CN105382992A - 一种耐热阻尼增强改性tpu复合材料的制备方法 - Google Patents
一种耐热阻尼增强改性tpu复合材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种耐热阻尼增强改性TPU复合材料的制备方法,包括如下步骤:(1)制备热还原石墨烯;(2)偶联改性硅藻土和蒙脱土;(3)一次混料;(4)二次混料;(5)挤出造粒;(6)注塑成型。本发明一种耐热阻尼增强改性TPU复合材料的制备方法,通过合理的工艺设计,有效改善了各组分与基体TPU之间的分散性,所制备的复合材料的阻尼性能提高,同时耐热性和力学性能均得到改善,综合性能优异,有助于进一步扩大TPU材料的应用领域。
Description
技术领域
本发明涉及TPU复合材料领域,特别是涉及一种耐热阻尼增强改性TPU复合材料的制备方法。
背景技术
热塑性聚氨酯(TPU)具有独特的微相分离结构,模量和强度高,密度较小,易于浇注,与金属的粘合性能良好,同时具有较好的加工性能,在国防、民用工业等方面得到广泛应用。但TPU的耐热性和阻尼性欠佳,限制了其进一步应用。
发明内容
本发明主要解决的技术问题是提供一种耐热阻尼增强改性TPU复合材料的制备方法。
为解决上述技术问题,本发明采用的一个技术方案是:提供一种耐热阻尼增强改性TPU复合材料的制备方法,包括如下步骤:
(1)制备热还原石墨烯:在惰性气体氛围下,于900~1000℃的马弗炉中烧结20~30s,然后在惰性气体氛围下随炉冷却至室温,得到热还原石墨烯,备用;
(2)偶联改性硅藻土和蒙脱土:将硅藻土和蒙脱土按比例加入高速混合机中搅拌混匀,然后分三次加入用环己烷稀释的硅烷偶联剂,经高速搅拌改性后挥发掉环己烷,得到偶联改性硅藻土和蒙脱土;
(3)一次混料:向密炼机中加入50重量份的TPU颗粒和0.5~1重量份步骤(1)中制备的热还原石墨烯,密炼混合3~5min,得到一次混合基料;
(4)二次混料:向步骤(3)的密炼机中再加入50重量份的TPU颗粒,使其与所述一次混合基料密炼混合3~5min,得二次混合剂料;然后再向其中加入1~3重量份受阻酚和30~40重量份步骤(2)中得到的偶联改性硅藻土和蒙脱土,密炼混合5~10min后出料;
(5)挤出造粒:将步骤(4)中得到的混合物料用双螺杆挤出机挤出造粒;
(6)注塑成型:将步骤(5)中得到的粒料用注塑机注塑成型,得到所述耐热阻尼增强改性TPU复合材料。
在本发明一个较佳实施例中,所述步骤(2)中,所述硅藻土和蒙脱土的加入比例为3~5:2~3;所述硅烷偶联剂的用量为所述硅藻土和蒙脱土总重量的1/10,所述硅烷偶联剂和环己烷的稀释比例为1:50~100。
在本发明一个较佳实施例中,所述步骤(2)中,所述改性条件为:先在30~50℃下,以400~600r/min的速率搅拌1~2h;再在60~80℃下,以800~1000r/min的速率搅拌20~40。
在本发明一个较佳实施例中,所述步骤(3)和(4)中,所述密炼条件为:转速50~150r/min,温度80~100℃。
在本发明一个较佳实施例中,所述步骤(5)中,所述挤出机的螺杆转速为100~120r/min,挤出温度范围为200~225℃。
在本发明一个较佳实施例中,所述步骤(6)中,所述注塑机的螺杆转速为50~70r/min,注塑温度为200~225℃。
本发明的有益效果是:本发明一种耐热阻尼增强改性TPU复合材料的制备方法,通过合理的工艺设计,有效改善了各组分与基体TPU之间的分散性,所制备的复合材料的阻尼性能提高,同时耐热性和力学性能均得到改善,综合性能优异,有助于进一步扩大TPU材料的应用领域。
具体实施方式
下面对本发明的较佳实施例进行详细阐述,以使本发明的优点和特征能更易于被本领域技术人员理解,从而对本发明的保护范围做出更为清楚明确的界定。
本发明实施例包括:
实施例1
一种耐热阻尼增强改性TPU复合材料的制备方法,具体步骤如下:
(1)制备热还原石墨烯:在惰性气体氛围下,于900℃的马弗炉中烧结30s,然后在惰性气体氛围下随炉冷却至室温,得到热还原石墨烯,备用;
(2)偶联改性硅藻土和蒙脱土:将硅藻土和蒙脱土按3:2的质量比例加入高速混合机中搅拌2~3min至混匀,然后分三次加入用环己烷稀释的硅烷偶联剂,其中,硅烷偶联剂的用量为所述硅藻土和蒙脱土总重量的1/10,所述硅烷偶联剂和环己烷按1:100的质量比例进行稀释;当所有的偶联剂加入完后,进行偶联处理,具体为先在30℃下,以600r/min的速率搅拌2h,使硅藻土和蒙脱土与偶联剂充分混合并进行偶联处理,然后再在60℃下,以1000r/min的速率高速搅拌40min,一方面有助于进一步混合和偶联处理,另一方面使得环己烷充分挥发;
(3)一次混料:向密炼机中加入50重量份的TPU颗粒和0.5重量份步骤(1)中制备的热还原石墨烯,在80℃,150r/min的条件下密炼混合3min,得到一次混合基料;
