
Described stablizer is tellurium dioxide, bismuth citrate, thiocarbamide, the mixture of Potassium Iodate.
Described soluble copper salt is copper sulfate, and in the mixture of nanometer copper and copper sulfate, the mass percent of copper sulfate is 50%-57%.
The content of each composition of complexing agent of the present invention is: citric acid 2.5-8g/L, lactic acid 12-70 g/L, propionic acid 5-40 g/L, DL-oxysuccinic acid 2-10 g/L, succinic acid 2-8 g/L.
The each component content of stablizer of the present invention is: tellurium dioxide 0.001-0.0017g/L, bismuth citrate 0.1-0.3g/L, thiocarbamide 0.3-0.5 g/L, Potassium Iodate 0.2-0.5 g/L.
Advantage of the present invention is: coating can be made after adding this additive to reach the effect of entire bright, and it is fast to go out ray velocity, within general about 3 minutes, starts, in half light, within 10 minutes, just can reach mirror effect.And brightening agent consumption is few, plating solution remains stable state, and binding force of cladding material is good, the excellent corrosion resistance of coating, and with the test of nitric acid spot corrosion method, the time of resistance to nitric acid can reach more than 300 seconds.
The object of the present invention is to provide phosphorus chemistry nickel plating additive formulations in a kind of environment-friendly type height light, and acquisition goes out ray velocity faster, and coating has good bright in mirror surface effect, bonding force is good, excellent corrosion resistance.
Embodiment
Phosphorus chemistry nickel plating additive in a kind of environment-friendly type height light, it is made up of A and B two kinds of components, component A comprises the raw material of following concentration: the mixture of 2-5mg/L Nanometer Copper and soluble copper salt, the sulfuric acid rhenium of 2-4mg/L, 1-4mg/L sodium allyl sulfonate (ALS), complexing agent, stablizer, the NaOH of 20-40g/L; B component comprises the raw material of following concentration: the butynediol diethoxy ether (BEO) of 1-4mg/L, the N of 1-3mg/L, N-diethyl propargylamine (DEP), the BBI (BBI) of 1-4mg/L, the sodium hydroxymethane sulfonate (PN) of 2-4mg/L.
When preparing above-mentioned additive, Nanometer Copper, soluble copper salt, sulfuric acid rhenium, sodium allyl sulfonate (ALS), complexing agent, stablizer, NaOH are mixed together in water and form additive A, and butynediol diethoxy ether (BEO), N, N-diethyl propargylamine (DEP), BBI (BBI), sodium hydroxymethane sulfonate (PN) is mixed together in water and forms additive B, the method of additive application in chemical nickel-plating solution is: in each plating cycle, adds additive A and the B of 0.5-10mL in often liter of plating solution respectively.
The working temperature of chemical nickel-plating solution is 88-92 DEG C.
The pH scope of chemical nickel-plating solution is 4. 5-4. 9.
The plating loading capacity of chemical nickel-plating solution is 0. 5-2. 5 dm
2/ L.
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment 1.
Formula and operational condition as follows: single nickel salt 20g/L, inferior sodium phosphate 25g/L, crystallization sodium acetate 12g/L, lactic acid l0ml/L, copper sulfate 1 mg/L, additive 8ml/L (additive A 4ml/L, additive B 4ml/L), the pH value of plating solution is 4.5, and loading capacity is 1dm
2/ L, plating temperature is 88-92 DEG C, and plating time is 10 minutes.
Preparation plating solution: measured by the volume integral another name of the various medicines of above-mentioned calculated amount by plating solution, then with deionized water, solid medicine is dissolved completely, thick liquid chemicals dilating becomes dilute solution.First by single nickel salt and sodium acetate, lactic acid mixed dissolution, then will mix with the ortho phosphorous acid sodium solution dissolved, the amount of red-tape operati water, about 3/4 of configuration liquor capacity, can not exceed prescribed volume.Finally be diluted to prescribed volume with after 1:l ammoniacal liquor adjusted to ph to 4.5.
Test piece treatment before plating: electrochemical deoiling one flowing water cleaning one activation (1:1 hydrochloric acid) flowing water cleaning.
Plating: the plating solution prepared is put into thermostat water bath and is heated to 88 DEG C, measure the additive solution prepared with graduated cylinder, add in plating solution successively, adjusted to ph, again mark is carried out in iron-based test piece good for pre-treatment, entreat suspension in the plating solution, the reaction times is 10 minutes.
