CN106120458B - 一种聚酰亚胺导电纸的制备方法 - Google Patents

一种聚酰亚胺导电纸的制备方法 Download PDF

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CN106120458B
CN106120458B CN201610487328.XA CN201610487328A CN106120458B CN 106120458 B CN106120458 B CN 106120458B CN 201610487328 A CN201610487328 A CN 201610487328A CN 106120458 B CN106120458 B CN 106120458B
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龙柱
刘崇崇
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Lianyungang industrial investment Group Co., Ltd
Lianyungang New Fiber Materials Research Institute Co Ltd
Jiangnan University
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Abstract

本发明涉及一种聚酰亚胺导电纸的制备方法，属于耐高温、高导电纸基材料技术领域。其通过聚酰亚胺纤维的预处理、聚酰亚胺纤维原纸的制备、聚酰亚胺树脂溶液的配置和聚酰亚胺导电纸的制备制得最终产品。本发明所制备的聚酰亚胺导电纸具有良好的导电性能，还具有良好的耐高温性能、机械性能和柔韧性能，可以代替聚酰亚胺导电薄膜和芳纶导电纸用于电磁屏蔽、静电吸附等领域。

Description

一种聚酰亚胺导电纸的制备方法
技术领域
本发明涉及一种聚酰亚胺导电纸的制备方法，属于耐高温、高导电纸基材料技术领域。
背景技术
导电材料广泛用作通讯制品、医疗仪器、家用电子产品和航天国防等电子设备的电磁屏蔽材料和静电吸附材料。随着科技的快速发展，传统导电材料在环境要求高的领域的应用受到了限制。聚合物基导电复合材料由于其成型工艺简单、耐腐蚀等特点得到了广泛应用。聚合物基导电复合材料通常是在聚合物基体中添加导电材料（如碳材料、金属粉末、金属纤维等）制备得到的。芳香族聚酰胺和聚酰亚胺具有耐热、耐腐蚀等优越的综合性能，因此，芳纶导电材料和聚酰亚胺导电材料（如聚酰亚胺导电薄膜、聚酰亚胺导电涂料等）得到了广泛研究，但仍然存在一些缺陷。
具体如：专利文献1，杜邦帝人先进纸（日本）有限公司，CN201280027649.1，公开了在芳纶纤维中添加金属纤维或碳纤维制备得到芳纶导电纸，但其导电性和机械强度较差。专利文献2，北京化工大学，CN200510002082.4，提出对聚酰亚胺薄膜进行碱处理，引入银离子制备导电聚酰亚胺薄膜的方法，但其导电性和机械强度存在问题。专利文献3，北京化工大学常州先进材料研究院，CN201510350795.3，提出在聚酰胺酸溶液或聚酰亚胺树脂中添加导电填料，制备聚酰亚胺导电薄膜或聚酰亚胺导电涂料，但其柔韧性较差。
聚酰亚胺纸具有比芳纶纸更加优越的强度性能和耐高温性能，具有比聚酰亚胺薄膜更加优异的柔韧性能。目前，国内外还没有关于聚酰亚胺导电纸基材料的专利报导。
发明内容
本发明的目的在于针对现有导电材料存在的问题和聚酰亚胺导电纸基材料的技术空白，提供一种聚酰亚胺导电纸的制备方法。该纸基材料利用碳材料在聚酰亚胺树脂溶液中形成三维网络结构，金属粒子围绕网络结构富集，将聚酰亚胺原纸在此聚酰亚胺树脂溶液中浸渍，得到导电性能良好的聚酰亚胺纸基材料。同时，保留了聚酰亚胺纸基材料优异的耐高温性能、力学性能、柔韧性能和耐腐蚀性能。
按照本发明提供的技术方案，一种聚酰亚胺导电纸的制备方法，步骤如下：
（1）聚酰亚胺纤维的预处理：取聚酰亚胺纤维置于温度为20-60℃，含有0.01-10g/L十二烷基硫酸钠的、质量浓度为5%-30%的氢氧化钠或氢氧化钾溶液中，采用超声辅助处理；超声处理条件如下：温度为20-60℃，超声波频率为20-100 kHz，时间为0.5 -60min；取出处理后的聚酰亚胺纤维，用去离子水进行洗涤；
