CN103923560B - A kind of water-based plate close agent and preparation method thereof - Google Patents
A kind of water-based plate close agent and preparation method thereof Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000004814 polyurethane Substances 0.000 claims abstract description 36
- 229920002635 polyurethane Polymers 0.000 claims abstract description 36
- 239000013530 defoamer Substances 0.000 claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract 5
- 239000010703 silicon Substances 0.000 claims abstract 5
- 239000007864 aqueous solution Substances 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical class OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 16
- 239000002202 Polyethylene glycol Substances 0.000 claims description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 10
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 5
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 3
- OPZSCKKVQRQTSY-UHFFFAOYSA-N 2-[2-hydroxyethyl(methyl)amino]ethanol;hydrate Chemical compound O.OCCN(C)CCO OPZSCKKVQRQTSY-UHFFFAOYSA-N 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 14
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 7
- -1 polyoxyethylene Polymers 0.000 claims 7
- 238000010792 warming Methods 0.000 claims 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims 1
- 238000000605 extraction Methods 0.000 claims 1
- 230000007062 hydrolysis Effects 0.000 claims 1
- 238000006460 hydrolysis reaction Methods 0.000 claims 1
- 125000001261 isocyanato group Chemical group *N=C=O 0.000 claims 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 150000003839 salts Chemical class 0.000 abstract description 10
- 239000007921 spray Substances 0.000 abstract description 10
- 238000005260 corrosion Methods 0.000 abstract description 8
- 230000007797 corrosion Effects 0.000 abstract description 7
- 238000000576 coating method Methods 0.000 abstract description 6
- 238000007747 plating Methods 0.000 abstract description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 238000007789 sealing Methods 0.000 abstract description 4
- 229910052804 chromium Inorganic materials 0.000 abstract description 2
- 239000011651 chromium Substances 0.000 abstract description 2
- 239000000945 filler Substances 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- 238000009713 electroplating Methods 0.000 description 31
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 29
- 239000000565 sealant Substances 0.000 description 25
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 21
- 239000002518 antifoaming agent Substances 0.000 description 16
- 239000010410 layer Substances 0.000 description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 14
- 229920001296 polysiloxane Polymers 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 7
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 125000005442 diisocyanate group Chemical group 0.000 description 4
- 229940008841 1,6-hexamethylene diisocyanate Drugs 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 238000013035 low temperature curing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
Description
技术领域technical field
本发明涉及高分子材料技术领域，具体涉及一种金属电镀铬后表面封孔保护的高分子水性涂料及其制备方法。The invention relates to the technical field of polymer materials, in particular to a polymer water-based paint for sealing and protecting the surface of metal after chrome plating and a preparation method thereof.
背景技术Background technique
金属表面电镀铬是增强金属抗腐蚀性和装饰性的常用方法，但在电镀过程中镀铬层不可避免地会产生一些孔隙和裂纹，使其耐腐蚀性降低。增强镀铬层抗腐性的一种有效方法是在镀层表面涂装一层高分子树脂堵塞和封闭镀层中的微孔和裂隙，用以隔绝外来物质的侵蚀。Chromium electroplating on metal surfaces is a common method to enhance the corrosion resistance and decoration of metals, but some pores and cracks will inevitably occur in the chrome plating layer during the electroplating process, which will reduce its corrosion resistance. An effective way to enhance the corrosion resistance of the chrome plating layer is to coat a layer of polymer resin on the surface of the plating layer to block and seal the micropores and cracks in the plating layer to isolate the erosion of foreign substances.
常用电镀封闭剂有溶剂型和水性两大类。溶剂型由于存在对人和环境的危害，已逐渐被水性封闭剂取代。水性电镀封闭剂目前使用最普遍的为水性丙烯酸树脂，但这类封闭剂存在着耐候、耐水性不理想，用其封闭的镀件抗蚀性能随时间的延长很快降低。水性有机硅树脂是近年来发展的新型的电镀封闭剂，它具有与电镀层附着力强，涂层光亮，耐水性好的优点。潘慧铭等报道了一种用有机硅单体制备的水性有机硅电镀封闭剂，CN102719121A介绍了一种有机-无机杂化硅烷材料制备的低温固化水性金属防腐蚀涂料。但已有的一些研究指出，单用水性有机硅树脂作封闭剂，其耐盐雾性能并不理想。There are two types of commonly used electroplating sealers: solvent-based and water-based. Solvent-based sealants have been gradually replaced by water-based sealants due to the hazards to humans and the environment. The water-based electroplating sealant is currently the most commonly used water-based acrylic resin, but this type of sealant has unsatisfactory weather resistance and water resistance, and the corrosion resistance of the plated parts sealed with it will quickly decrease with time. Water-based silicone resin is a new type of electroplating sealant developed in recent years. It has the advantages of strong adhesion to the electroplating layer, bright coating and good water resistance. Pan Huiming et al. reported a water-based silicone electroplating sealer prepared from silicone monomers, and CN102719121A introduced a low-temperature curing water-based metal anti-corrosion coating prepared from an organic-inorganic hybrid silane material. However, some existing studies have pointed out that the salt spray resistance performance of water-based silicone resin alone as a sealing agent is not ideal.