Performance test: when being 3 minutes when reacted, takes out test piece, and find test piece in half bright state, take out after 10 minutes, test piece coating almost can reach mirror effect, and brightness is excellent; Measure its erosion resistance with the salpeter solution prepared, the coating blackening time was more than 300 seconds; 180 degree of alternating bending test pieces five times, coating surface does not have peeling, decortication phenomenon.
Embodiment 2.
Formula and operational condition as follows: single nickel salt 22g/L, inferior sodium phosphate 28g/L, crystallization sodium acetate 15g/L, lactic acid 8ml/L, copper sulfate 1 mg/L, additive 8ml/L (additive A 2ml/L, additive B 6ml/L), the pH value of plating solution is 4.7, and loading capacity is 1.5 dm
2/ L, plating temperature is 88-92 DEG C, and plating time is 10 minutes.
The preparation of plating solution: measured by the volume integral another name of the various medicines of above-mentioned calculated amount by plating solution, then with deionized water, solid medicine is dissolved completely, thick liquid chemicals dilating becomes dilute solution.First by single nickel salt and sodium acetate, lactic acid mixed dissolution, then will mix with the ortho phosphorous acid sodium solution dissolved, the amount of red-tape operati water, about 3/4 of configuration liquor capacity, can not exceed prescribed volume.Finally be diluted to prescribed volume with after 1:l ammoniacal liquor adjusted to ph to 4.7.
Test piece treatment before plating: electrochemical deoiling one flowing water cleaning one activation (1:1 hydrochloric acid) flowing water cleaning.
Plating: the plating solution prepared is put into thermostat water bath and is heated to 88 DEG C, measure the additive solution prepared with graduated cylinder, add in plating solution successively.Adjusted to ph, then mark is carried out in iron-based test piece good for pre-treatment, entreat suspension in the plating solution, the reaction times is 10 minutes.
Performance test: when being 3 minutes when reacted, takes out test piece, and find test piece in half bright state, take out after 10 minutes, test piece coating almost can reach mirror effect, and brightness is excellent; Measure its erosion resistance with the salpeter solution prepared, the coating blackening time, 180 degree of alternating bending test pieces five times, coating surface did not have peeling, decortication phenomenon more than 300 seconds.
Embodiment 3.
Formula and operational condition as follows: single nickel salt 25g/L, inferior sodium phosphate 30g/L, crystallization sodium acetate 10g/L, lactic acid 5ml/L, copper sulfate 1 mg/L, additive 8ml/L (additive A 6ml/L, additive B 2ml/L), the pH value of plating solution is 4.9, and loading capacity is 2 dm
2/ L, plating temperature is 88-92 DEG C, and plating time is 10 minutes.
The preparation of plating solution: measured by the volume integral another name of the various medicines of above-mentioned calculated amount by plating solution, then with deionized water, solid medicine is dissolved completely, thick liquid chemicals dilating becomes dilute solution.First by single nickel salt and sodium acetate, lactic acid mixed dissolution, then will mix with the ortho phosphorous acid sodium solution dissolved, the amount of red-tape operati water, about 3/4 of configuration liquor capacity, can not exceed prescribed volume.Finally be diluted to prescribed volume with after 1:l ammoniacal liquor adjusted to ph to 4.9.
Test piece treatment before plating: electrochemical deoiling one flowing water cleaning one activation (1:1 hydrochloric acid) flowing water cleaning.
Plating: the plating solution prepared is put into thermostat water bath and is heated to 88 DEG C, measure the additive solution prepared with graduated cylinder, add in plating solution successively.Adjusted to ph, then mark is carried out in iron-based test piece good for pre-treatment, entreat suspension in the plating solution, the reaction times is 10 minutes.
Performance test: when being 3 minutes when reacted, takes out test piece, and find test piece in half bright state, take out after 10 minutes, test piece coating almost can reach mirror effect, and brightness is excellent; Measure its erosion resistance with the salpeter solution prepared, the coating blackening time was more than 300 seconds; 180 degree of alternating bending test pieces five times, coating surface does not have peeling, decortication phenomenon.
