CN117384557B - 一种耐低温聚丙烯酸酯压敏胶及其制备方法 - Google Patents
一种耐低温聚丙烯酸酯压敏胶及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种耐低温聚丙烯酸酯压敏胶及其制备方法,属于高分子材料技术领域。本发明的一种耐低温聚丙烯酸酯压敏胶的制备方法包括:(1)将聚氨酯4~10份、甲基丙烯酸甲酯10~15份、丙烯酸丙酯2~8份、丙烯酸2~8份、丙烯酸正丁酯10~25份、丙烯酸羟丁酯10~20份、溶剂20~50份混合均匀得到混合物;(2)在真空条件下,将所述混合物与0.1~0.3份有机硅气凝胶混合,在搅拌状态下滴加引发剂0.15~0.3份,并在50~100℃下搅拌反应4~6小时得到一种耐低温聚丙烯酸酯,所述有机硅为乙烯基三甲氧基硅烷。本发明的产品更稳定,耐低温性能好。
Description
技术领域
本发明涉及一种耐低温聚丙烯酸酯压敏胶及其制备方法,属于高分子材料技术领域。
背景技术
丙烯酸酯聚合物具有优良的成膜性、粘接性、保光性、耐候性、耐腐烛性和柔韧性,然而聚丙烯酸酯具有低温脆性,低温条件下聚丙烯酸酯压敏胶的性能下降,会影响产品的正常使用。冬天室外气温低,因此开发耐低温聚丙烯酸酯压敏胶具有重要意义。
用有机硅改性丙烯酸酯,可以综合二者的优点,改善丙烯酸酯“热黏冷脆”的缺陷,然而改善程度有待进一步提高。
CN114989731A一种聚丙烯酸酯/有机硅杂化压敏胶,包括,组分(A),(甲基)丙烯酸酯预聚物,组分(B),可自由基聚合反应的多官能度有机硅氧烷,组分(C),自由基光引发剂,以及,组分(D),抗氧剂。本发明的聚丙烯酸酯/有机硅杂化压敏胶,由于引入的有机硅成分在整个分子网络中形成了互穿聚合物网络(IPN),充分的利用了有机硅耐高温的特性,使得整个丙烯酸酯/有机硅杂化压敏胶体系能够显著提升耐温等级,从而扩大了应用范围。然而其主要提高耐高温性能,耐低温性能有待进一步提高。
CN115537158A公开了一种有机硅改性丙烯酸酯压敏胶及其生产工艺,利用化学反应,在纳米二氧化硅表面修饰烯基官能团,再通过半连续乳液聚合的方式,将硬单体、软单体、功能单体和有机硅改性单体在纳米二氧化硅核层形成丙烯酸酯共聚物壳,形成壳核双层结构的有机硅改性丙烯酸酯复合胶乳,从而以化学键的连接形式,提高了纳米二氧化硅与有机硅改性丙烯酸酯共聚物之间的界面相容性,进而有效地提高了丙烯酸酯压敏胶的初粘性、持粘性和耐高温等综合性能。然而其也主要提高耐高温性能,耐低温性能有待进一步提高。
气凝胶是指通过溶胶凝胶法,用一定的干燥方式使气体取代凝胶中的液相而形成的一种纳米级多孔固态材料。最轻的气凝胶比空气密度还低。气凝胶的种类很多,有硅系,碳系,硫系,金属氧化物系,金属系等。现有的硅系气凝胶技术成熟。还没有将其应用于耐低温聚丙烯酸酯压敏胶。
发明内容
本发明的第一个目的是提供一种新的耐低温聚丙烯酸酯压敏胶的制备方法。
为达到本发明的第一个目的,本发明的一种耐低温聚丙烯酸酯压敏胶的制备方法包括:
(1)将聚氨酯4~10份、甲基丙烯酸甲酯10~15份、丙烯酸丙酯2~8份、丙烯酸2~8份、丙烯酸正丁酯10~25份、丙烯酸羟丁酯10~20份、溶剂20~50份混合均匀得到混合物;
(2)在真空条件下,将所述混合物与0.1~0.3份有机硅气凝胶混合,在搅拌状态下滴加引发剂0.15~0.3份,并在50~100℃下搅拌反应4~6小时得到一种耐低温聚丙烯酸酯,所述有机硅为乙烯基三甲氧基硅烷;
(3)将步骤(2)得到的耐低温聚丙烯酸酯加入固化剂,混合均匀后均匀涂布在基材上,烘干得一种耐低温聚丙烯酸酯压敏胶。
步骤(2)在真空条件下混合物充分填充气凝胶缝隙,排出有机硅气凝胶中的排出气泡,有利于提高产品性能。
在一种具体实施方式中,步骤(1)所述聚氨酯4~8份、甲基丙烯酸甲酯12~15份、丙烯酸丙酯4~6份、丙烯酸2~8份、丙烯酸正丁酯15~25份、丙烯酸羟丁酯10~15份、溶剂20~50份。
