CN106914197A - 一种sps‑pedot复合微球的制备方法 - Google Patents
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Abstract
本发明公开了一种SPS‑PEDOT复合微球的制备方法,该方法包括如下步骤:(1)制备磺化苯乙烯微球作为复合微球的硬模板;(2)在磺化苯乙烯微球表面原位聚合3,4‑乙烯二氧噻吩,制得SPS‑PEDOT复合微球。本发明复合微球解决了传统PEDOT耐水性差和不溶不熔的问题,本发明复合微球具有价格低廉,制备简单等优点。
Description
技术领域
本发明涉及导电材料技术领域,尤其是涉及一种制备导电SPS-PEDOT复合微球的方法。
背景技术
聚3,4-乙烯二氧噻吩(PEDOT)是在1989年由德国Bayer公司合成的新型导电高分子聚合物,因其具有高电导率、良好的环境稳定性以及高透光率等优势被广泛的应用在柔性电极、传感器、OLED、电磁屏蔽材料、太阳能电池中,但PEDOT自身具有不熔不溶的性质,同时也需要通过进一步的掺杂来提高其水分散性和导电性。为了克服这个难题,软模板法掺杂PEDOT被广泛的应用。
聚苯乙烯磺酸钠(PSS)做为软模板掺杂PEDOT已经商品化被用于导电墨水,抗静电涂层中,然而PEDOT:PSS由于PSS的吸水性导致PEDOT:PSS形成的导电膜吸湿性强,PEDOT与PSS进行复合时,PEDOT易形成低聚物的短链段,且在水作为溶剂时,PSS与PEDOT复合后,易形成导电聚合物是核,空间稳定剂为壳的微球,对导电性有一定的影响。
目前,Foulger,王昭群等课题组以聚苯乙烯微球为模板制备PEDOT微球,Shin S.等以功能化纳米Fe3O4磁性粒子做为模板制备PEDOT微球,这类基于乳胶粒子制备的PEDOT水分散体具有的优势是用很少的导电聚合物就能达到较好的电性能,而且导电聚合物做为次要成分,只占总量的5-20%,可以达到节省成本,制备简单等优点。
发明内容
针对现有技术存在的上述问题,本申请人提供了一种SPS-PEDOT复合微球的制备方法。本发明复合微球解决了传统PEDOT耐水性差和不溶不熔的问题,本发明复合微球具有价格低廉,制备简单等优点。
本发明的技术方案如下:
一种SPS-PEDOT复合微球的制备方法,所述方法包括如下步骤:
(1)制备磺化苯乙烯微球作为复合微球的硬模板;
(2)在磺化苯乙烯微球表面原位聚合3,4-乙烯二氧噻吩,制得SPS-PEDOT复合微球。
所述磺化苯乙烯微球的制备方法为:
(1)将苯乙烯磺酸钠与苯乙烯按1:9~3:2的摩尔比在30~60g去离子水中混合,倒入三口烧瓶中后,室温超声20~40min至形成粗乳化液体;
(2)再在室温下,将步骤(1)制得的微乳化液体通过机械搅拌下通氮气处理20~40min,然后升温至65~85℃,冷凝回流1~3h至细乳化液体;
(3)再将过硫酸铵水溶液滴入步骤(2)得到的细乳化液体中,继续反应20~28h结束反应;
(4)将步骤(3)的反应产物依次经过离心、无水乙醇洗3~5次、水洗3~5次,最后冷冻干燥得到磺化苯乙烯微球粉末。
步骤(1)中所述超声的功率为50W~600W。
步骤(2)中所述机械搅拌的转速为250~500rpm。
步骤(3)中所述过硫酸铵水溶液的质量浓度为5~20%;所述过硫酸铵水溶液中过硫酸铵的质量与苯乙烯磺酸钠和苯乙烯总量的比为0.01~0.05:1。
