CN104130511A - 一种辐照硫化制备氯化聚乙烯发泡材料的方法 - Google Patents

一种辐照硫化制备氯化聚乙烯发泡材料的方法 Download PDF

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CN104130511A
CN104130511A CN201310157024.3A CN201310157024A CN104130511A CN 104130511 A CN104130511 A CN 104130511A CN 201310157024 A CN201310157024 A CN 201310157024A CN 104130511 A CN104130511 A CN 104130511A
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chlorinatedpolyethylene
foam material
radiation
chlorinated polyethylene
vulanization
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刘伟
郝建钢
张玥
叶明旸
靳健乔
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TIANJIN INSTITUTE OF TECHNICAL PHYSICS
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Abstract

本发明属于氯化聚乙烯发泡材料及其制造方法。氯化聚乙烯发泡材料，其组份和重量百分比含量如下：氯化聚乙烯30～97％，其它烯烃聚合物0～57％，发泡剂2～20％，助硫化剂0.1～5％。制造方法是采用辐射硫化方法：将混合物在100～150℃熔融共混成型，将成型物进行辐射硫化，辐射剂量为10～200kGy；辐照后再经过高温发泡为成品，常压发泡温度控制在180～350℃；加压发泡温度控制在180～300℃。本发明的效果：(1)本发明所述的氯化聚乙烯发泡材料使用辐射方法进行硫化，可以摆脱氯化聚乙烯化学硫化时分子链易断裂的难题；(2)本发明可以实现工业化批量生产。

