CN110437721A - 一种石墨烯基弹性阻燃电热膜及其制备方法 - Google Patents
一种石墨烯基弹性阻燃电热膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种石墨烯基弹性阻燃电热膜,包括以下重量份材料:100份水性阻燃涂覆树脂、150‑200份石墨烯和碳纳米管复合分散液、1‑10份分散剂以及200份溶剂;所述水性阻燃涂覆树脂包括以下重量份材料:100份的水性丙烯酸树脂和水性聚氨酯分散体及水性聚氨酯乳液组合物、1‑10份的硅烷偶联剂和1‑25份的阻燃剂。本发明的目的是公开一种石墨烯基弹性阻燃电热膜及其制备方法,通过开发一种水性阻燃涂覆树脂,同时开发一种高导电的石墨烯和碳纳米管的复合水性分散液,然后配合助剂将树脂和分散液进行混合,制成涂料,通过印刷或涂布工艺印制在阻燃基材上制备电热膜,达到阻燃的目的;在燃烧初期,无卤阻燃剂形成的覆盖层与石墨烯的片状屏蔽协同作用,提升了阻燃性能。
Description
技术领域
本发明涉及阻燃材料技术领域,具体涉及一种石墨烯基弹性阻燃电热膜及其制备方法。
背景技术
随着人类生活水平的提高,采暖***已成为冬季必不可少的设备,然而北方传统燃料锅炉集中供暖存在众多弊端,如污染环境、不利于节能、占用空间等。电热膜辐射供暖可以很好的解决上述问题,且具有热舒适高和能产生对人体有益的红外线等特点,因而得到了迅速发展,具有广阔的发展前景。而电热膜产品的安全性能提升一直是企业和用户关注的重点。
目前,国内的电热膜产品绝大多数是由导电油墨印刷在聚酯薄膜上制成的,而对于过热或者燃烧的防护处理一般为铺设工程中,布设少量的温度传感器点,起不到较好的预防和阻燃效果。
发明内容
本发明的目的在于提供一种石墨烯基弹性阻燃电热膜及其制备方法,通过开发一种水性阻燃涂覆树脂,同时开发一种高导电的石墨烯/碳纳米管的复合水性分散液,然后配合助剂将树脂和分散液进行混合,制成涂料,通过印刷/涂布工艺印制在阻燃基材上制备电热膜,达到阻燃的目的。
为实现上述目的,本发明提供的技术方案如下:
一种石墨烯基弹性阻燃电热膜,包括以下重量份材料:100份水性阻燃涂覆树脂、150-200份石墨烯和碳纳米管复合分散液、1-10份分散剂以及200份溶剂;
所述水性阻燃涂覆树脂包括以下重量份材料:100份的水性丙烯酸树脂和水性聚氨酯分散体及水性聚氨酯乳液组合物、1-10份的硅烷偶联剂和1-25份的阻燃剂。
进一步地,所述水性丙烯酸、水性聚氨酯分散体和水性聚氨酯乳液的重量份比值为5-30:20-30:25-60。
进一步地,所述阻燃剂包括磷系阻燃剂和/或氮磷复合阻燃剂。
进一步地,所述阻燃剂为DMMP。
进一步地,所述碳纳米管:石墨烯重量份比值为5-8:1。
进一步地,所述石墨烯由膨胀剥离法或氧化还原法制备得到。
进一步地,所述石墨烯和碳纳米管复合分散液中的分散介质包括去离子水、NMP和DMF中的一种或几种。
进一步地,所述分散剂包括DEGO760W,曲拉通X-100、十二烷基苯磺酸钠、聚氧乙烯月桂醚、***树胶粉、阴离子聚丙烯酰胺中的至少一种。
进一步地,所述溶剂包括纯水和/或醇类。
这种石墨烯基弹性阻燃电热膜的制备方法,步骤包括:
(1)水性阻燃树脂的制备:将水性丙烯酸、水性聚氨酯分散体和水性聚氨酯乳液加入到搅拌容器中,在搅拌过程中加入硅烷偶联剂并搅拌,随后加入阻燃剂后并搅拌;过滤出料,得到水性阻燃树脂;
