CN105040048A - Silver plating brightening agent and preparing method thereof - Google Patents
Silver plating brightening agent and preparing method thereof Download PDFInfo
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- CN105040048A CN105040048A CN201510487722.9A CN201510487722A CN105040048A CN 105040048 A CN105040048 A CN 105040048A CN 201510487722 A CN201510487722 A CN 201510487722A CN 105040048 A CN105040048 A CN 105040048A
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Abstract
The invention discloses a silver plating brightening agent and a preparing method thereof. The preparing method comprises the steps that (1) pyridinium propyl sulfobetaine, 1,4-butynediol, chitosan, nonylphenol polyoxyethylene ether, monopotassium phosphate, nitric acid, citric acid, anion surface active agents and water are mixed to obtain a mixture M1; (2), ammonia water is dropwise added into the mixture M1, the pH is adjusted to be 4.5-6, and a mixture M2 is obtained; and (3) heat treatment is conducted on the mixture M2, so that the silver plating brightening agent is obtained. The brightening effect of the silver plating brightening agent prepared through the method is excellent during electroplating, and a silver-plated layer obtained through electroplating is smooth and good in glossiness.
Description
Technical field
The present invention relates to electrosilvering field, particularly, relate to a kind of silver-plating brightener and preparation method thereof.
Background technology
In order to make workpiece to be plated, there is higher electroconductibility light reflective and to organic acid, the chemical stability of alkali, usually electroplate precious metal on workpiece to be plated, because the cost of silvered film is lower than Gold plated Layer comparatively speaking, thus the functional platings such as decorative electroplating electron device are widely used in, in silver plating process, the silvered film of workpiece surface to be plated there will be the lacklustre phenomenon of obfuscation, existing technique normally adds the problem that brightening agent solves surface obfuscation in silvered film, almost complete absorption monolayer is formed on the surface at plating piece at brightening agent, adsorption plane occurs continuously formed and the micropore disappeared, metal can form deposition at these micropore places, because micropore is chaotic distribution, therefore metal deposition is equally distributed, cause coating light and planarization is good.
At present, silver-plating brightener conventional in silver plating process is mainly organic brightening agent of sulfur-bearing, and this kind of brightening agent bright current density range is wider, and the operational humidity upper limit is higher, but the brightness effect of this kind of brightening agent is poor, silvered film unfairness, low in glossiness.
Summary of the invention
The object of this invention is to provide a kind of silver-plating brightener and preparation method thereof, the silver-plating brightener prepared by this preparation method brightness effect in plating is excellent, and electroplates that the silvered film obtained is smooth and glossiness good.
To achieve these goals, the invention provides a kind of preparation method of silver-plating brightener, this preparation method comprises:
(1) by obtained for the mixing of propane sulfonic acid pyridinium salt, Isosorbide-5-Nitrae-butynediol, chitosan, polyoxyethylene nonylphenol ether, potassium primary phosphate, nitric acid, citric acid, anion surfactant and water mixture M 1;
(2) in described mixture M 1, drip ammoniacal liquor regulate pH to 4.5-6, obtained mixture M 2;
(3) thermal treatment of described mixture M 2 is obtained silver-plating brightener.
Pass through technique scheme, silver-plating brightener provided by the invention is by by propane sulfonic acid pyridinium salt, 1,4-butynediol, chitosan, polyoxyethylene nonylphenol ether, potassium primary phosphate, nitric acid, citric acid, anion surfactant and water are mixed to get mixture, adjust ph is to 4.5-6, and last thermal treatment is prepared and obtains.In preparation process, with the addition of propane sulfonic acid pyridinium salt, 1,4-butynediol, chitosan, polyoxyethylene nonylphenol ether, potassium primary phosphate, nitric acid and citric acid, mutually synergy is there occurs between these seven kinds of components, make the silver-plating brightener brightness effect excellence obtained, the silvered film that plating obtains is smooth and glossiness good.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of preparation method of silver-plating brightener, the method comprises:
(1) by obtained for the mixing of propane sulfonic acid pyridinium salt, Isosorbide-5-Nitrae-butynediol, chitosan, polyoxyethylene nonylphenol ether, potassium primary phosphate, nitric acid, citric acid, anion surfactant and water mixture M 1;
(2) in described mixture M 1, drip ammoniacal liquor regulate pH to 4.5-6, obtained mixture M 2;
(3) thermal treatment of described mixture M 2 is obtained silver-plating brightener.
In the present invention, the weight-average molecular weight of the weight-average molecular weight of polyoxyethylene nonylphenol ether can be selected in wide scope, and in order to make the silver-plating brightener bright property that obtains more excellent, preferably, the weight-average molecular weight of polyoxyethylene nonylphenol ether is 22000-28000.