优选的,所述溶剂为甲苯。
优选的,所述引发剂为过氧化苯甲酰、过氧化二异丙苯。
步骤(2)搅拌的转速不宜过快,转速过快影响产品的稳定性,转速过慢不利于传热和产品的稳定性,搅拌的转速为120~200转/min产品的性能好,因此优选的,所述搅拌的转速为120~200转/min。
优选的,步骤(2)所述引发剂的滴加时间2小时以上;优选步骤(2)所述引发剂的滴加时间2~3小时。
优选的,步骤(2)所述有机硅气凝胶的密度为0.035g/cm3~0.045g/cm3,步骤(2)所述有机硅气凝胶的粒度50微米~600微米。
步骤(2)所述有机硅气凝胶的制备方法可以为:将有机硅聚合物、二月桂酸二丁基锡的乙醇溶液、甲基异丁基酮混合得到有机硅溶液,将有机硅溶液润湿碳酸铵粉末,静置45~48小时,真空条件下升温气化碳酸铵得到有机硅气凝胶;
所述有机硅溶液中有机硅的质量浓度为5%~10%,二月桂酸二丁基锡的质量浓度为0.2%~0.3%;
所述升温气化为40℃~60保持1.5~2.5小时,然后以1℃/秒~3℃℃/秒的加热速率升温到140~150℃,在此温度下保持0.8~1.2小时。
优选的,步骤(3)所述基材为PVC、BOPP或PET。
优选的,步骤(3)所述固化剂为乙酰丙酮铝,所述乙酰丙酮铝的量为步骤(2)得到的耐低温聚丙烯酸酯质量的0.1~0.2%。
本发明的第二个目的是提供一种耐低温聚丙烯酸酯压敏胶。
为达到本发明的第二个目的,所述一种耐低温聚丙烯酸酯压敏胶采用上述的方法制备得到。
有益效果
本发明的一种耐低温聚丙烯酸酯压敏胶引入乙烯基三甲氧基硅烷有机硅气凝胶、聚氨酯、并调整软、硬单体以及功能单体的比例,引入少量的有机硅,产品更稳定,耐低温性能好。
实施方式
为达到本发明的第一个目的,本发明的一种耐低温聚丙烯酸酯压敏胶的制备方法包括:
(1)将聚氨酯4~10份、甲基丙烯酸甲酯10~15份、丙烯酸丙酯2~8份、丙烯酸2~8份、丙烯酸正丁酯10~25份、丙烯酸羟丁酯10~20份、溶剂20~50份混合均匀得到混合物;
(2)在真空条件下,将所述混合物与0.1~0.3份有机硅气凝胶混合,在搅拌状态下滴加引发剂0.15~0.3份,并在50~100℃下搅拌反应4~6小时得到一种耐低温聚丙烯酸酯,所述有机硅为乙烯基三甲氧基硅烷;
(3)将步骤(2)得到的耐低温聚丙烯酸酯加入固化剂,混合均匀后均匀涂布在基材上,烘干得一种耐低温聚丙烯酸酯压敏胶。
步骤(2)在真空条件下混合物充分填充气凝胶缝隙,排出有机硅气凝胶中的排出气泡,有利于提高产品性能。
在一种具体实施方式中,步骤(1)所述聚氨酯4~8份、甲基丙烯酸甲酯12~15份、丙烯酸丙酯4~6份、丙烯酸2~8份、丙烯酸正丁酯15~25份、丙烯酸羟丁酯10~15份、溶剂20~50份。
优选的,所述溶剂为甲苯。
优选的,所述引发剂为过氧化苯甲酰、过氧化二异丙苯。
步骤(2)搅拌的转速不宜过快,转速过快影响产品的稳定性,转速过慢不利于传热和产品的稳定性,搅拌的转速为120~200转/min产品的性能好,因此优选的,所述搅拌的转速为120~200转/min。
优选的,步骤(2)所述引发剂的滴加时间2小时以上;优选步骤(2)所述引发剂的滴加时间2~3小时。
优选的,步骤(2)所述有机硅气凝胶的密度为0.035g/cm3~0.045g/cm3,步骤(2)所述有机硅气凝胶的粒度50微米~600微米。
步骤(2)所述有机硅气凝胶的制备方法可以为:将有机硅聚合物、二月桂酸二丁基锡的乙醇溶液、甲基异丁基酮混合得到有机硅溶液,将有机硅溶液润湿碳酸铵粉末,静置45~48小时,真空条件下升温气化碳酸铵得到有机硅气凝胶;
所述有机硅溶液中有机硅的质量浓度为5%~10%,二月桂酸二丁基锡的质量浓度为0.2%~0.3%;
所述升温气化为40℃~60保持1.5~2.5小时,然后以1℃/秒~3℃℃/秒的加热速率升温到140~150℃,在此温度下保持0.8~1.2小时。
