CN107200946A - 一种氯磺化聚乙烯微孔发泡材料及其制备方法 - Google Patents
一种氯磺化聚乙烯微孔发泡材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种氯磺化聚乙烯橡胶微孔发泡材料及其制备方法,其配方如下:氯磺化聚乙烯100份,稳定剂1-6份,填料0-100份,增塑剂0-30份,防老剂1-3份,硫化剂0.5-20份,促进剂5-12份;并以上述配方提供了制备方法:将氯磺化聚乙烯橡胶与稳定剂、填料、增塑剂、防老剂、硫化剂、促进剂混炼均匀,下片、成型、预硫化后,放入发泡装置中,制备得到氯磺化聚乙烯橡胶发泡材料。本发明提供的发泡材料质轻,微孔,力学性能较好,且无毒环保,可广泛用于耐热、耐辐射电缆护套、橡胶地板地垫、鞋材、塑胶跑道、汽车、航空航天等各种领域。
Description
技术领域
本发明属于高分子材料领域,具体涉及一种氯磺化聚乙烯微孔发泡材料及其制备方法。
背景技术
氯磺化聚乙烯是以聚乙烯主原料经氯化、氯磺化反应而制得的具有高饱和化学结构的含氯特殊弹性体材料,属高性能品质的特种橡胶品种。其外观呈白色或乳白色弹性材料,有热塑性。由于分子结构中含有氯磺酰活性基团,故表现出高活性,而尤以耐化学介质腐蚀、抗臭氧氧化及耐油侵蚀、阻燃等性能突出,还具有抗候变、耐热、抗离子辐射、耐低温、抗磨蚀和电绝缘性及优异的机械性能。CSM在电线电缆、防水卷材、汽车工业等领域已得到广泛应用,成为常用的特种橡胶。
CSM发泡材料具有质量轻、性能优异、经济实用、性能特殊等优点,国内外对此展开了大量的研究工作。CSM在我国就应用来说相对较少,用于制造发泡胶鞋的工艺仍处在起步阶段,而在汽车零部件等方面的应用则仍属于开发阶段。因此,我国还需要加大氯磺化聚乙烯在应用方面的研究投资,发展出新的应用方式,不断的扩大其所应用的范围。CSM发泡鞋材在目前制鞋业中算是比较高档的制作方式,一般用于高档运动鞋。如NIKE,ADI,ASICS等,成本比较高。最早使用CSM发泡用于鞋材是台湾的宝成集团。
发明内容
本发明的目的是提供一种氯磺化聚乙烯微孔发泡材料及其制备方法,本发明所制备的氯磺化聚乙烯橡胶的微孔发泡材料。通过调整硫化剂用量、预硫化时间以及饱和压力和时间,制备得到不同密度的微孔发泡材料,可用于发泡地垫、鞋材、电线电缆护套等,还可用于减震、吸水、耐磨材料及密封材料。
一种氯磺化聚乙烯微孔发泡材料及其制备方法,其配方如下:氯磺化聚乙烯100份,稳定剂1-6份,填料0-100份,增塑剂0-30份,防老剂0.5-1份,硫化剂0.5-20份,促进剂5-12份。
填料为炭黑、白炭黑、碳酸钙、高岭土中的一种或多种;
增塑剂为邻苯二甲酸二辛脂(DOP)、己二酸二异辛酯(DIOA)、氯化石蜡油中的一种或多种;
防老剂为防老剂2246或防老剂1010;
硫化剂为高活性氧化镁,过氧化二异丙苯(DCP)中的一种。。
硫化促进剂为季戊四醇(PER)、氧化锌(ZnO)、四硫化双五亚甲基秋兰姆(DPTT)、四甲基二硫代秋兰姆(TMTD)、三烯丙基异氰脲酸酯(TAIC)、氧化铅(PbO)中的一种或多种。
一种氯磺化聚乙烯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防老剂、硫化剂和促进剂,得到混炼胶。。
2)预硫化
(1)挤出成型预硫化
将混炼胶压片,制得片材,然后放入100-160℃的烘道进行预硫化,预硫化时间为1min-45min,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1-30min,之后将胶料从模具中拿出,得到预硫化材料。
3)微孔发泡
预硫化好的样品放入高压反应釜中,通入物理发泡剂并升温、加压,当物理发泡剂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。其中物理发泡剂为CO2,N2、丁烷、戊烷中一种或几种。
