CN116836364A - 一种有机硅改性型水性聚氨酯胶粘剂的制备工艺 - Google Patents
一种有机硅改性型水性聚氨酯胶粘剂的制备工艺 Download PDFInfo
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Abstract
本发明提供一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,涉及改性型水性聚氨酯胶粘剂领域。有机硅改性型水性聚氨酯胶粘剂包括以下重量份组成:二羟甲基丙酸:10~20份;端羟基聚二甲基硅氧烷:1~10份;氨内基甲基二甲氧基硅烷:18~26份。本发明通过选用氨内基甲基二甲氧基硅烷替代常规脂肪二胺和低分子氨烃基硅烷偶联剂作扩链剂,使合成的水性有机硅-聚氨酯嵌段共和物分子链中有机硅氧烷链段含量大大增加,提高了薄膜的拒水性与耐热稳定性等性能,同时增加了水性聚氨酯胶粘剂的乳液稳定性,选用了蓖麻油作为原料,在水性有机硅-聚氨酯嵌段共和物分子中引入内交联和疏水的长脂肪链,进一步提高了耐水性。
Description
技术领域
本发明涉及改性型水性聚氨酯胶粘剂领域,具体为一种有机硅改性型水性聚氨酯胶粘剂的制备工艺。
背景技术
有机硅~聚氨酯共聚物是一类新型高分子材料,从分子链段结构来看,它既含有优异介电性、柔韧性、耐水性、透气性及生物相容性的有机硅链段,同时又具有良好的热稳定性、耐候性及耐磨性的聚氨酯链段,已被广泛应用于电子工业及人造器官等领。
目前含氨基的有机硅共聚改性聚氨酯的方式主要有两种,一种是利用双氨基封端的聚二甲基硅氧烷与聚氨酯形成嵌段共聚物,另一种是利用侧链含有多氨基基团的聚二甲基硅氧烷与聚氨酯接枝反应形成有机硅~聚氨酯共聚物,前者硅氧烷链段被嵌在聚氨酯主链中,它向表面迁移的能力受到主链的牵制,所以为了获得较好的表面改性效果,常需加入大量的氨基硅油。
目前市场上的有机硅类防水剂品种繁多,使用效果各不相同,主要分为甲基硅醇盐、硅树脂、硅烷、有机硅乳液几大类,甲基硅醇盐作为第一代有机硅防水剂,但甲基硅树脂防水层的光泽度高、不耐擦洗,影响了建筑物的外观,且防水层会在几个月或1~2年后失效3年,有机硅乳液为线型聚有机硅氧烷在水中形成的乳液,但乳液的稳定性一直是需要解决的关键问题,同时现有的水性聚氨酯胶粘剂的耐水性能较差。
发明内容
(一)解决的技术问题
针对现有技术的不足,本发明提供了一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,解决了目前市场上的有机硅类防水剂品种繁多,使用效果各不相同,主要分为甲基硅醇盐、硅树脂、硅烷、有机硅乳液几大类,甲基硅醇盐作为第一代有机硅防水剂,但甲基硅树脂防水层的光泽度高、不耐擦洗,影响了建筑物的外观,且防水层会在几个月或1~2年后失效3年,有机硅乳液为线型聚有机硅氧烷在水中形成的乳液,但乳液的稳定性一直是需要解决的关键问题,同时现有的水性聚氨酯胶粘剂的耐水性能较差的问题。
(二)技术方案
为实现以上目的,本发明通过以下技术方案予以实现:一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,所述有机硅改性型水性聚氨酯胶粘剂包括以下重量份组成:
二羟甲基丙酸:10~20份;
端羟基聚二甲基硅氧烷:1~10份;
氨内基甲基二甲氧基硅烷:18~26份;
聚氧化丙烯二醇:10~16份;
蓖麻油:8~12份;
2,4-甲苯二异氰酸酯:4~8份;
丙酮:5~10份;
三乙胺:1~3份;
阻燃聚醚多元醇:20~30份;
异佛尔酮二异氰酸酯:15~20份;
还包括以下制备步骤:
步骤一:将端羟基聚二甲基硅氧烷和氨内基甲基二甲氧基硅烷放入蒸馏器中搅拌加热反应,反应结束后冷却至室温,合成N-叔丁基-2-苯并噻唑次磺酰胺;