(2)水性石墨烯和碳纳米管分散液的制备:将去离子水、分散剂加入到容器中搅拌混合均匀,然后在搅拌下将碳纳米管、石墨烯粉体加入到搅拌容器中,搅拌混合均匀;将混合液超声后转入卧式研磨机研磨,得到水性石墨烯和碳纳米管分散液;
(3)水性石墨烯阻燃导电涂料的制备:将水性阻燃树脂,水性石墨烯和碳纳米管分散液加入到容器中搅拌并混合均匀,过滤出料,得到水性石墨烯阻燃导电涂料;
(4)石墨烯基弹性阻燃电热膜的制备:将水性石墨烯阻燃涂料采用印刷或者涂布的方式均匀分布到基材表面,得到导电层;并在导电层上进行电极压制,或电极印刷,可制得阻燃电热膜。
本发明的优点在于:
通过开发一种水性阻燃涂覆树脂,同时开发一种高导电的石墨烯/碳纳米管的复合水性分散液,然后配合助剂将树脂和分散液进行混合,制成涂料,通过印刷/涂布工艺印制在阻燃基材上制备电热膜,达到阻燃的目的,在燃烧初期,无卤阻燃剂形成的覆盖层与石墨烯的片状屏蔽协同作用,实现阻燃性能的提升。
具体实施方式
下面结合具体实施例对本发明的技术方案作进一步描述,但是本领域技术人员将会理解,下列所述的实施例仅用于说明如何使用本发明,而不应视为限制本发明的范围。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
在这里专用的词“实施例”,作为“示例性”所说明的任何实施例不必解释为优于或好于其它实施例。本法实施例中性能指标测试,除非特别说明,采用本领域常规试验方法,测试条件为通常实验条件。
在本发明中,所述阻燃剂包括但不限于磷系阻燃剂和/或氮磷复合阻燃剂;所述硅烷偶联剂包括但不限于KH550;所述石墨烯和碳纳米管复合分散液中的分散介质包括但不限于去离子水、NMP和DMF中的一种或几种;所述分散剂包括但不限于DEGO760W,曲拉通X-100、十二烷基苯磺酸钠、聚氧乙烯月桂醚、***树胶粉、阴离子聚丙烯酰胺中的至少一种;所述溶剂包括但不限于纯水和/或醇类。
这种石墨烯基弹性阻燃电热膜的制备方法,步骤包括:
(1)水性阻燃树脂的制备:将水性丙烯酸、水性聚氨酯分散体和水性聚氨酯乳液加入到搅拌容器中,在搅拌过程中加入硅烷偶联剂并搅拌,随后加入阻燃剂后并搅拌;过滤出料,得到水性阻燃树脂;
(2)水性石墨烯和碳纳米管分散液的制备:将去离子水、分散剂加入到容器中搅拌混合均匀,然后在搅拌下将碳纳米管、石墨烯粉体加入到搅拌容器中,搅拌混合均匀;将混合液超声后转入卧式研磨机研磨,得到水性石墨烯和碳纳米管分散液;
(3)水性石墨烯阻燃导电涂料的制备:将水性阻燃树脂,水性石墨烯和碳纳米管分散液加入到容器中搅拌并混合均匀,过滤出料,得到水性石墨烯阻燃导电涂料;
(4)石墨烯基弹性阻燃电热膜的制备:将水性石墨烯阻燃涂料采用印刷或者涂布的方式均匀分布到基材表面,得到导电层;并在导电层上进行电极压制,或电极印刷,可制得阻燃电热膜。
以下给出4个具体的实施例并对制备得到的阻燃电热膜进行性能测试:
实施例1
本发明提供一种石墨烯基弹性阻燃电热膜,其制备方法的步骤包括:
将100份的水性丙烯酸树脂和水性聚氨酯分散体及水性聚氨酯乳液组合物加入到搅拌容器中,其中,水性丙烯酸:水性聚氨酯分散体:水性聚氨酯乳液的比例为=15:30:55,在搅拌过程中加入2质量份的KH550,搅拌30min后,加入10份的DMMP阻燃剂,搅拌30min;过滤出料,得到水性阻燃树脂;