发明内容Contents of the invention
针对现有技术中存在的不足，本发明的目的在于提供一种有机硅改性的水性聚氨酯电镀封闭剂及其制备方法，用有机硅改性的水性聚氨酯作成膜剂，用硅溶胶作填料，辅以消泡剂、流平剂制成有机硅改性的电镀封闭剂，与电镀层附着力强，具有优良的耐蚀性、耐水性及耐磨性。其具体指标如下：与电镀层附着力0级，耐盐雾实验≥96小时，光泽度大于100，耐水实验≥164小时。In view of the deficiencies in the prior art, the object of the present invention is to provide a silicone-modified water-based polyurethane electroplating sealant and a preparation method thereof, wherein the silicone-modified water-based polyurethane is used as a film-forming agent, and silica sol is used as a filler. Supplemented with defoaming agent and leveling agent to make a silicone modified electroplating sealant, it has strong adhesion to the electroplating layer and has excellent corrosion resistance, water resistance and wear resistance. The specific indicators are as follows: adhesion to electroplating layer 0, salt spray resistance test ≥ 96 hours, glossiness greater than 100, water resistance test ≥ 164 hours.
本发明的目的主要通过以下技术方案来实现：The purpose of the present invention is mainly achieved through the following technical solutions:
一种水性电镀封闭剂，其由重量份如下的组分组成：A water-based electroplating sealant, which consists of the following components in parts by weight:
有机硅改性的水性聚氨酯20-60份、硅溶胶10-30份、流平剂水溶液1-5份、消泡剂水溶液5-10份最后用去离子水补至100份；20-60 parts of silicone-modified water-based polyurethane, 10-30 parts of silica sol, 1-5 parts of leveling agent aqueous solution, 5-10 parts of defoaming agent aqueous solution, and finally make up to 100 parts with deionized water;
所述有机硅改性的水性聚氨酯按照如下方法制备：The water-based polyurethane modified by the organosilicon is prepared according to the following method:
在四口烧瓶中投入聚乙二醇、2，2-二羟甲基丙酸，升温至80℃，真空脱水2小时；降温至室温，加入丙酮，通氮气，搅拌至2，2-二羟甲基丙酸完全溶解，升温至60℃，缓慢滴加二异氰酸酯，维持60℃～65℃反应4小时，升温至80℃反应0.5小时；然后加入3-氨丙基三甲氧基硅烷，反应1小时，降温到35℃，加入水及N-甲基二乙醇胺，以1200r/min的速度搅拌0.5小时，然后加入2M的氨水调节至pH＝9～10，得透明的有机硅改性的水性聚氨酯。Put polyethylene glycol and 2,2-dimethylolpropionic acid into a four-neck flask, heat up to 80°C, and vacuum dehydrate for 2 hours; cool down to room temperature, add acetone, blow nitrogen, and stir until 2,2-dihydroxy Completely dissolve methacrylic acid, raise the temperature to 60°C, slowly add diisocyanate dropwise, maintain the reaction at 60°C-65°C for 4 hours, raise the temperature to 80°C for 0.5 hour; then add 3-aminopropyltrimethoxysilane, react 1 hour, lower the temperature to 35°C, add water and N-methyldiethanolamine, stir at a speed of 1200r/min for 0.5 hour, then add 2M ammonia water to adjust the pH to 9-10, and obtain transparent silicone-modified waterborne polyurethane .
所述聚乙二醇分子量为400～2000；The polyethylene glycol molecular weight is 400～2000;
所述二异氰酸酯为甲苯二异氰酸酯、异佛尔酮二异氰酸酯、1，6－己二异氰酸酯、甲基环己基二异氰酸酯中的任意一种。The diisocyanate is any one of toluene diisocyanate, isophorone diisocyanate, 1,6-hexamethylene diisocyanate and methylcyclohexyl diisocyanate.
所述二异氰酸酯中的异氰酸基与羟基(聚乙二醇和2，2-二羟甲基丙酸中的羟基之和)(NCO/OH)的摩尔比为1.05/1；The mol ratio of the isocyanate group in the diisocyanate to the hydroxyl group (the sum of the hydroxyl group in polyethylene glycol and 2,2-dimethylol propionic acid) (NCO/OH) is 1.05/1;
所述2，2-二羟甲基丙酸的质量为聚乙二醇和二异氰酸酯质量之和的5.0％；The quality of the 2,2-dimethylolpropionic acid is 5.0% of the sum of polyethylene glycol and diisocyanate quality;
所述3-氨丙基三甲氧基硅烷与聚乙二醇的摩尔比为1/5；The mol ratio of described 3-aminopropyltrimethoxysilane to Polyethylene Glycol is 1/5;
所述N-甲基二乙醇胺与聚乙二醇的摩尔比为1/1；The mol ratio of described N-methyldiethanolamine and polyethylene glycol is 1/1;
所述丙酮的量(体积)与聚乙二醇的量(质量)的比为1/1(ml/g)；The ratio of the amount (volume) of the acetone to the amount (mass) of polyethylene glycol is 1/1 (ml/g);
所述有机硅改性的水性聚氨酯制备过程中所加水的质量为聚乙二醇质量的10倍；The quality of water added in the preparation process of the organosilicon-modified waterborne polyurethane is 10 times of the quality of polyethylene glycol;
所述硅溶胶按如下方法制备：Described silica sol is prepared as follows:
将1000ml水、2M的醋酸溶液10ml加入2000ml烧杯中，然后缓慢加入5g正硅酸乙酯、20g3-氨丙基三乙氧基硅烷及10gγ-(2,3-环氧丙氧基)丙基三甲氧基硅烷，搅拌下室温水解1小时，然后用2M氨水调节至pH＝8～9，升温至100℃，蒸出乙醇得无色透明的硅溶胶。Add 1000ml of water and 10ml of 2M acetic acid solution into a 2000ml beaker, then slowly add 5g of ethyl orthosilicate, 20g of 3-aminopropyltriethoxysilane and 10g of γ-(2,3-epoxypropoxy)propyl Trimethoxysilane was hydrolyzed at room temperature for 1 hour under stirring, then adjusted to pH = 8-9 with 2M ammonia water, heated to 100°C, and distilled off ethanol to obtain a colorless and transparent silica sol.
