CN109023450B - Sulfosalicylic acid silver plating additive, preparation method thereof and electroplating solution containing sulfosalicylic acid silver plating additive - Google Patents
Sulfosalicylic acid silver plating additive, preparation method thereof and electroplating solution containing sulfosalicylic acid silver plating additive Download PDFInfo
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- CN109023450B CN109023450B CN201811132651.0A CN201811132651A CN109023450B CN 109023450 B CN109023450 B CN 109023450B CN 201811132651 A CN201811132651 A CN 201811132651A CN 109023450 B CN109023450 B CN 109023450B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/46—Electroplating: Baths therefor from solutions of silver
Abstract
The invention discloses a sulfosalicylic acid silver plating additive, a preparation method thereof and electroplating liquid containing the sulfosalicylic acid silver plating additive, wherein the sulfosalicylic acid silver plating additive comprises 10-15g/L of polyethylene glycol, 30-50g/L of paranitroaniline, 8-10g/L of azodiisobutyronitrile, 8-12g/L, EDTA (ethylene diamine tetraacetic acid) 200-400g/L of n-propylbenzene, 100-200g/L of sodium dimercaptopropane sulfonate and the balance of water. The silver plating additive provided by the invention has the advantages that the dispersibility, stability, electroplating property and the like of the electroplating solution are remarkably improved, the pH value does not need to be repeatedly adjusted in the electroplating process, the performances of smoothness, adhesion, glossiness, discoloration resistance and the like of a silver plating layer are remarkably improved, the thickness of the plating layer is reduced, and the phenomena of cracking and the like are avoided; the electroplating solution does not contain cyanide, and the plating layer has bright mirror surface, small brittleness, good adhesive force, smooth surface, brightness, good color change resistance and strong heat resistance, can meet the application in various fields of decorative electroplating, functional electroplating and the like, can be directly used for workpieces such as brass, copper, chemical nickel and the like, does not need pre-plating, and can ensure the binding force.
Description
Technical Field
The invention relates to a sulfosalicylic acid silver plating additive, a preparation method thereof and an electroplating solution containing the sulfosalicylic acid silver plating additive, belonging to the field of silver plating.
Background
Silver has unique silvery luster, excellent conductivity and solderability, stable chemical properties to organic acids and alkalis, and lower price than other noble metals, and the silver coating is widely applied to the fields of tableware, jewelry, artworks, electric contact materials in the electrical and electronic industries and the like.
So far, most of the electroplating silver processes at home and abroad adopt cyanogen series silver plating, because the cyanogen series silver plating process has good plating solution stability, better uniform plating capability and depth capability and fine plating layer crystallization. However, cyanide is a highly toxic substance, has great harm to the health of field operators, requires good ventilation equipment during production, and simultaneously discharges sewage which is not beneficial to environmental protection.
With the development of industry, environmental pollution is more and more serious, environmental protection awareness of countries in the world is continuously strengthened and relevant policies are issued, the cyanogen silver plating is gradually eliminated, however, the existing cyanogen-free silver plating has the defects of dull luster, uneven silver plating layer, poor color change resistance, thick plating layer, poor adhesion, easy cracking and the like.
Disclosure of Invention
In order to solve the above problems in the prior art, the present invention provides a sulfosalicylic acid silver plating additive, a preparation method thereof and an electroplating solution containing the same.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a silver plating additive for sulfosalicylic acid comprises 10-15g/L of polyethylene glycol, 30-50g/L of paranitroaniline, 8-10g/L of azodiisobutyronitrile, 8-12g/L, EDTA (ethylene diamine tetraacetic acid) 200-400g/L of n-propylbenzene, 100-200g/L of sodium dimercaptopropane sulfonate and the balance of water.
The applicant finds that the additive is added into the silver plating solution, so that the dispersibility, the stability, the electroplating property and the like of the plating solution are remarkably improved, the pH value does not need to be repeatedly adjusted in the electroplating process, the performances of smoothness, adhesion, glossiness, discoloration resistance and the like of a silver plating layer are remarkably improved, the thickness of the plating layer is reduced, and the phenomena of cracking and the like are avoided.
The above additive is particularly suitable for silver plating of sulfosalicylic acid.
In order to further improve the stability and electroplating effect of the electroplating solution, the sulfosalicylic acid silver plating additive also comprises 1-3g/L of alcohol ether phosphate, 3-5g/L of triethylamine, 3-5g/L of diphenylmethane and 50-100g/L of thioglycolic acid.