Certainly, in step (1), the consumption of each component all can be selected in wide scope, the silver-plating brightener bright property that carry out to make concerted reaction faster and making obtains is more excellent, preferably, relative to the described propane sulfonic acid pyridinium salt of 100 weight parts, 1, the consumption of 4-butynediol is 55-70 total amount part, the consumption of chitosan is 40-50 weight part, the consumption of polyoxyethylene nonylphenol ether is 20-30 weight part, the consumption of potassium primary phosphate is 25-40 weight part, the consumption of nitric acid is 6-10 weight part, the consumption of citric acid is 8-15 weight part, the consumption of anion surfactant is 2-8 weight part, the consumption of water is 150-300 weight part.
Similarly, the concrete kind of anion surfactant has diversity, can be dialkyl benzene sulfonic acids sodium and sodium lauryl sulphate, also can be Aerosol OT and triethanolamine lauryl sulfate, in order to better promote that concerted reaction is carried out, preferably, anion surfactant is selected from one or more in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate and Aerosol OT.
Meanwhile, the concentration of nitric acid also can be selected in wide scope, and in order to make the silver-plating brightener bright property that obtains more excellent, preferably, the concentration of nitric acid is 45-55 % by weight.
In the present invention, thermal treatment temp in step (3) and time all can be selected in wide scope, in order to make silvered film more smooth, preferably, thermal treatment at least meets the following conditions: thermal treatment temp is 60-90 DEG C, and heat treatment time is 30-60min.
Present invention also offers a kind of silver-plating brightener, this silver-plating brightener is prepared by above-mentioned preparation method and obtains.
Below will be described the present invention by embodiment.In following examples, propane sulfonic acid pyridinium salt is the commercially available product of Roche development in science and technology company limited of Wuhan City, 1,4-butynediol is the commercially available product of prosperous source, Hubei along company limited, chitosan is purchased from Shanghai Bang Jing Chemical Co., Ltd., polyoxyethylene nonylphenol ether is purchased from Guang Dahuaxin Chemical Co., Ltd., and potassium primary phosphate is purchased from Shifang City starfish Chemical Co., Ltd., and citric acid is Suzhou Min Hong Chemical Co., Ltd..
Embodiment 1
(1) at 25 DEG C, by 100g propane sulfonic acid pyridinium salt, Isosorbide-5-Nitrae-butynediol 65g, 45g chitosan, 25g polyoxyethylene nonylphenol ether (weight-average molecular weight is 25000), 35g potassium primary phosphate, 50 % by weight nitric acid 8g, 12g citric acid, 6g Sodium dodecylbenzene sulfonate and the obtained mixture M 1 of 220g water mixing;
(2) in described mixture M 1, drip ammoniacal liquor regulate pH to 5, obtained mixture M 2;
(3) described mixture M 2 thermal treatment 40min at 70 DEG C is obtained silver-plating brightener A1.
Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Embodiment 2
(1) at 25 DEG C, by 100g propane sulfonic acid pyridinium salt, Isosorbide-5-Nitrae-butynediol 55g, 40g chitosan, 20g polyoxyethylene nonylphenol ether (weight-average molecular weight is 22000), 25g potassium primary phosphate, 45 % by weight nitric acid 6g, 8g citric acid, 2g sodium lauryl sulphate and the obtained mixture M 1 of 150g water mixing;
(2) in described mixture M 1, drip ammoniacal liquor regulate pH to 4.5, obtained mixture M 2;
(3) described mixture M 2 thermal treatment 60min at 60 DEG C is obtained silver-plating brightener A2.
Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Embodiment 3
(1) at 25 DEG C, by 100g propane sulfonic acid pyridinium salt, Isosorbide-5-Nitrae-butynediol 70g, 50g chitosan, 30g polyoxyethylene nonylphenol ether (weight-average molecular weight is 28000), 40g potassium primary phosphate, 55 % by weight nitric acid 10g, 15g citric acid, 8g Aerosol OT and the obtained mixture M 1 of 300g water mixing;
(2) in described mixture M 1, drip ammoniacal liquor regulate pH to 6, obtained mixture M 2;
(3) described mixture M 2 thermal treatment 30min at 90 DEG C is obtained silver-plating brightener A3.
Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Comparative example 1
Silver-plating brightener B1 is obtained according to the method for embodiment 1, unlike, do not use propane sulfonic acid pyridinium salt.Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Comparative example 2
Silver-plating brightener B2 is obtained according to the method for embodiment 1, unlike, do not use Isosorbide-5-Nitrae-butynediol.Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Comparative example 3
Silver-plating brightener B3 is obtained according to the method for embodiment 1, unlike, do not use chitosan.Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Comparative example 4
Silver-plating brightener B4 is obtained according to the method for embodiment 1, unlike, do not use polyoxyethylene nonylphenol ether.Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Comparative example 5
Silver-plating brightener B5 is obtained according to the method for embodiment 1, unlike, do not use potassium primary phosphate.Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Comparative example 6
Silver-plating brightener B6 is obtained according to the method for embodiment 1, unlike, do not use nitric acid.Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Comparative example 7
Silver-plating brightener B7 is obtained according to the method for embodiment 1, unlike, do not use citric acid.Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Comparative example 8
Silver-plating brightener B8 is obtained according to the method for embodiment 1, unlike, in step (2), be 7 by pH regulator.Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Comparative example 9
Silver-plating brightener B9 is obtained according to the method for embodiment 1, unlike, in step (2), be 4 by pH regulator.Electroplated by this silver-plating brightener, silvered film outward appearance is as shown in table 1.
