CN108559439A - 一种用于导电聚氨酯热熔胶及制备方法 - Google Patents
一种用于导电聚氨酯热熔胶及制备方法 Download PDFInfo
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Abstract
本发明涉及一种用于导电聚氨酯热熔胶及制备方法,按质量份数计,其原料包括:聚酯多元醇,10-65份;聚醚多元醇,20-55份;石墨烯,0.1‑20份;异氰酸酯,5-30份;催化剂,0.0001-0.001份。本发明用于导电聚氨酯热熔胶是由含有活性基团(羟基)的多元醇与异氰酸酯基团(NCO)共聚制备,聚合物链末端含有活性基团NCO,而NCO会与空气中或者被粘物中的水分发生不可逆的交联反应,从而最终获得高的粘接强度。
Description
技术领域
本发明涉及一种用于导电聚氨酯热熔胶及制备方法,属于反应型聚氨酯热熔胶,属于聚氨酯热熔胶制备技术领域。
背景技术
PUR(Polyurethane Reactive),中文全称为湿气固化反应型聚氨酯热熔胶。主要成分是端异氰酸酯聚氨酯预聚体,PUR的粘接性和韧性(弹性)可调节,并有着优异的粘接强度,耐温性,耐化学腐蚀性和耐老化性。近年来已成为胶粘剂产业的重要品种之一。现广泛应用于包装,木材加工,汽车,纺织,机电,航空航天等国民经济领域。
石墨烯是碳原子之间sp2杂化成键,排列成二维蜂窝状晶格的单原子层平面晶体,具有大比表面积,优异的电学、热学和力学性能。目前,石墨烯最吸引研究者的特性是其优异的力学性能,石墨烯是人类已知强度最高的物质,比钻石还坚硬,强度比世界上最好的钢铁还要高上100倍。使用石墨烯与基体聚合物复合制备复合材料或纤维,能够明显改善材料的性能,如提高物理机械性质,改善电学、耐热性能等。目前制备石墨烯/聚合物复合材料的方法 主要有:溶液共混法、机械共混法和原位聚合法。 关于石墨烯混杂聚合物复合材料的制备技术已有报道,例如:中国专利 CN200910067708.8陈永胜等,《石墨烯与碳纤维复合材料及其制备方法》,其主要特征包括: 它是以石墨烯和碳纤维材料为原料,通过涂覆的方法在碳纤维材料表面涂覆石墨烯涂层制备 而成。中国专利,CN101474897陈永胜等,《石墨烯-有机材料层状组装膜及其制备方法》,其特征包括:以石墨烯材料和有机材料为原料,通过旋涂、喷涂、浸渍-提拉等薄膜制备方法层 层叠加成膜。前人在利用石墨烯导电的性能方面做了很多努力,但是利用石墨烯与聚氨酯热熔胶的制备导电胶方法及工艺却未见报道。
发明内容
本发明提供了一种用于导电聚氨酯热熔胶及制备方法。
本发明提供的技术方案为:一种用于导电聚氨酯热熔胶,其特征在于:按质量份数计,其原料包括:聚酯多元醇,10-65份;聚醚多元醇,20-55份;石墨烯,0.1-20份;异氰酸酯,5-30份;催化剂,0.0001-0.001份。本发明用于导电聚氨酯热熔胶是由含有活性基团(羟基)的多元醇与异氰酸酯基团(NCO)共聚制备,聚合物链末端含有活性基团NCO,而NCO会与空气中或者被粘物中的水分发生不可逆的交联反应,从而最终获得高的粘接强度。
本发明所述石墨烯为单层石墨烯粉末、单层氧化石墨烯、氮掺杂石墨烯、羧基化石墨烯、氨基化石墨烯、负载金属石墨烯、还原石墨烯、巯基化石墨烯、纳米石墨粉、磁性石墨烯、咪唑修饰石墨烯中的一种或几种。这些石墨烯是目前主流产品,目的是涵盖石墨烯产品种类广。
本发明所述催化剂为二月桂酸二丁基锡、辛酸亚锡、辛酸铅、三乙胺、三亚乙基二胺、辛酸钴、辛酸铁、环烷酸辛、钛酸四异丁酯、二吗啉基二乙基醚中的一种或几种。这些主要的催化剂涵盖广。