In order to further improve the stability of the electroplating solution and the adhesion of the plating layer, the sulfosalicylic acid silver plating additive preferably further comprises 3-5g/L of polyoxyethylene amide, 1-3g/L of ethylene imine, 0.5-0.8g/L of naphthalene and 30-60g/L of triethanolamine.
In order to further improve the color degree of the coating, preferably, the sulfosalicylic acid silver plating additive also comprises 1-3g/L of high-carbon fatty alcohol polyoxyethylene ether, 0.1-0.4g/L of pyrrolidine, 0.1-0.3g/L of anthracene, 10-20g/L of ammonium fluoride and 20-50g/L of potassium chromate.
In order to further improve the discoloration resistance of the plating layer, the sulfosalicylic acid silver plating additive preferably further comprises 0.5-1g/L of alkylphenol polyoxyethylene, 10-20g/L of acetylacetone and 20-30g/L of tartaric acid.
In order to further improve the glossiness and the flatness of the plating layer, the sulfosalicylic acid silver plating additive preferably further comprises 10-20g/L of ethylenediamine tetrapropionic acid.
The applicant finds that the effect of the paranitroaniline, the azodiisobutyronitrile, the triethylamine, the ethylene imine, the pyrrolidine and the like on improving the glossiness of the coating is very obvious; n-propylbenzene, diphenylmethane, naphthalene, anthracene and the like have very obvious effects on improving the flatness of the plating; EDTA (ethylene diamine tetraacetic acid), sodium dimercaptopropane sulfonate, thioglycolic acid, ammonium fluoride, potassium chromate, acetylacetone, tartaric acid, triethanolamine, ethylene diamine tetrapropionic acid and the like are beneficial to improving the stability of the electroplating solution and reducing the dosage of the electroplating solution; polyethylene glycol, alcohol ether phosphate, polyoxyethylene amide, high-carbon fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether and the like are beneficial to improving the stability of the electroplating solution and the anti-color change performance of the coating; the applicant finds that the substances have obvious synergistic promotion effect, so that the comprehensive properties of the coating such as color, smoothness, discoloration resistance and adhesive force are obviously improved, the thickness of the coating can be obviously reduced, and the electroplating cost is reduced.
The preparation method of the sulfosalicylic acid silver plating additive comprises the following steps:
1) heating water to 80-90 ℃, adding polyethylene glycol under the stirring of 1000-;
2) sequentially adding EDTA (ethylene diamine tetraacetic acid) and sodium dimercaptopropane sulfonate into the material obtained in the step 1), and then stirring for 10-20min at 80-90 ℃ and 1000-1200 r/min;
3) sequentially adding p-nitroaniline, azodiisobutyronitrile and n-propylbenzene into the material obtained in the step 2), and then stirring for 30-40min at 80-90 ℃ and 1000-1200r/min to obtain the sulfosalicylic acid silver plating additive.
The control of the adding sequence and the conditions of the materials in the preparation method of the additive is very critical, otherwise, the stability of the additive, the stability of the electroplating solution and the performance of the plating layer are obviously deteriorated.
In order to further improve the comprehensive performance of the plating layer, the preparation method of the sulfosalicylic acid silver plating additive comprises the following steps:
1) heating water to 80-90 ℃, sequentially adding polyethylene glycol, alcohol ether phosphate, polyoxyethylene amide, high-carbon fatty alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether under the stirring of 1000-1200r/min, and continuing stirring for 20-30min at 80-90 ℃ under the stirring of 1000-1200 r/min;
2) sequentially adding EDTA (ethylene diamine tetraacetic acid), sodium dimercaptopropane sulfonate, thioglycolic acid, triethanolamine, ammonium fluoride, potassium chromate, acetylacetone, tartaric acid and ethylene diamine tetrapropionic acid into the material obtained in the step 1), and stirring at 80-90 ℃ and 1000-1200r/min for 10-20 min;
3) sequentially adding p-nitroaniline, azodiisobutyronitrile, triethylamine, ethylene imine, pyrrolidine, n-propylbenzene, diphenylmethane, naphthalene and anthracene into the material obtained in the step 2), and then stirring for 30-40min at 80-90 ℃ and 1200r/min of 1000-materials to obtain the silver plating additive of sulfosalicylic acid.
The sulfosalicylic acid silver plating electroplating solution containing the sulfosalicylic acid silver plating additive comprises 200-300mL/L of the sulfosalicylic acid silver plating additive, 200-200 g/L of sulfosalicylic acid, 50-80g/L of silver nitrate, 20-30g/L of ammonium propionate, 15-20g/L of sodium hydroxide and the balance of water.