Description

一种辐照硫化制备氯化聚乙烯发泡材料的方法
技术领域
本发明涉及一种辐射硫化氯化聚乙烯发泡材料新的制备方法。
背景技术
氯化聚乙烯的分子结构具有与原料聚乙烯相同的主链结构，只是主链碳原子上的部分氢原子被氯原子取代。从氯化聚乙烯的分子结构式看，它是一种饱和的聚合物，可以看作乙烯、氯乙烯、1，2二氯乙烯的三元聚合体，只有在氯含量很高时，偏二氯乙烯型链节才有可能存在。采用不同的氯化工艺方法和工艺条件所得产物的乙烯、氯乙烯、1，2二氯乙烯各自的含量及分布排列不同，氯化聚乙烯所呈现出来的物理性能亦不相同。此外，氯化聚乙烯不同含氯量、分子量分布也是影响其性能的重要因素。
氯化聚乙烯的特征
1)氯化聚乙烯是一种饱和橡胶，有优秀的耐热氧老化、臭氧老化、耐酸碱、化学药品性能。
2)氯化聚乙烯耐油性能优秀，其中耐ASTM1号油、ASTM2号油性能极佳，与NBR相当；耐ASTM3号油性能优良，优于CR，与CSM相当。
3)氯化聚乙烯中含有氯元素，具有极佳的阻燃性能，且有燃烧防滴下特性。其与锑系阻燃剂、氯化石蜡、Al(OH)3三者适当的比例配合可得到阻燃性能优良、成本低廉的阻燃材料。
4)氯化聚乙烯无毒，不含重金属及PAHS，其完全符合环保要求。
5)氯化聚乙烯具有高填充性能，可制得符合各种不同性能要求的产品。氯化聚乙烯的加工性能好，门尼粘度在50-100间有多种牌号可供选择。
氯化聚乙烯的拉伸性、耐候性、耐臭氧性、耐热性、耐寒性、阻燃性、颜色稳定性均为优良。在耐热、耐臭氧等方面优于氯丁橡胶。耐老化性能优于氯醚橡胶、丁腈橡胶、氯丁橡胶和氯磺化聚乙烯橡胶。具有较好的阻燃性同时能耐大多数腐蚀性介质，如高浓度的无机酸、碱和盐的溶液，但不耐强氧化剂和溶剂化作用的药品，如浓硝酸、铬酸、高氯酸和有机胺等。除上述优点外，加工性能优良，可制得表面光滑、圆整的橡胶制品。本身为洁白粉末，有良好的着色性和耐老化性，可以制成色彩艳丽并耐久的橡胶制品。
电子加速器产生的高能射线具有以下特点：(1)任何形状的聚合物与单体都可使用，可以完成化学法难以进行的反应。(2)射线能量高，穿透能力强，反应可以深入到物质内部。(3)操作简单易行，反应时间短，稳定性高。不需交联剂和引发剂，不需要进行后处理。电子加速器高能电子束利用带电粒子对材料进行辐射聚合，具有无二次污染，能够连续化生产加工等优点。为辐射硫化氯化聚乙烯发泡材料进一步的产业化发展提供了可能性。
专利200710057856.2提供了一种属于聚丙烯发泡材料及其制造方法。聚丙烯发泡材料，其组份和重量百分比含量如下：聚丙烯树脂30～97％，其它烯烃聚合物0～57％，发泡剂2～20％，助交联剂0.1～5％。制造方法是采用辐射交联方法：将混合物在110～160℃熔融共混成型，将成型物进行辐射交联，辐射剂量为10～200kGY；辐照后再经过高温发泡为成品，常压发泡温度控制在200～350℃；加压发泡温度控制在200～300℃。
专利201210125819.1提供了一种辐照交联氯化聚乙烯绝缘软电缆，该电缆包括缆芯，所述缆芯由若干根线芯绞合而成，所述线芯包括中间的镀锡铜线绞合导体以及依次设置在该导体外的导体隔离层和氯化聚乙烯绝缘层，在缆芯中的间隙填充有填充物、在缆芯外依次设置缆芯隔离层及外护层。本发明的结构满足使用条件对高电气性能，耐油、耐臭氧、耐气候、耐热、阻燃和高强度性能的要求，同时具有节能环保的功能。
本专利本项目以性能优异的氯化聚乙烯替代传统的发泡材料。以辐射硫化代替传统的橡胶硫化的方式。
发明内容
辐射硫化氯化聚乙烯发泡材料，其特征是组份和重量百分比含量如下：
氯化聚乙烯    30～97％，
其它烯烃聚合物    0～57％，
发泡剂    2～20％，
助硫化剂    0.1～5％。
本发明优选的组份和重量百分比含量如下：
氯化聚乙烯    50～80％，
其它烯烃聚合物    15～45％，
发泡剂    3～17.5％，
助硫化剂    1～3％。
根据需要，配方体系中也可加入抗氧剂、润滑剂、着色剂、填料等常见塑料助剂。
