CN111409317A - 一种阻燃防毒耐高温聚丙烯共挤膜及其制备方法 - Google Patents

一种阻燃防毒耐高温聚丙烯共挤膜及其制备方法 Download PDF

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CN111409317A
CN111409317A CN202010234563.2A CN202010234563A CN111409317A CN 111409317 A CN111409317 A CN 111409317A CN 202010234563 A CN202010234563 A CN 202010234563A CN 111409317 A CN111409317 A CN 111409317A
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temperature
flame
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张�杰
陈祯
张婷婷
任玮
韩德孝
孙红月
肖大君
楚鑫鑫
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Beijing Bangwei High Tech New Material Technology Co ltd
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Abstract

本发明公开了一种阻燃防毒耐高温聚丙烯共挤膜及其制备方法。该共挤膜包括由外至内的外层、黏合层、中间层、黏合层和内层；外层原料为聚烯烃树脂、阻燃剂和色母粒的共混物；黏合层原料为马来酸酐改性聚丙烯聚合物、乙烯‑甲基丙烯酸共聚物、线型低密度聚乙烯或乙烯‑醋酸乙烯共聚物中的任意一种；中间层原料为聚偏二氯乙烯、乙烯‑乙烯醇共聚物或聚酰胺中的任意一种；内层原料为增韧树脂、阻燃剂和色母粒的共混物。该方法是将各层原料通过多层共挤出复合设备采用多层共挤出复合工艺制备得到五层共挤膜。本发明将阻燃、防毒、耐高温集成到聚丙烯薄膜中，阻燃性、耐热老化性、阻隔性、抗撕裂性优异，手感柔软，适用于防护装备和生化包装材料领域。

Description

一种阻燃防毒耐高温聚丙烯共挤膜及其制备方法
技术领域
本发明涉及聚丙烯膜，具体是一种阻燃防毒耐高温聚丙烯共挤膜及其制备方法。
背景技术
聚丙烯膜因其低成本、高阻隔、易成型及稳定性等特点，广泛应用于包装、化工、建筑、纺织等行业中。现有技术涉及功能聚丙烯膜的有阻燃聚丙烯膜、阻隔聚丙烯膜和耐低温聚丙烯膜等。
聚丙烯因自身结构特点，极限氧指数约为18％，属于易燃性材料，一般采用添加阻燃剂及协效剂的方式提高其阻燃性。现有聚丙烯阻燃技术多应用在汽车、机械设备的零部件以及电线电缆电器等领域。聚丙烯制品通常厚度大、结构层数少，多为单层共混材料，阻隔性能一般。采用专门适用于薄膜塑料阻燃等级评定的UL94《Tests for Flammability ofPlastic Materials for Parts in Devices and Appliances》方法测试，阻燃聚丙烯膜仍然很难达到VTM-2级，而且薄膜厚度越低其阻燃性越难实现。
现有涉及聚丙烯阻隔性能的技术很多，多集中在土工膜、棚膜、食品包装膜等领域。然而，其防护对象均为氧气、氢气、空气、水蒸气等普通气体，目前尚无针对军用毒剂“芥子气”的研究报道。
目前尚未见应用于防护材料或防护装备上的功能聚丙烯膜的报道，特别是耐高温聚丙烯技术。防护装备因其使用性要求，需要薄膜手感柔软，通常采用在其树脂配方上增加增韧树脂的方式降低聚丙烯硬度，提高韧性，但是带来的潜在危害是显著降低了聚丙烯膜的耐温性能，特别是在高温环境下持续放置，聚丙烯膜表面会出现变色、发粘、变脆等现象，影响装备外观及使用可靠性。
