CN106753182B - 一种低粘度高初黏强度聚氨酯热熔胶 - Google Patents

一种低粘度高初黏强度聚氨酯热熔胶 Download PDF

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CN106753182B
CN106753182B CN201611012018.9A CN201611012018A CN106753182B CN 106753182 B CN106753182 B CN 106753182B CN 201611012018 A CN201611012018 A CN 201611012018A CN 106753182 B CN106753182 B CN 106753182B
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刘文涛
王建斌
陈田安
解海华
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Yantai Darbond Technology Co Ltd
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Abstract

本发明涉及一种低粘度高初黏强度聚氨酯热熔胶,首先采用结晶性聚酯多元醇、邻苯二甲酸酐聚酯多元醇、环氧丙烷聚醚多元醇和端羟基聚丁二烯同二异氰酸酯反应合成预聚物然后在避光条件下加入二丙稀基单体和其他助剂搅拌均匀得到。本发明聚氨酯热熔胶具有粘度低、初黏强度的特点,可以在短时间内达到较高强度,可用于家电、家具和电子元器件等的粘接。

Description

一种低粘度高初黏强度聚氨酯热熔胶
技术领域
本发明属于热熔胶制备技术领域,尤其涉及一种低粘度高初黏强度聚氨酯热熔胶。
背景技术
反应型聚氨酯热熔胶(Hot melt polyurethanesealant)系以聚氨酯预聚体为主要成分的热熔胶。由于其可以提供较强的初黏强度以及固化速度快等优点广泛应用于电子组装领域。但是现有的聚氨酯热熔胶初黏强度相比UV胶等胶种来说还是较小(UV胶可以在几秒内最终固化),应用于大型电子设备如手机时需要保压1-2小时,降低了效率。因此,提高聚氨酯热熔胶的初黏强度需求很迫切。现在增加初黏强度的方法是通过增加粘度和UV双固化来实现的,如P201310201090.6 公开了一种增加聚氨酯热熔胶双固化制备方法。但是现在的这些方法都存在粘度高的问题,带来了如拉丝、无法快速适应流水线生产等问题。
发明内容
本发明针对上述现有技术存在的不足,提供一种低粘度高初黏强度聚氨酯热熔胶。该热熔胶粘度低,在100℃下粘度为1000-2000mpa.s施胶到元器件后采用紫外灯照射,二丙烯酸酯单体同端羟基聚丁二烯主链中的丙烯基聚合使粘快速增大产生极大的初黏力在5min内便可以达到20-50%的最终粘接强度,达到极好的粘接效果,同时具备了快速固化和低粘度的优点。
本发明解决上述技术问题的技术方案如下:一种低粘度高初黏强度聚氨酯热熔胶,其配方如下,按质量份计:
结晶性己二酸聚酯多元醇 50-60份
邻苯二甲酸酐聚酯二醇 40-50份
环氧丙烷聚醚二元醇 40-50份
端羟基聚丁二烯 20-30份
二异氰酸酯 24-58份
二丙烯酸酯基单体 1-5份
助剂 0.4-1.0份
进一步,配方中所述的结晶性聚酯多元醇为分子量在3000-4000的聚己二酸己二醇酯二醇。
进一步,配方中所述的邻苯二甲酸酐聚酯二醇为分子量1600的聚邻苯二甲酸一缩二乙二醇酯二醇。
进一步,配方中所述的环氧丙烷聚醚多元醇为分子量在1000-2000的聚氧化丙烯二醇。
进一步,配方中所述的端羟基聚丁二烯为分子量在2000-3000。
进一步,配方中所述的二异氰酸酯为苯二亚甲基二异氰酸酯XDI、4,4’-二苯基甲烷二异氰酸酯MDI一种或两种的混合物。
进一步,配方中所述的二丙烯酸酯单体为二甲基丙烯酸乙二醇酯、1,6-己二醇二丙烯酸酯的一种或两种的混合物。
进一步,配方中所述的一种低粘度高初黏强度聚氨酯热熔胶的制备方法,其特征在于,所述的助剂包括偶联剂为KH560、KH590中的一种或两种混合物,其用量为0.1-0.3份;光引发剂为2-羟基-2-甲基-1-苯基丙酮、 2,4,6-三甲基苯甲酰基-二苯基氧化膦、2,4,6-三甲基苯甲酰基苯基膦酸乙酯中一种或几种的混合物,其用量为0.2-0.4份;催化剂为二吗啉二乙基醚,用量为0.1-0.3份。
进一步,配方中所述的制备方法,其特征在于,其步骤为:
将结晶性聚酯多元醇、邻苯二甲酸酐聚酯二醇、环氧丙烷聚醚二元醇、端羟基聚丁二烯在120℃下抽真空(真空度-0.095- -0.1MPa)脱水两小时,然后降温至80℃加入二异氰酸酯,升温至100℃反应1.5h;然后在避光条件下加入经分子筛脱水的二丙烯酸酯单体和助剂抽真空搅拌至均匀无气泡,出料并避光保存。
具体实施方式
以下结合实例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。
实施例1