将200份的去离子水、2质量份的DEGO760W加入到容器中搅拌10min混合均匀,然后在搅拌下将6份碳纳米管、1份石墨烯粉体加入到搅拌容器中,搅拌30min混合均匀;将混合液超声30min,转入卧式研磨机研磨30min,得到水性石墨烯和碳纳米管分散液;
将100份水性阻燃树脂,150份水性石墨烯和碳纳米管分散液加入到容器中搅拌30min混合均匀,过滤出料,得到水性石墨烯阻燃导电涂料。
将水性石墨烯阻燃导电涂料通过涂布的方式涂覆在PET膜上,湿膜厚50μm,烘干后在表面印刷电极,得到石墨烯基弹性阻燃电热膜。
实施例2
本发明提供一种石墨烯基弹性阻燃电热膜,其制备方法的步骤包括:
将100份的水性丙烯酸树脂和水性聚氨酯分散体及水性聚氨酯乳液组合物加入到搅拌容器中,其中,水性丙烯酸:水性聚氨酯分散体:水性聚氨酯乳液的比例为=15:30:55,在搅拌过程中加入2质量份的KH550,搅拌30min后,加入1份的DMMP阻燃剂,搅拌30min。过滤出料,得到水性阻燃树脂;
将200份的去离子水、2质量份的曲拉通X-100加入到容器中搅拌10min混合均匀,然后在搅拌下将5份碳纳米管、2份石墨烯粉体加入到搅拌容器中,搅拌30min混合均匀。将混合液超声30min,转入卧式研磨机研磨30min,得到水性石墨烯和碳纳米管分散液;
将100份水性阻燃树脂,150份水性石墨烯和碳纳米管分散液加入到容器中搅拌30min混合均匀,过滤出料,得到水性石墨烯阻燃导电涂料。
将水性石墨烯阻燃导电涂料通过涂布的方式涂覆在PET膜上,湿膜厚50μm,烘干后在表面印刷电极,得到石墨烯基弹性阻燃电热膜。
实施例3
本发明提供一种石墨烯基弹性阻燃电热膜,其制备方法的步骤包括:
将100份的水性丙烯酸树脂和水性聚氨酯分散体及水性聚氨酯乳液组合物加入到搅拌容器中,其中,水性丙烯酸:水性聚氨酯分散体:水性聚氨酯乳液的比例为=15:30:55,在搅拌过程中加入2质量份的KH550,搅拌30min后,加入10份的DMMP阻燃剂,搅拌30min;过滤出料,得到水性阻燃树脂;
将200份的去离子水、2质量份的聚氧乙烯月桂醚加入到容器中搅拌10min混合均匀,然后在搅拌下将5份碳纳米管、1份石墨烯粉体加入到搅拌容器中,搅拌30min混合均匀。将混合液超声30min,转入卧式研磨机研磨30min,得到水性石墨烯和碳纳米管分散液;
将100份水性阻燃树脂,150份水性石墨烯和碳纳米管分散液加入到容器中搅拌30min混合均匀,过滤出料,得到水性石墨烯阻燃导电涂料。
将水性石墨烯阻燃导电涂料通过涂布的方式涂覆在PET膜上,湿膜厚50μm,烘干后在表面印刷电极,得到石墨烯基弹性阻燃电热膜。
实施例4
本发明提供一种石墨烯基弹性阻燃电热膜,其制备方法的步骤包括:
将100份的水性丙烯酸树脂和水性聚氨酯分散体及水性聚氨酯乳液组合物加入到搅拌容器中,其中,水性丙烯酸:水性聚氨酯分散体:水性聚氨酯乳液的比例为=65:20:15,在搅拌过程中加入2质量份的KH550,搅拌30min后,加入10份的DMMP阻燃剂,搅拌30min;过滤出料,得到水性阻燃树脂;
将200份的去离子水、2质量份的聚氧乙烯月桂醚加入到容器中搅拌10min混合均匀,然后在搅拌下将5份碳纳米管、1份石墨烯粉体加入到搅拌容器中,搅拌30min混合均匀。将混合液超声30min,转入卧式研磨机研磨30min,得到水性石墨烯和碳纳米管分散液;
