CN112341687A - 一种高回弹、抗冲击型聚烯烃泡沫材料及其制备工艺 - Google Patents
一种高回弹、抗冲击型聚烯烃泡沫材料及其制备工艺 Download PDFInfo
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- CN112341687A CN112341687A CN202011164871.9A CN202011164871A CN112341687A CN 112341687 A CN112341687 A CN 112341687A CN 202011164871 A CN202011164871 A CN 202011164871A CN 112341687 A CN112341687 A CN 112341687A
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- C08K5/14—Peroxides
Abstract
本发明涉及一种高回弹、抗冲击型聚烯烃泡沫材料及其制备工艺。该聚烯烃泡沫材料,原料按重量份计,包括:复合弹性体母粒、发泡剂母粒、催化剂母粒和无机填料母粒;复合弹性体母粒的原料包括:改性胶粉、热塑性弹性体、聚烯烃树脂、相容剂、润滑剂和硫化剂;发泡剂母粒的原料包括:发泡剂和聚烯烃树脂;催化剂母粒的原料包括:催化剂和聚烯烃树脂;无机填料母粒的原料包括:无机填料和聚烯烃树脂。本发明通过将废弃胶粉改性后制备复合弹性体母粒,随后与发泡剂母粒、催化剂母粒和无机填料母粒混合制备聚烯烃泡沫材料,原料来源广、价格低,有利于降低生产成本,所得聚烯烃泡沫材料具有高弹性、高拉伸性能、高耐冲击性能、抗老化好、高阻尼特点。
Description
技术领域
本发明涉及高分子材料加工技术领域,尤其涉及一种高回弹、抗冲击型聚烯烃泡沫材料及其制备工艺。
背景技术
聚烯烃发泡材料具有密度低、轻便、环保、隔音性能好、耐老化、保温、防潮、成型性好等优点,广泛应用于工业、农业、建筑等各个领域。然而其经反复踩踏、长期承载重物后泡沫材料中的气体会挤出而影响压缩永久变形能力和回弹能力,其应对重物低速冲击能力不够强,面对震动的阻尼效果差。
废旧胶粉由废旧橡胶制品经粉碎而成的橡胶粉末,其为橡胶、炭黑、软化剂、硫化促进剂等多成分组成的交联结构材料,具有来源广泛、成本低、弹性好的优点。然而其表面呈惰性,与塑料基体之间表面性质存在较大差异,相容性差。
中国专利CN101870169A公开了一种废旧轮胎胶粉/聚乙烯发泡材料的制备方法,通过以废旧轮胎胶粉与聚乙烯粒料为主要原料制备发泡材料,其中废旧轮胎胶粉的掺量较低,不利于降低成本,且所得发泡材料回弹性和抗冲击性能仍然较差。
发明内容
有鉴于此,有必要提供一种高回弹、抗冲击型聚烯烃泡沫材料及其制备工艺,用以解决现有的聚烯烃发泡材料回弹性和抗冲击性能差的技术问题。
本发明的第一方面提供了一种高回弹、抗冲击型聚烯烃泡沫材料,原料按重量份计,包括:复合弹性体母粒90~110份、发泡剂母粒15~30份、催化剂母粒2.5~5.5份和无机填料母粒3~8份;其中,
上述复合弹性体母粒的原料按重量份计包括:改性胶粉45~65份、热塑性弹性体5~15份、聚烯烃树脂30~45份、相容剂4~6份、润滑剂0.3~0.6份和硫化剂0.2~0.8份;
上述发泡剂母粒的原料按重量份计包括:发泡剂3~10份和聚烯烃树脂12~20份;
