CN109957299B - 一种光固化水性丙烯酸阴极电泳涂料 - Google Patents
一种光固化水性丙烯酸阴极电泳涂料 Download PDFInfo
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- CN109957299B CN109957299B CN201910302157.2A CN201910302157A CN109957299B CN 109957299 B CN109957299 B CN 109957299B CN 201910302157 A CN201910302157 A CN 201910302157A CN 109957299 B CN109957299 B CN 109957299B
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- 238000000576 coating method Methods 0.000 title claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 67
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 30
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 24
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
本发明涉及一种光固化水性丙烯酸阴极电泳涂料的组成及制备方法。所述电泳涂料的基体树脂结构中含有苄基酯结构，所述苄基酯结构由丙烯酸苄酯提供，此光敏性水性丙烯酸树脂可以通过紫外光照射进行辐射固化，相比于传统的热固化，此方法更加节能环保快速，同时涂层可以应用于热敏性基材。制备的涂层兼具一定的防腐性以及装饰性，可应用于饰品、家电、五金等轻防腐以及装饰领域。
Description
技术领域
本发明涉及涂料领域，具体涉及一种光固化水性丙烯酸阴极电泳涂料及其制备方法。
背景技术
阴极电泳涂装是一种特殊的涂装方法，是利用外加电场，使水性涂料中的树脂和颜填料等微粒定向迁移并沉积于阴极的基底表面成膜。相比于其它涂装方式，例如滚涂、喷涂、浸涂，阴极电泳涂装具有涂料利用率高、自动化程度高和漆膜耐腐蚀性优良等优势，还能避免阳极电泳存在的阳极溶解缺陷，更加符合涂料绿色环保的趋势。
为了解决应用过程中出现的问题以及满足不同领域对涂料的不同要求，电泳涂料的种类逐渐丰富。目前按照基体树脂分类，可分为环氧电泳涂料、丙烯酸电泳涂料、聚氨酯电泳涂料等。其中丙烯酸树脂漆具有优异的光泽度及抗户外老化性，在近几十年的发展中，丙烯酸树脂涂料的总产量占据合成树脂涂料的第二位。但在水性电泳涂料的应用过程中，一些问题也相应显现出来，比如涂层与基材的粘附力不佳，树脂的泳透力不佳，高体积收缩产生内应力导致涂层遭到破坏而失去保护基材的作用；同时传统的电泳漆采用热固化，其固化温度高、固化时间长。因此，合成一种新型树脂并且采用其他固化方式以有效解决以上问题是研究和应用的热点。
紫外光固化是辐射固化的一种，是一种环境友好型固化方式，能够大幅度降低固化能耗，能源利用率高，可以适用于热敏基材，具有无污染、固化速度快、涂膜质量高及适合连续化大生产等优点。光固化技术能够解决传统热固化的高能耗和污染的问题。
