CN112390964A - 一种pedot分散液的制备方法 - Google Patents

一种pedot分散液的制备方法 Download PDF

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CN112390964A
CN112390964A CN202011289179.9A CN202011289179A CN112390964A CN 112390964 A CN112390964 A CN 112390964A CN 202011289179 A CN202011289179 A CN 202011289179A CN 112390964 A CN112390964 A CN 112390964A
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pedot
dispersion liquid
sulfonic acid
polyanion
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张茂华
陈伟科
黎民
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Guangdong Huahong Technology Co ltd
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Abstract

本发明公开了一种PEDOT分散液的制备方法，涉及高分子材料技术领域。本发明所述PEDOT分散液的制备原料使用了改性的聚阴离子，通过改性的聚阴离子和EDOT单体的剪切乳化，得到Pickering乳液，然后在乳液中加入氧化剂，反应完成后，得到所述PEDOT分散液。本发明所述PEDOT分散液制备完成后无需除杂，简化了PEDOT分散液的合成工艺；并且制备出的PEDOT分散液导电率高、透明度好，稳定性高。

Description

一种PEDOT分散液的制备方法
技术领域
本发明涉及高分子材料技术领域，尤其涉及一种PEDOT分散液的制备方法。
背景技术
PEDOT分散液一般是指PEDOT/PSS分散液、磺酸衍生物掺杂的PEDOT分散液，该产品是由PEDOT和PSS(或者磺酸衍生物)两种物质构成。PEDOT是EDOT(3，4-乙烯二氧噻吩单体)的聚合物，PSS是聚苯乙烯磺酸盐。PSS或者磺酸衍生物的加入极大的提高了PEDOT的溶解性和电导率。根据不同的应用领域可以开发设计不同结构、不同性能、不同导电率的PEDOT分散液。PEDOT分散液在固态电容器的应用是将PEDOT分散液含浸或者涂覆在电容器上，干燥蒸发移除分散剂，形成PEDOT膜制备固态电容器。所以要求PEDOT分散液具有较高的电导率。PEDOT分散液在防静电涂层的应用除了高电导率外，还要求具有较高的透明度。
目前PEDOT/PSS合成通常在：PSS溶液中加入氧化剂(过硫酸氨等过硫酸盐、高锰酸盐等高价盐)、催化剂(氯化铁、硫化亚铁等盐)、EDOT进行聚合反应。反应结束后进行除杂，除去合成过程中加入的各类盐。合成过程加入大量的固体高价盐，需要进行溶解投入，投料不如液体方便。合成过程中加入的大量的高价盐在聚合反应结束后，需要进行繁琐的提纯除杂，以得到杂质含量低、稳定性好的PEDOT/PSS分散液。除杂过程会损失大量PEDOT/PSS，造成PEDOT/PSS收率偏低，且损失的PEDOT/PSS会产生大量的废水。除杂提纯处理会造成各类污染、产生大量废水，而当前环保要求日益严格，污水等处理费用高昂，增加了生产成本。废水回收利用价值不高，回收提纯工艺复杂、回收成本高。且制备得到的PEDOT/PSS分散液性能难以满足高端需求。
发明内容
本发明的目的在于克服上述现有技术的不足之处而提供一种制备简便，无需提纯除杂的PEDOT分散液的制备方法，制备出的PEDOT分散液具有良好的导电性和透明度。
为实现上述目的，本发明所采取的技术方案为：一种PEDOT分散液的制备方法，包括如下步骤：
(1)将聚阴离子加入水中，搅拌均匀，得到混合液A；
(2)向混合液A中加入单体，剪切乳化，得到Pickering乳液；
(3)向Pickering乳液中加入氧化剂，发生聚合反应，反应完成后，得到所述PEDOT分散液；
所述步骤(1)中的聚阴离子包括磺化的聚苯乙烯-丁二烯共聚物、磺化的丁烯-乙烯-苯乙烯共聚物、酯化的聚苯乙烯磺酸、十二烷基苯磺酸中的至少一种；
所述步骤(2)中的单体包含3,4-乙撑二氧噻吩、苯胺及苯胺衍生物中的至少一种。
优选地，所述磺化的聚苯乙烯-丁二烯共聚物是以磺酸和聚苯乙烯-丁二烯共聚物以质量比为(0.01-10)：1制备出来的；所述磺化的丁烯-乙烯-苯乙烯共聚物是以磺酸和丁烯-乙烯-苯乙烯共聚物以质量比为(0.01-10)：1制备出来的；所述酯化的聚苯乙烯磺酸是以聚苯乙烯磺酸和乙醇以质量比为1：(0.01～10)制备出来的。
优选地，所述单体、聚阴离子、水、氧化剂的质量比为：单体：聚阴离子：水：氧化剂＝1：(0.2-20)：(10-200)：(0.2-1)。
优选地，所述单体、聚阴离子、水、氧化剂的质量比为：单体：聚阴离子：水：氧化剂＝1：(0.5-15)：(50-100)：(0.3-0.5)。
优选地，所述单体、聚阴离子、水、氧化剂的质量比为：单体：聚阴离子：水：氧化剂＝1：10：80：0.4。
优选地，所述单体中3,4-乙撑二氧噻吩与苯胺或苯胺衍生物的质量比为1:(0.01-0.5)。
优选地，所述聚阴离子中，磺化的聚苯乙烯-丁二烯共聚物、磺化的丁烯-乙烯-苯乙烯共聚物、酯化的聚苯乙烯磺酸的质量比为：磺化的聚苯乙烯-丁二烯共聚物：磺化的丁烯-乙烯-苯乙烯共聚物：酯化的聚苯乙烯磺酸＝1:1:2。
优选地，所述步骤(3)中的氧化剂为H2O2。
