CN108299581B - 一种交联聚苯乙烯保温材料的制备方法 - Google Patents

一种交联聚苯乙烯保温材料的制备方法 Download PDF

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CN108299581B
CN108299581B CN201710753325.0A CN201710753325A CN108299581B CN 108299581 B CN108299581 B CN 108299581B CN 201710753325 A CN201710753325 A CN 201710753325A CN 108299581 B CN108299581 B CN 108299581B
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Abstract

本发明公开了一种交联聚苯乙烯保温材料的制备方法,本发明采用三聚氰胺处理蒙脱土,然后通过丙烯酸与四甲基二硅氧烷的交联反应,将蒙脱土有效的分散到聚合物溶液中,有效的降低了团聚,改善了蒙脱土与聚合物间的相容性,提高了成品材料的稳定性。

Description

一种交联聚苯乙烯保温材料的制备方法
技术领域
本发明属于材料领域,具体涉及一种交联聚苯乙烯保温材料的制备方法。
背景技术
聚苯乙烯电绝缘性较好,无色透明,透光率仅次于有机玻璃,着色性耐水性,化学稳定性良好,强度一般,但质脆,易产生应力脆裂。聚苯乙烯树脂组合物由于具有优异的加工性能、力学性能和耐热性能,在打印机、复印机、计算机等办公设备壳体领域或家电领域得到广泛的应用;发泡聚苯乙烯树脂的用途也非常广泛,由于其具有高强度、质量轻、极佳的保温绝热性能和高吸收能量能力,可以用作各种仪表、贵重物品、精密仪器、蔬 菜水果和水产品等的包装材料;而因为其具有热传导率低、吸水性小、电绝缘性好、隔音、防潮以及成型工艺简单等优良特性,而被广泛应用在道路桥梁的路基铺设和房屋建筑以及渔业捕捞和冷藏行业的保温材料等方面。其中,作为一种优良的建筑材料,发泡聚苯乙烯树脂主要用于建筑物的屋面和墙体,其作为外保温复合墙体具有十分良好的节能效果;而作为保温屋面适用于住宅、工厂、平式和柏油屋面,可以起到隔音、挡水蒸汽、密封和保温隔热等作用;
然而,目前为了提高聚苯乙烯保温材料的自身强度、保温等性能,通常会引入无机填料,然而无机填料与聚合物基体的相容性较差,容易导致成品的稳定性降低。
发明内容
本发明的目的在于针对现有技术中聚苯乙烯材料的力学性能差的问题,提供一种交联聚苯乙烯保温材料的制备方法。
为实现上述目的,本发明采用以下技术方案:
一种交联聚苯乙烯保温材料的制备方法,包括以下步骤:
(1)取2-3重量份的引发剂,加入到其重量20-30倍的去离子水中,搅拌均匀;
(2)取4-7重量份的丙烯酸、110-120重量份的苯乙烯混合,加入到混合料重量13-20倍的去离子水中,搅拌均匀,送入到反应釜中,通入氮气,调节反应釜温度为60-65℃,滴加上述引发剂溶液,滴加完毕后保温搅拌3-4小时,出料冷却,得酸性聚合物溶液;
(3)取13-20重量份的蒙脱土粉,在700-800℃下煅烧1-2小时,冷却后磨成细粉,与1-2重量份的三聚氰胺混合,加入到混合料重量1.5-2倍的无水乙醇中,搅拌均匀,升高温度为50-60℃,保温搅拌20-30分钟,蒸馏除去乙醇,常温干燥,得氰胺化蒙脱土;
(4)取0.3-1重量份的叔丁基对二苯酚,加入到其重量16-20倍的异丙醇中,搅拌均匀,加入3-4重量份的四甲基二硅氧烷,在50-60℃下保温搅拌20-30分钟,得硅烷醇分散液;
(5)取上述氰胺化蒙脱土,加入到上述硅烷醇分散液中,超声10-20分钟,与上述酸性聚合物溶液混合,搅拌均匀,加入0.04-0.05重量份的二氧化铂,在40-50℃下保温反应10-15小时,得交联聚合物溶液;
(6)取上述交联聚合物溶液,加入1-2重量份的硬脂酸锌、3-4重量份的增塑剂,在90-95℃下保温搅拌15-20分钟,过滤,将沉淀水洗,真空50-60℃下干燥1-2小时,与10-13重量份的ac发泡剂混合,升高温度为110-120℃,保温1-2小时,冷却出料,将产物经过洗涤、干燥、筛分后送入到发泡机中,在0.25-0.3Mpa、130-140℃下蒸汽加热1-2小时,出料,室温冷却,冷却,即得所述交联聚苯乙烯保温材料。
所述的一种交联聚苯乙烯保温材料的制备方法,所述的引发剂为过硫酸铵、过硫酸钠、过硫酸钾中的一种。
所述的一种交联聚苯乙烯保温材料的制备方法,所述的增塑剂为邻苯二甲酸丁苄酯、柠檬酸三丁酯、氯化石蜡中的一种。
本发明的优点:
本发明以苯乙烯为单体,通过丙烯酸掺杂,在引发剂作用下聚合,得到酸性聚合物溶液;然后采用三聚氰胺处理蒙脱土,得氰胺化蒙脱土,再将四甲基二硅氧烷分散到异丙醇中,与含有丙烯酸的聚合物溶液共混,以二氧化铂为催化剂,得交联聚合物溶液;
本发明采用三聚氰胺处理蒙脱土,然后通过丙烯酸与四甲基二硅氧烷的交联反应,将蒙脱土有效的分散到聚合物溶液中,有效的降低了团聚,改善了蒙脱土与聚合物间的相容性,提高了成品材料的力学性能,增强了成品的稳定性强度。
具体实施方式
实施例1
一种交联聚苯乙烯保温材料的制备方法,包括以下步骤:
(1)取3重量份的引发剂,加入到其重量20倍的去离子水中,搅拌均匀;
(2)取4重量份的丙烯酸、120重量份的苯乙烯混合,加入到混合料重量13倍的去离子水中,搅拌均匀,送入到反应釜中,通入氮气,调节反应釜温度为65℃,滴加上述引发剂溶液,滴加完毕后保温搅拌4小时,出料冷却,得酸性聚合物溶液;
(3)取20重量份的蒙脱土粉,在700℃下煅烧2小时,冷却后磨成细粉,与2重量份的三聚氰胺混合,加入到混合料重量1.5倍的无水乙醇中,搅拌均匀,升高温度为60℃,保温搅拌20分钟,蒸馏除去乙醇,常温干燥,得氰胺化蒙脱土;
(4)取0.3重量份的叔丁基对二苯酚,加入到其重量20倍的异丙醇中,搅拌均匀,加入4重量份的四甲基二硅氧烷,在50℃下保温搅拌30分钟,得硅烷醇分散液;
(5)取上述氰胺化蒙脱土,加入到上述硅烷醇分散液中,超声20分钟,与上述酸性聚合物溶液混合,搅拌均匀,加入0.04重量份的二氧化铂,在40℃下保温反应15小时,得交联聚合物溶液;
(6)取上述交联聚合物溶液,加入1重量份的硬脂酸锌、3重量份的增塑剂,在90℃下保温搅拌15分钟,过滤,将沉淀水洗,真空50℃下干燥1小时,与10重量份的ac发泡剂混合,升高温度为110℃,保温1小时,冷却出料,将产物经过洗涤、干燥、筛分后送入到发泡机中,在0.25Mpa、130℃下蒸汽加热1-2小时,出料,室温冷却,冷却,即得所述交联聚苯乙烯保温材料。
所述的引发剂为过硫酸钾。
所述的增塑剂为氯化石蜡。
实施例2
一种交联聚苯乙烯保温材料的制备方法,包括以下步骤:
(1)取2重量份的引发剂,加入到其重量30倍的去离子水中,搅拌均匀;
(2)取7重量份的丙烯酸、120重量份的苯乙烯混合,加入到混合料重量20倍的去离子水中,搅拌均匀,送入到反应釜中,通入氮气,调节反应釜温度为65℃,滴加上述引发剂溶液,滴加完毕后保温搅拌4小时,出料冷却,得酸性聚合物溶液;
(3)取20重量份的蒙脱土粉,在800℃下煅烧2小时,冷却后磨成细粉,与2重量份的三聚氰胺混合,加入到混合料重量2倍的无水乙醇中,搅拌均匀,升高温度为60℃,保温搅拌30分钟,蒸馏除去乙醇,常温干燥,得氰胺化蒙脱土;
(4)取1重量份的叔丁基对二苯酚,加入到其重量20倍的异丙醇中,搅拌均匀,加入4重量份的四甲基二硅氧烷,在60℃下保温搅拌30分钟,得硅烷醇分散液;
(5)取上述氰胺化蒙脱土,加入到上述硅烷醇分散液中,超声20分钟,与上述酸性聚合物溶液混合,搅拌均匀,加入0.05重量份的二氧化铂,在50℃下保温反应15小时,得交联聚合物溶液;
(6)取上述交联聚合物溶液,加入2重量份的硬脂酸锌、4重量份的增塑剂,在95℃下保温搅拌20分钟,过滤,将沉淀水洗,真空60℃下干燥2小时,与13重量份的ac发泡剂混合,升高温度为120℃,保温2小时,冷却出料,将产物经过洗涤、干燥、筛分后送入到发泡机中,在0.3Mpa、140℃下蒸汽加热2小时,出料,室温冷却,冷却,即得所述交联聚苯乙烯保温材料。
所述的引发剂为过硫酸钠。
所述的增塑剂为柠檬酸三丁酯。
实施例3
一种交联聚苯乙烯保温材料的制备方法,其特征在于,包括以下步骤:
(1)取2重量份的引发剂,加入到其重量25倍的去离子水中,搅拌均匀;
(2)取5重量份的丙烯酸、115重量份的苯乙烯混合,加入到混合料重量15倍的去离子水中,搅拌均匀,送入到反应釜中,通入氮气,调节反应釜温度为62℃,滴加上述引发剂溶液,滴加完毕后保温搅拌3小时,出料冷却,得酸性聚合物溶液;
(3)取16重量份的蒙脱土粉,在750℃下煅烧1小时,冷却后磨成细粉,与1-2重量份的三聚氰胺混合,加入到混合料重量1.8倍的无水乙醇中,搅拌均匀,升高温度为55℃,保温搅拌25分钟,蒸馏除去乙醇,常温干燥,得氰胺化蒙脱土;
(4)取0.7重量份的叔丁基对二苯酚,加入到其重量18倍的异丙醇中,搅拌均匀,加入3重量份的四甲基二硅氧烷,在54℃下保温搅拌24分钟,得硅烷醇分散液;
(5)取上述氰胺化蒙脱土,加入到上述硅烷醇分散液中,超声15分钟,与上述酸性聚合物溶液混合,搅拌均匀,加入0.04重量份的二氧化铂,在45℃下保温反应12小时,得交联聚合物溶液;
(6)取上述交联聚合物溶液,加入1重量份的硬脂酸锌、3重量份的增塑剂,在92℃下保温搅拌15-20分钟,过滤,将沉淀水洗,真空55℃下干燥1小时,与12重量份的ac发泡剂混合,升高温度为115℃,保温1小时,冷却出料,将产物经过洗涤、干燥、筛分后送入到发泡机中,在0.27Mpa、135℃下蒸汽加热1小时,出料,室温冷却,冷却,即得所述交联聚苯乙烯保温材料。
所述的引发剂为过硫酸铵。
所述的增塑剂为邻苯二甲酸丁苄酯。
性能测试:
将本实施例1-3的交联聚苯乙烯保温材料,与市售聚苯乙烯发泡材料的力学性能、保温性能进行对比测试,结果表明:
实施例1的交联聚苯乙烯保温材料弯曲强度 0.46Mpa,压缩强度 0.24Mpa,导热系数 0.030w/m.k;
实施例2的交联聚苯乙烯保温材料弯曲强度 0.51Mpa,压缩强度 0.27Mpa,导热系数 0.033w/m.k;
实施例3的交联聚苯乙烯保温材料弯曲强度 0.48Mpa,压缩强度 0.23Mpa,导热系数 0.035w/m.k;
市售聚苯乙烯发泡材料的弯曲强度 0.25Mpa,压缩强度 0.17Mpa,导热系数0.057w/m.k。