（2）聚酰亚胺纤维原纸的制备：利用湿法抄造的方法，将经过处理的聚酰亚胺纤维制备成聚酰亚胺纤维原纸；
（3）聚酰亚胺树脂溶液的配置：
a、超声分散：取纳米级的碳材料、纳米级的金属粉和有机溶剂，碳材料：金属粉：有机溶剂重量比为5-35：5-35：20-80；首先将纳米级的碳材料加入到有机溶剂中，进行超声分散处理。超声处理条件如下：温度为20-50℃，超声波频率为20-100 kHz，时间为10min-8h；然后加入金属粉，搅拌5min-3h，再进行超声处理，超声处理条件如下：温度为20-50℃，超声波频率为20 -100kHz，时间为1min-4h。
b、溶液配置：在上述有机溶剂中加入聚酰亚胺树脂，使得聚酰亚胺树脂质量浓度为0.5%-20%，不断搅拌使碳材料和金属粉均匀分散在聚酰亚胺树脂溶液中；
（4）聚酰亚胺导电纸的制备：将步骤（2）制备所得的聚酰亚胺纤维原纸在步骤（3）制备所得的聚酰亚胺树脂溶液中充分浸渍，然后在70-90℃下将导电纸的干度烘干至90%以上，并热压，即得到产品聚酰亚胺导电纸。
步骤（3）所述纳米级的碳材料为碳系导电颗粒，具体为炭黑、碳纳米管或碳纳米纤维中的一种。步骤（3）所述纳米级的金属粉为银粉、镍粉、银包铜粉或镍包铜粉中的一种或多种。步骤（3）所述有机溶剂为N,N-二甲基甲酰胺、N,N-二甲基乙酰胺或N-甲基吡咯烷酮中的一种。
步骤（4）所述热压工艺如下：所述热压为一阶段热压、二阶段热压或三阶段热压；热压参数均为温度80-300℃，压力2-30MPa，时间1s-10min。
制备所得聚酰亚胺导电纸厚度为0.02-0.8mm，导电粒子占整个聚酰亚胺导电纸重量的2%-50%。
本发明的有益效果：本发明所制备的聚酰亚胺导电纸具有良好的导电性能，还具有良好的耐高温性能、机械性能和柔韧性能，可以代替聚酰亚胺导电薄膜和芳纶导电纸用于电磁屏蔽、静电吸附等领域。
附图说明
图1是本发明具体工艺流程图。
具体实施方式
为了能够更清楚地理解本发明的技术内容，特举以下实施例详细说明，其目的仅在于更好理解本发明的内容而非限制本发明的保护范围。
以下实施例中具体湿法抄造的方法如CN201110300366.7所示。
实施例1
（1）聚酰亚胺纤维的预处理：将适量聚酰亚胺纤维置于温度为20℃，质量分数为20%，添加了0.5 g/L十二烷基硫酸钠的氢氧化钠溶液中，超声辅助处理2min，超声处理条件如下：温度为20℃，超声波频率为50kHz；然后，用去离子水进行洗涤。
（2）将经过处理的聚酰亚胺纤维，利用湿法抄造的方法制备聚酰亚胺纤维原纸。
（3）聚酰亚胺树脂溶液的配置：将15份炭黑加入到65份N,N-二甲基乙酰胺中，在20℃、30kHz的条件下超声处理2h。然后，加入20份纳米银粉，搅拌5min，再在50℃、20kHz的条件下超声处理2h。使炭黑和银粉均匀分散在N,N-二甲基乙酰胺中。用此N,N-二甲基乙酰胺溶液配置浓度为5%的聚酰亚胺树脂溶液，不断搅拌使炭黑和银粉均匀分散在聚酰亚胺树脂溶液中。
（4）聚酰亚胺导电纸的制备：将聚酰亚胺纤维原纸在聚酰亚胺树脂溶液中充分浸渍，然后，80℃烘干并热压，热压工艺如下：第一阶段：120℃、5MPa、1min；第二阶段：180℃、10MPa、1min；第三阶段：290℃、15MPa、1min，即得到导电聚酰亚胺纸基材料。
实施例2
（1）聚酰亚胺纤维的预处理：将适量聚酰亚胺纤维置于温度为40℃，质量分数为10%，添加了0.5g/L十二烷基硫酸钠的氢氧化钾溶液中，超声辅助处理5min，超声处理条件如下：温度为40℃，超声波频率为100kHz；然后，用去离子水进行洗涤。
（2）将经过处理的聚酰亚胺纤维，利用湿法抄造的方法制备聚酰亚胺纤维原纸。
（3）聚酰亚胺树脂溶液的配置：将10份炭黑加入到70份N,N-二甲基甲酰胺中，在20℃、50kHz的条件下超声处理1h，然后，加入20份纳米银粉，搅拌10min，再在40℃、50kHz的条件下超声处理15min，使炭黑和银粉均匀分散在N,N-二甲基甲酰胺中。用此N,N-二甲基甲酰胺溶液配置浓度为5%的聚酰亚胺树脂溶液，不断搅拌使使炭黑和银粉均匀分散在聚酰亚胺树脂溶液中。
（4）聚酰亚胺导电纸的制备：将聚酰亚胺纤维原纸在聚酰亚胺树脂溶液中充分浸渍，然后，90℃烘干并热压，热压工艺如下：温度为290℃，压力为15MPa、时间为1min，即得到导电聚酰亚胺纸基材料。
