CN106634516A - 一种具有高耐蚀的水性电镀封闭剂及其制备方法 - Google Patents
一种具有高耐蚀的水性电镀封闭剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及精细高分子技术领域，具体涉及一种具有高耐蚀的水性电镀封闭剂及其制备方法，所述的电镀封闭剂是以二氧化碳共聚物多元醇为基础原料，通过有机‑无机复合改性制备的水性乳液。本发明首次将二氧化碳基共聚物多元醇用于电镀封闭剂，利用二氧化碳共聚物多元醇优良的隔氧性，大幅度提高镀层的耐蚀性；通过有机‑无机复合，得到高硬度、高耐磨性的封闭剂。同时使用二氧化碳共聚物多元醇制备，克服聚醚多元醇制备的水性涂层硬度低，聚酯多元醇制备的水性涂层容易水解脱落的缺点，形成硬度与韧性结合的电镀封闭剂。
Description
技术领域
本发明涉及精细高分子技术领域，具体涉及一种具有高耐蚀的水性电镀封闭剂及其制备方法。
背景技术
金属材料在使用过程中，在不同条件下会产生腐蚀，金属腐蚀之后会显著降低其塑性和韧性，大大缩短了金属的使用寿命。为改善其耐腐蚀性，常常对钢铁金属表面镀锌并进行钝化处理，以提高其耐腐蚀性能，同时还可以改善制品外观，提供一定的装饰性。传统的锌及锌合金钝化工艺一般采用铬酸盐钝化，其成本低廉，使用简单，耐蚀性好，在航空、电子和其它工业领域得到广泛应用。铬酸盐钝化膜中铬主要以六价和三价形式存在，三价铬作为钝化膜的骨架，六价铬能够对钝化膜的裸露处镀层再次钝化，对腐蚀起到进一步的抑制作用。然而六价铬具有一定的致癌性，大量使用严重污染环境和影响人类的健康，欧盟已于2006年7月1日正式实施了RoHS指令，以限制六价铬的使用。三价铬在许多方面有着十分类似于六价铬的特性，同时三价铬具有毒性较低的优点。
电镀过程中镀铬层不可避免地会产生一些孔隙和裂纹，由于三价铬钝化膜不具备自愈能力，在孔隙和裂纹处耐腐蚀性降低，为了增强镀铬层抗腐性，目前多采用封闭剂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。
任艳萍(镀锌层三价铬钝化工艺的研究，腐蚀与防护，2007，28(1)，13-16，19)等在钝化液中加入丙烯酸树脂，发现三价铬钝化膜表面的裂纹被丙烯酸树脂完全覆盖，膜层致密度提高。采用三价铬加丙烯酸树脂钝化均可推迟镀锌层出现白锈的时间，与相同条件但未加丙烯酸树脂的膜层相比，耐蚀性明显提高。丙烯酸树脂耐水性较差，长期水浸后反而引起腐蚀。中国专利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。中国专利CN103923560B使用有机硅改性聚乙二醇型聚氨酯水溶液，制备水溶型封闭剂，耐盐雾有大幅度提升。但是由于聚乙二醇为水溶性聚合物，产品在使用过程中容易吸潮，产生腐蚀，同时聚氨酯层本身硬度较低，长期耐磨性较差。
发明内容
本发明第一个目的是针对现有技术的不足提供一种具有高耐蚀的水性电镀封闭剂。
本发明的另一个目的是提供一种具有高耐蚀的水性电镀封闭剂的制备方法。
为了实现以上目的，本发明提供以下技术方案：
一种具有高耐蚀的水性电镀封闭剂，包括以下重量份的组分：
作为优选的，一种具有高耐蚀的水性电镀封闭剂，包括以下重量份的组分：
作为优选的，所述二氧化碳基共聚物多元醇是以二氧化碳为起始原料，在引发剂、催化剂作用下与环氧丙烷共聚合成的二醇，其羟基官能度为2，分子量为2000-4000。
进一步优选的，所述二氧化碳共聚物多元醇的分子量为3000-4000。
作为优选的，所述脂肪族二异氰酸酯是异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、氢化二苯基甲烷二异氰酸酯中的任意一种或几种的混合物。
作为优选的，所述亲水扩链剂为乙二胺基乙磺酸钠、1,4-丁二醇-2-2磺酸钠、二羟甲基丁酸、二羟甲基丙酸中的任意一种或几种混合物。
作为优选的，所述催化剂为辛酸亚锡、异辛酸亚锡、二月桂酸二丁基锡中的任意一种或几种混合物。
作为优选的，所述中和剂为三乙胺三丙胺、三丁胺、氢氧化钠、氨水中的一种或几种的混合物。