取分子量为3000的聚己二酸己二醇酯二醇60kg、分子量为1600的聚邻苯二甲酸一缩乙二醇酯二醇50kg、分子量1000的环氧丙烷聚醚二元醇50kg和分子量为2000的端羟基聚丁二烯30kg混合后在120℃下抽真空(真空度-0.095- -0.1MPa)脱水两小时,然后降温至80℃加入58kg MDI,升温至100℃反应1.5h至NCO为3.93%;然后在避光条件下加入经分子筛脱水的二甲基丙烯酸乙二醇酯5kg,0.1kg的2-羟基-2-甲基-1-苯基丙酮,0.2kg的2,4,6-三甲基苯甲酰基苯基膦酸乙酯,0.4kg二吗啉二乙基醚和0.3kg的KH560抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶。
实施例2
取分子量为3000的聚己二酸己二醇酯二醇30kg、分子量为4000的聚己二酸己二醇酯二醇30kg、分子量为1600的聚邻苯二甲酸一缩乙二醇酯二醇45kg、分子量1000的环氧丙烷聚醚二元醇45kg和分子量为2000的端羟基聚丁二烯25kg混合后在120℃下抽真空(真空度-0.095- -0.1MPa)脱水两小时,然后降温至80℃加入51.6kg MDI,升温至100℃反应1.5h至NCO为3.8%;然后在避光条件下加入经分子筛脱水的1kg二甲基丙烯酸乙二醇酯,2kg 1,6-己二醇二丙烯酸酯,0.28kg的2,4,6-三甲基苯甲酰基苯基膦酸乙酯,0.3kg二吗啉二乙基醚和0.2kg的KH590抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶。
实施例3
取分子量为3500的聚己二酸己二醇酯二醇50kg、分子量为1600的聚邻苯二甲酸一缩乙二醇酯二醇50kg、分子量1000的环氧丙烷聚醚二元醇20kg和分子量1000的环氧丙烷聚醚二元醇20kg、分子量为2000的端羟基聚丁二烯20kg混合后在120℃下抽真空(真空度-0.095- -0.1MPa)脱水两小时,然后降温至80℃加入21.16kg MDI和15.9Kg XDI,升温至100℃反应1.5h至NCO为3.55%;然后在避光条件下加入经分子筛脱水的4kg二甲基丙烯酸乙二醇酯,0.24kg的2,4,6-三甲基苯甲酰基-二苯基氧化膦,0.2kg二吗啉二乙基醚和0.2kg的KH560抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶。
实施例4
取分子量为3000的聚己二酸己二醇酯二醇55kg、分子量为1600的聚邻苯二甲酸一缩乙二醇酯二醇40kg、分子量2000的环氧丙烷聚醚二元醇50kg、分子量为2000的端羟基聚丁二烯10kg和分子量为3000的端羟基聚丁二烯20kg混合后在120℃下抽真空(真空度-0.095- -0.1MPa)脱水两小时,然后降温至80℃加入30.1Kg XDI,升温至100℃反应1.5h至NCO为3.27%;然后在避光条件下加入经分子筛脱水的3kg 1,6-己二醇二丙烯酸酯,0.33kg的2,4,6-三甲基苯甲酰基-二苯基氧化膦,0.2kg二吗啉二乙基醚,0.1kg的KH560和0.2kg的KH590抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶。
实施例5
取分子量为4000的聚己二酸己二醇酯二醇50kg、分子量为1600的聚邻苯二甲酸一缩乙二醇酯二醇40kg、分子量2000的环氧丙烷聚醚二元醇40kg和分子量为3000的端羟基聚丁二烯20kg混合后在120℃下抽真空(真空度-0.095- -0.1MPa)脱水两小时,然后降温至80℃加入24kg XDI,升温至100℃反应1.5h至NCO为3.1%;然后在避光条件下加入经分子筛脱水的1kg 1,6-己二醇二丙烯酸酯和0.1kg的2-羟基-2-甲基-1-苯基丙酮,0.2kg二吗啉二乙基醚和0.1kg的KH560抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶。
对比实施例
一种聚氨酯密热熔胶的制备方法,步骤如下:
将分子量为2000的聚氧化丙烯二醇60kg、分子量为3500的聚己二酸己二醇酯二醇85kg与26.78kg MDI在100℃条件下反应1.5h,测得NCO 终点为2.6%,然后0.4kg的二吗啉二乙基醚和0.6kg的KH560抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶;备用。
将上述实施例 1-5 制得的高初黏强度聚氨酯热熔胶与对比实施例制备的聚氨酯热熔胶经国家标准力学性能测试,数据结果如表1所示。
表1 高初黏强度聚氨酯热熔胶与对比实施例性能比较
测试项目 100℃粘度(25℃,50%RH)(mpa.s) 5min剪切强度(25℃,50%RH)(MPa) 1h剪切强度(25℃,50%RH)(min) 24h剪切强度(25℃,50%RH)(min) 7d剪切强度(25℃,50%RH)(MPa)
实施例1 1000 3.5 3.5 6 7
实施例2 1200 1.8 2.5 6.2 8
实施例3 1500 2.5 3 4.8 6.5
实施例4 1800 2 2.5 5.2 6
实施例5 2000 1.5 2.3 4.6 5.5
对比实施例 3000 0.2 1.2 3.8 6
由表1的性能测试对照表能够看出,本发明制备的高初黏强度聚氨酯热熔胶相对于常规的聚氨酯热熔胶表现出优良的初黏强度,使用10min后即可获得较高强度,大大缩短了工艺间隔时间,而且其粘度非常低,节省成本的同时提高了工艺效率,可用于家电、家具和电子元器件等的粘接。
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 (5)