上述催化剂母粒的原料按重量份计包括:催化剂0.5~1份和聚烯烃树脂2~4.5份;
上述无机填料母粒的原料按重量份计包括:无机填料0.5~1.5份和聚烯烃树脂2.5~6.5份。
进一步地,上述聚烯烃树脂与改性胶粉、热塑性弹性体的质量比为1:(0.11~0.5):(1.1~2.2)。
进一步地,上述改性胶粉通过将废弃胶粉脱硫后与改性剂、软化剂混合塑化得到;所述废弃胶粉、改性剂、软化剂的质量比为1:(0.02~0.03):(0.02~0.03)。
更进一步地,上述软化剂为邻苯二甲酸二辛酯、石油树脂中的一种或两种;所述改性剂为有机胺、改性酚醛树脂、液体聚烯烃中的一种或多种。
进一步地,上述热塑性弹性体为乙烯-辛烯共聚物、三元乙丙橡胶、天然橡胶、硅橡胶中的一种或多种,其断裂应变1000~2000%,拉伸强度10~40MPa。
进一步地,上聚烯烃树脂为聚丙烯、聚乙烯、丙烯-乙烯共聚物、乙烯-辛烯共聚物中的一种或多种。
进一步地,上述相容剂为乙烯-醋酸乙烯共聚物、苯乙烯-聚(乙烯-丁烯)-聚苯乙烯嵌段共聚物、氯化聚乙烯、环氧天然橡胶中的一种亦或多种复合;上述硫化剂为过氧化二异丙苯、双(叔丁过氧基)二异丙苯中的一种或两种;上述润滑剂为硬脂酸、硬脂酸锌、硬脂酸钙、硬脂酸镁中的一种或多种。
进一步地,上述发泡剂为AC发泡剂,粒径≤400目;上述无机填料为滑石粉、纳米级碳酸钙、炭黑中的一种或两种;上述催化剂为ZnO、碳酸锌、醋酸锌、硬脂酸锌中的一种或多种。
进一步地,上述高回弹、抗冲击型聚烯烃泡沫材料的密度为0.030~0.2g/cm3,其沿厚度方向的孔隙直径为20~150μm,孔隙率为70~95%,25%压缩应力为150~500KPa,抗冲击强度为55~95KJ/m2,比拉伸强度为2~6MPa/(g/cm3),回弹率≥90%,压缩永久变形≤5%。
本发明的第二方面提供了一种高回弹、抗冲击型聚烯烃泡沫材料的制备工艺,包括以下步骤:
将改性胶粉、聚烯烃树脂、热塑性弹性体、相容剂、润滑剂、硫化剂按照配方比例加入密炼机中进行混炼,随后经挤出造粒、烘干,制备复合弹性体母粒;
将发泡剂与聚烯烃树脂进行混合密炼造粒、烘干,制备发泡剂母粒;
将催化剂与聚烯烃树脂进行混合密炼造粒、烘干,制备催化剂母粒;
将无机填料与聚烯烃树脂进行混合密炼造粒、烘干,制备无机填料母粒;
以及,将所述复合弹性体母粒、发泡剂母粒、催化剂母粒和无机填料母粒由先至后依次交联、发泡得到高回弹、抗冲击型聚烯烃泡沫材料。
本发明第二方面提供的高回弹、抗冲击型聚烯烃泡沫材料的制备工艺用于得到本发明第一方面提供的高回弹、抗冲击型聚烯烃泡沫材料。
与现有技术相比,本发明的有益效果为:
本发明通过将废弃胶粉改性后制备复合弹性体母粒,随后与发泡剂母粒、催化剂母粒和无机填料母粒混合制备聚烯烃泡沫材料,原料来源广、价格低,有利于降低生产成本,能有效利用废旧轮胎胶粉减少污染,所得聚烯烃泡沫材料具有高弹性、高拉伸性能、高耐冲击性能、抗老化好、高阻尼特点。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
本发明的第一方面提供了一种高回弹、抗冲击型聚烯烃泡沫材料,其原料按重量份计,包括:复合弹性体母粒90~110份、发泡剂母粒15~30份、催化剂母粒2.5~5.5份和无机填料母粒3~8份;其中,
复合弹性体母粒的原料按重量份计包括:改性胶粉45~65份、热塑性弹性体5~15份、聚烯烃树脂30~45份、相容剂4~6份、润滑剂0.3~0.6份和硫化剂0.2~0.8份;
