CN106589200B - 一种阻燃型聚苯乙烯的制备方法 - Google Patents
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Abstract
本发明提供了一种阻燃型聚苯乙烯的制备方法，加入苯乙烯，磷酸三烯丙酯、异戊烯基聚氧乙烯醚，N‑羟基‑5‑降冰片烯‑2,3‑二甲酰亚胺，1,8‑二氮杂双环[5.4.0]十一碳‑7‑烯等进行悬浮聚合得到阻燃型聚苯乙烯产品。
Description
技术领域
本发明涉及一种聚苯乙烯的制备方法，尤其是一种阻燃型聚苯乙烯的制备方法。
背景技术
传统EPS膨胀聚苯板属易燃材料，加入有机阻燃剂虽可提高其阻燃性，但随着有机阻燃剂的挥发，EPS膨胀聚苯板阻燃性能也随着下降，经检测其阻燃性能只能达到B1级；此外，传统EPS膨胀聚苯板属于热塑性材料，遇火攻击后收缩、熔化、流淌，火灾过程中伴随着浓烈的烟雾，不仅严重污染环境，而且火灾蔓延速度快，过火面积大，难以扑救，往往造成重大的人员伤亡，2011年3月15日，由公安部消防局发布了《关于进一步明确民用建筑外保材料消防监督管理有关要求的通知》的65号文件，无论是住宅、公建、既有建筑改造所用保温材料的燃烧性能必须达到A级。自65号文件发布以来， 中国保温市场上大量的无机材料纷纷上墙，虽然解决了防火的问题，但是引发了更大的问题： 建筑节能不达标。
CN102775690A提供了公开了公开了一种阻燃型聚苯乙烯保温材料，其特征在于：主要成分及重量百分比为：聚苯乙烯EPS发泡颗粒80％-90％、高效阻燃剂10％-20％，所述高效阻燃剂的成分及重量百分比为：氢氧化镁阻燃剂3-5％、超细石墨1％-6％、高岭土1％-3％、颜料1-3％、水3％。
CN104164006A公开了一种可阻燃型聚苯乙烯保温泡沫材料，其特征在于，包括下列重量份数的物质：聚苯乙烯80-99份，可膨胀石墨35-41份，钛白粉10-15份，玻璃微珠13-25份，云母粉3-11份，聚对苯二甲酸丁二醇酯5-9份，环氧糠油酸丁酯13-34份，N-乙基对甲苯磺酰胺10-15份，枸橼酸5-9份，红磷15-30份，氢氧化铝12-19份，可再分散乳胶粉10-17份，晶石1-8份，碳酸钙3-5份。
CN103435927B公开了一种A级阻燃改性聚苯板及其制备方法，所述聚苯板，按重量计，包括阻燃型聚苯乙烯树脂20～25份、发泡剂0.4～0.5份、滑石粉40～50份、氢氧化铝6～10份、表面活性剂2～4份、固化剂3～5份。还公开了相应的制备方法。
现有技术中的阻燃改性聚苯板在聚苯乙烯中掺杂各种阻燃剂，分散效果差，造成树脂和阻燃剂之间相容性差，影响到制品的阻燃稳定性。
发明内容
本发明目的在于解决现有技术中存在的上述技术问题，提供一种阻燃型聚苯乙烯的制备方法。
为了解决上述技术问题，本发明采用如下技术方案：一种阻燃型聚苯乙烯的制备方法，其特征在于制备步骤包括：
在反应釜中，按重量份计加入100份苯乙烯，10-30份磷酸三烯丙酯、0.1-1份异戊烯基聚氧乙烯醚，0.01-0.1份N-羟基-5-降冰片烯-2,3-二甲酰亚胺，0.01-0.1份1,8-二氮杂双环[5.4.0]十一碳-7-烯，1000-2000份水，1-5份分散剂，1-4份自由基聚合引发剂，在70℃-110℃反应4-15h，过滤，烘干后得到产品。
所述的磷酸三烯丙酯，异戊烯基聚氧乙烯醚，N-羟基-5-降冰片烯-2,3-二甲酰亚胺，1,8-二氮杂双环[5.4.0]十一碳-7-烯均为市售产品。
所述的引发剂为自由基聚合引发剂，包括：偶氮化合物以及氧化还原体系引发剂。优选过氧化苯甲酰，偶氮二异庚腈。