所述流平剂水溶液为10％(质量百分比)的silok-8255水性流平剂水溶液。The leveling agent aqueous solution is 10% (mass percentage) silok-8255 aqueous leveling agent aqueous solution.
所述消泡剂水溶液为5％(质量百分比)的SILCOLAPSEC546水性有机硅消泡剂水溶液。The antifoaming agent aqueous solution is 5% (mass percentage) SILCOLAPSEC546 aqueous silicone antifoaming agent aqueous solution.
与现有技术相比，本发明的优点和有益效果在于：Compared with prior art, advantage and beneficial effect of the present invention are:
1、具有优良的耐候性和耐蚀性，涂层不易变色，装饰性好。1. It has excellent weather resistance and corrosion resistance, the coating is not easy to change color, and the decoration is good.
2、由于采用了有机硅改性的聚氨酯和硅溶胶复合体系，最后形成的保护层既具有良好有韧性，又有一定的硬度；克服了水性高分子涂层硬度不足、易划伤的缺点。2. Due to the use of silicone-modified polyurethane and silica sol composite system, the final protective layer has good toughness and certain hardness; it overcomes the shortcomings of insufficient hardness and easy scratching of water-based polymer coatings.
具体实施方式detailed description
下面申请人将结合具体的实施例对本发明的产品及其制备方法加以详细说明。Below the applicant will describe in detail the product of the present invention and its preparation method in conjunction with specific examples.
以下实施例1-6中，所得产品的检测方法的标准如下：In following embodiment 1-6, the standard of the detection method of gained product is as follows:
电镀层附着力按GB/T9286-1998测试；Electroplating layer adhesion is tested according to GB/T9286-1998;
耐盐雾实验按GB/T10125-2012测试；The salt spray test is tested according to GB/T10125-2012;
光泽度按GB/T9754-2007中的方法测试；Gloss is tested according to the method in GB/T9754-2007;
耐水实验按GB/T1733-93中的方法1测试。The water resistance test is tested according to method 1 in GB/T1733-93.
实施例1Example 1
一种水性电镀封闭剂，由有机硅改性的水性聚氨酯、硅溶胶、流平剂水溶液、消泡剂水溶液以及去离子水组成。A water-based electroplating sealant is composed of silicone-modified water-based polyurethane, silica sol, leveling agent aqueous solution, defoamer aqueous solution and deionized water.
其中，有机硅改性的水性聚氨酯的制备方法如下：Wherein, the preparation method of the waterborne polyurethane modified by organosilicon is as follows:
在四口烧瓶中投入40.0g聚乙二醇(分子量400)，3.1g2，2-二羟甲基丙酸，升温至80℃，真空脱水2小时；降温至室温，加入40ml丙酮，通氮气，搅拌至2，2-二羟甲基丙酸完全溶解，升温至60℃，缓慢滴加21.9g甲苯二异氰酸酯，维持60℃～65℃反应4小时，然后升温至80℃反应0.5小时；然后加入3.58g3-氨丙基三甲氧基硅烷，反应1小时，降温到35℃，加入400ml水及12.0gN-甲基二乙醇胺，以1200r/min的速度搅拌0.5小时，加入2M的氨水调节至pH＝9～10，得透明的有机硅改性的水性聚氨酯。Put 40.0g polyethylene glycol (molecular weight 400) and 3.1g 2,2-dimethylolpropionic acid into a four-neck flask, heat up to 80°C, and vacuum dehydrate for 2 hours; cool down to room temperature, add 40ml acetone, and blow nitrogen, Stir until the 2,2-dimethylolpropionic acid is completely dissolved, raise the temperature to 60°C, slowly add 21.9g of toluene diisocyanate dropwise, maintain the reaction at 60°C-65°C for 4 hours, then raise the temperature to 80°C for 0.5 hours; then add 3.58g of 3-aminopropyltrimethoxysilane, reacted for 1 hour, cooled to 35°C, added 400ml of water and 12.0g of N-methyldiethanolamine, stirred at a speed of 1200r/min for 0.5 hours, added 2M ammonia water to adjust the pH= 9 to 10, to obtain transparent silicone-modified water-based polyurethane.