步骤二:将蓖麻油和聚氧化丙烯二醇均进行减压脱水处理,丙酮进行蒸馏;
步骤三:蓖麻油、聚氧化丙烯二醇、聚氧化丙烯二醇、二羟甲基丙酸和丙酮加入搅拌机中加热进行均匀搅拌;
步骤四:在三乙胺中加入去离子水进行稀释,得到稀释三乙胺溶液;
步骤五:加入2,4-甲苯二异氰酸酯继续搅拌,搅拌完成后,对搅拌机降温,加入N-叔丁基-2-苯并噻唑次磺酰胺,继续搅拌至分散,脱水缓慢加入稀释三乙胺溶液,得到混合液;
步骤六:将混合液放入蒸馏器中将丙酮蒸馏出,得到水性有机硅-聚氨酯嵌段共和物;
步骤七:将水性有机硅-聚氨酯嵌段共和物、蓖麻油、聚酯多元醇和异佛尔酮二异氰酸酯放入搅拌机中进行加热搅拌,缓慢加入丙酮,对搅拌机进行升温,得到黏稠胶体;
步骤八:将黏稠胶体放入蒸馏器中将丙酮蒸馏出,得到有机硅改性型水性聚氨酯胶粘剂。
优选的,所述步骤一的蒸馏器温度为100~120℃,反应时间为4~6h。
进一步,所述步骤二减压脱水温度为50~90℃,时间为1~1.5h。
更进一步,所述步骤三搅拌机的温度为70~90℃。
更加进一步,所述步骤五搅拌机降温至50~60℃,所述分散时间为1~1.5h。
更加进一步,所述步骤七中搅拌机的加热温度至45~50℃。
更加进一步,所述搅拌机升温至55~60℃,所述搅拌时间为4~6h。
(三)有益效果
本发明提供了一种有机硅改性型水性聚氨酯胶粘剂的制备工艺。具备以下有益效果:
1、本发明通过选用氨内基甲基二甲氧基硅烷替代常规脂肪二胺和低分子氨烃基硅烷偶联剂作扩链剂,使合成的水性有机硅-聚氨酯嵌段共和物分子链中有机硅氧烷链段含量大大增加,提高了薄膜的拒水性与耐热稳定性等性能,同时增加了水性聚氨酯胶粘剂的乳液稳定性,选用了蓖麻油作为原料,在水性有机硅-聚氨酯嵌段共和物分子中引入内交联和疏水的长脂肪链,进一步提高了耐水性。
2、本发明采用阻燃聚醚多元醇,因此制成的水性有机硅-聚氨酯嵌段共和物中含有磷、氮、硅,在磷、氮、硅的协同作用下,增加了水性有机硅-聚氨酯嵌段共和物的阻燃效果,从而增加了水分散液的稳定性、流变特性、成膜性,因此耐热性和机械强度均有提高。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,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他实施例,都属于本发明保护的范围。
实施例一:
本发明实施例提供一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,有机硅改性型水性聚氨酯胶粘剂包括以下重量份组成:
二羟甲基丙酸:16份;
端羟基聚二甲基硅氧烷:8份;
氨内基甲基二甲氧基硅烷:22份;
聚氧化丙烯二醇:13份;
蓖麻油:10份;
2,4-甲苯二异氰酸酯:6份;
丙酮:8份;
三乙胺:2份;
阻燃聚醚多元醇:25份;
异佛尔酮二异氰酸酯:17份;
还包括以下制备步骤:
步骤一:将端羟基聚二甲基硅氧烷和氨内基甲基二甲氧基硅烷放入蒸馏器中搅拌加热反应,加热温度至110℃,反应时间为6h,反应结束后冷却至室温,合成N-叔丁基-2-苯并噻唑次磺酰胺;
步骤二:将蓖麻油和聚氧化丙烯二醇均进行减压脱水处理,温度为80℃,时间为1.2h,丙酮进行蒸馏;
步骤三:蓖麻油、聚氧化丙烯二醇、聚氧化丙烯二醇、二羟甲基丙酸和丙酮加入搅拌机中加热进行均匀搅拌,温度为85℃;
步骤四:在三乙胺中加入去离子水进行稀释,得到稀释三乙胺溶液;
步骤五:加入2,4-甲苯二异氰酸酯继续搅拌,搅拌完成后,对搅拌机降温至55℃,加入N-叔丁基-2-苯并噻唑次磺酰胺,继续搅拌至分散,分散时间为1.2h,脱水缓慢加入稀释三乙胺溶液,得到混合液;
步骤六:将混合液放入蒸馏器中将丙酮蒸馏出,得到水性有机硅-聚氨酯嵌段共和物;
