CN117447887A - 一种有机玻璃用氟硅改性丙烯酸树脂涂料及其制备和使用方法 - Google Patents
一种有机玻璃用氟硅改性丙烯酸树脂涂料及其制备和使用方法 Download PDFInfo
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Abstract
本发明公开了一种有机玻璃用氟硅改性丙烯酸树脂涂料及其制备和使用方法,由由20‑30%改性丙烯酸树脂,10‑20%3390固化剂,30‑50%醋酸丁酯,10‑30%二甲苯组成,其中改性丙烯酸树脂由20‑30%甲基丙烯酸甲酯,10‑20%季戊四醇三丙烯酸酯,10‑15%甲基丙烯酸六氟丁酯,1‑3%羟基硅油,0.5‑1%甲基丙烯酸,30‑40%醋酸丁酯,15‑20%二甲苯,0.5‑2%过氧化苯甲酰组成。本发明制备的涂料涂覆在有机玻璃基材上,漆膜具备较强的附着力以及足够的硬度,极大拓展了丙烯酸树脂涂料的应用范围与发展空间,而且制备工艺安全环保,漆膜固化较快,极大提升了工作效率。
Description
技术领域
本发明涉及涂料领域,具体为一种有机玻璃用氟硅改性丙烯酸树脂涂料及其制备和使用方法。
背景技术
丙烯酸树脂涂料能够占据一定的市场份额并应用于多个军民行业中,得益于其适用于涂覆包括有机玻璃在内的多种基材。但常规丙烯酸树脂涂料涂覆有机玻璃基材时也存在以下几个典型缺陷:
1.丙烯酸树脂涂料成膜温度要求较高,但绝大部分有机玻璃基材不能长时间暴露于高温环境中,这就导致涂覆时不得不采用相对低温但长时间的固化工艺,降低了工作效率;
2.有机玻璃基材自身是状态相当稳定的高分子树脂且表面十分光滑,这就导致丙烯酸树脂涂料漆膜在有机玻璃基材上的附着力较差;
3.丙烯酸树脂的自身结构导致涂料漆膜硬度不足。
目前尚无很好的方法解决上述问题,主要还是以向体系中加入各类附着力促进剂、表面改性剂等助剂。但这不仅增加了成本,也或多或少影响了涂料的整体性能,治标不治本。
发明内容
本发明提供了一种有机玻璃用氟硅改性丙烯酸树脂涂料,将氟元素与硅氧键接入丙烯酸树脂中,该涂料涂覆在有机玻璃基材上,漆膜具备较强的附着力以及足够的硬度,极大拓展了丙烯酸树脂涂料的应用范围与发展空间,而且制备工艺安全环保,漆膜固化较快,极大提升了工作效率。
本发明的有机玻璃用氟硅改性丙烯酸树脂涂料各组分的质量含量以及制备方法:
本发明的有机玻璃用氟硅改性丙烯酸树脂涂料组分中改性丙烯酸树脂反应物各组分的质量含量以及制备方法:
所述羟基硅油为α,ω-二羟基封端聚二甲基硅氧烷
所述改性丙烯酸树脂制备方法为:
步骤1:羟基硅油预处理,将羟基硅油运用旋转蒸发器在减压0.08MPa以上、蒸馏温度(100±2)℃条件下除去水分与杂质备用;
步骤2:制备物料混合物,取所述量80%的甲基丙烯酸甲酯、80%的季戊四醇三丙烯酸酯、80%的甲基丙烯酸六氟丁酯、80%的甲基丙烯酸和所述量20%的醋酸丁酯、20%的二甲苯以及所述量70%的过氧化苯甲酰均匀混合成物料混合物;
步骤3:取所述量20%的甲基丙烯酸甲酯、20%的季戊四醇三丙烯酸酯、20%的甲基丙烯酸六氟丁酯、20%的甲基丙烯酸和所述量60%的醋酸丁酯、60%的二甲苯投入釜中加热搅拌并持续通氮气保护直至回流;
步骤4:步骤3体系在氮气保护条件下搅拌回流30min后,开始滴加步骤2制备的物料混合物,要求滴速均匀,滴加时间保持在60min~120min,滴加过程中继续保持氮气保护并搅拌回流;