优选的,步骤(3)所述基材为PVC、BOPP或PET。
优选的,步骤(3)所述固化剂为乙酰丙酮铝,所述乙酰丙酮铝的量为步骤(2)得到的耐低温聚丙烯酸酯质量的0.1~0.2%。
为达到本发明的第二个目的,所述一种耐低温聚丙烯酸酯压敏胶采用上述的方法制备得到。
下面结合实施例对本发明的具体实施方式做进一步的描述,并不因此将本发明限制在所述的实施例范围之中。
实施例
耐低温聚丙烯酸酯压敏胶的制备:
(1)将聚氨酯5份、甲基丙烯酸甲酯10份、丙烯酸丙酯3份、丙烯酸2份、丙烯酸正丁酯10份、丙烯酸羟丁酯15份、甲苯35份混合均匀得到混合物;
(2)在真空条件下,将混合物与0.2份密度为0.036g/cm3,粒度50微米~600微米的乙烯基三甲氧基硅烷有机硅气凝胶混合,在搅拌状态下将0.15份过氧化苯甲酰2h缓慢滴入,并在50~80℃下搅拌反应5小时得到一种耐低温聚丙烯酸酯,搅拌的转速设置在150转/min;
(3)将步骤(2)得到的耐低温聚丙烯酸酯加入乙酰丙酮铝,乙酰丙酮铝的量为步骤(2)得到的耐低温聚丙烯酸酯质量的0.15%,混合均匀后均匀涂布在PET膜上,110℃烘2min得一种耐低温聚丙烯酸酯压敏胶。
实施例
耐低温聚丙烯酸酯压敏胶的制备:
(1)将聚氨酯8份、甲基丙烯酸甲酯10份、丙烯酸丙酯3份、丙烯酸2份、丙烯酸正丁酯10份、丙烯酸羟丁酯15份、甲苯35份混合均匀得到混合物;
(2)在真空条件下,将混合物与0.2份密度为0.036g/cm3,粒度50微米~600微米的乙烯基三甲氧基硅烷有机硅气凝胶混合,在搅拌状态下将0.15份过氧化苯甲酰2h缓慢滴入,并在50~80℃下搅拌反应5小时得到一种耐低温聚丙烯酸酯,搅拌的转速设置在150转/min;
(3)将步骤(2)得到的耐低温聚丙烯酸酯加入乙酰丙酮铝,乙酰丙酮铝的量为步骤(2)得到的耐低温聚丙烯酸酯质量的0.15%,混合均匀后均匀涂布在PET膜上,110℃烘2min得一种耐低温聚丙烯酸酯压敏胶。
实施例
耐低温聚丙烯酸酯压敏胶的制备:
(1)将聚氨酯5份、甲基丙烯酸甲酯10份、丙烯酸丙酯3份、丙烯酸2份、丙烯酸正丁酯10份、丙烯酸羟丁酯15份、甲苯35份混合均匀得到混合物;
(2)在真空条件下,将混合物与0.1份密度为0.036g/cm3,粒度50微米~600微米的乙烯基三甲氧基硅烷有机硅气凝胶混合,在搅拌状态下将0.15份过氧化苯甲酰2h缓慢滴入,并在50~80℃下搅拌反应5小时得到一种耐低温聚丙烯酸酯,搅拌的转速设置在150转/min;
(3)将步骤(2)得到的耐低温聚丙烯酸酯加入乙酰丙酮铝,乙酰丙酮铝的量为步骤(2)得到的耐低温聚丙烯酸酯质量的0.15%,混合均匀后均匀涂布在PET膜上,110℃烘2min得一种耐低温聚丙烯酸酯压敏胶。
实施例
耐低温聚丙烯酸酯压敏胶的制备:
(1)将聚氨酯10份、甲基丙烯酸甲酯10份、丙烯酸丙酯3份、丙烯酸2份、丙烯酸正丁酯15份、丙烯酸羟丁酯15份、甲苯35份混合均匀得到混合物;
(2)在真空条件下,将混合物与0.2份密度为0.036g/cm3,粒度50微米~600微米的乙烯基三甲氧基硅烷有机硅气凝胶混合,在搅拌状态下滴加将0.15份过氧化苯甲酰2h缓慢滴入,并在50~80℃下搅拌反应5小时得到一种耐低温聚丙烯酸酯,搅拌的转速设置在150转/min;
(3)将步骤(2)得到的耐低温聚丙烯酸酯加入乙酰丙酮铝,乙酰丙酮铝的量为步骤(2)得到的耐低温聚丙烯酸酯质量的0.15%,混合均匀后均匀涂布在PET膜上,110℃烘2min得一种耐低温聚丙烯酸酯压敏胶。
耐低温聚丙烯酸酯压敏胶的制备:
(1)将聚氨酯5份、甲基丙烯酸甲酯10份、丙烯酸丙酯3份、丙烯酸2份、丙烯酸正丁酯10份、丙烯酸羟丁酯15份、甲苯35份混合均匀得到混合物;