实施例3
（1）聚酰亚胺纤维的预处理：将适量聚酰亚胺纤维置于温度为20℃，质量分数为20%，添加了1g/L十二烷基硫酸钠的氢氧化钠溶液中，超声辅助处理8 min，超声处理条件如下：温度为20-60℃，超声波频率为30kHz；然后，用去离子水进行洗涤。
（2）将经过处理的聚酰亚胺纤维，利用湿法抄造的方法制备聚酰亚胺纤维原纸。
（3）聚酰亚胺树脂溶液的配置：将20份碳纳米管加入到60份N-甲基吡咯烷酮中，在30℃、50kHz的条件下超声处理1h。然后，加入20份纳米镍粉，搅拌10min，在30℃、20kHz的条件下超声处理10min，使碳纳米管和镍粉均匀分散在N-甲基吡咯烷酮中。用此N-甲基吡咯烷酮溶液配置浓度为8%的聚酰亚胺树脂溶液，不断搅拌使碳纳米管和镍粉均匀分散在聚酰亚胺树脂溶液中。
（4）聚酰亚胺导电纸的制备：将聚酰亚胺纤维原纸在聚酰亚胺树脂溶液中充分浸渍，然后，80℃烘干并热压，热压工艺如下：第一阶段：120℃、5MPa、30s；第二阶段：290℃、15MPa、30s，即得到导电聚酰亚胺纸基材料。
实施例4
（1）聚酰亚胺纤维的预处理：将适量聚酰亚胺纤维置于温度为60℃，质量分数为10%，添加了1g/L十二烷基硫酸钠的氢氧化钾溶液中，超声辅助处理5 min，超声处理条件如下：温度为60℃，超声波频率为70kHz；然后，用去离子水进行洗涤。
（2）将经过处理的聚酰亚胺纤维，利用湿法抄造的方法制备聚酰亚胺纤维原纸。
（3）聚酰亚胺树脂溶液的配置：将15份碳纳米纤维加入到70份N-甲基吡咯烷酮中，在20℃、100kHz的条件下超声处理20min。然后，加入15份银包铜粉，搅拌30min，再在40℃、30kHz的条件下超声处理10min，使碳纳米纤维和银包铜粉均匀分散在N-甲基吡咯烷酮中。用此N-甲基吡咯烷酮溶液配置浓度为10%的聚酰亚胺树脂溶液，不断搅拌使碳纳米纤维和银包铜粉均匀分散在聚酰亚胺树脂溶液中。
（4）聚酰亚胺导电纸的制备：将聚酰亚胺纤维原纸在聚酰亚胺树脂溶液中充分浸渍，然后，90℃烘干并热压，热压工艺如下：温度为250℃，压力为20MPa、时间为10min，即得到导电聚酰亚胺纸基材料。
实施例5
（1）聚酰亚胺纤维的预处理：将适量聚酰亚胺纤维置于温度为30℃，质量分数为25%，添加了0.8g/L十二烷基硫酸钠的氢氧化钾溶液中，超声辅助处理5min，超声处理条件如下：温度为20-60℃，超声波频率为80kHz；然后，用去离子水进行洗涤。
（2）聚酰亚胺纤维原纸的制备：将经过处理的聚酰亚胺纤维，利用湿法抄造的方法制备聚酰亚胺纤维原纸。
（3）聚酰亚胺树脂溶液的配置：将25份碳纳米管加入到55份N,N-二甲基乙酰胺中，在30℃、20kHz的条件下超声处理4h。然后，加入15份银包铜粉，搅拌2h，在20℃、100kHz的条件下超声处理4h，使碳纳米管和银包铜粉均匀分散在N,N-二甲基乙酰胺中。用此N,N-二甲基乙酰胺溶液配置浓度为2%的聚酰亚胺树脂溶液，不断搅拌使碳纳米管和银包铜粉均匀分散在聚酰亚胺树脂溶液中。
（4）聚酰亚胺导电纸的制备：将聚酰亚胺纤维原纸在聚酰亚胺树脂溶液中充分浸渍，然后，70℃烘干并热压，热压工艺如下：温度为280℃，压力为20MPa、时间为30s，即得到导电聚酰亚胺纸基材料。
实施例6
（1）聚酰亚胺纤维的预处理：将适量聚酰亚胺纤维置于温度为60℃，质量分数为20%，添加了5g/L十二烷基硫酸钠的氢氧化钠溶液中，超声辅助处理2 min，然后，用去离子水进行洗涤。
（2）聚酰亚胺纤维原纸的制备：将经过处理的聚酰亚胺纤维，利用湿法抄造的方法制备聚酰亚胺纤维原纸。
（3）聚酰亚胺树脂溶液的配置：将25份碳纳米纤维加入到50份N-甲基吡咯烷酮中，在40℃、20kHz的条件下超声处理1h。然后，加入25份银粉，搅拌1h，在30℃、30kHz的条件下超声处理1h，使碳纳米纤维和银粉均匀分散在N-甲基吡咯烷酮中。用此N-甲基吡咯烷酮溶液配置浓度为8%的聚酰亚胺树脂溶液，不断搅拌使碳纳米纤维和银粉均匀分散在聚酰亚胺树脂溶液中。
（4）聚酰亚胺导电纸的制备：将聚酰亚胺纤维原纸在聚酰亚胺树脂溶液中充分浸渍，然后，70℃烘干并热压，热压工艺如下：第一阶段：80℃、5MPa、5s；第二阶段：200℃、10MPa、5s；第三阶段：280℃、20MPa、1min，即得到导电聚酰亚胺纸基材料。

