CN116218451A - 一种汽车复合材料粘接用聚氨酯结构胶 - Google Patents
一种汽车复合材料粘接用聚氨酯结构胶 Download PDFInfo
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Abstract
本发明涉及一种汽车复合材料粘接用聚氨酯结构胶,由A组分和B组分组成,A组分包括:改性聚酯多元醇、聚醚改性硅烷、端羟基聚异戊二烯、端羧基聚丁二烯、分散剂、碳黑、催化剂、轻钙填料、重钙填料、除水剂、气硅;B组分包括:二聚酸聚酯多元醇、端羟基聚丁二烯、异氰酸酯、分散剂、硅微粉填料,钛白粉。本发明制备结构胶具有极低模量,常温下接近硅橡胶,并且粘度低,触变好,利于各种复杂环境施胶,对各种基材粘接性能优良,耐候耐震效果优异。突出特点是剥离强度高,价格优势明显,经济效益高。
Description
技术领域
本发明涉及聚氨酯结构胶领域,尤其涉及一种汽车多样化复合材料结构粘接用聚氨酯结构胶。
背景技术
随着国际局势日益紧张,全球能源战略资源价格居高不下,中国作为一个石油进口大国,能源问题始终无法解决,导致国内原油价格持续增高,造成燃油汽车使用成本增高,带来的是运输成本增高进而影响物价,直接关系到人们的衣食住行。
在这一背景下,新能源汽车应运而生,全国新能源汽车爆发式增长,货车、公家车、家用车均面临新一轮迭代,汽车行业未来发展前景广阔
对于整车来说,汽车装饰条以及内饰地板等复合材料,结构多样,材料种类多样,粘接环境复杂且需求量大,需要一款能同时满足各种不同应用场景的胶粘剂,由于粘接材料多样且刚性材料与挠性材料均有,故而对胶水抗震动以及剥离强度提出更高的要求,本发明就是针对这一点进行设计。
发明内容
为解决以上问题,本发明制备的聚氨酯结构胶可以有效满足汽车复合材料粘接,具有工艺性好,设计多样化的特点,通过引入橡胶树脂,起到了高剥离,低模量,高可靠性和耐震动的效果。
本发明解决上述技术问题的技术方案如下:一种汽车复合材料粘接用聚氨酯结构胶,由A组分和B组分组成,A组分和B组分的重量比为(1-3):1,按重量份计,A组分包括:改性聚酯多元醇12-16份、聚醚改性硅烷14-24份、端羟基聚异戊二烯5-10份、端羧基聚丁二烯3-8份、分散剂0.3-1.2份、碳黑0.1-0.3份、催化剂0.1-0.5份、轻钙填料6-11份、重钙填料6-10份、除水剂1-4份、气硅1-3份;B组分包括:二聚酸聚酯多元醇15-25份、端羟基聚丁二烯10-15份、异氰酸酯15-25份、分散剂0.1-0.4份和硅微粉填料15-20份,钛白粉0.1-0.3份。
进一步,所述改性聚酯多元醇的分子量为470g/mol,官能度为2,羟值230 -250mgKOH·g-1,制备步骤如下:
基础反应方程式如下所示:
(1)2,5-呋喃二羧酸(FDCA)100g和二甘醇(DEG)160g加入四口烧瓶中,插上温度计和冷凝管,并充满氮气进行搅拌;
(2)加热油浴锅设置温度140℃,控制反应体系温度为135℃,通过冷凝管分离处酯化反应产生的水分,反应1h;
(3)升温至180℃持续反应,观察体系基本无冷凝水生成,将温度升至270℃并抽真空,将体系内多余的二甘醇DEG和水分脱离干净,制得所需改性聚酯多元醇。
进一步,聚醚改性硅烷分子量为2000,优选为迈图股份有限公司L1160、端羟基聚异戊二烯分子量为3500,优选为淄博齐龙化工有限公司、端羧基聚丁二烯分子量为3000,优选为武汉拉那白医药化工有限公司CTPB。引入橡胶树脂可以有限改善聚氨酯在低温时的柔韧性和拉伸强度,能降低产品模量,使聚氨酯胶粘剂具有橡胶的部分性能。
进一步,分散剂优选为毕克助剂BYK-W966、炭黑优选为天津华冉化工科技有限公司N966、催化剂为有机铋催化剂,优选为广州优润化学有限公司WCAT-NS01。
进一步,轻钙填料为1250目,优选为山东今朝化工有限公司JZ-38、重钙填料为1250目,优选为灵寿县昌森矿产品有限公司CHANGSEN—042。轻钙和重钙的合理搭配既可以对体系进行一定程度的补强,又可以有效控制产品粘度和触变,使其能更好的适用于应用场景。
进一步,除水剂为3A分子筛活化粉,优选为奥斯催化材料(大连)有限公司AS-103、气硅优选为湖北汇富纳米材料股份有限公司HB-132。
进一步,二聚酸聚酯多元醇分子量为2000,优选为德国赢创化学T-568、端羟基聚丁二烯分子量为3600,优选为德国赢创化学HT。
