CN106589440A - 一种发泡聚乙烯/聚苯乙烯珠粒的生产方法 - Google Patents
一种发泡聚乙烯/聚苯乙烯珠粒的生产方法 Download PDFInfo
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- CN106589440A CN106589440A CN201611174809.1A CN201611174809A CN106589440A CN 106589440 A CN106589440 A CN 106589440A CN 201611174809 A CN201611174809 A CN 201611174809A CN 106589440 A CN106589440 A CN 106589440A
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Abstract
本发明公开了一种发泡聚乙烯/聚苯乙烯珠粒的生产方法，其特征在于，包括以下步骤：(1)将聚乙烯树脂、聚苯乙烯树脂、相容剂、结晶成核助剂及其他加工助剂混合均匀，经挤出机混炼、挤出、拉丝、切粒，制备成改性聚乙烯/聚苯乙烯微粒。(2)将改性聚乙烯/聚苯乙烯微粒投入反应釜，注入超临界CO2，加热下分段逐步加压，气体充分浸入改性聚乙烯/聚苯乙烯树脂中并产生向外膨胀的内部压力，一定时间以后，再瞬间释放至大气压，得到一定倍率的发泡聚乙烯/聚苯乙烯珠粒。该发明弥补了EPS珠粒间粘结强度弱和EPE刚性差的缺陷。同时，该发泡工艺生产成本低，生产效率高，易实现产业化，可广泛应用于汽车内饰件，包装材料、建筑材料，隔热材料等领域。
Description
技术领域
本发明涉及发泡材料领域，尤其是涉及发泡聚乙烯/聚苯乙烯珠粒。
背景技术
发泡聚苯乙烯(EPS)作为传统的发泡材料，以其优异的隔热性、力学刚性等性能深受国内外厂商青睐，其产量在发泡制品行业中约占95％以上。但EPS发泡珠粒存在一个致命的缺陷，即在加工成型为制品后珠粒与珠粒之间粘结性较差。发泡聚乙烯(EPE)是隔热、抗压、缓冲性能优良的新型环保材料，而且相对于EPS来说，EPE粒子之间的粘结强度更强。但是EPE材料由于其分子链多为烯烃类结构，其材料的力学刚性较弱。
发泡聚乙烯/聚苯乙烯复合材料，不仅具有原来EPS和EPE材料轻质、隔热等性能优势，又赋予了复合材料新的特点，即发泡聚乙烯/聚苯乙烯复合材料力学性能更为优异，粒子之间的粘结性能更强，而且发泡聚乙烯/聚苯乙烯复合材料的抗形变能力明显增强，因此，发泡聚乙烯/聚苯乙烯复合材料已经成为继EPS和EPE以后，人们关注的又一类新型环保复合材料。但是，由于聚乙烯(PE)与聚苯乙烯(PS)在结构和性能上的不同，在生产发泡聚乙烯/聚苯乙烯复合材料时，不仅需要考虑PE与PS的相容性问题，而且需要采用先进和合理的发泡工艺。
发明内容
本发明的目的在于弥补EPS珠粒间粘结强度弱、EPE刚性差的缺陷，采用独特的共混技术，对聚乙烯(PE)与聚苯乙烯(PS)进行共混改性，进而采用先进的超临界CO2釜式发泡和温度、CO2压力的精确控制及可控的泄压技术，利用分阶式的发泡方式，制备高倍率发泡聚乙烯/聚苯乙烯珠粒，产品达到90％以上的闭孔率。
本发明是通过以下技术方案实现的：
一种发泡聚乙烯/聚苯乙烯珠粒的生产方法，其特征在于，包括以下步骤：
(1)将聚乙烯树脂、聚苯乙烯树脂和相容剂、结晶成核助剂及其他加工助剂高速混合均匀，经挤出机混炼、挤出、拉丝、切粒，制备成改性聚乙烯/聚苯乙烯微粒；
(2)将上述改性聚乙烯/聚苯乙烯微粒投入反应釜，注入超临界CO2，加热下分段逐步加压，反应釜内，CO2气体充分浸入改性聚乙烯/聚苯乙烯树脂中并产生向外膨胀的内部压力，经过一定时间以后，再瞬间释放至大气压，从而得到一定倍率的发泡聚乙烯/聚苯乙烯珠粒；