发泡剂母粒的原料按重量份计包括:发泡剂3~10份和聚烯烃树脂12~20份;
催化剂母粒的原料按重量份计包括:催化剂0.5~1份和聚烯烃树脂2~4.5份;
无机填料母粒的原料按重量份计包括:无机填料0.5~1.5份和聚烯烃树脂2.5~6.5份。
本发明中,所得复合弹性体母粒的拉伸率为800%~1400%,拉伸强度为10~30Mpa;所得高回弹、抗冲击型聚烯烃泡沫材料的密度为0.030~0.2g/cm3,其沿厚度方向的孔隙直径为20~150μm,孔隙率为70~95%,25%压缩应力为150~500KPa,抗冲击强度为55~95KJ/m2,比拉伸强度为2~6MPa/(g/cm3),回弹率≥90%,压缩永久变形≤5%,可起到缓冲、减震、降噪的作用。
本发明中,通过采用预先制备的复合弹性体母粒、发泡剂母粒、催化剂母粒和无机填料母粒作为原料制备聚烯烃泡沫材料,能使改性胶粉、热塑性弹性体、发泡剂、催化剂和无机填料更好的分散在聚烯烃树脂中,更有利于提高聚烯烃泡沫材料的性能;通过采用改性胶粉作为原料制备复合弹性母粒,更有利于实现改性胶粉在树脂基体的均匀分散,进一步提高改性胶粉的掺量,降低生产成本,提高聚烯烃泡沫材料的韧性。
本实施方式中,选用的聚烯烃树脂与改性胶粉、热塑性弹性体的质量比为1:(0.11~0.5):(1.1~2.2),优选为1:(0.2~0.5):(1.1~1.5)。在该范围内,能更好的兼顾性能和成本。
本实施方式中,改性胶粉通过将废弃胶粉脱硫后与改性剂、软化剂混合塑化得到。该过程中,选用的废弃胶粉为废旧轮胎粉末,其主要成分为天然橡胶、丁苯橡胶和顺丁橡胶的混合物;选用的废弃胶粉目数为40~100目。脱硫过程具体为:将废弃胶粉采用双螺杆挤出机剪切脱硫得到。经剪切脱硫后,胶粉粒度区间窄,比表面积大,表面凸起加长,胶粉凝胶量55~70%,可增加胶粉与改性剂、聚烯烃的有效接触面积。进一步地,塑化过程在塑化装置中进行,塑化转速150~300r/min,塑化时间30~150min。进一步地,选用的软化剂为邻苯二甲酸二辛酯、石油树脂中的一种或两种,选用的改性剂为有机胺、改性酚醛树脂、液体聚烯烃中的一种或多种。更进一步地,选用的改性剂为二乙烯三胺、三乙烯四胺、四乙烯五胺中的一种或多种。更进一步地,废弃胶粉、改性剂、软化剂的质量比为1:(0.02~0.03):(0.02~0.03)。本发明中,通过对胶粉改性,能够改善废弃胶粉的表面活性,提高废弃胶粉与聚烯烃的界面相容性,有利于提高橡塑比,实现废胶粉的高效利用。
本实施方式中,选用的热塑性弹性体为乙烯-辛烯共聚物(POE)、三元乙丙橡胶(EPDM)、天然橡胶、硅橡胶中的一种或多种,其断裂应变1000~2000%,拉伸强度10~40MPa。本发明中,通过将热塑性弹性体的断裂应变和拉伸强度控制在该范围内,更有利于提高聚烯烃泡沫材料的力学性能。
本实施方式中,选用的聚烯烃树脂为聚丙烯、聚乙烯、丙烯-乙烯共聚物、乙烯-辛烯共聚物中的一种或多种。进一步地,选用的聚烯烃树脂为低密度聚乙烯、高密度聚乙烯中的一种或多种。
本实施方式中,选用的相容剂为乙烯-醋酸乙烯共聚物(EVA)、苯乙烯-聚(乙烯-丁烯)-聚苯乙烯嵌段共聚物(SEBS)、氯化聚乙烯(CPE)、环氧天然橡胶(ENR)中的一种亦或多种复合,选用的硫化剂为过氧化二异丙苯、双(叔丁过氧基)二异丙苯中的一种或两种;选用的润滑剂为硬脂酸、硬脂酸锌、硬脂酸钙、硬脂酸镁中的一种或多种。