将100份水性阻燃树脂,150份水性石墨烯和碳纳米管分散液加入到容器中搅拌30min混合均匀,过滤出料,得到水性石墨烯阻燃导电涂料。
将水性石墨烯阻燃导电涂料通过涂布的方式涂覆在PET膜上,湿膜厚50μm,烘干后在表面印刷电极,得到石墨烯基弹性阻燃电热膜。
将实施例1-4中制备得到的石墨烯基弹性阻燃电热膜进行检测,得到的结果如下表所示:
结果表明,聚氨酯的用量与涂膜弹性正相关,涂膜阻燃性能与复合用阻燃剂的量呈正相关,涂膜电阻与石墨烯和碳纳米管的总用量呈正相关。
最后应说明的是:以上实施例仅用以说明本发明而并非限制本发明所描述的技术方案;本领域的普通技术人员应当理解,仍然可以对本发明进行修改或等同替换;而一切不脱离本发明的精神和范围的技术方案及其改进,其均应涵盖在本发明的权利要求范围中。
Claims (10)
1.一种石墨烯基弹性阻燃电热膜,其特征在于,包括以下重量份材料:100份水性阻燃涂覆树脂、150-200份石墨烯和碳纳米管复合分散液、1-10份分散剂以及200份溶剂;
所述水性阻燃涂覆树脂包括以下重量份材料:100份的水性丙烯酸树脂和水性聚氨酯分散体及水性聚氨酯乳液组合物、1-10份的硅烷偶联剂和1-25份的阻燃剂。
2.根据权利要求1所述的石墨烯基弹性阻燃电热膜,其特征在于,所述水性丙烯酸、水性聚氨酯分散体和水性聚氨酯乳液的重量份比值为5-30:20-30:25-60。
3.根据权利要求1所述的石墨烯基弹性阻燃电热膜,其特征在于,所述阻燃剂包括磷系阻燃剂和/或氮磷复合阻燃剂。
4.根据权利要求1所述的石墨烯基弹性阻燃电热膜,其特征在于,所述阻燃剂为DMMP。
5.根据权利要求1所述的石墨烯基弹性阻燃电热膜,其特征在于,所述碳纳米管:石墨烯重量份比值为5-8:1。
6.根据权利要求5所述的石墨烯基弹性阻燃电热膜,其特征在于,所述石墨烯由膨胀剥离法或氧化还原法制备得到。
7.根据权利要求1所述的石墨烯基弹性阻燃电热膜,其特征在于,所述石墨烯和碳纳米管复合分散液中的分散介质包括去离子水、NMP和DMF中的一种或几种。
8.根据权利要求1所述的石墨烯基弹性阻燃电热膜,其特征在于,所述分散剂包括DEGO760W,曲拉通X-100、十二烷基苯磺酸钠、聚氧乙烯月桂醚、***树胶粉、阴离子聚丙烯酰胺中的至少一种。
9.根据权利要求1所述的石墨烯基弹性阻燃电热膜,其特征在于,所述溶剂包括纯水和/或醇类。
10.如权利要求1-9任一项所述的石墨烯基弹性阻燃电热膜的制备方法,其特征在于,步骤包括:
(1)水性阻燃树脂的制备:将水性丙烯酸、水性聚氨酯分散体和水性聚氨酯乳液加入到搅拌容器中,在搅拌过程中加入硅烷偶联剂并搅拌,随后加入阻燃剂后并搅拌;过滤出料,得到水性阻燃树脂;
(2)水性石墨烯和碳纳米管分散液的制备:将去离子水、分散剂加入到容器中搅拌混合均匀,然后在搅拌下将碳纳米管、石墨烯粉体加入到搅拌容器中,搅拌混合均匀;将混合液超声后转入卧式研磨机研磨,得到水性石墨烯和碳纳米管分散液;
(3)水性石墨烯阻燃导电涂料的制备:将水性阻燃树脂,水性石墨烯和碳纳米管分散液加入到容器中搅拌并混合均匀,过滤出料,得到水性石墨烯阻燃导电涂料;
(4)石墨烯基弹性阻燃电热膜的制备:将水性石墨烯阻燃涂料采用印刷或者涂布的方式均匀分布到基材表面,得到导电层;并在导电层上进行电极压制,或电极印刷,可制得阻燃电热膜。
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