进一步,异氰酸酯为液化MDI,优选为万华化学YHMDI、分散剂优选为毕克助剂BYK-W966和硅微粉填料为1250目,优选为连云港淼晶硅材料有限公司MJ-2000,钛白粉优选为南阳恒翔化工产品有限公司HA100。
进一步,本聚氨酯结构胶中通过引入端羧基聚丁二烯能有效提高胶水对各种基材附着力尤其对铝材粘接较为突出,通过引入端羧基聚异戊二烯和端羟基聚丁二烯能改变聚氨酯胶固化状态,达到一种橡胶态,起到低模量高剥离的优异效果,同时由于引入橡胶树脂,大大提高了聚氨酯的耐候性,引入聚醚改性有机硅树脂能降低胶水整体表面能,使其对各种复合材料,比如FR4板、ABS等均具有较好粘接性,同时耐候耐水性大幅提高,相互配合使胶水性能达到最优。
本发明的有益效果是:本发明制备结构胶具有极低模量,常温下接近硅橡胶,并且粘度低,触变好,利于各种复杂环境施胶,对各种基材粘接性能优良,耐候耐震效果优异。突出特点是剥离强度高,价格优势明显,经济效益高。
具体实施方式
以下对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。
改性聚酯多元醇合成步骤包括:
1)2,5-呋喃二羧酸(FDCA)(阿拉丁试剂)100g和二甘醇(DEG)(阿拉丁试剂)160g加入四口烧瓶中,插上温度计和冷凝管,并充满氮气进行搅拌;
(2)加热油浴锅设置温度140℃,控制反应体系温度为135℃,通过冷凝管分离处酯化反应产生的水分,反应1h;
(3)升温至180℃持续反应,观察体系基本无冷凝水生成,将温度升至270℃并抽真空,将体系内多余的DEG和水分脱离干净,制得所需聚酯多元醇。改性聚酯多元醇的分子量为470,羟值为230-250mgKOH·g–1。
实施例1
先加入改性聚酯多元醇13.0g、聚醚改性硅烷L1160 15.0g、端羟基聚异戊二烯6.0g、端羧基聚丁二烯CTPB 5.0g、分散剂BYK-W966 0.4g、碳黑N966 0.3g,混合均匀,再加入催化剂WCAT-NS01 0.2g、轻钙填料JZ-389.0g、重钙填料CHANGSEN-042 10.0g、除水剂AS-103 3.0g、气硅HB-1321.0g,脱泡混合均匀,即得所述A组分结构胶;B组分:先将二聚酸聚酯多元醇T-568 17.0g、端羟基聚丁二烯HT 12.0g和异氰酸酯YHMDI 25.0g在80℃下预聚合2h,待温度降至常温后,加入分散剂BYK-W966 0.1g和硅微粉填料MJ-2000 20.0g,钛白粉HA-100 0.3g,脱泡混合均匀,即得所述B组分。使用时,AB组分按2:1混合均匀后灌胶于待注胶工件上,常温固化或者80℃以下温度加热固化即可。
实施例2
先加入改性聚酯多元醇13.5g、聚醚改性硅烷L1160 16.0g、端羟基聚异戊二烯6.0g、端羧基聚丁二烯CTPB 5.0g、分散剂BYK-W966 0.5g、碳黑N966 0.4g,混合均匀,再加入催化剂WCAT-NS01 0.2g、轻钙填料JZ-3810.0g、重钙填料CHANGSEN-042 9.0g、除水剂AS-103 3.0g、气硅HB-1321.0g,脱泡混合均匀,即得所述A组分结构胶;B组分:先将二聚酸聚酯多元醇T-568 17.0g、端羟基聚丁二烯HT 12.0g和异氰酸酯YHMDI 26.0g在80℃下预聚合2h,待温度降至常温后,加入分散剂BYK-W966 0.1g和硅微粉填料MJ-2000 21.0g,钛白粉HA-100 0.3g,脱泡混合均匀,即得所述B组分。使用时,AB组分按2:1混合均匀后灌胶于待注胶工件上,常温固化或者80℃以下温度加热固化即可。
实施例3
先加入改性聚酯多元醇13.0g、聚醚改性硅烷L1160 15.0g、端羟基聚异戊二烯6.0g、端羧基聚丁二烯CTPB 4.0g、分散剂BYK-W966 0.5g、碳黑N966 0.4g,混合均匀,再加入催化剂WCAT-NS01 0.2g、轻钙填料JZ-388.0g、重钙填料CHANGSEN-042 11.0g、除水剂AS-103 3.0g、气硅HB-1321.0g,脱泡混合均匀,即得所述A组分结构胶;B组分:先将二聚酸聚酯多元醇T-568 17.0g、端羟基聚丁二烯HT 12.0g和异氰酸酯YHMDI 26.0g在80℃下预聚合2h,待温度降至常温后,加入分散剂BYK-W966 0.1g和硅微粉填料MJ-2000 21.0g,钛白粉HA-100 0.3g,脱泡混合均匀,即得所述B组分。使用时,AB组分按2:1混合均匀后灌胶于待注胶工件上,常温固化或者80℃以下温度加热固化即可。
对比例1
