CN107828039A - 水性聚氨酯分散体的制备方法 - Google Patents

水性聚氨酯分散体的制备方法 Download PDF

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CN107828039A
CN107828039A CN201711074757.5A CN201711074757A CN107828039A CN 107828039 A CN107828039 A CN 107828039A CN 201711074757 A CN201711074757 A CN 201711074757A CN 107828039 A CN107828039 A CN 107828039A
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methyl propane
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王耀斌
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Shaanxi Shengmai Petroleum Co Ltd
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Abstract

本发明公开一种水性聚氨酯分散体的制备方法，包括以下步骤：（1）将三羟基甲基丙烷、月桂酸、二甲苯搅拌混合，升温，加入催化剂，回流反应，然后在260℃下反应，得到扩链剂三羟甲基丙烷月桂酸单酯；（2）将聚醚二醇和异佛尔酮二异氰酸酯混合，在75℃下反应，后降温至70℃，然后加入步骤（1）得到的扩链剂反应；（3）加入二羟基甲基丙酸和三羟基甲基丙烷，反应，得到聚氨酯预聚体；（4）将聚氨酯预聚体冷却至40‑50℃，加入三乙胺，搅拌，加入乙二胺扩链反应，真空干燥，即得到水性聚氨酯分散体。本发明制备得到的水性聚氨酯分散体的助成膜能力强，可取代小分子成膜助剂，制备超低VOC含量水性木器涂料。

Description

水性聚氨酯分散体的制备方法
技术领域
本发明属于聚氨酯技术领域，具体涉及一种水性聚氨酯分散体的制备方法。
背景技术
水性木器涂料常用高玻璃转化温度（Tg）的聚丙烯酸酯乳液（PA）为成膜物，需加5%～15%的有机小分子溶剂辅助成膜，使涂料中挥发性有机化合物（VOC）含量居高不下，难以满足环保法规日益严格的要求。通常，采用活性成膜助剂、核壳聚合物乳液和软/硬聚合物乳液复配技术来降低涂料最低成膜温度（MFT）和VOC 含量。有研究发现甲基丙烯酸双环戊二烯氧基乙酯（DPOMA）类活性成膜助剂，能在钴催化剂作用下参与成膜，但其助成膜能力不足，还会降低乳液及涂料的贮存稳定性。现有能在5℃或以下成膜的核壳结构PA，其涂膜硬度不高，而采用乳液复配技术降低水性涂料VOC 含量成为研究热点。
聚氨酯水分散体（PUD）的软段玻璃化温度低至零下60℃，赋予其优异的低温成膜性能。同时，改变PUD 憎水和亲水链段的比例和结构，可调控PUD 成膜性及与其他树脂的相容性。
但是，目前水性聚氨酯的成膜能力差，而且得率低，导致生产成本高。
发明内容
针对现有技术的缺陷，本发明提供一种水性聚氨酯分散体的制备方法。
水性聚氨酯分散体的制备方法，包括以下步骤：
（1）将三羟基甲基丙烷、月桂酸、二甲苯搅拌混合，升温至180-200℃，加入催化剂，回流反应4-5h，然后在260℃下反应4h，得到扩链剂三羟甲基丙烷月桂酸单酯；
（2）将聚醚二醇和异佛尔酮二异氰酸酯混合，在75℃下反应2-3h，后降温至70℃，然后加入步骤（1）得到的三羟甲基丙烷月桂酸单酯进行扩链反应2h；
（3）向步骤（2）的产物中加入二羟基甲基丙酸和三羟基甲基丙烷，反应30min，得到聚氨酯预聚体；
（4）将聚氨酯预聚体冷却至40-50℃，加入三乙胺中和反应3min，在3000rpm的转速下搅拌反应30min，然后加入乙二胺扩链反应20-40min，在60℃下真空干燥3h，即得到水性聚氨酯分散体。
优选地，步骤（1）中的催化剂为N-乙基吡咯烷酮。
优选地，步骤（1）中，三羟基甲基丙烷、月桂酸、二甲苯、催化剂的质量比为20:9:5:1。
优选地，步骤（2）中聚醚二醇、异佛尔酮二异氰酸酯、步骤（1）得到的三羟甲基丙烷月桂酸单酯的质量比为6：5：1。
优选地，步骤（3）中，步骤（2）的产物、二羟基甲基丙酸、三羟基甲基丙烷的质量比为15:9:8。
本发明的优点：
本发明先合成了含长支链的新型二元醇扩链剂三羟甲基丙烷月桂酸单酯，通过预聚体分散法合成新型水性聚氨酯分散体，该水性聚氨酯分散体的助成膜能力强，VOC含量低至30g/L，可取代小分子成膜助剂，制备超低VOC 含量水性木器涂料。
具体实施方式
实施例1
水性聚氨酯分散体的制备方法，包括以下步骤：
（1）将三羟基甲基丙烷、月桂酸、二甲苯搅拌混合，升温至180℃，加入催化剂N-乙基吡咯烷酮，回流反应4h，然后在260℃下反应4h，得到扩链剂三羟甲基丙烷月桂酸单酯；其中，三羟基甲基丙烷、月桂酸、二甲苯、催化剂的质量比为20:9:5:1；
（2）将聚醚二醇和异佛尔酮二异氰酸酯混合，在75℃下反应2h，后降温至70℃，然后加入步骤（1）得到的三羟甲基丙烷月桂酸单酯进行扩链反应2h；其中，步骤（2）中聚醚二醇、异佛尔酮二异氰酸酯、步骤（1）得到的三羟甲基丙烷月桂酸单酯的质量比为6：5：1；
（3）向步骤（2）的产物中加入二羟基甲基丙酸和三羟基甲基丙烷，反应30min，得到聚氨酯预聚体；其中，步骤（2）的产物、二羟基甲基丙酸、三羟基甲基丙烷的质量比为15:9:8；
（4）将聚氨酯预聚体冷却至40-50℃，加入三乙胺中和反应3min，在3000rpm的转速下搅拌反应30min，然后加入乙二胺扩链反应20min，在60℃下真空干燥3h，即得到水性聚氨酯分散体。
实施例2
水性聚氨酯分散体的制备方法，包括以下步骤：
（1）将三羟基甲基丙烷、月桂酸、二甲苯搅拌混合，升温至200℃，加入催化剂N-乙基吡咯烷酮，回流反应5h，然后在260℃下反应4h，得到扩链剂三羟甲基丙烷月桂酸单酯；其中，三羟基甲基丙烷、月桂酸、二甲苯、催化剂的质量比为20:9:5:1；
（2）将聚醚二醇和异佛尔酮二异氰酸酯混合，在75℃下反应3h，后降温至70℃，然后加入步骤（1）得到的三羟甲基丙烷月桂酸单酯进行扩链反应2h；其中，步骤（2）中聚醚二醇、异佛尔酮二异氰酸酯、步骤（1）得到的三羟甲基丙烷月桂酸单酯的质量比为6：5：1；
（3）向步骤（2）的产物中加入二羟基甲基丙酸和三羟基甲基丙烷，反应30min，得到聚氨酯预聚体；其中，步骤（2）的产物、二羟基甲基丙酸、三羟基甲基丙烷的质量比为15:9:8；
（4）将聚氨酯预聚体冷却至40-50℃，加入三乙胺中和反应3min，在3000rpm的转速下搅拌反应30min，然后加入乙二胺扩链反应40min，在60℃下真空干燥3h，即得到水性聚氨酯分散体。
实施例3
水性聚氨酯分散体的制备方法，包括以下步骤：
（1）将三羟基甲基丙烷、月桂酸、二甲苯搅拌混合，升温至190℃，加入催化剂N-乙基吡咯烷酮，回流反应4.5h，然后在260℃下反应4h，得到扩链剂三羟甲基丙烷月桂酸单酯；其中，三羟基甲基丙烷、月桂酸、二甲苯、催化剂的质量比为20:9:5:1；
（2）将聚醚二醇和异佛尔酮二异氰酸酯混合，在75℃下反应2.5h，后降温至70℃，然后加入步骤（1）得到的三羟甲基丙烷月桂酸单酯进行扩链反应2h；其中，步骤（2）中聚醚二醇、异佛尔酮二异氰酸酯、步骤（1）得到的三羟甲基丙烷月桂酸单酯的质量比为6：5：1；
（3）向步骤（2）的产物中加入二羟基甲基丙酸和三羟基甲基丙烷，反应30min，得到聚氨酯预聚体；其中，步骤（2）的产物、二羟基甲基丙酸、三羟基甲基丙烷的质量比为15:9:8；
（4）将聚氨酯预聚体冷却至40-50℃，加入三乙胺中和反应3min，在3000rpm的转速下搅拌反应30min，然后加入乙二胺扩链反应30min，在60℃下真空干燥3h，即得到水性聚氨酯分散体。