作为优选的，所述扩链剂为乙二胺、三甲基己二胺、四乙烯五胺、二乙烯三胺中的任意一种或几种混合物。
作为优选的，所述水性流平剂为质量百分比为5％的silok-8255水性流平剂水溶液。
作为优选的，所述水性消泡剂为质量百分比为5％的silcolapse C546水性有机硅消泡剂水溶液。
一种水性电镀封闭剂的制备方法，包括以下步骤：
取二氧化碳基共聚物多元醇60份，脂肪族二异氰酸酯20-60份，亲水扩链剂3-6份，催化剂0.05-0.5份，升温至80-95℃，反应3-5h，降温到35℃左右，加入中和剂中和直至pH值达到7，加入KH-560 0.5-2份，搅拌反应1-2h，加入150-200份去离子水乳化，加入0.5-2份后扩链剂扩链，然后加入3-5份正硅酸己酯，加入氨水调节pH值至8-10，搅拌1-2h，加入1-5份的水性流平剂，1-5份的水性消泡剂，得到所述的水性电镀封闭剂。
作为优选的，所述中和剂为三乙胺三丙胺、三丁胺、氢氧化钠、氨水中的任意一种或几种的混合物。
与现有技术相比，本发明具有的有益效果为：
本发明提供一种具有高耐蚀的水性电镀封闭剂及其制备方法，所述的电镀封闭剂是以二氧化碳基共聚物多元醇为基础原料，通过有机-无机复合改性制备的水性乳液。本发明首次将二氧化碳共聚物多元醇用于电镀封闭剂，利用二氧化碳共聚物多元醇优良的隔氧性，大幅度提高镀层的耐蚀性；通过有机-无机复合，得到高硬度、高耐磨性的封闭剂。同时使用二氧化碳共聚物多元醇制备，克服聚醚多元醇制备的水性涂层硬度低，聚酯多元醇制备的水性涂层容易水解脱落的缺点，形成硬度与韧性结合的电镀封闭剂。
具体实施方式
下面结合具体实施例对本发明做进一步的详细说明，但不构成的对本发明的任何限制。
以下实施例1-5中，所得产品的检测方法的标准如下:电镀层附着力按GB/T9286-1998测试；耐盐雾实验按GB/T10125-2012测试；耐水实验按GB/T1733-93中的方法1测试。
实施例1。
取二氧化碳基共聚物多元醇60份，异佛尔酮二异氰酸酯25份，亲水扩链剂二羟甲基丙酸4.7份，辛酸亚锡0.1份，升温至80℃，反应3h，降温到35℃左右，加入三乙胺中和至pH值7左右，加入KH-560 1份，搅拌反应1-2h，加入200份去离子水乳化，加入1份乙二胺后扩链剂扩链，然后加入3份正硅酸己酯，加入氨水调节pH值至8-10，搅拌2h，加入5份的质量百分比为5％的silok-8255水性流平剂水溶液，5份的水性消泡剂，得到所述的水性电镀封闭剂。
实验测试得到该封闭剂与电镀层附着力为0级，耐盐雾实验144h，耐水实验168h，耐热水实验5h。
实施例2。
取二氧化碳基共聚物多元醇60份，二异氰酸酯20份，亲水扩链剂二羟甲基丙酸3份，催化剂0.2份，升温至80℃，反应5h，降温到35℃左右，加入中和剂中和至pH值7左右，加入KH-560 0.5份，搅拌反应1h，加入150份去离子水乳化，加入0.5份二乙烯三胺后扩链剂扩链，然后加入3份正硅酸己酯，加入氨水调节pH值至10，搅拌1h，加入1份的水性流平剂，1份的水性消泡剂，得到所述的水性电镀封闭剂。
实验测试得到该封闭剂与电镀层附着力为0级，耐盐雾实验168h，耐水实验240h，耐热水实验8h。
实施例3。
取二氧化碳基共聚物多元醇60份，氢化二苯基甲烷二异氰酸酯60份，亲水扩链剂二羟甲基丁酸6份，辛酸亚锡0.5份，升温至80℃，反应3h，降温到35℃左右，加入三乙胺中和至pH值7左右，加入KH-560 2份，搅拌反应2h，加入200份去离子水乳化，加入2份后扩链剂扩链，然后加入5份正硅酸己酯，加入氨水调节pH值至10，搅拌2h，加入5份的质量百分比为5％的silok-8255水性流平剂水溶液，5份的水性消泡剂，得到所述的水性电镀封闭剂。
实验测试得到该封闭剂与电镀层附着力为0级，耐盐雾实验96h，耐水实验168h，耐热水实验5h。
实施例4。