因此，作为阻隔膜将聚丙烯应用于防护装备中时，聚丙烯无法同时兼顾阻燃、防毒、耐高温和柔韧性，致使聚丙烯膜的优异性能无法发挥，限定了其应用范围。
发明内容
针对现有技术的不足，本发明拟解决的技术问题是，提供一种阻燃防毒耐高温聚丙烯共挤膜及其制备方法。
本发明解决所述共挤膜技术问题的技术方案是，提供一种阻燃防毒耐高温聚丙烯共挤膜，其特征在于该共挤膜包括由外至内的外层、黏合层、中间层、黏合层和内层；
外层原料为聚烯烃树脂、阻燃剂和色母粒的共混物；黏合层原料为马来酸酐改性聚丙烯聚合物、乙烯-甲基丙烯酸共聚物、线型低密度聚乙烯或乙烯-醋酸乙烯共聚物中的任意一种；中间层原料为聚偏二氯乙烯、乙烯-乙烯醇共聚物或聚酰胺中的任意一种；内层原料为增韧树脂、阻燃剂和色母粒的共混物。
本发明解决所述方法技术问题的技术方案是，提供一种阻燃防毒耐高温聚丙烯共挤膜的制备方法，其特征在于该方法是：将各层原料采用多层共挤出复合工艺制备得到阻燃防毒耐高温聚丙烯共挤膜。
与现有技术相比，本发明有益效果在于：
(1)本发明将阻燃、防毒、耐高温集成到聚丙烯薄膜中，制备的阻燃防毒耐高温聚丙烯膜的阻燃性能好(大于VTM-2级)，对芥子气的阻隔性优异(芥子气“液-气”防护时间大于150min)，125℃下老化24h后薄膜表面不粘不脆，耐热老化性能优异。
(2)本发明赋予了聚丙烯膜良好的手感及物理机械性能，克服了现有聚丙烯膜阻燃性差、手感脆硬、抗撕裂性差、不耐折叠的缺点，提升了聚丙烯膜的使用性；解决了现有聚丙烯薄膜阻燃、防毒、耐高温的相容性技术难题，可应用于防护装备、耐高温蒸煮膜材、危化品包装材料、生化战剂阻隔袋、棚膜、柔性掩蔽体、防护帐篷等产品中，提升了聚丙烯膜的产品价值及市场潜力。
(3)本方法采用多层共挤出复合工艺，一次成型，无溶剂污染，清洁环保，快速高效。
具体实施方式
下面给出本发明的具体实施例。具体实施例仅用于进一步详细说明本发明，不限制本申请权利要求的保护范围。
本发明提供了一种阻燃防毒耐高温聚丙烯共挤膜(简称共挤膜)，其特征在于该共挤膜采用多层共挤出复合工艺，得到由外至内依次为外层、黏合层、中间层、黏合层和内层的五层结构薄膜材料；
外层原料为聚烯烃树脂、阻燃剂和色母粒的共混物；黏合层原料为马来酸酐改性聚丙烯聚合物、乙烯-甲基丙烯酸共聚物、线型低密度聚乙烯或乙烯-醋酸乙烯共聚物中的任意一种；中间层原料为聚偏二氯乙烯、乙烯-乙烯醇共聚物或聚酰胺中的任意一种；内层原料为增韧树脂、阻燃剂和色母粒的共混物。
所述聚烯烃树脂由聚丙烯均聚树脂与增韧树脂组成；
所述增韧树脂为聚丙烯共聚树脂、低密度聚乙烯、线型低密度聚乙烯(LLDPE)、聚烯烃塑性体或聚烯烃弹性体中的至少一种；
所述阻燃剂为金属氧化物和卤代烃的混合物、磷酸酯或膨胀型阻燃剂中的至少一种；所述金属氧化物和卤代烃的混合物为十溴二苯醚和氧化锑的混合物；所述磷酸酯为甲基膦酸二甲酯。
优选地，外层原料为100重量份的聚烯烃树脂、12～25重量份的阻燃剂和4～8重量份的色母粒的共混物；内层原料为100重量份的增韧树脂、12～25重量份的阻燃剂和4～8重量份的色母粒的共混物；
优选地，所述聚烯烃树脂由100重量份的聚丙烯均聚树脂与60～300重量份的增韧树脂组成；
所述共挤膜的厚度为50～250um，其中外层的厚度为20～100um，黏合层的厚度为5～15um，中间层的厚度为5～30um，内层的厚度为20～100um。
本发明同时提供了一种阻燃防毒耐高温聚丙烯共挤膜的制备方法(简称方法)，其特征在于该方法是：将各层原料通过多层共挤出复合设备采用多层共挤出复合工艺制备得到阻燃防毒耐高温聚丙烯共挤膜。
多层共挤出复合工艺中，外层的挤出机加工温度为：一温区175～225℃，二温区175～225℃，三温区180～220℃，四温区165～195℃；黏合层的挤出机加工温度为：一温区145～175℃，二温区180～195℃，三温区180～195℃，四温区170～190℃；中间层的挤出机加工温度为：一温区165～200℃，二温区165～200℃，三温区160～175℃，四温区145～155℃；内层的挤出机加工温度为：一温区175～220℃，二温区175～220℃，三温区180～205℃，四温区160～175℃；多层共挤出复合模头加工温度为190～205℃。