所述的分散剂包括明胶，聚乙烯醇，羟甲基纤维素。
本发明由于采用了上述技术方案，具有以下有益效果：
通过悬浮聚合方式，苯乙烯和磷酸三烯丙酯生成交联聚合物，同时异戊烯基聚氧乙烯醚，N-羟基-5-降冰片烯-2,3-二甲酰亚胺，1,8-二氮杂双环[5.4.0]十一碳-7-烯等单体的亚胺基团，二氮杂双环基团的引入，提高了阻燃效果，聚苯乙烯的极限氧指数可提高50%以上。
具体实施方式
以下实例仅仅是进一步说明本发明，并不是限制本发明保护的范围。
实施例1：在3000L反应釜中加入100Kg苯乙烯，26Kg磷酸三烯丙酯，然后加入0.5Kg异戊烯基聚氧乙烯醚，0.05KgN-羟基-5-降冰片烯-2,3-二甲酰亚胺，0.05Kg1,8-二氮杂双环[5.4.0]十一碳-7-烯，1500Kg水,3Kg明胶，2Kg过氧化苯甲酰，在90℃反应6h，过滤，烘干后得到产品。产品编号M-1。
实施例2：
在3000L反应釜中加入100Kg苯乙烯，10Kg磷酸三烯丙酯，然后加入0.1Kg异戊烯基聚氧乙烯醚，0.01KgN-羟基-5-降冰片烯-2,3-二甲酰亚胺，0.01Kg1,8-二氮杂双环[5.4.0]十一碳-7-烯，1000Kg水,1Kg聚乙烯醇，1Kg偶氮二异庚腈，在70℃反应15h，过滤，烘干后得到产品。产品编号M-2。
实施例3：
在3000L反应釜中加入100Kg苯乙烯，30Kg磷酸三烯丙酯，然后加入1Kg异戊烯基聚氧乙烯醚，0.1KgN-羟基-5-降冰片烯-2,3-二甲酰亚胺，0.1Kg1,8-二氮杂双环[5.4.0]十一碳-7-烯，2000Kg水,5Kg羟甲基纤维素，4Kg过氧化苯甲酰，在110℃反应4h，过滤，烘干后得到产品。产品编号M-3。
比较例1：磷酸三烯丙酯不加入，其它同实施例1。所得产品编号为M-4。
比较例2：异戊烯基聚氧乙烯醚不加入，其它同实施例1。所得产品编号为M-5。
比较例3：N-羟基-5-降冰片烯-2,3-二甲酰亚胺不加入，其它同实施例1。所得产品编号为M-6。
比较例4：
1,8-二氮杂双环[5.4.0]十一碳-7-烯不加入，其它同实施例1。所得产品编号为M-7。
实施例4：
将加入实施例1-3以及对比例1-4的阻燃型聚苯乙烯按GB/T 2406-1993检测极限氧指数LOI。
表1不同工艺做出的试验样品阻燃性能的比较
| 编号 | LOI% |
| M-1 | 28.9 |
| M-2 | 27.6 |
| M-3 | 29.1 |
| M-4 | 21.1 |
| M-5 | 24.8 |
| M-6 | 24.8 |
| M-7 | 24.3 |
| 纯聚苯乙烯 | 18.6 |
由表1可知：阻燃型聚苯乙烯阻燃性的提高非常显著，LOI增加量也非常显著。
Claims (3)
1.一种阻燃型聚苯乙烯的制备方法，其特征在于制备方法包括以下步骤：
在反应釜中，按重量份计加入100份苯乙烯，10-30份磷酸三烯丙酯、0.1-1份异戊烯基聚氧乙烯醚，0.01-0.1份N-羟基-5-降冰片烯-2,3-二甲酰亚胺，0.01-0.1份1,8-二氮杂双环[5.4.0]十一碳-7-烯，1000-2000份水，1-5份分散剂，1-4份自由基聚合引发剂，在70℃-110℃反应4-15h，过滤，烘干后得到产品。
2.根据权利要求1的一种阻燃型聚苯乙烯的制备方法，其特征在于所述的自由基聚合引发剂包括偶氮化合物以及氧化还原体系引发剂。
3.根据权利要求1的一种阻燃型聚苯乙烯的制备方法，其特征在于所述的所述的分散剂包括明胶，聚乙烯醇，羟甲基纤维素。
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