CN107200941A - 一种氯化聚乙烯弹性体微孔发泡材料及其制备方法 - Google Patents

一种氯化聚乙烯弹性体微孔发泡材料及其制备方法 Download PDF

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CN107200941A
CN107200941A CN201610150884.8A CN201610150884A CN107200941A CN 107200941 A CN107200941 A CN 107200941A CN 201610150884 A CN201610150884 A CN 201610150884A CN 107200941 A CN107200941 A CN 107200941A
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chlorinated polyethylene
parts
polyethylene elastomer
foam material
microcellular foam
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张振秀
张昕
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Qingdao University of Science and Technology
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Abstract

本发明公开了一种氯化聚乙烯弹性体微孔发泡材料及其制备方法，其配方如下：氯化聚乙烯弹性体100份，填料0-300份，增塑剂0-60份，防老剂1-3份，硫化剂1-5份，硫化促进剂0-5份，活性剂0.5-2份，并以上述配方提供了制备方法。本发明提供的氯化聚乙烯弹性体微孔发泡材料具有优异的耐油性、耐热性、抗臭氧性、耐候性，且采用超临界发泡方法，制备得到的材料无毒、环保、无污染。

Description

一种氯化聚乙烯弹性体微孔发泡材料及其制备方法
技术领域
本发明涉及高分子材料领域，尤其涉及一种氯化聚乙烯弹性体微孔发泡材料及其制备方法。
背景技术
橡胶发泡材料符合国家倡导的低碳环保的要求，不仅能够节约能源降低成本，而且具有较高的性价比和特殊功能性的应用，在我们的日常生活、生产、交通、建筑、医疗卫生方面应用广泛。因此研究开发新型的橡胶发泡材料以及应用领域得到人们重视，而且随着科技的发展和人们安全意识的提高，在评价、选择材料性能时，除了考虑其基本的力学参数外，那些具有较高性能和较低价格的高性价比产品，逐渐的被人们研究利用，以达到较好的效果。
氯化聚乙烯(CM)是一种新型的高分子弹性体材料，分子中不含对热、化学性不稳定的双键，而且氯原子是沿聚乙烯无规结合，是一种较为稳定的橡胶，其主要特性如下：优良的耐候性和自由着色性；优良的耐臭氧性。良好的耐老化性；优异的阻燃性；良好的耐油性；出色的电性能及电气特性，可以高填充以降低成本，耐龟裂、耐磨性及机械损伤等。CM发泡产品也具有优良的性能，包括制品成型、泡孔结构、弹性、柔顺性、压变型等，可以单独使用或替代目前橡胶发泡制品。CM可以代替丁苯橡胶发泡材料，来提高发泡材料的耐候性；CM发泡材料也可以作为地垫使用，而具有良好的着色行；低密度的CM发泡材料还可以代替目前传统的NBR/PVC保温材料，而之后还将开发出更多CM发泡材料的应用领域。
