CN109023450A - A kind of sulfosalicylic acid plating silver additive, preparation method and the electroplate liquid comprising it - Google Patents
A kind of sulfosalicylic acid plating silver additive, preparation method and the electroplate liquid comprising it Download PDFInfo
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract
The invention discloses a kind of sulfosalicylic acid plating silver additive, preparation method and include its electroplate liquid, sulfosalicylic acid plates silver additive, the water including polyethylene glycol 10-15g/L, paranitroanilinum 30-50g/L, azodiisobutyronitrile 8-10g/L, n-proplbenzene 8-12g/L, EDTA (ethylenediamine tetra-acetic acid) 200-400g/L, Sodium Dimercapto Sulfonate 100-200g/L and surplus.The present invention plates silver additive, so that the dispersibility of electroplate liquid, stability, plating resistance etc. have the promotion of highly significant, without going adjustment pH value repeatedly in the plating process, the performances such as the planarization, adhesive force, glossiness anti-discoloration of silvering are significantly improved simultaneously, also it is thinned the thickness of coating, and phenomena such as no cracking；Electroplate liquid of the present invention is free of cyanide, coating bright in mirror surface, brittleness are small, adhesive force is good, surfacing, light, anti-discoloration is good, heat resistance is strong, the multi-field application such as decorative electroplating and functional plating can be met, it can be directly used for the workpiece such as brass, copper, chemical nickel, without preplating, binding force can also be guaranteed.
Description
Technical field
The present invention relates to a kind of sulfosalicylic acid plating silver additive, preparation method and comprising its electroplate liquid, belong to plating
Silver-colored field.
Background technique
Silver has unique silvery white gloss, with excellent electric conductivity and soldering property, chemically to organic bronsted lowry acids and bases bronsted lowry
Matter is more stable, and price is relatively inexpensive compared to other noble metals, and silvering is widely used in tableware, jewellery, the art work, electrical
With the fields such as contact material in electronics industry.
So far, plating silver process both domestic and external is most or silver-plated using cyanogen system, and reason is cyanogen system silver plating process
Bath stability is good, and covering power and depth capability are preferable, and coating crystallization is careful.But cyanide is extremely toxic substance, to scene
The Health cost of operator is big, requires have good ventilation equipment when production, while the sewage discharged is also unfavorable for environment
Protection.
With the development of industry, environmental pollution is increasingly severe, countries in the world environmental protection consciousness also constantly reinforce and
The appearance of relevant policies, cyanogen system is silver-plated to be gradually eliminated, however there are dull, silver coating are uneven for existing non-cyanide silver coating
It is whole, anti-discoloration is poor, thickness of coating is thick, poor adhesive force, the defects of being easily cracked.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provide a kind of sulfosalicylic acid plating silver additive,
Preparation method and electroplate liquid comprising it.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows:
A kind of sulfosalicylic acid plating silver additive, including polyethylene glycol 10-15g/L, paranitroanilinum 30-50g/L, azo
Bis-isobutyronitrile 8-10g/L, n-proplbenzene 8-12g/L, EDTA (ethylenediamine tetra-acetic acid) 200-400g/L, Sodium Dimercapto Sulfonate
The water of 100-200g/L and surplus.
Applicant it has been investigated that, by above-mentioned additive addition in plate silver plating solution so that electroplate liquid is dispersed, steady
The promotion for having highly significant such as qualitative, plating resistance significantly improves simultaneously without going adjustment pH value repeatedly in the plating process
The performances such as planarization, adhesive force, the glossiness anti-discoloration of silvering are also thinned the thickness of coating, and phenomena such as no cracking.
It is silver-plated that above-mentioned additive is particularly suitable for sulfosalicylic acid.
In order to further increase the stability and electroplating effect of electroplate liquid, above-mentioned sulfosalicylic acid plates silver additive, also wraps
Include alcohol ether phosphate 1-3g/L, triethylamine 3-5g/L, diphenyl-methane 3-5g/L and thioacetic acid 50-100g/L.
In order to further increase the stability of electroplate liquid and the adhesive force of coating, it is preferable that above-mentioned sulfosalicylic acid is silver-plated to be added
Add agent, further includes polyoxyethylate amide 3-5g/L, aziridine 1-3g/L, naphthalene 0.5-0.8g/L and triethanolamine 30-60g/L.