所述多层共挤出复合设备包括共挤出平膜生产线或共挤出管膜生产线；
所述多层共挤出复合工艺包括共挤出吹塑成膜法、共挤出流延成膜法等；
该方法的具体是：将各层原料分别加入到各自的挤出机中，在各自的挤出机中分别熔融塑化后，流入同一个多层共挤出复合模头中并按照一定的层间结构均匀分布在模头中，然后经过挤出复合、冷却成型后，得到阻燃防毒耐高温聚丙烯共挤膜。
当采用共挤出管膜生产线时，将各层原料分别加入到各自的挤出机中，经过每层各自的挤出机分别熔融塑化后，流入多层共挤出管状复合模头中并按照一定的层间结构均匀分布在模头中，模口挤出、吹胀冷却后，得到阻燃防毒耐高温聚丙烯共挤膜。
当采用共挤出平膜生产线时，将各层原料分别加入到各自的挤出机中，经过每层各自的挤出机分别熔融塑化后，流入多层共挤出流延复合模头中并按照一定的层间结构均匀分布在模头中，模口挤出、流延冷却后，得到阻燃防毒耐高温聚丙烯共挤膜。
实施例1
共挤膜外层的厚度为25um，黏合层厚度为5um，中间层厚度为10um，内层厚度为25um。
外层的原料配方由100重量份的聚烯烃树脂、13重量份的十溴二苯醚和氧化锑的混合物以及5重量份的色母粒混合组成。其中：聚烯烃树脂由100重量份的聚丙烯均聚树脂和60重量份的聚烯烃塑性体组成。
黏合层的原料配方为马来酸酐改性聚丙烯聚合物。
中间层的原料配方为聚偏二氯乙烯。
内层的原料配方由100重量份的增韧树脂、13重量份的十溴二苯醚和氧化锑的混合物以及5重量份的色母粒混合组成。其中：增韧树脂为聚烯烃弹性体。
上述原料准备好后分别添加至不同的挤出机进料斗中，通过吹膜机(即共挤出管膜生产线)将各层原料挤出成型。
外层的挤出机加工温度为：一温区225℃，二温区225℃，三温区220℃，四温区195℃。
黏合层的挤出机加工温度为：一温区175℃，二温区195℃，三温区195℃，四温区190℃。
中间层的挤出机加工温度为：一温区165℃，二温区165℃，三温区160℃，四温区145℃。
内层的挤出机加工温度为：一温区205℃，二温区205℃，三温区200℃，四温区175℃。
多层共挤出复合模头加工温度为205℃。
制成的阻燃防毒耐高温聚烯烃膜的厚度65um，阻燃性为VTM-2级，防毒时间163min，在125℃高温下放置24h表面不粘不脆，直角撕裂强度为148KN/m。
实施例2
共挤膜外层的厚度为60um，黏合层厚度为5um，中间层厚度为10um，内层厚度为60um。
外层的原料配方由100重量份的聚烯烃树脂、22重量份的膨胀型阻燃剂和7重量份的色母粒混合组成。其中：聚烯烃树脂由100重量份的聚丙烯均聚树脂和300重量份的聚丙烯共聚树脂组成。
黏合层的原料配方为乙烯-醋酸乙烯共聚物。
中间层的原料配方为乙烯-乙烯醇共聚物。
内层的原料配方由100重量份的增韧树脂、22重量份的膨胀型阻燃剂和7重量份的色母粒混合组成。其中：增韧树脂由100重量份的线型低密度聚乙烯树脂和10重量份的聚烯烃塑性体组成。
上述原料准备好后分别添加至不同的挤出机进料斗中，通过流延机(即共挤出平膜生产线)将各层原料挤出成型。
外层的挤出机加工温度为：一温区220℃，二温区220℃，三温区205℃，四温区175℃。
黏合层的挤出机加工温度为：一温区165℃，二温区185℃，三温区185℃，四温区175℃。
中间层的挤出机加工温度为：一温区200℃，二温区200℃，三温区175℃，四温区155℃。
内层的挤出机加工温度为：一温区220℃，二温区220℃，三温区205℃，四温区175℃。
多层共挤出复合模头加工温度为190℃。
制成的阻燃防毒耐高温聚烯烃膜的厚度135um，阻燃性为VTM-0级，防毒时间198min，在125℃高温下放置24h表面不粘不脆，直角撕裂强度为121KN/m。
实施例3
共挤膜外层的厚度为30um，黏合层厚度为13um，中间层厚度为30um，内层厚度为100um。