步骤七:将水性有机硅-聚氨酯嵌段共和物、蓖麻油、聚酯多元醇和异佛尔酮二异氰酸酯放入搅拌机中进行加热搅拌,加热至50℃,缓慢加入丙酮,对搅拌机进行升温,升温至60℃,时间为5h,得到黏稠胶体;
步骤八:将黏稠胶体放入蒸馏器中将丙酮蒸馏出,得到有机硅改性型水性聚氨酯胶粘剂。
实施例二:
本发明实施例提供一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,根据具体实施例一中的内容进行进一步扩充:
其中,有机硅改性型水性聚氨酯胶粘剂包括以下重量份组成:
二羟甲基丙酸:18份;
端羟基聚二甲基硅氧烷:6份;
氨内基甲基二甲氧基硅烷:20份;
聚氧化丙烯二醇:14份;
蓖麻油:9份;
2,4-甲苯二异氰酸酯:5份;
丙酮:6份;
三乙胺:3份;
阻燃聚醚多元醇:28份;
异佛尔酮二异氰酸酯:16份;
还包括以下制备步骤:
步骤一:将端羟基聚二甲基硅氧烷和氨内基甲基二甲氧基硅烷放入蒸馏器中搅拌加热反应,加热温度至100℃,反应时间为4h,反应结束后冷却至室温,合成N-叔丁基-2-苯并噻唑次磺酰胺;
步骤二:将蓖麻油和聚氧化丙烯二醇均进行减压脱水处理,温度为70℃,时间为1h,丙酮进行蒸馏;
步骤三:蓖麻油、聚氧化丙烯二醇、聚氧化丙烯二醇、二羟甲基丙酸和丙酮加入搅拌机中加热进行均匀搅拌,温度为75℃;
步骤四:在三乙胺中加入去离子水进行稀释,得到稀释三乙胺溶液;
步骤五:加入2,4-甲苯二异氰酸酯继续搅拌,搅拌完成后,对搅拌机降温至50℃,加入N-叔丁基-2-苯并噻唑次磺酰胺,继续搅拌至分散,分散时间为1h,脱水缓慢加入稀释三乙胺溶液,得到混合液;
步骤六:将混合液放入蒸馏器中将丙酮蒸馏出,得到水性有机硅-聚氨酯嵌段共和物;
步骤七:将水性有机硅-聚氨酯嵌段共和物、蓖麻油、聚酯多元醇和异佛尔酮二异氰酸酯放入搅拌机中进行加热搅拌,加热至45℃,缓慢加入丙酮,对搅拌机进行升温,升温至55℃,时间为4h,得到黏稠胶体;
步骤八:将黏稠胶体放入蒸馏器中将丙酮蒸馏出,得到有机硅改性型水性聚氨酯胶粘剂。
实施例三:
本发明实施例提供一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,根据具体实施例一中的内容进行进一步扩充:
其中,有机硅改性型水性聚氨酯胶粘剂包括以下重量份组成:
二羟甲基丙酸:20份;
端羟基聚二甲基硅氧烷:10份;
氨内基甲基二甲氧基硅烷:26份;
聚氧化丙烯二醇:16份;
蓖麻油:12份;
2,4-甲苯二异氰酸酯:8份;
丙酮:10份;
三乙胺:3份;
阻燃聚醚多元醇:30份;
异佛尔酮二异氰酸酯:20份;
还包括以下制备步骤:
步骤一:将端羟基聚二甲基硅氧烷和氨内基甲基二甲氧基硅烷放入蒸馏器中搅拌加热反应,加热温度至100℃,反应时间为4.5h,反应结束后冷却至室温,合成N-叔丁基-2-苯并噻唑次磺酰胺;
步骤二:将蓖麻油和聚氧化丙烯二醇均进行减压脱水处理,温度为90℃,时间为1h,丙酮进行蒸馏;
步骤三:蓖麻油、聚氧化丙烯二醇、聚氧化丙烯二醇、二羟甲基丙酸和丙酮加入搅拌机中加热进行均匀搅拌,温度为70℃;
步骤四:在三乙胺中加入去离子水进行稀释,得到稀释三乙胺溶液;
步骤五:加入2,4-甲苯二异氰酸酯继续搅拌,搅拌完成后,对搅拌机降温至50℃,加入N-叔丁基-2-苯并噻唑次磺酰胺,继续搅拌至分散,分散时间为1h,脱水缓慢加入稀释三乙胺溶液,得到混合液;
步骤六:将混合液放入蒸馏器中将丙酮蒸馏出,得到水性有机硅-聚氨酯嵌段共和物;
步骤七:将水性有机硅-聚氨酯嵌段共和物、蓖麻油、聚酯多元醇和异佛尔酮二异氰酸酯放入搅拌机中进行加热搅拌,加热至45℃,缓慢加入丙酮,对搅拌机进行升温,升温至55℃,时间为4h,得到黏稠胶体;
