CN110819288B - 一种高透湿反应型聚氨酯热熔胶及其制备方法 - Google Patents

一种高透湿反应型聚氨酯热熔胶及其制备方法 Download PDF

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CN110819288B
CN110819288B CN201911104152.5A CN201911104152A CN110819288B CN 110819288 B CN110819288 B CN 110819288B CN 201911104152 A CN201911104152 A CN 201911104152A CN 110819288 B CN110819288 B CN 110819288B
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姜海龙
刘成刚
王旭涛
张泽绮
刘少勇
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Jiangsu Huada New Material Co ltd
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Abstract

本发明涉及一种高透湿反应型聚氨酯热熔胶及其制备方法，按重量百分含量计，所述聚氨酯热熔胶的原料配方包括以下组分：聚酯多元醇20~30%；聚醚多元醇40~60%；扩链剂0~2%；异氰酸酯10~35%；助剂0.01~0.25%；副反应阻止剂0.001~0.01%；催化剂0.01~0.2%；其中，所述聚酯多元醇为华大化学的CMA‑1000PN、CMA‑3566、CMA‑1024、CMA‑3500SH中的一种或多种的组合；所述聚醚多元醇的数均分子量为2000~3000。本发明的反应型聚氨酯热熔胶采用华大化学生产的特定的聚酯多元醇配合分子量在2000~3000的聚醚多元醇、异氰酸酯、助剂、阻止剂、催化剂、或/和扩链剂制备的热熔胶用于高透湿复合面料，具有初始粘强度高，开放时间缩短，透湿效果大大提高。