升温法:将预硫化材料装入高压釜内,然后密封,控制反应釜温度为0-80℃,将物理发泡剂注入高压釜内,使压力达到5-60MPa,恒压饱和4-72h。然后迅速卸压至常压,最后在130-180℃温度烘箱或平板硫化机加热样品0-10min发泡后冷却,得到发泡材料。
降压法:将预硫化材料装入高压釜内,然后密封,控制反应釜温度为80-160℃,将物理发泡剂注入高压釜内,使压力达到5-60MPa,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;
将微孔发泡材料二次硫化、定型,硫化时间为10-60min。
其中,步骤4)中的所述硫化方式为热空气硫化、微波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:
CSM发泡橡胶因其含有极性氯原子和氯磺酰基的饱和链结构,具有优异的耐化学药品性、耐臭氧性、难燃性能,具有良好的电绝缘性、阻燃性、耐摩擦性和机械损伤性;且本发泡材料质轻、微孔、力学性能较好,本发泡工艺中不使用发泡剂,无发泡剂残留,可用于室内装饰材料以及鞋材等对环保要求较高的产品。
附图说明
图1本发明制备方法中,实施例1的氯磺化聚乙烯发泡材料的扫描电镜图;
图2本发明制备方法中,实施例2的氯磺化聚乙烯发泡材料的扫描电镜图;
图3本发明制备方法中,实施例3的氯磺化聚乙烯发泡材料的扫描电镜图;
图4本发明制备方法中,实施例4的氯磺化聚乙烯发泡材料的扫描电镜图。
具体实施方式
实施例1
氯磺化聚乙烯100份,稳定剂2份,填料10份,防老剂1份,硫化剂4份,促进剂6份。
填料为炭黑;防老剂为4010NA;硫化剂为高活性氧化镁;硫化促进剂为季戊四醇、TAIC、DPTT并用。
将配方中各种原料按所需重量份称好后投入密炼机中,密炼机温度为90℃,混炼时间为5min,之后将其放入开炼机上精炼5min,制得混炼胶。之后将混炼胶在开炼机下片,然后用平板硫化机将胶片在140℃下预硫化5min,之后取出样品片,放入发泡装置中,装置设置温度130℃,通入CO2气体至压力为16Mpa,饱和1h后取出,之后在170℃烘箱中二次硫化20min,冷却得到微孔发泡样品。
实施例2
氯磺化聚乙烯100份,稳定剂2份,填料20份,防老剂1份,硫化剂4份,促进剂6份。
填料为高岭土,1250目;防老剂为4010NA并用;硫化剂为高活性氧化镁;
硫化促进剂为季戊四醇、TAIC、DPTT并用。
将配方中各种原料按所需重量份称好后投入密炼机中,密炼机温度为90℃,混炼时间为5min,之后将其放入开炼机上精炼5min,制得混炼胶。之后将混炼胶在开炼机下片,然后用平板硫化机将胶片在130℃下预硫化10min,之后取出样品片,放入发泡装置中,装置设置温度140℃,通入CO2气体至压力为16Mpa,饱和2h后取出,之后在170℃烘箱中二次硫化30min,冷却得到微孔发泡样品。
实施例3
氯磺化聚乙烯100份,稳定剂2份,填料15份,增塑剂2份,防老剂1份,硫化剂3.3份,促进剂5.5份。
填料为白炭黑;增塑剂为DIOA;防老剂为防老剂2246;硫化剂为高活性氧化镁;硫化促进剂为季戊四醇、TAIC、ZnO并用。
将配方中各种原料按所需重量份称好后投入密炼机中,密炼机温度为100℃,混炼时间为7min,之后将其放入开炼机上精炼5min,制得混炼胶。之后将混炼胶在开炼机下片,然后用平板硫化机将胶片在150℃下预硫化12min,之后取出样品片,放入发泡装置中,装置设置温度为室温,通入N2气体至压力为16Mpa,饱和48h后取出,之后在170℃烘箱中二次硫化25min,冷却得到微孔发泡样品。此配方得到的微孔发泡样品可以用于鞋中底发泡材料部分。
实施例4
氯磺化聚乙烯100份,稳定剂2份,填料0份,防老剂1份,硫化剂8份,促进剂6份。
防老剂为防老剂2246;硫化剂为高活性氧化镁;硫化促进剂为季戊四醇、DPTT并用。
将配方中各种原料按所需重量份称好后投入密炼机中,密炼机温度为95℃,混炼时间为3min,之后将其放入开炼机上精炼5min,制得混炼胶。之后将混炼胶在开炼机下片,然后用平板硫化机将胶片在120℃下预硫化15min,之后取出样品片,放入发泡装置中,装置设置温度140℃,通入CO2气体至压力为16Mpa,饱和4h后取出,之后在170℃烘箱中二次硫化35min,冷却得到微孔发泡样品。
