CN105949374A - 一种用于多彩涂料的改性硅丙水包水乳液的制备方法 - Google Patents

一种用于多彩涂料的改性硅丙水包水乳液的制备方法 Download PDF

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CN105949374A
CN105949374A CN201610512065.3A CN201610512065A CN105949374A CN 105949374 A CN105949374 A CN 105949374A CN 201610512065 A CN201610512065 A CN 201610512065A CN 105949374 A CN105949374 A CN 105949374A
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刘都宝
赵洪涛
陶杰
鲍俊杰
刘藏
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Anhui Zhong En Chemical Co Ltd
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Abstract

多彩涂料的改性硅丙水包水乳液的制备方法，是在反应容器中加入40～75份去离子水、1～3份十二烷基苯磺酸钠、1～5份OP‑10、30～50份丙烯酸酯单体、1～10份有机氟和5～20份有机硅单体，常温下高速分散得到单体预乳化液；在另一反应容器中加入5～15份去离子水、0.2～0.8份碳酸氢钠、0.2～0.5份过硫酸铵和10～30份单体预乳化液，升温至75～95℃，待乳液出现蓝光时保温30～60min，在2～4h内滴加完剩余的预乳化液和0.5～2.0质量份20%的过硫酸铵溶液，保温1～2h，降温至50℃以下，用调节pH 至8.0，过滤得到改性硅丙水包水乳液。本发明工艺简单，制备的改性硅丙水包水乳液具有高硬度、高附着力和优异的耐候、耐水性，可用于制备高性能的水包水多彩涂料。

