CN107200878B - 一种反式聚异戊二烯及其与橡胶并用微孔材料及其制备方法 - Google Patents
一种反式聚异戊二烯及其与橡胶并用微孔材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种反式聚异戊二烯及其与橡胶并用微孔发泡材料及其制备方法,其配方如下:反式聚异戊二烯与橡胶共混材料100份,填料0‑100份,增塑剂0‑50份,活性剂2‑3份,硫化剂0.5‑4份,硫化助剂1‑8份,发泡剂0‑12份,防老剂0.5‑2份。本发明利用反式聚异戊二烯常温下有固定形变且长期保持相对高强度、高冲击性能及耐磨性能,通过与橡胶并用制得发泡材料,既保持了反式聚异戊二烯橡胶的相对大的硬度及高冲击性能和耐磨性,又有橡胶相的弹性,并且通过发泡工艺增强其减震效果,提高阻尼性能,保持舒适性,可广泛作为运动鞋、皮鞋等鞋底材料,也可代替石膏用作医用夹板固定材料。
Description
技术领域
本发明高分子材料领域,具体涉及一种反式聚异戊二烯及其与橡胶并用微孔发泡材料及其制备方法,此材料可用于鞋材、运动康复护具等。
背景技术
反式-1,4-聚异戊二烯(TPI)化学组成与异戊橡胶(IR)和天然橡胶(NR)完成相同。由于分子链中的双键结构为反式构型,分子链具有较好的柔顺性,使其成为优良的弹性体。TPI具有反式结构并且有较高的有序性,使其易于有序聚集而结晶,以更类似塑料的面貌出现;而它又是柔性链,其玻璃化温度基本与天然橡胶接近。TPI不结晶,就可能变成弹性体,因此考虑到TPI单独使用性能的局限性,与其他材料并用共混阻止TPI的结晶性能,可以制备弹性体材料,这是TPI应用的另一有利途径。TPI可以采用传统硫黄硫化体系进行硫化,硫化过程有明显的三阶段特性:零交联阶段,低交联阶段和临界交联阶段。零交联阶段作为低熔点塑料制作医用“石膏”绷带、夹板、矫形部件、假肢等;低交联阶段作为硬质热刺激弹性体,用作热刺激型形状记忆材料;临界交联阶段作为柔软的弹性体,可用作橡胶制品。现阶段对TPI的研究大多集中在轮胎工业领域,而TPI的滚动阻力低、动态生热低、动态疲劳性好等特点正好是减震制品所需要的。同时,TPI与NR,SBR,BR等通用橡胶有共混硫化性能,因此TPI与各种橡胶并用得到长足发展。顺丁橡胶(BR)也为结晶性橡胶,但结晶能力不强,所以自补强能力较小。而其弹性好、耐磨性强,其在无补强填料填充时,硫化胶的拉伸强度低,基本无实用价值,因此很少单独使用,通常是与其他弹性体并用。同时TPI也可制作发泡材料,TPI发泡材料较TPI硫化胶具有更高的弹性,抗变形能力强,可用作医用夹板、护肘等固定材料,也可以用于防滑垫等家居用品。目前利用TPI为基体橡胶做发泡材料鲜有报道。
发明内容
本发明的目的是提供一种反式聚异戊二烯及其与橡胶并用微孔发泡材料及其制备方法,本发明通过化学方法和超临界方法制备不同的反式聚异戊二烯与橡胶并用微孔发泡材料,此种材料可用来制作家居防滑垫、鞋材、运动康复护具等。
一种反式聚异戊二烯与橡胶并用微孔发泡材料及其制备方法,其配方如下:反式聚异戊二烯与橡胶共混材料100份,填料0-100份,增塑剂0-50份,活性剂2-3份,硫化剂0.5-4份,硫化助剂1-8份,发泡剂0-12份,防老剂0.5-2份。其中填料为炭黑、白炭黑、碳酸钙、滑石粉、短纤维中的一种或多种;增塑剂为石蜡油、邻苯二甲酸二辛脂、癸二酸二辛酯中的一种;活性剂为硬脂酸、硬脂酸锌、氧化锌中的一种或多种。硫化剂为硫磺、过氧化异丙苯中的一种;硫化助剂为N-叔丁基-2苯度并噻唑次磺酰胺、2,2’-二硫代二苯并噻唑硬脂(TAIC)中的一种或多种;防老剂为防老剂1010、防老剂264中的任一种。
其中,所述反式聚异戊二烯与橡胶共混材料为反式聚异戊二烯(TPI)0-100份;顺丁橡胶(BR)0-40份;丁苯橡胶(SBR)0-20份;1,3聚丁二烯橡胶0-30份。
其中,所述发泡材料的制备方法包括化学发泡和超临界发泡。
其中,所述化学发泡配方为:反式聚异戊二烯与橡胶共混材料100份,填料0-100份,增塑剂0-50份,活性剂2-3份,硫化剂1-4份,硫化助剂3-8份,发泡剂0-12份,防老剂0.5-2份。
制备方法如下:
1)混炼胶制备