丙烯酸类电泳涂料常常用作面漆，用于对被涂覆物的装饰。随着行业的发展，单一的修饰作用已经无法满足多样化的应用领域，高性能型涂层成为电泳发展趋势之一。经对现有科技文献的检索发现，为了提高漆膜性能，宫晟东等制备了有机硅改性环氧丙烯酸阴极电泳涂料，漆膜耐酸碱性优异(涂料工业,2013,43(07):52-56)；陈峰等在环氧丙烯酸阳离子树脂中引入氟离子，提高了涂层的耐老化、耐盐水和耐冲击性，但是其采用的是传统的热固化，限制了涂层在热敏性基材上的应用(材料保护,2018,51(01):76-78)；殷妹等制备了一种含有长烷基侧链的丙烯酸酯电泳涂料，耐水性能优异，但是附着力欠佳(中国发明专利，申请号201710936519.4)。因此，为了满足多样化的领域要求，可UV光固化的高性能丙烯酸阴极电泳涂料的研发与制备是十分必要的。
发明内容
为了克服现有技术的不足，本发明的目的在于提供一种高性能的光固化水性丙烯酸阴极电泳涂料。采用的固化方式为光固化，符合绿色、环保、节能的趋势。
本发明的目的是通过以下技术方案实现的。
一种光固化水性丙烯酸阴极电泳涂料，该丙烯酸阴极电泳涂料树脂结构中侧链含有苄基酯结构。
该涂料是由以下方法制备得到的：
步骤(1)：由含苄基的丙烯酸酯单体，含亲水基团的丙烯酸酯单体，含有羟基的丙烯酸酯单体以及其他常用单体在自由基引发剂作用下聚合制得水性丙烯酸酯树脂，树脂中含羟基官能团；再将水性丙烯酸酯树脂与甲基丙烯酸异氰基乙酯在催化剂和阻聚剂的作用下反应，引入光固化所需的双键，制得光敏性水性丙烯酸酯树脂，反应式如下：
步骤(2)：在光敏性水性丙烯酸酯树脂中加入溶剂、中和酸以及光引发剂，加入去离子水乳化制得光固化水性丙烯酸阴极电泳涂料。
上述步骤(1)中，含苄基的丙烯酸酯单体10wt％-40wt％(优选范围：20wt％-30wt％)，含亲水基团的丙烯酸酯单体5wt％-20wt％(优选范围：10wt％-15wt％)，含有羟基的丙烯酸酯单体15wt％-25wt％(优选范围：20wt％-25wt％)。具体地说，步骤(1)中所述含苄基的丙烯酸酯单体为丙烯酸苄酯、甲基丙烯酸苄酯和2-丙基丙烯酸苄酯中的一种或多种；所述含亲水基团的丙烯酸酯单体为含叔胺亲水官能团的丙烯酸酯单体或含羧基亲水官能团的丙烯酸酯单体，其中，所述含叔胺亲水官能团的甲基丙烯酸酯单体包括甲基丙烯酸二甲氨基乙酯、甲基丙烯酸酯-2-(二乙氨基)乙酯和3-(二甲氨基)2,2-二甲基丙烯酸酯中的一种或多种，所述含羧基亲水官能团的丙烯酸酯单体包括甲基丙烯酸、乙基丙烯酸酯和琥珀酸单(2-丙烯酰氧代乙酯)中的一种或多种。
步骤(1)中所述含有羟基的丙烯酸酯单体包含(甲基)丙烯酸-2-羟基乙酯、(甲基)丙烯酸-3-羟基丙酯中的一种或多种；所述其他常用单体为本领域常用的可聚合单体，具体可以是苯乙烯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、丙烯酸丁酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸异冰片酯、丙烯酸异丙酯中的一种或多种。
步骤(1)中所述自由基引发剂含偶氮二异丁腈、偶氮二异庚腈、过氧化二苯甲酰、叔丁基过氧化氢中的一种或多种；所述催化剂含二月桂酸二丁基锡、三乙烯二胺、四丁基硫酸氢胺、四丁基溴化胺、三乙基苄基氯化胺的一种或多种；所述阻聚剂为对苯二酚、对苯醌、2,6-二叔丁基对甲苯酚、对叔丁基邻苯二酚中的一种或多种。
步骤(2)中，所述光固化水性丙烯酸阴极电泳涂料由以下各重量份组分制备而成：
所述溶剂为丙二醇甲醚醋酸酯、乙二醇单丁醚、乙酸乙酯、丙二醇甲醚、甲醇、甲基异丁基酮、甲基乙基酮、环己酮中的一种或多种。
所述光引发剂为2-羟基-2-甲基苯丙酮、1-羟基环己基苯基甲酮、2,4,6-三甲基苯甲酰基-二苯基氧化膦、二苯甲酮、邻苯甲酰苯甲酸甲酯中的一种或多种。
所述中和酸为甲酸、冰醋酸、乳酸、烷基磺酸中的一种或多种。