Table 1
| Silvered film outward appearance | |
| A1 | Coating is smooth, bright, have silvery white gloss |
| A2 | Coating is smooth, bright, have silvery white gloss |
| A3 | Coating is smooth, bright, have silvery white gloss |
| B1 | Coating is smooth, obfuscation, tarnish |
| B2 | Coating is smooth, obfuscation, tarnish |
| B3 | Coating be spongy, have particle, tarnish |
| B4 | Coating is smooth, shades, has silvery white gloss |
| B5 | Coating be spongy, have particle, tarnish |
| B6 | Coating is smooth, shades, has silvery white gloss |
| B7 | Coating be spongy, have particle, tarnish |
| B8 | Coating is smooth, obfuscation, tarnish |
| B9 | Coating is smooth, obfuscation, tarnish |
As shown in Table 1, silver-plating brightener provided by the invention has excellent bright performance, use this silver-plating brightener electroplate the silvered film coating obtained smooth, bright, have silvery white gloss.Relative to A1-A3, use B1-B7 electroplate the silvered film obtained there will be in spongy, have particle, obfuscation, lacklustre outward appearance, describe propane sulfonic acid pyridinium salt, 1,4-butynediol, chitosan, polyoxyethylene nonylphenol ether, potassium primary phosphate, nitric acid and citric acid, mutually there occurs synergy between these seven kinds of components, make the silver-plating brightener brightness effect excellence obtained.Relative to A1-A3, although it is smooth to use B8-B9 to electroplate the silvered film obtained, coating shades, matt.The bright property of pH value on silver-plating brightener describing system has larger impact.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (7)
1. a preparation method for silver-plating brightener, is characterized in that, described preparation method comprises:
(1) by obtained for the mixing of propane sulfonic acid pyridinium salt, Isosorbide-5-Nitrae-butynediol, chitosan, polyoxyethylene nonylphenol ether, potassium primary phosphate, nitric acid, citric acid, anion surfactant and water mixture M 1;
(2) in described mixture M 1, drip ammoniacal liquor regulate pH to 4.5-6, obtained mixture M 2;
(3) thermal treatment of described mixture M 2 is obtained silver-plating brightener.
2. preparation method according to claim 1, wherein, the weight-average molecular weight of described polyoxyethylene nonylphenol ether is 22000-28000.
3. preparation method according to claim 2, wherein, relative to the described propane sulfonic acid pyridinium salt of 100 weight parts, described 1, the consumption of 4-butynediol is 55-70 weight part, the consumption of described chitosan is 40-50 weight part, the consumption of described polyoxyethylene nonylphenol ether is 20-30 weight part, the consumption of described potassium primary phosphate is 25-40 weight part, the consumption of described nitric acid is 6-10 weight part, the consumption of described citric acid is 8-15 weight part, and the consumption of described anion surfactant is 2-8 weight part, and the consumption of described water is 150-300 weight part.
4. preparation method according to claim 1, wherein, described anion surfactant be selected from Sodium dodecylbenzene sulfonate, sodium lauryl sulphate and Aerosol OT one or more.
5. according to the preparation method in claim 1-4 described in any one, wherein, the concentration of described nitric acid is 45-55 % by weight.
6. preparation method according to claim 6, wherein, the thermal treatment described in step (3) at least meets the following conditions: thermal treatment temp is 60-90 DEG C, and heat treatment time is 30-60min.
7. a silver-plating brightener, is characterized in that, described silver-plating brightener obtains according to the method preparation in claims 1-6 described in any one.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071445A (en) * | 2011-02-28 | 2011-05-25 | 济南德锡科技有限公司 | Non-cyanide silvering brightener and plating solution thereof |
| CN102995078A (en) * | 2012-10-12 | 2013-03-27 | 张家港祥新电镀材料有限公司 | Cyaniding silver plating brightening agent and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071445A (en) * | 2011-02-28 | 2011-05-25 | 济南德锡科技有限公司 | Non-cyanide silvering brightener and plating solution thereof |
| CN102995078A (en) * | 2012-10-12 | 2013-03-27 | 张家港祥新电镀材料有限公司 | Cyaniding silver plating brightening agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 肖文涛: "2,2 -联吡啶光亮剂对5,5 -二甲基乙内酰脲无氰镀银性能的影响", 《材料保护》 * |
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Inventor after: Ding Xianfeng Inventor after: Tian Zhibin Inventor before: Shen Fujian Inventor before: Jiang Hao Inventor before: Chu Shiquan Inventor before: Ji Yanhai |
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Effective date of registration: 20180419 Address after: 510663 room 1201, main building 111, science Road, Guangzhou high tech Industrial Development Zone, Guangdong Applicant after: Guangzhou Hao Yue new Mstar Technology Ltd Address before: 244000 Jinqiao Industrial Park, Tongling, Anhui Applicant before: Anhui Jiangwei Precision Manufacturing Co., Ltd. |
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