CN106543559B - 一种发泡聚丙烯珠粒的制备方法 - Google Patents
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Abstract
本发明公开了一种发泡聚丙烯珠粒的制备方法,其包括以下步骤:1)将聚丙烯树脂、活性填料和助剂加入高速混合机,10~20℃混合均匀,得到聚丙烯发泡料;2)将聚丙烯发泡料加入三螺杆挤出机,进行塑化和混炼,再加注超临界流体,控制口模压力为5~25MPa,口模温度为110~160℃,再经口模瞬间释压,进行发泡,得到超细微孔发泡聚丙烯;3)超细微孔发泡聚丙烯经模面水环热切造粒、干燥、过筛,得到发泡聚丙烯珠粒。本发明的方法生产成本低,产能大,安全环保,制备的发泡聚丙烯珠粒中无发泡剂分解残留物,可二次发泡,发泡倍率可调,成品回弹性高,易分解和回收,可广泛用在塑料包装、交通运输业、军事航天及办公日用品等领域。
Description
技术领域
本发明涉及一种发泡聚丙烯珠粒的制备方法,具体涉及一种采用三螺杆挤出机制备发泡聚丙烯珠粒的方法,属于聚合物发泡技术领域。
背景技术
泡沫塑料具有质轻、吸能、隔音、隔热、比强度高等优点,在塑料包装、交通运输业、军事航天、办公日用品等领域应用广泛。发泡聚丙烯(EPP)与发泡聚乙烯(EPE)和发泡聚苯乙烯(EPS)等相比,具备许多独特的优点:1)力学性能:由于聚丙烯的弯曲模量远大于聚乙烯,使得EPP在抗静态负载能力优于EPE,抗冲击能力优于EPS;2)耐热性:EPP可以在120℃左右的高温环境中长期使用,是泡沫塑料中耐热性最好的;3)降解性:聚丙烯分子上存在一个甲基,其降解性能将明显优于聚乙烯和聚苯乙烯。此外,EPP还具有优良的耐化学腐蚀性能和耐应力开裂性能。EPP材料在汽车工业、运输业、包装行业的应用极具竞争力,可以替代EPS材料和EPE材料,应用前景非常广阔。
目前,聚丙烯泡沫塑料成型品的制备方法主要有挤出法、模压法等。挤出法一般只能用于片材、板材等产品的生产,难以制备形状复杂的产品。模压法是将发泡珠粒放入特定形状的模具中,然后利用蒸汽加热加压使发泡珠粒之间熔接起来形成制品,被广泛用于制备形状复杂的制品。EPP珠粒发泡工艺分为两类:间歇式釜压发泡法、连续式挤出发泡法。间歇式釜压发泡法工艺条件容易控制,可以制备倍率和闭孔率可调控的发泡珠粒,但要求压力高,设备投入大,成本高,生产周期长,在世界范围内仅有JSP、BASF、KANKA等公司采用该方法进行生产。连续式挤出发泡法是将含有发泡剂的聚丙烯均相熔体从机头口模直接挤出,通过快速泄压,进行相分离,使溶于聚丙烯均相熔体的气体膨胀,再随着气泡成核、长大、固化,一次性完成挤出和发泡,工艺流程简单,工业化生产效率高。
本发明公开了一种采用三螺杆挤出机制备发泡聚丙烯珠粒的方法,首先将聚丙烯树脂与其他原料或助剂进行低温高速混合,得到高熔体强度聚丙烯发泡料,再将高熔体强度聚丙烯发泡料加入品字型三螺杆挤出机,进行塑化混炼,并将超临界流体加注到三螺杆挤出机均化段形成均相体,再在模口发泡,经水环热切造粒,形成超细微孔聚丙烯珠粒,最后经离心脱水干燥、振动过筛,得到发泡聚丙烯珠粒。
发明内容
本发明的目的在于提供一种发泡聚丙烯珠粒的制备方法。
本发明所采取的技术方案是:
一种发泡聚丙烯珠粒的制备方法,包括以下步骤:
1)将聚丙烯树脂、活性填料和助剂加入高速混合机,10~20℃混合均匀,得到聚丙烯发泡料;