(2)将混合物与0.2份乙烯基三甲氧基硅烷有机硅混合,在搅拌状态下将0.15份过氧化苯甲酰2h缓慢滴入,并在50~80℃下搅拌反应5小时得到一种耐低温聚丙烯酸酯,搅拌的转速设置在150转/min;
(3)将步骤(2)得到的耐低温聚丙烯酸酯加入乙酰丙酮铝,乙酰丙酮铝的量为步骤(2)得到的耐低温聚丙烯酸酯质量的0.15%,混合均匀后均匀涂布在PET膜上,110℃烘2min得一种耐低温聚丙烯酸酯压敏胶。
通过对实施例及对比例的样品进行低温180。(-30℃)剥离强度测试得到以下性能参数,见表1。
表1 实施例1-4及对比例1样品低温180。(-30℃)剥离强度测试
样品 | 低温180。剥离强度(-30℃,N/mm) |
实施例1 | 0.62 |
实施例2 | 0.69 |
实施例3 | 0.67 |
实施例4 | 0.73 |
对比例1 | 0.41 |
由表1可见,本发明添加少量的有机硅气凝胶产品的耐低温性能好,实施例4的产品耐低温性能最佳,对比例1仅添加少量的有机硅,性能差。
Claims (10)
1.一种耐低温聚丙烯酸酯压敏胶的制备方法,其特征在于,所述方法包括:
(1)将聚氨酯4-10份、甲基丙烯酸甲酯10-15份、丙烯酸丙酯2-8份、丙烯酸2-8份、丙烯酸正丁酯10-25份、丙烯酸羟丁酯10-20份、溶剂20-50份混合均匀得到混合物;
(2)在真空条件下,将所述混合物与0.1-0.3份有机硅气凝胶混合,在搅拌状态下滴加引发剂0.15-0.3份,并在50-100℃下搅拌反应4-6小时得到一种耐低温聚丙烯酸酯,所述有机硅为乙烯基三甲氧基硅烷;
(3)将步骤(2)得到的耐低温聚丙烯酸酯加入固化剂,混合均匀后均匀涂布在基材上,烘干得一种耐低温聚丙烯酸酯压敏胶。
2.根据权利要求1所述一种耐低温聚丙烯酸酯压敏胶的制备方法,其特征在于,步骤(1)所述聚氨酯4-8份、甲基丙烯酸甲酯12-15份、丙烯酸丙酯4-6份、丙烯酸2-8份、丙烯酸正丁酯15-25份、丙烯酸羟丁酯10-15份、溶剂20-50份。
3.根据权利要求1或2所述一种耐低温聚丙烯酸酯压敏胶的制备方法,其特征在于,步骤(1)所述溶剂为甲苯。
4.根据权利要求1或2所述一种耐低温聚丙烯酸酯压敏胶的制备方法,其特征在于,步骤(2)所述引发剂为过氧化苯甲酰、过氧化二异丙苯。
5.根据权利要求1或2所述一种耐低温聚丙烯酸酯压敏胶的制备方法,其特征在于,所述搅拌的转速为120-200转/min。
6.根据权利要求1或2所述一种耐低温聚丙烯酸酯压敏胶的制备方法,其特征在于,步骤(2)所述引发剂的滴加时间2-3小时。
7.根据权利要求1或2所述一种耐低温聚丙烯酸酯压敏胶的制备方法,其特征在于,步骤(2)所述有机硅气凝胶的密度为0.035g/cm3-0.045g/cm3,步骤(2)所述有机硅气凝胶的粒度50微米-600微米。
8.根据权利要求1所述一种耐低温聚丙烯酸酯压敏胶的制备方法,其特征在于,步骤(3)所述基材为PVC、BOPP或PET。
9.根据权利要求1所述一种耐低温聚丙烯酸酯压敏胶的制备方法,其特征在于,步骤(3)所述固化剂为乙酰丙酮铝,所述乙酰丙酮铝的量为步骤(2)得到的耐低温聚丙烯酸酯质量的0.1-0.2%。
10.一种耐低温聚丙烯酸酯压敏胶,其特征在于,所述一种耐低温聚丙烯酸酯压敏胶采用权利要求1-7任一项的方法制备得到。
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100741699B1 (ko) * | 2006-04-13 | 2007-07-23 | 한국생산기술연구원 | 아크릴레이트 개질된 에어로겔의 제조방법 및 이로부터제조되는 에어로겔 |
CN104194625A (zh) * | 2014-08-15 | 2014-12-10 | 山东天宇圣邦涂料有限公司 | 一种有机硅改性乳液及太阳能反射隔热涂料 |
CN105199521A (zh) * | 2015-09-22 | 2015-12-30 | 天长市开林化工有限公司 | 一种疏水性二氧化硅气凝胶改性丙烯酸酯乳液涂料 |