所述原位聚合的具体步骤为:
(1)将磺化苯乙烯微球与3,4-乙烯二氧噻吩单体按照5~1:1的质量比混合在30~60g去离子水中,倒入三口烧瓶中后,室温超声20~50min至3,4-乙烯二氧噻吩均匀的吸附在磺化苯乙烯微球的表面;
(2)用盐酸将反应溶液的pH值调为3~5,通氮气,在转速为300~700rpm的条件下磁力搅拌20min,再加入引发剂,室温下继续搅拌反应20~30h;
(3)将步骤(2)所得反应产物透析至pH值为6~7,通过冷冻干燥得到蓝色SPS-PEDOT复合微球粉末。
步骤(1)中所述超声的功率为50~600W。
步骤(2)中所述引发剂为过硫酸铵与硫酸铁的混合溶液,其中过硫酸铵、硫酸铁与3,4-乙烯二氧噻吩的摩尔比为1~3:0.01~0.1:0.8~1.2。
本发明有益的技术效果在于:
(1)本发明先制备了可在水中分散的SPS微球,再以SPS微球作为模板法制得在水中高度分散的SPS-PEDOT复合微球,使PEDOT更易被进一步的加工,制备方法简单易得。
(2)本发明以两步法制备SPS-PEDOT复合微球,SPS微球表面的磺酸根带有负电荷,可以吸附弱正电的EDOT单体,保证了PEDOT可以包覆在SPS微球的表面上形成SPS为核,PEDOT为壳的SPS-PEDOT复合微球,同时单体EDOT原材料较为昂贵,将导电聚合物作为次要成分聚合在SPS复合微球的表面上,可以大大降低对EDOT的使用,节省成本。
(2)本发明制备的SPS微球表面的磺酸根对PEDOT的掺杂作用赋予了微球导电性,且微球之间导电聚合物壳PEDOT的直接接触,降低了不导电模板对电性能的影响,提高PEDOT的电性能。
附图说明
图1为本发明在实施例1中制备的SPS微球和SPS-PEDOT复合微球的TEM图;
其中,a、SPS微球;b、SPS-PEDOT复合微球。
图2为实施例1制得的SPS微球和实施例1~3制得的SPS-PEDOT复合微球配制的浓度为1mg/ml水分散液(静置七天)。
具体实施方式
下面结合附图和实施例,对本发明进行具体描述。
实施例1
一种SPS-PEDOT复合微球的制备方法,所述方法包括如下步骤:
(1)制备磺化苯乙烯微球作为复合微球的硬模板;
①将1.146g苯乙烯磺酸钠与5.2g苯乙烯在30g去离子水中混合,倒入三口烧瓶中后,在50W的功率下室温超声20min至形成粗乳化液体;
②再在室温下,将步骤①制得的微乳化液体通过250rpm的机械搅拌下通氮气处理20min,然后升温至65℃,冷凝回流1h得到细乳化液体;
③再将1.26ml过硫酸铵水溶液(质量浓度为5%)滴入步骤②的细乳化液体中,继续反应20h结束反应;
④将步骤③的反应产物依次经过离心、无水乙醇洗3次、水洗3次,最后冷冻干燥得到磺化苯乙烯微球粉末。
(2)在磺化苯乙烯微球表面原位聚合3,4-乙烯二氧噻吩,制得SPS-PEDOT复合微球;
①将1g磺化苯乙烯微球与0.2g 3,4-乙烯二氧噻吩单体混合在30g去离子水中,倒入三口烧瓶中后,在50W的功率下室温超声20min至3,4-乙烯二氧噻吩均匀的吸附在磺化苯乙烯微球的表面;
②用盐酸将反应溶液的pH值调为3,通氮气,在转速为300rpm的条件下磁力搅拌20min,再加入0.4g过硫酸铵与0.075g硫酸铁引发剂,室温下继续搅拌反应20h;
③将步骤②所得反应产物透析至pH值为6,通过冷冻干燥得到蓝色SPS-PEDOT复合微球粉末。