外层的原料配方由100重量份的聚烯烃树脂、18重量份的磷酸酯阻燃剂和4重量份的色母粒混合组成。其中：聚烯烃树脂由100重量份的聚丙烯均聚树脂和100重量份的聚烯烃弹性体组成。
黏合层的原料配方为线型低密度聚乙烯。
中间层的原料配方为聚酰胺。
内层的原料配方由100重量份的增韧树脂、18重量份的磷酸酯阻燃剂和4重量份的色母粒混合组成。其中：增韧树脂由20重量份的聚丙烯共聚树脂和100重量份的聚烯烃弹性体组成。
上述原料准备好后分别添加至不同的挤出机进料斗中，通过流延机将各层原料挤出成型。
外层的挤出机加工温度为：一温区175℃，二温区175℃，三温区180℃，四温区165℃。
黏合层的挤出机加工温度为：一温区145℃，二温区180℃，三温区180℃，四温区170℃。
中间层的挤出机加工温度为：一温区165℃，二温区165℃，三温区160℃，四温区155℃。
内层的挤出机加工温度为：一温区175℃，二温区175℃，三温区180℃，四温区160℃。
多层共挤出复合模头加工温度为200℃。
制成的阻燃防毒耐高温聚烯烃膜的厚度173um，阻燃性为VTM-0级，防毒时间288min，在125℃高温下放置24h表面不粘不脆，直角撕裂强度为153KN/m。
实施例4
共挤膜外层的厚度为40um，黏合层厚度为8um，中间层厚度为10um，内层厚度为80um。
外层的原料配方由100重量份的聚烯烃树脂、12重量份的十溴二苯醚和氧化锑混合物阻燃剂以及6重量份的色母粒混合组成。其中：聚烯烃树脂由100重量份的聚丙烯均聚树脂和180重量份的低密度聚乙烯组成。
黏合层的原料配方为乙烯-甲基丙烯酸共聚物。
中间层的原料配方为聚偏二氯乙烯。
内层的原料配方由100重量份的增韧树脂、12重量份的十溴二苯醚和氧化锑混合物阻燃剂以及6重量份的色母粒混合组成。其中：增韧树脂为低密度聚乙烯树脂。
上述原料准备好后分别添加至不同的挤出机进料斗中，通过吹膜机将各层原料挤出成型。
外层的挤出机加工温度为：一温区195℃，二温区195℃，三温区190℃，四温区180℃。
黏合层的挤出机加工温度为：一温区165℃，二温区185℃，三温区185℃，四温区175℃。
中间层的挤出机加工温度为：一温区165℃，二温区165℃，三温区160℃，四温区145℃。
内层的挤出机加工温度为：一温区200℃，二温区200℃，三温区190℃，四温区180℃。
多层共挤出复合模头加工温度为185℃。
制成的阻燃防毒耐高温聚烯烃膜的厚度138um，阻燃性为VTM-2级，防毒时间169min，在125℃高温下放置24h表面不粘不脆，直角撕裂强度为189KN/m。
实施例5
共挤膜外层的厚度为80um，黏合层厚度为10um，中间层厚度为30um，内层厚度为100um。
外层的原料配方由100重量份的聚烯烃树脂、20重量份的膨胀型阻燃剂和6重量份的色母粒混合组成。其中：聚烯烃树脂由100重量份的聚丙烯均聚树脂和150重量份的线型低密度聚乙烯组成。
黏合层的原料配方为乙烯-醋酸乙烯共聚物。
中间层的原料配方为聚酰胺。
内层的原料配方由100重量份的增韧树脂、20重量份的膨胀型阻燃剂和6重量份的色母粒混合组成。其中：增韧树脂由40重量份的聚丙烯共聚树脂和100重量份的聚烯烃塑性体组成。
上述原料准备好后分别添加至不同的挤出机进料斗中，通过流延机将各层原料挤出成型。
外层的挤出机加工温度为：一温区210℃，二温区210℃，三温区195℃，四温区175℃。
黏合层的挤出机加工温度为：一温区165℃，二温区165℃，三温区185℃，四温区175℃。
中间层的挤出机加工温度为：一温区165℃，二温区165℃，三温区160℃，四温区155℃。
内层的挤出机加工温度为：一温区190℃，二温区190℃，三温区180℃，四温区175℃。
多层共挤出复合模头加工温度为195℃。
制成的阻燃防毒耐高温聚烯烃膜的厚度220um，阻燃性为VTM-0级，防毒时间459min，在125℃高温下放置24h表面不粘不脆，直角撕裂强度为137KN/m。