一种用于导电聚氨酯热熔胶的制备方法,其特征在于:包括如下步骤:按质量份数计,将10-65份的聚酯多元醇、20-55份的聚醚多元醇和0.1-20份的石墨烯加热搅拌超声分散0.5-10h,并伴随抽真空,直至被加入的石墨烯分散均匀,然后加入10-20份的异氰酸酯,搅拌反应1-5h,并抽真空,当NCO达到理论值时,加入0.0001-0.001份的催化剂,抽真空搅拌30 min,在通入氮气保护条件下倒出产物,密封包装,得到用于导电聚氨酯热熔胶。
本发明分散石墨烯时加热温度为50-200℃,搅拌速率10-500转/分钟,超声频率为10-100KHz。
本发明分散石墨烯时加热温度为100-150℃,搅拌速率50-200转/分钟,超声频率为20-50KHz。
相比现有技术,本发明具有如下优点:优异的导电性,接触电阻率小于1Ω;
初期粘接强度:大于5N/25mm;优异的最终剥离强度:大于500N/25mm;长的开放时间:大于3min;优异的耐高温性:160℃下无软化流淌;优异的耐低温性:-40℃下无开裂;较低的施胶温度:90℃粘度小于5000cps,施胶温度低,可以对温度敏感的基材很好的保护;方法工艺简便易行,设备简单,易于规模化生产。
具体实施方式
下面结合实施例对本发明做进一步的详细说明,以下实施例是对本发明的解释而本发明并不局限于以下实施例。
实施例1。
本实施例提供了一种用于导电聚氨酯热熔胶的制备方法,其具体步骤如下:按质量份数计,将30份的己二酸-1,4-丁二醇(PBA)、50份的聚丙二醇和1份的单层石墨烯粉末置于反应釜中,加热至120℃,搅拌速率50转/分钟,超声频率为30KHz,分散3h,同时伴随真空脱水,直至单层石墨烯粉末分散均匀。然后加入异氰酸酯20份,搅拌下反应3h,并抽真空,当NCO达到理论值时,加入0.0001份的辛酸亚锡作为催化剂,抽真空搅拌30 min,在通入氮气保护条件下倒出产物,密封包装,得到用于导电聚氨酯热熔胶。
该用于导电聚氨酯热熔胶的初期粘接强度5N/25mm(基材为铜板),最终剥离强度为500N/25mm(基材为铜板)。开放时间为3min。耐高温:160℃下,无软化流淌。耐低温:-40℃下无开裂。粘度:在90℃下,5000/cps。接触电阻率为0.8Ω。
实施例2。
本实施例提供了一种用于导电聚氨酯热熔胶的制备方法,其具体步骤如下:按质量份数计,将45份的己二酸-1,4-丁二醇(PBA)、45份的聚丙二醇和0.3份的羧基化石墨烯置于反应釜中,加热至120℃,搅拌速率150转/分钟,超声频率为50KHz,分散3h,同时伴随真空脱水,直至羧基化石墨烯分散均匀。然后加入异氰酸酯19.7份,搅拌下反应3h,并抽真空,当NCO达到理论值时,加入0.001份的辛酸亚锡作为催化剂,抽真空搅拌30 min,在通入氮气保护条件下倒出产物,密封包装,得到用于导电聚氨酯热熔胶。
该用于导电聚氨酯热熔胶的初期粘接强度6N/25mm(基材为铜板),最终剥离强度为560N/25mm(基材为铜板)。开放时间为4min。耐高温:160℃下,无软化流淌。耐低温:-40℃下无开裂。粘度:在90℃下,6500/cps。接触电阻率为1Ω。
实施例3。
本实施例提供了一种用于导电聚氨酯热熔胶的制备方法,其具体步骤如下:按质量份数计,将30份的邻苯二甲酸-1,4-丁二醇酯、50份的聚丙二醇、0.5份的单层石墨烯粉末和0.5份的氮掺杂石墨烯置于反应釜中,加热至120℃,搅拌速率120转/分钟,超声频率为50KHz,分散4h,同时伴随真空脱水,直至单层石墨烯粉末和氮掺杂石墨烯分散均匀。然后加入异氰酸酯19份,搅拌下反应3h,并抽真空,当NCO达到理论值时,加入0.01份的二吗啉基二乙基醚作为催化剂,抽真空搅拌30 min,在通入氮气保护条件下倒出产物,密封包装,得到用于导电聚氨酯热熔胶。