发明内容
本发明的目的是提供一种氯化聚乙烯橡胶微孔发泡材料及其制备方法，本发明采用，还可用于减震、吸水、耐磨材料及密封材料。
一种氯化聚乙烯弹性体微孔发泡材料，其配方如下：氯化聚乙烯弹性体100份，稳定剂4-10份，填料0-300份，增塑剂0-60份，防老剂1-3份，硫化剂1-5份，硫化促进剂0-5份，活性剂0.5-2份。
其中，所述氯化聚乙烯弹性体为氯化聚乙烯或氯化聚乙烯与聚氯乙烯混合物或者氯化聚乙烯与氯化聚氯乙烯混合物。
其中，所述稳定剂为硬脂酸，硬脂酸锌，硬脂酸钙，硬脂酸铅中的任一种。
其中，所述填料为炭黑、白炭黑、碳酸钙、高岭土中的一种或多种。
其中，所述增塑剂为氯化石蜡油、环烷油、DOP中的一种或多种。
其中，所述防老剂为抗紫外老化剂UV-531和抗氧剂1010并用。
其中，所述硫化剂为为过氧化二异丙苯，双(叔丁过氧基)二异丙苯或2,5-二甲基2,5-双(叔丁过氧基)己烷中的任一种。
其中，所述硫化促进剂为三烯丙基异三聚氰酸酯(TAIC)、N，N'-间苯撑双马来酰亚胺(HVA-2)中的一种或多种。
一种氯化聚乙烯弹性体微孔发泡材料的制备方法，其步骤如下：
1)混炼胶制备
(1)按重量分别称取所需生胶、填料及增塑剂；(2)密炼机温度设置为60-100℃，转速为40-60rpm，将生胶、填料、增塑剂投入密炼机中，混炼均匀，控制排胶温度低于120℃；(3)混炼胶排胶、压片、冷却停放12h；(4)将停放后的胶料在开炼机上加硫化体系。
2)预硫化
(1)挤出成型预硫化
将混炼胶切片，投入挤出机中，挤出机温度设置为80-120℃，挤出板材、管材或者条状，之后在100-180℃的烘道进行预硫化，预硫化时间为1min-15min，硫化方式为热空气硫化、微波辐射交联或者红外辐射交联等。
(2)模压成型预硫化
将混炼胶放入所需模具中，热压机压力为5-10MPa，温度100-180℃，预硫化时间为1-12min，之后将胶料从模具中拿出，得到预硫化材料。
3)超临界发泡
预硫化好的样品放入高压反应釜中，通入超临界流体并升温、加压使其变为超临界状态，当超临界流体在预硫化物胶中达到饱和后，采用快速降压法、或快速升温法，制得微孔材料。其中超临界流体为CO2，N2、丁烷、戊烷等。
升温法：将预硫化材料装入高压釜内，先用少量CO2吹洗2～3min，然后密封，反应釜温度为40-140℃，用超临界注气系统将超临界流体注入高压釜内，使压力达到5-30MPa，恒压饱和0.5-4h。然后迅速卸压至常压，最后在160-250℃温度的油浴中加热样品一定时间使之发泡后放入水中冷却，得到发泡材料。
降压法：将预硫化材料装入高压釜内，先用少量CO2吹洗2～3min，然后密封，反应釜温度为40-140℃，用超临界注气系统将超临界流体注入高压釜内，使压力达到5-30MPa，恒压饱和0.5-4h。然后迅速卸压至常压，卸压时间为0-80s，得到发泡材料。
4)二次硫化、定型；
将微发泡材料放入另一烘道中二次硫化、定型，其中烘道温度为120-220℃，硫化时间为10-60min，硫化方式为热空气硫化、微波辐射交联或者红外辐射交联等。
其中，步骤4)中的所述硫化方式为热空气硫化、电子束辐射交联或者红外辐射交联。
与现有技术相比，本发明具有以下有益效果：
1.氯化聚乙烯弹性体微孔发泡材料具有优异的耐油性、耐热性、抗臭氧性、耐候性。
2.本发明采用超临界发泡方法，制备得到的材料无毒、环保、无污染。
3.本发明提供的材料具有优异的阻燃性能。
附图说明
