CN103788649B - 一种高强度硬质聚酰亚胺泡沫塑料的制备方法 - Google Patents
一种高强度硬质聚酰亚胺泡沫塑料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种高强度硬质聚酰亚胺泡沫塑料的制备方法,a、在反应釜中加入有机溶剂N,N‑二甲基乙酰胺,并依次加入均苯四甲酸二酐(PMDA),异佛尔酮二胺,丙三醇,充入氮气,控制温度60~200℃,反应1~8h;b、向上述反应釜中加入醋酸酐,减压至绝压下控制温度130~150℃继续反应1~8h,并回收溶剂及低分子反应物,得到PMDA的聚酰亚胺产物;c、向上述产物中加入称量的聚甲基丙烯酸甲酯,聚四氟乙烯,聚醚改性有机硅油SF‑8427,水,升温至180℃,高速搅拌;d、产生泡体时立即注入已预热的铝制模具中发泡,经胀定,脱模,即得聚酰亚胺硬泡塑料制品。
Description
技术领域
本发明属于工程塑料领域,特别涉及一种高强度硬质聚酰亚胺泡沫塑料的制备方法。
背景技术
聚酰亚胺作为一种特种工程材料,已广泛应用在航空、航天、微电子、纳米、液晶、分离膜、激光等领域。近来,各国都在将聚酰亚胺的研究、开发及利用列入 21世纪最有希望的工程塑料之一。聚酰亚胺泡沫塑料综合了聚酰亚胺树脂和泡沫塑料的结构与性能优点。是一种高性能的泡沫塑料。首先,聚酰亚胺泡沫塑料的热稳定性最好,其长期可耐250~300℃。短期可耐400一500℃,弹性聚酰亚胺泡沫塑料可耐极低温,在一269℃的液态氦中仍不会脆裂:其次,聚酰亚胺泡沫塑料具有优异的阻燃性能,为自熄性泡沫塑料,氧指数高达42%:第三,聚酰亚胺泡沫塑料具有很高的耐辐照性能。在5×109 md剂量辐照后,强度仍能保持80%左右;第四,聚酰亚胺泡沫塑料还具有很好的介电性能,介电常数为3.4左右,如引入空气以纳米尺寸分散在聚酰亚胺泡沫中制成的聚酰亚胺纳米泡沫塑料,介电常数可降到2.5左右,介电损耗因数为1×lO。3,介电强度为100—300 kv/mm,体积电阻率高达l
017 Q·cm。
聚酰亚胺泡沫塑料从分子链结构上分主要有3种类型:一是酰亚胺环在主链上的聚酰亚胺泡沫塑料;二是酰亚胺环在侧链上的聚酰亚胺泡沫塑料(如聚甲基丙烯酰亚胺泡沫塑料);三是将热不稳定的脂肪链引入聚酰亚胺分子主链然后在高温下裂解得新型聚酰亚胺纳米泡沫塑料。聚酰亚胺,因其在性能和合成方面的突出特点,不论是作为结构材料或是作为功能性材料,其巨大的应用前景已经得到充分的认识,被称为是"解决问题的能手"(protion solver),并认为"没有聚酰亚胺就不会有今天的微电子技术"。目前,正是由于聚酰亚胺泡沫塑料所具有的上述优异性能,才使得人们对聚酰亚胺泡沫塑料的研究一直没有间断过,美国、英国、德国、日本和中国等已对其进行了大量的研究,但由于价格高限制了其广泛使用,现主要用于环境条件十分苛刻的航空航天等特殊领域。有研究报道,采用3,3’,4,4’一二苯甲酮四酸二(BTDA)在四氢呋喃(THF)/甲醇混合溶液中反应生成BTDA的二元酯后加入MDA反应成盐,然后在70℃下加热去溶剂得到先驱体粉末,最后在220℃下加热发泡成为聚酰亚胺泡沫塑料。
发明内容:
本发明的目的是针对现有技术中的不足,提供一种发泡温度低,操作简便,成本较低,适于工业化生产的高强度聚酰亚胺硬质泡沫塑料的制备方法。
技术方案:为实现上述发明目的,一种高强度聚酰亚胺硬质泡沫塑料的制备方法,包括以下技术步骤:
a、在反应釜中加入有机溶剂N,N-二甲基乙酰胺,并依次加入均苯四甲酸二酐(PMDA),异佛尔酮二胺,丙三醇,充入氮气,控制温度60~200℃,反应1~8h;