Description

一种高透湿反应型聚氨酯热熔胶及其制备方法
技术领域
本发明属于聚氨酯树脂技术领域，具体涉及一种高透湿反应型聚氨酯热熔胶及其制备方法和应用。
背景技术
反应型聚氨酯热熔胶是热塑性大分子中引入可反应基团，当胶水被涂在被粘物后，通过活性基团的反应而固化。它具备环保无溶剂、粘接迅速、适合多种材料、施用方便等一系列优点，又具有高透湿、耐蠕变、强度高、耐热、耐溶剂、耐药品等性能。
目前反应型聚氨酯热熔胶在纺织方面飞速发展，不仅对胶水的需求大幅增加，而且对其技术的改进和功能化极为期望。市场上开发出高透湿复合面料，选用普通的胶水主要存在初始粘强度不高、开放时间较长，透湿效果差等问题。也有人研制一种高透湿功能面料用反应型聚氨酯热熔胶，如中国专利CN108251039A公开了一种高透湿功能面料用反应型聚氨酯热熔胶及其制备方法，该热熔胶由聚酯多元醇5～30份、聚醚多元醇5～40份、扩链剂0～15份、特殊多元醇0～40份、附着力促进剂0～5份、抗氧剂0～2份、紫外线吸收剂0～2份、稳定剂0～1份、二异氰酸酯10～15份、催化剂0～1份、硅烷偶联剂0～5份制备而成。然而该热熔胶的配方复杂，同时粘度稍大，流动性差，而若采用提高温度来降低粘度，又限制了应用，特别在高透膜与布复合方面。
发明内容
本发明目的是为了克服现有技术的不足而提供一种高透湿反应型聚氨酯热熔胶及其制备方法。
为达到上述目的，本发明所采用的技术方案为：
一种反应型聚氨酯热熔胶，按重量百分含量计，所述聚氨酯热熔胶的原料配方包括以下组分：
Figure BDA0002270758930000011
其中，所述聚酯多元醇为华大化学的CMA-1000PN、CMA-3566、CMA-1024、CMA-3500SH中的一种或多种的组合；所述聚醚多元醇的数均分子量为2000～3000。
根据本发明的一些实施方面，所述聚醚多元醇为聚氧化乙烯二醇、聚氧化丙烯二醇中的一种或几种的组合。
根据本发明的一些实施方面，所述扩链剂为三羟甲基丙烷、1，4-丁二醇中的一种或二者的组合。
根据本发明的一些实施方面，所述异氰酸酯为二苯基甲烷二异氰酸酯。
根据本发明的一些实施方面，所述助剂为抗氧剂、流平剂中的一种或二者的组合。
根据本发明的一些实施方面，所述抗氧剂的添加量为0.05～0.15％，所述流平剂的添加量为0～0.1％。
根据本发明的一些实施方面，所述副反应阻止剂为苯甲酰氯、磷酸中的一种或二者的组合。
根据本发明的一些实施方面，所述催化剂为二吗啉基二乙基醚、二月桂酸二丁基锡中的一种或二者的组合。
本发明采取的另一技术方案为：一种上述所述的反应型聚氨酯热熔胶的制备方法，其包括：使聚酯多元醇、聚醚多元醇、助剂在温度100～120℃条件下搅拌抽真空0.5～2h；然后加入副反应阻止剂、或/和扩链剂，在温度80～90℃条件下搅拌抽真空10～30min；然后加入异氰酸酯，在温度80～90℃条件下抽真空反应1.5～2.5h；然后加入催化剂进行真空脱泡，制得所述聚氨酯热熔胶。
所述聚氨酯热熔胶的NCO％含量为1.8-6.0％。
由于上述技术方案运用，本发明与现有技术相比具有下列优点：
本发明采用华大化学生产的特定的聚酯多元醇配合分子量在2000～3000的聚醚多元醇、异氰酸酯、助剂、阻止剂、催化剂、或/和扩链剂制备的热熔胶用于高透湿复合面料，将高透TPU膜涂胶贴合加压后，自然放置3min，剥离膜与基布，不易剥离甚至膜被破坏，开放时间缩短，透湿效果大大提高的优点。
本发明的反应型聚氨酯热熔胶的制备方法简单，且在加入异氰酸酯后选择在温度80～90℃条件下反应1.5～2.5h，此温度条件下异氰酸酯与多元醇反应充分，若温度低于80℃，需要延长反应时间，而温度高于90℃，NCO的含量比理论中偏大，同时热熔胶的粘度稍大。
具体实施方式
下面结合具体实施例对本发明的具体实施作进一步详细说明，但本发明的实施和保护范围不限于此。
实施例1
本实施例提供的一种高透湿反应型聚氨酯热熔胶，通过以下方法制备得到：
将35份数均分子量为1000的聚酯多元醇CMA-1000PN、65份数均分子量为2000的聚氧化乙烯二醇、0.1份抗氧剂1010加入反应釜中，升温到110℃后开启搅拌，转速设置为60转，保持温度为110℃，开启真空泵保持真空度为-0.098Mpa以下，抽气1小时后，降温至90℃，停止抽真空，加入0.005份副反应阻止剂磷酸，继续抽真空，降温至70℃时，停止抽真空，加入33份二苯基甲烷二异氰酸酯，转速设置为100转，升温并保持温度90℃，搅拌120分钟后，加入0.1份催化剂二吗啉基二乙基醚，开启真空抽气15分钟，停止抽真空，出料密封保存。
实施例2
本实施例提供的一种高透湿反应型聚氨酯热熔胶，通过以下方法制备得到：
将30份数均分子量为3500的聚酯多元醇CMA-3566、70份数均分子量为2000的聚氧化乙烯二醇、0.1份抗氧剂1010、0.05份流平剂TEGO410加入反应釜，升温到110℃后开启搅拌，转速设置为60转，保持温度为110℃，开启真空泵保持真空度为-0.098Mpa以下，抽气1小时后，降温至90℃，停止抽真空，加入0.005份副反应阻止剂苯甲酰氯，继续抽真空，降温至70℃时，停止抽真空，加入19.8份二苯基甲烷二异氰酸酯，转速设置为100转，升温并保持温度90℃，搅拌120分钟后，加入0.1份催化剂二吗啉基二乙基醚，开启真空抽气15分钟，停止抽真空，出料密封保存。
实施例3
本实施例提供的一种高透湿反应型聚氨酯热熔胶，通过以下方法制备得到：
