CN111978724A - 一种阻燃性聚醚酰亚胺树脂及其制备方法 - Google Patents
一种阻燃性聚醚酰亚胺树脂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种阻燃性聚醚酰亚胺树脂及其制备方法,涉及聚醚酰亚胺树脂技术领域。包括按照重量份数比的以下组分:聚醚酰亚胺树脂:65~75份,卤素阻燃剂:12~14份,十溴二苯乙烷:4~6份,促进剂:2‑4份,三氧化钼:3~9份,硼:4~6份,锌:3~5份,可膨胀石墨:4~6份,耐热剂:4~7份;双氰胺:1~3份;填料:12~15份。本发明制备的阻燃性聚醚酰亚胺树脂具有优良的阻燃效果。
Description
技术领域
本发明涉及聚醚酰亚胺树脂技术领域,特别是涉及一种阻燃性聚醚酰亚胺树脂及其制备方法。
背景技术
聚醚酰亚胺树脂是一种无定形热塑性树脂,它具有杰出的耐高温、高强度、高模量及广泛的耐化学性剂性。性能与可加工性的良好平衡,为设计工程师进行创新提供了异乎寻常的灵活性和自由度。
在电讯应用领域,对光纤和电缆等产品的需求不断增长,聚醚酰亚胺树脂具有适合薄壁设计的耐高温和高流动性的特点,能够替代汽车部件中的铝和热固性塑料,但是现有技术中的聚醚酰亚胺树脂的阻燃性能不够优良,不具备较好的阻燃效果,一旦有明火,光纤和电缆会损毁比较严重,造成较大的经济损失。
发明内容
本发明所要解决的技术问题是如何提高聚醚酰亚胺树脂的阻燃性能。
为了解决以上技术问题,本发明提供一种阻燃性聚醚酰亚胺树脂,包括按照重量份数比的以下组分:聚醚酰亚胺树脂:65~75份,卤素阻燃剂:12~14份,十溴二苯乙烷:4~6份,促进剂:2-4份,三氧化钼:3~9份,硼:4~6份,锌:3~5份,可膨胀石墨:4~6份,耐热剂:4~7份;双氰胺:1~3份;填料:12~15份。
本发明进一步限定的技术方案是:包括按照重量份数比的以下组分:聚醚酰亚胺树脂:69份,卤素阻燃剂:13份,十溴二苯乙烷:5份,促进剂:3份,三氧化钼:6份,硼:5份,锌:4份,可膨胀石墨:5份,耐热剂:5.5份;双氰胺:2份;填料:13.5份。
进一步的,所述耐热剂为莫来石粉。
前所述的方法,所述填料包括玻璃纤维和复合陶瓷化粉,且所述玻璃纤维和复合陶瓷化粉的含量比为2:5。
前所述的方法,所述防老剂为防老剂RD和防老剂4020,且所述防老剂RD与防老剂4020的重量比为1:3。
前所述的方法,所述三氧化钼的粒径为13-17纳米。
一种阻燃性聚醚酰亚胺树脂的制备方法,包括以下步骤:
T1、按上述比例配比称取三氧化钼、可膨胀石墨、填料、耐热剂置于球磨罐中,将盛有混料的球磨罐置于球磨机上,进行球磨混料,球磨混料转速790-810r/min,时间15-20min,得到混合料A;
T2、按照上述比例称取硼、锌和促进剂放入反应釜中,低温搅拌15-18min,充分混合后,迅速升温至720-750℃,搅拌30-35min,得到混合料B;
T3、将步骤a中研磨好的混合料A、步骤b中的混合料B加入到熔炼机中,升温至230-250℃,反应10min,然后加入聚醚酰亚胺树脂、卤素阻燃剂、十溴二苯乙烷、促进剂、磷酸盐、丙烯酸丁酯和双氰胺加入到熔炼机中,首先搅拌2min,然后逐渐升温至1200-1500℃,熔炼1-1.5小时,得到混炼胶;