The preparation method of the sulfosalicylic acid silver plating solution comprises the following steps:
1) dissolving sulfosalicylic acid in water to obtain a solution I;
2) dissolving sodium hydroxide in water, and adding the solution into the solution I to obtain a solution II;
3) dissolving silver nitrate in water, and adding the solution into the solution II to obtain a solution III;
4) dissolving ammonium propionate in water, and adding the solution into the solution III to obtain a solution IV;
5) and adding the sulfosalicylic acid silver plating additive into the solution IV, adding water to a required amount, and then adjusting the pH value to 9 to obtain the sulfosalicylic acid silver plating electroplating solution.
The prior art is referred to in the art for techniques not mentioned in the present invention.
The sulfosalicylic acid silver plating additive disclosed by the invention has the advantages that the dispersibility, stability, electroplating property and the like of electroplating solution are remarkably improved, the pH value does not need to be repeatedly adjusted in the electroplating process, the performances of smoothness, adhesion, glossiness, discoloration resistance and the like of a silver plating layer are remarkably improved, the thickness of the plating layer is reduced, and the phenomena of cracking and the like are avoided; the electroplating solution does not contain cyanide, and the plating layer has bright mirror surface, small brittleness, good adhesive force, smooth surface, brightness, good color change resistance and strong heat resistance, can meet the application in various fields of decorative electroplating, functional electroplating and the like, can be directly used for workpieces such as brass, copper, chemical nickel and the like, does not need pre-plating, and can ensure the binding force.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
TABLE 1 Sulfosalicylic acid silver plating additive composition Table
In the above table, polyethylene glycol is polyethylene glycol 10000, alcohol ether phosphate is fatty alcohol ether phosphate potassium salt, the model is AEPK-350, polyoxyethylene amide is Antarox G-200 polyoxyethylene fatty amide, high-carbon fatty alcohol polyoxyethylene ether is purchased from Rong Dainiji chemical industry Co., Ltd, and alkylphenol polyoxyethylene ether is OP-10.
The preparation method of the sulfosalicylic acid silver plating additive comprises the following steps:
1) heating water to 80-90 deg.C, sequentially adding polyethylene glycol, alcohol ether phosphate, polyoxyethylene amide, high-carbon fatty alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether under stirring at 1100r/min, and stirring at 80-90 deg.C and 1100r/min for 25 min;
2) adding ethylene diamine tetraacetic acid, sodium dimercaptopropane sulfonate, thioglycolic acid, triethanolamine, ammonium fluoride, potassium chromate, acetylacetone, tartaric acid and ethylene diamine tetrapropionic acid into the material obtained in the step 1) in sequence, and stirring at 80-90 ℃ and 1100r/min for 15 min;
3) sequentially adding p-nitroaniline, azodiisobutyronitrile, triethylamine, ethylene imine, pyrrolidine, n-propylbenzene, diphenylmethane, naphthalene and anthracene into the material obtained in the step 2), and stirring at 80-90 ℃ and 1100r/min for 35min to obtain the sulfosalicylic acid silver plating additive.
Comparative example 3
Essentially the same as in example 6, except that: when the silver-plating additive is prepared, water is heated to 80-90 ℃, polyethylene glycol, alcohol ether phosphate, polyoxyethylene amide, high-carbon fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, ethylene diamine tetraacetic acid, sodium dimercaptopropane sulfonate, thioglycolic acid, triethanolamine, ammonium fluoride, potassium chromate, acetylacetone, tartaric acid, ethylene diamine tetrapropionic acid, paranitroaniline, azodiisobutyronitrile, triethylamine, ethyleneimine, pyrrolidine, n-propylbenzene, diphenylmethane, naphthalene and anthracene are sequentially added under the stirring of 1100r/min, and then the silver-plating additive of sulfosalicylic acid is obtained after stirring for 75min at 80-90 ℃ and 1100 r/min.
Comparative example 4
Essentially the same as in example 6, except that: during preparation, polyethylene glycol, alcohol ether phosphate, polyoxyethylene amide, high-carbon fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene, ethylene diamine tetraacetic acid, sodium dimercaptopropane sulfonate, thioglycolic acid, triethanolamine, ammonium fluoride, potassium chromate, acetylacetone, tartaric acid, ethylene diamine tetrapropionic acid, paranitroaniline, azodiisobutyronitrile, triethylamine, ethyleneimine, pyrrolidine, n-propylbenzene, diphenylmethane, naphthalene and anthracene are added into water at room temperature (about 25 ℃) under the stirring of 1100r/min in sequence, and then the sulfosalicylic acid silver-plating additive is obtained after stirring for 75min at 1100 r/min.