步骤5:滴加完毕继续保持氮气保护并搅拌回流30min后,将所述量20%的醋酸丁酯和20%的二甲苯、所述量100%的羟基硅油、所述量30%的过氧化苯甲酰充分混合均匀滴加,滴加时间保持在60min~90min,滴加过程中继续保持氮气保护并搅拌回流;
步骤6:滴加完毕后继续保持氮气保护并搅拌回流共聚240min,随后降温出料,得到无色透明澄清树脂,及改性丙烯酸树脂。
所述有机玻璃用氟硅改性丙烯酸树脂涂料制备方法:
取所述量改性丙烯酸树脂、3390固化剂、醋酸丁酯、二甲苯加入烧杯,常温常压环境下搅拌混合均匀即可。搅拌会产生气泡,应待涂料中气泡数量较少或消失后再行使用。
所述有机玻璃用氟硅改性丙烯酸树脂涂料使用方法:
步骤1.使用醋酸丁酯或二甲苯对基材进行擦洗,使基材表面洁净并放至干燥;
步骤2.将有机玻璃用氟硅改性丙烯酸树脂涂料均匀喷覆或者淋涂于有机玻璃基材表面,涂覆量根据实际使用情况决定。然后将基材置于常温常压环境条件下静置30min待其表干;
步骤3.表干后将基材静置于60℃环境中进行热固化,固化时间不低于60min。
本发明的有益效果是:
1.本发明涂料正确涂覆在有机玻璃基材上具有相较常规丙烯酸树脂涂料更短的固化时间、更低的固化温度;同时漆膜具有常规丙烯酸树脂涂料不具备的优异附着力、优异硬度。
2.本发明涂料树脂在合成时均匀分散于回流溶剂中,温度变化范围较为固定不易发生爆聚、胶化现象;
3.本发明涂料树脂合成工艺安全、简单、环保、无色透明,全过程中整个体系均较为稳定且树脂反应充分,无明显有毒有害副产物;
4.本发明涂料树脂合成工艺所需实验仪器简单常见,受外界环境影响较小。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施方式,都属于本发明保护的范围。
实施例1
合成改性丙烯酸树脂:先将羟基硅油预处理;取所述量4g的甲基丙烯酸甲酯、4g的季戊四醇三丙烯酸酯、2g的甲基丙烯酸六氟丁酯、0.2g的甲基丙烯酸和18g的醋酸丁酯、9g的二甲苯投入釜中加热搅拌并持续通氮气保护直至回流;体系在氮气保护条件下搅拌回流30min后,开始滴加物料混合物,保持滴速均匀,滴加时间60min,滴加过程中继续保持氮气保护并搅拌回流。该物料混合物由16g的甲基丙烯酸甲酯、16g的季戊四醇三丙烯酸酯、8g的甲基丙烯酸六氟丁酯、0.8g的甲基丙烯酸和6g的醋酸丁酯、3g的二甲苯以及1.4g的过氧化苯甲酰均匀混合组成;滴加完毕继续保持氮气保护并搅拌回流30min后,将剩余6g的醋酸丁酯和3g的二甲苯、全部2g的羟基硅油、0.6g的过氧化苯甲酰充分混合均匀滴加,滴加时间90min,滴加过程中继续保持氮气保护并搅拌回流;滴加完毕后继续保持氮气保护并搅拌回流共聚240min,随后降温出料,得到无色透明澄清树脂。
配制有机玻璃用氟硅改性丙烯酸树脂涂料:将20g改性丙烯酸树脂、10g的3390固化剂、30g的醋酸丁酯、10g的二甲苯在常温常压环境下搅拌混合均匀得到有机玻璃用氟硅改性丙烯酸树脂涂料。
涂料使用:先使用醋酸丁酯或二甲苯对基材进行擦洗,使基材表面洁净并放至干燥;将有机玻璃用氟硅改性丙烯酸树脂涂料淋涂于有机玻璃基材,然后将样板置于常温常压通风条件下静置30min后,再将样板放入60℃恒温烘箱中进行进一步热固化80min后,取出样板降温至室温后待测。
实施例2