Description

一种用于多彩涂料的改性硅丙水包水乳液的制备方法
技术领域
本发明属于油墨树脂技术领域，具体是一种用于多彩涂料的改性硅丙水包水乳液的制备方法。
背景技术
水包水多彩涂料是一种水性环保涂料，是为满足现今不断发展的建筑外墙涂料市场而诞生的。水包水多彩涂料是由改性树脂及稳定性好的颜料制成的，全水性、一次性喷涂的多彩花岗岩涂料，产生的色彩逼真、耐久，仿真程度可达到99%，是替代外墙花岗岩的最佳产品。在水包水多彩涂料中，作为连续相的成膜物质决定了多彩涂料的最终性能，例如耐水白、耐沾污、耐候性和附着力等，同时连续相用乳液与保护胶体系的配伍性对水包水多彩涂料的稳定性具有较大的影响。目前水包水多彩涂料连续相用乳液主要有纯丙乳液、苯丙乳液、硅丙乳液以及氟碳乳液等，其中硅丙乳液以其优异的性价比是目前使用最广泛的乳液。硅丙涂膜具有较好的耐候性和耐水性，但是，在水包水涂料中仍然普遍存在涂膜耐水白性不好的问题，需要使用高价格的氟碳树脂进行表面罩光。
发明内容
本发明的目的在于提供一种用于多彩涂料的改性硅丙水包水乳液的制备方法，制备工艺简单，制备的改性硅丙水包水乳液VOC含量低，具有高硬度、高附着力和优异的耐候、耐水性，可用于制备高性能的水包水多彩涂料。
为实现上述目的，本发明提供了一种用于多彩涂料的改性硅丙水包水乳液的制备方法，包括以下步骤：
（1）在反应容器中加入40～75质量份去离子水、1～3质量份十二烷基苯磺酸钠、1～5质量份非离子乳化剂、30～50质量份丙烯酸酯单体、1～10质量份有机氟和5～20质量份有机硅单体，在常温下高速分散 15～60 min，得到乳白色的单体预乳化液；
（2）在另一反应容器中加入5～15质量份去离子水、0.2～0.8 质量份碳酸氢钠、0.2～0.5质量份过硫酸铵和10～30 质量份单体预乳化液，升温至 75～95℃ ，待乳液出现蓝光时保温 30～60 min，然后在2～4 h 内滴加完剩余的预乳化液和0.5～2.0质量份质量分数为20%的过硫酸铵溶液，滴加完毕后保温 1～2 h，降温至 50 ℃以下，用氨水调节 pH 至8.0，过滤得到改性硅丙水包水乳液。
所述的非离子乳化剂是OP-10；所述的丙烯酸酯单体是丙烯酸甲酯、丙烯酸丁酯、丙烯酸-2-羟基乙酯或甲基丙烯酸；所述的有机氟是甲基丙烯酸十二氟庚酯、全(十三)氟辛基三乙氧基硅烷、十二氟庚基丙基甲基二甲氧基硅烷、甲基丙烯酸三氟乙酯、全氟烷基乙基丙烯酸酯或甲基丙烯酸六氟丁酯；所述的有机硅单体是γ-甲基丙烯酰氧基丙基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三乙氧基硅烷或γ-甲基丙烯酰氧基丙基三异丙氧基硅烷。
本发明工艺简单，制备的改性硅丙水包水乳液具有高硬度、高附着力、优异的耐候性和耐水性能等优点，可用于制备高性能的水包水多彩涂料。
具体实施方式
以下结合实施例进一步说明发明。
实施例1
用于多彩涂料的改性硅丙水包水乳液的制备方法，包括以下步骤：
（1）在烧瓶中45 g去离子水、1 g十二烷基苯磺酸钠、2 g OP-10、30 g丙烯酸甲酯、5 g甲基丙烯酸十二氟庚酯和10 g γ-甲基丙烯酰氧基丙基三甲氧基硅烷，在常温下高速分散15 min，得到乳白色的单体预乳化液；
（2）在另一烧瓶中加入5 g去离子水、0.3 g碳酸氢钠、0.2 g过硫酸铵和10 g单体预乳化液，升温至 75 ℃ ，待乳液出现蓝光时保温30 min，然后在2 h 内滴加完剩余的预乳化液和0.5g质量分数为20%的过硫酸铵溶液，滴加完毕后保温1 h，降温至 50 ℃以下，用氨水调节 pH 至8.0，过滤得到改性硅丙水包水乳液。
实施例2
用于多彩涂料的改性硅丙水包水乳液的制备方法，包括以下步骤：
（1）在烧瓶中加入75 g去离子水、3 g十二烷基苯磺酸钠、5 g OP-10、45 g丙烯酸丁酯、10 g全(十三)氟辛基三乙氧基硅烷和5g γ-甲基丙烯酰氧基丙基三乙氧基硅烷，在常温下高速分散60 min，得到乳白色的单体预乳化液；
（2）在另一烧瓶中加入15 g去离子水、0.8 g碳酸氢钠、0.3 g过硫酸铵和30 g单体预乳化液，升温至 95℃ ，待乳液出现蓝光时保温 60 min，然后在4 h 内滴加完剩余的预乳化液和2.0 g质量分数为20%的过硫酸铵溶液，滴加完毕后保温 2 h，降温至 50 ℃以下，用氨水调节 pH 至8.0，过滤得到改性硅丙水包水乳液。
实施例3
用于多彩涂料的改性硅丙水包水乳液的制备方法，包括以下步骤：
（1）在烧瓶中加入60 g去离子水、2 g十二烷基苯磺酸钠、5 g OP-10、40 g丙烯酸丁酯、1 g十二氟庚基丙基甲基二甲氧基硅烷和20 g γ-甲基丙烯酰氧基丙基三乙氧基硅烷，在常温下高速分散30 min，得到乳白色的单体预乳化液；
（2）在另一烧瓶中加入12 g去离子水、0.5 g碳酸氢钠、0.5 g过硫酸铵和20 g单体预乳化液，升温至 80℃ ，待乳液出现蓝光时保温45 min，然后在2.5 h 内滴加完剩余的预乳化液和1.2 g质量分数为20%的过硫酸铵溶液，滴加完毕后保温1.5h，降温至 50 ℃以下，用氨水调节 pH 至8.0，过滤得到改性硅丙水包水乳液。
实施例4
用于多彩涂料的改性硅丙水包水乳液的制备方法，包括以下步骤：
（1）在烧瓶中加入50 g去离子水、2 g十二烷基苯磺酸钠、3 g OP-10、35 g丙烯酸-2-羟基乙酯、8 g全氟烷基乙基丙烯酸酯和12 g γ-甲基丙烯酰氧基丙基三异丙氧基硅烷，在常温下高速分散40 min，得到乳白色的单体预乳化液；
（2）在另一烧瓶中加入10 g去离子水、0.3 g碳酸氢钠、0.4 g过硫酸铵和18 g单体预乳化液，升温至 90℃ ，待乳液出现蓝光时保温 35 min，然后在2 h 内滴加完剩余的预乳化液和0.8 g质量分数为20%的过硫酸铵溶液，滴加完毕后保温1h，降温至 50 ℃以下，用氨水调节 pH 至8.0，过滤得到改性硅丙水包水乳液。
实施例5
用于多彩涂料的改性硅丙水包水乳液的制备方法，包括以下步骤：
（1）在烧瓶中加入48 g去离子水、2.4 g十二烷基苯磺酸钠、2.5 g OP-10、30 g甲基丙烯酸、5 g甲基丙烯酸六氟丁酯和12 g γ-甲基丙烯酰氧基丙基三异丙氧基硅烷，在常温下高速分散 45 min，得到乳白色的单体预乳化液；
（2）在另一烧瓶中加入10 g去离子水、0.2 g碳酸氢钠、0.3 g过硫酸铵和12 g单体预乳化液，升温至 80 ℃ ，待乳液出现蓝光时保温35 min，然后在2.5 h 内滴加完剩余的预乳化液和0.5 g质量分数为20%的过硫酸铵溶液，滴加完毕后保温 1 h，降温至 50 ℃以下，用氨水调节 pH 至8.0，过滤得到改性硅丙水包水乳液。
实施例6
用于多彩涂料的改性硅丙水包水乳液的制备方法，包括以下步骤：
（1）在烧瓶中加入40 g去离子水、1 g十二烷基苯磺酸钠、2 g OP-10、30 g丙烯酸甲酯、4 g甲基丙烯酸三氟乙酯和15 g γ-甲基丙烯酰氧基丙基三乙氧基硅烷，在常温下高速分散45 min，得到乳白色的单体预乳化液；
（2）在另一烧瓶中加入12 g去离子水、0.3 g碳酸氢钠、0.2 g过硫酸铵和10 g单体预乳化液，升温至 80℃ ，待乳液出现蓝光时保温30 min，然后在3 h 内滴加完剩余的预乳化液和1.5 g质量分数为20%的过硫酸铵溶液，滴加完毕后保温 1.5 h，降温至 50 ℃以下，用氨水调节 pH 至8.0，过滤得到改性硅丙水包水乳液。
对实施例1～6制备的改性硅丙水包水乳液及这些改性硅丙水包水乳液涂膜相关性能进行测试，测试结果如下表所示：
实施例 硬度/HR 附着力/级 耐水性/（浸泡7天） 耐人工老化性/2000 h
1 3 2 无异常 不起泡、不剥落、无裂纹
2 4 3 无异常 不起泡、不剥落、局部裂纹
3 6 1 无异常 不起泡、不剥落、无裂纹
4 7 1 无异常 不起泡、不剥落、无裂纹
5 5 1 无异常 不起泡、不剥落、无裂纹
6 3 2-3 无异常 不起泡、不剥落、无裂纹
由上可知，本发明制备的硅丙水包水乳液具有较高的硬度、较好的附着力、优异的耐水性能和耐候性，可提高涂料的综合性能，用于制备高性能的多彩涂料。

