CN114456761B - 一种聚氨酯断面密封胶及其制备方法 - Google Patents
一种聚氨酯断面密封胶及其制备方法 Download PDFInfo
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Abstract
本发明公开一种聚氨酯断面密封胶及其制备方法,所述聚氨酯断面密封胶包括以下成分:NCO封端的聚氨酯预聚体;碳酸钙;除水剂;粘接促粘剂;催化剂。所述聚氨酯断面密封胶的制备方法:按比例将NCO封端的聚氨酯预聚体、碳酸钙、除水剂、粘接促粘剂、催化剂加入到搅拌机中,在真空状态下搅拌分散1小时,得到聚氨酯断面密封胶。本发明制得的聚氨酯断面密封胶吸湿性低,可直接添加使用不需烘干,且具有良好的触变性和出色的力学性能。
Description
技术领域
本发明属于装修建材领域,特别涉及一种聚氨酯断面密封胶及其制备方法。
背景技术
系统门窗相比传统铝合金等门窗,具有优异的节能效应,随着建筑节能成为我国发展的主要趋势,使其在市场上强势推进,因此聚氨酯断面密封胶也迎来快速发展。
聚氨酯断面密封胶是系统门窗上的新产品,用于粘接型材角部45°连接处拼缝缝隙,起密封和隔水隔汽作用,能有效解决系统门窗窗角在运输、安装和使用过中开裂、错位、变形和渗漏等诸多问题,从而保证了系统门窗的隔热性、气密性和水密性。因此,它需对铝型材具有良好的粘接性且耐老化性能好。
目前,现有的聚氨酯断面密封胶产品都添加了增塑剂,在室外承受温差变化后,可能会出现渗油导致基材脱离,且会污染相邻材料和相邻组角结构胶,严重可导致结构失效。
发明内容
本发明的目的是提供一种聚氨酯断面密封胶,吸湿性低,可直接添加使用不需烘干,且具有良好的触变性和出色的力学性能。
有必要地,本发明还提供了上述聚氨酯断面密封胶的制备方法。
一种聚氨酯断面密封胶,包括以下成分:
NCO封端的聚氨酯预聚体;
碳酸钙;
除水剂;
粘接促粘剂;
催化剂。
优选地,所述一种聚氨酯断面密封胶,按其重量份包括以下成分:
其中,所述NCO封端的聚氨酯预聚体由聚碳酸亚丙酯二元醇、聚醚三元醇和二异氰酸酯聚合得到,所述聚碳酸亚丙酯二元醇、聚醚三元醇和二异氰酸酯的重量比是(150-800):(700-1200):(203-304);
其中,聚碳酸亚丙酯二元醇的数均分子量为1000-3000,聚醚三元醇的数均分子量为5000-7000;所述聚醚三元醇和聚碳酸亚丙酯二元醇的羟基基团比(1-3):1。
进一步地,所述NCO封端的聚氨酯预聚体由以下方法制备得到:
按比例将聚碳酸亚丙酯二元醇和聚醚三元醇加入至干燥的搅拌釜中边搅拌边升温至60-100℃,再缓慢加入二异氰酸酯,真空下将温度控制在70-90℃,恒温反应3-6h,当-NCO含量达到2-5%后,得到NCO封端的聚氨酯预聚体得到预聚体,更优选地是,当NCO封端的聚氨酯预聚体的-NCO含量为3%,停止反应得到NCO封端的聚氨酯预聚体得到预聚体。
本发明所述的-NCO含量的测试方法是滴定法。
其中,所述粘接促进剂为γ-氨丙基三甲氧基硅烷、二-(γ-三甲氧基甲硅烷基丙基)胺和γ-缩水甘油醚氧丙基三甲氧基硅烷经缩合反应得到,其中γ-氨丙基三甲氧基硅烷、二-(γ-三甲氧基甲硅烷基丙基)胺和γ-缩水甘油醚氧丙基三甲氧基硅烷的基团摩尔比为(2-4):(3-4):1。
优选地,所述粘接促进剂按以下方法制备:
将4重量份的γ-氨丙基三甲氧基硅烷、3重量份的二-(γ-三甲氧基甲硅烷基丙基)胺和1重量份的γ-缩水甘油醚氧丙基三甲氧基硅烷加入到带有搅拌、真空和回流装置的烧瓶中,开启搅拌,升温至120℃聚合3小时,即得到粘接促进剂。
