CN105860052A - 一种改善聚醚多元醇颜色的方法 - Google Patents

一种改善聚醚多元醇颜色的方法 Download PDF

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CN105860052A
CN105860052A CN201610490669.2A CN201610490669A CN105860052A CN 105860052 A CN105860052 A CN 105860052A CN 201610490669 A CN201610490669 A CN 201610490669A CN 105860052 A CN105860052 A CN 105860052A
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应珏
翟洪金
李怀阁
田永辉
陈映欧
欧阳春兰
潘慧
戴钰
张荣珍
陈瑾
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Jurong Ningwu New Material Co Ltd
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Abstract

本发明公开了一种改善聚醚多元醇颜色的方法，该方法采用二步法：在聚醚多元醇制备过程中的第一阶段结束后，即高压反应釜内起始剂与环氧乙烷反应结束后将脱色剂H2O2加入到反应釜内，加热升温，真空30分钟除去脱色剂；在聚醚多元醇制备结束后，将复配脱色剂加入至反应釜内，加热升温，然后过滤除去脱色剂，得颜色改善后的聚醚多元醇。本发明得到的聚醚多元醇具有产率高、可降低生产成本、过程操作简单、脱色剂易除去无杂质引入等优点。

Description

一种改善聚醚多元醇颜色的方法
技术领域
本发明涉及一种聚醚多元醇的制备方法，具体地说是一种提高聚醚多元醇产率、降低生产成本的改善聚醚多元醇颜色的方法。
背景技术
由于现有聚醚多元醇生产工艺是在高温、高压下通过起始剂与环氧乙烷和环氧丙烷聚合反应制得，反应过程不易观察，其中副反应低聚物不易控制，反应温度过高、反应时间过长都会影响产物的颜色，会导致产率不高、产物色度指标达不到要求、生产成本高等问题的产生。
发明内容
为了解决现有聚醚多元醇存在的色度问题，本发明的目的是提供一种改善聚醚多元醇颜色的方法，该方法在聚醚多元醇生产过程中将脱色剂分阶段加入到反应釜内，利用脱色剂优良的脱色能力达到改善聚醚多元醇颜色的目的，且该方法使用的脱色剂易去除不会影响聚醚的成分。
本发明的目的是通过以下技术方案来实现的：
一种改善聚醚多元醇颜色的方法，其特征在于该方法包括以下步骤：
1）在聚醚多元醇制备过程中的第一阶段结束后，即高压反应釜内起始剂与环氧乙烷或环氧丙烷在碱性催化下反应结束后将部分脱色剂加入到反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟除去脱色剂；
2）在聚醚多元醇制备结束后，将余下部分脱色剂加入至反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟，然后过滤除去脱色剂，得颜色改善后的聚醚多元醇；原料以起始剂、环氧乙烷或环氧丙烷重量100%计，其中起始剂占总量的0.4~6%，环氧乙烷或环氧丙烷占总量的1~95%，碱性催化剂用量为总量的0.2~5%，脱色剂为总量的0.2~8%。
本发明中，所述起始剂为含有活泼氢化合物，包括：胺类，所用的胺类为甲苯二胺或乙二胺；醇类，所用的醇类为烯丙基醇或丙三醇或山梨醇；糖类，所用糖类为蔗糖、葡萄糖、淀粉类；含有活泼氢的聚合物。
脱色剂为H2O2、活性炭、白土、吸附树脂的一种或它们的混合物，加入量为总量的0.2%~8%；其中，第一次加入量为脱色剂总量的20%~40%；第一次加入为H2O2，第二次加入为至少两种混合的复配脱色剂。
所述的碱性催化剂为氢氧化钠或氢氧化钾或氢氧化铯或它们的混合物，平均粒径处于60~425目，加入量为总量的0.2~5%。
该方法利用脱色剂的优良脱色能力，分阶段加入到聚醚多元醇的生产过程中，可显著改善聚醚多元醇的颜色。本发明得到的聚醚多元醇产率高、可降低生产成本、过程操作简单、色度好、无杂质引入、脱色剂易去除。
具体实施方式
实施例1
一种改善聚醚多元醇颜色的方法，由以下方法得到：
1）将30克乙二胺和6克氢氧化钾加入带有搅拌、冷凝装置的反应器中，加热升温，通入240克环氧丙烷，控制温度在115~145oC、压力在0.4MPa下，使其充分反应，将脱色剂H2O210克加入到反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟除去脱色剂。
2）控制温度在115~145oC、压力在0.4MPa下，通入320克环氧乙烷，充分反应后，将复配脱色剂H2O2和活性炭18克加入至反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟，然后过滤除去脱色剂，得颜色改善后的聚醚多元醇。
实施例2
一种改善聚醚多元醇颜色的方法，由以下方法得到：
1）将20克丙三醇和4克氢氧化钾加入带有搅拌、冷凝装置的反应器中，加热升温，通入160克环氧丙烷，控制温度在115~145oC、压力在0.4MPa下，使其充分反应，将脱色剂H2O28克加入到反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟除去脱色剂。
2）控制温度在115~145oC、压力在0.4MPa下，通入210克环氧乙烷，充分反应后，将复配脱色剂H2O2和活性炭20克加入至反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟，然后过滤除去脱色剂，得颜色改善后的聚醚多元醇。
实施例3
一种改善聚醚多元醇颜色的方法，由以下方法得到：
1）将30克甲苯二胺和6克氢氧化钾加入带有搅拌、冷凝装置的反应器中，加热升温，通入240克环氧丙烷，控制温度在115~145oC、压力在0.4MPa下，使其充分反应，将脱色剂H2O212克加入到反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟除去脱色剂。
2）控制温度在115~145oC、压力在0.4MPa下，通入320克环氧乙烷，充分反应后，将复配脱色剂H2O2和白土18克加入至反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟，然后过滤除去脱色剂，得颜色改善后的聚醚多元醇。
实施例4
一种改善聚醚多元醇颜色的方法，由以下方法得到：
1）将40克蔗糖和7克氢氧化钾加入带有搅拌、冷凝装置的反应器中，加热升温，通入320克环氧丙烷，控制温度在115~145oC、压力在0.4MPa下，使其充分反应，将脱色剂H2O214克加入到反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟除去脱色剂。
2）控制温度在115~145oC、压力在0.4MPa下，通入400克环氧乙烷，充分反应后，将复配脱色剂H2O2和活性炭22克加入至反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟，然后过滤除去脱色剂，得颜色改善后的聚醚多元醇。

