CN111116891A - 一种低溶点农药水悬制剂用高分子烷基嵌段聚醚的制备方法 - Google Patents

一种低溶点农药水悬制剂用高分子烷基嵌段聚醚的制备方法 Download PDF

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CN111116891A
CN111116891A CN201911384120.5A CN201911384120A CN111116891A CN 111116891 A CN111116891 A CN 111116891A CN 201911384120 A CN201911384120 A CN 201911384120A CN 111116891 A CN111116891 A CN 111116891A
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尹艳洪
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Nanjing Lianzhi Technology Co Ltd
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Abstract

本发明涉及一种高分子烷基嵌段聚醚的制备方法，所用原料为脂肪烷基醇、环氧乙烷和环氧丙烷，具体的反应步骤如下：步骤一，脂肪烷基醇与环氧丙烷在催化剂作用下进行开环反应，得到脂肪烷基醇聚氧丙烯醚；步骤二，脂肪烷基醇聚氧丙烯醚与环氧乙烷在催化剂作用下进行乙氧基化反应，得到脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物；步骤三，脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物再与环氧丙烷在催化剂作用下反应，得到脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物；步骤四，脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物与环氧乙烷在催化剂作用下反应，得到所述的高分子烷基嵌段聚醚。本发明解决了低溶点农药水容易产生稠化的问题。