本实施例制备的SPS微球和SPS-PEDOT复合微球的TEM图如图1所示,由图可以看出,本发明制备的微球的形状规则圆润,且得到的SPS-PEDOT复合微球与光滑的SPS微球相比,表面变粗糙,也表明PEDOT成功复合在SPS微球的表面上。
将本发明实施例中制得的SPS微球和SPS-PEDOT复合微球配制的浓度为1mg/ml水分散液后静置七天,观察分散液的状态,如图2所示,由图2可以看出,本发明制备微球在水中具有较好的分散稳定性。
实施例2
一种SPS-PEDOT复合微球的制备方法,所述方法包括如下步骤:
(1)制备磺化苯乙烯微球作为复合微球的硬模板;
①将6.87g苯乙烯磺酸钠与5.2g苯乙烯在50g去离子水中混合,倒入三口烧瓶中后,在100W的功率下室温超声30min至形成粗乳化液体;
②再在室温下,将步骤①制得的微乳化液体通过300rpm的机械搅拌下通氮气处理30min,然后升温至75℃,冷凝回流1.5h得到细乳化液体;
③再将6ml过硫酸铵水溶液(质量浓度为10%)滴入步骤②的细乳化液体中,继续反应25h结束反应;
④将步骤③的反应产物依次经过离心、无水乙醇洗3次、水洗4次,最后冷冻干燥得到磺化苯乙烯微球粉末。
(2)在磺化苯乙烯微球表面原位聚合3,4-乙烯二氧噻吩,制得SPS-PEDOT复合微球;
①将1g磺化苯乙烯微球与0.33g 3,4-乙烯二氧噻吩单体混合在40g去离子水中,倒入三口烧瓶中后,在300W的功率下室温超声40min至3,4-乙烯二氧噻吩均匀的吸附在磺化苯乙烯微球的表面;
②用盐酸将反应溶液的pH值调为4,通氮气,在转速为400rpm的条件下磁力搅拌20min,再加入1.05g过硫酸铵与0.46g硫酸铁引发剂,室温下继续搅拌反应25h;
③将步骤②所得反应产物透析至pH值为6,通过冷冻干燥得到蓝色SPS-PEDOT复合微球粉末。
将本发明实施例中制得的SPS-PEDOT复合微球配制的浓度为1mg/ml水分散液后静置七天,观察分散液的状态,如图2所示。
实施例3
一种SPS-PEDOT复合微球的制备方法,所述方法包括如下步骤:
(1)制备磺化苯乙烯微球作为复合微球的硬模板;
①将15.4g苯乙烯磺酸钠与5.2g苯乙烯在60g去离子水中混合,倒入三口烧瓶中后,在100W的功率下室温超声40min至形成粗乳化液体;
②再在室温下,将步骤①制得的微乳化液体通过500rpm的机械搅拌下通氮气处理40min,然后升温至85℃,冷凝回流3h得到细乳化液体;
③再将5.15ml过硫酸铵水溶液(质量浓度为20%)滴入步骤②的细乳化液体中,继续反应28h结束反应;
④将步骤③的反应产物依次经过离心、无水乙醇洗5次、水洗5次,最后冷冻干燥得到磺化苯乙烯微球粉末。
(2)在磺化苯乙烯微球表面原位聚合3,4-乙烯二氧噻吩,制得SPS-PEDOT复合微球;
①将1g磺化苯乙烯微球与1g 3,4-乙烯二氧噻吩单体混合在60g去离子水中,倒入三口烧瓶中后,在600W的功率下室温超声50min至3,4-乙烯二氧噻吩均匀的吸附在磺化苯乙烯微球的表面;
②用盐酸将反应溶液的pH值调为5,通氮气,在转速为700rpm的条件下磁力搅拌20min,再加入4.01g过硫酸铵与0.23g硫酸铁引发剂,室温下继续搅拌反应30h;
③将步骤②所得反应产物透析至pH值为7,通过冷冻干燥得到蓝色SPS-PEDOT复合微球粉末。
