CN109054002A - 线性聚酯多元醇的制备与应用 - Google Patents
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Abstract
本发明提供一种线性聚酯多元醇的制备与应用技术。将二元羧酸/或酸酐和二元醇单体进行聚合反应，形成端羧基封端的线性聚酯。根据应用需要来设计所需体系酸值及分子量大小。随后加入双端含有环氧基的环氧树脂和催化剂进行扩链反应，使一端环氧基和一端的羧基反应开环变成羟基，即可生成线性聚酯多元醇。本发明制备的线性聚酯多元醇，是聚氨酯的主要原料，广泛应用于皮革、胶黏剂、油墨和涂层等。还可以与氨基树脂复配，应用于高档汽车热固化涂料，玻璃纤维三维取向成型材料等。
Description
技术领域
一种线性聚酯多元醇的制备与应用，本发明所制备的产品是聚氨酯和氨基树脂的主要原料，广泛应用于皮革、胶黏剂、油墨、涂层和玻璃纤维三维取向成型材料等，属于高分子化学及聚合物领域。
背景技术
传统聚酯涂料通常包括不饱和聚酯涂料和饱和聚酯涂料两种。不饱和聚酯涂料由分装的四组分不饱和聚酯树脂的苯乙烯溶液、有机过氧化物等引发剂（交联催化剂）、环烷酸钴等促进剂、石蜡的苯乙烯等混合制得。苯乙烯起着溶剂合成膜物质的双重作用。饱和聚酯涂料是含端羟基官能团的聚酯树脂，通过与异氰酸酯、氨基树脂等树脂交联固化成膜，它的特点是泽度高、丰满度好、硬度高、柔韧性好、耐磨和耐热性好、保光和保色性良好。在汽车喷漆、船舶和轨道交通等应用十分广泛
本发明中线性聚酯多元醇可以用作含端羟基官能团的聚酯树脂，与传统聚酯多元醇合成方法相比具有很多优势。传统的聚酯多元醇合成方法，一般采用有机二元羧酸（酸酐或酯）与多元醇（包括二元醇）缩合（或酯交换）或由内脂与多元醇聚合而成。醇酸缩聚反应非常慢，将酸值降到5mg KOH/g 以下需要反应温度高和时间长，很难控制羟基的官能度，容易形成凝胶。本发明的特点是反应温度低，合成时间短，羟基的官能度可以控制且聚合物呈线性结构，合成过程中不会发生凝胶现象。此外，可通过环氧树脂种类来优化聚酯多元醇的结构及形态如无定型、半结晶态和结晶态。同时还可以降低聚酯多元醇的粘度，代替传统聚酯多元醇，能满足绝大部分传统聚酯多元醇的使用要求。
发明内容
针对目前聚酯汽车面漆采用传统聚酯多元醇因其粘度大、溶剂用量多等缺点，本发明目的在于提供一种线性聚酯多元醇的合成工艺
本发明目的通过下述方案实现：一种线性聚酯多元醇的制备与应用，其特征在于包括如下步骤：
（1）二元羧酸/或酸酐和二元醇单体进行聚合反应，控制终点酸值在30~50mg KOH/g 之间；
（2）加入一定有机溶剂芳香100，控制可操作粘度，适合环氧树脂与上述步骤产物进行反应；
（3）加入环氧树脂和催化剂进行反应，使环氧基团与聚酯的端羧基进行开环反应，反应直至酸值降到5mg KOH/g以下；
（4）加入一定量的添加剂
步骤（1）中，二元羧酸或酸酐为邻苯二甲酸酐、间苯二甲酸、对苯二甲酸、甲基四氢苯酐、六氢化邻苯二甲酸酐、氢化间苯二甲酸、丙二酸、丁二酸、己二酸，十二烷二酸；二元醇为乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、二甘醇、一缩二丙二醇，1,4-环己醇，新戊二醇；二元醇与二元羧酸或酸酐的摩尔比小于等于1,反应温度在150℃先反应，防止放热反应和过多的醇蒸发流失，然后升温到200~210℃进行酯化反应。
步骤（3）中环氧树脂为单基和/或双端基线性环氧树脂，如双酚A型环氧树脂、双酚F环氧树脂、酚醛环氧树脂、脂肪族线性环氧树脂和胺改性环氧树脂；反应温度为100～120℃，最佳倾向于110～115℃。