In order to further increase the color of coating, it is preferable that above-mentioned sulfosalicylic acid plates silver additive, further includes high-carbon rouge
Fat alcohol polyoxyethylene ether 1-3g/L, pyrrolidines 0.1-0.4g/L, anthracene 0.1-0.3g/L, ammonium fluoride 10-20g/L and potassium chromate 20-
50g/L。
In order to further increase the discoloration-resisting of coating, it is preferable that above-mentioned sulfosalicylic acid plates silver additive, further includes alkane
Base phenol polyethenoxy ether 0.5-1g/L, acetylacetone,2,4-pentanedione 10-20g/L and tartaric acid 20-30g/L.
In order to further increase the glossiness and planarization of coating, it is preferable that sulfosalicylic acid plates silver additive, further includes second
Four propionic acid 10-20g/L of diamines.
Applicant it has been investigated that, above-mentioned paranitroanilinum, azodiisobutyronitrile, triethylamine, aziridine, pyrrolidines etc.
Effect in terms of promoting coating glossiness is clearly；N-proplbenzene, diphenyl-methane, naphthalene, anthracene etc. are improving coating planarization side
The effect in face is clearly；EDTA (ethylenediamine tetra-acetic acid), Sodium Dimercapto Sulfonate, thioacetic acid, ammonium fluoride, potassium chromate,
Acetylacetone,2,4-pentanedione, tartaric acid, triethanolamine, ethylenediamine tetrapropionic acid etc. are conducive to improve the stability of electroplate liquid, reduce plating solution dosage；
Polyethylene glycol, alcohol ether phosphate, polyoxyethylate amide, high-carbon fatty alcohol polyoxyethylene ether and alkyl phenol polyoxyethylene ether etc. are advantageous
In the anti-discoloration performance for the stability and coating for improving electroplate liquid；And applicant has been surprisingly found that, has between above-mentioned each substance bright
Aobvious collaboration promotes effect, and the comprehensive performances such as color, planarization, anti-discoloration, the adhesive force of coating can not only be made to have significantly
It is promoted, and thickness of coating can obviously be thinned, reduce electroplating cost.
The preparation method of above-mentioned sulfosalicylic acid plating silver additive, includes the following steps:
1) 80-90 DEG C is heated the water to, under the stirring of 1000-1200r/min, after polyethylene glycol is added, is continued in 80-
90 DEG C, stir 20-30min under 1000-1200r/min；
2) EDTA (ethylenediamine tetra-acetic acid) and Sodium Dimercapto Sulfonate are sequentially added in the resulting material of step 1), so
10-20min is stirred at 80-90 DEG C, 1000-1200r/min afterwards；
3) paranitroanilinum, azodiisobutyronitrile and n-proplbenzene are sequentially added in the resulting material of step 2), is then existed
80-90 DEG C, stir 30-40min under 1000-1200r/min, obtain sulfosalicylic acid plating silver additive.
The control of the order of addition, condition of material is very crucial in above-mentioned addictive preparation method, otherwise additive
Stability, the stability of electroplate liquid and coating performance can obviously be deteriorated.
In order to further increase the comprehensive performance of coating, above-mentioned sulfosalicylic acid plates the preparation method of silver additive, including
Following steps:
1) 80-90 DEG C is heated the water to, under the stirring of 1000-1200r/min, sequentially adds polyethylene glycol, alcohol ether phosphorus
After hydrochlorate, polyoxyethylate amide, high-carbon fatty alcohol polyoxyethylene ether and alkyl phenol polyoxyethylene ether, continue 80-90 DEG C,
20-30min is stirred under 1000-1200r/min；
2) by EDTA (ethylenediamine tetra-acetic acid), Sodium Dimercapto Sulfonate, thioacetic acid, triethanolamine, ammonium fluoride, chromic acid
Potassium, acetylacetone,2,4-pentanedione, tartaric acid and ethylenediamine tetrapropionic acid sequentially add in the resulting material of step 1), then 80-90 DEG C,
10-20min is stirred under 1000-1200r/min；
3) by paranitroanilinum, azodiisobutyronitrile, triethylamine, aziridine, pyrrolidines, n-proplbenzene, diphenyl-methane, naphthalene
It is sequentially added in the resulting material of step 2) with anthracene, then stirs 30-40min at 80-90 DEG C, 1000-1200r/min, obtain
Sulfosalicylic acid plates silver additive.
Sulfosalicylic acid plate silver plating solution comprising above-mentioned sulfosalicylic acid plating silver additive, including sulfosalicylic acid are silver-plated
Additive 200-300mL/L, sulfosalicylic acid 150-200g/L, silver nitrate 50-80g/L, propionic acid ammonium 20-30g/L, sodium hydroxide
The water of 15-20g/L and surplus.
