CN111995740A - 一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法 - Google Patents
一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法 Download PDFInfo
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Abstract
本发明公开了一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，包括以下步骤：将合成芳香族聚酯多元醇的原料放置到反应设备中进行氮气置换；对反应设备进行升温，使得芳香族聚酯多元醇原料进行酯化反应；对反应设备进行抽真空，然后进行降温出料，得到芳香族聚酯多元醇。本发明所述的一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，本发明制得的芳香族聚酯多元醇具有良好的戊烷相容性，可以用于预混戊烷体系的组合聚酯多元醇，用于对阻燃有较高要求的聚氨酯硬泡***，而且整个制备具有良好戊烷相容性芳香族聚酯多元醇的方法简单，使用效果相对于传统方式更好，且成本较低，能够便于人们大规模生产，带来更好的使用前景。
Description
技术领域
本发明涉及发泡剂领域，特别涉及一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法。
背景技术
聚氨酯硬泡被广泛应用于保温材料中，在需要高阻燃的应用场景中，芳香族聚酯多元醇被广泛使用，传统上发泡剂为141B，出于环保的压力，戊烷类发泡剂被用于替代141B等发泡剂，但戊烷类发泡剂与芳香族聚酯多元醇相容性极差，一般芳香族聚酯多元醇无法用于预混戊烷的***，只能适用于在线混合的场景，但相当部分的生产商由于设备限制，需要发泡剂预混好的产品，因此，现有的芳香族聚酯多元醇满足不了人们的使用要求，为此，我们提出一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法。
发明内容
本发明的主要目的在于提供一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，可以有效解决背景技术中的问题。
为实现上述目的，本发明采取的技术方案为：
一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，包括以下步骤：
(1)、将合成芳香族聚酯多元醇的原料放置到反应设备中进行氮气置换；
(2)、对反应设备进行升温，使得芳香族聚酯多元醇原料进行酯化反应；
(3)、对反应设备进行抽真空，然后进行降温出料，得到芳香族聚酯多元醇。
优选的，步骤(1)中合成芳香族聚酯多元醇的原料包括二元醇、三元醇、长碳链单羧酸以及苯酐或对苯二甲酸，长碳链单羧酸含量占芳香族聚酯多元醇重量比的5-25％。
优选的，三元醇为甘油或三羟甲基丙烷的一种或两种，二元醇为乙二醇、丙二醇、二乙二醇、二丙二醇、己二醇和新戊二醇中的一种或多种，长碳链单羧酸为油酸、亚油酸、硬脂酸和软脂酸中的一种或多种。
优选的，步骤(2)中反应设备升温至100-180℃，酯化反应的时间为3-8h。
优选的，步骤(2)中：酯化反应需要酯化催化剂，酯化催化剂为T9、T12、T120和酞酸酯中的一种，酯化催化剂为合成芳香族聚酯多元醇的原料的0.01％-0.2％。
优选的，步骤(3)中抽真空时的温度为125-135℃，抽真空的时间为2.5-3.5h，得到的芳香族聚酯多元醇的羟值为150-350mgKOH/g。
戊烷指的是环戊烷、正戊烷和异戊烷。
与现有技术相比，本发明具有如下有益效果：该一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，本发明制得的芳香族聚酯多元醇具有良好的戊烷相容性，可以用于预混戊烷体系的组合聚酯多元醇，用于对阻燃有较高要求的聚氨酯硬泡***，而且整个制备具有良好戊烷相容性芳香族聚酯多元醇的方法简单，操作方便，使用效果相对于传统方式更好，而且成本较低，能够便于人们大规模生产。
附图说明
图1为本发明一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法的整体结构流程图。
具体实施方式
为使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施方式，进一步阐述本发明。
实施例1
在1.5L4口烧瓶中接上分水器、搅拌器、冷凝器、温度计和电加热器，加入70g甘油、450g二丙二醇、150g硬脂酸、350g苯酐和0.2gT9，氮气置换后升温至150℃进行酯化反应，5h后降温到130℃抽真空3h，降温出料，得到棕黄色透明产品，对棕黄色透明产品进行检测，羟值测试结果为220mgKOH/g，粘度为9000cps(25℃)。
实施例2
在1.5L4口烧瓶中接上分水器、搅拌器、冷凝器、温度计和电加热器，加入70g甘油、450g二丙二醇、100g软脂酸、350g苯酐和0.2gT9，氮气置换后升温至150℃进行酯化反应，5h后降温到130℃抽真空3h，降温出料，得到棕黄色透明产品，羟值测试结果为250mgKOH/g，粘度为12000cps(25℃)。