Claims (1)
1. phosphorus chemistry nickel plating additive in an environment-friendly type height light, it is characterized in that: it is made up of A and B two kinds of components, component A comprises the raw material of following concentration: the mixture of the nanometer copper and copper sulfate of 2-5mg/L, wherein the mass percent of copper sulfate is 50%-57%, the sulfuric acid rhenium of 2-4mg/L, the sodium allyl sulfonate (ALS) of 1-4mg/L, the NaOH of 20-40g/L, complexing agent, the water of stablizer and surplus, described complexing agent is citric acid, lactic acid, propionic acid, DL-oxysuccinic acid, the mixture of succinic acid, in complexing agent, the content of each composition is: citric acid 2.5-8g/L, lactic acid 12-70g/L, propionic acid 5-40 g/L, DL-oxysuccinic acid 2-10g/L, succinic acid 2-8g/L, described stablizer is tellurium dioxide, bismuth citrate, thiocarbamide, the mixture of Potassium Iodate, in stablizer, the content of each composition is: tellurium dioxide 0.001-0.0017g/L, bismuth citrate 0.1-0.3g/L, thiocarbamide 0.3-0.5g/L, Potassium Iodate 0.2-0.5g/L, B component comprises the raw material of following concentration: the butynediol diethoxy ether (BEO) of 1-4mg/L, the N of 1-3mg/L, N-diethyl propargylamine (DEP), the BBI (BBI) of 1-4mg/L, the sodium hydroxymethane sulfonate (PN) of 2-4mg/L and the water of surplus.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104561948A (en) * | 2015-01-28 | 2015-04-29 | 哈尔滨三泳金属表面技术有限公司 | Additive for quick chemical nickel-phosphorus plating of environment-friendly aluminum alloy |
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| CN105039940B (en) * | 2015-07-13 | 2017-12-01 | 宁波市鄞州双诺机械有限公司 | A kind of nickel plating process of bearing cap |
| CN108251825A (en) * | 2018-04-12 | 2018-07-06 | 朱玉兰 | It is a kind of to plate the fast iron oxygen magnetic core chemical nickel-plating solution of speed |
| CN108728833A (en) * | 2018-08-24 | 2018-11-02 | 朱玉兰 | A kind of high rigidity chemical nickel-plating solution and its chemical plating process for aluminium alloy |
| CN109609936B (en) * | 2018-12-26 | 2022-01-04 | 江南大学 | Self-catalytic alloy coating |
| CN113802114B (en) * | 2021-09-16 | 2024-02-02 | 深圳市大正瑞地科技有限公司 | Lead-free environment-friendly chemical nickel solution and chemical nickel plating process using same |
| CN114411129A (en) * | 2021-12-29 | 2022-04-29 | 广东利尔化学有限公司 | Environment-friendly high-phosphorus nickel plating additive |
| CN115418631A (en) * | 2022-09-05 | 2022-12-02 | 吉安宏达秋科技有限公司 | Environment-friendly bright medium-phosphorus chemical nickel plating solution and application thereof |
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|---|---|---|---|---|
| US4467067A (en) * | 1982-12-27 | 1984-08-21 | Shipley Company | Electroless nickel plating |
| CN101638778A (en) * | 2009-02-27 | 2010-02-03 | 郑建国 | Nickel-phosphorus chemical precipitation plating layer of aluminium alloy |
| CN102140631A (en) * | 2011-04-01 | 2011-08-03 | 广州市二轻工业科学技术研究所 | Environment-friendly high-phosphorus chemical nickel additive |
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2014
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|---|---|---|---|---|
| US4467067A (en) * | 1982-12-27 | 1984-08-21 | Shipley Company | Electroless nickel plating |
| CN101638778A (en) * | 2009-02-27 | 2010-02-03 | 郑建国 | Nickel-phosphorus chemical precipitation plating layer of aluminium alloy |
| CN102140631A (en) * | 2011-04-01 | 2011-08-03 | 广州市二轻工业科学技术研究所 | Environment-friendly high-phosphorus chemical nickel additive |
Non-Patent Citations (1)
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Cited By (1)
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|---|---|---|---|---|
| CN104561948A (en) * | 2015-01-28 | 2015-04-29 | 哈尔滨三泳金属表面技术有限公司 | Additive for quick chemical nickel-phosphorus plating of environment-friendly aluminum alloy |
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