The preparation method of above-mentioned sulfosalicylic acid plate silver plating solution, includes the following steps:
1) sulfosalicylic acid is dissolved in water, obtains solution one；
2) by sodium hydroxide be dissolved in water after, be added in solution one, obtain solution two；
3) it after silver nitrate being dissolved in water, is added in solution two, obtains solution three；
4) it after propionic acid ammonium being dissolved in water, is added in solution three, obtains solution four；
5) sulfosalicylic acid plating silver additive is added in solution four, adds water to aequum, then adjusts pH to 9,
Up to sulfosalicylic acid plate silver plating solution.
The unmentioned technology of the present invention is referring to the prior art.
Sulfosalicylic acid of the present invention plates silver additive, so that the dispersibility of electroplate liquid, stability, plating resistance etc. have very
It is obviously improved, without going adjustment pH value repeatedly in the plating process, while significantly improving the planarization of silvering, attachment
The performances such as power, glossiness anti-discoloration are also thinned the thickness of coating, and phenomena such as no cracking；Electroplate liquid of the present invention is free of cyanogen
Compound, coating bright in mirror surface, brittleness are small, adhesive force is good, surfacing, light, anti-discoloration is good, heat resistance is strong, can meet dress
The multi-field application such as the plating of decorations property and functional plating, can be directly used for the workpiece such as brass, copper, chemical nickel, be not necessarily to preplating, knot
Resultant force can also be guaranteed.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
The component table of 1 sulfosalicylic acid of table plating silver additive
In upper table, polyethylene glycol is polyethylene glycol 10000, and alcohol ether phosphate is fatty alcohol ether phosphate kalium salt, model
AEPK-350, polyoxyethylate amide are Antarox G-200 Polyoxyethylene fatty acid amides fatty acid ester, and high-carbon fatty alcohol polyoxyethylene ether is purchased from
Rongcheng market day jump Chemical Co., Ltd., alkyl phenol polyoxyethylene ether OP-10.
The preparation method of the sulfosalicylic acid plating silver additive of above-mentioned each example, includes the following steps:
1) heat the water to 80-90 DEG C, under the stirring of 1100r/min, sequentially add polyethylene glycol, alcohol ether phosphate,
After polyoxyethylate amide, high-carbon fatty alcohol polyoxyethylene ether and alkyl phenol polyoxyethylene ether, continue in 80-90 DEG C, 1100r/min
Lower stirring 25min；
2) by ethylenediamine tetra-acetic acid, Sodium Dimercapto Sulfonate, thioacetic acid, triethanolamine, ammonium fluoride, potassium chromate, second
Acyl acetone, tartaric acid and ethylenediamine tetrapropionic acid sequentially add in the resulting material of step 1), then in 80-90 DEG C, 1100r/min
Lower stirring 15min；
3) by paranitroanilinum, azodiisobutyronitrile, triethylamine, aziridine, pyrrolidines, n-proplbenzene, diphenyl-methane, naphthalene
It is sequentially added in the resulting material of step 2) with anthracene, then stirs 35min at 80-90 DEG C, 1100r/min, obtain sulfosalisylic
Acid plating silver additive.
Comparative example 3
It is substantially the same manner as Example 6, except that: in the preparation, 80-90 DEG C is heated the water to, 1100r/min's
Under stirring, it is poly- to sequentially add polyethylene glycol, alcohol ether phosphate, polyoxyethylate amide, high-carbon fatty alcohol polyoxyethylene ether, alkyl phenol
Ethylene oxide ether, ethylenediamine tetra-acetic acid, Sodium Dimercapto Sulfonate, thioacetic acid, triethanolamine, ammonium fluoride, potassium chromate, levulinic
Ketone, tartaric acid, ethylenediamine tetrapropionic acid, paranitroanilinum, azodiisobutyronitrile, triethylamine, aziridine, pyrrolidines, n-proplbenzene,
Then diphenyl-methane, naphthalene and anthracene stir 75min at 80-90 DEG C, 1100r/min, obtain sulfosalicylic acid plating silver additive.
