CN107503217A - 一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸及其制备方法 - Google Patents
一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸及其制备方法,其特征在于,将乙醇水浴加热,加硬脂酸、干燥粉碎的铝粉,搅拌,静置分层,吸去上层溶液,烘干后与二甲基硅油混合,搅拌,焙烧得硬脂酸表面处理的铝粉导热硅脂;向碳纤维中加丙酮,浸泡处理,再浸泡于浓硝酸中,得表面氧化处理的碳纤维;向木质纸浆中加蒸馏水、对甲苯磺酸、氯化铁,调pH,置于冰水浴中,用液体取样器滴加吡咯单体,反应得复合导电纤维;将复合导电纤维与水溶性聚乙烯醇纤维、前面所得物料混合,用打浆机进行疏解打浆,使纤维分丝帚化,在标准纸页成型器上成型抄纸,用油压机压榨,置于的减压烘缸内干燥,得到复合导电纸。
Description
技术领域
本发明涉及导电纸领域,具体涉及一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸及其制备方法。
背景技术
随着LED在生活生产中的广泛应用,发现LED的芯片在使用的过程中产生大量的热量,热量的积累会缩短其寿命,所以如何改善LED 封装材料的导热性能,是急需解决的难题。
李巧梅在其硕士学位论文《导热微粒烧结和复合材料取向对大功率LED散热的影响》中,以环氧树脂为基体,分别以二氧化硅、碳化硅为导热微粒,制备了高比例导热微粒陶瓷片和取向型高导热聚合物基复合材料,其中高比例导热微粒陶瓷片用在LED的陶瓷片上,而取向型复合材料用在LED的封装上。用硅烷偶联剂对导热颗粒进行表面处理,用氧化钇和氧化镁作为烧结剂,得到高导热的碳化硅共烧陶瓷片。但是存在导热性能、力学性能不足。
发明内容
本发明主要解决的技术问题是提供一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸及其制备方法,依照该工艺制备的复合导电纸具有良好的力学性能和导电导热性能。
本发明所要解决的技术问题采用以下的技术方案来实现:
一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸的制备方法,其特征在于,按以下步骤进行:
a. 将乙醇水浴加热到60-70℃,加入1-2重量份硬脂酸,搅拌溶解,投入干燥粉碎的铝粉,在70-80℃下搅拌1-2h,静置分层,吸去上层溶液,放入80-90℃烘箱烘干2-3h,与4-7重量份二甲基硅油混合,放入胶体搅拌器搅拌1-2h,将所得硅脂在140-150℃下焙烧4-5h,再机械搅拌1-2h,得硬脂酸表面处理的铝粉导热硅脂;
b. 向5-8重量份碳纤维中1:5-10加入丙酮,浸泡处理4-6h,反复水洗,除去丙酮及杂质,再1:3-5浸泡于浓硝酸中1-2h,用蒸馏水清洗3-5次,超声振荡清洗1-2h,置于干燥箱中在90-100℃下干燥4-5h,得表面氧化处理的碳纤维;
c. 复合导电纤维的合成:
向40-50重量份木质纸浆中1:15-20加入蒸馏水,搅拌10-20min分散均匀,得到纸浆纤维悬浮液;加入2-4重量份对甲苯磺酸,搅拌20-30min,加入5-9重量份氯化铁,再搅拌10-20min,用稀盐酸调pH为2-3,搅拌10-20min,置于冰水浴中,用液体取样器滴加1-2重量份吡咯单体,反应1-2h,静置,倒去上层清液,减压过滤、洗涤3-5次,得复合导电纤维;
d. 复合导电纸的制备:
将c中所得复合导电纤维与10-20重量份水溶性聚乙烯醇纤维、a、b中所得物料混合,用打浆机进行疏解打浆,使纤维分丝帚化,在标准纸页成型器上成型抄纸,用油压机在0.5-1MPa下压榨5-10min,再置于105-115℃的减压烘缸内干燥10-20min,取出冷却至室温,得到复合导电纸。
其中,步骤a中所述干燥粉碎的铝粉是指将6-9重量份铝粉在105-115℃下真空干燥5-7h,机械研磨粉碎,过600-800目筛。步骤c中所述稀盐酸质量分数为5-10%。步骤d中所述打浆度为45-50ºSR。
本发明的反应机理及有益效果如下:
以水溶性聚乙烯醇(PVA)纤维为基材,以三氯化铁为氧化剂,吡咯单体在基材表面具有良好的吸附性能,通过原位合成法,将聚吡咯导电性能与基材优异的力学性能相结合,制备了聚吡咯包覆的复合导电纸。先对铝粉填料进行了研磨粉碎处理,其粒径越小,导热硅脂热导率越高;用硬脂酸对填料铝粉进行表面处理,在铝粉表面形成一层有机包覆层,有利于提高导热硅脂的热导率;采用液相氧化法对碳纤维进行表面氧化处理,提高其与基材的相容性,通过碳纤维增强复合导电纸的力学性能,增强效果好。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例,进一步阐述本发明。
实施例
