CN116217812A - 一种无卤阻燃聚乙烯泡沫材料和制备方法 - Google Patents
一种无卤阻燃聚乙烯泡沫材料和制备方法 Download PDFInfo
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Abstract
本发明涉及聚乙烯阻燃技术领域,且公开了一种无卤阻燃聚乙烯泡沫材料和制备方法,利用氧化二异丙苯或过氧化二苯甲酰作为交联剂,将烯基磷酸酯苯并噁嗪无卤阻燃剂于聚乙烯进行熔融接枝反应,将磷酸酯苯并噁嗪阻燃剂接枝到聚乙烯的分子链中,然后经过模压发泡,得到无卤阻燃聚乙烯泡沫材料,苯并噁嗪结构的热分解温度大、耐热性好,成炭性高,接枝到聚乙烯中可以提高泡沫材料的热稳定性能,同时含有磷酸酯阻燃成分,进一步提高聚乙烯泡沫材料的阻燃性能,降低了材料的燃烧时的热释放速率和总热释放量。
Description
技术领域
本发明涉及聚乙烯阻燃技术领域,具体为一种无卤阻燃聚乙烯泡沫材料和制备方法。
背景技术
聚乙烯泡沫塑料的耐热性号、吸水性小、化学性能稳定、机械性能优良,并且具有加工性能好,易于成型等优点,在精密仪器仪表、家用电器、绝热容器、包装材料等利用,对聚乙烯泡沫进行阻燃改性,拓展其在耐燃和防火材料等方面的应用具有重要的意义,论文《膨胀阻燃聚乙烯泡沫材料结构与性能的研究》,报道了利用木质素或淀粉、聚磷酸铵、三聚氰胺氰尿酸盐形成膨胀阻燃剂,提高了聚乙烯泡沫的极限氧指数和垂直燃烧等级等阻燃性能。
阻燃剂是赋予高分子聚合物等材料难燃性的功能性助剂,主要分为含卤阻燃剂、膨胀阻燃剂、含磷阻燃剂等,其中含磷阻燃剂具有制备方法多样、绿色污染小、阻燃性能优良等优点,广泛应用在聚乙烯等高分子材料中。苯并噁嗪是一种热固性树脂,热分解温度大、耐热性好,成炭性高等优点,可以提高聚乙烯等材料的综合性能,如会议论文《烯丙基苯并噁嗪与聚乙烯接枝共聚物的制备与表征》,报道了以烯丙基苯并噁嗪作为接枝单体,通过反应挤出接枝的方法,制备了苯并噁嗪-聚乙烯接枝共聚物,具有更高的结晶温度和良好的憎水性。
发明内容
(一)解决的技术问题
针对现有技术的不足,本发明提供了一种热稳定性和阻燃性优异的无卤阻燃聚乙烯泡沫材料。
(二)技术方案
一种无卤阻燃聚乙烯泡沫材料,以重量份计包括如下组份:100份聚乙烯、15-25份发泡剂偶氮二甲酰胺、1-1.5份交联剂、3-15份烯基磷酸酯苯并噁嗪无卤阻燃剂,所述聚乙烯泡沫材料的制备方法为:
S1:向乙醇中加入100份苯胺和120-160份对羟基苯甲醛,搅拌进行缩合反应,然后再加入130-180份亚磷酸二乙酯,进行加成反应,反应后减压蒸馏,乙醚洗涤后、粗产物溶解到二氯甲烷中并重结晶,得到苯酚基亚胺磷酸二乙酯。
S2:向1,4-二氧六环溶剂中加入100份烯丙基胺和含有80-120份甲醛的水溶液,在0-5℃中搅拌2-4h,然后加入600-850份的苯酚基亚胺磷酸二乙酯,搅拌进行环化反应,反应后减压蒸馏,乙醇中并重结晶,得到烯基磷酸酯苯并噁嗪无卤阻燃剂。
S3:依次将聚乙烯、烯基磷酸酯苯并噁嗪无卤阻燃剂、交联剂加入到双螺杆挤出机中,在170-200℃的温度中熔融共混、挤出造粒;然后再将物料与发泡剂偶氮二甲酰胺混合,在双螺杆挤出机中,在110-125℃的温度下低温共混、挤出母粒,最后将母粒采用模压法进行发泡,得到无卤阻燃聚乙烯泡沫材料。