CN108047478A (zh) * | 2018-02-02 | 2018-05-18 | 兰州交通大学 | 一种有机硅气凝胶的常压制备方法 |
WO2020247743A2 (en) * | 2019-06-06 | 2020-12-10 | Blueshift Materials, Inc. | Aerogels having a core-spoke polymeric matrix, methods of making, and uses thereof |
CN114989731A (zh) * | 2022-05-22 | 2022-09-02 | 江苏翎慧材料科技有限公司 | 一种聚丙烯酸酯/有机硅杂化压敏胶 |
CN116396450A (zh) * | 2023-04-12 | 2023-07-07 | 江苏泰伦特新材料科技有限公司 | 一种气凝胶复合改性的方法 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2019014403A1 (en) * | 2017-07-12 | 2019-01-17 | Dow Silicones Corporation | LIQUID SILICONE RUBBER COMPOSITION |
US11767670B2 (en) * | 2020-04-28 | 2023-09-26 | Taiwan Aerogel Technology Material Co., Ltd. | Method for producing a heat insulating material composed of a hydrophobic aerogel and the application thereof |
-
2023
- 2023-11-01 CN CN202311440717.3A patent/CN117384557B/zh active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100741699B1 (ko) * | 2006-04-13 | 2007-07-23 | 한국생산기술연구원 | 아크릴레이트 개질된 에어로겔의 제조방법 및 이로부터제조되는 에어로겔 |
CN104194625A (zh) * | 2014-08-15 | 2014-12-10 | 山东天宇圣邦涂料有限公司 | 一种有机硅改性乳液及太阳能反射隔热涂料 |
CN105199521A (zh) * | 2015-09-22 | 2015-12-30 | 天长市开林化工有限公司 | 一种疏水性二氧化硅气凝胶改性丙烯酸酯乳液涂料 |
CN108047478A (zh) * | 2018-02-02 | 2018-05-18 | 兰州交通大学 | 一种有机硅气凝胶的常压制备方法 |
WO2020247743A2 (en) * | 2019-06-06 | 2020-12-10 | Blueshift Materials, Inc. | Aerogels having a core-spoke polymeric matrix, methods of making, and uses thereof |
CN114989731A (zh) * | 2022-05-22 | 2022-09-02 | 江苏翎慧材料科技有限公司 | 一种聚丙烯酸酯/有机硅杂化压敏胶 |
CN116396450A (zh) * | 2023-04-12 | 2023-07-07 | 江苏泰伦特新材料科技有限公司 | 一种气凝胶复合改性的方法 |
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