2)将聚丙烯发泡料加入三螺杆挤出机,进行塑化和混炼,再将超临界流体加注到三螺杆挤出机的均化段,控制口模压力为5~25MPa,口模温度为110~160℃,再经口模瞬间释压,进行发泡,得到超细微孔发泡聚丙烯;
3)超细微孔发泡聚丙烯经模面水环热切造粒、干燥、过筛,得到发泡聚丙烯珠粒。
步骤1)所述的聚丙烯树脂为均聚聚丙烯、无规共聚聚丙烯、嵌段共聚聚丙烯中的至少一种。
步骤1)所述的聚丙烯树脂为均聚聚丙烯、无规共聚聚丙烯、嵌段共聚聚丙烯中的至少一种与长支链聚丙烯所组成的混合物,其中长支链聚丙烯的质量分数为5%~15%。
步骤1)所述的活性填料为经偶联剂活化处理过的纳米级滑石粉、苯甲酸钠、碳酸钙、二氧化钛、蒙脱土、二氧化硅中的至少一种,添加量为聚丙烯树脂质量的0.5%~2%。
步骤1)所述的助剂为偶联剂、润滑剂、抗氧剂、着色剂中的至少一种。
所述的润滑剂为硬脂酸、硬脂酸盐中的至少一种,添加量为聚丙烯树脂质量的0.5%~2%;所述的抗氧剂为抗氧剂1010、抗氧剂1098、抗氧剂1076、抗氧剂量168、抗氧剂264、抗氧剂626中的至少一种,添加量为聚丙烯树脂质量的0.1%~0.5%;所述的着色剂为炭黑、色母粒中的至少一种,添加量为聚丙烯树脂质量的5%~10%。
步骤2)所述的三螺杆挤出机的机头设置有换网器、熔体泵、口模和模面水环热切粒机。
步骤2)所述的超临界流体的添加量为聚丙烯发泡料质量的2%~10%。
步骤2)所述的超临界流体为超临界CO2、超临界N2中的至少一种。
步骤3)进行模面水环热切造粒时的水温为40~70℃。
本发明的有益效果是:
1)本发明所采用的聚丙烯树脂中未添加或仅添加少量高熔体强度聚丙烯,和完全采用高熔体强度聚丙烯相比,可以减少约一半成本;
2)本发明采用的是三螺杆挤出机,和单螺杆挤出机或者双螺杆挤出机相比,具备更强大的物料输送、建压、混炼、分散、均化和剪切能力,产能大;
3)本发明通过将活化填料均匀分散在树脂中来降低树脂结晶成核的界面自由能,增加气泡异相成核,且活化填料在通过三螺杆挤出机进行混炼分散时起到物理交联点的作用,可有效提高物料的熔体强度,提高树脂的可发泡能力;
4)本发明采用超临界流体作为发泡剂,安全、环境友好、发泡倍率可调;
5)本发明制备的发泡聚丙烯珠粒无发泡剂分解残留物,可二次发泡,成品回弹性高,易分解和回收,可广泛用在塑料包装、交通运输业、军事航天及办公日用品等领域。
具体实施方式
一种发泡聚丙烯珠粒的制备方法,包括以下步骤:
1)将聚丙烯树脂、活性填料和助剂加入高速混合机,10~20℃混合均匀,得到聚丙烯发泡料;
2)将聚丙烯发泡料加入三螺杆挤出机,进行塑化和混炼,再将超临界流体加注到三螺杆挤出机的均化段,控制口模压力为5~25MPa,口模温度为110~160℃,再经口模瞬间释压,进行发泡,得到超细微孔发泡聚丙烯;
3)超细微孔发泡聚丙烯经模面水环热切造粒、干燥、过筛,得到发泡聚丙烯珠粒。
优选的,步骤1)所述的聚丙烯树脂为均聚聚丙烯、无规共聚聚丙烯、嵌段共聚聚丙烯中的至少一种。
优选的,步骤1)所述的聚丙烯树脂为均聚聚丙烯、无规共聚聚丙烯、嵌段共聚聚丙烯中的至少一种与长支链聚丙烯所组成的混合物,其中长支链聚丙烯的质量分数为5%~15%。
优选的,步骤1)所述的活性填料为经偶联剂活化处理过的纳米级滑石粉、苯甲酸钠、碳酸钙、二氧化钛、蒙脱土、二氧化硅中的至少一种,添加量为聚丙烯树脂质量的0.5%~2%。
进一步优选的,所述的活性填料为经偶联剂活化处理过的纳米级滑石粉。