该用于导电聚氨酯热熔胶的初期粘接强度3N/25mm(基材为铜板),最终剥离强度为600N/25mm(基材为铜板)。开放时间为4min。耐高温:160℃下,无软化流淌。耐低温:-40℃下无开裂。粘度:在90℃下,4500/cps。接触电阻率为0.3Ω。
实施例4。
本实施例提供了一种用于导电聚氨酯热熔胶的制备方法,其具体步骤如下:按质量份数计,将50份的己二酸-1,4-丁二醇(PBA)、30份的聚丙二醇、0.5份的负载金属石墨烯、0.5份的氮掺杂石墨烯和0.5份的咪唑修饰石墨烯置于反应釜中,加热至130℃,搅拌速率100转/分钟,超声频率为70KHz,分散3h,同时伴随真空脱水,直至负载金属石墨烯、氮掺杂石墨烯和咪唑修饰石墨烯分散均匀。然后加入异氰酸酯18.5份,搅拌下反应3h,并抽真空,当NCO达到理论值时,加入0.01份的二月桂酸二丁基锡作为催化剂,抽真空搅拌30 min,在通入氮气保护条件下倒出产物,密封包装,得到用于导电聚氨酯热熔胶。
该用于导电聚氨酯热熔胶的初期粘接强度6N/25mm(基材为铜板),最终剥离强度为650N/25mm(基材为铜板)。开放时间为4min。耐高温:160℃下,无软化流淌。耐低温:-40℃下无开裂。粘度:在90℃下,5000/cps。接触电阻率为0.2Ω。
实施例5。
本实施例提供了一种用于导电聚氨酯热熔胶的制备方法,其具体步骤如下:按质量份数计,将30份的邻苯二甲酸-1,4-丁二醇酯、50份的聚丙二醇、1份的负载金属石墨烯、0.5份的氮掺杂石墨烯和0.5份的咪唑修饰石墨烯置于反应釜中,加热至120℃,搅拌速率50转/分钟,超声频率为30KHz,分散3h,同时伴随真空脱水,直至负载金属石墨烯、氮掺杂石墨烯和咪唑修饰石墨烯分散均匀。然后加入异氰酸酯18份,搅拌下反应3h,并抽真空,当NCO达到理论值时,加入0.0001份的辛酸亚锡作为催化剂,抽真空搅拌30 min,在通入氮气保护条件下倒出产物,密封包装,得到用于导电聚氨酯热熔胶。
该用于导电聚氨酯热熔胶的初期粘接强度4.5N/25mm(基材为铜板),最终剥离强度为750N/25mm(基材为铜板)。开放时间为5min。耐高温:160℃下,无软化流淌。耐低温:-40℃下无开裂。粘度:在90℃下,7500/cps。接触电阻率为0.2Ω。
实施例6。
本实施例提供了一种用于导电聚氨酯热熔胶的制备方法,其具体步骤如下:按质量份数计,将50份的邻苯二甲酸-1,4-丁二醇酯、40份的聚丙二醇、1份的负载金属石墨烯、0.6份的巯基化石墨烯和0.4份的咪唑修饰石墨烯置于反应釜中,加热至120℃,搅拌速率150转/分钟,超声频率为90KHz,分散5h,同时伴随真空脱水,直至负载金属石墨烯、巯基化石墨烯和咪唑修饰石墨烯分散均匀。然后加入异氰酸酯8份,搅拌下反应3h,并抽真空,当NCO达到理论值时,加入0.01份的三亚乙基二胺作为催化剂,抽真空搅拌30 min,在通入氮气保护条件下倒出产物,密封包装,得到用于导电聚氨酯热熔胶。
该用于导电聚氨酯热熔胶的初期粘接强度7N/25mm(基材为铜板),最终剥离强度为350N/25mm(基材为铜板)。开放时间为3min。耐高温:160℃下,无软化流淌。耐低温:-40℃下无开裂。粘度:在90℃下,7500/cps。接触电阻率为0.05Ω。
实施例1-6利用聚酯二元醇、聚醚二元醇、异氰酸酯、石墨烯等为反应原料,得到导电聚氨酯热熔胶。用于导电聚氨酯热熔胶具有高的高粘接强度,优异的导电性,施胶温度低,开放时间长,优异的耐高低温等性能。
对比实施例1。