其中，测试方法是：
阻燃性，采用UL94《Tests for Flammability of Plastic Materials for Partsin Devices and Appliances》中11Thin Material Vertical Burning Test；VTM-0,VTM-1,or VTM-2测定。
防毒性(防军用毒剂芥子气(液-气)穿透时间)，采用GJB 535-1988《隔绝式防毒衣材料对芥子气(液-气)防毒时间的测定方法》测定。
耐高温性，采用HGT 3049-1999《橡胶或塑料涂覆织物加速老化试验》测定。
直角撕裂性能，采用QBT 1130-1991《塑料直角撕裂性能试验方法》测定。
本发明未述及之处适用于现有技术。

Claims (10)

1.一种阻燃防毒耐高温聚丙烯共挤膜，其特征在于该共挤膜包括由外至内的外层、黏合层、中间层、黏合层和内层；
外层原料为聚烯烃树脂、阻燃剂和色母粒的共混物；黏合层原料为马来酸酐改性聚丙烯聚合物、乙烯-甲基丙烯酸共聚物、线型低密度聚乙烯或乙烯-醋酸乙烯共聚物中的任意一种；中间层原料为聚偏二氯乙烯、乙烯-乙烯醇共聚物或聚酰胺中的任意一种；内层原料为增韧树脂、阻燃剂和色母粒的共混物。
2.根据权利要求1所述的阻燃防毒耐高温聚丙烯共挤膜，其特征在于外层原料为100重量份的聚烯烃树脂、12～25重量份的阻燃剂和4～8重量份的色母粒的共混物；内层原料为100重量份的增韧树脂、12～25重量份的阻燃剂和4～8重量份的色母粒的共混物。
3.根据权利要求1或2所述的阻燃防毒耐高温聚丙烯共挤膜，其特征在于所述聚烯烃树脂由聚丙烯均聚树脂与增韧树脂组成。
4.根据权利要求1或2所述的阻燃防毒耐高温聚丙烯共挤膜，其特征在于所述聚烯烃树脂由100重量份的聚丙烯均聚树脂与60～300重量份的增韧树脂组成。
5.根据权利要求3或4所述的阻燃防毒耐高温聚丙烯共挤膜，其特征在于所述增韧树脂为聚丙烯共聚树脂、低密度聚乙烯、线型低密度聚乙烯、聚烯烃塑性体或聚烯烃弹性体中的至少一种。
6.根据权利要求1或2所述的阻燃防毒耐高温聚丙烯共挤膜，其特征在于所述阻燃剂为金属氧化物和卤代烃的混合物、磷酸酯或膨胀型阻燃剂中的至少一种。
7.根据权利要求6所述的阻燃防毒耐高温聚丙烯共挤膜，其特征在于所述金属氧化物和卤代烃的混合物为十溴二苯醚和氧化锑的混合物；所述磷酸酯为甲基膦酸二甲酯。
8.根据权利要求1或2所述的阻燃防毒耐高温聚丙烯共挤膜，其特征在于所述共挤膜的厚度为50～250um，外层的厚度为20～100um，黏合层的厚度为5～15um，中间层的厚度为5～30um，内层的厚度为20～100um。
9.一种权利要求1-8任一所述阻燃防毒耐高温聚丙烯共挤膜的制备方法，其特征在于该方法是：将权利要求1-8任一所述的各层原料采用多层共挤出复合工艺制备得到阻燃防毒耐高温聚丙烯共挤膜。
10.根据权利要求9所述的阻燃防毒耐高温聚丙烯共挤膜的制备方法，其特征在于该方法的具体是：将各层原料分别加入到各自的挤出机中，在各自的挤出机中分别熔融塑化后，流入多层共挤出复合模头中并按照一定的层间结构分布，然后经过挤出复合、冷却成型后，得到阻燃防毒耐高温聚丙烯共挤膜；
外层的挤出机加工温度为：一温区175～225℃，二温区175～225℃，三温区180～220℃，四温区165～195℃；
黏合层的挤出机加工温度为：一温区145～175℃，二温区180～195℃，三温区180～195℃，四温区170～190℃；
中间层的挤出机加工温度为：一温区165～200℃，二温区165～200℃，三温区160～175℃，四温区145～155℃；
内层的挤出机加工温度为：一温区175～220℃，二温区175～220℃，三温区180～205℃，四温区160～175℃；
多层共挤出复合模头加工温度为190～205℃。
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