Claims (2)

1.一种用于多彩涂料的改性硅丙水包水乳液的制备方法，其特征在于，包括以下步骤：
（1）在反应容器中加入40～75质量份去离子水、1～3质量份十二烷基苯磺酸钠、1～5质量份非离子乳化剂、30～50质量份丙烯酸酯单体、1～10质量份有机氟和5～20质量份有机硅单体，在常温下高速分散 15～60 min，得到乳白色的单体预乳化液；
（2）在另一反应容器中加入5～15质量份去离子水、0.2～0.8 质量份碳酸氢钠、0.2～0.5质量份过硫酸铵和10～30 质量份单体预乳化液，升温至 75～95℃ ，待乳液出现蓝光时保温 30～60 min，然后在2～4 h 内滴加完剩余的预乳化液和0.5～2.0质量份质量分数为20%的过硫酸铵溶液，滴加完毕后保温 1～2 h，降温至 50 ℃以下，用氨水调节 pH 至8.0，过滤得到改性硅丙水包水乳液。
2.根据权利要求1所述的用于多彩涂料的改性硅丙水包水乳液的制备方法，其特征在于：所述的非离子乳化剂是OP-10；所述的丙烯酸酯单体是丙烯酸甲酯、丙烯酸丁酯、丙烯酸-2-羟基乙酯或甲基丙烯酸；所述的有机氟是甲基丙烯酸十二氟庚酯、全(十三)氟辛基三乙氧基硅烷、十二氟庚基丙基甲基二甲氧基硅烷、甲基丙烯酸三氟乙酯、全氟烷基乙基丙烯酸酯或甲基丙烯酸六氟丁酯；所述的有机硅单体是γ-甲基丙烯酰氧基丙基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三乙氧基硅烷或γ-甲基丙烯酰氧基丙基三异丙氧基硅烷。
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