本实施例提供了一种用于导电聚氨酯热熔胶的制备方法,其具体步骤如下:按质量份数计,将31份的己二酸-1,4-丁二醇(PBA)和50份的聚丙二醇置于反应釜中,加热至120℃,搅拌速率50转/分钟,超声频率为30KHz,分散3h,同时伴随真空脱水。然后加入异氰酸酯20份,搅拌下反应3h,并抽真空,当NCO达到理论值时,加入0.0001份的辛酸亚锡作为催化剂,抽真空搅拌30 min,在通入氮气保护条件下倒出产物,密封包装,得到用于导电聚氨酯热熔胶。
该用于导电聚氨酯热熔胶的初期粘接强度5N/25mm(基材为铜板),最终剥离强度为500N/25mm(基材为铜板)。开放时间为3min。耐高温:160℃下,无软化流淌。耐低温:-40℃下无开裂。粘度:在90℃下,5000/cps。接触电阻率为20Ω。
对比实施例2。
本实施例提供了一种用于导电聚氨酯热熔胶的制备方法,其具体步骤如下:按质量份数计,将45份的己二酸-1,4-丁二醇(PBA)和45份的聚丙二醇置于反应釜中,加热至120℃,搅拌速率150转/分钟,超声频率为50KHz,分散3h,同时伴随真空脱水。然后加入异氰酸酯20份,搅拌下反应2h,并抽真空,当NCO达到理论值时,加入0.001份的辛酸亚锡作为催化剂,抽真空搅拌30 min,在通入氮气保护条件下倒出产物,密封包装,得到用于导电聚氨酯热熔胶。
该用于导电聚氨酯热熔胶的初期粘接强度6N/25mm(基材为铜板),最终剥离强度为560N/25mm(基材为铜板)。开放时间为4min。耐高温:160℃下,无软化流淌。耐低温:-40℃下无开裂。粘度:在90℃下,6500/cps。接触电阻率为18Ω。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员,在不脱离本发明构思的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围内。虽然本发明已以实施例公开如上,但其并非用以限定本发明的保护范围,任何熟悉该项技术的技术人员,在不脱离本发明的构思和范围内所作的变动与润饰,均应属于本发明的保护范围。
Claims (6)
1.一种用于导电聚氨酯热熔胶,其特征在于:按质量份数计,其原料包括:聚酯多元醇,10-65份;聚醚多元醇,20-55份;石墨烯,0.1-20份;异氰酸酯,5-30份;催化剂,0.0001-0.001份。
2.根据权利要求1所述的用于导电聚氨酯热熔胶,其特征在于:所述石墨烯为单层石墨烯粉末、单层氧化石墨烯、氮掺杂石墨烯、羧基化石墨烯、氨基化石墨烯、负载金属石墨烯、还原石墨烯、巯基化石墨烯、纳米石墨粉、磁性石墨烯、咪唑修饰石墨烯中的一种或几种。
3.根据权利要求1所述的用于导电聚氨酯热熔胶,其特征在于:所述催化剂为二月桂酸二丁基锡、辛酸亚锡、辛酸铅、三乙胺、三亚乙基二胺、辛酸钴、辛酸铁、环烷酸辛、钛酸四异丁酯、二吗啉基二乙基醚中的一种或几种。
4.一种如权利要求1或2或3所述的用于导电聚氨酯热熔胶的制备方法,其特征在于:包括如下步骤:按质量份数计,将10-65份的聚酯多元醇、20-55份的聚醚多元醇和0.1-20份的石墨烯加热搅拌超声分散0.5-10h,并伴随抽真空,直至被加入的石墨烯分散均匀,然后加入10-20份的异氰酸酯,搅拌反应1-5h,并抽真空,当NCO达到理论值时,加入0.0001-0.001份的催化剂,抽真空搅拌30 min,在通入氮气保护条件下倒出产物,密封包装,得到用于导电聚氨酯热熔胶。
5.根据权利要求4所述的用于导电聚氨酯热熔胶的制备方法,其特征在于:分散石墨烯时加热温度为50-200℃,搅拌速率10-500转/分钟,超声频率为10-100KHz。
6.根据权利要求5所述的用于导电聚氨酯热熔胶的制备方法,其特征在于:分散石墨烯时加热温度为100-150℃,搅拌速率50-200转/分钟,超声频率为20-50KHz。
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