其中，硅溶胶的制备方法如下：Wherein, the preparation method of silica sol is as follows:
将1000ml水、2M的醋酸溶液10ml加入2000ml烧杯中，然后缓慢加入5g正硅酸乙酯、20g3-氨丙基三乙氧基硅烷及10gγ-(2,3-环氧丙氧基)丙基三甲氧基硅烷，搅拌下室温水解1小时，用2M氨水调节pH＝8～9，升温至100℃，蒸出乙醇得无色透明的硅溶胶。Add 1000ml of water and 10ml of 2M acetic acid solution into a 2000ml beaker, then slowly add 5g of ethyl orthosilicate, 20g of 3-aminopropyltriethoxysilane and 10g of γ-(2,3-epoxypropoxy)propyl Trimethoxysilane was hydrolyzed at room temperature for 1 hour under stirring, adjusted to pH=8-9 with 2M ammonia water, heated to 100°C, and distilled off ethanol to obtain a colorless and transparent silica sol.
其中，流平剂水溶液为10％(质量百分比)的silok-8255水性流平剂水溶液。Wherein, the leveling agent aqueous solution is 10% (mass percentage) silok-8255 aqueous leveling agent aqueous solution.
消泡剂水溶液为5％(质量百分比)的SILCOLAPSEC546水性有机硅消泡剂水溶液。The antifoaming agent aqueous solution is 5% (mass percentage) SILCOLAPSEC546 aqueous silicone antifoaming agent aqueous solution.
将上述有机硅改性的水性聚氨酯20g、硅溶胶30g、流平剂水溶液1g、消泡剂水溶液5g以及去离子水44ml搅拌混合均匀，得水性电镀封闭剂。实验测得该封闭剂与电镀层附着力为0级，耐盐雾实验96小时，光泽度100，耐水实验172小时。Stir and mix the above silicone-modified waterborne polyurethane 20g, silica sol 30g, leveling agent aqueous solution 1g, defoamer aqueous solution 5g and deionized water 44ml evenly to obtain an aqueous electroplating sealant. According to the test, the adhesion between the sealant and the electroplating layer is 0, the salt spray test is 96 hours, the gloss is 100, and the water resistance test is 172 hours.
实施例2Example 2
一种水性电镀封闭剂，由有机硅改性的水性聚氨酯、硅溶胶、流平剂水溶液、消泡剂水溶液以及去离子水组成。A water-based electroplating sealant is composed of silicone-modified water-based polyurethane, silica sol, leveling agent aqueous solution, defoamer aqueous solution and deionized water.
其中，有机硅改性的水性聚氨酯的制备方法如下：Wherein, the preparation method of the waterborne polyurethane modified by organosilicon is as follows:
在四口烧瓶中投入60.0g聚乙二醇(分子量600)、4.6g2，2-二羟甲基丙酸，升温至80℃，真空脱水2小时；降温至室温，加入60ml丙酮，通氮气，搅拌至2，2-二羟甲基丙酸完全溶解，升温至60℃，缓慢滴加31.3g异佛尔酮二异氰酸酯，维持60℃～65℃反应4小时，升温至80℃反应0.5小时；然后加入3.58g3-氨丙基三甲氧基硅烷，反应1小时，降温到35℃，加入600ml水及12.0gN-甲基二乙醇胺，以1200r/min的速度搅拌0.5小时，然后加入2M的氨水调节pH＝9～10，得透明的有机硅改性的水性聚氨酯。Put 60.0g of polyethylene glycol (molecular weight 600) and 4.6g of 2,2-dimethylolpropionic acid into a four-neck flask, heat up to 80°C, and vacuum dehydrate for 2 hours; cool down to room temperature, add 60ml of acetone, and blow nitrogen, Stir until the 2,2-dimethylolpropionic acid is completely dissolved, raise the temperature to 60°C, slowly add 31.3g of isophorone diisocyanate dropwise, keep the reaction at 60°C-65°C for 4 hours, then raise the temperature to 80°C for 0.5 hour; Then add 3.58g of 3-aminopropyltrimethoxysilane, react for 1 hour, cool down to 35°C, add 600ml of water and 12.0g of N-methyldiethanolamine, stir at a speed of 1200r/min for 0.5 hour, then add 2M ammonia water to adjust pH = 9-10, to obtain transparent organosilicon-modified water-based polyurethane.
其中，硅溶胶的制备方法如下：Wherein, the preparation method of silica sol is as follows:
将1000ml水、2M的醋酸溶液10ml加入2000ml烧杯中，然后缓慢加入5g正硅酸乙酯、20g3-氨丙基三乙氧基硅烷及10gγ-(2,3-环氧丙氧基)丙基三甲氧基硅烷，搅拌下室温水解1小时，然后用2M氨水调节pH＝8～9，升温至100℃，蒸出乙醇得无色透明的硅溶胶。Add 1000ml of water and 10ml of 2M acetic acid solution into a 2000ml beaker, then slowly add 5g of ethyl orthosilicate, 20g of 3-aminopropyltriethoxysilane and 10g of γ-(2,3-epoxypropoxy)propyl Trimethoxysilane was hydrolyzed at room temperature for 1 hour under stirring, then the pH was adjusted to 8-9 with 2M ammonia water, the temperature was raised to 100°C, and ethanol was distilled off to obtain a colorless and transparent silica sol.