一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸的制备方法,其特征在于,按以下步骤进行:
a. 将乙醇水浴加热到60-70℃,加入1kg硬脂酸,搅拌溶解,投入干燥粉碎的铝粉,在70-80℃下搅拌1h,静置分层,吸去上层溶液,放入80-90℃烘箱烘干2h,与4kg二甲基硅油混合,放入胶体搅拌器搅拌1h,将所得硅脂在140-150℃下焙烧4h,再机械搅拌1h,得硬脂酸表面处理的铝粉导热硅脂;
b. 向5kg碳纤维中1:5加入丙酮,浸泡处理4h,反复水洗,除去丙酮及杂质,再1:5浸泡于浓硝酸中1h,用蒸馏水清洗3次,超声振荡清洗1h,置于干燥箱中在90-100℃下干燥4h,得表面氧化处理的碳纤维;
c. 复合导电纤维的合成:
向50kg木质纸浆中1:20加入蒸馏水,搅拌20min分散均匀,得到纸浆纤维悬浮液;加入2kg对甲苯磺酸,搅拌20-30min,加入5kg氯化铁,再搅拌20min,用稀盐酸调pH为2-3,搅拌20min,置于冰水浴中,用液体取样器滴加2kg吡咯单体,反应2h,静置,倒去上层清液,减压过滤、洗涤5次,得复合导电纤维;
d. 复合导电纸的制备:
将c中所得复合导电纤维与20kg水溶性聚乙烯醇纤维、a、b中所得物料混合,用打浆机进行疏解打浆,使纤维分丝帚化,在标准纸页成型器上成型抄纸,用油压机在1MPa下压榨10min,再置于105-115℃的减压烘缸内干燥20min,取出冷却至室温,得到复合导电纸。
其中,步骤a中所述干燥粉碎的铝粉是指将6kg铝粉在105-115℃下真空干燥6h,机械研磨粉碎,过600目筛。步骤c中所述稀盐酸质量分数为5%。步骤d中所述打浆度为45ºSR。
Claims (5)
1.一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸的制备方法,其特征在于:
将乙醇水浴加热,加硬脂酸、干燥粉碎的铝粉,搅拌,静置分层,吸去上层溶液,烘干后与二甲基硅油混合,搅拌,焙烧得硬脂酸表面处理的铝粉导热硅脂;向碳纤维中加丙酮,浸泡处理,再浸泡于浓硝酸中,得表面氧化处理的碳纤维;向木质纸浆中加蒸馏水、对甲苯磺酸、氯化铁,调pH,置于冰水浴中,用液体取样器滴加吡咯单体,反应得复合导电纤维;将复合导电纤维与水溶性聚乙烯醇纤维、前面所得物料混合,用打浆机进行疏解打浆,使纤维分丝帚化,在标准纸页成型器上成型抄纸,用油压机压榨,置于的减压烘缸内干燥,得到复合导电纸。
2.一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸的制备方法,其特征
在于:
a. 将乙醇水浴加热到60-70℃,加入1-2重量份硬脂酸,搅拌溶解,投入干燥粉碎的铝粉,在70-80℃下搅拌1-2h,静置分层,吸去上层溶液,放入80-90℃烘箱烘干2-3h,与4-7重量份二甲基硅油混合,放入胶体搅拌器搅拌1-2h,将所得硅脂在140-150℃下焙烧4-5h,再机械搅拌1-2h,得硬脂酸表面处理的铝粉导热硅脂;
b. 向5-8重量份碳纤维中1:5-10加入丙酮,浸泡处理4-6h,反复水洗,除去丙酮及杂质,再1:3-5浸泡于浓硝酸中1-2h,用蒸馏水清洗3-5次,超声振荡清洗1-2h,置于干燥箱中在90-100℃下干燥4-5h,得表面氧化处理的碳纤维;
c. 复合导电纤维的合成:
向40-50重量份木质纸浆中1:15-20加入蒸馏水,搅拌10-20min分散均匀,得到纸浆纤维悬浮液;加入2-4重量份对甲苯磺酸,搅拌20-30min,加入5-9重量份氯化铁,再搅拌10-20min,用稀盐酸调pH为2-3,搅拌10-20min,置于冰水浴中,用液体取样器滴加1-2重量份吡咯单体,反应1-2h,静置,倒去上层清液,减压过滤、洗涤3-5次,得复合导电纤维;
d. 复合导电纸的制备:
将c中所得复合导电纤维与10-20重量份水溶性聚乙烯醇纤维、a、b中所得物料混合,用打浆机进行疏解打浆,使纤维分丝帚化,在标准纸页成型器上成型抄纸,用油压机在0.5-1MPa下压榨5-10min,再置于105-115℃的减压烘缸内干燥10-20min,取出冷却至室温,得到复合导电纸。
3.根据权利要求2所述的一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸的制备方法,其特征在于,步骤a中所述干燥粉碎的铝粉是指将6-9重量份铝粉在105-115℃下真空干燥5-7h,机械研磨粉碎,过600-800目筛。
4.根据权利要求2所述的一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸的制备方法,其特征在于,步骤c中所述稀盐酸质量分数为5-10%。
5.根据权利要求2所述的一种聚乙烯醇纤维增强的聚吡咯包覆的复合导电纸的制备方法,其特征在于,步骤d中所述打浆度为45-50ºSR。
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