Claims (4)

1.一种改善聚醚多元醇颜色的方法，其特征在于该方法包括以下步骤：
1）在聚醚多元醇制备过程中的第一阶段结束后，即高压反应釜内起始剂与环氧乙烷或环氧丙烷在碱性催化下反应结束后将部分脱色剂加入到反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟除去脱色剂；
2）在聚醚多元醇制备结束后，将余下部分脱色剂加入至反应釜内，搅拌1~3小时，加热升温，控制温度在120~165oC，真空30分钟，然后过滤除去脱色剂，得颜色改善后的聚醚多元醇；原料以起始剂、环氧乙烷或环氧丙烷重量100%计，其中起始剂占总量的0.4~6%，环氧乙烷或环氧丙烷占总量的1~95%，碱性催化剂用量为总量的0.2~5%，脱色剂为总量的0.2~8%。
2.根据权利要求1所述的改善聚醚多元醇颜色的方法，其特征在于：所述起始剂为含有活泼氢化合物，包括：胺类，所用的胺类为甲苯二胺或乙二胺；醇类，所用的醇类为烯丙基醇或丙三醇或山梨醇；糖类，所用糖类为蔗糖、葡萄糖、淀粉类；含有活泼氢的聚合物。
3.根据权利要求1所述的改善聚醚多元醇颜色的方法，其特征在于：脱色剂为H2O2、活性炭、白土、吸附树脂的一种或它们的混合物，加入量为总量的0.2%~8%；其中，第一次加入量为脱色剂总量的20%~40%；第一次加入为H2O2，第二次加入为至少两种混合的复配脱色剂。
4.根据权利要求1所述的改善聚醚多元醇颜色的方法，其特征在于：所述的碱性催化剂为氢氧化钠或氢氧化钾或氢氧化铯或它们的混合物，平均粒径处于60~425目，加入量为总量的0.2~5%。
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CN109534969B (zh) * 2018-11-19 2022-06-21 上海多纶化工有限公司 低环氧乙烷加成数仲醇聚氧乙烯醚的制备方法
CN111269093A (zh) * 2018-12-05 2020-06-12 上海多纶化工有限公司 仲醇聚氧乙烯醚的制备方法
CN111269093B (zh) * 2018-12-05 2022-10-11 上海多纶化工有限公司 仲醇聚氧乙烯醚的制备方法

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