本实施方式中,选用的发泡剂为AC发泡剂,粒径≤400目;选用的无机填料为滑石粉、纳米级碳酸钙、炭黑中的一种或两种;选用的催化剂为ZnO、碳酸锌、醋酸锌、硬脂酸锌中的一种或多种。
本发明中,发泡剂用于调整聚烯烃泡沫材料的最终密度,无机填料不仅可提高聚烯烃泡沫材料的强度,还能作为成核剂使用,催化剂用于调节发泡剂的分解温度和分解速率。本发明通过严格控制体系中发泡剂、无机填料和催化剂用量,更有利于控制反应过程,所得聚烯烃泡沫材料具有高回弹、强度高、耐冲击的特性。
本发明的第二方面提供了一种高回弹、抗冲击型聚烯烃泡沫材料的制备工艺,包括以下步骤:S1制备复合弹性体母粒;S2制备发泡剂母粒;S3制备催化剂母粒;S4制备无机填料母粒;S5将复合弹性体母粒、发泡剂母粒、催化剂母粒和无机填料母粒由先至后依次交联、发泡得到高回弹、抗冲击型聚烯烃泡沫材料。下面对步骤S1~S5进行分别详述。
步骤S1制备复合弹性体母粒具体为:将改性胶粉、聚烯烃树脂、热塑性弹性体、相容剂、润滑剂、硫化剂按照配方比例加入密炼机中进行混炼,随后经挤出造粒、烘干,得到复合弹性体母粒。
步骤S2制备发泡剂母粒具体为:将发泡剂与聚烯烃树脂进行混合密炼造粒,并烘干备用。
步骤S3制备催化剂母粒具体为:将催化剂与聚烯烃树脂进行混合密炼造粒,并烘干备用。
步骤S4制备无机填料母粒具体为:将无机填料与聚烯烃树脂进行混合密炼造粒,并烘干备用。
步骤S5将复合弹性体母粒、发泡剂母粒、催化剂母粒和无机填料母粒由先至后依次交联、发泡得到高回弹、抗冲击型聚烯烃泡沫材料具体为:将复合弹性体母粒、发泡剂母粒、催化剂母粒和无机填料母粒在混合机中混合,随后经挤出机挤出、辐照交联和自由式发泡,得到高回弹、抗冲击型聚烯烃泡沫材料。
上述步骤S1中,混炼的温度130~135℃,混炼的时间15~30min,烘干的温度75~85℃,烘干的时间4~8h;上述步骤S2~S4中,密炼的温度125~130℃,密炼的时间15~20min,烘干的温度60~70℃,烘干的时间4~5h;上述步骤S5中,混合机的转速15~45r/min,挤出机的主机转速15~25r/min,挤出机机筒温度设置区域为100~140℃,T形模具各温区温度设置范围115~140℃;辐照交联采用电子辐照加速器进行,电子辐照加速器的电子能量为0.2MeV~5MeV,辐照剂量控制为3~30兆拉德,辐照层数控制为2~8层。
本发明中,步骤S5中,挤出机挤出为片材,片材厚度为0.2~2.5mm,宽度为300~800mm。
本发明第二方面提供的高回弹、抗冲击型聚烯烃泡沫材料的制备工艺用于得到本发明第一方面提供的高回弹、抗冲击型聚烯烃泡沫材料。
为避免赘述,本发明以下各实施例和对比例中,改性胶粉通过以下步骤得到:将40~80目废弃胶粉进行烘干处理,处理温度50~60℃,处理时间4~8h,烘干完后放置干燥室备用;将烘干后的废旧胶粉采用双螺杆挤出机进行剪切脱硫,随后按照废旧胶粉:改性剂:软化剂为1:0.025:0.025的质量比将三乙烯四胺和邻苯二甲酸二辛酯加入高脚塑化装置进行改性塑化,塑化转速150~300r/min,塑化时间30~150min。所得改性胶粉凝胶量45~55%。
实施例1
本实施提供了一种高回弹、抗冲击型聚烯烃泡沫材料,其原料见表表1。
本实施例还提供了一种高回弹、抗冲击型聚烯烃泡沫材料及其制备工艺,包括以下步骤:
(1)制备复合弹性体母粒:将改性胶粉、聚烯烃树脂、热塑性弹性体、相容剂、润滑剂、硫化剂按照配方比例加入密炼机中进行混炼,随后经挤出造粒、烘干,得到复合弹性体母粒;其中,混炼的温度130~135℃,混炼的时间20min,烘干的温度80℃,烘干的时间6h;