步骤(1)中，所述的聚乙烯树脂为聚乙烯树，其熔点在100℃～130℃；
步骤(1)中，所述的聚苯乙烯树脂为高抗冲的聚苯乙烯树脂(HIPS)；
聚乙烯树脂与聚苯乙烯的质量比为50-70：50-30。
步骤(1)中的相容剂是对苯乙烯-乙烯-丁二烯-苯乙烯聚合物(SEBS)和/或苯乙烯-丁二烯聚合物(SBS)，其中，相容剂为聚乙烯和聚苯乙烯总质量的5％-10％；
步骤(1)中还需要添加结晶成核剂，其中结晶成核剂为聚乙烯和聚苯乙烯总质量的0.1％～3％，颗粒的粒子在0.5～2μm之间；
步骤(2)中采用分四段逐步加压，每段加压压力P为：0.4～1.0MPa，1.0～2.5MPa，2.5～4.5MPa，4.5～6MPa；时间为30min～60min；
进一步，所述的结晶成核剂为无机物或者有机物；无机成核剂包括氮化硼、碳酸钠、碳酸钾、硼酸锌、二氧化钛、滑石粉、碳酸镁等；有机成核剂包括苯甲酸、己二酸、苯甲酸钠、硬脂酸钠、硬脂酸钙、苯酚钠等；使用时是单一添加或组合添加。
进一步，结晶成核剂将无机和有机成核剂按1：2重量比添加；
进一步，步骤(2)中，所述反应釜内还包括助剂，所述助剂为分散剂、表面活性剂、消泡剂中的一种或几种，添加量为聚乙烯和聚苯乙烯总质量的0.6％～4％；
进一步，步骤(2)重复2-3次可以发泡到40倍-60倍以上的体积。
发明人按照CN103289118A的教导，参照发泡聚丙烯材料的制备方法，尤其是当压力分别是0.5MPa、2.0MPa、4.0MPa、6.0MPa时，发现：当压力较低时，发泡倍率低于15倍；当压力较高时，发泡倍率得以提高，但是泡孔不均匀，且珠粒表面粗糙。发明人通过不断试验和改进，发现分段压力和适当延长浸入时间，可以调整发泡聚乙烯/聚苯乙烯的泡孔均匀性和改善珠粒表面的光滑性。
本发明的有益效果：本发明同时弥补了EPS珠粒间粘结强度弱、EPE刚性差的缺陷。聚乙烯(PE)与聚苯乙烯(PS)进行共混改性后，进而采用先进的超临界CO2釜式发泡和温度、CO2压力的精确控制及可控的泄压技术，利用分阶式的发泡方式，制备高倍率发泡聚乙烯/聚苯乙烯珠粒，产品达到90％以上的闭孔率。PE与PS共混改性后，取长补短，所制备的微粒既具备了PE的高粘结强度，也拥有了PS的高刚性。同时，该发泡工艺降低了生产成本，提高了生产效率，更有利于进行产业化生产。整个过程不存在化学交联反应，完全可回收再利用，绿色环保，且生产效率与发泡倍率较高，完全符合工业化生产的需要，可广泛应用于汽车内饰件，包装材料、建筑材料，隔热材料等领域。
附图说明
图1是实施例1所得的发泡聚乙烯/聚苯乙烯的扫描电镜照片。
图2是实施例4所得的发泡聚乙烯/聚苯乙烯的扫描电镜照片。
具体实施方式
下面结合附图对本发明作进一步的详细描述。
表一是主要材料的配料表(表中所列为重量份)
表二是助剂配料表(表中所列为重量份)
分散剂可以选用高岭土、磷酸钙等，消泡剂可以选用硅烷类消泡剂，表面活性剂可以选用硬脂酸钙、十二烷基苯磺酸钠、十六烷基三甲基溴化铵等。
表三加压压力和时间表
加压方式采取注入超临界CO2，进行气化加压。在达到相同压力情况下，采取分段加压的方式可有效控制发泡聚乙烯/聚苯乙烯的泡孔均匀性，而且，延长浸入时间，也可以提高发泡聚乙烯/聚苯乙烯的膨胀倍率。选择较高的压力和延长浸入时间，可以提高发泡聚乙烯/聚苯乙烯的膨胀倍率。相同条件下，经过多次发泡以后，比如一次发泡以后，可以得到20～30倍的体积，2～3次发泡以后，可发泡到50～70倍以上的体积。
发泡聚乙烯/聚苯乙烯的生产方法，包括以下步骤：(1)将定量的PE树脂、HIPS树脂和相容剂、结晶成核助剂及其他加工助剂高速混合均匀，经挤出机混炼、挤出、拉丝、切粒，制备成改性聚乙烯/聚苯乙烯微粒；