密炼机温度设定为70-130℃,将TPI橡胶以及并用材料投入密炼机中,加入填料、活性剂等,混炼5-6min,出料。在开炼机上加入硫化剂、硫化助剂、发泡剂,混炼4-5min,最后调整辊距,下片出料,得到混炼胶。
2)硫化发泡
模压发泡工艺,将混炼胶置入模具,压力10-20MPa,温度150-180℃,时间3-15min,采用跳模发泡法,即将称量好的胶片装入到模具内,在规定的时间、压力和温度下饱和后,打开模具得到发泡板材,室温下冷却,制得发泡材料。
其中,所述超临界发泡配方为:反式聚异戊二烯与橡胶共混材料100份,填料0-100份,增塑剂0-50份,活性剂2-3份,硫化剂0.5-4份,硫化助剂3-8份,防老剂0.5-2份。
制备方法如下:
1)混炼胶制备
密炼机温度设定为70-130℃,将TPI橡胶以及并用材料投入密炼机中,加入填料、活性剂等,混炼5-6min,出料。在开炼机上加入硫化剂、硫化助剂、发泡剂,混炼4-5min,最后调整辊距,下片出料,得到混炼胶。
2)预硫化
将混炼胶挤出,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;或者将混炼胶放入所需模具中,热压机压力为5-20MPa,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)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,反应釜温度为0-160℃,将超临界流体注入高压釜内,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100-180℃温度的烘箱加热样品0-10min发泡后冷却,得到发泡材料。
其中,所述发泡剂为偶氮二甲酰胺(AC),OBSH、碳酸氢钠中的任一种。
其中,所述超临界流体为CO2,N2中一种或两种气体的混合气体。
其中,所述反式聚异戊二烯与橡胶并用微孔发泡材料可用于家居防滑垫、鞋材、运动康复护具等。
与现有技术相比,本发明具有以下有益效果:
1.发泡TPI材料相比于其他发泡橡胶材料其具有相对大的硬度,优良的耐冲击和耐磨性能。2.发泡TPI材料密度小,质量轻便,利于奔跑,保证了良好的舒适性。3、发泡TPI材料具有弹性记忆效应,材料变形后更易于恢复。4、发泡TPI材料弹性大,减震效果强。
附图说明
图1本发明制备方法中,实施例1中(1-1)化学发泡的扫描电镜图及(1-2)物理发泡的扫描电镜图;
图2本发明制备方法中,实施例2中(2-1)化学发泡的扫描电镜图及(2-2)物理发泡的扫描电镜图;
图3本发明制备方法中,实施例3中(3-1)化学发泡的扫描电镜图及(3-2)物理发泡的扫描电镜图;
具体实施方式
实施例1
化学发泡
反式聚异戊二烯100份,活性剂3份,硫化剂4份,硫化助剂6份,发泡剂12份,防老剂0.5份。
活性剂为TBBS;硫化剂为硫磺;硫化助剂为硬脂酸和氧化锌;化学发泡剂为偶氮二甲酰胺;防老剂为防老剂1010。
密炼机温度设定为80℃,将TPI投入密炼机中,混炼2min,加入活性剂、硫化剂、硫化助剂、发泡剂,混炼3min,出料,得到混炼胶。将混炼胶置入模具,压力10MPa,温度175℃,时间6min,采用跳模发泡法,得到发泡材料,其扫描电镜图片见图1的1-1。
物理发泡
反式聚异戊二烯100份,活性剂3份,硫化剂4份,硫化助剂6份,防老剂0.5份。
活性剂为TBBS;硫化剂为硫磺;硫化助剂为硬脂酸和氧化锌;防老剂为防老剂1010。
密炼机温度设定为80℃,将TPI投入密炼机中,混炼2min,加入活性剂、硫化剂、硫化助剂、混炼3min,出料,得到混炼胶。将混炼胶置入模具,压力10MPa,温度160℃,时间6min进行预硫化;将成型并预硫化的样品放入高压釜中,通先用氮气清扫高压釜内空气1分钟后,通入氮气并加压到20MPa,温度130℃,饱和3h后以20MPa/min的速度释放压力,样品取出并冷却,得到微孔发泡TPI材料,其扫描电镜图片见图1的1-2。
实施例2
化学发泡
TPI 60份,BR 20份,SBR 20份;活性剂2份,硫化剂3份,硫化助剂5份,发泡剂6份,防老剂0.5份。
活性剂为TBBS;硫化剂为硫磺;硫化助剂为硬脂酸和氧化锌;发泡剂为偶氮二甲酰胺;防老剂为防老剂1010。