Description

一种低溶点农药水悬制剂用高分子烷基嵌段聚醚的制备方法
技术领域
本发明涉及多聚物的制备技术领域，具体涉及一种低溶点农药水悬制剂用高分子烷基嵌段聚醚的制备方法。
背景技术
现在农药剂型的发展趋势是向水基化方向发展，对于低熔点农药制备成水悬制剂，有很大的难度，极易在生产和储存过程中产生稠化，膏化，粒径急剧增加。市场上采用多芳基酚醚磷酸酯胺盐，聚丙烯酸类分散剂。还是不能很好的解决此问题。而我们采用烷基醇醚为起始剂，通过调节不同的聚氧丙烯和聚氧乙烯的配比和组合。合成具有光普性非离子型高分子聚醚。
聚醚是利用分子中含有活泼氢的化合物作为起始剂，与环氧乙烷、环氧丙烷发生聚合反应得到的一类嵌段共聚物，是一类典型的两亲高分子表面活性剂。脂肪醇聚氧丙烯聚氧乙烯嵌段共聚物是一类新型的非离子表面活性剂，聚氧丙烯嵌段为油溶性，这使得活性剂分子的疏水基相对增加了很多，油溶作用大大增强；同时由于分子量的增加，在一定浓度下胶团互相接近而呈网状结构或聚集形成棒状胶束的可能性增加，溶液会变得很粘稠。由于脂肪醇聚氧丙烯聚氧乙烯嵌段共聚物的这些特性，在某些特定领域具有很好的应用前景。
发明内容
为解决现有技术中存在的问题，本发明提供了一种低溶点农药水悬制剂用高分子烷基嵌段聚醚的制备方法，具体的技术方案如下所述：
一种低溶点农药水悬制剂用高分子烷基嵌段聚醚的制备方法，所用原料为脂肪烷基醇、环氧乙烷和环氧丙烷，
具体的反应步骤如下：
步骤一，脂肪烷基醇与环氧丙烷在催化剂作用下进行开环反应，并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯醚；
步骤二，步骤一中制备得到的脂肪烷基醇聚氧丙烯醚与环氧乙烷在催化剂作用下进行乙氧基化反应并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物；
步骤三，步骤二中制备得到的脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物再与环氧丙烷在催化剂作用下反应，并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物；
步骤四，步骤三中制备得到的脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物与环氧乙烷在催化剂作用下反应，并经过后处理，得到纯度较高的所述的高分子烷基嵌段聚醚；
具体的反应过程为：
REOX+n1PO+m2EO+n2PO+m2EO
其中，REOX中R的碳原子数为3-18，x为1—6；
n1为10--60；n2为1--10；m1为10--60,m2为10—60，且x、n1、n2、m1、m2均为整数。
进一步地，所述的步骤一、步骤二、步骤三和步骤四均在无水条件下进行。
进一步地，所述步骤开环反应或乙氧基化反应用催化剂选自氢氧化钾、氢氧化钠、甲醇钠、乙醇钠、烷氧基铝磺酸盐、稀有金属烷氧硫酸盐、碱土金属氧化物与磷酸的复合物中的一种。
进一步地，所述步骤开环反应或乙氧基化反应用酸性催化剂选自BF3、SbCl5、SnCl4、固体酸、杂多酸、负载型分子筛催化剂中的一种。
进一步地，所述的高分子烷基嵌段聚醚应用在农药制剂方面，将低熔点农药制备成水悬制剂。
本发明的有益效果为：本发明是解决了低熔点农药水悬时，容易产生稠化，膏化，粒径长大的问题。本发明通过设计高分子烷基嵌段聚醚的结构，环氧丙烷与环氧乙烷的比例，分子量的大小，催化剂的选择，合成了一个能很好的解决低熔点农药水悬膏化，抑制粒径长大的问题。
具体实施方式：
为了加深对本发明的理解，下面结合实施例对本发明的实施例做详细的说明。
实施例1
一种低溶点农药水悬制剂用高分子烷基嵌段聚醚的制备方法，所用原料为脂肪烷基醇、环氧乙烷和环氧丙烷，
具体的反应步骤如下：
步骤一，脂肪烷基醇与环氧丙烷在催化剂作用下进行开环反应，并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯醚；
步骤二，步骤一中制备得到的脂肪烷基醇聚氧丙烯醚与环氧乙烷在催化剂作用下进行乙氧基化反应并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物；
步骤三，步骤二中制备得到的脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物再与环氧丙烷在催化剂作用下反应，并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物；
步骤四，步骤三中制备得到的脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物与环氧乙烷在催化剂作用下反应，并经过后处理，得到纯度较高的所述的高分子烷基嵌段聚醚；
具体的反应过程为：
异构C10醇EO5醚+42PO+18EO+2PO+28EO
进一步地，所述的步骤一、步骤二、步骤三和步骤四均在无水条件下进行。
进一步地，所述步骤开环反应或乙氧基化反应用催化剂选自氢氧化钾、氢氧化钠、甲醇钠、乙醇钠、烷氧基铝磺酸盐、稀有金属烷氧硫酸盐、碱土金属氧化物与磷酸的复合物中的一种。
进一步地，所述步骤开环反应或乙氧基化反应用酸性催化剂选自BF3、SbCl5、SnCl4、固体酸、杂多酸、负载型分子筛催化剂中的一种。
进一步地，所述的高分子烷基嵌段聚醚应用在农药制剂方面，将低熔点农药制备成水悬制剂。
具体应用如下：
25％吡唑醚菌酯SC
Figure BDA0002343076650000031
实施例2
一种低溶点农药水悬制剂用高分子烷基嵌段聚醚的制备方法，所用原料为脂肪烷基醇、环氧乙烷和环氧丙烷，
具体的反应步骤如下：
步骤一，脂肪烷基醇与环氧丙烷在催化剂作用下进行开环反应，并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯醚；
步骤二，步骤一中制备得到的脂肪烷基醇聚氧丙烯醚与环氧乙烷在催化剂作用下进行乙氧基化反应并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物；
步骤三，步骤二中制备得到的脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物再与环氧丙烷在催化剂作用下反应，并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物；
步骤四，步骤三中制备得到的脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物与环氧乙烷在催化剂作用下反应，并经过后处理，得到纯度较高的所述的高分子烷基嵌段聚醚；
具体的反应过程为：
异构C13醇EO6醚+42PO+18EO+2PO+28EO
进一步地，所述的步骤一、步骤二、步骤三和步骤四均在无水条件下进行。
进一步地，所述步骤开环反应或乙氧基化反应用催化剂选自氢氧化钾、氢氧化钠、甲醇钠、乙醇钠、烷氧基铝磺酸盐、稀有金属烷氧硫酸盐、碱土金属氧化物与磷酸的复合物中的一种。
进一步地，所述步骤开环反应或乙氧基化反应用酸性催化剂选自BF3、SbCl5、SnCl4、固体酸、杂多酸、负载型分子筛催化剂中的一种。
进一步地，所述的高分子烷基嵌段聚醚应用在农药制剂方面，将低熔点农药制备成水悬制剂。具体应用如下：
25％吡唑醚菌酯SC
Figure BDA0002343076650000041
Figure BDA0002343076650000051
实施例3
一种低溶点农药水悬制剂用高分子烷基嵌段聚醚的制备方法，所用原料为脂肪烷基醇、环氧乙烷和环氧丙烷，
具体的反应步骤如下：
步骤一，脂肪烷基醇与环氧丙烷在催化剂作用下进行开环反应，并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯醚；
步骤二，步骤一中制备得到的脂肪烷基醇聚氧丙烯醚与环氧乙烷在催化剂作用下进行乙氧基化反应并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物；
步骤三，步骤二中制备得到的脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物再与环氧丙烷在催化剂作用下反应，并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物；
步骤四，步骤三中制备得到的脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物与环氧乙烷在催化剂作用下反应，并经过后处理，得到纯度较高的所述的高分子烷基嵌段聚醚；
具体的反应过程为：
丁基C4+EO2+40PO+18EO+2PO+28EO
进一步地，所述的步骤一、步骤二、步骤三和步骤四均在无水条件下进行。
进一步地，所述步骤开环反应或乙氧基化反应用催化剂选自氢氧化钾、氢氧化钠、甲醇钠、乙醇钠、烷氧基铝磺酸盐、稀有金属烷氧硫酸盐、碱土金属氧化物与磷酸的复合物中的一种。
进一步地，所述步骤开环反应或乙氧基化反应用酸性催化剂选自BF3、SbCl5、SnCl4、固体酸、杂多酸、负载型分子筛催化剂中的一种。
进一步地，所述的高分子烷基嵌段聚醚应用在农药制剂方面，将低熔点农药制备成水悬制剂。
具体应用如下：
25％吡唑醚菌酯SC
Figure BDA0002343076650000061
本发明方案所公开的技术手段不仅限于上述技术手段所公开的技术手段，还包括由以上技术特征等同替换所组成的技术方案。本发明的未尽事宜，属于本领域技术人员的公知常识。

