CN105906798A - 一种低粘度硬泡聚醚的制备方法 - Google Patents

一种低粘度硬泡聚醚的制备方法 Download PDF

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CN105906798A
CN105906798A CN201610489281.0A CN201610489281A CN105906798A CN 105906798 A CN105906798 A CN 105906798A CN 201610489281 A CN201610489281 A CN 201610489281A CN 105906798 A CN105906798 A CN 105906798A
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翟洪金
应珏
郑磊
王飞
于文超
栾春晖
任翠环
李培
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Jurong Ningwu New Material Co Ltd
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    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
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    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
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Abstract

本发明公开了一种低粘度硬泡聚醚的制备方法，是由三乙烯四胺与季戊四醇共起始剂在碱性催化剂的作用下与氧化烯烃反应制得。将三乙烯四胺与季戊四醇作为共起始剂按照一定比例加入反应器中，加入催化剂，在一定温度、压力下通入氧化烯烃反应制得官能度4～6的硬泡聚醚多元醇。采用该方法制得的聚醚多元醇生产的聚氨酯泡沫耐热性与尺寸稳定性较好。

Description

一种低粘度硬泡聚醚的制备方法
技术领域
本发明属于有机高分子化合物的制备方法，具体的说是一种聚氨酯用低粘度硬泡聚醚的制备方法。
背景技术
聚醚多元醇是制备聚氨酯材料的重要原料，粘度较高的硬泡聚醚多元醇流动性差，与其他发泡组分相溶性差。
发明内容
本发明的目的是提供一种低粘度硬泡聚醚的制备方法，采用该聚醚制备的聚氨酯泡沫塑料泡沫耐热性与尺寸稳定性较好。
本发明的目的是通过以下技术方案来实现的：
一种低粘度硬泡聚醚的制备方法，其特征在于：该方法以三乙烯四胺、季戊四醇为共起始剂，氢氧化钾为催化剂；与环氧丙烷开环聚合反应，包括如下步骤：
1）将三乙烯四胺、季戊四醇、氢氧化钾投入到反应器中，然后在惰性气体保护下，115-125℃通入环氧丙烷，环氧丙烷投加结束后，搅拌1-3小时，使充分反应，然后抽真空，冷却后制得粗聚醚；其中，原料重量份数为：三乙烯四胺10；季戊四醇1-10；氢氧化钾0.5-1；环氧丙烷50-100；
2）将粗聚醚投入到反应器中，加入水，控制温度在80-90℃，搅拌1-2小时后加入磷酸中和，搅拌1-2小时，然后加入占粗聚醚质量份数1%的精制吸附剂升温至120-130℃，进行真空脱水，水份合格后经过过滤得到低粘度硬泡聚醚。水份合格是指水份质量份数低于0.05%。
步骤1）中，三乙烯四胺和季戊四醇为共起始剂，比例为三乙烯四胺：季戊四醇=10：1～1：1。
本发明通过以三乙烯四胺和季戊四醇为共起始剂制得低粘度的硬泡聚醚，通过调整共起始剂的比例可以得到不同粘度的硬泡聚醚多元醇。制得的硬泡聚醚应用在聚氨酯泡沫中，生产的聚氨酯泡沫耐热性与尺寸稳定性较好。
具体实施方式
下面通过具体实施例对本发明作进一步的说明，但各实施例均不是对本发明的具体限制。
实施例1
一种低粘度硬泡聚醚的制备方法，以三乙烯四胺、季戊四醇为共起始剂；氢氧化钾为催化剂；与环氧丙烷开环聚合反应制备。包括如下步骤：
①原料重量份数为三乙烯四胺10份；季戊四醇1份，氢氧化钾（江苏优利德化工有限公司）0.5份；环氧丙烷（利安德公司）50份；
②将三乙烯四胺、季戊四醇、氢氧化钾投入到反应器中，然后在惰性气体保护下，115-125℃通入环氧丙烷，环氧丙烷投加结束后，搅拌1-3小时，使充分反应，然后抽真空，冷却后制得粗聚醚。
③将粗聚醚投入到反应器中，加入定量的水，控制温度在80-90℃，搅拌1-2小时后加入磷酸中和，保证溶液中性。搅拌1-2小时，然后加入占粗聚醚质量份数1%的精制吸附剂（精制吸附剂生产厂家为枣阳市永华化工有限公司，牌号为ZH-AD100NS），升温至120-130℃，进行真空除水，水份合格后经过过滤得到低粘度硬泡聚醚。水份合格是指水份质量份数低于0.05%。羟值360mgKOH/g，粘度4100mPa.s。该聚醚粘度适中，应用方便，用其制备的聚氨酯泡沫塑料泡沫耐热性与尺寸稳定性较好。
实施例2
一种低粘度硬泡聚醚的制备方法，以三乙烯四胺、季戊四醇为共起始剂；氢氧化钾为催化剂；与环氧丙烷开环聚合反应制备。包括如下步骤：
①原料重量份数为三乙烯四胺10份；季戊四醇10份，氢氧化钾（江苏优利德化工有限公司）1份；环氧丙烷（利安德公司）100份；
②将三乙烯四胺、季戊四醇、氢氧化钾投入到反应器中，然后在惰性气体保护下，115-125℃通入环氧丙烷，环氧丙烷投加结束后，搅拌1-3小时，使充分反应，然后抽真空，冷却后制得粗聚醚。
③将粗聚醚投入到反应器中，加入定量的水，控制温度在80-90℃，搅拌1-2小时后加入磷酸中和，搅拌1-2小时，然后加入精制吸附剂升温至120-130℃，进行真空除水，然后经过过滤得到低粘度硬泡聚醚，羟值280mgKOH/g，粘度3200mPa.s。该聚醚粘度适中，应用方便，用其制备的聚氨酯泡沫塑料泡沫耐热性与尺寸稳定性较好。

Claims (3)

1.一种低粘度硬泡聚醚的制备方法，其特征在于：该方法以三乙烯四胺、季戊四醇为共起始剂，氢氧化钾为催化剂；与环氧丙烷开环聚合反应，包括如下步骤：
1）将三乙烯四胺、季戊四醇、氢氧化钾投入到反应器中，然后在惰性气体保护下，115-125℃通入环氧丙烷，环氧丙烷投加结束后，搅拌1-3小时，使充分反应，然后抽真空，冷却后制得粗聚醚；其中，原料重量份数为：三乙烯四胺10；季戊四醇1-10；氢氧化钾0.5-1；环氧丙烷50-100；
2）将粗聚醚投入到反应器中，加入水，控制温度在80-90℃，搅拌1-2小时后加入磷酸中和，搅拌1-2小时，然后加入占粗聚醚质量份数1%的精制吸附剂升温至120-130℃，进行真空脱水，水份合格后经过过滤得到低粘度硬泡聚醚。
2.根据权利要求1所述的低粘度硬泡聚醚的制备方法，其特征在于：步骤1）中，三乙烯四胺和季戊四醇为共起始剂，比例为三乙烯四胺：季戊四醇=10：1～1：1。
3.根据权利要求1所述的低粘度硬泡聚醚的制备方法，其特征在于：水份合格是指水份质量分数低于0.05%。
CN201610489281.0A 2016-06-29 2016-06-29 一种低粘度硬泡聚醚的制备方法 Pending CN105906798A (zh)

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CN114874425B (zh) * 2022-05-13 2023-10-13 万华化学（宁波）有限公司 一种胺基聚醚多元醇及其制备方法

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Application publication date: 20160831