CN106188521A - 合成聚合物多元醇用高分子分散剂 - Google Patents
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Abstract
本发明涉及一种合成聚合物多元醇用高分子分散剂,包括以下重量份数的原料:水杨醇:50‑100份,化合物A:1500‑4000份,催化剂a:6‑13份,酸酐:15.5‑40.5份,催化剂b:0.31‑0.91份,环氧乙烷:150‑300份,吗啉:3‑9份。本发明使得体系中的固体乙烯基单体颗粒能够更好溶解在基础聚醚中,防止颗粒的聚集和沉降,形成稳定悬浮液。本发明同时提供其制备方法,采用水杨醇为料头制备的分散剂在聚合物多元醇反应过程中,因其与苯乙烯共有的苯环结构而具有相似相容的优势。
Description
技术领域
本发明涉及一种合成聚合物多元醇用高分子分散剂。
背景技术
随着聚氨酯材料不段发展,聚合物多元醇作为聚氨酯材料中的重要原料,已经被业内广泛使用。如今的聚合物多元醇正向着低气味、高硬度、高固含量、流动性优良的方向发展。聚合物固含量的不断提高,在生产过程中需要高分子分散剂对体系进行稳定,体系受大分子分散剂性能上的差异影响,效果差的分散剂使得聚合物的粒径变大,体系粘度升高,给POP后处理及大型精密设备的快速发泡带来了诸多不便。
发明内容
本发明目的在于提供一种合成聚合物多元醇用高分子分散剂,使得体系中的固体乙烯基单体颗粒能够更好溶解在基础聚醚中,防止颗粒的聚集和沉降,形成稳定悬浮液。本发明同时提供其制备方法,采用水杨醇为料头制备的分散剂在聚合物多元醇反应过程中,因其与苯乙烯共有的苯环结构而具有相似相容的优势。
本发明所述的合成聚合物多元醇用高分子分散剂,包括以下重量份数的原料:
水杨醇:50-100份,化合物A:1500-4000份,催化剂a:6-13份,酸酐:15.5-40.5份,催化剂b:0.31-0.91份,环氧乙烷:150-300份,吗啉:3-9份。
其中:化合物A为环氧丙烷或环氧乙烷中的一种或两种。
酸酐为富马酸或邻苯二甲酸酐。
催化剂a和催化剂b为碱性催化剂或磷腈类催化剂中的一种。
催化剂a和催化剂b为KOH或NaOH。
所述的合成聚合物多元醇用高分子分散剂的制备方法,包括以下步骤:在氮气保护下,将起始剂水杨醇、催化剂a和化合物A混合后发生聚合反应,制得PPG;将PPG、酸酐、催化剂b混合后,加热升温,至酸值达到理论值,然后用环氧乙烷封端,再用吗啉异构化制得高分子分散剂。
用吗啉异构化的温度为150-160℃。
PPG采用两步法聚合制得,包括以下步骤:
(1)第一步聚合:将水杨醇、催化剂a混合搅拌,氮气置换,升温,通入部分化合物A进行反应,反应压力为0.1-0.5MPa,反应结束后进行熟化反应至无压降,反应时间为4-8h,得到低聚物备用;
(2)第二步聚合:将得到低聚物升温,通入剩余化合物A进行反应,反应压力为0.1-0.5MPa,反应结束后进行熟化反应至无压降,反应时间为6-10h,得到反应产物PPG。
聚合反应后进行脱单体反应,反应时间为1-3h,同时降温至70-90℃,然后加入中和至PH在4.8-5.5,加入精制剂精制,干燥过滤,得到PPG。
PPG、酸酐、催化剂反应温度为90-120℃。
环氧乙烷进行封端的反应温度为130-150℃。
中和剂为磷酸或草酸中的一种;精制剂为硅酸镁。
高分子分散剂的分子量为5000-7000。
本发明所述的合成聚合物多元醇用高分子分散剂,尤其应用于生产上制备聚合物多元醇工序中,对生产中聚合物体系起到稳定作用。
本发明与现有技术相比,具有以下有益效果。
本专利制备分散剂的方法,使得体系中的固体乙烯基单体颗粒能够更好溶解在基础聚醚中,防止颗粒的聚集和沉降,形成稳定悬浮液。采用水杨醇为料头制备的分散剂在聚合物多元醇反应过程中,因其与苯乙烯共有的苯环结构而具有相似相容的优势。
具体实施方式
下面结合实施例对本发明做进一步说明。
实施例1
原料重量份数:
水杨醇:50份
催化剂a(氢氧化钾):6.2份
环氧丙烷(第一步):400份
环氧丙烷/环氧乙烷(第二步):1320/240份
酸酐 15.5
催化剂b(氢氧化钾) 0.31
封端剂(环氧乙烷):150份
吗啉 3.1。
制备方法:
(1)聚合反应采用两步法聚合:
第一步聚合:将水杨醇、氢氧化钾投入密闭聚合釜中,搅拌,氮气置换,升温至反应温度,通入部分环氧丙烷进行反应,反应压力<0.44MPa,反应结束后进行熟化反应至无明显压降,反应时间为4h,得到低聚物备用;
第二步聚合:将得到低聚物升温至反应温度,通入其余化合物A进行反应,反应压力为为<0.44MPa,反应结束后进行熟化反应至无明显压降,反应时间为6h,得到反应产物;
(2)将步骤(1)反应产物进行脱单体反应,反应时间为1h,同时降温至90℃,然后加入磷酸中和,加入硅酸镁精制,干燥过滤,得到PPG;
(3)将PPG、酸酐、催化剂b投入反应釜,升温150℃至酸值达到理论值;