取二氧化碳基共聚物多元醇60份，异佛尔酮二异氰酸酯20份，六亚甲基二异氰酸酯5份，亲水扩链剂二羟甲基丙酸4.7份，辛酸亚锡0.2份，升温至90℃，反应4h，降温到35℃左右，加入氨水中和至pH值7左右，加入KH-560 1份，搅拌反应2h，加入180份去离子水乳化，加入1.5份后扩链剂扩链，然后加入4份正硅酸己酯，加入氨水调节pH值至8，搅拌2h，加入5份的质量百分比为5％的silok-8255水性流平剂水溶液，5份的水性消泡剂，得到所述的水性电镀封闭剂。
实验测试得到该封闭剂与电镀层附着力为0级，耐盐雾实验144h，耐水实验196h，耐热水实验6h。
实施例5。
取二氧化碳基共聚物多元醇60份，异佛尔酮二异氰酸酯25份，亲水扩链剂二羟甲基丙酸4.7份，辛酸亚锡0.1份，升温至90℃，反应4h，降温到35℃左右，加入三乙胺中和至pH值7左右，加入KH-560 1.5份，搅拌反应1-2h，加入150份去离子水乳化，加入1份后扩链剂扩链，然后加入3.5份正硅酸己酯，加入氨水调节pH值至8，搅拌2h，加入5份的质量百分比为5％的silok-8255水性流平剂水溶液，5份的水性消泡剂，得到所述的水性电镀封闭剂。
实验测试得到该封闭剂与电镀层附着力为0级，耐盐雾实验144h，耐水实验168h，耐热水实验5h。
本发明首次将二氧化碳共聚物多元醇用于电镀封闭剂，利用二氧化碳共聚物多元醇优良的隔氧性，大幅度提高镀层的耐蚀性；通过有机-无机复合，得到高硬度、高耐磨性的封闭剂。同时使用二氧化碳共聚物多元醇制备，克服聚醚多元醇制备的水性涂层硬度低，聚酯多元醇制备的水性涂层容易水解脱落的缺点，形成硬度与韧性结合的电镀封闭剂。
上述的实施例仅为本发明的优选实施例，不能以此来限定本发明的权利范围，因此，依本发明申请专利范围所作的等同变化，仍属本发明所涵盖的范围。
Claims (10)
1.一种具有高耐蚀的水性电镀封闭剂，其特征在于，包括以下重量份的组分：
2.根据权利要求1所述的具有高耐蚀的水性电镀封闭剂，其特征在于，包括以下重量份的组分：
3.根据权利要求1或2所述的具有高耐蚀的水性电镀封闭剂，其特征在于，所述二氧化碳基共聚物多元醇是以二氧化碳为起始原料，在引发剂、催化剂作用下与环氧丙烷共聚合成的二醇，其羟基官能度为2，分子量为2000-4000。
4.根据权利要求1或2所述的具有高耐蚀的水性电镀封闭剂，其特征在于，所述脂肪族二异氰酸酯是异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、氢化二苯基甲烷二异氰酸酯中的任意一种或几种的混合物。
5.根据权利要求1或2所述的具有高耐蚀的水性电镀封闭剂，其特征在于，所述亲水扩链剂为乙二胺基乙磺酸钠、1,4-丁二醇-2-2磺酸钠、二羟甲基丁酸、二羟甲基丙酸中的任意一种或几种混合物。
6.根据权利要求1或2所述的具有高耐蚀的水性电镀封闭剂，其特征在于，所述催化剂为辛酸亚锡、异辛酸亚锡、二月桂酸二丁基锡中的任意一种或几种混合物。
7.根据权利要求1或2所述的具有高耐蚀的水性电镀封闭剂，其特征在于，所述扩链剂为乙二胺、三甲基己二胺、四乙烯五胺、二乙烯三胺中的任意一种或几种混合物。
8.根据权利要求1或2所述的具有高耐蚀的水性电镀封闭剂，其特征在于，所述水性流平剂为质量百分比为5％的silok-8255水性流平剂水溶液，所述水性消泡剂为质量百分比为5％的silcolapse C546水性有机硅消泡剂水溶液。
9.一种水性电镀封闭剂的制备方法，其特征在于，包括以下步骤：
取二氧化碳共聚物多元醇60份，脂肪族二异氰酸酯20-60份，亲水扩链剂3-6份，催化剂0.05-0.5份，升温至80-95℃，反应3-5h，降温到35℃左右，加入中和剂中和直至pH值达到7，加入KH-560 0.5-2份，搅拌反应1-2h，加入150-200份去离子水乳化，加入0.5-2份后扩链剂扩链，然后加入3-5份正硅酸己酯，加入氨水调节pH值至8-10，搅拌1-2h，加入1-5份的水性流平剂，1-5份的水性消泡剂，得到所述的水性电镀封闭剂。
10.根据权利要求9所述的水性电镀封闭剂的制备方法，其特征在于，所述中和剂为三乙胺三丙胺、三丁胺、氢氧化钠、氨水中的任意一种或几种的混合物。
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