步骤（2）中加入的溶剂可以为芳香100、乙酸丁酯、乙酸乙酯等。根据不同使用要求，所加入的溶剂一般占整个体系的0%~70%，最佳溶剂用量一般在30%~40%。
步骤（3）所选用催化剂为含氮和磷化合物或金属盐或络合物如叔胺、季铵盐、三烷基磷、季鏻盐，加入量为总反应物重量的0.01%~0.5%。
步骤（4）中所指加入添加剂为颜料，抗氧剂等助剂等
本发明提供一种线性聚酯多元醇的制备与应用，根据上述任一项所述方法制备得到。
本发明提供一种线性聚酯多元醇的制备与应用技术，本发明所制备的产品是聚氨酯和氨基树脂的主要原料，广泛应用于皮革、胶黏剂、油墨、涂层和玻璃纤维三维取向成型材料等。
通过本发明可以制得线性聚酯多元醇，通过设计反应物摩尔比例，控制步骤1中的酸值可以根据不同的使用要求来调控聚酯的分子量大小，其具有直线型，分子量可控，不宜交联，成膜性、流延性好等优点，能满足作为汽车面漆的基本要求，也能作为胶黏剂使用。
Claims (8)
1.一种线性聚酯多元醇的制备与应用技术，其特征在于包括如下步骤：
（1）二元羧酸/或酸酐和二元醇单体进行聚合反应，通过所需体系酸值来控制分子量大小，分子量大小一般控制在500~2000；
（2）根据反应产物粘度及应用情况加入一定溶剂；
（3）根据第一步酸值大小加入环氧树脂和催化剂进行反应，使环氧基团与聚酯的端羧基进行开环反应，同时在分子链上产生羟基，让酸值降到5mg KOH/g以下，合成高分子量的线性聚酯多元醇；
（4）加入一定量的添加剂。
2.如权利要求1所述一种线性聚酯多元醇的制备与应用，其特征在于，根据体系酸值来控制分子量大小。
3.如权利要求1所述一种线性聚酯多元醇的制备与应用，其特征在于，步骤（1）中，二元羧酸或酸酐为邻苯二甲酸酐、间苯二甲酸、对苯二甲酸、甲基四氢苯酐、六氢化邻苯二甲酸酐、氢化间苯二甲酸、丙二酸、丁二酸、己二酸，十二烷二酸等；二元醇为乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、二甘醇、一缩二丙二醇，1,4-环己醇，新戊二醇；二元醇与二元羧酸或酸酐的摩尔比小于等于1,反应温度在150℃先反应，防止放热反应和过多的醇蒸发流失，然后升温到200~210℃进行酯化反应。
4.如权利要求1中所述一种线性聚酯多元醇的制备与应用，其特征在于，可以根据不同使用情况加入一定的溶剂，步骤（2）中加入的溶剂可以为芳香100、乙酸丁酯、乙酸乙酯等，根据不同使用要求，所加入的溶剂一般占整个体系的0%~70%，最佳溶剂用量一般在30%~40%。
5.如权利要求1所述一种多线性聚酯多元醇的制备与应用，其特征在于，步骤（3）中环氧树脂为单和/或双端基线性环氧树脂，如双酚A型环氧树脂，双酚F环氧树脂，酚醛环氧树脂，脂肪族线性环氧树脂，胺改性环氧树脂等，反应温度为100～120℃，最佳倾向于110～115℃。
6.如权利要求1所述一种线性聚酯多元醇的制备与应用，其特征在于，步骤（3）所选用催化剂为含氮和磷化合物或金属盐或络合物如叔胺、季铵盐、三烷基磷、季鏻盐，加入量为总反应物重量的0.01%~0.5%。
7.如权利要求1所述一种线性聚酯多元醇的制备与应用，其特征在于，步骤（4）中所加入添加剂为抗氧剂、颜料和填料等添加剂。
8.一种线性聚酯多元醇的制备与应用，其特征在于根据权利要求1至7之任一项所述方法制备得到。
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