图1本发明制备方法中，实施例1的扫描电镜图；
图2本发明制备方法中，实施例2的扫描电镜图；
图3本发明制备方法中，实施例3的扫描电镜图。
具体实施方式
实施例1
氯化聚乙烯弹性体100份，填料10份，防老剂1份，硫化剂0.6份。
其中，所述氯化聚乙烯弹性体为氯化聚乙烯；所述填料为碳酸钙；所述防老剂为抗氧剂1010；所述硫化剂为BIPB。
密炼机温度设定为90℃，将氯化聚乙烯投入密炼机中，依次加入填料、防老剂、硫化剂等，控制排胶温度低于120℃，混炼6min，出料、下片，得到混炼胶。然后用平板硫化机将胶片在150℃下预硫化8min，之后取出样品片，放入发泡装置中，装置设置温度80℃，通入N2气体至压力为20Mpa，饱和6h后取出，之后在165℃烘箱中二次硫化10min，冷却得到氯化聚乙烯弹性体微孔发泡材料。
实施例2
氯化聚乙烯弹性体100份，稳定剂6份，填料100份，增塑剂50份，防老剂1份，硫化剂0.8份，硫化促进剂0.2份。
其中，所述氯化聚乙烯弹性体为氯化聚乙烯/聚氯乙烯共混物，其配比为80/20；所述稳定剂为硬脂酸锌；所述填料为碳酸钙；所述增塑剂为DOP，所述防老剂为抗氧剂1010；所述硫化剂为2,5-二甲基2,5-双(叔丁过氧基)己烷，所述硫化促进剂为HVA-2。
密炼机温度设定为165℃，先将聚氯乙烯投入密炼机中，加入稳定剂，混炼3min后，加入氯化聚乙烯，继续混炼2min，然后依次加入填料、防老剂、增塑剂，出料，制得母炼胶，之后在开炼机上加入硫化剂及硫化促进剂，精炼后下片值得混炼胶。将混炼胶裁片，投入挤出机中，挤出机温度设置为100-120℃，挤出条状，然后通过170℃烘道，时间为5min，之后将胶条盘好，放入发泡装置中，装置设置温度120℃，通入N2气体至压力为20Mpa，饱和2h后取出，得到氯化聚乙烯弹性体微孔发泡胶条。
实施例3
氯化聚乙烯弹性体100份，稳定剂8份，填料50份，增塑剂30份，防老剂1份，硫化剂1份，硫化促进剂0.3份。
其中，所述氯化聚乙烯弹性体为氯化聚乙烯/氯化聚氯乙烯共混物，其配比为85/15；所述稳定剂为硬脂酸锌；所述填料为高岭土；所述增塑剂为DOP，所述防老剂为抗氧剂1010；所述硫化剂为2,5-二甲基2,5-双(叔丁过氧基)己烷，所述硫化促进剂为HVA-2。
密炼机温度设定为180℃，先将氯化聚氯乙烯投入密炼机中，加入稳定剂，混炼3min后，加入氯化聚乙烯，继续混炼2min，然后依次加入填料、防老剂、增塑剂，出料，制得母炼胶，之后在开炼机上加入硫化剂及硫化促进剂，精炼后下片制得混炼胶。将混炼胶裁片，投入挤出机中，挤出机温度设置为100-120℃，挤出板材，然后通过电子束辐射预硫化，之后将预硫化板材放入发泡装置中，装置设置温度100℃，通入N2气体至压力为18Mpa，饱和2.5h后取出，得到氯化聚乙烯弹性体微孔发泡板材。
将上述实施例1至实施例3的产品按测试标准制得样品，并对其进行检测，其检测结果见表1
检测项目 实施例1 实施例2 实施例3
硬度(邵A) 38 45 46
密度/g·cm-3 0.374 0.528 0.679
拉伸强度/MPa 1.83 2.79 2.94
氧指数/％ 25 30 32
最后应说明的是：以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管前述实施例对本发明进行了详细的说明，本领域的普通技术人员依然可以对前述各实施例的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。