相比于现有技术，本发明的有益效果为：本发明利用双氧水作为氧化剂，氧化合成PEDOT分散液，双氧水分解形成两个羟基自由基，无其他盐类物质的产生。因此合成得到的PEDOT分散液无需后续提纯除杂处理。简化了PEDOT分散液的合成工艺，提高了PEDOT分散的收率；并且，本发明通过对聚阴离子进行选择，制备得到的PEDOT分散液电导率高、透明度好、稳定性高。
具体实施方式
为更好地说明本发明的目的、技术方案和优点，下面将结合具体实施例对本发明作进一步说明。
实施例1
本发明所述PEDOT分散液的制备方法的一种实施例，本实施例所述制备方法包括如下步骤：
(1)以0.5g磺酸和10g聚苯乙烯-丁二烯共聚物制备磺化的聚苯乙烯-丁二烯共聚物；以0.5g磺酸和10g丁烯-乙烯-苯乙烯共聚物制备磺化的丁烯-乙烯-苯乙烯共聚物；以10g聚苯乙烯磺酸和0.5g乙醇制备酯化的聚苯乙烯磺酸。
(2)将2.5g磺化的聚苯乙烯-丁二烯共聚物、2.5g磺化的丁烯-乙烯-苯乙烯共聚物、5g酯化的聚苯乙烯磺酸和80g水混合均匀，得到混合液A；
(3)将0.8g EDOT、0.2g苯胺加入混合液A中，剪切乳化，得到Pickering乳液；
(4)向Pickering乳液中加入0.4g双氧水(H2O2的质量分数为30％)，待聚合反应完成后，得到所述PEDOT分散液。
实施例2
本发明所述PEDOT分散液的制备方法的一种实施例，本实施例所述制备方法包括如下步骤：
(1)采用与实施例1相同的方式制备磺化和酯化的聚阴离子；
(2)将3.75g磺化的聚苯乙烯-丁二烯共聚物、3.75g磺化的丁烯-乙烯-苯乙烯共聚物、7.5g酯化的聚苯乙烯磺酸和100g水混合均匀，得到混合液A；
(3)将0.8g EDOT、0.2g苯胺加入混合液A中，剪切乳化，得到Pickering乳液；
(4)向Pickering乳液中加入0.5g双氧水，待聚合反应完成后，得到所述PEDOT分散液。
实施例3
本发明所述PEDOT分散液的制备方法的一种实施例，本实施例所述制备方法包括如下步骤：
(1)采用与实施例1相同的方式制备磺化和酯化的聚阴离子；
(2)将0.125g磺化的聚苯乙烯-丁二烯共聚物、0.125g磺化的丁烯-乙烯-苯乙烯共聚物、0.25g酯化的聚苯乙烯磺酸和50g水混合均匀，得到混合液A；
(3)将0.8g EDOT、0.2g苯胺加入混合液A中，剪切乳化，得到Pickering乳液；
(4)向Pickering乳液中加入0.3g双氧水，待聚合反应完成后，得到所述PEDOT分散液。
实施例4
本发明所述PEDOT分散液的制备方法的一种实施例，本实施例所述制备方法包括如下步骤：
(1)采用与实施例1相同的方式制备磺化和酯化的聚阴离子；
(2)将0.05g磺化的聚苯乙烯-丁二烯共聚物、0.05g磺化的丁烯-乙烯-苯乙烯共聚物、0.1g酯化的聚苯乙烯磺酸和10g水混合均匀，得到混合液A；
(3)将0.8g EDOT、0.2g苯胺加入混合液A中，剪切乳化，得到Pickering乳液；
(4)向Pickering乳液中加入0.2g双氧水，待聚合反应完成后，得到所述PEDOT分散液。
实施例5
本发明所述PEDOT分散液的制备方法的一种实施例，本实施例所述制备方法包括如下步骤：
(1)采用与实施例1相同的方式制备磺化和酯化的聚阴离子；
(2)将5g磺化的聚苯乙烯-丁二烯共聚物、5g磺化的丁烯-乙烯-苯乙烯共聚物、10g酯化的聚苯乙烯磺酸和200g水混合均匀，得到混合液A；
(3)将0.8g EDOT、0.2g苯胺加入混合液A中，剪切乳化，得到Pickering乳液；
(4)向Pickering乳液中加入1g双氧水，待聚合反应完成后，得到所述PEDOT分散液。
实施例6
本发明所述PEDOT分散液的制备方法的一种实施例，本实施例所述制备方法中，聚阴离子为5g磺化的聚苯乙烯-丁二烯共聚物和5g酯化的聚苯乙烯磺酸。其余制备条件与实施例1相同。
实施例7
本发明所述PEDOT分散液的制备方法的一种实施例，本实施例所述制备方法中，聚阴离子为5g磺化的丁烯-乙烯-苯乙烯共聚物和5g酯化的聚苯乙烯磺酸。其余制备条件与实施例1相同。
实施例8
本发明所述PEDOT分散液的制备方法的一种实施例，本实施例所述制备方法中，聚阴离子为4g磺化的聚苯乙烯-丁烯共聚物、4g磺化的丁烯-乙烯-苯乙烯共聚物和2g酯化的聚苯乙烯磺酸。其余制备条件与实施例1相同。
对比例1
一种PEDOT分散液的制备方法，所述制备方法包括如下步骤：
(1)将2.5g聚苯乙烯-丁二烯共聚物、2.5g丁烯-乙烯-苯乙烯共聚物、5g聚苯乙烯磺酸和80g水混合均匀，得到混合液A；
(2)将0.8g EDOT、0.2g苯胺加入混合液A中，剪切乳化，得到Pickering乳液；
(3)向Pickering乳液中加入0.4g双氧水，待聚合反应完成后，得到所述PEDOT分散液。
对比例2
一种PEDOT分散液的制备方法，所述制备方法中，氧化剂为过硫酸铵，其余制备条件均与实施例1相同。
性能测试
1、电导率
电导率测试方法：在上述制备的PEDOT分散液中加入5％的DMSO搅拌均匀，涂膜干燥后，用四探针测试其PEDOT膜的电导率。
对实施例1～8和对比例1～2制备的PEDOT分散液进行电导率测试，测试结果如表1所示。
表1电导率(S/cm)
Figure BDA0002781814290000061
2、透明度
将PEDOT分散液旋涂在透明PET片上，干燥成膜后，测试550nm处的透光率，从而计算出透明度。
表2透明度率(％)
Figure BDA0002781814290000071
从上述性能测试结果中可知，由本发明公开的方法制备的PEDOT分散液兼具良好的电导率及透明度，表明本发明公开的制备方法适于制备高电导率和高透明度的PEDOT分散液。
最后所应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，但并不脱离本发明技术方案的实质和范围。