T4、将混炼胶加入稀释剂搅拌均匀,得到成品,过滤分装。
本发明的有益效果是:
(1)本发明以聚醚酰亚胺树脂为基础原料,其中添加的卤素阻燃剂在燃烧条件下分解时会产生卤化氢,其可以消除高分子材料燃烧反应产生活性自由基,另外,卤素阻燃剂在燃烧后会产生残留物,此残留物可以促进聚合物材料的脱水炭化,形成难燃的炭化层,可以抑制明火扩张,添加的十溴二苯乙烷为阻燃剂的一种,可以协助碳化层提高阻燃性能,此外,其溴含量高,热稳定性好,抗紫外线性能佳,不易自燃,较其他溴系阻燃剂的渗出性低,本发明可以提高材料的阻燃性能,防止材料大面积燃烧,减少损失;
(2)本发明中添加的可膨胀石墨受热一定时间后开始膨胀,形成一个很厚的多孔炭层,其在膨胀的过程中吸热,可以降低周围的温度,进一步的提高材料的耐火性能,且形成的多孔炭层可以阻挡热量传播,并配合碳化层,进一步的提高抑火性能,此外,添加的双氰胺在受热时开始分解放出气体,并开始大量吸热,减缓火势的增长,其挥发时分解出的气体可以协助可膨胀石墨迅速膨胀,从而迅速形成稳定的防火层;
(3)本发明中添加的三氧化钼时一种抑烟剂,可以使生烟量降低30~80%,氧指数提高10~20%。
具体实施方式
实施例1:一种阻燃性聚醚酰亚胺树脂,包括按照重量份数比的以下组分:聚醚酰亚胺树脂:65份,卤素阻燃剂:12份,十溴二苯乙烷:4份,促进剂:2份,三氧化钼:3份,硼:4份,锌:3份,可膨胀石墨:4份,耐热剂:4份;双氰胺:1份;填料:12份。
其中,耐热剂为莫来石粉,填料包括玻璃纤维和复合陶瓷化粉,且所述玻璃纤维和复合陶瓷化粉的含量比为2:5,防老剂为防老剂RD和防老剂4020,且所述防老剂RD与防老剂4020的重量比为1:3。
本实施例中,三氧化钼的粒径为13-17纳米,优选为15纳米。
一种阻燃性聚醚酰亚胺树脂的制备方法,包括以下步骤:
T1、按上述比例配比称取三氧化钼、可膨胀石墨、填料、耐热剂置于球磨罐中,将盛有混料的球磨罐置于球磨机上,进行球磨混料,球磨混料转速790-810r/min,时间15-20min,得到混合料A;
T2、按照上述比例称取硼、锌和促进剂放入反应釜中,低温搅拌15-18min,充分混合后,迅速升温至720-750℃,搅拌30-35min,得到混合料B;
T3、将步骤a中研磨好的混合料A、步骤b中的混合料B加入到熔炼机中,升温至230-250℃,反应10min,然后加入聚醚酰亚胺树脂、卤素阻燃剂、十溴二苯乙烷、促进剂、磷酸盐、丙烯酸丁酯和双氰胺加入到熔炼机中,首先搅拌2min,然后逐渐升温至1200-1500℃,熔炼1-1.5小时,得到混炼胶;
T4、将混炼胶加入稀释剂搅拌均匀,得到成品,过滤分装。
实施例2:一种阻燃性聚醚酰亚胺树脂,与实施例1不同之处在于,包括按照重量份数比的以下组分:聚醚酰亚胺树脂:69份,卤素阻燃剂:13份,十溴二苯乙烷:5份,促进剂:3份,三氧化钼:6份,硼:5份,锌:4份,可膨胀石墨:5份,耐热剂:5.5份;双氰胺:2份;填料:13.5份。
实施例3:一种阻燃性聚醚酰亚胺树脂,与实施例1不同之处在于,包括按照重量份数比的以下组分:聚醚酰亚胺树脂:75份,卤素阻燃剂:14份,十溴二苯乙烷: 6份,促进剂:4份,三氧化钼: 9份,硼: 6份,锌:3~5份,可膨胀石墨: 6份,耐热剂:7份;双氰胺:3份;填料15份。
