CN105968333A - 一种均苯四甲酸类聚酯多元醇的制备方法 - Google Patents

一种均苯四甲酸类聚酯多元醇的制备方法 Download PDF

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CN105968333A
CN105968333A CN201610313550.8A CN201610313550A CN105968333A CN 105968333 A CN105968333 A CN 105968333A CN 201610313550 A CN201610313550 A CN 201610313550A CN 105968333 A CN105968333 A CN 105968333A
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周家仁
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    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
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Abstract

一种均苯四甲酸类聚酯多元醇的制备方法，其特征是：选用均苯四甲酸酐和小分子二元醇加入反应物，通过开环聚合反应制得;方法是：将均苯四甲酸酐、小分子二元醇、催化剂投入聚酯反应瓶中，通过n2保护，缓慢升温至230～240度c，当酸值≤20mgkch/g时，抽真空，待产物酸值≤1.5mgkoh/g时停止反应；冷却至90度c以下压滤出料，即得均苯四甲酸类聚酯多元醇，数据：羟值200‑450mgkoh/g、酸值0.9～1.5mgkoh/g，由于苯环的引入，均苯四甲酸类聚酯多元醇对于聚氨酯泡沫材料的阻燃性能有所提高。

Description

一种均苯四甲酸类聚酯多元醇的制备方法
技术领域
本发明涉及化工合成技术领域，尤其是一种均苯四甲酸类聚酯多元醇的制备方法。
背景技术
聚酯多元醇是聚氨酯泡沬材料的主要原材料之一，聚氨酯泡沬的性能好坏与聚酯多元醇的质量有着密不可分的关系，未经处理的硬质聚氨酯泡沫的性能存在着一些缺陷，比如阻燃性能差，强度不高，耐巷化性能较弱等，通过提升聚酯多元醇的质量来改善聚氨酯泡沫材料的性能是研究者一直所重视的工作。本发明是通过合成均苯四甲酸酐类聚酯多元醇。均苯四甲酸类聚酯多元醇是一种高性能的聚酯多元醇，真与异青酸酯反应制得的聚氨酯硬泡沫具有尺寸稳定性好，阻燃性能优异以及耐老化性能好等优点。
发明内容
本发明的目的就是为了解决上述技术的不足而设计的一种均苯四甲酸类聚酯多元醇的制备方法。
为了实现上述目的，一种均苯四甲酸类聚酯多元醇采用了如下技术方案,以提高聚氨酯泡沫材料的性能。
一种均苯四甲酸类聚酯多元醇的制备方法，其特征是：包括以下步骤，将均苯四甲酸酐、二元醇和催化剂依次加入四口烧瓶中，通氮气密封、加热，当温度升至130～155度c时调节加热速率，控制回流塔顶温度在100～102度c，控制冷凝器出水速度，防止水蒸气将小量二元醇带出分流冷凝器；将温度缓幔升至175～180度c，保温2～4h，然后将温度升至210～220度c，当水分完全停止后，酯化反应基本完成，停止通冷却水，抽真空，降温，制得均苯四甲酸类聚脂多元醇；所述均苯四甲酸类聚酯多元醇，羟值为200～450mg空号/g，酸值≤1.5mgkoh/g，含水率≤0.03%
所述的一种均苯四甲酸类聚酯多元醇的制备方法，其特征是：所述均苯四甲酪酐与二元醇的摩尔比为1：4～1：1：6。
所述的一种均苯四甲酸类聚酯多元醇的制备方法，其特是：所述二元醇为乙二醇、1.4丁二醇或一缩二乙二醇的一种或者多种。
所述的一种均苯四甲酸类聚酯多元醇的制备方法，其特征是：所述与催化剂的重量比为100：0.03～0.1。
所述的一种均苯四甲酸类聚酯多元醇的制备方法,其特征是：所述催化剂氟钛酸钾或二丁基氧化锡。
本发明所得到的一种均苯四甲酸类聚酯多元醇的制备方法的有益效果是：由于苯环的引入，均苯四甲酸类聚酯多元醇对于聚氨酯泡沫材料的阻燃性能有所提高，多功能度的结构利于生产交联度高的泡沫材料，对于泡沫材料的强度和耐老化性能均有所提高。
具体实施方式
下面通过实施例对本发明作进一步的描述。
实施例1
本发明公开的一种均苯四甲酸类聚酯多元醇的制备方法,其特征是：包括以下步骤，将均苯四甲酸酐、二元醇和催化剂依次加入四口烧瓶中，通氮气密封、加热，当温度升至130～155度c时调节加热速率，控制回流塔顶温度在100～102度c，控制冷凝器出水速度，防止水蒸气将小量二元醇带出分流冷凝器；将温度缓幔升至175～180度c，保温2～4h，然后将温度升至210～220度c，当水分完全停止后，酯化反应基本完成，停止通冷却水，抽真空，降温，制得均苯四甲酸类聚脂多元醇；所述均苯四甲酸类聚酯多元醇，羟值为200～450mg空号/g，酸值≤1.5mgkoh/g，含水率≤0.03%
所述的一种均苯四甲酸类聚酯多元醇的制备方法，其特征是：所述均苯四甲酪酐与二元醇的摩尔比为1：4～1：1：6。
所述的一种均苯四甲酸类聚酯多元醇的制备方法，其特是：所述二元醇为乙二醇、1.4丁二醇或一缩二乙二醇的一种或者多种。
所述的一种均苯四甲酸类聚酯多元醇的制备方法，其特征是：所述与催化剂的重量比为100：0.03～0.1。
所述的一种均苯四甲酸类聚酯多元醇的制备方法,其特征是：所述催化剂氟钛酸钾或二丁基氧化锡。
本发明所得到的一种均苯四甲酸类聚酯多元醇的制备方法的有益效果是：由于苯环的引入，均苯四甲酸类聚酯多元醇对于聚氨酯泡沫材料的阻燃性能有所提高，多功能度的结构利于生产交联度高的泡沫材料，对于泡沫材料的强度和耐老化性能均有所提高。
本文中所描述的具体实施例仅仅是对本发明的构思作举例说明。本发明所属技术领域的技术人员可以对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，但并不会偏离本发明的精神或者超越所附权利要求书所定义的范围。