Comparative example 4
It is substantially the same manner as Example 6, except that: in the preparation, at room temperature (25 DEG C or so), 1100r/min's
Under stirring, successively by polyethylene glycol, alcohol ether phosphate, polyoxyethylate amide, high-carbon fatty alcohol polyoxyethylene ether, alkyl phenol polyoxy
Vinethene, ethylenediamine tetra-acetic acid, Sodium Dimercapto Sulfonate, thioacetic acid, triethanolamine, ammonium fluoride, potassium chromate, levulinic
Ketone, tartaric acid, ethylenediamine tetrapropionic acid, paranitroanilinum, azodiisobutyronitrile, triethylamine, aziridine, pyrrolidines, n-proplbenzene,
Diphenyl-methane, naphthalene and anthracene are added to the water, and then stir 75min at 1100r/min, obtain sulfosalicylic acid plating silver additive.
The preparation of electroplate liquid:
By above-described embodiment 1-6 and the resulting additive of comparative example 1-4 according to being prepared as electroplate liquid as following formula: sulfo group water
Poplar acid plates silver additive 250mL/L, sulfosalicylic acid 180g/L, silver nitrate 60g/L, propionic acid ammonium 25g/L, sodium hydroxide 18g/L
With the water of surplus；
Electroplate liquid the preparation method comprises the following steps: including the following steps:
1) sulfosalicylic acid is dissolved in water, obtains solution one；
2) by sodium hydroxide be dissolved in water after, be added in solution one, obtain solution two；
3) it after silver nitrate being dissolved in water, is added in solution two, obtains solution three；
4) it after propionic acid ammonium being dissolved in water, is added in solution three, obtains solution four；
5) sulfosalicylic acid plating silver additive is added in solution four, adds water to aequum, then adjusts pH to 9,
Up to sulfosalicylic acid plate silver plating solution.
Comparative example 5
It is substantially the same manner as Example 6, except that: in electroplate liquid, sulfosalicylic acid 120g/L, silver nitrate 40g/
L, propionic acid ammonium are 15g/L, sodium hydroxide 10g/L.
Comparative example 6
It is substantially the same manner as Example 6, except that: in electroplate liquid, sulfosalicylic acid 220g/L, silver nitrate is
100g/L, propionic acid ammonium are 35g/L, sodium hydroxide 25g/L.
Comparative example 7
It is substantially the same manner as Example 6, except that: in the preparation of electroplate liquid, pH to 10 is adjusted in step 5).
The preparation of silvering:
Embodiment 1-6 and the resulting electroplate liquid of comparative example 1-7 are used respectively, prepares silvering, and test piece is through oil removing and polishing
5 × 5cm2Pure copper sheet, method particularly includes: in the plating process, plating solution is maintained 28 DEG C, then, by test piece access electricity
Road is simultaneously immersed in electroplate liquid, cathode-current density 0.3A/dm2, use plating mode for rack plating, electroplating time is 15 minutes,
Silver-plated sample is obtained, thickness of coating is 8-12 μm.
The performance table of coating obtained by each example of table 2
In upper table, adhesive force is measured referring to GB/T9286；The test method of planarization is to measure coating surface with thickness gauge
Maximum gauge it is poor；Impact strength measurement method is the steel ball with 64g in the height freely falling body of 1m, observes whether glass has
Crackle, breakage, if intactly, passing through；Glossiness visually measures；Heat resistance is to toast 30 minutes discolorations at 200 DEG C and rise
Skin phenomenon；Color visually measures；Room temperature anti-discoloration test method is lower 6 months discoloration situations of room temperature；High temperature anti-discoloration
It is the discoloration situation of 2min at 300 DEG C.
Claims (10)
1. a kind of sulfosalicylic acid plates silver additive, it is characterised in that: including polyethylene glycol 10-15g/L, paranitroanilinum 30-
50g/L, azodiisobutyronitrile 8-10g/L, n-proplbenzene 8-12g/L, ethylenediamine tetra-acetic acid 200-400g/L, dimercaptopropane
The water of sodium 100-200g/L and surplus.
2. sulfosalicylic acid as described in claim 1 plates silver additive, it is characterised in that: further include alcohol ether phosphate 1-3g/
L, triethylamine 3-5g/L, diphenyl-methane 3-5g/L and thioacetic acid 50-100g/L.
3. sulfosalicylic acid as claimed in claim 1 or 2 plates silver additive, it is characterised in that: further include polyoxyethylate amide
3-5g/L, aziridine 1-3g/L, naphthalene 0.5-0.8g/L and triethanolamine 30-60g/L.
4. sulfosalicylic acid as claimed in claim 1 or 2 plates silver additive, it is characterised in that: further include that high-carbon fatty alcohol is poly-
Ethylene oxide ether 1-3g/L, pyrrolidines 0.1-0.4g/L, anthracene 0.1-0.3g/L, ammonium fluoride 10-20g/L and potassium chromate 20-50g/L.