(4)二次混料:向步骤(3)的密炼机中再加入50重量份的TPU颗粒,使其与所述一次混合基料在80℃,150r/min的条件下密炼混合3min,得二次混合剂料;然后再向其中加入3重量份受阻酚和40重量份步骤(2)中得到的偶联改性硅藻土和蒙脱土,在相同的条件下密炼混合5min后出料;
(5)挤出造粒:将步骤(4)中得到的混合物料用双螺杆挤出机在100r/min的螺杆转速和200~225℃的挤出温度下挤出造粒;
(6)注塑成型:将步骤(5)中得到的粒料用注塑机注塑成型,得到所述耐热阻尼增强改性TPU复合材料,其中,注塑机的螺杆转速为50r/min,注塑温度为200~225℃。
实施例2
一种耐热阻尼增强改性TPU复合材料的制备方法,具体步骤如下:
(1)制备热还原石墨烯:在惰性气体氛围下,于1000℃的马弗炉中烧结20s,然后在惰性气体氛围下随炉冷却至室温,得到热还原石墨烯,备用;
(2)偶联改性硅藻土和蒙脱土:将硅藻土和蒙脱土按5:3的质量比例加入高速混合机中搅拌2~3min至混匀,然后分三次加入用环己烷稀释的硅烷偶联剂,其中,硅烷偶联剂的用量为所述硅藻土和蒙脱土总重量的1/10,所述硅烷偶联剂和环己烷按1:50的质量比例进行稀释;当所有的偶联剂加入完后,进行偶联处理,具体为先在50℃下,以400r/min的速率搅拌1h,使硅藻土和蒙脱土与偶联剂充分混合并进行偶联处理,然后再在80℃下,以800r/min的速率高速搅拌20min,一方面有助于进一步混合和偶联处理,另一方面使得环己烷充分挥发;
(3)一次混料:向密炼机中加入50重量份的TPU颗粒和1重量份步骤(1)中制备的热还原石墨烯,在100℃,50r/min的条件下密炼混合5min,得到一次混合基料;
(4)二次混料:向步骤(3)的密炼机中再加入50重量份的TPU颗粒,使其与所述一次混合基料在100℃,50r/min的条件下密炼混合5min,得二次混合剂料;然后再向其中加入1重量份受阻酚和30重量份步骤(2)中得到的偶联改性硅藻土和蒙脱土,在相同的条件下密炼混合10min后出料;
(5)挤出造粒:将步骤(4)中得到的混合物料用双螺杆挤出机在120r/min的螺杆转速和200~225℃的挤出温度下挤出造粒;
(6)注塑成型:将步骤(5)中得到的粒料用注塑机注塑成型,得到所述耐热阻尼增强改性TPU复合材料,其中,注塑机的螺杆转速为70r/min,注塑温度为200~225℃。
上述方法所述制备的耐热阻尼增强改性TPU复合材料失重30%时的热分解温度为359~362℃,与纯TPU材料相比,其损耗锋向高温方向移动,力学综合性能提高20~23%。
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。
Claims (6)
1.一种耐热阻尼增强改性TPU复合材料的制备方法,其特征在于,包括如下步骤:
(1)制备热还原石墨烯:在惰性气体氛围下,于900~1000℃的马弗炉中烧结20~30s,然后在惰性气体氛围下随炉冷却至室温,得到热还原石墨烯,备用;
(2)偶联改性硅藻土和蒙脱土:将硅藻土和蒙脱土按比例加入高速混合机中搅拌混匀,然后分三次加入用环己烷稀释的硅烷偶联剂,经高速搅拌改性后挥发掉环己烷,得到偶联改性硅藻土和蒙脱土;
(3)一次混料:向密炼机中加入50重量份的TPU颗粒和0.5~1重量份步骤(1)中制备的热还原石墨烯,密炼混合3~5min,得到一次混合基料;
(4)二次混料:向步骤(3)的密炼机中再加入50重量份的TPU颗粒,使其与所述一次混合基料密炼混合3~5min,得二次混合剂料;然后再向其中加入1~3重量份受阻酚和30~40重量份步骤(2)中得到的偶联改性硅藻土和蒙脱土,密炼混合5~10min后出料;
(5)挤出造粒:将步骤(4)中得到的混合物料用双螺杆挤出机挤出造粒;
(6)注塑成型:将步骤(5)中得到的粒料用注塑机注塑成型,得到所述耐热阻尼增强改性TPU复合材料。
2.根据权利要求1所述的耐热阻尼增强改性TPU复合材料的制备方法,其特征在于,所述步骤(2)中,所述硅藻土和蒙脱土的加入比例为3~5:2~3;所述硅烷偶联剂的用量为所述硅藻土和蒙脱土总重量的1/10,所述硅烷偶联剂和环己烷的稀释比例为1:50~100。
3.根据权利要求1所述的耐热阻尼增强改性TPU复合材料的制备方法,其特征在于,所述步骤(2)中,所述改性条件为:先在30~50℃下,以400~600r/min的速率搅拌1~2h;再在60~80℃下,以800~1000r/min的速率搅拌20~40。
4.根据权利要求1所述的耐热阻尼增强改性TPU复合材料的制备方法,其特征在于,所述步骤(3)和(4)中,所述密炼条件为:转速50~150r/min,温度80~100℃。
5.根据权利要求1所述的耐热阻尼增强改性TPU复合材料的制备方法,其特征在于,所述步骤(5)中,所述挤出机的螺杆转速为100~120r/min,挤出温度范围为200~225℃。
6.根据权利要求1所述的耐热阻尼增强改性TPU复合材料的制备方法,其特征在于,所述步骤(6)中,所述注塑机的螺杆转速为50~70r/min,注塑温度为200~225℃。
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