Claims (4)

1.一种均苯四甲酸类聚酯多元醇的制备方法，其特征是：包括以下步骤，将均苯四甲酸酐、二元醇和催化剂依次加入四口烧瓶中，通氮气密封、加热，当温度升至130～155度c时调节加热速率，控制回流塔顶温度在100～102度c，控制冷凝器出水速度，防止水蒸气将小量二元醇带出分流冷凝器；将温度缓幔升至175～180度c，保温2～4h，然后将温度升至210～220度c，当水分完全停止后，酯化反应基本完成，停止通冷却水，抽真空，降温，制得均苯四甲酸类聚脂多元醇；所述均苯四甲酸类聚酯多元醇，羟值为200～450mg空号/g，酸值≤1.5mgkoh/g，含水率≤0.03，所述均苯四甲酪酐与二元醇的摩尔比为1：4～1：1：6。
2.根据权利要求1所述的一种均苯四甲酸类聚酯多元醇的制备方法，其特是：所述二元醇为乙二醇、1.4丁二醇或一缩二乙二醇的一种或者多种。
3.根据权利要求1所述的一种均苯四甲酸类聚酯多元醇的制备方法，其特征是：所述与催化剂的重量比为100：0.03～0.1。
4.根据权利要求1所述的一种均苯四甲酸类聚酯多元醇的制备方法,其特征是：所述催化剂氟钛酸钾或二丁基氧化锡。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108467478A (zh) * 2018-04-20 2018-08-31 范月娥 一种均苯四甲酸类聚酯多元醇的制作
CN111164122A (zh) * 2017-07-07 2020-05-15 斯蒂潘公司 用于聚氨酯应用的低粘度多元醇

Citations (1)

* Cited by examiner, † Cited by third party
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CN104910356A (zh) * 2015-07-07 2015-09-16 北京市建筑工程研究院有限责任公司 一种均苯四甲酸类聚酯多元醇的制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104910356A (zh) * 2015-07-07 2015-09-16 北京市建筑工程研究院有限责任公司 一种均苯四甲酸类聚酯多元醇的制备方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111164122A (zh) * 2017-07-07 2020-05-15 斯蒂潘公司 用于聚氨酯应用的低粘度多元醇
CN111164122B (zh) * 2017-07-07 2022-01-04 斯蒂潘公司 用于聚氨酯应用的低粘度多元醇
CN108467478A (zh) * 2018-04-20 2018-08-31 范月娥 一种均苯四甲酸类聚酯多元醇的制作

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