步骤八:将黏稠胶体放入蒸馏器中将丙酮蒸馏出,得到有机硅改性型水性聚氨酯胶粘剂。
实施例四:
本发明实施例提供一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,根据具体实施例一中的内容进行进一步扩充:
其中,有机硅改性型水性聚氨酯胶粘剂包括以下重量份组成:
二羟甲基丙酸:10份;
端羟基聚二甲基硅氧烷:1份;
氨内基甲基二甲氧基硅烷:18份;
聚氧化丙烯二醇:10份;
蓖麻油:8份;
2,4-甲苯二异氰酸酯:4份;
丙酮:5份;
三乙胺:1份;
阻燃聚醚多元醇:20份;
异佛尔酮二异氰酸酯:15份;
还包括以下制备步骤:
步骤一:将端羟基聚二甲基硅氧烷和氨内基甲基二甲氧基硅烷放入蒸馏器中搅拌加热反应,加热温度至120℃,反应时间为6h,反应结束后冷却至室温,合成N-叔丁基-2-苯并噻唑次磺酰胺;
步骤二:将蓖麻油和聚氧化丙烯二醇均进行减压脱水处理,温度为60℃,时间为1.5h,丙酮进行蒸馏;
步骤三:蓖麻油、聚氧化丙烯二醇、聚氧化丙烯二醇、二羟甲基丙酸和丙酮加入搅拌机中加热进行均匀搅拌,温度为90℃;
步骤四:在三乙胺中加入去离子水进行稀释,得到稀释三乙胺溶液;
步骤五:加入2,4-甲苯二异氰酸酯继续搅拌,搅拌完成后,对搅拌机降温至60℃,加入N-叔丁基-2-苯并噻唑次磺酰胺,继续搅拌至分散,分散时间为1.5h,脱水缓慢加入稀释三乙胺溶液,得到混合液;
步骤六:将混合液放入蒸馏器中将丙酮蒸馏出,得到水性有机硅-聚氨酯嵌段共和物;
步骤七:将水性有机硅-聚氨酯嵌段共和物、蓖麻油、聚酯多元醇和异佛尔酮二异氰酸酯放入搅拌机中进行加热搅拌,加热至50℃,缓慢加入丙酮,对搅拌机进行升温,升温至60℃,时间为6h,得到黏稠胶体;
步骤八:将黏稠胶体放入蒸馏器中将丙酮蒸馏出,得到有机硅改性型水性聚氨酯胶粘剂。
实施例五:
本发明实施例提供一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,根据具体实施例一中的内容进行进一步扩充:
其中,有机硅改性型水性聚氨酯胶粘剂包括以下重量份组成:
二羟甲基丙酸:18份;
端羟基聚二甲基硅氧烷:3份;
氨内基甲基二甲氧基硅烷:23份;
聚氧化丙烯二醇:14份;
蓖麻油:9份;
2,4-甲苯二异氰酸酯:5份;
丙酮:7份;
三乙胺:2份;
阻燃聚醚多元醇:23份;
异佛尔酮二异氰酸酯:12份;
还包括以下制备步骤:
步骤一:将端羟基聚二甲基硅氧烷和氨内基甲基二甲氧基硅烷放入蒸馏器中搅拌加热反应,加热温度至113℃,反应时间为5.5h,反应结束后冷却至室温,合成N-叔丁基-2-苯并噻唑次磺酰胺;
步骤二:将蓖麻油和聚氧化丙烯二醇均进行减压脱水处理,温度为80℃,时间为1h,丙酮进行蒸馏;
步骤三:蓖麻油、聚氧化丙烯二醇、聚氧化丙烯二醇、二羟甲基丙酸和丙酮加入搅拌机中加热进行均匀搅拌,温度为75℃;
步骤四:在三乙胺中加入去离子水进行稀释,得到稀释三乙胺溶液;
步骤五:加入2,4-甲苯二异氰酸酯继续搅拌,搅拌完成后,对搅拌机降温至53℃,加入N-叔丁基-2-苯并噻唑次磺酰胺,继续搅拌至分散,分散时间为1h,脱水缓慢加入稀释三乙胺溶液,得到混合液;
步骤六:将混合液放入蒸馏器中将丙酮蒸馏出,得到水性有机硅-聚氨酯嵌段共和物;
步骤七:将水性有机硅-聚氨酯嵌段共和物、蓖麻油、聚酯多元醇和异佛尔酮二异氰酸酯放入搅拌机中进行加热搅拌,加热至48℃,缓慢加入丙酮,对搅拌机进行升温,升温至57℃,时间为5h,得到黏稠胶体;
步骤八:将黏稠胶体放入蒸馏器中将丙酮蒸馏出,得到有机硅改性型水性聚氨酯胶粘剂。
本申请人为了更好地体现出,本发明有机硅改性型水性聚氨酯胶粘剂性能的优越性,将本发明有机硅改性型水性聚氨酯胶粘剂与传统有机硅改性型水性聚氨酯胶粘剂进行对比,在两者之间进行实验得出两者的接触角、吸水率、抗拉强度、断裂伸长率和乳液稳定性,并在下方进行数据对比:
由此得出:本发明有机硅改性型水性聚氨酯胶粘剂的接触角、吸水率、抗拉强度、断裂伸长率和乳液稳定性优越传统有机硅改性型水性聚氨酯胶粘剂的接触角、吸水率、抗拉强度、断裂伸长率和乳液稳定性,通过上述表格得出,实施例一中有机硅改性型水性聚氨酯胶粘剂接触角、吸水率、抗拉强度、断裂伸长率和乳液稳定性高于实施例二、实施例三、实施例四和实施例五中有机硅改性型水性聚氨酯胶粘剂的接触角、吸水率、抗拉强度、断裂伸长率和乳液稳定性。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (7)
1.一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,其特征在于:其特征在于:所述有机硅改性型水性聚氨酯胶粘剂包括以下重量份组成:
二羟甲基丙酸:10~20份;
端羟基聚二甲基硅氧烷:1~10份;
氨内基甲基二甲氧基硅烷:18~26份;
聚氧化丙烯二醇:10~16份;
蓖麻油:8~12份;
2,4-甲苯二异氰酸酯:4~8份;
丙酮:5~10份;
三乙胺:1~3份;
阻燃聚醚多元醇:20~30份;
异佛尔酮二异氰酸酯:15~20份;
还包括以下制备步骤:
步骤一:将端羟基聚二甲基硅氧烷和氨内基甲基二甲氧基硅烷放入蒸馏器中搅拌加热反应,反应结束后冷却至室温,合成N-叔丁基-2-苯并噻唑次磺酰胺;
步骤二:将蓖麻油和聚氧化丙烯二醇均进行减压脱水处理,丙酮进行蒸馏;
步骤三:蓖麻油、聚氧化丙烯二醇、聚氧化丙烯二醇、二羟甲基丙酸和丙酮加入搅拌机中加热进行均匀搅拌;
步骤四:在三乙胺中加入去离子水进行稀释,得到稀释三乙胺溶液;
步骤五:加入2,4-甲苯二异氰酸酯继续搅拌,搅拌完成后,对搅拌机降温,加入N-叔丁基-2-苯并噻唑次磺酰胺,继续搅拌至分散,脱水缓慢加入稀释三乙胺溶液,得到混合液;
步骤六:将混合液放入蒸馏器中将丙酮蒸馏出,得到水性有机硅-聚氨酯嵌段共和物;
步骤七:将水性有机硅-聚氨酯嵌段共和物、蓖麻油、聚酯多元醇和异佛尔酮二异氰酸酯放入搅拌机中进行加热搅拌,缓慢加入丙酮,对搅拌机进行升温,得到黏稠胶体;
步骤八:将黏稠胶体放入蒸馏器中将丙酮蒸馏出,得到有机硅改性型水性聚氨酯胶粘剂。
2.根据权利要求1所述的一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,其特征在于:所述步骤一的蒸馏器温度为100~120℃,反应时间为4~6h。
3.根据权利要求1所述的一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,其特征在于:所述步骤二减压脱水温度为50~90℃,时间为1~1.5h。
4.根据权利要求1所述的一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,其特征在于:所述步骤三搅拌机的温度为70~90℃。
5.根据权利要求1所述的一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,其特征在于:所述步骤五搅拌机降温至50~60℃,所述分散时间为1~1.5h。
6.根据权利要求1所述的一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,其特征在于:所述步骤七中搅拌机的加热温度至45~50℃。
7.根据权利要求1所述的一种有机硅改性型水性聚氨酯胶粘剂的制备工艺,其特征在于:所述搅拌机升温至55~60℃,所述搅拌时间为4~6h。
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