先加入蓖麻油多元醇H368(伊藤制油株式会社)13.0g、聚醚改性硅烷L116015.0g、端羟基聚异戊二烯6g、端羧基聚丁二烯CTPB 5g、分散剂BYK-W966 0.4g、碳黑N9660.3g,混合均匀,再加入催化剂WCAT-NS010.2g、轻钙填料JZ-38 9g、重钙填料CHANGSEN-04210g、除水剂AS-1033g、气硅HB-132 1g,脱泡混合均匀,即得所述A组分结构胶;B组分:先将二聚酸聚酯多元醇T-568 17g、端羟基聚丁二烯HT 12g和异氰酸酯YHMDI 25g在80℃下预聚合2h,待温度降至常温后,加入分散剂BYK-W966 0.1g和硅微粉填料MJ-2000 20g,钛白粉HA-100 0.3g,脱泡混合均匀,即得所述B组分。使用时,AB组分按2:1混合均匀后灌胶于待注胶工件上,常温固化或者80℃以下温度加热固化即可。
将实施例1-3和对比例1所得结构胶进行测试,重复对比测试;热固化条件为以80℃,4h加热固化。结果如表1所示。
表1.实施例1-3结构胶性能检测
通过上述对比试验,可以看出使用改性聚酯多元醇相较于市售蓖麻油多元醇,制备的聚氨酯结构胶具有更低的模量,搭配橡胶树脂时具有更好的相容性,有效提高了对各种基材的粘接力,剥离强度提高明显,断裂伸长率显著提高。
本发明相较于市场上主流的聚氨酯结构胶,引入了大量的橡胶树脂和聚醚改性硅树脂,大大降低了胶水的模量,使其具有更高的耐震和耐候性,同时对各种复合材料的粘接性高,剥离强度提升明显。适用性更广泛,是一款覆盖面较高的胶水。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.一种汽车复合材料粘接用聚氨酯结构胶,其特征在于,由A组分和B组分组成,A组分和B组分的重量比为(1-3):1,按重量份计,A组分包括:改性聚酯多元醇12-16份、聚醚改性硅烷14-24份、端羟基聚异戊二烯5-10份、端羧基聚丁二烯3-8份、分散剂0.3-1.2份、碳黑0.1-0.3份、催化剂0.1-0.5份、轻钙填料6-11份、重钙填料6-10份、除水剂1-4份、气硅1-3份;B组分包括:二聚酸聚酯多元醇15-25份、端羟基聚丁二烯10-15份、异氰酸酯15-25份、分散剂0.1-0.4份和硅微粉填料15-20份,钛白粉0.1-0.3份;
所述改性聚酯多元醇的分子量为470g/mol,官能度为2,羟值230
-250mgKOH·g-1。
2.根据权利要求1所述的汽车复合材料粘接用聚氨酯结构胶,其特征在于,所述改性聚酯多元醇制备步骤如下:
(1)2,5-呋喃二羧酸100g和二甘醇160g加入四口烧瓶中,插上温度计和冷凝管,并充满氮气进行搅拌;
(2)加热油浴锅设置温度140℃,控制反应体系温度为135℃,通过冷凝管分离处酯化反应产生的水分,反应1h;
(3)升温至180℃持续反应,观察体系基本无冷凝水生成,将温度升至270℃并抽真空,将体系内多余的二甘醇和水分脱离干净,制得所需改性聚酯多元醇。
3.根据权利要求1所述的汽车复合材料粘接用聚氨酯结构胶,其特征在于,所述聚醚改性硅烷分子量为2000,为迈图股份有限公司L1160;所述端羟基聚异戊二烯分子量为3500,为淄博齐龙化工有限公司;所述端羧基聚丁二烯分子量为3000,为武汉拉那白医药化工有限公司CTPB。
4.根据权利要求1所述的汽车复合材料粘接用聚氨酯结构胶,其特征在于,所述分散剂为毕克助剂BYK-W966、所述催化剂为有机铋催化剂,为广州优润化学有限公司WCAT-NS01。
5.根据权利要求1所述的汽车复合材料粘接用聚氨酯结构胶,其特征在于,所述轻钙填料为1250目,为山东今朝化工有限公司JZ-38;所述重钙填料为1250目,为灵寿县昌森矿产品有限公司CHANGSEN—042。
6.根据权利要求1所述的汽车复合材料粘接用聚氨酯结构胶,其特征在于,所述除水剂为3A分子筛活化粉,为奥斯催化材料(大连)有限公司AS-103;所述气硅为湖北汇富纳米材料股份有限公司HB-132。
7.根据权利要求1所述的汽车复合材料粘接用聚氨酯结构胶,其特征在于,所述二聚酸聚酯多元醇分子量为2000,为德国赢创化学T-568;所述端羟基聚丁二烯分子量为3600,为德国赢创化学HT。
8.根据权利要求1所述的汽车复合材料粘接用聚氨酯结构胶,其特征在于,所述异氰酸酯为液化MDI;所述分散剂为毕克助剂BYK-W966;所述硅微粉填料为1250目,为连云港淼晶硅材料有限公司MJ-2000;所述钛白粉为南阳恒翔化工产品有限公司HA100。
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