Claims (5)

1.水性聚氨酯分散体的制备方法，其特征在于：包括以下步骤：
（1）将三羟基甲基丙烷、月桂酸、二甲苯搅拌混合，升温至180-200℃，加入催化剂，回流反应4-5h，然后在260℃下反应4h，得到扩链剂三羟甲基丙烷月桂酸单酯；
（2）将聚醚二醇和异佛尔酮二异氰酸酯混合，在75℃下反应2-3h，后降温至70℃，然后加入步骤（1）得到的三羟甲基丙烷月桂酸单酯进行扩链反应2h；
（3）向步骤（2）的产物中加入二羟基甲基丙酸和三羟基甲基丙烷，反应30min，得到聚氨酯预聚体；
（4）将聚氨酯预聚体冷却至40-50℃，加入三乙胺中和反应3min，在3000rpm的转速下搅拌反应30min，然后加入乙二胺扩链反应20-40min，在60℃下真空干燥3h，即得到水性聚氨酯分散体。
2.根据权利要求1所述水性聚氨酯分散体的制备方法，其特征在于：步骤（1）中的催化剂为N-乙基吡咯烷酮。
3.根据权利要求2所述水性聚氨酯分散体的制备方法，其特征在于：步骤（1）中，三羟基甲基丙烷、月桂酸、二甲苯、催化剂的质量比为20:9:5:1。
4.根据权利要求1所述水性聚氨酯分散体的制备方法，其特征在于：步骤（2）中聚醚二醇、异佛尔酮二异氰酸酯、步骤（1）得到的三羟甲基丙烷月桂酸单酯的质量比为6：5：1。
5.根据权利要求1所述水性聚氨酯分散体的制备方法，其特征在于：步骤（3）中，步骤（2）的产物、二羟基甲基丙酸、三羟基甲基丙烷的质量比为15:9:8。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109054610A (zh) * 2018-07-11 2018-12-21 合肥伊只门窗有限公司 一种铝合金门窗用防腐涂料及其制备方法
CN110713592A (zh) * 2018-07-11 2020-01-21 广东华润涂料有限公司 包含聚醚改性聚酯的高固低粘树脂组合物

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109054610A (zh) * 2018-07-11 2018-12-21 合肥伊只门窗有限公司 一种铝合金门窗用防腐涂料及其制备方法
CN110713592A (zh) * 2018-07-11 2020-01-21 广东华润涂料有限公司 包含聚醚改性聚酯的高固低粘树脂组合物

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