其中，流平剂水溶液为10％(质量百分比)的silok-8255水性流平剂水溶液。Wherein, the leveling agent aqueous solution is 10% (mass percentage) silok-8255 aqueous leveling agent aqueous solution.
消泡剂水溶液为5％(质量百分比)的SILCOLAPSEC546水性有机硅消泡剂水溶液。The antifoaming agent aqueous solution is 5% (mass percentage) SILCOLAPSEC546 aqueous silicone antifoaming agent aqueous solution.
将上述有机硅改性的水性聚氨酯30g、硅溶胶20g、消泡剂水溶液7g、流平剂水溶液3g以及去离子水40ml搅拌混合均匀，得水性电镀封闭剂。实验测得该封闭剂与电镀层附着力为0级，耐盐雾实验126小时，光泽度105，耐水实验182小时。Stir and mix the above-mentioned organosilicon-modified water-based polyurethane 30g, silica sol 20g, defoamer aqueous solution 7g, leveling agent aqueous solution 3g and deionized water 40ml to obtain an aqueous electroplating sealant. According to the test, the adhesion between the sealing agent and the electroplating layer is 0, the salt spray test is 126 hours, the gloss is 105, and the water resistance test is 182 hours.
实施例3Example 3
一种水性电镀封闭剂，由有机硅改性的水性聚氨酯、硅溶胶、流平剂水溶液、消泡剂水溶液以及去离子水组成。A water-based electroplating sealant is composed of silicone-modified water-based polyurethane, silica sol, leveling agent aqueous solution, defoamer aqueous solution and deionized water.
其中，有机硅改性的水性聚氨酯的制备方法如下：Wherein, the preparation method of the waterborne polyurethane modified by organosilicon is as follows:
在四口烧瓶中投入60.0g聚乙二醇(分子量600)、4.2g2，2-二羟甲基丙酸，升温至80℃，真空脱水2小时；降温至室温，加入60ml丙酮，通氮气，搅拌至2，2-二羟甲基丙酸完全溶解，升温至60℃，缓慢滴加23.1g1，6－己二异氰酸酯，维持60℃～65℃反应4小时，升温至80℃反应0.5小时。然后加入3.58g3-氨丙基三甲氧基硅烷，反应1小时，降温到35℃，加入600ml水及12.0gN-甲基二乙醇胺，以1200r/min的速度搅拌0.5小时，然后加入2M的氨水调节pH＝9～10，得透明的有机硅改性的水性聚氨酯。Put 60.0g of polyethylene glycol (molecular weight 600) and 4.2g of 2,2-dimethylolpropionic acid into a four-neck flask, heat up to 80°C, and vacuum dehydrate for 2 hours; cool down to room temperature, add 60ml of acetone, and blow nitrogen, Stir until the 2,2-dimethylolpropionic acid is completely dissolved, raise the temperature to 60°C, slowly add 23.1g of 1,6-hexamethylene diisocyanate dropwise, keep the reaction at 60°C-65°C for 4 hours, then raise the temperature to 80°C for 0.5 hour. Then add 3.58g of 3-aminopropyltrimethoxysilane, react for 1 hour, cool down to 35°C, add 600ml of water and 12.0g of N-methyldiethanolamine, stir at a speed of 1200r/min for 0.5 hour, then add 2M ammonia water to adjust pH = 9-10, to obtain transparent organosilicon-modified water-based polyurethane.
其中，硅溶胶的制备方法如下：Wherein, the preparation method of silica sol is as follows:
将1000ml水、2M的醋酸溶液10ml加入2000ml烧杯中，然后缓慢加入5g正硅酸乙酯、20g3-氨丙基三乙氧基硅烷及10gγ-(2,3-环氧丙氧基)丙基三甲氧基硅烷，搅拌下室温水解1小时，然后用2M氨水调节pH＝8～9，升温至100℃，蒸出乙醇得无色透明的硅溶胶。Add 1000ml of water and 10ml of 2M acetic acid solution into a 2000ml beaker, then slowly add 5g of ethyl orthosilicate, 20g of 3-aminopropyltriethoxysilane and 10g of γ-(2,3-epoxypropoxy)propyl Trimethoxysilane was hydrolyzed at room temperature for 1 hour under stirring, then the pH was adjusted to 8-9 with 2M ammonia water, the temperature was raised to 100°C, and ethanol was distilled off to obtain a colorless and transparent silica sol.
其中，流平剂水溶液为10％(质量百分比)的silok-8255水性流平剂水溶液。Wherein, the leveling agent aqueous solution is 10% (mass percentage) silok-8255 aqueous leveling agent aqueous solution.
消泡剂水溶液为5％(质量百分比)的SILCOLAPSEC546水性有机硅消泡剂水溶液。The antifoaming agent aqueous solution is 5% (mass percentage) SILCOLAPSEC546 aqueous silicone antifoaming agent aqueous solution.