Claims (3)

1.一种聚酰亚胺导电纸的制备方法，其特征是步骤如下：
（1）聚酰亚胺纤维的预处理：取聚酰亚胺纤维置于温度为20-60℃，含有0.01-10g/L十二烷基硫酸钠的、质量浓度为5%-30%的氢氧化钠或氢氧化钾溶液中，采用超声辅助处理；超声处理条件如下：温度为20-60℃，超声波频率为20-100kHz，时间为0.5-60min；取出处理后的聚酰亚胺纤维，用去离子水进行洗涤；
（2）聚酰亚胺纤维原纸的制备：利用湿法抄造的方法，将经过处理的聚酰亚胺纤维制备成聚酰亚胺纤维原纸；
（3）聚酰亚胺树脂溶液的配置：
a、超声分散：取纳米级的碳材料、纳米级的金属粉和有机溶剂，碳材料：金属粉：有机溶剂重量比为5-35：5-35：20-80；首先将纳米级的碳材料加入到有机溶剂中，进行超声分散处理；
超声处理条件如下：温度为20-50℃，超声波频率为20-100kHz，时间为10min-8h；然后加入金属粉，搅拌5min-3h，再进行超声处理，超声处理条件如下：温度为20-50℃，超声波频率为20-100kHz，时间为1min-4h；
b、溶液配置：在上述有机溶剂中加入聚酰亚胺树脂，使得聚酰亚胺树脂质量浓度为0.5%-20%，不断搅拌使碳材料和金属粉均匀分散在聚酰亚胺树脂溶液中；
（4）聚酰亚胺导电纸的制备：将步骤（2）制备所得的聚酰亚胺纤维原纸在步骤（3）制备所得的聚酰亚胺树脂溶液中充分浸渍，然后在70-90℃下将导电纸的干度烘干至90%以上，并热压，即得到产品聚酰亚胺导电纸；
步骤（3）所述有机溶剂为N,N-二甲基甲酰胺、N,N-二甲基乙酰胺或N-甲基吡咯烷酮中的一种；
步骤（4）所述热压工艺如下：所述热压为一阶段热压、二阶段热压或三阶段热压；热压参数均为温度80-300℃，压力2-30MPa，时间1s-10min；
制备所得聚酰亚胺导电纸厚度为0.02-0.8mm，导电粒子占整个聚酰亚胺导电纸重量的2%-50%。
2.如权利要求1所述聚酰亚胺导电纸的制备方法，其特征是：步骤（3）所述纳米级的碳材料为炭黑、碳纳米管或碳纳米纤维中的一种。
3.如权利要求1所述聚酰亚胺导电纸的制备方法，其特征是：步骤（3）所述纳米级的金属粉为银粉、镍粉、银包铜粉或镍包铜粉中的一种或多种。
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