其中,所述除水剂为噁唑烷除水剂和分子筛活化粉中的一种或多种。
其中,所述碳酸钙的含水率≤500ppm。
其中,所述催化剂为铋锌复合催化剂,铋锌元素质量比例为1:(1-5),优选地,铋锌元素质量比例为1:2.5。
一种如上所述的聚氨酯断面密封胶的制备方法:
按比例将NCO封端的聚氨酯预聚体、碳酸钙、除水剂、粘接促粘剂、催化剂加入到搅拌机中,在真空状态下搅拌分散1小时,得到聚氨酯断面密封胶。
相较于现有技术,本发明有以下有益效果:
1)本发明制备的聚氨酯断面密封胶不含溶剂和邻苯类增塑剂,不会出现渗油情况,且符合环保要求。
2)本发明制备的聚氨酯断面密封胶所用粘接促进剂为环氧硅烷偶联剂、仲氨基硅烷偶联剂和叔氨基硅烷在120℃下回流6小时后的共聚物,比单独使用环氧硅烷偶联剂或氨基硅烷偶联剂对铝材的粘接性更好。
3)本发明制备的聚氨酯断面密封胶所用纳米碳酸钙含水率低,吸湿性低,可直接添加使用不需烘干,且具有良好的触变性和出色的力学性能。
具体实施方式
为了使本技术领域的人员更好地理解本发明方案,下面结合具体实施方式对本发明作进一步的详细说明。
本发明所用物质来源如下:
聚碳酸亚丙酯二元醇:惠州大亚湾达志精细化工有限公司;
聚醚三元醇:万华化学集团股份有限公司;
二苯基甲烷二异氰酸酯:市售;
除水剂:
噁唑烷除水剂:苏州湘园新材料股份有限公司;
分子筛活化粉:洛阳建龙微纳新材料股份有限公司;
碳酸钙:欧米亚(上海)投资有限公司,含水率200ppm;
γ-氨丙基三甲氧基硅烷:市售;
二-(γ-三甲氧基甲硅烷基丙基)胺:市售;
γ-缩水甘油醚氧丙基三甲氧基硅烷:市售;
催化剂:型号Valikat ZB8,来源优美科金属国际贸易(上海)有限公司,铋锌元素质量比1:2.5;
其余原料来自市售。
实施例1
1)NCO封端的聚氨酯预聚体的制备:
按表1所示的原料和配比备料,然后将聚碳酸亚丙酯二元醇和聚醚三元醇加入至干燥的搅拌釜中边搅拌边升温至60-100℃,再缓慢加入二异氰酸酯,真空下将温度控制在70-90℃,恒温反应3-6h,当-NCO含量达到3%后,得到NCO封端的聚氨酯预聚体得到预聚体。
2)粘接促进剂的制备:
按表2所示的摩尔份将γ-氨丙基三甲氧基硅烷、二-(γ-三甲氧基甲硅烷基丙基)胺和γ-缩水甘油醚氧丙基三甲氧基硅烷加入到带有搅拌、真空和回流装置的烧瓶中,开启搅拌,升温至120℃聚合3小时,即得到粘接促进剂。
3)聚氨酯断面密封胶的制备:
按表3所示的重量份将制备得到的NCO封端的聚氨酯预聚体、碳酸钙、除水剂、制备得到的粘接促粘剂、催化剂加入到搅拌机中,在真空状态下搅拌分散1小时,得到聚氨酯断面密封胶。
实施例21)NCO封端的聚氨酯预聚体的制备:
按表1所示的原料和配比备料,然后将聚碳酸亚丙酯二元醇和聚醚三元醇加入至干燥的搅拌釜中边搅拌边升温至60-100℃,再缓慢加入二异氰酸酯,真空下将温度控制在70-90℃,恒温反应3-6h,当-NCO含量达到2%后,得到NCO封端的聚氨酯预聚体得到预聚体。
2)粘接促进剂的制备:
按表2所示的摩尔份将γ-氨丙基三甲氧基硅烷、二-(γ-三甲氧基甲硅烷基丙基)胺和γ-缩水甘油醚氧丙基三甲氧基硅烷加入到带有搅拌、真空和回流装置的烧瓶中,开启搅拌,升温至120℃聚合3小时,即得到粘接促进剂。
3)聚氨酯断面密封胶的制备:
按表3所示的重量份将制备得到的NCO封端的聚氨酯预聚体、碳酸钙、除水剂、制备得到的粘接促粘剂、催化剂加入到搅拌机中,在真空状态下搅拌分散1小时,得到聚氨酯断面密封胶。
实施例3
1)NCO封端的聚氨酯预聚体的制备:
按表1所示的原料和配比备料,然后将聚碳酸亚丙酯二元醇和聚醚三元醇加入至干燥的搅拌釜中边搅拌边升温至60-100℃,再缓慢加入二异氰酸酯,真空下将温度控制在70-90℃,恒温反应3-6h,当-NCO含量达到5%后,得到NCO封端的聚氨酯预聚体得到预聚体。
2)粘接促进剂的制备:
按表2所示的摩尔份将γ-氨丙基三甲氧基硅烷、二-(γ-三甲氧基甲硅烷基丙基)胺和γ-缩水甘油醚氧丙基三甲氧基硅烷加入到带有搅拌、真空和回流装置的烧瓶中,开启搅拌,升温至120℃聚合3小时,即得到粘接促进剂。
3)聚氨酯断面密封胶的制备:
按表3所示的重量份将制备得到的NCO封端的聚氨酯预聚体、碳酸钙、除水剂、制备得到的粘接促粘剂、催化剂加入到搅拌机中,在真空状态下搅拌分散1小时,得到聚氨酯断面密封胶。
对比例1
1)NCO封端的聚氨酯预聚体的制备:
按表1所示的原料和配比备料,然后将聚碳酸亚丙酯二元醇和聚醚三元醇加入至干燥的搅拌釜中边搅拌边升温至60-100℃,再缓慢加入二异氰酸酯,真空下将温度控制在70-90℃,恒温反应3-6h,当-NCO含量达到2%后,得到NCO封端的聚氨酯预聚体得到预聚体。
2)粘接促进剂的制备:
按表2所示的摩尔份将γ-氨丙基三甲氧基硅烷和γ-缩水甘油醚氧丙基三甲氧基硅烷加入到带有搅拌、真空和回流装置的烧瓶中,开启搅拌,升温至120℃聚合3小时,即得到粘接促进剂。
3)聚氨酯断面密封胶的制备:
按表3所示的重量份将制备得到的NCO封端的聚氨酯预聚体、碳酸钙、除水剂、制备得到的粘接促粘剂、催化剂加入到搅拌机中,在真空状态下搅拌分散1小时,得到聚氨酯断面密封胶。
对比例2
1)NCO封端的聚氨酯预聚体的制备:
按表1所示的原料和配比备料,然后将聚碳酸亚丙酯二元醇和聚醚三元醇加入至干燥的搅拌釜中边搅拌边升温至60-100℃,再缓慢加入二异氰酸酯,真空下将温度控制在70-90℃,恒温反应3-6h,当-NCO含量达到2%后,得到NCO封端的聚氨酯预聚体得到预聚体。
2)粘接促进剂的制备:
按表2所示的摩尔份将二-(γ-三甲氧基甲硅烷基丙基)胺和γ-缩水甘油醚氧丙基三甲氧基硅烷加入到带有搅拌、真空和回流装置的烧瓶中,开启搅拌,升温至120℃聚合3小时,即得到粘接促进剂。
3)聚氨酯断面密封胶的制备:
按表3所示的重量份将制备得到的NCO封端的聚氨酯预聚体、碳酸钙、除水剂、制备得到的粘接促粘剂、催化剂加入到搅拌机中,在真空状态下搅拌分散1小时,得到聚氨酯断面密封胶。
对比例3
1)NCO封端的聚氨酯预聚体的制备:
按表1所示的原料和配比备料,然后将聚碳酸亚丙酯二元醇和聚醚三元醇加入至干燥的搅拌釜中边搅拌边升温至60-100℃,再缓慢加入二异氰酸酯,真空下将温度控制在70-90℃,恒温反应3-6h,当-NCO含量达到2%后,得到NCO封端的聚氨酯预聚体得到预聚体。
2)聚氨酯断面密封胶的制备:
按比表3所示的重量份将制备得到的NCO封端的聚氨酯预聚体、碳酸钙、除水剂和粘接促粘剂、催化剂加入到搅拌机中,在真空状态下搅拌分散1小时,得到聚氨酯断面密封胶。
对比例4和5
1)NCO封端的聚氨酯预聚体的制备:
按表1所示的原料和配比备料,然后将聚碳酸亚丙酯二元醇和聚醚三元醇加入至干燥的搅拌釜中边搅拌边升温至60-100℃,再缓慢加入二异氰酸酯,真空下将温度控制在70-90℃,恒温反应3-6h,当-NCO含量达到2%后,得到NCO封端的聚氨酯预聚体得到预聚体。
2)粘接促进剂的制备:
按表2所示的摩尔份将γ-氨丙基三甲氧基硅烷、二-(γ-三甲氧基甲硅烷基丙基)胺和γ-缩水甘油醚氧丙基三甲氧基硅烷加入到带有搅拌、真空和回流装置的烧瓶中,开启搅拌,升温至120℃聚合3小时,即得到粘接促进剂。
