CN111793301A - 一种气凝胶发泡材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种气凝胶发泡材料,按照重量份计,包括以下原料:A组分填料50‑70份、B组分填料40‑60份,A组分填料按照重量份计,包括以下原料:无水乙醇20‑30份、醋酸30‑35份、pH调节剂10‑20份、去离子水30‑40份,B组分填料按照重量份计,包括以下原料:可发泡弹性体100‑170份、异氰酸酯50‑60份、气凝胶粉末10‑40份、玻璃纤维10‑16份、发泡剂5‑10份、抗氧剂2‑5份、促进剂2‑3份、泡沫稳定剂1‑2份、交联剂0.2‑0.6份、增塑剂4‑8份。该气凝胶发泡材料及其制备方法有效提高发泡材料保温性能,降低发泡材料应用体积,在需保温的单位面积上,对比传统的发泡材料,该气凝胶发泡材料能以明显的轻薄优势达到同样的保温性能;而且而且加入了阻燃剂,使得制备的气凝胶发泡材料的阻燃效果更好。
Description
技术领域
本发明属于发泡材料技术领域,具体涉及一种气凝胶发泡材料及其制备方法。
背景技术
发泡材料相对普遍存在的密实材料而言,其共同特点是密度小,质量轻,比面积大,力学性能高,阻尼性能好。发泡材料按基体不同分为金属发泡材料、陶瓷玻璃发泡材料、木材发泡材料、高分子泡沫材料,而高分子泡沫材料又包括塑料发泡材料和橡胶发泡材料。对于橡塑发泡材料,其具有优异的缓冲、压缩、密封、隔热、隔音等性能,可将它作为缓冲、衬垫、隔热、密封、防水、减震等材料,在机动车、石油化工、机械建筑、航空航天、纺织、包装等领域获得了广泛应用。
在专利CN201910783676.5一种抗寒保暖用二氧化硅气凝胶发泡材料,由改性聚氯乙烯、溴化丁基橡胶、丙烯酸酯橡胶,乙烯三元共聚物、无机纳米粒子熔融捏合制得的可发泡弹性体与二氧化硅气凝胶和其他助剂共混发泡制得的发泡材料不仅保暖性好、质量轻、弹性好,还兼具抗寒、耐磨等性能。同时,改性聚氯乙烯交联后形成网状结构,有效抑制小分子增塑剂的迁移和逸出,提高发泡材料的力学性能和稳定性。虽然解决了发泡材料力学性能和稳定性的问题,但是仍然存在保温效果差、阻燃效果差的问题,给使用带来不便,所以我们需要一款新型的凝胶发泡材料来解决上述问题问题,满足人们的需求。
发明内容
本发明的目的在于提供一种气凝胶发泡材料及其制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:一种气凝胶发泡材料,按照重量份计,包括以下原料:A组分填料50-70份、B组分填料40-60份,A组分填料按照重量份计,包括以下原料:无水乙醇20-30份、醋酸30-35份、pH调节剂10-20份、去离子水30-40份,B组分填料按照重量份计,包括以下原料:可发泡弹性体100-170份、异氰酸酯50-60份、气凝胶粉末10-40份、玻璃纤维10-16份、发泡剂5-10份、抗氧剂2-5份、促进剂2-3份、泡沫稳定剂1-2份、交联剂0.2-0.6份、增塑剂4-8份、阻燃剂5-8份。
优选的是,所述可发泡弹性体以重量份计,包括以下组分:改性聚氯乙烯30-40份、溴化丁基橡胶20-40份、丙烯酸酯橡胶10-30份、乙烯三元共聚物2-15份、无机纳米粒子1-3份,且在160-180℃下熔融捏合得到。
上述任一方案中优选的是,所述改性聚氯乙烯制备原料中包括氯乙烯和二丙-2-烯基苯-1,4-二羧酸酯,且二者的质量比为5:1-15:1。
上述任一方案中优选的是,所述乙烯三元共聚物为乙烯-醋酸乙烯酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-缩水甘油酯的三元共聚物中的一种或多种的组合。
上述任一方案中优选的是,所述无机纳米粒子为纳米二氧化硅、纳米碳酸钙中的一种或两种组合。
上述任一方案中优选的是,所述玻璃纤维为经过硅烷偶联剂KH550处理过。
上述任一方案中优选的是,所述气凝胶粉末的直径不大于3μm。
上述任一方案中优选的是,所述异氰酸酯为脂肪族二异氰酸酯、脂环族二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸、多亚甲基多苯基异氰酸酯中的一种或多种的组合。
一种气凝胶发泡材料的其制备方法,按照先后顺序包括以下步骤:
S1:制备A溶液:搅拌罐内保持25℃,向其中加入A组分填料,具体添加顺序为先加入去离子水,边加入边搅拌,然后依次加入无水乙醇、醋酸和pH调节剂,混匀后得pH为6.8-7.0的A溶液;