将10份数均分子量为1000的聚酯多元醇CMA-1024、79.55份数均分子量为2000的聚氧化乙烯二醇、10份数均分子量为3500的聚酯多元醇CMA-3500SH、0.45份三羟甲基丙烷、0.1份抗氧剂1010、0.05份流平剂TEGO410加入反应釜中，升温到110℃后开启搅拌，转速设置为60转，保持温度为110℃，开启真空泵保持真空度为-0.098Mpa以下，抽气1小时后，降温至90℃，停止抽真空，加入0.005份副反应阻止剂苯甲酰氯和1.2份1.4丁二醇，继续抽真空，降温至70℃时，停止抽真空，加入29.4份二苯基甲烷二异氰酸酯MDI-50，转速设置为100转，升温并保持温度80℃，搅拌120分钟后，加入0.1份催化剂二吗啉基二乙基醚，开启真空抽气15分钟，停止抽真空，出料密封保存。
实施例4
本实施例提供的一种高透湿反应型聚氨酯热熔胶，通过以下方法制备得到：
将35份数均分子量为1000的聚酯多元醇CMA-1000PN、30份数均分子量为3000的聚氧化丙烯二醇、35份数均分子量为2000的聚氧化乙烯二醇、0.1份抗氧剂1010、0.05份流平剂TEGO410加入反应釜中，升温到110℃后开启搅拌，转速设置为60转，保持温度为110℃，开启真空泵保持真空度为-0.098Mpa以下，抽气1小时后，降温至90℃，停止抽真空，加入0.005份副反应阻止剂苯甲酰氯，继续抽真空，降温至70℃时，停止抽真空，加入30.8份二苯基甲烷二异氰酸酯，转速设置为100转，升温并保持温度80℃，搅拌120分钟后，加入0.05份催化剂二月桂酸二丁基锡，开启真空抽气15分钟，停止抽真空，出料密封保存。
实施例5
本实施例提供的一种高透湿反应型聚氨酯热熔胶，通过以下方法制备得到：
将35份数均分子量为1000的聚酯多元醇CMA-1000PN、65份数均分子量为3000的聚氧化丙烯二醇、0.1份抗氧剂1010、0.05份流平剂TEGO410加入反应釜中，升温到110℃后开启搅拌，转速设置为60转，保持温度为110℃，开启真空泵保持真空度为-0.098Mpa以下，抽气1小时后，降温至90℃，停止抽真空，加入0.005份副反应阻止剂苯甲酰氯，继续抽真空，降温至70℃时，停止抽真空，加入29份二苯基甲烷二异氰酸酯，转速设置为100转，升温并保持温度90℃，搅拌120分钟后，加入0.1份催化剂二吗啉基二乙基醚，开启真空抽气15分钟，停止抽真空，出料密封保存。
实施例6
本实施例提供的一种高透湿反应型聚氨酯热熔胶，通过以下方法制备得到：
将35份数均分子量为2000的聚酯多元醇CMA-24、25份数均分子量为3000的聚氧化丙烯二醇、40份数均分子量为2000的聚氧化乙烯二醇、0.1份抗氧剂1010、0.05份流平剂加入反应釜中，升温到110℃后开启搅拌，转速设置为60转，保持温度为110℃，开启真空泵保持真空度为-0.098Mpa以下，抽气1小时后，降温至90℃，停止抽真空，加入0.005份副反应阻止剂苯甲酰氯，继续抽真空，降温至70℃时，停止抽真空，加入26.2份二苯基甲烷二异氰酸酯，转速设置为100转，升温并保持温度80℃，搅拌120分钟后，加入0.05份催化剂二月桂酸二丁基锡，开启真空抽气15分钟，停止抽真空，出料密封保存。
将实施例1～6的热熔胶通过以下方法进行性能测试，测试结果见表1所示。
检测方法：
1、NCO％：按标准HG/T2409-92测定，取样品(准确到0.001g)置于锥形瓶中，用移液管准确移取10ml的二正丁胺-甲苯溶液加入锥形瓶中(测定纯MDI样品时，移取20ml的二正丁胺-甲苯溶液加入锥形瓶中)，然后再加入20ml的甲苯轻轻摇动使之溶解，最后加入80ml无水异丙醇。静置15分钟，以溴甲酚绿为指示剂，用1mol/L盐酸标准溶液进行滴定当溶液由蓝色变为黄色且30s不变色即为滴定终点，(按同样的方式做空白试验)。
2、粘度测试：采用BROOKFIELD黏度计(自带温度控制)进行粘度测定。
3、开放时间：按标准HG/T3716-2003测定，具体步骤如下：
1)将热熔胶和涂胶器放入恒定温箱内直至温度稳定。
2)试验在无空气流动的常温室内进行，将涂胶底纸粘贴到低传热系数的平整垫板上。
3)将贴纸以间距6mm整齐排列，
4)将热熔胶从恒温箱中取出，使用涂胶器将热熔胶涂到胶底纸上，计时开始，相隔一定时间覆盖粘接纸条并加压，直到胶层不能粘接纸条。
4、透湿性测试：采用GB/T12704.2-2009中倒杯法，条件为温度(38±2)℃，相对湿度(50±2)％。
透湿面料的制备：
1)采用高透湿TPU膜
2)使用熔胶机在温度90℃下的热涂反应型热熔胶，上胶于TPU膜上，涂胶量为4-6g/m2，再与布贴合，收卷，在25℃的温度和50％RH湿度下固化24小时。
3)将固化后的面料按照GB/T12704.2-2009标准裁样、测试。
表1为实施例1～6的热熔胶的性能测试结果
Figure BDA0002270758930000051
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。

Claims (1)

1.一种反应型聚氨酯热熔胶的制备方法，其特征在于，所述制备方法包括：使聚酯多元醇、聚醚多元醇、抗氧剂在温度100~120℃条件下搅拌抽真空0.5~2小时；然后加入副反应阻止剂，在温度80~90℃条件下搅拌抽真空10~30分钟；然后加入异氰酸酯，在温度80~90℃条件下抽真空反应1.5~2.5小时；然后加入催化剂进行真空脱泡，制得所述聚氨酯热熔胶；所述聚氨酯热熔胶的NCO%含量为1.8-6.0%；
所述聚氨酯热熔胶的原料配方由以下组分构成：35份数均分子量为1000的聚酯多元醇CMA-1000PN、65份数均分子量为2000的聚氧化乙烯二醇、0.1份抗氧剂1010、0.005份副反应阻止剂磷酸、33份二苯基甲烷二异氰酸酯和0.1份催化剂二吗啉基二乙基醚。
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