Claims (8)

1.一种PEDOT分散液的制备方法，其特征在于，包括如下步骤：
(1)将聚阴离子加入水中，搅拌均匀，得到混合液A；
(2)向混合液A中加入单体，剪切乳化，得到Pickering乳液；
(3)向Pickering乳液中加入氧化剂，发生聚合反应，反应完成后，得到所述PEDOT分散液；
所述步骤(1)中的聚阴离子包括磺化的聚苯乙烯-丁二烯共聚物、磺化的丁烯-乙烯-苯乙烯共聚物、酯化的聚苯乙烯磺酸、十二烷基苯磺酸中的至少一种；
所述步骤(2)中的单体包含3,4-乙撑二氧噻吩和苯胺及苯胺衍生物中的至少一种。
2.如权利要求1所述的PEDOT分散液的制备方法，其特征在于，所述磺化的聚苯乙烯-丁二烯共聚物是以磺酸和聚苯乙烯-丁二烯共聚物以质量比为(0.01-10)：1制备出来的；所述磺化的丁烯-乙烯-苯乙烯共聚物是以磺酸和丁烯-乙烯-苯乙烯共聚物以质量比为(0.01-10)：1制备出来的；所述酯化的聚苯乙烯磺酸是以聚苯乙烯磺酸和乙醇以质量比为1：(0.01～10)制备出来的。
3.如权利要求1所述的PEDOT分散液的制备方法，其特征在于，所述单体、聚阴离子、水、氧化剂的质量比为：单体：聚阴离子：水：氧化剂＝1：(0.2-20)：(10-200)：(0.2-1)。
4.如权利要求3所述的PEDOT分散液的制备方法，其特征在于，所述单体、聚阴离子、水、氧化剂的质量比为：单体：聚阴离子：水：氧化剂＝1：(0.5-15)：(50-100)：(0.3-0.5)。
5.如权利要求4所述的PEDOT分散液的制备方法，其特征在于，所述单体、聚阴离子、水、氧化剂的质量比为：单体：聚阴离子：水：氧化剂＝1：10：80：0.4。
6.如权利要求3～5任一项所述的PEDOT分散液的制备方法，其特征在于，所述单体中3,4-乙撑二氧噻吩与苯胺或苯胺衍生物的质量比为1:(0.01-0.5)。
7.如权利要求3～5任一项所述的PEDOT分散液的制备方法，其特征在于，所述聚阴离子中，磺化的聚苯乙烯-丁二烯共聚物、磺化的丁烯-乙烯-苯乙烯共聚物、酯化的聚苯乙烯磺酸的质量比为：磺化的聚苯乙烯-丁二烯共聚物：磺化的丁烯-乙烯-苯乙烯共聚物：酯化的聚苯乙烯磺酸＝1:1:2。
8.如权利要求1所述的PEDOT分散液的制备方法，其特征在于，所述氧化剂为H2O2。
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