此外，本发明还包括一种光固化水性丙烯酸阴极电泳涂料的制备方法，如下：
步骤(1)：将含苄基的丙烯酸酯单体，含亲水基团的丙烯酸酯单体，含有羟基的丙烯酸酯单体、自由基引发剂以及其他常用单体混合，采用滴加的方式，滴加2-4小时，在65-80℃下反应6-15小时制得水性丙烯酸酯树脂；再将水性丙烯酸酯树脂与甲基丙烯酸异氰基乙酯在催化剂和阻聚剂的作用下50-60℃反应3-5小时，引入光固化所需官能团，制得光敏性水性丙烯酸酯树脂；
步骤(2)：在光敏性水性丙烯酸酯树脂中加入适量中和酸以及光引发剂，加入去离子水乳化制得光固化水性丙烯酸阴极电泳涂料，固含量为10-20％。
本发明的技术方案还包括一种电泳涂料的用途，该电泳涂料可以用于饰品、家电、五金等轻防腐以及装饰领域。
本发明有益的技术效果在于：水性丙烯酸酯合成单体中引入含苄基的丙烯酸酯单体，能够降低树脂的粘度，提高涂层的硬度和粘附力，同时提高涂层防腐性能；采用阴极电泳方式制备涂层，相比于其他涂装方式，所制备的涂层更加致密平整；采用光固化，固化速率快，节能环保。
附图说明
图1为实施例1-3、比较例制备的丙烯酸电泳涂层的电化学阻抗测试结果。
具体实施方式
实施例1
(1)首先将8.5g甲基丙烯酸苄酯、10g甲基丙烯酸甲酯、11.4g甲基丙烯酸丁酯、5.8g甲基丙烯酸二甲氨基乙酯、11.6g丙烯酸羟乙酯和0.95g偶氮二异丁腈混合，再采用滴加的方式加入到30g丙二醇甲醚醋酸酯中，滴加3小时，然后在70℃下进行自由基溶液聚合，反应12小时直至单体反应完全；随后将反应体系温度调至50℃，加入12.4g甲基丙烯酸异氰基乙酯，以二月桂酸二丁基锡为催化剂，以2,6-二叔丁基-4-甲基苯酚为阻聚剂，反应4小时，直至体系中的-NCO完全反应,得到光敏性水性丙烯酸酯树脂。
(2)以步骤(1)中制备的光敏性水性丙烯酸酯树脂为基体树脂55g，加入1.65mL乙酸，保温1小时；再加入1173光引发剂2g、400g去离子水，高速搅拌乳化制得光固化水性丙烯酸阴极电泳涂料。
实施例2
(1)首先将15.08g甲基丙烯酸苄酯、10g甲基丙烯酸甲酯、11.4g甲基丙烯酸丁酯、5.8g甲基丙烯酸二甲氨基乙酯、11.6g丙烯酸羟乙酯和0.95g偶氮二异丁腈混合，再采用滴加的方式加入到36g丙二醇甲醚醋酸酯中，然后在70℃下进行自由基溶液聚合，反应12小时直至单体反应完全；随后将反应体系温度调至50℃，加入12.4g甲基丙烯酸异氰基乙酯，以二月桂酸二丁基锡为催化剂，以2,6-二叔丁基-4-甲基苯酚为阻聚剂，反应4小时，直至体系中的-NCO完全反应，得到光敏性水性丙烯酸酯树脂。
(2)以步骤(1)中制备的光敏性水性丙烯酸酯树脂为基体树脂，加入1.65mL乙酸，保温1小时；再加入1173光引发剂，450g去离子水，高速搅拌乳化制得光固化水性丙烯酸阴极电泳涂料。
实施例3
(1)首先将23.78g甲基丙烯酸苄酯、10g甲基丙烯酸甲酯、11.4g甲基丙烯酸丁酯、5.8g甲基丙烯酸二甲氨基乙酯、11.6g丙烯酸羟乙酯和0.95g偶氮二异丁腈混合，再采用滴加的方式加入到36g丙二醇甲醚醋酸酯中，然后在70℃下进行自由基溶液聚合，反应12小时直至单体反应完全；随后将反应体系温度调至50℃，加入12.4g甲基丙烯酸异氰基乙酯，以二月桂酸二丁基锡为催化剂，以2,6-二叔丁基-4-甲基苯酚为阻聚剂，反应4小时，直至体系中的-NCO完全反应,得到光敏性水性丙烯酸酯树脂。
(2)以步骤(1)中制备的光敏性水性丙烯酸酯树脂为基体树脂，加入1.65mL乙酸，保温1小时；再加入1173光引发剂，520g去离子水，高速搅拌乳化制得光固化水性丙烯酸阴极电泳涂料。
实施例4