将上述有机硅改性的水性聚氨酯35g、硅溶胶15g、消泡剂水溶液7g、流平剂水溶液4g以及去离子水39ml搅拌混合均匀，得水性电镀封闭剂。实验测得该封闭剂与电镀层附着力为0级，耐盐雾实验134小时，光泽度105，耐水实验176小时。Stir and mix the above silicone-modified water-based polyurethane 35g, silica sol 15g, defoamer aqueous solution 7g, leveling agent aqueous solution 4g and deionized water 39ml to obtain a water-based electroplating sealant. According to the test, the adhesion between the sealant and the electroplating layer is 0, the salt spray test is 134 hours, the gloss is 105, and the water resistance test is 176 hours.
实施例4Example 4
一种水性电镀封闭剂，由有机硅改性的水性聚氨酯、硅溶胶、流平剂水溶液、消泡剂水溶液以及去离子水组成。A water-based electroplating sealant is composed of silicone-modified water-based polyurethane, silica sol, leveling agent aqueous solution, defoamer aqueous solution and deionized water.
其中，有机硅改性的水性聚氨酯的制备方法如下：Wherein, the preparation method of the waterborne polyurethane modified by organosilicon is as follows:
在四口烧瓶中投入100.0g聚乙二醇(分子量1000)，6.8g2，2-二羟甲基丙酸，升温至80℃，真空脱水2小时；降温至室温，加入100ml的丙酮，通氮气，搅拌至2，2-二羟甲基丙酸完全溶解，升温至60℃，缓慢滴加35.2g异佛尔酮二异氰酸酯，维持60℃～65℃反应4小时，升温至80℃反应0.5小时；然后加入3.58g3-氨丙基三甲氧基硅烷，反应1小时，降温到35℃，加入1000ml水及12.0gN-甲基二乙醇胺，以1200r/min的速度搅拌0.5小时，然后加入2M的氨水调节pH＝9～10，得透明的有机硅改性的水性聚氨酯。Put 100.0g polyethylene glycol (molecular weight 1000) and 6.8g 2,2-dimethylolpropionic acid into a four-neck flask, heat up to 80°C, vacuum dehydrate for 2 hours; cool down to room temperature, add 100ml of acetone, and blow nitrogen , stir until 2,2-dimethylolpropionic acid is completely dissolved, heat up to 60°C, slowly add 35.2g of isophorone diisocyanate dropwise, maintain 60°C~65°C for 4 hours, heat up to 80°C for 0.5 hours ; Then add 3.58g of 3-aminopropyltrimethoxysilane, react for 1 hour, cool down to 35°C, add 1000ml of water and 12.0g of N-methyldiethanolamine, stir at a speed of 1200r/min for 0.5 hours, then add 2M ammonia water Adjust pH=9-10 to obtain transparent organosilicon-modified water-based polyurethane.
其中，硅溶胶的制备方法如下：Wherein, the preparation method of silica sol is as follows:
将1000ml水、2M的醋酸溶液10ml加入2000ml烧杯中，然后缓慢加入5g正硅酸乙酯、20g3-氨丙基三乙氧基硅烷及10gγ-(2,3-环氧丙氧基)丙基三甲氧基硅烷，搅拌下室温水解1小时，然后用2M氨水调节pH＝8～9，升温至100℃，蒸出乙醇得无色透明的硅溶胶。Add 1000ml of water and 10ml of 2M acetic acid solution into a 2000ml beaker, then slowly add 5g of ethyl orthosilicate, 20g of 3-aminopropyltriethoxysilane and 10g of γ-(2,3-epoxypropoxy)propyl Trimethoxysilane was hydrolyzed at room temperature for 1 hour under stirring, then the pH was adjusted to 8-9 with 2M ammonia water, the temperature was raised to 100°C, and ethanol was distilled off to obtain a colorless and transparent silica sol.
其中，流平剂水溶液为10％(质量百分比)的silok-8255水性流平剂水溶液。Wherein, the leveling agent aqueous solution is 10% (mass percentage) silok-8255 aqueous leveling agent aqueous solution.
消泡剂水溶液为5％(质量百分比)的SILCOLAPSEC546水性有机硅消泡剂水溶液。The antifoaming agent aqueous solution is 5% (mass percentage) SILCOLAPSEC546 aqueous silicone antifoaming agent aqueous solution.
将上述有机硅改性的水性聚氨酯40g、硅溶胶20g、消泡剂水溶液8g、流平剂水溶液4g以及去离子水28ml搅拌混合均匀，得水性电镀封闭剂。实验测得该封闭剂与电镀层附着力为0级，耐盐雾实验178小时，光泽度110，耐水实验168小时。Stir and mix the above-mentioned organosilicon-modified water-based polyurethane 40g, silica sol 20g, defoamer aqueous solution 8g, leveling agent aqueous solution 4g and deionized water 28ml to obtain an aqueous electroplating sealant. According to the test, the adhesion between the sealant and the electroplating layer is 0, the salt spray test is 178 hours, the gloss is 110, and the water resistance test is 168 hours.
实施例5Example 5
一种水性电镀封闭剂，由有机硅改性的水性聚氨酯、硅溶胶、流平剂水溶液、消泡剂水溶液以及去离子水组成。A water-based electroplating sealant is composed of silicone-modified water-based polyurethane, silica sol, leveling agent aqueous solution, defoamer aqueous solution and deionized water.