按常规方法对上述实施例所制得的氯磺化聚乙烯发泡材料的各项性能指标进行检测,实施例1-4检测结果见表1
检测项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 |
发泡后密度/g·cm-3 | 0.618 | 0.768 | 0.610 | 0.260 |
硬度(邵氏A) | 49 | 55 | 43 | 26 |
拉伸强度/MPa | 8.29 | 4.57 | 3.85 | 2.53 |
扯断伸长率/% | 508.12 | 385.25 | 326.85 | 438.30 |
100%定伸/MPa | 1.25 | 1.62 | 1.50 | 0.42 |
以上所述仅为本发明的一实施例,并不限制本发明,凡采用等同替换或等效变换的方式所获得的技术方案,均落在本发明的保护范围内。
Claims (8)
1.一种氯磺化聚乙烯微孔发泡材料,其特征在于:其配方如下:氯磺化聚乙烯100份,稳定剂1-6份,填料0-100份,增塑剂0-30份,防老剂0.5-1份,硫化剂0.5-20份,促进剂5-12份。
2.根据权利要求书1所述的一种氯磺化聚乙烯微孔发泡材料,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。
3.根据权利要求书1所述的一种氯磺化聚乙烯微孔发泡材料,其特征在于,所述增塑剂为邻苯二甲酸二辛脂(DOP)、己二酸二异辛酯(DIOA)、氯化石蜡油中的一种或多种。
4.根据权利要求书1所述的一种氯磺化聚乙烯微孔发泡材料,其特征在于,所述防老剂为防老剂2246或防老剂1010.。
5.根据权利要求书1所述的一种氯磺化聚乙烯微孔发泡材料,其特征在于,所述硫化剂为高活性氧化镁,过氧化二异丙苯(DCP)中的一种。
6.根据权利要求书1所述的一种氯磺化聚乙烯微孔发泡材料,其特征在于,所述硫化促进剂为季戊四醇(PER)、氧化锌(ZnO)、四硫化双五亚甲基秋兰姆(DPTT)、四甲基二硫代秋兰姆(TMTD)、三烯丙基异氰脲酸酯(TAIC)、氧化铅(PbO)中的一种或多种。
7.一种氯磺化聚乙烯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防老剂、硫化剂和促进剂,得到混炼胶。
2)预硫化
(1)挤出成型预硫化
将混炼胶压片,制得片材,然后放入100-160℃的烘道进行预硫化,预硫化时间为1min-45min。
(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1-30min,之后将胶料从模具中拿出,得到预硫化材料。
3)微孔发泡
预硫化好的样品放入高压反应釜中,通入物理发泡剂并升温、加压,使得物理发泡剂溶于预硫化胶中后,采用快速降压法、或快速升温法,制得微孔材料。其中物理发泡剂为CO2,N2、丁烷、戊烷中的一种或几种。
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,反应釜温度为室温-80℃,用高压泵将物理发泡剂注入高压釜内,使压力达到5-60MPa,恒压饱和4-72h。然后迅速卸压至常压,最后在130-180℃温度的烘箱或平板硫化剂加热样品0-10min发泡后冷却,得到发泡材料。
降压法:将预硫化材料装入高压釜内,密封,控制反应釜温度为80-160℃,用高压泵将物理发泡剂注入高压釜内,使压力达到5-60MPa,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;
将微孔发泡材料二次硫化、定型,硫化时间为10-60min。
8.根据权利要求书7所述的一种氯磺化聚乙烯微孔发泡材料,其特征在于,步骤4)中的所述硫化方式为热空气硫化、微波辐射交联或者红外辐射交联。
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