CN106008952B - 硬泡聚醚多元醇的制备方法 - Google Patents

硬泡聚醚多元醇的制备方法 Download PDF

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CN106008952B
CN106008952B CN201610623902.XA CN201610623902A CN106008952B CN 106008952 B CN106008952 B CN 106008952B CN 201610623902 A CN201610623902 A CN 201610623902A CN 106008952 B CN106008952 B CN 106008952B
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polyether polyol
rigid
preparation
foam polyether
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CN106008952A (zh
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董伟
耿佃勇
荆晓东
孙言丛
荣若贵
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Zibo Dexin Lianbang Chemical Industry Co Ltd
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Zibo Dexin Lianbang Chemical Industry Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • 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
    • C08G65/26—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 from cyclic ethers and other compounds
    • C08G65/2603—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 from cyclic ethers and other compounds the other compounds containing oxygen
    • C08G65/2606—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 from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
    • C08G65/2609—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 from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/487—Polyethers containing cyclic groups
    • C08G18/4883—Polyethers containing cyclic groups containing cyclic groups having at least one oxygen atom in the ring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2110/00—Foam properties
    • C08G2110/0025—Foam properties rigid

Abstract

本发明涉及一种硬泡聚醚多元醇的制备方法，属于聚醚多元醇的制备技术领域。本发明所述的硬泡聚醚多元醇的制备方法，由以下重量份数的原料制成：蔗糖450‑600份，含活性氢的化合物100‑180份，催化剂12‑18份，分散剂300‑450份，环氧丙烷630‑790份。本发明简单易行，反应周期短，起始剂的转化率高，制得的聚醚多元醇的分子链分布更均匀。

Description

硬泡聚醚多元醇的制备方法
技术领域
本发明涉及一种硬泡聚醚多元醇的制备方法，属于聚醚多元醇的制备技术领域。
背景技术
硬泡聚醚多元醇多用于生产硬泡泡沫，广泛应用于保温保冷、喷涂施工、冰箱用隔热材料等领域，由于要求聚醚的官能度较高(5以上)，多用蔗糖或山梨醇作为起始剂，传统的硬泡聚醚多元醇存在反应周期较长，蔗糖或山梨醇的转化率较低等问题。
发明内容
本发明的目的是提供一种硬泡聚醚多元醇的制备方法，其简单易行，反应周期短，起始剂的转化率高，制得的聚醚多元醇的分子链分布更均匀。
本发明所述的硬泡聚醚多元醇的制备方法，由以下重量份数的原料制成：蔗糖450-600份，含活性氢的化合物100-180份，催化剂12-18份，分散剂300-450份，环氧丙烷630-790份。
所述含活性氢的化合物为丙二醇、二乙二醇、乙二醇或二丙二醇。
所述催化剂为二甲胺或乙二胺。
所述分散剂为德信联邦公司生产的分子量为2000-6000、OHV为30-40mgKOH/g、官能度为2-3的聚醚多元醇。具体制备过程中，先将环氧丙烷接枝到分子量3000，再将环氧丙烷和环氧乙烷混投接至分子量6000。
所述的硬泡聚醚多元醇的制备方法，包括以下步骤：将蔗糖、含活性氢的化合物和分散剂在20-30℃下搅拌溶解至均相，氮气置换，负压抽入催化剂，升温至50-60℃预滴30-60份的环氧丙烷，待压降后缓慢升温至90-110℃，连续通入剩余环氧丙烷，熟化3小时，脱单体得成品。
本发明中分散剂的加入使得制得的聚醚产品的反应更好更迅速，蔗糖的转化率更高，聚醚的分子量分布更加均匀，产品的质量性能较不加分散剂的传统硬泡聚醚更好。
本发明具有以下有益效果：
本发明简单易行，反应周期短，起始剂的转化率高，制得的聚醚多元醇的分子链分布更均匀。
具体实施方式
下面结合实施例对本发明作进一步的说明，但其并不限制本发明的实施。
实施例原料用量均为重量份数。
所述分散剂为德信联邦公司生产的分子量为2000-6000、OHV为30-40mgKOH/g、官能度为2-3的聚醚多元醇。
实施例1
将500份蔗糖、180份二丙二醇和350份分散剂在30℃下搅拌溶解至均相，氮气置换，负压抽入二甲胺12份，升温至55℃预滴40份的环氧丙烷，待压降后缓慢升温至105℃，连续通入剩余的680份环氧丙烷，熟化3小时，脱单体得成品。
所得产品的羟值为471.2mgKOH/g，酸值为0.047mgKOH/g，水分为0.029％，钾离子浓度为1ppm，色值为1GD，pH为6.34。
实施例2
将450份蔗糖、120份乙二醇和300份分散剂在20℃下搅拌溶解至均相，氮气置换，负压抽入二甲胺15份，升温至50℃预滴30份的环氧丙烷，待压降后缓慢升温至100℃，连续通入剩余的630份环氧丙烷，熟化3小时，脱单体得成品。
所得产品的羟值为468.9mgKOH/g，酸值为0.042mgKOH/g，水分为0.032％，钾离子浓度为1ppm,色值为1GD，pH为6.50。
实施例3
将600份蔗糖、100份丙二醇和450份分散剂在25℃下搅拌溶解至均相，氮气置换，负压抽入二甲胺18份，升温至60℃预滴50份的环氧丙烷，待压降后缓慢升温至110℃，连续通入剩余的790份环氧丙烷，熟化3小时，脱单体得成品。
所得产品的羟值为474.2mgKOH/g，酸值为0.041mgKOH/g，水分为0.019％，钾离子浓度为1ppm,色值为1GD，pH为6.57。

Claims (3)

1.一种硬泡聚醚多元醇的制备方法，其特征在于由以下重量份数的原料制成：蔗糖450-600份，含活性氢的化合物100-180份，催化剂12-18份，分散剂300-450份，环氧丙烷630-790份；
所述分散剂为分子量为2000-6000、OHV为30-40mgKOH/g、官能度为2-3的聚醚多元醇；
所述的硬泡聚醚多元醇的制备方法，包括以下步骤：将蔗糖、含活性氢的化合物和分散剂在20-30℃下搅拌溶解至均相，氮气置换，负压抽入催化剂，升温至50-60℃预滴30-60份的环氧丙烷，待压降后升温至90-110℃，连续通入剩余环氧丙烷，熟化3小时，脱单体得成品。
2.根据权利要求1所述的硬泡聚醚多元醇的制备方法，其特征在于：含活性氢的化合物为丙二醇、二乙二醇、乙二醇或二丙二醇。
3.根据权利要求1所述的硬泡聚醚多元醇的制备方法，其特征在于：催化剂为二甲胺或乙二胺。
CN201610623902.XA 2016-07-30 2016-07-30 硬泡聚醚多元醇的制备方法 Active CN106008952B (zh)

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