其中，有机硅改性的水性聚氨酯的制备方法如下：Wherein, the preparation method of the waterborne polyurethane modified by organosilicon is as follows:
在四口烧瓶中投入200.0g聚乙二醇(分子量2000)、11.77g2，2-二羟甲基丙酸，升温至80℃，真空脱水2小时；降温至室温，加入200ml丙酮，通氮气，搅拌至2，2-二羟甲基丙酸完全溶解，升温至60℃，缓慢滴加35.49g甲基环己基二异氰酸酯，维持60℃～65℃反应4小时，升温至80℃反应0.5小时。然后加入3.58g3-氨丙基三甲氧基硅烷，反应1小时，降温到35℃，加入2000ml水及12.0gN-甲基二乙醇胺，以1200r/min的速度搅拌0.5小时，然后加入2M的氨水调节pH＝9～10，得乳白色半透明的有机硅改性的水性聚氨酯。Put 200.0g polyethylene glycol (molecular weight 2000) and 11.77g 2,2-dimethylolpropionic acid into a four-neck flask, heat up to 80°C, and vacuum dehydrate for 2 hours; cool down to room temperature, add 200ml acetone, blow nitrogen, Stir until the 2,2-dimethylolpropionic acid is completely dissolved, raise the temperature to 60°C, slowly add 35.49g of methylcyclohexyl diisocyanate dropwise, keep the reaction at 60°C-65°C for 4 hours, then raise the temperature to 80°C for 0.5 hour. Then add 3.58g of 3-aminopropyltrimethoxysilane, react for 1 hour, cool down to 35°C, add 2000ml of water and 12.0g of N-methyldiethanolamine, stir at a speed of 1200r/min for 0.5 hours, then add 2M ammonia water to adjust pH = 9-10, to obtain milky white translucent silicone-modified water-based polyurethane.
其中，硅溶胶的制备方法如下：Wherein, the preparation method of silica sol is as follows:
将1000ml水、2M的醋酸溶液10ml加入2000ml烧杯中，然后缓慢加入5g正硅酸乙酯、20g3-氨丙基三乙氧基硅烷及10gγ-(2,3-环氧丙氧基)丙基三甲氧基硅烷，搅拌下室温水解1小时，然后用2M氨水调节pH＝8～9，升温至100℃，蒸出乙醇得无色透明的硅溶胶。Add 1000ml of water and 10ml of 2M acetic acid solution into a 2000ml beaker, then slowly add 5g of ethyl orthosilicate, 20g of 3-aminopropyltriethoxysilane and 10g of γ-(2,3-epoxypropoxy)propyl Trimethoxysilane was hydrolyzed at room temperature for 1 hour under stirring, then the pH was adjusted to 8-9 with 2M ammonia water, the temperature was raised to 100°C, and ethanol was distilled off to obtain a colorless and transparent silica sol.
其中，流平剂水溶液为10％(质量百分比)的silok-8255水性流平剂水溶液。Wherein, the leveling agent aqueous solution is 10% (mass percentage) silok-8255 aqueous leveling agent aqueous solution.
消泡剂水溶液为5％(质量百分比)的SILCOLAPSEC546水性有机硅消泡剂水溶液。The antifoaming agent aqueous solution is 5% (mass percentage) SILCOLAPSEC546 aqueous silicone antifoaming agent aqueous solution.
将上述有机硅改性的水性聚氨酯50g、硅溶胶15g、消泡剂水溶液8g、流平剂水溶液5g以及去离子水22ml搅拌混合均匀，得水性电镀封闭剂。实验测得该封闭剂与电镀层附着力为0级，耐盐雾实验96小时，光泽度105，耐水实验164小时。Stir and mix the above-mentioned organosilicon-modified water-based polyurethane 50g, silica sol 15g, defoamer aqueous solution 8g, leveling agent aqueous solution 5g and deionized water 22ml to obtain a water-based electroplating sealant. According to the test, the adhesion between the sealant and the electroplating layer is 0, the salt spray test is 96 hours, the gloss is 105, and the water resistance test is 164 hours.
实施例6Example 6
一种水性电镀封闭剂，由有机硅改性的水性聚氨酯、硅溶胶、流平剂水溶液、消泡剂水溶液以及去离子水组成。A water-based electroplating sealant is composed of silicone-modified water-based polyurethane, silica sol, leveling agent aqueous solution, defoamer aqueous solution and deionized water.
