CN104530374A - 一种环氧改性水性聚氨酯合成方法 - Google Patents
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Abstract
本发明涉及一种环氧改性水性聚氨酯合成方法,包括如下步骤:利用一NC0基团和一0H基团的反应,合成交联结构的水性聚氨酯乳液;在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡反应;用滴液漏斗缓慢滴加l,4一丁二醇,滴加亲水扩链剂DMPA和环氧树脂,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂反应;加入三乙胺搅拌中和,在快速搅拌的条件下滴加适量去离子水进行乳化分散;将少量乙二胺溶解在欲滴加的去离子水中,在乳化分散过程中产生少量交联;进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮。本发明方法简单、成本低廉,获得的环氧改性水性聚氨酯涂料性能稳定、分散性好。
Description
技术领域
本发明涉及有机涂料合成技术领域,尤其涉及一种环氧改性水性聚氨酯合成方法。
背景技术
聚氨酯制备过程中的水性化,即以水代替有机溶剂,不仅提高了生产和施工的安全性,避免了有机溶剂的可燃性和毒性,而且减少或消除了聚氨酯使用过程中有机溶剂挥发带来的环境问题。同时,由于水性聚氨酯以水为介质,具有不燃、气味小、不污染、节能、操作加工方便等优点,水性聚氨酯的研究日益受到人们的广泛的重视。但水性聚氨酯涂膜的耐水性和耐溶剂性较差,在一定领域的使用中受到了限制。环氧树脂具有高模量、高强度和耐化学性好、热稳定性好等优点,而且可直接参与水性聚氨酯的合成反应,从而提高聚氨酯的耐水、耐溶剂、耐热蠕变性能及拉伸强度等。
发明内容
本发明所要解决的技术问题是提供一种方法简单、成本低廉,获得的环氧改性水性聚氨酯涂料性能稳定、分散性好的环氧改性水性聚氨酯合成方法。
本发明解决上述技术问题的技术方案如下:一种环氧改性水性聚氨酯合成方法,包括如下步骤:
利用一NC0基团和一0H基团的反应,合成交联结构的水性聚氨酯乳液;
在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡反应;
用滴液漏斗缓慢滴加1,4一丁二醇,滴加亲水扩链剂DMPA和环氧树脂,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂反应;
加入三乙胺搅拌中和,在快速搅拌的条件下滴加适量去离子水进行乳化分散;
将少量乙二胺溶解在欲滴加的去离子水中,在乳化分散过程中产生少量交联;
进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮。
在上述技术方案的基础上,本发明还可以做如下改进。
进一步,所述在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡反应步骤的具体实现如下:
在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡,在30~60℃条件下反应20~60min,然后升温至70~90℃恒温反应,整个预聚过程持续1~2h。
进一步,所述用滴液漏斗缓慢滴加1,4一丁二醇,滴加亲水扩链剂DMPA和环氧树脂,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂反应步骤的具体实现如下:
降温至70~75℃,用滴液漏斗缓慢滴加1,4一丁二醇,恒温反应0.5~1h;
降温至65~70℃,滴加亲水扩链剂DMPA和环氧树脂,恒温反应1~3h,加入丙酮控制黏度;
降温至60~65℃,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂,恒温反应1~3h。
进一步,所述加入三乙胺搅拌中和,在快速搅拌的条件下滴加适量去离子水进行乳化分散步骤的具体实现如下:
降温至60~65℃,加入三乙胺搅拌中和10~40min,在20~55℃条件下,快速搅拌的条件下滴加适量去离子水进行乳化分散。
进一步,所述进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮步骤的具体实现如下:
将体系温度升至60~70℃恒温10~40min,进行进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮。
本发明的有益效果是:方法简单、成本低廉,获得的环氧改性水性聚氨酯涂料性能稳定、分散性好。
具体实施方式
以下结合实例对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。
一种环氧改性水性聚氨酯合成方法,包括如下步骤:
利用一NC0基团和一0H基团的反应,合成交联结构的水性聚氨酯乳液;
在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡反应;
用滴液漏斗缓慢滴加1,4一丁二醇,滴加亲水扩链剂DMPA和环氧树脂,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂反应;
加入三乙胺搅拌中和,在快速搅拌的条件下滴加适量去离子水进行乳化分散;
将少量乙二胺溶解在欲滴加的去离子水中,在乳化分散过程中产生少量交联;
进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮。