b、向上述反应釜中加入醋酸酐,减压至绝压下控制温度130~150℃继续反应1~8h,并回收溶剂及低分子反应物,得到PMDA的聚酰亚胺产物;
c、向上述产物中加入称量的聚甲基丙烯酸甲酯,聚四氟乙烯,聚醚改性有机硅油SF-8427,水,升温至180℃,高速搅拌;
d、产生泡体时立即注入已预热的铝制模具中发泡,经胀定,脱模,即得聚酰亚胺硬泡塑料制品。
所述的聚甲基丙烯酸甲酯与PMDA聚酰亚胺产物的质量比为1:3~8。
所述的聚四氟乙烯与均PMDA的聚酰亚胺产物的质量比为1:20~100。
所述的聚四氟乙烯粒径为20~200目。
所述的绝压为0.05~0.8Kpa。
根据以上的技术方案,可以实现以下的有益效果:与现有技术相比,本发明具有以下优点:1、操作简便,发泡温度低,成本较低,适于工业化生产;2、所制备泡沫塑料耐热性好、强度高、自熄性强、透气性小、安全无毒。
具体实施方式:
下面结合实施例对本发明做进一步地详细说明,但是本发明要求保护的范围并不局限于实施例表示的范围。
实施例1:
在反应釜中加入有机溶剂N,N-二甲基乙酰胺(85.0kg),并依次加入均苯四甲酸二酐PMDA(400.0kg),异佛尔酮二胺(350.0kg),丙三醇(45.0kg),充入氮气,控制温度180℃,反应7h;向反应釜中加入醋酸酐(23.5kg),减压至0.15Kpa,控制温度130~150℃继续反应7h,并回收溶剂及低分子反应物,得到PMDA的聚酰亚胺产物;
称取PMDA的聚酰亚胺产物(700.0kg),聚甲基丙烯酸甲酯(200.0kg),聚四氟乙烯(22.5kg),聚醚改性有机硅油SF-8427(235.0kg),水(5.0kg),升温至180℃,高速搅拌;待产生泡体时立即注入已预热的铝制模具中发泡,经胀定,脱模,即得聚酰亚胺硬泡塑料制品。
实施例2:
在反应釜中加入有机溶剂N,N-二甲基乙酰胺(85.0kg),并依次加入均苯四甲酸二酐PMDA(400.0kg),异佛尔酮二胺(350.0kg),丙三醇(45.0kg),充入氮气,控制温度180℃,反应7h;向反应釜中加入醋酸酐(23.5kg),减压至0.15Kpa,控制温度130~150℃继续反应7h,并回收溶剂及低分子反应物,得到PMDA的聚酰亚胺产物;
称取PMDA的聚酰亚胺产物(700.0kg),聚甲基丙烯酸甲酯(100.0kg),聚四氟乙烯(31.5kg),聚醚改性有机硅油SF-8427(235.0kg),水(5.0kg),升温至180℃,高速搅拌;待产生泡体时立即注入已预热的铝制模具中发泡,经胀定,脱模,即得聚酰亚胺硬泡塑料制品。
Claims (2)
1.一种高强度硬质聚酰亚胺泡沫塑料的制备方法,其特征在于,包括以下技术步骤:
a、在反应釜中加入有机溶剂N,N-二甲基乙酰胺,并依次加入均苯四甲酸二酐(PMDA),异佛尔酮二胺,丙三醇,充入氮气,控制温度60~200℃,反应1~8h;
b、向上述反应釜中加入醋酸酐,减压至绝压下控制温度130~150℃继续反应1~8h,并回收溶剂及低分子反应物,得到PMDA的聚酰亚胺产物;
c、向上述产物中加入称量的聚甲基丙烯酸甲酯,聚四氟乙烯,聚醚改性有机硅油SF-8427,水,升温至180℃,高速搅拌;
d、产生泡体时立即注入已预热的铝制模具中发泡,经胀定,脱模,即得聚酰亚胺硬泡塑料制品;聚甲基丙烯酸甲酯与PMDA聚酰亚胺产物的质量比为1:3~8;聚四氟乙烯与PMDA的聚酰亚胺产物的质量比为1:20~100; 绝压为0.05~0.8Kpa。
2.如权利要求1所述一种高强度硬质聚酰亚胺泡沫塑料的制备方法,其特征在于:聚四氟乙烯粒径为20~200目。
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