Claims (5)

1.一种低溶点农药水悬制剂用高分子烷基嵌段聚醚的制备方法，其特征在于，所用原料为脂肪烷基醇、环氧乙烷和环氧丙烷，
具体的反应步骤如下：
步骤一，脂肪烷基醇与环氧丙烷在催化剂作用下进行开环反应，并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯醚；
步骤二，步骤一中制备得到的脂肪烷基醇聚氧丙烯醚与环氧乙烷在催化剂作用下进行乙氧基化反应并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物；
步骤三，步骤二中制备得到的脂肪烷基醇聚氧丙烯聚氧乙烯嵌段共聚物再与环氧丙烷在催化剂作用下反应，并经过后处理，得到纯度较高的脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物；
步骤四，步骤三中制备得到的脂肪烷基醇聚氧丙烯聚氧乙烯聚氧丙烯嵌段共聚物与环氧乙烷在催化剂作用下反应，并经过后处理，得到纯度较高的所述的高分子烷基嵌段聚醚；
具体的反应过程为：
REOX+n1PO+m2EO+n2PO+m2EO
其中，REOX中R的碳原子数为3-18，x为1—6；
n1为10--60；n2为1--10；m1为10--60,m2为10—60，且x、n1、n2、m1、m2均为整数。
2.根据权利要求1所述的制备方法，其特征在于：所述的步骤一、步骤二、步骤三和步骤四均在无水条件下进行。
3.根据权利要求1所述的制备方法，其特征在于：所述步骤开环反应或乙氧基化反应用催化剂选自氢氧化钾、氢氧化钠、甲醇钠、乙醇钠、烷氧基铝磺酸盐、稀有金属烷氧硫酸盐、碱土金属氧化物与磷酸的复合物中的一种。
4.根据权利要求1所述的制备方法，其特征在于：所述步骤开环反应或乙氧基化反应用酸性催化剂选自BF3、SbCl5、SnCl4、固体酸、杂多酸、负载型分子筛催化剂中的一种。
5.如权利要求1～4任意一项所述制备方法得到的高分子烷基嵌段聚醚的应用，其特征在于，所述的高分子烷基嵌段聚醚应用在农药制剂方面，将低熔点农药制备成水悬制剂。
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