(2)将上述改性聚乙烯/聚苯乙烯微粒投入反应釜，注入超临界CO2，加热下分段逐步加压，反应釜内，CO2气体充分浸入改性聚乙烯/聚苯乙烯树脂中并产生向外膨胀的内部压力，经过一定时间以后，再瞬间释放至大气压，从而得到一定倍率的发泡聚乙烯/聚苯乙烯珠粒；
聚乙烯树脂与聚苯乙烯的质量比为50-70：50-30。
步骤(1)中的相容剂是对苯乙烯-乙烯-丁二烯-苯乙烯聚合物(SEBS)和/或苯乙烯-丁二烯聚合物(SBS)，其中，相容剂为聚乙烯和聚苯乙烯总质量的5％-10％；
步骤(1)中还需要添加结晶成核剂，其中结晶成核剂为聚乙烯和聚苯乙烯总质量的0.1％～3％，颗粒的粒子在0.5～2μm之间；
步骤(2)中采用分四段逐步加压，每段加压压力P为：0.4～1.0MPa，1.0～2.5MPa，2.5～4.5MPa，4.5～6MPa；时间为30min～60min；
以上所述仅为本发明的具体实施例而已，并不用于限制本发明，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (6)
1.一种发泡聚乙烯/聚苯乙烯珠粒的生产方法，其特征在于，包括以下步骤：
(1)将聚乙烯树脂、聚苯乙烯树脂和相容剂、结晶成核助剂及其他加工助剂高速混合均匀，经挤出机混炼、挤出、拉丝、切粒，制备成改性聚乙烯/聚苯乙烯微粒；
(2)将上述改性聚乙烯/聚苯乙烯微粒投入反应釜，注入超临界CO2，加热下分段逐步加压，反应釜内，CO2气体充分浸入改性聚乙烯/聚苯乙烯树脂中并产生向外膨胀的内部压力，经过一定时间以后，再瞬间释放至大气压，
从而得到一定倍率的发泡聚乙烯/聚苯乙烯珠粒；
在步骤(2)中采用分四段逐步加压，每段加压压力P为：0.4～1.0MPa，1.0～2.5MPa，2.5～4.5MPa，4.5～6MPa；时间为30min～60min。
2.根据权利要求1所述的一种发泡聚乙烯/聚苯乙烯珠粒的生产方法，其特征在于，步骤(1)中，所述的聚乙烯树脂(PE)，其熔点在100℃～130℃；
步骤(1)中，所述的聚苯乙烯树脂为高抗冲的聚苯乙烯树脂(HIPS)；
聚乙烯树脂与聚苯乙烯的质量比为50-70：50-30。
3.根据权利要求1所述的一种发泡聚乙烯/聚苯乙烯珠粒的生产方法，其特征在于，步骤(1)中的相容剂是对苯乙烯-乙烯-丁二烯-苯乙烯聚合物(SEBS)和/或苯乙烯-丁二烯聚合物(SBS)，其中，相容剂为聚乙烯和聚苯乙烯总质量的5％-10％。
4.根据权利要求1所述的一种发泡聚乙烯/聚苯乙烯珠粒的生产方法，其特征在于，步骤(1)中的结晶成核剂为聚乙烯和聚苯乙烯总质量的0.1％～3％，颗粒的粒子在0.5～2μm之间；
进一步，所述的结晶成核剂为无机物或者有机物；无机成核剂包括氮化硼、碳酸钠、碳酸钾、硼酸锌、二氧化钛、滑石粉、碳酸镁等；有机成核剂包括苯甲酸、己二酸、苯甲酸钠、硬脂酸钠、硬脂酸钙、苯酚钠等；使用时是单一添加或组合添加；
进一步，结晶成核剂将无机和有机成核剂按1：2重量比添加。
5.根据权利要求1所述的一种发泡聚乙烯/聚苯乙烯珠粒的生产方法，其特征在于，步骤(2)中，所述反应釜内还包括助剂，所述助剂为分散剂、表面活性剂、消泡剂中的一种或几种，添加量为聚乙烯和聚苯乙烯总质量的0.6％～4％。
6.根据权利要求1-5所述的一种发泡聚乙烯/聚苯乙烯珠粒的生产方法，其特征在于，步骤(2)重复2-3次可以发泡到40倍-60倍以上的体积。
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| CN114316458B (zh) * | 2022-01-26 | 2023-07-11 | 无锡会通轻质材料股份有限公司 | 一种发泡聚烯烃珠粒及其模塑制件 |
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