S2:制备B溶液:向开炼机中加入B组分填料,具体添加顺序为按配方称取可发泡弹性体置于开炼机中开炼,开炼机的温度以10℃/min的速率升温,达到180℃,停止升温,此时加入气凝胶粉末和玻璃纤维,接着以2℃/min的速率进行升温,达到190℃后停止升温,然后再依次加入发泡剂、抗氧剂、促进剂、泡沫稳定剂、交联剂和增塑剂,边加入边搅拌,当全部加入后停止搅拌,并以2℃/min的速率进行升温,达到200℃后停止升温,得B溶液;
S3:将上述B溶液降温,降到25℃后向其加入S1步骤中的A溶液,边加入边搅拌,在加入A溶液的同时向其加入甲酰胺,经过醇洗后置于平板硫化机中定型、冷压出片,得料片;
S4:将上述步骤中的料片置于模具中,放入硫化压片机中进行模压发泡,以10℃/min的速率升温,升至180-190℃后停止升温,然后保持15-30min进行发泡,发泡结束后关闭硫化压片机,取出模具,待冷却后得到气凝胶发泡材料。
优选的是,所述步骤S4中发泡压力设置为9-14MPa。
本发明的技术效果和优点:该气凝胶发泡材料及其制备方法有效提高发泡材料保温性能,降低发泡材料应用体积,在需保温的单位面积上,对比传统的发泡材料,该气凝胶发泡材料能以明显的轻薄优势达到同样的保温性能;而且加入了阻燃剂,使得制备的气凝胶发泡材料的阻燃效果更好。
具体实施方式
下面将结合本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1:
一种气凝胶发泡材料,按照重量份计,包括以下原料:A组分填料50份、B组分填料40份,A组分填料按照重量份计,包括以下原料:无水乙醇20份、醋酸30份、pH调节剂10份、去离子水30份,B组分填料按照重量份计,包括以下原料:可发泡弹性体100份、可发泡弹性体以重量份计,包括以下组分:改性聚氯乙烯30-40份、改性聚氯乙烯制备原料中包括氯乙烯和二丙-2-烯基苯-1,4-二羧酸酯,且二者的质量比为5:1-15:1,溴化丁基橡胶20-40份、丙烯酸酯橡胶10-30份、乙烯三元共聚物2-15份、乙烯三元共聚物为乙烯-醋酸乙烯酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-缩水甘油酯的三元共聚物中的一种或多种的组合,无机纳米粒子1-3份,无机纳米粒子为纳米二氧化硅、纳米碳酸钙中的一种或两种组合,且在160-180℃下熔融捏合得到,异氰酸酯50份、异氰酸酯为脂肪族二异氰酸酯、脂环族二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸、多亚甲基多苯基异氰酸酯中的一种或多种的组合,气凝胶粉末10份、气凝胶粉末的直径不大于3μm,玻璃纤维10份、玻璃纤维为经过硅烷偶联剂KH550处理过,发泡剂5份、抗氧剂2份、促进剂2份、泡沫稳定剂1份、交联剂0.2份、增塑剂4份、阻燃剂5份。
实施例2:
一种气凝胶发泡材料,按照重量份计,包括以下原料:A组分填料60份、B组分填料50份,A组分填料按照重量份计,包括以下原料:无水乙醇25份、醋酸32份、pH调节剂15份、去离子水35份,B组分填料按照重量份计,包括以下原料:可发泡弹性体135份、可发泡弹性体以重量份计,包括以下组分:改性聚氯乙烯30-40份、改性聚氯乙烯制备原料中包括氯乙烯和二丙-2-烯基苯-1,4-二羧酸酯,且二者的质量比为5:1-15:1,溴化丁基橡胶20-40份、丙烯酸酯橡胶10-30份、乙烯三元共聚物2-15份、乙烯三元共聚物为乙烯-醋酸乙烯酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-缩水甘油酯的三元共聚物中的一种或多种的组合,无机纳米粒子1-3份,无机纳米粒子为纳米二氧化硅、纳米碳酸钙中的一种或两种组合,且在160-180℃下熔融捏合得到,异氰酸酯55份、异氰酸酯为脂肪族二异氰酸酯、脂环族二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸、多亚甲基多苯基异氰酸酯中的一种或多种的组合,气凝胶粉末25份、气凝胶粉末的直径不大于3μm,玻璃纤维13份、玻璃纤维为经过硅烷偶联剂KH550处理过,发泡剂7份、抗氧剂3份、促进剂2.5份、泡沫稳定剂1.5份、交联剂0.4份、增塑剂6份、阻燃剂7份。
实施例3:
一种气凝胶发泡材料,按照重量份计,包括以下原料:A组分填料70份、B组分填料60份,A组分填料按照重量份计,包括以下原料:无水乙醇30份、醋酸35份、pH调节剂20份、去离子水40份,B组分填料按照重量份计,包括以下原料:可发泡弹性体170份、可发泡弹性体以重量份计,包括以下组分:改性聚氯乙烯30-40份、改性聚氯乙烯制备原料中包括氯乙烯和二丙-2-烯基苯-1,4-二羧酸酯,且二者的质量比为5:1-15:1,溴化丁基橡胶20-40份、丙烯酸酯橡胶10-30份、乙烯三元共聚物2-15份、乙烯三元共聚物为乙烯-醋酸乙烯酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-缩水甘油酯的三元共聚物中的一种或多种的组合,无机纳米粒子1-3份,无机纳米粒子为纳米二氧化硅、纳米碳酸钙中的一种或两种组合,且在160-180℃下熔融捏合得到,异氰酸酯60份、异氰酸酯为脂肪族二异氰酸酯、脂环族二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸、多亚甲基多苯基异氰酸酯中的一种或多种的组合,气凝胶粉末40份、气凝胶粉末的直径不大于3μm,玻璃纤维16份、玻璃纤维为经过硅烷偶联剂KH550处理过,发泡剂10份、抗氧剂5份、促进剂3份、泡沫稳定剂2份、交联剂0.6份、增塑剂8份、阻燃剂8份。
实施例4:
在上述任一实施例中,可发泡弹性体以重量份计,包括以下组分:改性聚氯乙烯30份、改性聚氯乙烯制备原料中包括氯乙烯和二丙-2-烯基苯-1,4-二羧酸酯,且二者的质量比为5:1,溴化丁基橡胶20份、丙烯酸酯橡胶10份、乙烯三元共聚物2份、乙烯三元共聚物为乙烯-醋酸乙烯酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-缩水甘油酯的三元共聚物中的一种或多种的组合,无机纳米粒子1份;
优选的是,可发泡弹性体以重量份计,包括以下组分:改性聚氯乙烯40份、改性聚氯乙烯制备原料中包括氯乙烯和二丙-2-烯基苯-1,4-二羧酸酯,且二者的质量比为15:1,溴化丁基橡胶40份、丙烯酸酯橡胶30份、乙烯三元共聚物15份、乙烯三元共聚物为乙烯-醋酸乙烯酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-缩水甘油酯的三元共聚物中的一种或多种的组合,无机纳米粒子3份
最优选的是,可发泡弹性体以重量份计,包括以下组分:改性聚氯乙烯35份、改性聚氯乙烯制备原料中包括氯乙烯和二丙-2-烯基苯-1,4-二羧酸酯,且二者的质量比为10:1,溴化丁基橡胶30份、丙烯酸酯橡胶20份、乙烯三元共聚物9份、乙烯三元共聚物为乙烯-醋酸乙烯酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-缩水甘油酯的三元共聚物中的一种或多种的组合,无机纳米粒子2份。
实施例5:
一种气凝胶发泡材料的其制备方法,按照先后顺序包括以下步骤:
S1:制备A溶液:搅拌罐内保持25℃,向其中加入A组分填料,具体添加顺序为先加入去离子水,边加入边搅拌,然后依次加入无水乙醇、醋酸和pH调节剂,混匀后得pH为6.8-7.0的A溶液;
S2:制备B溶液:向开炼机中加入B组分填料,具体添加顺序为按配方称取可发泡弹性体置于开炼机中开炼,开炼机的温度以10℃/min的速率升温,达到180℃,停止升温,此时加入气凝胶粉末和玻璃纤维,接着以2℃/min的速率进行升温,达到190℃后停止升温,然后再依次加入发泡剂、抗氧剂、促进剂、泡沫稳定剂、交联剂和增塑剂,边加入边搅拌,当全部加入后停止搅拌,并以2℃/min的速率进行升温,达到200℃后停止升温,得B溶液;
S3:将上述B溶液降温,降到25℃后向其加入S1步骤中的A溶液,边加入边搅拌,在加入A溶液的同时向其加入甲酰胺,经过醇洗后置于平板硫化机中定型、冷压出片,得料片;
S4:将上述步骤中的料片置于模具中,放入硫化压片机中进行模压发泡,以10℃/min的速率升温,升至180-190℃后停止升温,然后保持15-30min、发泡压力设置为9-14MPa进行发泡,发泡结束后关闭硫化压片机,取出模具,待冷却后得到气凝胶发泡材料。
实施例6:
采用实施例1中组分配合实施例5中的制备方法制得气凝胶发泡材料。
实施例7:
采用实施例2中组分配合实施例5中的制备方法制得气凝胶发泡材料。
实施例8:
采用实施例3中组分配合实施例5中的制备方法制得气凝胶发泡材料。
实施例9:
采用实施例4中组分配合实施例5中的制备方法制得气凝胶发泡材料。
表1.实施例6-9所制得的气凝胶发泡材料的性能测试结果。