(4)将步骤(3)中产物用封端剂环氧乙烷进行封端,温度130℃,再用吗啉进行高温异构化制得成品。
实施例2
原料重量份数:
水杨醇:100
催化剂a(氢氧化钠):12.4
酸酐:40.5份
催化剂b(氢氧化钠):0.91份
环氧丙烷(第一步):800
环氧丙烷/环氧乙烷(第二步):2640/480
封端剂(环氧乙烷):300
吗啉:9份
制备方法:
(1)聚合反应采用两步法聚合:
第一步聚合:将水杨醇、氢氧化钾投入密闭聚合釜中,搅拌,氮气置换,升温至反应温度,通入部分环氧丙烷进行反应,反应压力为<0.44MPa,反应结束后进行熟化反应至无明显压降,反应时间为6h,得到低聚物备用;
第二步聚合:将得到低聚物升温至反应温度,通入其余化合物A进行反应,反应压力为为<0.44MPa,反应结束后进行熟化反应至无明显压降,反应时间为h,得到反应产物;
(2)将步骤(1)反应产物进行脱单体反应,反应时间为8h,同时降温至90℃,然后加入磷酸中和,加入硅酸镁精制,干燥过滤,得到PPG;
(3)将PPG、酸酐、催化剂b投入反应釜,升温155℃至酸值达到理论值;
(4)将步骤(3)中产物用封端剂环氧乙烷进行封端,温度135℃,再用吗啉进行高温异构化制得成品。
实施例3
原料重量份数:
水杨醇:75
催化剂a(氢氧化钾):9.3
酸酐:30
催化剂b(氢氧化钾):0.6
环氧丙烷(第一步):600
环氧丙烷/环氧乙烷(第二步):1980/360
封端剂(环氧乙烷):225
吗啉:6份
制备方法:
(1)聚合反应采用两步法聚合:
第一步聚合:将水杨醇、氢氧化钾投入密闭聚合釜中,搅拌,氮气置换,升温至反应温度,通入部分环氧丙烷进行反应,反应压力为<0.44MPa,反应结束后进行熟化反应至无明显压降,反应时间为5h,得到低聚物备用;
第二步聚合:将得到低聚物升温至反应温度,通入其余化合物A进行反应,反应压力为为<0.44MPa,反应结束后进行熟化反应至无明显压降,反应时间为h,得到反应产物;
(2)将步骤(1)反应产物进行脱单体反应,反应时间为7h,同时降温至90℃,然后加入磷酸中和,加入硅酸镁精制,干燥过滤,得到PPG;
(3)将PPG、酸酐、催化剂b投入反应釜,升温145℃至酸值达到理论值;
(4)将步骤(3)中产物用封端剂环氧乙烷进行封端,温度125℃,再用吗啉进行高温异构化制得成品。
在后期使用成品分散剂制备聚合物多元醇过程发现,新分散剂制备的聚合物多元醇具有更好的流动性。用100目金属滤网过滤发现几乎无肉眼可见颗粒,显微镜下观察,粒子呈现均匀的圆形。
Claims (10)
1.一种合成聚合物多元醇用高分子分散剂,其特征在于,包括以下重量份数的原料:
水杨醇:50-100份,化合物A:1500-4000份,催化剂a:6-13份,酸酐:15.5-40.5份,催化剂b:0.31-0.91份,环氧乙烷:150-300份,吗啉:3-9份。
其中:化合物A为环氧丙烷或环氧乙烷中的一种或两种。
2.根据权利要求1所述的合成聚合物多元醇用高分子分散剂,其特征在于,酸酐为富马酸或邻苯二甲酸酐。
3.根据权利要求1所述的合成聚合物多元醇用高分子分散剂,其特征在于,催化剂a和催化剂b为碱性催化剂或磷腈类催化剂中的一种。
4.根据权利要求1所述的合成聚合物多元醇用高分子分散剂,其特征在于,催化剂a和催化剂b为KOH或NaOH。
5.一种权利要求1-4任一所述的合成聚合物多元醇用高分子分散剂的制备方法,其特征在于,包括以下步骤:在氮气保护下,将起始剂水杨醇、催化剂a和化合物A混合后发生聚合反应,制得PPG;将PPG、酸酐、催化剂b混合后,加热升温,至酸值达到理论值,然后用环氧乙烷封端,再用吗啉异构化制得高分子分散剂。
6.根据权利要求5所述的合成聚合物多元醇用高分子分散剂的制备方法,其特征在于,PPG采用两步法聚合制得,包括以下步骤:
(1)将水杨醇、催化剂a混合搅拌,氮气置换,升温,通入部分化合物A进行反应,反应压力为0.1-0.5MPa,反应结束后进行熟化反应至无压降,反应时间为4-8h,得到低聚物备用;
(2)将得到低聚物升温,通入剩余化合物A进行反应,反应压力为0.1-0.5MPa,反应结束后进行熟化反应至无压降,反应时间为6-10h,得到反应产物PPG。
7.根据权利要求5或6所述的合成聚合物多元醇用高分子分散剂的制备方法,其特征在于,聚合反应后进行脱单体反应,反应时间为1-3h,同时降温至70-90℃,然后加入中和至PH在4.8-5.5,加入精制剂精制,干燥过滤,得到PPG。
8.根据权利要求5所述的合成聚合物多元醇用高分子分散剂的制备方法,其特征在于,PPG、酸酐、催化剂反应温度为90-120℃。
9.根据权利要求5所述的合成聚合物多元醇用高分子分散剂的制备方法,其特征在于,环氧乙烷进行封端的反应温度为130-150℃。
10.根据权利要求7所述的合成聚合物多元醇用高分子分散剂的制备方法,其特征在于,中和剂为磷酸或草酸中的一种;精制剂为硅酸镁。
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