CN113024810A - 一种单组份可自交联氟硅离型剂及其制备方法 - Google Patents
一种单组份可自交联氟硅离型剂及其制备方法 Download PDFInfo
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Abstract
Description
技术领域
本发明涉及有机硅剥离材料技术领域,具体地说涉及一种单组份可自交联氟硅离型剂及其制备方法。
背景技术
离型剂是一种起到辅助脱离作用的功能性加工助剂,其处于模具和成型制品之间,能够防止橡胶、树脂、塑料等弹性体及其他一些材料的制件粘在模具表面上,可以使得制品很容易从模具中脱出,同时保证制品表面质量和模具完好无损。它广泛用于包装、印刷、丝印、移印、铭板、薄膜开关、柔性线路、绝缘制品、线路板、激光防伪、贴合、电子、密封材料用膜、反光材料、防水材料、医药(膏药用纸)、卫生用纸、胶粘制品、模切冲型加工等行业领域。
离型剂主要分为含硅离型剂、非硅离型剂以及含氟离型剂。其中,含硅类的离型剂成本较低可适用于大部分场合,但存在硅迁移的问题(影响二次加工等),且不适用于超轻剥离力要求的领域。非硅类离型剂应用较早,但其离型力较大,更无法满足需轻离型力要求的领域。氟素离型剂具有剥离力轻、化学稳定性高等优点,但是其制备工艺复杂,单体昂贵,难以大规模应用。因此,可结合硅离型剂与氟素离型剂的优点,生产出氟硅离型剂。
就常规离型剂来说,其组分一般为四部分,分别为基胶、交联剂、催化剂、锚固剂。使用时需要按照一定的比例混合。操作麻烦,且部分组分相容性也较差,这就使得应用受到限制,增加了成本。
发明内容
本发明要解决的问题是克服现有离型剂的部分缺陷,提供一种无需锚固剂可自交联氟硅离型剂及其制备方法。本发明的离型剂稳定性好,成本低廉,制备方法简便,使用方便,便于产业化生产。
为了解决上述技术问题,本发明提供了如下的技术方案:
一种单组份可自交联氟硅离型剂,具有如下化学结构式:
其中Rf为含氟烷基;R1为氢或乙烯基;R2、R3为C1~C6烷基之一;R4、R5乙烯基或氢。n1为1~20的整数;n2为1~30的整数。
优选地,所述含氟烷基为:—(CH2)mCF3,m为0~5的整数。
优选地,所述R1、R4、R5中,氢和乙烯基至少有两种。
优选地,所述的可自交联氟硅离型剂,其产品为无色透明,粘度极低的液体,室温下其粘度在20~100mpa/s。
本发明公开了单组份可自交联氟硅离型剂的制备方法,包括以下步骤:
①将封端剂加入到一定量的含氟官能团取代的硅氧烷环聚体,含氢(乙烯基)官能团取代的硅氧烷环聚体和环硅氧烷单体中,加入固体催化剂后在40~90℃下反应1~9h得到反应产物。
②将步骤①的反应产物中的催化剂除去,而后将产物在一定温度下减压蒸馏除去低沸点馏分即得到所述的自交联氟硅离型剂。
优选地,步骤①所述含氟官能团取代的硅氧烷环聚体为结构式如下式所示的硅氧烷环聚体,
其中,R2为C1~C6烷基之一;m为0-5的整数,p为2~5的整数;
所述含氢(乙烯基)官能团取代的硅氧烷环聚体为结构式如下式所示的硅氧烷环聚体,
其中,R1为氢或乙烯基之一;R4为C1~C6烷基之一;q为3~5的整数。
优选地,步骤①所述封端剂为四甲基二乙烯基二硅氧烷、四甲基二氢二硅氧烷中的一种,加入量为其含氢链节与乙烯基链节摩尔比为1:1~30。
优选地,步骤①所述催化剂为强酸或大孔强酸阳离子交换树脂之一,用量以反应产物的总质量计算,加入量为1%~9%。
本发明的有益效果为:本发明的氟硅离型剂具有较短的固化时间、良好的储存性能和耐高低温性能、优良的剥离力性能,其制备方法简单,成本较低,使用方便,具有较大的市场前景。
附图说明
附图用来提供对本发明的进一步理解,并且构成说明书的一部分,与本发明的实用实施例一起用于解释本发明,并不应用于限定本发明。
图1为本发明实施例1的合成过程示意图。
图2是本发明实施例1的红外谱图。
图3是本发明实施例1的核磁共振氢谱(1H-NMR)。
具体实施方式
以下结合附图对本发明的优选实施例进行说明,应当理解,此处所描述的优选实施例仅用于说明和解释本发明,并不用于限定本发明。
实施例1