上述翘曲度的数值为制备得到气凝胶发泡材料时、3个月后、6个月后的测得数据的平均值,从上述数据得出本发明的实施例中气凝胶发泡材料各项性能指标都是优等,说明本发明得到的气凝胶发泡材料具有很好的保温性能,而且气具有良好的力学性能和稳定性,采用了阻燃测试,发现阻燃效果优,说明本发明的气凝胶发泡材料阻燃效果好。
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例揭露如上,然而并非用以限定本发明,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,当可利用上述揭示的方法及技术内容作出些许的更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明技术方案的范围内。
Claims (10)
1.一种气凝胶发泡材料,其特征在于:按照重量份计,包括以下原料:A组分填料50-70份、B组分填料40-60份;
A组分填料按照重量份计,包括以下原料:无水乙醇20-30份、醋酸30-35份、pH调节剂10-20份、去离子水30-40份;
B组分填料按照重量份计,包括以下原料:可发泡弹性体100-170份、异氰酸酯50-60份、气凝胶粉末10-40份、玻璃纤维10-16份、发泡剂5-10份、抗氧剂2-5份、促进剂2-3份、泡沫稳定剂1-2份、交联剂0.2-0.6份、增塑剂4-8份、阻燃剂5-8份。
2.根据权利要求1所述的一种气凝胶发泡材料,其特征在于:所述可发泡弹性体以重量份计,包括以下组分:改性聚氯乙烯30-40份、溴化丁基橡胶20-40份、丙烯酸酯橡胶10-30份、乙烯三元共聚物2-15份、无机纳米粒子1-3份,且在160-180℃下熔融捏合得到。
3.根据权利要求1所述的一种气凝胶发泡材料,其特征在于:所述改性聚氯乙烯制备原料中包括氯乙烯和二丙-2-烯基苯-1,4-二羧酸酯,且二者的质量比为5:1-15:1。
4.根据权利要求1所述的一种气凝胶发泡材料,其特征在于:所述乙烯三元共聚物为乙烯-醋酸乙烯酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-羰基的三元共聚物、乙烯-丙烯酸正丁酯-缩水甘油酯的三元共聚物中的一种或多种的组合。
5.根据权利要求1所述的一种气凝胶发泡材料,其特征在于:所述无机纳米粒子为纳米二氧化硅、纳米碳酸钙中的一种或两种组合。
6.根据权利要求1所述的一种气凝胶发泡材料,其特征在于:所述玻璃纤维为经过硅烷偶联剂KH550处理过。
7.根据权利要求1所述的一种气凝胶发泡材料,其特征在于:所述气凝胶粉末的直径不大于3μm。
8.根据权利要求1所述的一种气凝胶发泡材料,其特征在于:所述异氰酸酯为脂肪族二异氰酸酯、脂环族二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸、多亚甲基多苯基异氰酸酯中的一种或多种的组合。
9.一种根据权利要求1所述的气凝胶发泡材料的其制备方法,其特征在于:按照先后顺序包括以下步骤:
S1:制备A溶液:搅拌罐内保持25℃,向其中加入A组分填料,具体添加顺序为先加入去离子水,边加入边搅拌,然后依次加入无水乙醇、醋酸和pH调节剂,混匀后得pH为6.8-7.0的A溶液;
S2:制备B溶液:向开炼机中加入B组分填料,具体添加顺序为按配方称取可发泡弹性体置于开炼机中开炼,开炼机的温度以10℃/min的速率升温,达到180℃,停止升温,此时加入气凝胶粉末和玻璃纤维,接着以2℃/min的速率进行升温,达到190℃后停止升温,然后再依次加入发泡剂、抗氧剂、促进剂、泡沫稳定剂、交联剂和增塑剂,边加入边搅拌,当全部加入后停止搅拌,并以2℃/min的速率进行升温,达到200℃后停止升温,得B溶液;
S3:将上述B溶液降温,降到25℃后向其加入S1步骤中的A溶液,边加入边搅拌,在加入A溶液的同时向其加入甲酰胺,经过醇洗后置于平板硫化机中定型、冷压出片,得料片;
S4:将上述步骤中的料片置于模具中,放入硫化压片机中进行模压发泡,以10℃/min的速率升温,升至180-190℃后停止升温,然后保持15-30min进行发泡,发泡结束后关闭硫化压片机,取出模具,待冷却后得到气凝胶发泡材料。
10.根据权利要求1所述的一种气凝胶发泡材料的其制备方法,其特征在于:所述步骤S4中发泡压力设置为9-14MPa。
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