Preparing an electroplating solution:
the additives obtained in examples 1 to 6 and comparative examples 1 to 4 were prepared as plating solutions according to the following formulations: 250mL/L of sulfosalicylic acid silver plating additive, 180g/L of sulfosalicylic acid, 60g/L of silver nitrate, 25g/L of ammonium propionate, 18g/L of sodium hydroxide and the balance of water;
the preparation method of the electroplating solution comprises the following steps: the method comprises the following steps:
1) dissolving sulfosalicylic acid in water to obtain a solution I;
2) dissolving sodium hydroxide in water, and adding the solution into the solution I to obtain a solution II;
3) dissolving silver nitrate in water, and adding the solution into the solution II to obtain a solution III;
4) dissolving ammonium propionate in water, and adding the solution into the solution III to obtain a solution IV;
5) and adding the sulfosalicylic acid silver plating additive into the solution IV, adding water to a required amount, and then adjusting the pH value to 9 to obtain the sulfosalicylic acid silver plating electroplating solution.
Comparative example 5
Essentially the same as in example 6, except that: in the electroplating solution, sulfosalicylic acid is 120g/L, silver nitrate is 40g/L, ammonium propionate is 15g/L, and sodium hydroxide is 10 g/L.
Comparative example 6
Essentially the same as in example 6, except that: in the electroplating solution, sulfosalicylic acid is 220g/L, silver nitrate is 100g/L, ammonium propionate is 35g/L, and sodium hydroxide is 25 g/L.
Comparative example 7
Essentially the same as in example 6, except that: in the preparation of the plating solution, the pH is adjusted to 10 in step 5).
Preparing a silver plating layer:
using the plating liquids obtained in examples 1 to 6 and comparative examples 1 to 7, respectively, silver plating was prepared as test pieces of 5X 5cm degreased and polished2The specific method of the pure copper sheet comprises the following steps: in the course of electroplatingThe plating solution is maintained at 28 ℃, and then the test piece is connected into a circuit and immersed into the plating solution, wherein the cathode current density is 0.3A/dm2The plating mode is rack plating, the electroplating time is 15 minutes, and a silver-plated sample is obtained, wherein the thickness of the plating layer is 8-12 mu m.
TABLE 2 Properties of the coatings obtained in the examples
In the above table, adhesion is measured with reference to GB/T9286; the testing method of the flatness is to measure the maximum thickness difference of the surface of the coating by a thickness meter; the impact strength measurement method comprises the steps of using a 64g steel ball to freely fall at a height of 1m, observing whether glass has cracks and damages, and if the glass is intact, passing the glass; visual measurement of gloss; the heat resistance is the phenomena of color change and peeling after being baked for 30 minutes at 200 ℃; visual measurement of color; the normal temperature discoloration resistance test method is the discoloration condition of 6 months at normal temperature; the high temperature discoloration resistance was 2min at 300 ℃.
Claims (9)
1. The sulfosalicylic acid silver plating additive is characterized in that: comprises 10-15g/L of polyethylene glycol, 30-50g/L of p-nitroaniline, 8-10g/L of azodiisobutyronitrile, 8-12g/L of n-propylbenzene, 400g/L of ethylenediamine tetraacetic acid, 200g/L of sodium dimercaptopropane sulfonate, 1-3g/L of alcohol ether phosphate, 3-5g/L of triethylamine, 3-5g/L of diphenylmethane, 50-100g/L of thioglycolic acid and the balance of water.
2. The sulfosalicylic acid silver plating additive of claim 1 wherein: also comprises 3-5g/L of polyoxyethylene amide, 1-3g/L of ethylene imine, 0.5-0.8g/L of naphthalene and 30-60g/L of triethanolamine.
3. The sulfosalicylic acid silver plating additive of claim 1 or 2 wherein: also comprises 1-3g/L of high-carbon fatty alcohol polyoxyethylene ether, 0.1-0.4g/L of pyrrolidine, 0.1-0.3g/L of anthracene, 10-20g/L of ammonium fluoride and 20-50g/L of potassium chromate.
4. The sulfosalicylic acid silver plating additive of claim 1 or 2 wherein: also comprises 0.5-1g/L of alkylphenol polyoxyethylene, 10-20g/L of acetylacetone and 20-30g/L of tartaric acid.
5. The sulfosalicylic acid silver plating additive of claim 1 or 2 wherein: also comprises 10-20g/L of ethylenediamine tetrapropionic acid.