Claims (3)

1.一种交联聚苯乙烯保温材料的制备方法,其特征在于,包括以下步骤:
(1)取2-3重量份的引发剂,加入到其重量20-30倍的去离子水中,搅拌均匀;
(2)取4-7重量份的丙烯酸、110-120重量份的苯乙烯混合,加入到混合料重量13-20倍的去离子水中,搅拌均匀,送入到反应釜中,通入氮气,调节反应釜温度为60-65℃,滴加上述引发剂溶液,滴加完毕后保温搅拌3-4小时,出料冷却,得酸性聚合物溶液;
(3)取13-20重量份的蒙脱土粉,在700-800℃下煅烧1-2小时,冷却后磨成细粉,与1-2重量份的三聚氰胺混合,加入到混合料重量1.5-2倍的无水乙醇中,搅拌均匀,升高温度为50-60℃,保温搅拌20-30分钟,蒸馏除去乙醇,常温干燥,得氰胺化蒙脱土;
(4)取0.3-1重量份的叔丁基对二苯酚,加入到其重量16-20倍的异丙醇中,搅拌均匀,加入3-4重量份的四甲基二硅氧烷,在50-60℃下保温搅拌20-30分钟,得硅烷醇分散液;
(5)取上述氰胺化蒙脱土,加入到上述硅烷醇分散液中,超声10-20分钟,与上述酸性聚合物溶液混合,搅拌均匀,加入0.04-0.05重量份的二氧化铂,在40-50℃下保温反应10-15小时,得交联聚合物溶液;
(6)取上述交联聚合物溶液,加入1-2重量份的硬脂酸锌、3-4重量份的增塑剂,在90-95℃下保温搅拌15-20分钟,过滤,将沉淀水洗,真空50-60℃下干燥1-2小时,与10-13重量份的ac发泡剂混合,升高温度为110-120℃,保温1-2小时,冷却出料,将产物经过洗涤、干燥、筛分后送入到发泡机中,在0.25-0.3Mpa、130-140℃下蒸汽加热1-2小时,出料,室温冷却,冷却,即得所述交联聚苯乙烯保温材料。
2.根据权利要求1所述的一种交联聚苯乙烯保温材料的制备方法,其特征在于,所述的引发剂为过硫酸铵、过硫酸钠、过硫酸钾中的一种。
3.根据权利要求1所述的一种交联聚苯乙烯保温材料的制备方法,其特征在于,所述的增塑剂为邻苯二甲酸丁苄酯、柠檬酸三丁酯、氯化石蜡中的一种。
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