实施例3
在1.5L4口烧瓶中接上分水器、搅拌器、冷凝器、温度计和电加热器，加入70g甘油、400g二丙二醇、200g油酸、350g苯酐和0.2gT9，氮气置换后升温至150℃进行酯化反应，5h后降温到130℃抽真空3h，降温出料，得到棕黄色透明产品，羟值测试结果为170mgKOH/g，粘度为13000cps(25℃)。
实施例4
在1.5L4口烧瓶中接上分水器、搅拌器、冷凝器、温度计和电加热器，加入100g甘油、400g二丙二醇、100g硬脂酸、450g对苯二甲酸和0.2gT9，氮气置换后升温至150℃进行酯化反应，5h后降温到130℃抽真空3h，降温出料，得到棕黄色透明产品，羟值测试结果为210mgKOH/g，粘度为12000cps(25℃)。
实施例5
在1.5L4口烧瓶中接上分水器、搅拌器、冷凝器、温度计和电加热器，加入100g甘油、400g二乙二醇、150g油酸、500g对苯二甲酸和0.2gT9，氮气置换后升温至150℃进行酯化反应，5h后降温到130℃抽真空3h，降温出料，得到棕黄色透明产品，羟值测试结果为230mgKOH/g，粘度为10000cps(25℃)。
实施例6
在1.5L4口烧瓶中接上分水器、搅拌器、冷凝器、温度计和电加热器，加入60g甘油、400g丙二醇、150g硬脂酸、500g对苯二甲酸和0.2g酞酸酯，氮气置换后升温至140℃进行酯化反应，5h后降温到130℃抽真空3h，降温出料，得到棕黄色透明产品，羟值测试结果为330mgKOH/g，粘度为7000cps(25℃)。
实施例7
在1.5L4口烧瓶中接上分水器、搅拌器、冷凝器、温度计和电加热器，加入50g甘油、450g新戊二醇、150g油酸、400g对苯二甲酸和0.2gT9，氮气置换后升温至150℃进行酯化反应，5h后降温到130℃抽真空3h，降温出料，得到棕黄色透明产品，羟值测试结果为280mgKOH/g，粘度为8000cps(25℃)。
实施例8
在1.5L4口烧瓶中接上分水器、搅拌器、冷凝器、温度计和电加热器，加入70g三羟甲基丙烷、500g二丙二醇、200g油酸、350g对苯二甲酸和0.1gT12，氮气置换后升温至160℃进行酯化反应，5h后降温到130℃抽真空3h，降温出料，得到棕黄色透明产品，羟值测试结果为230mgKOH/g，粘度为9000cps(25℃)。
配制基于实施例1、实施例2、实施例3和实施例4中聚酯多元醇(实施例中的反应设备还可以采用具有相同功能的其他设备替代)，并PS 3152为参照物，观察比较溶解性。
由上表可知，该一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，本发明制得的芳香族聚酯多元醇具有良好的戊烷相容性，可以用于预混戊烷体系的组合聚酯多元醇，用于对阻燃有较高要求的聚氨酯硬泡***，而且整个制备具有良好戊烷相容性芳香族聚酯多元醇的方法简单，操作方便，使用效果相对于传统方式更好，而且成本较低，能够便于人们大规模生产。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (6)
1.一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，其特征在于：包括以下步骤：
(1)、将合成芳香族聚酯多元醇的原料放置到反应设备中进行氮气置换；
(2)、对反应设备进行升温，使得芳香族聚酯多元醇原料进行酯化反应；
(3)、对反应设备进行抽真空，然后进行降温出料，得到芳香族聚酯多元醇。
2.根据权利要求1所述的一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，其特征在于：步骤(1)中合成芳香族聚酯多元醇的原料包括二元醇、三元醇、长碳链单羧酸以及苯酐或对苯二甲酸，长碳链单羧酸含量占芳香族聚酯多元醇重量比的5-25％。
3.根据权利要求2所述的一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，其特征在于：三元醇为甘油或三羟甲基丙烷的一种或两种，二元醇为乙二醇、丙二醇、二乙二醇、二丙二醇、己二醇和新戊二醇中的一种或多种，长碳链单羧酸为油酸、亚油酸、硬脂酸和软脂酸中的一种或多种。
4.根据权利要求1所述的一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，其特征在于：步骤(2)中反应设备升温至100-180℃，酯化反应的时间为3-8h。
5.根据权利要求1所述的一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，其特征在于：步骤(2)中：酯化反应需要酯化催化剂，酯化催化剂为T9、T12、T120和酞酸酯中的一种，酯化催化剂为合成芳香族聚酯多元醇的原料的0.01％-0.2％。
6.根据权利要求1所述的一种制备具有良好戊烷相容性芳香族聚酯多元醇的方法，其特征在于：步骤(3)中抽真空时的温度为125-135℃，抽真空的时间为2.5-3.5h，得到的芳香族聚酯多元醇的羟值为150-350mgKOH/g。
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