密炼机温度设定为80℃,将橡胶投入密炼机中,混炼2min,加入活性剂、硫化剂、硫化助剂、发泡剂,混炼3min,出料,得到混炼胶。将混炼胶置入模具,压力10MPa,温度165℃,时间12min,采用跳模发泡法,得到发泡材料,其扫描电镜图片见图2的2-1。
物理发泡
TPI 60份,BR 20份,SBR 20份;活性剂2份,硫化剂3份,硫化助剂5份,发泡剂6份,防老剂0.5份。
活性剂为TBBS;硫化剂为硫磺;硫化助剂为硬脂酸和氧化锌;防老剂为防老剂1010。
密炼机温度设定为80℃,将TPI、BR及SBR投入密炼机中,混炼2min,加入活性剂、硫化剂、硫化助剂、混炼3min,出料,得到混炼胶。将混炼胶置入模具,压力10MPa,温度160℃,时间6min进行预硫化;将成型并预硫化的样品放入高压釜中,通先用氮气清扫高压釜内空气1分钟后,通入氮气并加压到20MPa,温度140℃,饱和3h后以20MPa/min的速度释放压力,样品取出并冷却,得到微孔发泡TPI/BR/SBR共混胶微孔发泡材料,其扫描电镜图片见图2的2-2。
实施例3
化学发泡
TPI 40份,BR 20份;SBR 20份;PB 20份,活性剂2份,硫化剂4份,硫化助剂4份,发泡剂8份,防老剂1份。
活性剂为TBBS;硫化剂为硫磺;硫化助剂为硬脂酸和氧化锌;发泡剂为AC;防老剂为防老剂264。
密炼机温度设定为80℃,将橡胶投入密炼机中,混炼2min,加入活性剂、硫化剂、硫化助剂、发泡剂,混炼3min,出料,得到混炼胶。将混炼胶置入模具,压力10MPa,温度160℃,时间15min,采用跳模发泡法,得到发泡材料,其扫描电镜图片见图3的3-1。
物理发泡
TPI 40份,BR 20份;SBR 20份;PB 20份,活性剂2份,硫化剂4份,硫化助剂4份,防老剂1份。
活性剂为TBBS;硫化剂为硫磺;硫化助剂为硬脂酸和氧化锌;防老剂为防老剂264。
密炼机温度设定为80℃,将TPI、BR、PB及SBR投入密炼机中,混炼2min,加入活性剂、硫化剂、硫化助剂、混炼3min,出料,得到混炼胶。将混炼胶置入模具,压力10MPa,温度160℃,时间6min进行预硫化;将成型并预硫化的样品放入高压釜中,通先用氮气清扫高压釜内空气1分钟后,通入氮气并加压到25MPa,温度130℃,饱和3h后以20MPa/min的速度释放压力,样品取出并冷却,得到微孔发泡TPI/BR/SBR共混胶微孔发泡材料,其扫描电镜图片见图3的3-2。
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 (2)
1.一种反式聚异戊二烯及其与橡胶并用微孔发泡材料,其配方如下: 反式聚异戊二烯与橡胶共混材料100份,活性剂2-3份,硫化剂0.5-4份,硫化助剂1-8份,发泡剂0-12份,防老剂0.5-2份;其中反式聚异戊二烯与橡胶共混材料为反式聚异戊二烯(TPI)40-100份,顺丁橡胶(BR)0-40份,丁苯橡胶 (SBR) 0-20份,1,3聚丁二烯(PB)0-40 份;活性剂为硬脂酸、硬脂酸锌、氧化锌中的一种或多种,硫化剂为硫磺、过氧化异丙苯中的一种;硫化助剂为N-叔丁基-2苯并噻唑次磺酰胺(TBBS);防老剂为防老剂1010、防老剂264中的任一种;发泡材料的制备方法为超临界氮气发泡,其制备方法如下:
1)混炼胶制备
密炼机温度设定为80℃,将TPI橡胶以及并用材料投入密炼机中,加入活性剂,防老剂,混炼5-6min,出料,在开炼机上加入硫化剂、硫化助剂、混炼4-5 min,最后调整辊距,下片出料,得到混炼胶;
2)预硫化
将混炼胶放入所需模具中,热压机压力为10MPa,温度160℃,预硫化时间为6min,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,通入超临界流体氮气并升温、加压,反应釜温度为130-140℃,将超临界流体氮气注入高压釜内,使压力达到20-25 MPa,恒压饱和3h,然后迅速卸压至常压,冷却后得到发泡材料。
2.根据权利要求1所述的一种反式聚异戊二烯及其与橡胶并用微孔发泡材料,其特征在于,所述反式聚异戊二烯与橡胶并用微孔发泡材料用于家居防滑垫、鞋材、运动康复护具。
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