本发明所述的氯化聚乙烯发泡材料的制造方法，其特征是采用辐射硫化方法。具体方法如下：
(1)将组份按含量配比混合或先分别造粒成母料再均匀混合；
(2)将混合物在100～150℃熔融共混成型；
(3)将成型物进行辐射硫化，辐射介质包括但不限于：α射线、β射线、γ射线、X射线、高能电子束或紫外线，辐射剂量为5～60kGy；
(4)辐照后再经过高温发泡为成品，常压发泡温度控制在200～350℃；加压发泡温度控制在200～300℃。
本发明中所述的发泡材料的倍率可以通过调整发泡剂的添加量来调整，可以达到的倍率为4～36倍。
本发明采用的工艺流程为：
(1)将基体树脂与化学发泡剂、助硫化剂和其它助剂按配比均匀混合或先分别造粒成母料再均匀混合。
(2)将第(1)步的混合物熔融共混成型，可成型为片材或异型材。共混设备可用开炼机、密炼机、单螺杆挤出机或双螺杆挤出机等。为保证在成型过程稳定，共混成型温度应控制在100～150℃，优选为125～150℃。
(3)将上一步的成型物进行辐射硫化。辐射介质包括但不限于：α射线、β射线、γ射线、X射线、高能电子束或紫外线，优选为高能电子加速器的高能电子束；辐射剂量为5～60kGy，优选为10～40kGy。
(4)辐照后再经过高温发泡为产品。发泡装置可采用常压发泡装置如水平发泡炉、垂直发泡炉、盐浴发泡炉等，也可采用加压发泡装置如模压发泡设备等。常压发泡温度控制在200～350℃，优选240～310℃；加压发泡温度控制在200～300℃，优选为230～260℃。
本发明中所用的发泡剂要求分解温度在185.260℃，优选为190-250℃。包含偶氮二甲酰胺(AC)、对甲苯磺酰氨基脲(TSSC)、5.苯基四唑(5.PT)、N，N’.二亚甲基五亚甲基四胺(DNPT)中的一种或几种的混合物，优选为偶氮二甲酰胺(AC)。
本发明中所用的助硫化剂是一种二官能团或多官能团化合物，包含但不限于三羟甲基丙烷三甲基丙烯酸酯(TMPTMA)、三羟甲基丙烷三丙烯酸酯(TMPTA)、二羟甲基丙烷二甲基丙烯酸酯(DMPDMA)、异氰脲酸三烯丙酯(TAIC)、氰脲酸三烯丙酯(TAC)、1，4.丁二醇二丙烯酸酯(BDDA)、1，6一己二醇二丙烯酸酯(HDDA)中的一种或几种的混合物，优选三羟甲基丙烷三甲基丙烯酸酯(TMPTMA)。
本发明的效果：
(1)本发明所述的辐射硫化氯化聚乙烯发泡材料使用辐射方法进行硫化，可以摆脱氯化聚乙烯加热硫化时分子链易断裂的难题；
(2)本发明可以实现工业化批量生产。
具体实施方式
下面用实施例进一步描述本发明，但本发明的范围不受这些实施例的限制。
本发明实施例采用的方法如下为：
(1)将基体树脂与化学发泡剂、助硫化剂和其它助剂按配比均匀混合或先分别造粒成母料再均匀混合。
(2)将第(1)步的混合物熔融共混成型，可成型为片材或异型材。共混设备可用开炼机、密炼机、单螺杆挤出机或双螺杆挤出机等。为保证在成型过程稳定，共混成型温度应控制在100～150℃，优选为125～150℃。
(3)将上一步的成型物进行辐射硫化。辐射介质包括但不限于：α射线、β射线、γ射线、X射线、高能电子束或紫外线，优选为高能电子加速器的高能电子束；辐射剂量为5～60kGy，优选为10～40kGy。
(4)辐照后再经过高温发泡为产品。发泡装置可采用常压发泡装置如水平发泡炉、垂直发泡炉、盐浴发泡炉等，也可采用加压发泡装置如模压发泡设备等。常压发泡温度控制在200～350℃，优选240～310℃；加压发泡温度控制在200～300℃，优选为230～260℃。
本发明中所用的发泡剂要求分解温度在185.260℃，优选为190.250℃。包含偶氮二甲酰胺(AC)、对甲苯磺酰氨基脲(TSSC)、5.苯基四唑(5.PT)、N，N’一二亚甲基五亚甲基四胺(DNPT)中的一种或几种的混合物，优选为偶氮二甲酰胺(AC)。
本发明的有益效果是：1)本发明选择了一种新的发泡材料，该发泡材料具有诸多的优异性能；2)本发明使用辐射硫化橡胶发泡的方法，缩短了反应时间，简化了反应过程。