其中，有机硅改性的水性聚氨酯的制备方法如下：Wherein, the preparation method of the waterborne polyurethane modified by organosilicon is as follows:
在四口烧瓶中投入40.0g聚乙二醇(分子量400)，3.47g2，2-二羟甲基丙酸，升温至80℃，真空脱水2小时；降温至室温，加入40ml丙酮，通氮气，搅拌至2，2-二羟甲基丙酸完全溶解，升温至60℃，缓慢滴加29.4g异佛尔酮二异氰酸酯，维持60℃～65℃反应4小时，升温至80℃反应0.5小时；然后加入3.58g3-氨丙基三甲氧基硅烷，反应1小时，降温到35℃，加入400ml水及12.0gN-甲基二乙醇胺，以1200r/min的速度搅拌0.5小时，然后加入2M的氨水调节pH＝9～10，得透明的有机硅改性的水性聚氨酯。Put 40.0g polyethylene glycol (molecular weight 400) and 3.47g 2,2-dimethylolpropionic acid into a four-neck flask, heat up to 80°C, and vacuum dehydrate for 2 hours; cool down to room temperature, add 40ml acetone, and blow nitrogen, Stir until the 2,2-dimethylolpropionic acid is completely dissolved, raise the temperature to 60°C, slowly add 29.4g of isophorone diisocyanate dropwise, maintain the reaction at 60°C to 65°C for 4 hours, then raise the temperature to 80°C for 0.5 hour; Then add 3.58g of 3-aminopropyltrimethoxysilane, react for 1 hour, cool down to 35°C, add 400ml of water and 12.0g of N-methyldiethanolamine, stir at a speed of 1200r/min for 0.5 hour, then add 2M ammonia water to adjust pH = 9-10, to obtain transparent organosilicon-modified water-based polyurethane.
其中，硅溶胶的制备方法如下：Wherein, the preparation method of silica sol is as follows:
将1000ml水、2M的醋酸溶液10ml加入2000ml烧杯中，然后缓慢加入5g正硅酸乙酯、20g3-氨丙基三乙氧基硅烷及10gγ-(2,3-环氧丙氧基)丙基三甲氧基硅烷，搅拌下室温水解1小时，然后用2M氨水调节pH＝8～9，升温至100℃，蒸出乙醇得无色透明的硅溶胶。Add 1000ml of water and 10ml of 2M acetic acid solution into a 2000ml beaker, then slowly add 5g of ethyl orthosilicate, 20g of 3-aminopropyltriethoxysilane and 10g of γ-(2,3-epoxypropoxy)propyl Trimethoxysilane was hydrolyzed at room temperature for 1 hour under stirring, then the pH was adjusted to 8-9 with 2M ammonia water, the temperature was raised to 100°C, and ethanol was distilled off to obtain a colorless and transparent silica sol.
其中，流平剂水溶液为10％(质量百分比)的silok-8255水性流平剂水溶液。Wherein, the leveling agent aqueous solution is 10% (mass percentage) silok-8255 aqueous leveling agent aqueous solution.
消泡剂水溶液为5％(质量百分比)的SILCOLAPSEC546水性有机硅消泡剂水溶液。The antifoaming agent aqueous solution is 5% (mass percentage) SILCOLAPSEC546 aqueous silicone antifoaming agent aqueous solution.
将上述有机硅改性的水性聚氨酯60g、硅溶胶10g、消泡剂水溶液10g、流平剂水溶液5g以及去离子水15ml搅拌混合均匀，得水性电镀封闭剂。实验测得该封闭剂与电镀层附着力为0级，耐盐雾实验176小时，光泽度105，耐水实验198小时。Stir and mix the above silicone-modified water-based polyurethane 60g, silica sol 10g, defoamer aqueous solution 10g, leveling agent aqueous solution 5g and deionized water 15ml to obtain a water-based electroplating sealant. According to the test, the adhesion between the sealant and the electroplating layer is 0 grade, the salt spray test is 176 hours, the gloss is 105, and the water resistance test is 198 hours.
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| CN104277699A (en) * | 2014-10-29 | 2015-01-14 | 芜湖县双宝建材有限公司 | High-strength modified waterborne polyurethane coating |
| CN104451638B (en) * | 2014-12-16 | 2017-02-08 | 武汉迪赛新材料有限公司 | Self-lubricating chromium-free passivator and preparation method thereof |
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| CN106634516B (en) * | 2016-12-27 | 2020-01-14 | 广东达志环保科技股份有限公司 | High-corrosion-resistance water-based electroplating sealing agent and preparation method thereof |
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| CN112144050B (en) * | 2020-09-24 | 2022-12-23 | 蚌埠学院 | Silicon-based chromium-free passivation solution for Bundy tube and preparation method thereof |
| CN112323053B (en) * | 2020-10-14 | 2021-12-28 | 蚌埠学院 | A kind of silicon-based chromium-free passivation solution for brass surface and preparation method thereof |
| CN112646360A (en) * | 2020-12-24 | 2021-04-13 | 淮北五星铝业有限公司 | Preparation method of functional waterborne polyurethane-based nano composite protective film |
| CN113402689A (en) * | 2021-06-23 | 2021-09-17 | 科文特亚环保电镀技术（江苏）有限公司 | Sealing agent for corrosion-resistant electroplated nickel layer |
| CN115011226A (en) * | 2022-01-17 | 2022-09-06 | 德锡化学(山东)有限公司 | Water-soluble zinc-plating and zinc alloy sealant with low sagging and high corrosion resistance |
| CN115651520B (en) * | 2022-11-02 | 2023-09-08 | 深圳市深赛尔股份有限公司 | High-hardness high-wear-resistance quick-drying water-based automotive topcoat and preparation method thereof |
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Denomination of invention: A water-based electroplating sealing agent and its preparation method Granted publication date: 20160406 Pledgee: Agricultural Bank of China Limited Ezhou Gedian Development Zone Branch Pledgor: WUHAN DESYTEK NEW MATERIAL CO.,LTD. Registration number: Y2024980047484 |