5. sulfosalicylic acid as claimed in claim 1 or 2 plates silver additive, it is characterised in that: further include alkyl phenol polyoxy second
Alkene ether 0.5-1g/L, acetylacetone,2,4-pentanedione 10-20g/L and tartaric acid 20-30g/L.
6. sulfosalicylic acid as claimed in claim 1 or 2 plates silver additive, it is characterised in that: further include ethylenediamine tetrapropionic acid
10-20g/L。
7. the preparation method of sulfosalicylic acid plating silver additive as claimed in any one of claims 1 to 6, it is characterised in that:
Include the following steps:
1) 80-90 DEG C is heated the water to, under the stirring of 1000-1200r/min, after polyethylene glycol is added, is continued in 80-90
DEG C, stir 20-30min under 1000-1200r/min；
2) ethylenediamine tetra-acetic acid and Sodium Dimercapto Sulfonate are sequentially added in the resulting material of step 1), then in 80-90
DEG C, stir 10-20min under 1000-1200r/min；
3) paranitroanilinum, azodiisobutyronitrile and n-proplbenzene are sequentially added in the resulting material of step 2), then in 80-90
DEG C, stir 30-40min under 1000-1200r/min, obtain sulfosalicylic acid plating silver additive.
8. the method for claim 7, characterized by the following steps:
1) heat the water to 80-90 DEG C, under the stirring of 1000-1200r/min, sequentially add polyethylene glycol, alcohol ether phosphate,
After polyoxyethylate amide, high-carbon fatty alcohol polyoxyethylene ether and alkyl phenol polyoxyethylene ether, continue in 80-90 DEG C, 1000-
20-30min is stirred under 1200r/min；
2) by ethylenediamine tetra-acetic acid, Sodium Dimercapto Sulfonate, thioacetic acid, triethanolamine, ammonium fluoride,
Potassium chromate, acetylacetone,2,4-pentanedione, tartaric acid and ethylenediamine tetrapropionic acid sequentially add in the resulting material of step 1), then in 80-
90 DEG C, stir 10-20min under 1000-1200r/min；
3) by paranitroanilinum, azodiisobutyronitrile, triethylamine, aziridine, pyrrolidines, n-proplbenzene, diphenyl-methane, naphthalene and anthracene
It sequentially adds in the resulting material of step 2), then stirs 30-40min at 80-90 DEG C, 1000-1200r/min, obtain sulfo group
Salicylic acid plates silver additive.
9. the silver-plated plating of sulfosalicylic acid comprising sulfosalicylic acid as claimed in any one of claims 1 to 6 plating silver additive
Liquid, it is characterised in that: plate silver additive 200-300mL/L, sulfosalicylic acid 150-200g/L, silver nitrate including sulfosalicylic acid
50-80g/L, propionic acid ammonium 20-30g/L, the water of sodium hydroxide 15-20g/L and surplus.
10. the preparation method of sulfosalicylic acid plate silver plating solution as claimed in claim 9, characterized by the following steps:
1) sulfosalicylic acid is dissolved in water, obtains solution one；
2) by sodium hydroxide be dissolved in water after, be added in solution one, obtain solution two；
3) it after silver nitrate being dissolved in water, is added in solution two, obtains solution three；
4) it after propionic acid ammonium being dissolved in water, is added in solution three, obtains solution four；
5) sulfosalicylic acid plating silver additive is added in solution four, is added water to aequum, then adjust pH to 9 to get
Sulfosalicylic acid plate silver plating solution.
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| CN201811132651.0A CN109023450B (en) | 2018-09-27 | 2018-09-27 | Sulfosalicylic acid silver plating additive, preparation method thereof and electroplating solution containing sulfosalicylic acid silver plating additive |
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| CN201811132651.0A CN109023450B (en) | 2018-09-27 | 2018-09-27 | Sulfosalicylic acid silver plating additive, preparation method thereof and electroplating solution containing sulfosalicylic acid silver plating additive |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111519219A (en) * | 2019-12-21 | 2020-08-11 | 东莞奕创表面处理科技有限公司 | Silver electroplating liquid composite additive and preparation method and application thereof |
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111519219A (en) * | 2019-12-21 | 2020-08-11 | 东莞奕创表面处理科技有限公司 | Silver electroplating liquid composite additive and preparation method and application thereof |
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