利用本发明实施例1-实施例3制备的阻燃性聚醚酰亚胺树脂制成的成品和普通聚醚酰亚胺树脂制成的成品进行对比试验,观察处理效果,试验结果测得,在相同的燃烧条件下,即时间相同,火力相同,在火力相同的情况下,燃烧15min时,本发明的成品表面轻微焦黑,无烟雾产生,普通抑烟阻燃材料大面积焦黑,且伴随少量烟雾产生;燃烧35min时,本发明的阻燃绝缘材料表面少面积焦黑,少量烟雾产生,普通阻燃绝缘材料严重焦黑,且伴随大量烟雾产生,且表面迅速燃烧,并向周围成品蔓延,有刺鼻气味产生;经过以上试验可知,本发明的阻燃性聚醚酰亚胺树脂在阻燃性能方面有着显著的提高。
除上述实施例外,本发明还可以有其他实施方式。凡采用等同替换或等效变换形成的技术方案,均落在本发明要求的保护范围。
Claims (7)
1.一种阻燃性聚醚酰亚胺树脂,其特征在于:包括按照重量份数比的以下组分:聚醚酰亚胺树脂:65~75份,卤素阻燃剂:12~14份,十溴二苯乙烷:4~6份,促进剂:2-4份,三氧化钼:3~9份,硼:4~6份,锌:3~5份,可膨胀石墨:4~6份,耐热剂:4~7份;双氰胺:1~3份;填料:12~15份。
2.根据权利要求1所述的一种阻燃性聚醚酰亚胺树脂,其特征在于:包括按照重量份数比的以下组分:聚醚酰亚胺树脂:69份,卤素阻燃剂:13份,十溴二苯乙烷:5份,促进剂:3份,三氧化钼:6份,硼:5份,锌:4份,可膨胀石墨:5份,耐热剂:5.5份;双氰胺:2份;填料:13.5份。
3.根据权利要求1所述的一种阻燃性聚醚酰亚胺树脂,其特征在于:所述耐热剂为莫来石粉。
4.根据权利要求1所述的一种阻燃性聚醚酰亚胺树脂,其特征在于:所述填料包括玻璃纤维和复合陶瓷化粉,且所述玻璃纤维和复合陶瓷化粉的含量比为2:5。
5.根据权利要求1所述的一种阻燃性聚醚酰亚胺树脂,其特征在于:所述防老剂为防老剂RD和防老剂4020,且所述防老剂RD与防老剂4020的重量比为1:3。
6.根据权利要求1所述的一种阻燃性聚醚酰亚胺树脂,其特征在于:所述三氧化钼的粒径为13-17纳米。
7.如权利要求1-6任意一项权利要求所述的一种阻燃性聚醚酰亚胺树脂的制备方法,其特征在于,包括以下步骤:
T1、按上述比例配比称取三氧化钼、可膨胀石墨、填料、耐热剂置于球磨罐中,将盛有混料的球磨罐置于球磨机上,进行球磨混料,球磨混料转速790-810r/min,时间15-20min,得到混合料A;
T2、按照上述比例称取硼、锌和促进剂放入反应釜中,低温搅拌15-18min,充分混合后,迅速升温至720-750℃,搅拌30-35min,得到混合料B;
T3、将步骤a中研磨好的混合料A、步骤b中的混合料B加入到熔炼机中,升温至230-250℃,反应10min,然后加入聚醚酰亚胺树脂、卤素阻燃剂、十溴二苯乙烷、促进剂、磷酸盐、丙烯酸丁酯和双氰胺加入到熔炼机中,首先搅拌2min,然后逐渐升温至1200-1500℃,熔炼1-1.5小时,得到混炼胶;
T4、将混炼胶加入稀释剂搅拌均匀,得到成品,过滤分装。
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