实施例1:
利用一NC0基团和一0H基团的反应,合成交联结构的水性聚氨酯乳液;在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡,在30℃条件下反应20min,然后升温至70℃恒温反应,整个预聚过程持续1h;降温至70℃,用滴液漏斗缓慢滴加1,4一丁二醇,恒温反应0.5h;降温至65℃,滴加亲水扩链剂DMPA和环氧树脂,恒温反应1h,加入丙酮控制黏度;降温至60℃,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂,恒温反应1h;降温至60℃,加入三乙胺搅拌中和10min,在20℃条件下,快速搅拌的条件下滴加适量去离子水进行乳化分散;将体系温度升至60℃恒温10min,进行进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮。
实施例2:
利用一NC0基团和一0H基团的反应,合成交联结构的水性聚氨酯乳液;在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡,在50℃条件下反应30min,然后升温至80℃恒温反应,整个预聚过程持续1.5h;降温至72℃,用滴液漏斗缓慢滴加1,4一丁二醇,恒温反应0.55h;降温至68℃,滴加亲水扩链剂DMPA和环氧树脂,恒温反应2h,加入丙酮控制黏度;降温至62℃,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂,恒温反应2h;降温至63℃,加入三乙胺搅拌中和30min,在35℃条件下,快速搅拌的条件下滴加适量去离子水进行乳化分散;将体系温度升至65℃恒温30min,进行进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮。
实施例3:
利用一NC0基团和一0H基团的反应,合成交联结构的水性聚氨酯乳液;在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡,在60℃条件下反应60min,然后升温至90℃恒温反应,整个预聚过程持续2h;降温至75℃,用滴液漏斗缓慢滴加1,4一丁二醇,恒温反应1h;降温至70℃,滴加亲水扩链剂DMPA和环氧树脂,恒温反应3h,加入丙酮控制黏度;降温至65℃,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂,恒温反应3h;降温至65℃,加入三乙胺搅拌中和40min,在55℃条件下,快速搅拌的条件下滴加适量去离子水进行乳化分散;将体系温度升至70℃恒温40min,进行进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种环氧改性水性聚氨酯合成方法,其特征在于,包括如下步骤:
利用一NC0基团和一0H基团的反应,合成交联结构的水性聚氨酯乳液;
在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡反应;
用滴液漏斗缓慢滴加l,4一丁二醇,滴加亲水扩链剂DMPA和环氧树脂,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂反应;
加入三乙胺搅拌中和,在快速搅拌的条件下滴加适量去离子水进行乳化分散;
将少量乙二胺溶解在欲滴加的去离子水中,在乳化分散过程中产生少量交联;
进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮。
2.根据权利要求1所述一种环氧改性水性聚氨酯合成方法,其特征在于,所述在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡反应步骤的具体实现如下:
在四口烧瓶中,一次加入一定量的TDI和聚醚二元醇,滴入适量催化剂二丁基二月桂酸锡,在30~60℃条件下反应20~60min,然后升温至70~90℃恒温反应,整个预聚过程持续1~2h。
3. 根据权利要求1所述一种环氧改性水性聚氨酯合成方法,其特征在于,所述用滴液漏斗缓慢滴加l,4一丁二醇,滴加亲水扩链剂DMPA和环氧树脂,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂反应步骤的具体实现如下:
降温至70~75℃,用滴液漏斗缓慢滴加l,4一丁二醇,恒温反应0.5~1h;
降温至65~70℃,滴加亲水扩链剂DMPA和环氧树脂,恒温反应1~3h,加入丙酮控制黏度;
降温至60~65℃,加入丙烯酸羟丙酯、适量的阻聚剂和催化剂,恒温反应1~3h。
4. 根据权利要求1所述一种环氧改性水性聚氨酯合成方法,其特征在于,所述加入三乙胺搅拌中和,在快速搅拌的条件下滴加适量去离子水进行乳化分散步骤的具体实现如下:
降温至60~65℃,加入三乙胺搅拌中和10~40min,在20~55℃条件下,快速搅拌的条件下滴加适量去离子水进行乳化分散。
5. 根据权利要求1所述一种环氧改性水性聚氨酯合成方法,其特征在于,所述进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮步骤的具体实现如下:
将体系温度升至60~70℃恒温10~40min,进行进一步的交联,合成含不饱和双键的环氧改性水性聚氨酯溶液,最后减压蒸去丙酮。
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