(1)首先将15.08g甲基丙烯酸苄酯、10g甲基丙烯酸甲酯、11.4g甲基丙烯酸丁酯、5.8g甲基丙烯酸二甲氨基乙酯、11.6g丙烯酸羟乙酯和0.95g偶氮二异丁腈混合，再采用滴加的方式加入到36g丙二醇甲醚醋酸酯中，然后在70℃下进行自由基溶液聚合，反应12小时直至单体反应完全；随后将反应体系温度调至50℃，加入12.4g甲基丙烯酸异氰基乙酯，以二月桂酸二丁基锡为催化剂，以2,6-二叔丁基-4-甲基苯酚为阻聚剂，反应4小时，直至体系中的-NCO完全反应,得到光敏性水性丙烯酸酯树脂。
(2)以步骤(1)中制备的光敏性水性丙烯酸酯树脂为基体树脂，加入1.65mL乙酸，保温1小时；再加入1173光引发剂，270g去离子水，高速搅拌乳化制得光固化水性丙烯酸阴极电泳涂料。
实施例5
(1)首先将15.08g甲基丙烯酸苄酯、10g甲基丙烯酸甲酯、11.4g甲基丙烯酸丁酯、5.8g甲基丙烯酸二甲氨基乙酯、11.6g丙烯酸羟乙酯和0.95g偶氮二异丁腈混合，再采用滴加的方式加入到36g丙二醇甲醚醋酸酯中，然后在70℃下进行自由基溶液聚合，反应12小时直至单体反应完全；随后将反应体系温度调至50℃，加入12.4g甲基丙烯酸异氰基乙酯，以二月桂酸二丁基锡为催化剂，以2,6-二叔丁基-4-甲基苯酚为阻聚剂，反应4小时，直至体系中的-NCO完全反应,得到光敏性水性丙烯酸酯树脂。
(2)以步骤(1)中制备的光敏性水性丙烯酸酯树脂为基体树脂，加入1.65mL乙酸，保温1小时；再加入1173光引发剂，180g去离子水，高速搅拌乳化制得光固化水性丙烯酸阴极电泳涂料。
实施例6
(1)首先将15.08g甲基丙烯酸苄酯、10g甲基丙烯酸甲酯、11.4g甲基丙烯酸丁酯、5.8g甲基丙烯酸二甲氨基乙酯、11.6g丙烯酸羟乙酯和0.95g偶氮二异丁腈混合，再采用滴加的方式加入到36g丙二醇甲醚醋酸酯中，然后在70℃下进行自由基溶液聚合，反应12小时直至单体反应完全；随后将反应体系温度调至50℃，加入12.4g甲基丙烯酸异氰基乙酯，以二月桂酸二丁基锡为催化剂，以2,6-二叔丁基-4-甲基苯酚为阻聚剂，反应4小时，直至体系中的-NCO完全反应,得到光敏性水性丙烯酸酯树脂。
(2)以步骤(1)中制备的光敏性水性丙烯酸酯树脂为基体树脂，加入1.65mL乙酸，保温1小时；再加入1173光引发剂，270g去离子水，高速搅拌乳化制得光固化水性丙烯酸阴极电泳涂料。
比较例
(1)首先将10g甲基丙烯酸甲酯、11.4g甲基丙烯酸丁酯、5.8g甲基丙烯酸二甲氨基乙酯、11.6g丙烯酸羟乙酯和0.95g偶氮二异丁腈混合，再采用滴加的方式加入到30g丙二醇甲醚醋酸酯中，然后在70℃下进行自由基溶液聚合，反应12小时直至单体反应完全；随后将反应体系温度调至50℃，加入12.4g甲基丙烯酸异氰基乙酯，以二月桂酸二丁基锡为催化剂，以2,6-二叔丁基-4-甲基苯酚为阻聚剂，反应4小时，直至体系中的-NCO完全反应,得到光敏性水性丙烯酸酯树脂。
(2)以步骤(1)中制备的光敏性水性丙烯酸酯树脂为基体树脂，加入1.65mL乙酸，保温1小时；再加入1173光引发剂、450g去离子水，高速搅拌乳化制得光固化水性丙烯酸阴极电泳涂料。
实施例的实施效果：
图1为实施例1～3、比较例制备的丙烯酸电泳涂层的电化学阻抗测试结果。可以看出，水性丙烯酸树脂结构中的甲基丙烯酸苄酯含量不同，所制备的涂层的电化学阻抗不同，当甲基丙烯酸苄酯含量在25-30wt％时，所得涂层的防腐蚀性能最好。
表1是实施例1～3、比较例制备的丙烯酸电泳涂层的基本性质比较。可以看出，与未添加甲基丙烯酸苄酯的涂层(比较例)对比，本发明的涂层(实施例1～3)表面光滑平整，硬度高，粘附力强，耐水性、耐酸碱性都有较大提高。
表1