将本发明实施例中制得的SPS-PEDOT复合微球配制的浓度为1mg/ml水分散液后静置七天,观察分散液的状态,如图2所示。
测试例:
对实施例1~3中制备的SPS微球与SPS-PEDOT复合微球进行测试,通过元素分析测试仪测定SPS微球的磺酸根基团;通过Zeta纳米粒度仪测定稀释至1wt%的SPS微球与SPS-PEDOT复合微球的粒径并计算SPS-PEDOT复合微球的多分散性系数;再通过RTS-9型双电测四探针测试仪测定SPS-PEDOT复合微球粉末的电导率,测试值如表1所示。
表1
由表1可以看出,随着苯乙烯磺酸钠单体含量的增加,SPS微球的粒径逐渐下降,微球表面磺酸根的含量逐渐上升,SPS-PEDOT复合微球随着EDOT单体含量的增加,微球的导电性逐渐增强;SPS-PEDOT复合微球的多分散性系数(DW/DN)均小于0.1,表明了本发明制备的SPS-PEDOT复合微球的粒子分布集中,在水溶液中无聚集,呈现分散状态。
Claims (8)
1.一种SPS-PEDOT复合微球的制备方法,其特征在于所述方法包括如下步骤:
(1)制备磺化苯乙烯微球作为复合微球的硬模板;
(2)在磺化苯乙烯微球表面原位聚合3,4-乙烯二氧噻吩,制得SPS-PEDOT复合微球。
2.根据权利要求1所述的制备方法,其特征在于所述磺化苯乙烯微球的制备方法为:
(1)将苯乙烯磺酸钠与苯乙烯按1:9~3:2的摩尔比在30~60g去离子水中混合,倒入三口烧瓶中后,室温超声20~40min至形成粗乳化液体;
(2)再在室温下,将步骤(1)制得的微乳化液体通过机械搅拌下通氮气处理20~40min,然后升温至65~85℃,冷凝回流1~3h至细乳化液体;
(3)再将过硫酸铵水溶液滴入步骤(2)得到的细乳化液体中,继续反应20~28h结束反应;
(4)将步骤(3)的反应产物依次经过离心、无水乙醇洗3~5次、水洗3~5次,最后冷冻干燥得到磺化苯乙烯微球粉末。
3.根据权利要求2所述的制备方法,其特征在于步骤(1)中所述超声的功率为50W~600W。
4.根据权利要求2所述的制备方法,其特征在于步骤(2)中所述机械搅拌的转速为250~500rpm。
5.根据权利要求2所述的制备方法,其特征在于步骤(3)中所述过硫酸铵水溶液的质量浓度为5~20%;所述过硫酸铵水溶液中过硫酸铵的质量与苯乙烯磺酸钠和苯乙烯总量的比为0.01~0.05:1。
6.根据权利要求1所述的制备方法,其特征在于所述原位聚合的具体步骤为:
(1)将磺化苯乙烯微球与3,4-乙烯二氧噻吩单体按照5~1:1的质量比混合在30~60g去离子水中,倒入三口烧瓶中后,室温超声20~50min至3,4-乙烯二氧噻吩均匀的吸附在磺化苯乙烯微球的表面;
(2)用盐酸将反应溶液的pH值调为3~5,通氮气,在转速为300~700rpm的条件下磁力搅拌20min,再加入引发剂,室温下继续搅拌反应20~30h;
(3)将步骤(2)所得反应产物透析至pH值为6~7,通过冷冻干燥得到蓝色SPS-PEDOT复合微球粉末。
7.根据权利要求6所述的制备方法,其特征在于步骤(1)中所述超声的功率为50~600W。
8.根据权利要求6所述的制备方法,其特征在于步骤(2)中所述引发剂为过硫酸铵与硫酸铁的混合溶液,其中过硫酸铵、硫酸铁与3,4-乙烯二氧噻吩的摩尔比为1~3:0.01~0.1:0.8~1.2。
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