Claims (10)

1.一种氯化聚乙烯弹性体微孔发泡材料，其配方如下：氯化聚乙烯弹性体100份，稳定剂4-10份，填料0-300份，增塑剂0-60份，防老剂1-3份，硫化剂1-5份，硫化促进剂0-5份，活性剂0.5-2份。
2.根据权利要求书1所述的一种氯化聚乙烯弹性体微孔发泡材料，其特征在于，所述氯化聚乙烯弹性体为氯化聚乙烯或氯化聚乙烯与聚氯乙烯混合物或者氯化聚乙烯与氯化聚氯乙烯混合物。
3.根据权利要求书1所述的一种氯化聚乙烯弹性体微孔发泡材料，其特征在于，所述硬脂酸，硬脂酸锌，硬脂酸钙，硬脂酸铅中的任一种。
4.根据权利要求书1所述的一种氯化聚乙烯弹性体微孔发泡材料，其特征在于，所述填料为炭黑、白炭黑、碳酸钙、高岭土中的一种或多种。
5.根据权利要求书1所述的一种氯化聚乙烯弹性体微孔发泡材料，其特征在于，所述增塑剂为氯化石蜡油、环烷油、DOP中的一种或多种。
6.根据权利要求书1所述的一种氯化聚乙烯弹性体微孔发泡材料，其特征在于，所述防老剂为抗紫外老化剂UV-531和抗氧剂1010并用。
7.根据权利要求书1所述的一种氯化聚乙烯弹性体微孔发泡材料，其特征在于，所述硫化剂为为过氧化二异丙苯，双(叔丁过氧基)二异丙苯或2,5-二甲基2,5-双(叔丁过氧基)己烷中的任一种。
8.根据权利要求书1所述的一种氯化聚乙烯弹性体微孔发泡材料，其特征在于，所述硫化促进剂为三烯丙基异三聚氰酸酯(TAIC)、N，N'-间苯撑双马来酰亚胺(HVA-2)中的一种或多种。
9.一种氯化聚乙烯弹性体微孔发泡材料的制备方法，其特征在于：其步骤如下：
1)混炼胶制备
(1)按重量分别称取所需生胶、填料及增塑剂；(2)密炼机温度设置为60-100℃，转速为40-60rpm，将生胶、填料、增塑剂投入密炼机中，混炼均匀，控制排胶温度低于120℃；(3)混炼胶排胶、压片、冷却停放12h；(4)将停放后的胶料在开炼机上加硫化体系。
2)预硫化
(1)挤出成型预硫化
将混炼胶切片，投入挤出机中，挤出机温度设置为80-120℃，挤出板材、管材或者条状，之后在100-180℃的烘道进行预硫化，预硫化时间为1min-15min，硫化方式为热空气硫化、微波辐射交联或者红外辐射交联等。
(2)模压成型预硫化
将混炼胶放入所需模具中，热压机压力为5-10MPa，温度100-180℃，预硫化时间为1-12min，之后将胶料从模具中拿出，得到预硫化材料。
3)超临界发泡
预硫化好的样品放入高压反应釜中，通入超临界流体并升温、加压使其变为超临界状态，当超临界流体在预硫化物胶中达到饱和后，采用快速降压法、或快速升温法，制得微孔材料。其中超临界流体为CO2，N2、丁烷、戊烷等。
升温法：将预硫化材料装入高压釜内，先用少量CO2吹洗2～3min，然后密封，反应釜温度为40-140℃，用超临界注气系统将超临界流体注入高压釜内，使压力达到5-30MPa，恒压饱和0.5-4h。然后迅速卸压至常压，最后在160-250℃温度的油浴中加热样品一定时间使之发泡后放入水中冷却，得到发泡材料。
降压法：将预硫化材料装入高压釜内，先用少量CO2吹洗2～3min，然后密封，反应釜温度为40-140℃，用超临界注气系统将超临界流体注入高压釜内，使压力达到5-30MPa，恒压饱和0.5-4h。然后迅速卸压至常压，卸压时间为0-80s， 得到发泡材料。
4)二次硫化、定型；
将微发泡材料放入另一烘道中二次硫化、定型，其中烘道温度为120-220℃，硫化时间为10-60min。
10.根据权利要求书8所述的一种氯化聚乙烯弹性体微孔发泡材料的制备方法，其特征在于，步骤4)中的所述硫化方式为热空气硫化、电子束辐射交联或者红外辐射交联。
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