Claims (6)
1.一种光固化水性丙烯酸阴极电泳涂料，该丙烯酸阴极电泳涂料树脂结构中侧链含有苄基酯结构；
该涂料是由以下方法制备得到的：
步骤(1)：由含苄基的丙烯酸酯单体，含亲水基团的丙烯酸酯单体，含有羟基的丙烯酸酯单体以及其他常用单体在自由基引发剂作用下聚合制得水性丙烯酸酯树脂，树脂中含羟基官能团；再将水性丙烯酸酯树脂与甲基丙烯酸异氰基乙酯在催化剂和阻聚剂的作用下反应，引入光固化所需的双键，制得光敏性水性丙烯酸酯树脂；
步骤(2)：在光敏性水性丙烯酸酯树脂中加入溶剂、中和酸以及光引发剂，加入去离子水乳化制得光固化水性丙烯酸阴极电泳涂料；
上述步骤(1)中，含苄基的丙烯酸酯单体20wt％-30wt％，含亲水基团的丙烯酸酯单体5wt％-20wt％，含有羟基的丙烯酸酯单体15wt％-25wt％；所述含亲水基团的丙烯酸酯单体为含叔胺亲水官能团的丙烯酸酯单体；
所述光固化水性丙烯酸阴极电泳涂料由以下各重量份组分制备而成：
2.根据权利要求1所述的一种光固化水性丙烯酸阴极电泳涂料，其特征在于，步骤(1)中所述含苄基的丙烯酸酯单体为丙烯酸苄酯、甲基丙烯酸苄酯和2-丙基丙烯酸苄酯中的一种或多种；所述含叔胺亲水官能团的丙烯酸酯单体包括甲基丙烯酸二甲氨基乙酯、甲基丙烯酸酯-2-(二乙氨基)乙酯和3-(二甲氨基)2,2-二甲基丙烯酸酯中的一种或多种。
3.根据权利要求1所述的一种光固化水性丙烯酸阴极电泳涂料，其特征在于，步骤(1)中所述含有羟基的丙烯酸酯单体为(甲基)丙烯酸-2-羟基乙酯、(甲基)丙烯酸-3-羟基丙酯中的一种或多种；所述自由基引发剂为偶氮二异丁腈、偶氮二异庚腈、过氧化二苯甲酰、叔丁基过氧化氢中的一种或多种；所述催化剂为二月桂酸二丁基锡、三乙烯二胺、四丁基硫酸氢铵、四丁基溴化铵、三乙基苄基氯化铵的一种或多种；所述阻聚剂为对苯二酚、对苯醌、2,6-二叔丁基对甲苯酚、对叔丁基邻苯二酚中的一种或多种。
4.根据权利要求1所述的一种光固化水性丙烯酸阴极电泳涂料，其特征在于，所述溶剂为丙二醇甲醚醋酸酯、乙二醇单丁醚、乙酸乙酯、丙二醇甲醚、甲醇、甲基异丁基酮、甲基乙基酮、环己酮中的一种或多种；所述光引发剂为2-羟基-2-甲基苯丙酮、1-羟基环己基苯基甲酮、2,4,6-三甲基苯甲酰基-二苯基氧化膦、二苯甲酮、邻苯甲酰苯甲酸甲酯中的一种或多种；所述中和酸为甲酸、冰醋酸、乳酸、烷基磺酸中的一种或多种。
5.一种根据权利要求1所述的一种光固化水性丙烯酸阴极电泳涂料的制备方法，其特征在于，该电泳涂料通过以下方法制得：
步骤(1)：将含苄基的丙烯酸酯单体，含亲水基团的丙烯酸酯单体，含有羟基的丙烯酸酯单体、自由基引发剂以及其他常用单体混合，采用滴加的方式，滴加2-4小时，在65-80℃下反应6-15小时制得水性丙烯酸酯树脂；再将水性丙烯酸酯树脂与甲基丙烯酸异氰基乙酯在催化剂和阻聚剂的作用下50-60℃反应3-5小时，引入光固化所需官能团，制得光敏性水性丙烯酸酯树脂；
步骤(2)：在光敏性水性丙烯酸酯树脂中加入适量溶剂、中和酸以及光引发剂，加入去离子水乳化制得光固化水性丙烯酸阴极电泳涂料，固含量为10-20wt％。
6.一种根据权利要求1所述的一种光固化水性丙烯酸阴极电泳涂料的用途，其特征在于，该电泳涂料可以用于饰品、家电、五金的轻防腐以及装饰领域。
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| "水性丙烯酸酯汽车涂料制备及其漆膜性能研究";包春磊等;《热固性树脂》;20080131;第23卷(第1期);第1.2和2.1.3节 * |
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