(2)制备发泡剂母粒:将发泡剂与聚烯烃树脂进行混合密炼造粒,并烘干备用;其中,密炼的温度125~130℃,密炼的时间15~20min,烘干的温度60~70℃,烘干的时间4~5h;
(3)制备催化剂母粒:将催化剂与聚烯烃树脂进行混合密炼造粒,并烘干备用;其中,密炼的温度125~130℃,密炼的时间15~20min,烘干的温度60~70℃,烘干的时间4~5h;
(4)制备无机填料母粒:将无机填料与聚烯烃树脂进行混合密炼造粒,并烘干备用;其中,密炼的温度125~130℃,密炼的时间15~20min,烘干的温度60~70℃,烘干的时间4~5h;
(5)制备高回弹、抗冲击型聚烯烃泡沫材料:将复合弹性体母粒、发泡剂母粒、催化剂母粒和无机填料母粒在混合机中混合,随后经挤出机挤出、辐照交联和自由式发泡,得到高回弹、抗冲击型聚烯烃泡沫材料;其中,混合机的转速15~45r/min,挤出机的主机转速15~25r/min,挤出机机筒温度设置区域为100~140℃,T形模具各温区温度设置范围115~140℃;辐照交联采用电子辐照加速器进行,电子辐照加速器的电子能量为3MeV,辐照剂量控制为15兆拉德,辐照层数控制为5层。
实施例2~5
实施例2~5与实施例1的区别仅在于,原料组成和含量不同,具体见表1。
对比例1
对比例1与实施例1的区别仅在于,采用废弃胶粉替代改性胶粉。
对比例2
本对比例的制备工艺具体如下:
将改性胶粉、聚烯烃树脂、热塑性弹性体、相容剂、润滑剂、硫化剂、发泡剂、催化剂、无机填料按照配方比例加入密炼机中进行混炼,随后经挤出造粒、烘干,得到聚烯烃泡沫材料。
表1
试验组
对上述实施例1~5和对比例1~2所得聚烯烃泡沫材料进行性能测试,结果见表2。
表2
由表1和表2可以看出,本发明实施例1~5所得聚烯烃泡沫材料具有优异的回弹性和抗冲击性能,密度为0.030~0.2g/cm3,其沿厚度方向的孔隙直径为20~150μm,孔隙率为70~95%,25%压缩应力为150~500KPa,抗冲击强度为55~95KJ/m2,比拉伸强度为2~6MPa/(g/cm3),回弹率≥90%,压缩永久变形≤5%,可起到缓冲、减震、降噪的作用。
同时,与实施例1相比,本发明实施例4和5的回弹性和抗冲击性能较差,说明聚烯烃树脂与改性胶粉、热塑性弹性体的质量比对所得聚烯烃泡沫材料的性能具有极大影响,在实际生产过程中,需严格控制三者的质量比。
另外,对比例1中为废弃胶粉,胶粉与聚烯烃树脂的相容性差,最终导致其具有较差的力学性能;对比例2中未先制备复合弹性体母粒、发泡剂母粒、催化剂母粒和无机填料母粒,而是直接将原料混合,从而导致分散不均匀,各组分相容性差,最终导致所得聚烯烃泡沫材料具有较差的力学性能。
与现有技术相比,本发明的有益效果为:
本发明通过将废弃胶粉改性后制备复合弹性体母粒,随后与发泡剂母粒、催化剂母粒和无机填料母粒混合制备聚烯烃泡沫材料,原料来源广、价格低,有利于降低生产成本,能有效利用废旧轮胎胶粉减少污染,所得聚烯烃泡沫材料具有高弹性、高拉伸性能、高耐冲击性能、抗老化好、高阻尼特点。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种高回弹、抗冲击型聚烯烃泡沫材料,其特征在于,原料按重量份计,包括:复合弹性体母粒90~110份、发泡剂母粒15~30份、催化剂母粒2.5~5.5份和无机填料母粒3~8份;其中,