优选的,所述S1中缩合反应在60-80℃中进行3-6h,加成反应在70-100℃中进行6-12h。
优选的,所述S2中环化反应在75-90℃中进行6-18h。
优选的,所述模压法发泡的模压温度为190-220℃,压力为3-8MPa,模压时间为10-20min。
优选的,所述交联剂包括氧化二异丙苯或过氧化二苯甲酰。
(三)有益的技术效果
利用苯胺、对羟基苯甲醛、亚磷酸二乙酯作为反应原料,经过缩合反应和加成反应,合成了苯酚基亚胺磷酸二乙酯,然后再与烯丙基胺和甲醛进行环化反应,得到新型的烯基磷酸酯苯并噁嗪无卤阻燃剂,具有制备方法简单高效,反应条件绿色温和的优点。
利用氧化二异丙苯或过氧化二苯甲酰作为交联剂,将烯基磷酸酯苯并噁嗪无卤阻燃剂于聚乙烯进行熔融接枝反应,从而将阻燃剂接枝到聚乙烯的分子链中,然后经过模压发泡,得到无卤阻燃聚乙烯泡沫材料,苯并噁嗪结构的热分解温度大、耐热性好,成炭性高,接枝到聚乙烯中可以提高泡沫材料的热稳定性能,同时含有磷酸酯阻燃成分,进一步提高聚乙烯泡沫材料的阻燃性能,降低了材料的燃烧时的热释放速率和总热释放量。
附图说明
图1是无卤阻燃聚乙烯泡沫材料的热重测试曲线。
图2是无卤阻燃聚乙烯泡沫材料的热释放速率测试曲线。
图3是无卤阻燃聚乙烯泡沫材料的总热释放量测试曲线。
具体实施方式
实施例1
S1:向乙醇中加入3g苯胺和3.6g的对羟基苯甲醛,在80℃中搅拌进行缩合反应6h,然后再加入3.9g亚磷酸二乙酯,在70℃中进行加成反应8h,反应后减压蒸馏,乙醚洗涤后、粗产物溶解到二氯甲烷中并重结晶,得到苯酚基亚胺磷酸二乙酯,反应式为:
S2:向1,4-二氧六环溶剂中加入0.5g的烯丙基胺和含有0.5g的甲醛的水溶液,在0℃中搅拌4h,然后加入4.25g的苯酚基亚胺磷酸二乙酯,在90℃中搅拌进行环化反应12h,反应后减压蒸馏,乙醇中并重结晶,得到烯基磷酸酯苯并噁嗪无卤阻燃剂,反应式为:
S3:依次将200g的聚乙烯、6g烯基磷酸酯苯并噁嗪无卤阻燃剂、3g交联剂过氧化二异丙苯加入到双螺杆挤出机中,在180℃的温度中熔融共混、挤出造粒;然后再将物料与30g的发泡剂偶氮二甲酰胺混合,在双螺杆挤出机中,在15℃的温度下低温共混、挤出母粒,最后将母粒采用模压法进行发泡,模压温度为220℃,压力为3MPa,模压时间为15min,得到无卤阻燃聚乙烯泡沫材料。
实施例2
S1:向乙醇中加入3g苯胺和4.8g的对羟基苯甲醛,在80℃中搅拌进行缩合反应6h,然后再加入3.9g亚磷酸二乙酯,在100℃中进行加成反应12h,反应后减压蒸馏,乙醚洗涤后、粗产物溶解到二氯甲烷中并重结晶,得到苯酚基亚胺磷酸二乙酯,反应式为。
S2:向1,4-二氧六环溶剂中加入0.5g的烯丙基胺和含有0.5g的甲醛的水溶液,在5℃中搅拌2h,然后加入3g的苯酚基亚胺磷酸二乙酯,在90℃中搅拌进行环化反应12h,反应后减压蒸馏,乙醇中并重结晶,得到烯基磷酸酯苯并噁嗪无卤阻燃剂。
S3:依次将200g的聚乙烯、20g烯基磷酸酯苯并噁嗪无卤阻燃剂、2g交联剂过氧化二苯甲酰加入到双螺杆挤出机中,在200℃的温度中熔融共混、挤出造粒;然后再将物料与35g的发泡剂偶氮二甲酰胺混合,在双螺杆挤出机中,在125℃的温度下低温共混、挤出母粒,最后将母粒采用模压法进行发泡,模压温度为190℃,压力为5MPa,模压时间为20min,得到无卤阻燃聚乙烯泡沫材料。