合成改性丙烯酸树脂:先将羟基硅油预处理;取所述量60g的甲基丙烯酸甲酯、20g的季戊四醇三丙烯酸酯、20g的甲基丙烯酸六氟丁酯、2g的甲基丙烯酸和180g的醋酸丁酯、96g的二甲苯投入釜中加热搅拌并持续通氮气保护直至回流;体系在氮气保护条件下搅拌回流30min后,开始滴加物料混合物,保持滴速均匀,滴加时间60min,滴加过程中继续保持氮气保护并搅拌回流。该物料混合物由240g的甲基丙烯酸甲酯、80g的季戊四醇三丙烯酸酯、80g的甲基丙烯酸六氟丁酯、8g的甲基丙烯酸和60g的醋酸丁酯、32g的二甲苯以及7g的过氧化苯甲酰均匀混合组成;滴加完毕继续保持氮气保护并搅拌回流30min后,将剩余60g的醋酸丁酯和32g的二甲苯、全部20g的羟基硅油、3g的过氧化苯甲酰充分混合均匀滴加,滴加时间90min,滴加过程中继续保持氮气保护并搅拌回流;滴加完毕后继续保持氮气保护并搅拌回流共聚240min,随后降温出料,得到无色透明澄清树脂。
配制有机玻璃用氟硅改性丙烯酸树脂涂料:将30g改性丙烯酸树脂、20g的3390固化剂、50g的醋酸丁酯、30g的二甲苯在常温常压环境下搅拌混合均匀得到有机玻璃用氟硅改性丙烯酸树脂涂料。
涂料使用:先使用醋酸丁酯或二甲苯对基材进行擦洗,使基材表面洁净并放至干燥;将有机玻璃用氟硅改性丙烯酸树脂涂料喷涂于有机玻璃基材,然后将样板置于常温常压通风条件下静置30min后,再将样板放入60℃恒温烘箱中进行进一步热固化60min后,取出样板降温至室温后待测。
实施例3
合成改性丙烯酸树脂:先将羟基硅油预处理;取所述量12g的甲基丙烯酸甲酯、6g的季戊四醇三丙烯酸酯、9g的甲基丙烯酸六氟丁酯、0.3g的甲基丙烯酸和54g的醋酸丁酯、36g的二甲苯投入釜中加热搅拌并持续通氮气保护直至回流;体系在氮气保护条件下搅拌回流30min后,开始滴加物料混合物,保持滴速均匀,滴加时间60min,滴加过程中继续保持氮气保护并搅拌回流。该物料混合物由48g的甲基丙烯酸甲酯、24g的季戊四醇三丙烯酸酯、36g的甲基丙烯酸六氟丁酯、1.2g的甲基丙烯酸和18g的醋酸丁酯、12g的二甲苯以及4.2g的过氧化苯甲酰均匀混合组成;滴加完毕继续保持氮气保护并搅拌回流30min后,将剩余18g的醋酸丁酯和12g的二甲苯、全部7.5g的羟基硅油、1.8g的过氧化苯甲酰充分混合均匀滴加,滴加时间90min,滴加过程中继续保持氮气保护并搅拌回流;滴加完毕后继续保持氮气保护并搅拌回流共聚240min,随后降温出料,得到无色透明澄清树脂。
配制有机玻璃用氟硅改性丙烯酸树脂涂料:将20g改性丙烯酸树脂、20g的3390固化剂、30g的醋酸丁酯、30g的二甲苯在常温常压环境下搅拌混合均匀得到有机玻璃用氟硅改性丙烯酸树脂涂料。
涂料使用:先使用醋酸丁酯或二甲苯对基材进行擦洗,使基材表面洁净并放至干燥;将有机玻璃用氟硅改性丙烯酸树脂涂料喷涂于有机玻璃基材,然后将样板置于常温常压通风条件下静置30min后,再将样板放入60℃恒温烘箱中进行进一步热固化60min后,取出样板降温至室温后待测。
对比例1
合成丙烯酸树脂:称取100g甲基丙烯酸甲酯、5g过氧化苯甲酰,随后投入锥形瓶中水浴90℃加热并保持温度。注意观察引发剂是否完全分解,必须时刻监控整个反应过程,体系会在不定时间突然变得粘稠,易局部受热不均导致焦化等。待整体粘稠则降温出料。
配制涂料:将30g树脂、10g的3390固化剂和20g醋酸丁酯常温常压环境下搅拌混合均匀得到涂料。
使用配制得到的涂料对有机玻璃板材进行淋涂试验。将涂料淋涂于有机玻璃基材表面,然后将样板置于常温常压通风条件下静置3小时后,再将样板放入80℃烘箱中进行进一步热固化3小时后,取出样板降温至室温后待测。