所述复合弹性体母粒的原料按重量份计包括:改性胶粉45~65份、热塑性弹性体5~15份、聚烯烃树脂30~45份、相容剂4~6份、润滑剂0.3~0.6份和硫化剂0.2~0.8份;
所述发泡剂母粒的原料按重量份计包括:发泡剂3~10份和聚烯烃树脂12~20份;
所述催化剂母粒的原料按重量份计包括:催化剂0.5~1份和聚烯烃树脂2~4.5份;
所述无机填料母粒的原料按重量份计包括:无机填料0.5~1.5份和聚烯烃树脂2.5~6.5份。
2.根据权利要求1所述高回弹、抗冲击型聚烯烃泡沫材料,其特征在于,所述聚烯烃树脂与改性胶粉、热塑性弹性体的质量比为1:(0.11~0.5):(1.1~2.2)。
3.根据权利要求1所述高回弹、抗冲击型聚烯烃泡沫材料,其特征在于,所述改性胶粉通过将废弃胶粉脱硫后与改性剂、软化剂混合塑化得到;所述废弃胶粉、改性剂、软化剂的质量比为1:(0.02~0.03):(0.02~0.03)。
4.根据权利要求3所述高回弹、抗冲击型聚烯烃泡沫材料,其特征在于,所述软化剂为邻苯二甲酸二辛酯、石油树脂中的一种或两种;所述改性剂为有机胺、改性酚醛树脂、液体聚烯烃中的一种或多种。
5.根据权利要求3所述高回弹、抗冲击型聚烯烃泡沫材料,其特征在于,所述热塑性弹性体为乙烯-辛烯共聚物、三元乙丙橡胶、天然橡胶、硅橡胶中的一种或多种,其断裂应变1000~2000%,拉伸强度10~40MPa。
6.根据权利要求1所述高回弹、抗冲击型聚烯烃泡沫材料,其特征在于,所述聚烯烃树脂为聚丙烯、聚乙烯、丙烯-乙烯共聚物、乙烯-辛烯共聚物中的一种或多种。
7.根据权利要求1所述高回弹、抗冲击型聚烯烃泡沫材料,其特征在于,所述相容剂为乙烯-醋酸乙烯共聚物、苯乙烯-聚(乙烯-丁烯)-聚苯乙烯嵌段共聚物、氯化聚乙烯、环氧天然橡胶中的一种亦或多种复合;所述硫化剂为过氧化二异丙苯、双(叔丁过氧基)二异丙苯中的一种或两种;所述润滑剂为硬脂酸、硬脂酸锌、硬脂酸钙、硬脂酸镁中的一种或多种。
8.根据权利要求1所述高回弹、抗冲击型聚烯烃泡沫材料,其特征在于,所述发泡剂为AC发泡剂,粒径≤400目;所述无机填料为滑石粉、纳米级碳酸钙、炭黑中的一种或两种;所述催化剂为ZnO、碳酸锌、醋酸锌、硬脂酸锌中的一种或多种。
9.根据权利要求1所述高回弹、抗冲击型聚烯烃泡沫材料,其特征在于,所述高回弹、抗冲击型聚烯烃泡沫材料的密度为0.030~0.2g/cm3,其沿厚度方向的孔隙直径为20~150μm,孔隙率为70~95%,25%压缩应力为150~500KPa,抗冲击强度为55~95KJ/m2,比拉伸强度为2~6MPa/(g/cm3),回弹率≥90%,压缩永久变形≤5%。
10.一种如权利要求1~9中任一项所述高回弹、抗冲击型聚烯烃泡沫材料的制备工艺,其特征在于,包括以下步骤:
将改性胶粉、聚烯烃树脂、热塑性弹性体、相容剂、润滑剂、硫化剂按照配方比例加入密炼机中进行混炼,随后经挤出造粒、烘干,制备复合弹性体母粒;
将发泡剂与聚烯烃树脂进行混合密炼造粒、烘干,制备发泡剂母粒;
将催化剂与聚烯烃树脂进行混合密炼造粒、烘干,制备催化剂母粒;
将无机填料与聚烯烃树脂进行混合密炼造粒、烘干,制备无机填料母粒;
以及,将所述复合弹性体母粒、发泡剂母粒、催化剂母粒和无机填料母粒由先至后依次交联、发泡得到高回弹、抗冲击型聚烯烃泡沫材料。
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