实施例3
S1:向乙醇中加入3g苯胺和4g的对羟基苯甲醛,在60℃中搅拌进行缩合反应6h,然后再加入4.8g亚磷酸二乙酯,在100℃中进行加成反应6h,反应后减压蒸馏,乙醚洗涤后、粗产物溶解到二氯甲烷中并重结晶,得到苯酚基亚胺磷酸二乙酯,反应式为。
S2:向1,4-二氧六环溶剂中加入0.5g的烯丙基胺和含有0.6g的甲醛的水溶液,在2℃中搅拌2h,然后加入3.5g的苯酚基亚胺磷酸二乙酯,在80℃中搅拌进行环化反应18h,反应后减压蒸馏,乙醇中并重结晶,得到烯基磷酸酯苯并噁嗪无卤阻燃剂。
S3:依次将200g的聚乙烯、30g烯基磷酸酯苯并噁嗪无卤阻燃剂、2g交联剂过氧化二异丙苯加入到双螺杆挤出机中,在180℃的温度中熔融共混、挤出造粒;然后再将物料与40g的发泡剂偶氮二甲酰胺混合,在双螺杆挤出机中,在120℃的温度下低温共混、挤出母粒,最后将母粒采用模压法进行发泡,模压温度为220℃,压力为8MPa,模压时间为10min,得到无卤阻燃聚乙烯泡沫材料。
热失重分析:试样标准80mm×80mm×5mm,TGA热重分析仪,氮气气氛,测试温度25-800℃,升温速率20℃/min。
燃烧性能测试:试样标准100mm×100mm×3mm,锥形量热仪,热辐射功率35kW/m2。
Claims (5)
1.一种无卤阻燃聚乙烯泡沫材料,以重量份计包括如下组份:100份聚乙烯、15-25份发泡剂偶氮二甲酰胺、1-1.5份交联剂、3-15份烯基磷酸酯苯并噁嗪无卤阻燃剂,其特征在于:所述聚乙烯泡沫材料的制备方法为:
S1:向乙醇中加入100份苯胺和120-160份对羟基苯甲醛,搅拌进行缩合反应,然后再加入130-180份亚磷酸二乙酯,进行加成反应,反应后减压蒸馏,乙醚洗涤后、粗产物溶解到二氯甲烷中并重结晶,得到苯酚基亚胺磷酸二乙酯;
S2:向1,4-二氧六环溶剂中加入100份烯丙基胺和含有80-120份甲醛的水溶液,在0-5℃中搅拌2-4h,然后加入600-850份的苯酚基亚胺磷酸二乙酯,搅拌进行环化反应,反应后减压蒸馏,乙醇中并重结晶,得到烯基磷酸酯苯并噁嗪无卤阻燃剂;
S3:依次将聚乙烯、烯基磷酸酯苯并噁嗪无卤阻燃剂、交联剂加入到双螺杆挤出机中,在170-200℃的温度中熔融共混、挤出造粒;然后再将物料与发泡剂偶氮二甲酰胺混合,在双螺杆挤出机中,在110-125℃的温度下低温共混、挤出母粒,最后将母粒采用模压法进行发泡,得到无卤阻燃聚乙烯泡沫材料。
2.根据权利要求1所述的无卤阻燃聚乙烯泡沫材料,其特征在于:所述S1中缩合反应在60-80℃中进行3-6h,加成反应在70-100℃中进行6-12h。
3.根据权利要求1所述的无卤阻燃聚乙烯泡沫材料,其特征在于:所述S2中环化反应在75-90℃中进行6-18h。
4.根据权利要求1所述的无卤阻燃聚乙烯泡沫材料,其特征在于:所述模压法发泡的模压温度为190-220℃,压力为3-8MPa,模压时间为10-20min。
5.根据权利要求1所述的无卤阻燃聚乙烯泡沫材料,其特征在于:所述交联剂包括过氧化二异丙苯或过氧化二苯甲酰。
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