优选的,所述的经偶联剂活化处理过的纳米级滑石粉的制备方法如下:将纳米级滑石粉加入高速捏合机中,110℃~125℃高速搅拌15~20分钟,当含水量低于0.3%时,分三次添加偶联剂进行活化处理,总用量为纳米级滑石粉质量的0.5%~2%,每次间隔2分钟,总活化处理时间为8~12分钟。
优选的,所述的偶联剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂中的至少一种。
进一步优选的,所述的偶联剂为铝酸酯偶联剂。
优选的,步骤1)所述的助剂为润滑剂、抗氧剂、着色剂中的至少一种。
优选的,所述的润滑剂为硬脂酸、硬脂酸盐中的至少一种,添加量为聚丙烯树脂质量的0.5%~2%。
进一步优选的,所述的润滑剂为硬脂酸。
优选的,所述的抗氧剂为抗氧剂1010、抗氧剂1098、抗氧剂1076、抗氧剂量168、抗氧剂264、抗氧剂626中的至少一种,添加量为聚丙烯树脂质量的0.1%~0.5%。
进一步优选的,所述的抗氧剂为抗氧剂1010。
优选的,所述的着色剂为炭黑、色母粒中的至少一种,添加量为聚丙烯树脂质量的5%~10%。
优选的,步骤2)所述的三螺杆挤出机的机头设置有换网器、熔体泵、口模和模面水环热切粒机。
优选的,步骤2)所述的三螺杆挤出机为品字型三螺杆挤出机,螺杆直径为62mm,螺杆长径比L/D为36:1,螺杆最高转速为500r/min。
优选的,步骤2)所述的超临界流体的添加量为聚丙烯发泡料质量的2%~10%。
优选的,步骤2)所述的超临界流体为超临界CO2、超临界N2中的至少一种。
进一步优选的,步骤2)所述的超临界流体为超临界CO2。
优选的,步骤3)进行模面水环热切造粒时的水温为40~70℃。
下面结合具体实施例对本发明作进一步的解释和说明。
实施例1:
将100kg均聚聚丙烯、1kg经偶联剂活化处理过的纳米级滑石粉、0.5kg硬脂酸和0.2kg抗氧化剂1010和5kg纳米级炭黑加入低温高速混合机,混合均匀,再将物料用自动喂料***以10kg/h的速度转入三螺杆挤出机,在三螺杆挤出机的机筒均化段设置加注口,将超临界二氧化碳以300g/h的速度注入到机筒中,经熔体泵提高和稳定模口压力,通过机头口模发泡,模面水环热切造粒,脱水干燥,过筛,得到发泡聚丙烯珠粒。控制口模压力为8MPa,口模温度为138℃,得到发泡倍率为28倍的黑色珠粒,色泽均一。
实施例2:
将90kg均聚聚丙烯、10kg长支链聚丙烯、2kg经偶联剂活化处理过的纳米级滑石粉、1kg硬脂酸、0.5kg抗氧化剂1010和8kg粉色的色母粒加入低温高速混合机,混合均匀,再将物料用自动喂料***以10kg/h的速度转入三螺杆挤出机,在三螺杆挤出机的机筒均化段设置加注口,将超临界二氧化碳以800g/h的速度注入到机筒中,经熔体泵提高和稳定模口压力,通过机头口模发泡,模面水环热切造粒,脱水干燥,过筛,得到发泡聚丙烯珠粒。控制口模压力为17MPa,口模温度为125℃,得到发泡倍率为42倍的粉色珠粒,色泽均一。
实施例3:
将100kg无规共聚聚丙烯、0.5kg经偶联剂活化处理过的纳米级滑石粉和0.1kg抗氧化剂1010加入低温高速混合机,混合均匀,再将物料用自动喂料***以10kg/h的速度转入三螺杆挤出机,在三螺杆挤出机的机筒均化段设置加注口,将超临界二氧化碳以300g/h的速度注入到机筒中,经熔体泵提高和稳定模口压力,通过机头口模发泡,模面水环热切造粒,脱水干燥,过筛,得到发泡聚丙烯珠粒。控制口模压力为5MPa,口模温度为118℃,得到发泡倍率为8倍的白色珠粒。
实施例4:
将95kg无规共聚聚丙烯、5kg长支链聚丙烯、1kg经偶联剂活化处理过的纳米级滑石粉、1kg硬脂酸加入低温高速混合机,混合均匀,再将物料用自动喂料***以10kg/h的速度转入三螺杆挤出机,在三螺杆挤出机的机筒均化段设置加注口,将超临界二氧化碳以500g/h的速度注入到机筒中,经熔体泵提高和稳定模口压力,通过机头口模发泡,模面水环热切造粒,脱水干燥,过筛,得到发泡聚丙烯珠粒。控制口模压力为9MPa,口模温度为120℃,得到发泡倍率为18倍的白色珠粒。
实施例5:
将100kg嵌段共聚聚丙烯、0.5kg经偶联剂活化处理过的纳米级滑石粉、1kg硬脂酸和0.2kg抗氧化剂1010加入低温高速混合机,混合均匀,再将物料用自动喂料***以10kg/h的速度转入三螺杆挤出机,在三螺杆挤出机的机筒均化段设置加注口,将超临界二氧化碳以500g/h的速度注入到机筒中,经熔体泵提高和稳定模口压力,通过机头口模发泡,模面水环热切造粒,脱水干燥,过筛,得到发泡聚丙烯珠粒。控制口模压力为11MPa,口模温度为150℃,得到发泡倍率为36倍的白色珠粒。
实施例6:
将85kg嵌段共聚聚丙烯、15kg长支链聚丙烯、2kg经偶联剂活化处理过的纳米级滑石粉、2kg硬脂酸和0.5kg抗氧化剂1010加入低温高速混合机,混合均匀,再将物料用自动喂料***以10kg/h的速度转入三螺杆挤出机,在三螺杆挤出机的机筒均化段设置加注口,将超临界二氧化碳以900g/h的速度注入到机筒中,经熔体泵提高和稳定模口压力,通过机头口模发泡,模面水环热切造粒,脱水干燥,过筛,得到发泡聚丙烯珠粒。控制口模压力为18MPa,口模温度为146℃,得到发泡倍率为58倍的白色珠粒。
注:本发明的发泡聚丙烯珠粒的发泡倍率按标准ASTM D792-2008进行测试,发泡倍率公式为:n=ρ0/ρ,式中n为发泡倍率;ρ0为基体树脂的密度;ρ为发泡珠粒的密度。ρ的计算公式为:ρ=m/(m+m1-m2),式中m为发泡珠粒在空气中的质量,m1为使发泡样品浸入水中的金属帽在水中的质量,m2为发泡珠粒在水中的质量。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (1)
1.一种发泡聚丙烯珠粒的制备方法,其特征在于:包括以下步骤:
将90kg均聚聚丙烯、10kg长支链聚丙烯、2kg经偶联剂活化处理过的纳米级滑石粉、1kg硬脂酸、0.5kg抗氧化剂1010和8kg粉色的色母粒加入低温高速混合机,混合均匀,再将物料用自动喂料***以10kg/h的速度转入三螺杆挤出机,在三螺杆挤出机的机筒均化段设置加注口,将超临界二氧化碳以800g/h的速度注入到机筒中,经熔体泵提高和稳定模口压力,通过机头口模发泡,控制口模压力为17MPa,口模温度为125℃,模面水环热切造粒,脱水干燥,过筛,得到发泡聚丙烯珠粒;
或者,包括以下步骤:
将85kg嵌段共聚聚丙烯、15kg长支链聚丙烯、2kg经偶联剂活化处理过的纳米级滑石粉、2kg硬脂酸和0.5kg抗氧化剂1010加入低温高速混合机,混合均匀,再将物料用自动喂料***以10kg/h的速度转入三螺杆挤出机,在三螺杆挤出机的机筒均化段设置加注口,将超临界二氧化碳以900g/h的速度注入到机筒中,经熔体泵提高和稳定模口压力,通过机头口模发泡,控制口模压力为18MPa,口模温度为146℃,模面水环热切造粒,脱水干燥,过筛,得到发泡聚丙烯珠粒。
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