6. A process for preparing a silver-plating additive of sulfosalicylic acid according to any one of claims 1-5, wherein: the method comprises the following steps:
1) heating water to 80-90 ℃, adding polyethylene glycol and alcohol ether phosphate under the stirring of 1000-1200r/min, and continuing stirring for 20-30min at 80-90 ℃ under the stirring of 1000-1200 r/min;
2) adding ethylene diamine tetraacetic acid, sodium dimercaptopropane sulfonate and thioglycolic acid into the material obtained in the step 1) in sequence, and then stirring for 10-20min at 80-90 ℃ and 1000-;
3) sequentially adding p-nitroaniline, azodiisobutyronitrile, n-propylbenzene, triethylamine and diphenylmethane into the material obtained in the step 2), and then stirring for 30-40min at 80-90 ℃ and 1200r/min to obtain the silver plating additive of sulfosalicylic acid.
7. The method of claim 6, wherein: the method comprises the following steps:
1) heating water to 80-90 ℃, sequentially adding polyethylene glycol, alcohol ether phosphate, polyoxyethylene amide, high-carbon fatty alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether under the stirring of 1000-1200r/min, and continuing stirring for 20-30min at 80-90 ℃ under the stirring of 1000-1200 r/min;
2) adding ethylene diamine tetraacetic acid, sodium dimercaptopropane sulfonate, thioglycolic acid, triethanolamine, ammonium fluoride, potassium chromate, acetylacetone, tartaric acid and ethylene diamine tetrapropionic acid into the material obtained in the step 1) in sequence, and stirring for 10-20min at 80-90 ℃ and 1200 r/min;
3) sequentially adding p-nitroaniline, azodiisobutyronitrile, triethylamine, ethylene imine, pyrrolidine, n-propylbenzene, diphenylmethane, naphthalene and anthracene into the material obtained in the step 2), and then stirring for 30-40min at 80-90 ℃ and 1200r/min of 1000-materials to obtain the silver plating additive of sulfosalicylic acid.
8. A sulfosalicylic acid silver plating bath comprising the sulfosalicylic acid silver plating additive of any one of claims 1-5, wherein: comprises 300mL/L of sulfosalicylic acid silver plating additive, 200g/L of sulfosalicylic acid, 50-80g/L of silver nitrate, 20-30g/L of ammonium propionate, 15-20g/L of sodium hydroxide and the balance of water.
9. The process for preparing a sulfosalicylic acid silver plating bath as set forth in claim 8, wherein: the method comprises the following steps:
1) dissolving sulfosalicylic acid in water to obtain a solution I;
2) dissolving sodium hydroxide in water, and adding the solution into the solution I to obtain a solution II;
3) dissolving silver nitrate in water, and adding the solution into the solution II to obtain a solution III;
4) dissolving ammonium propionate in water, and adding the solution into the solution III to obtain a solution IV;
5) and adding the sulfosalicylic acid silver plating additive into the solution IV, adding water to a required amount, and then adjusting the pH value to 9 to obtain the sulfosalicylic acid silver plating electroplating solution.
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| CN102560571A (en) * | 2012-02-22 | 2012-07-11 | 江苏大学 | Cyanide-free silver plating stable electroplating solution and preparation method thereof, and silver plating method |
| CN104480500A (en) * | 2014-12-26 | 2015-04-01 | 贵州振华群英电器有限公司（国营第八九一厂） | Cyanide-free electroplating solution for silver plating of copper or copper alloy, preparation method and silver plating process |
| CN104611737A (en) * | 2013-11-05 | 2015-05-13 | 无锡市雪江环境工程设备有限公司 | Imidazole-sulfosalicylic acid silver plating solution and electroplating method |
| CN106283134A (en) * | 2016-09-09 | 2017-01-04 | 国家电网公司 | A kind of rare earth improves Brush Plating silver plating liquid and preparation technology thereof and using method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560571A (en) * | 2012-02-22 | 2012-07-11 | 江苏大学 | Cyanide-free silver plating stable electroplating solution and preparation method thereof, and silver plating method |
| CN104611737A (en) * | 2013-11-05 | 2015-05-13 | 无锡市雪江环境工程设备有限公司 | Imidazole-sulfosalicylic acid silver plating solution and electroplating method |
| CN104480500A (en) * | 2014-12-26 | 2015-04-01 | 贵州振华群英电器有限公司（国营第八九一厂） | Cyanide-free electroplating solution for silver plating of copper or copper alloy, preparation method and silver plating process |
| CN106283134A (en) * | 2016-09-09 | 2017-01-04 | 国家电网公司 | A kind of rare earth improves Brush Plating silver plating liquid and preparation technology thereof and using method |
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