向干燥的250ml三口烧瓶中加入96.2g四甲基四氢环四硅氧烷,65.6g三甲基三氟丙基环三硅氧烷,38.2g八甲基环四硅氧烷,6.2g四甲基二乙烯基二硅氧烷,放置油浴锅中加热至50℃搅拌10分钟充分混合均匀;而后加入10g固体酸催化剂HND-580,升温至60℃聚合反应6h。
反应结束后过滤除去催化剂,将清液进行减压蒸馏3h脱除低沸物,得到无色透明低粘度液体,即为目标产物。产率为89.4%,粘度(26℃)40mPa/s。
实施例2
向干燥的250ml三口烧瓶中加入38.2g八甲基环四硅氧烷,65.6g三甲基三氟丙基环三硅氧烷,96.2g四甲基四氢环四硅氧烷,6.2g四甲基二乙烯基二硅氧烷,放置油浴锅中加热至50℃搅拌10分钟充分混合均匀;而后加入10g固体酸催化剂HND-8,升温至80℃聚合反应6h。
反应结束后过滤除去催化剂,将清液进行减压蒸馏3h脱除低沸物,得到无色透明低粘度液体,即为目标产物。产率为84.7%,粘度(26℃)84mPa/s。
实施例3
向干燥的250ml三口烧瓶中加入64.1g四甲基四氢环四硅氧烷,41.6g三甲基三氟丙基环三硅氧烷,94.2g八甲基环四硅氧烷,3.1g四甲基二乙烯基二硅氧烷,放置油浴锅中加热至50℃搅拌10分钟充分混合均匀;而后加入10g固体酸催化剂HND-580,升温至65℃聚合反应6h。
反应结束后过滤除去催化剂,将清液进行减压蒸馏3h脱除低沸物,得到无色透明低粘度液体,即为目标产物。产率为87.7%,粘度(26℃)39mPa/s。
实施例4
向干燥的250ml三口烧瓶中加入96.2g四甲基四氢环四硅氧烷,65.6g三甲基三氟丙基环三硅氧烷,38.2g八甲基环四硅氧烷,6.2g四甲基二乙烯基二硅氧烷,放置油浴锅中加热至50℃搅拌10分钟充分混合均匀;而后加入10g固体酸催化剂HND-580,升温至60℃聚合反应3h。
反应结束后过滤除去催化剂,将清液进行减压蒸馏3h脱除低沸物,得到无色透明低粘度液体,即为目标产物。产率为88.4%,粘度(26℃)33mPa/s。
实施例4应用
对实施例4所得的自交联氟硅离型剂测定其热重、红外及其氢谱。按比例称取组分分配比:50份自交联氟硅离型剂、50ppm铂金催化剂,用涂布器涂布在未电晕的PET基材上面,然后入烘道烘烤进行固化,并用cheminstruments的180°剥离力测试仪进行剥离力测试,测定其剥离力。结果如下表所示:
表一:离型剂固化条件及配比
产品用量 | 催化剂用量(铂系) | 固化温度 | 固化时间 | |
实施例4 | 50g | 40ppm | 150℃ | 1min |
表二:离型性能结果
离型力(g/25mm) | 20h标测(N/25mm) | 残余附着力(%) | |
实施例4 | 7 | 0.27 | 96 |
以上所述仅表达了本发明的优选实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形、改进及替代,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (8)
2.根据权利要求1所述的单组份可自交联氟硅离型剂,其特征在于,所述含氟烷基为:—(CH2)mCF3,m为0~5的整数。
3.根据权利要求1所述的单组份可自交联氟硅离型剂,其特征在于,所述R1、R4、R5中,氢和乙烯基至少有两种。
4.根据权利要求1所述的单组份可自交联氟硅离型剂,其特征在于,其产品为无色透明,粘度极低的液体,室温下其粘度在20~100mpa/s。
5.一种单组份可自交联氟硅离型剂的制备方法,其特征在于,包括以下步骤:
①将封端剂加入到一定量的含氟官能团取代的硅氧烷环聚体,含氢或乙烯基官能团取代的硅氧烷环聚体和环硅氧烷单体中,加入固体催化剂后在40~90℃下反应1~9h得到反应产物;
②将步骤①的反应产物中的催化剂除去,而后将产物在一定温度下减压蒸馏除去低沸点馏分即得到所述的自交联氟硅离型剂。
7.根据权利要求5所述的制备方法,其特征在于,所述步骤①封端剂为四甲基二乙烯基二硅氧烷、四甲基二氢二硅氧烷中的一种,加入量为其含氢链节与乙烯基链节摩尔比为1:1~30。
8.根据权利要求5所述的制备方法,其特征在于,所述步骤①催化剂为强酸或大孔强酸阳离子交换树脂之一,用量以反应产物的总质量计算,加入量为1%~9%。
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