依据国家标准《GB/T 1728-2020漆膜、腻子膜干燥时间测定法》、《GB/T 6739-2006色漆和清漆铅笔法测定漆膜硬度》和《GB/T 9286-2021色漆和清漆划格试验》对涂层的附着力和硬度进行测试,测试结果如下:
由实施例与对比例可以看出:本发明制备的有机玻璃用氟硅改性丙烯酸树脂涂料无色澄清透明,制备工艺安全、简单、环保,无明显有毒有害副产物,涂覆在有机玻璃基材上具有相较常规丙烯酸树脂涂料更短的固化时间、更低的固化温度,漆膜具有常规丙烯酸树脂涂料不具备的优异附着力和硬度,极大拓展了丙烯酸树脂涂料的应用范围与发展空间。
本公开已由上述相关实施例加以描述,然而上述实施例仅为实施本公开的范例。必需指出的是,已揭露的实施例并未限制本公开的范围。相反,在不脱离本公开的精神和范围内所作的变动与润饰,均属本公开的专利保护范围。
Claims (5)
1.一种有机玻璃用氟硅改性丙烯酸树脂涂料,其特征在于:按质量百分计,由下列组分组成:
2.根据权利要求1所述的有机玻璃用氟硅改性丙烯酸树脂涂料,其特征在于:
所述的改性丙烯酸树脂按质量百分计,由下列各组分组成:
所述羟基硅油为α,ω-二羟基封端聚二甲基硅氧烷。
3.根据权利要求2所述的有机玻璃用氟硅改性丙烯酸树脂涂料,其特征在于:
所述的改性丙烯酸树脂制备方法如下:
步骤1:羟基硅油预处理,将羟基硅油运用旋转蒸发器在减压0.08MPa以上、蒸馏温度(10022)℃条件下除去水分与杂质备用;
步骤2:制备物料混合物,取所述量80%的甲基丙烯酸甲酯、80%的季戊四醇三丙烯酸酯、80%的甲基丙烯酸六氟丁酯、80%的甲基丙烯酸和所述量20%的醋酸丁酯、20%的二甲苯以及所述量70%的过氧化苯甲酰均匀混合成物料混合物;
步骤3:取所述量20%的甲基丙烯酸甲酯、20%的季戊四醇三丙烯酸酯、20%的甲基丙烯酸六氟丁酯、20%的甲基丙烯酸和所述量60%的醋酸丁酯、60%的二甲苯投入釜中加热搅拌并持续通氮气保护直至回流;
步骤4:步骤3体系在氮气保护条件下搅拌回流30min后,开始滴加步骤2制备的物料混合物,要求滴速均匀,滴加时间保持在60min~120min,滴加过程中继续保持氮气保护并搅拌回流;
步骤5:滴加完毕继续保持氮气保护并搅拌回流30min后,将所述量20%的醋酸丁酯和20%的二甲苯、所述量100%的羟基硅油、所述量30%的过氧化苯甲酰充分混合均匀滴加,滴加时间保持在60min~90min,滴加过程中继续保持氮气保护并搅拌回流;
步骤6:滴加完毕后继续保持氮气保护并搅拌回流共聚240min,随后降温出料,得到无色透明澄清树脂,及改性丙烯酸树脂。
4.权利要求1-3任一项所述有机玻璃用氟硅改性丙烯酸树脂涂料的制备方法:取所述量改性丙烯酸树脂、3390固化剂、醋酸丁酯、二甲苯加入烧杯,常温常压环境下搅拌混合均匀即可。
5.权利要求1-3任一项所述有机玻璃用氟硅改性丙烯酸树脂涂料的使用方法,其特征在于包括如下步骤:
(1)使用醋酸丁酯或二甲苯对基材进行擦洗,使基材表面洁净并放至干燥;
(2)将有机玻璃用氟硅改性丙烯酸树脂涂料均匀喷覆或者淋涂于有机玻璃基材表面,涂覆量根据实际使用情况决定,然后将基材置于常温常压环境条件下静置30min待其表干;
(3)表干后将基材静置于60℃环境中进行热固化,固化时间不低于60min。
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