1.一种低粘度高初黏强度聚氨酯热熔胶,其特征在于,制备方法包括: 取分子量为3000的聚己二酸己二醇酯二醇60kg、分子量为1600的聚邻苯二甲酸一缩乙二醇酯二醇50kg、分子量1000的环氧丙烷聚醚二元醇50kg和分子量为2000的端羟基聚丁二烯30kg混合后在120℃下抽真空,真空度-0.095- -0.1MPa脱水两小时,然后降温至80℃加入58kg MDI,升温至100℃反应1.5h至NCO为3.93%;然后在避光条件下加入经分子筛脱水的二甲基丙烯酸乙二醇酯5kg,0.1kg的2-羟基-2-甲基-1-苯基丙酮,0.2kg的2,4,6-三甲基苯甲酰基苯基膦酸乙酯,0.4kg二吗啉二乙基醚和0.3kg的KH560抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶。
2.一种低粘度高初黏强度聚氨酯热熔胶,其特征在于,制备方法包括: 取分子量为3000的聚己二酸己二醇酯二醇30kg、分子量为4000的聚己二酸己二醇酯二醇30kg、分子量为1600的聚邻苯二甲酸一缩乙二醇酯二醇45kg、分子量1000的环氧丙烷聚醚二元醇45kg和分子量为2000的端羟基聚丁二烯25kg混合后在120℃下抽真空,真空度-0.095- -0.1MPa脱水两小时,然后降温至80℃加入51.6kg MDI,升温至100℃反应1.5h至NCO为3.8%;然后在避光条件下加入经分子筛脱水的1kg二甲基丙烯酸乙二醇酯,2kg 1,6-己二醇二丙烯酸酯,0.28kg的2,4,6-三甲基苯甲酰基苯基膦酸乙酯,0.3kg二吗啉二乙基醚和0.2kg的KH590抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶。
3.一种低粘度高初黏强度聚氨酯热熔胶,其特征在于,制备方法包括: 取分子量为3500的聚己二酸己二醇酯二醇50kg、分子量为1600的聚邻苯二甲酸一缩乙二醇酯二醇50kg、分子量1000的环氧丙烷聚醚二元醇20kg和分子量1000的环氧丙烷聚醚二元醇20kg、分子量为2000的端羟基聚丁二烯20kg混合后在120℃下抽真空,真空度-0.095- -0.1MPa脱水两小时,然后降温至80℃加入21.16kg MDI和15.9Kg XDI,升温至100℃反应1.5h至NCO为3.55%;然后在避光条件下加入经分子筛脱水的4kg二甲基丙烯酸乙二醇酯,0.24kg的2,4,6-三甲基苯甲酰基-二苯基氧化膦,0.2kg二吗啉二乙基醚和0.2kg的KH560抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶。
4.一种低粘度高初黏强度聚氨酯热熔胶,其特征在于,制备方法包括: 取分子量为3000的聚己二酸己二醇酯二醇55kg、分子量为1600的聚邻苯二甲酸一缩乙二醇酯二醇40kg、分子量2000的环氧丙烷聚醚二元醇50kg、分子量为2000的端羟基聚丁二烯10kg和分子量为3000的端羟基聚丁二烯20kg混合后在120℃下抽真空,真空度-0.095- -0.1MPa脱水两小时,然后降温至80℃加入30.1Kg XDI,升温至100℃反应1.5h至NCO为3.27%;然后在避光条件下加入经分子筛脱水的3kg 1,6-己二醇二丙烯酸酯,0.33kg的2,4,6-三甲基苯甲酰基-二苯基氧化膦,0.2kg二吗啉二乙基醚,0.1kg的KH560和0.2kg的KH590抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶。
5.一种低粘度高初黏强度聚氨酯热熔胶,其特征在于,制备方法包括: 取分子量为4000的聚己二酸己二醇酯二醇50kg、分子量为1600的聚邻苯二甲酸一缩乙二醇酯二醇40kg、分子量2000的环氧丙烷聚醚二元醇40kg和分子量为3000的端羟基聚丁二烯20kg混合后在120℃下抽真空,真空度-0.095- -0.1MPa脱水两小时,然后降温至80℃加入24kg XDI,升温至100℃反应1.5h至NCO为3.1%;然后在避光条件下加入经分子筛脱水的1kg 1,6-己二醇二丙烯酸酯和0.1kg的2-羟基-2-甲基-1-苯基丙酮,0.2kg二吗啉二乙基醚和0.1kg的KH560抽真空搅拌至均匀无气泡,制得聚氨酯热熔胶。
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