3)聚氨酯断面密封胶的制备:
按表3所示的重量份将制备得到的NCO封端的聚氨酯预聚体、碳酸钙、除水剂、制备得到的粘接促粘剂(γ-缩水甘油醚氧丙基三甲氧基硅烷)、催化剂加入到搅拌机中,在真空状态下搅拌分散1小时,得到聚氨酯断面密封胶。
表1NCO封端的聚氨酯预聚体制备原料
表2粘接促进剂的制备原料(单位:摩尔份)
表3聚氨酯断面密封胶的制备原料(单位:重量份)
性能测试
将实施例和对比例制得断面密封胶进行以下测试,并将测试结构列于表4中。
断裂伸长率:按GB/T 528-2009规定进行试验,采用哑铃状1型试件,拉伸速度(50±5)mm/min,测试断裂伸长率。以5个试件的算数平均值作为试验结果。
铝塑面内聚破坏率:采用刀割法进行测试,铝逆面内聚破坏率越高,表示密封胶的粘性越好。
水蒸气透过量:按GB/T 17146-2015规定的湿法进行试验,试验温度(23.0±0.5)℃,试件两侧相对湿度差(93±3)%。取3个试件的算数平均值作为试验结果。
表4性能测试结果
上述结果表明,本发明实施例制得的聚氨酯断面密封胶,采用特定数均分子量和比例的聚碳酸亚丙酯二元醇、聚醚三元醇和二异氰酸酯聚合得到的NCO封端的聚氨酯预聚体,与γ-氨丙基三甲氧基硅烷、二-(γ-三甲氧基甲硅烷基丙基)胺和γ-缩水甘油醚氧丙基三甲氧基硅烷经缩合反应得到制得的粘接促进剂、碳酸钙、除水剂和催化剂制得的聚氨酯断面密封胶,其断裂伸长率和铝塑面内聚破坏率显著高于对比例制得的聚氨酯断面密封胶,水蒸气透过量也显著低于对比例。对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施例,而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (4)
1.一种聚氨酯断面密封胶,其特征在于按其重量份包括以下成分:
所述NCO封端的聚氨酯预聚体由聚碳酸亚丙酯二元醇、聚醚三元醇和二异氰酸酯聚合得到,所述聚碳酸亚丙酯二元醇、聚醚三元醇和二异氰酸酯的重量比是(150-800):(700-1200):(203-304);
其中,聚碳酸亚丙酯二元醇的数均分子量为1000-3000,聚醚三元醇的数均分子量为5000-7000;所述聚醚三元醇和聚碳酸亚丙酯二元醇的羟基基团比(1-3):1;所述NCO封端的聚氨酯预聚体由以下方法制备得到:
按比例将聚碳酸亚丙酯二元醇和聚醚三元醇加入至干燥的搅拌釜中边搅拌边升温至60-100℃,再缓慢加入二异氰酸酯,真空下将温度控制在70-90℃,恒温反应3-6h,当-NCO含量达到2-5%后,得到NCO封端的聚氨酯预聚体得到预聚体;
所述粘接促进剂为γ-氨丙基三甲氧基硅烷、二-(γ-三甲氧基甲硅烷基丙基)胺和γ-缩水甘油醚氧丙基三甲氧基硅烷经缩合反应得到,其中γ-氨丙基三甲氧基硅烷、二-(γ-三甲氧基甲硅烷基丙基)胺和γ-缩水甘油醚氧丙基三甲氧基硅烷的基团摩尔比为(2-4):(3-4):1;
所述碳酸钙的含水率≤500ppm。
2.如权利要求1所述的聚氨酯断面密封胶,其特征在于:
所述除水剂为噁唑烷除水剂和分子筛活化粉中的一种或多种。
3.如权利要求1所述的聚氨酯断面密封胶,其特征在于:
所述催化剂为铋锌复合催化剂,铋锌元素质量比例为1:(1-5)。
4.一种如权利要求1-3任一项所述的聚氨酯断面密封胶的制备方法,其特征在于:
按比例将NCO封端的聚氨酯预聚体、碳酸钙、除水剂、粘接促粘剂、催化剂加入到搅拌机中,在真空状态下搅拌分散1小时,得到聚氨酯断面密封胶。
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