Claims (8)

1.一种辐射硫化氯化聚乙烯发泡材料，其特征在于组份和重量百分比含量如下：
氯化聚乙烯    30～97％，
其它烯烃聚合物    0～57％，
发泡剂       2～20％，
助硫化剂     0.1～5％。
2.一种辐射硫化氯化聚乙烯发泡材料，其特征在于组份和重量百分比含量如下：
氯化聚乙烯    50～80％，
其它烯烃聚合物    15～45％，
发泡剂    3～17.5％，
助硫化剂    1～3％。
3.权利要求1及权利要求2所述的辐射硫化氯化聚乙烯发泡材料，其特征在于：所述的氯化聚乙烯的氯含量为30～45％。
4.权利要求1及权利要求2所述的辐射硫化氯化聚乙烯发泡材料，其特征在于：所述的其它烯烃聚合物包括：低密度聚乙烯、高密度聚乙烯、线性低密度聚乙烯、茂金属线性低密度聚乙烯、乙烯、醋酸乙烯共聚物、聚烯烃弹性体、苯乙烯、丁二烯、苯乙烯嵌段共聚物、氢化苯乙烯、丁二烯、苯乙烯嵌段共聚物或三元乙丙橡胶中的一种或几种的混合物。
5.权利要求1及权利要求2所述的辐射硫化氯化聚乙烯发泡材料，其特征在于：所述的发泡剂分解温度在185～260℃之间，且包含偶氮二甲酰胺、对甲苯磺酰氨基脲、5一苯基四唑或N，N’一二亚甲基五亚甲基四胺中的一种或几种的混合物。
6.权利要求1及权利要求2所述的辐射硫化氯化聚乙烯发泡材料，其特征在于：所述的助硫化剂是一种二官能团或多官能团化合物，包含三羟甲基丙烷三甲基丙烯酸酯、三羟甲基丙烷三丙烯酸酯、二羟甲基丙烷二甲基丙烯酸酯、异氰脲酸三烯丙酯、氰脲酸三烯丙酯、1，4.丁二醇二丙烯酸酯或1，6.己二醇二丙烯酸酯中的一种或几种的混合物。
7.权利要求1及权利要求2所述的辐射硫化氯化聚乙烯发泡材料的制造方法，其特征在于步骤如下：
(1)将组份按配比直接混合或先分别造粒成母料再均匀混合；
(2)将混合物在100～150℃熔融共混成型；
(3)将成型物进行辐射硫化，辐射吸收剂量为10～200kGy；
(4)辐照后再经过高温发泡，常压发泡温度控制在180～350℃；加压发泡温度控制在180～300℃。
8.权利要求1及权利要求2所述的辐射硫化氯化聚乙烯发泡材料的制造方法，其特征在于：将成型物进行辐射硫化，辐射介质包括但不限于：α射线、β射线、γ射线、X射线、高能电子束或紫外线，辐射剂量为10～200kGy。
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CN107880412A (zh) * 2016-09-29 2018-04-06 青岛科技大学 一种高弹环保塑胶跑道颗粒的制备方法
CN107880410A (zh) * 2016-09-29 2018-04-06 青岛科技大学 一种微发泡预制型塑胶跑道
CN107880409A (zh) * 2016-09-29 2018-04-06 青岛科技大学 一种缓冲减震塑胶颗粒及制备方法
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CN107880411A (zh) * 2016-09-29 2018-04-06 青岛科技大学 一种微发泡环保草坪颗粒
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CN105670144A (zh) * 2016-01-28 2016-06-15 泉州三盛橡塑发泡鞋材有限公司 一种橡胶型氯化聚乙烯发泡材料及其制备方法
CN105670144B (zh) * 2016-01-28 2018-11-13 泉州三盛橡塑发泡鞋材有限公司 一种橡胶型氯化聚乙烯发泡材料及其制备方法
CN107880412A (zh) * 2016-09-29 2018-04-06 青岛科技大学 一种高弹环保塑胶跑道颗粒的制备方法
CN107880410A (zh) * 2016-09-29 2018-04-06 青岛科技大学 一种微发泡预制型塑胶跑道
CN107880409A (zh) * 2016-09-29 2018-04-06 青岛科技大学 一种缓冲减震塑胶颗粒及制备方法
CN107880403A (zh) * 2016-09-29 2018-04-06 青岛科技大学 一种耐老化环保草坪颗粒
CN107880411A (zh) * 2016-09-29 2018-04-06 青岛科技大学 一种微发泡环保草坪颗粒
CN107880412B (zh) * 2016-09-29 2021-02-09 青岛科技大学 一种高弹环保塑胶跑道颗粒的制备方法
CN113105683A (zh) * 2021-04-09 2021-07-13 杭州科佳新材料股份有限公司 一种耐油超柔软聚乙烯材料及其制备方法

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