CN110669195A - 耐蒸煮二液型接着剂的制备方法 - Google Patents
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Abstract
本发明提供了一种耐蒸煮二液型接着剂的制备方法,先合成耐蒸煮型高分子量多元醇,再用耐蒸煮型高分子量多元醇与多异氰酸酯加成聚合制备聚氨酯树脂,反应过程中加入流平剂、界面剂、复合抗老化剂以及助剂对聚氨酯树脂进行改性,得到耐蒸煮二液型接着剂。本发明采用多耐蒸煮型高分子量多元醇与脂肪族异氰酸酯聚合制备聚氨酯树脂,其具备软硬相分离的聚集态合金结构,在保证抗老化、耐蒸煮性等综合性能不降低的条件下增加牢度,使用时间等性能。本发明生产出的接着剂耐蒸煮性能优异,在60度下可以在50个小时内保持牢度不降低。
Description
技术领域
本发明涉及接着剂领域,具体是一种耐蒸煮二液型接着剂。
背景技术
随着材料技术的进步,特别是工业的发展,对复合材料的一些基本性能指标、牢度、抗老化等提出了更高的要求。同时,可持续发展的经济模式和环境保护的迫切性,也要求对现有的生产工艺和原料做出合理的革新。将新技术引入传统工艺是重要的革新手段。
用复合工艺做的产品比如衣服、面具、运动鞋、包装袋等等在人们的日常生活中经常会接触到,这些产品的加工过程离不开接着剂的使用。耐蒸煮接着剂的概念不是一般水洗的概念,在温度600以上水温下洗的时候,普通耐水洗的牢度会呈现几何级数降低,而一些特殊场合中需要接着剂能够能克服高温水解。耐蒸煮型接着剂主要用于食品包装,反观材料,特殊服装(消防服,安全衣服),可煮袋等等 ,其中特殊服装(消防服,工业服等)对于接着剂的牢度要求特别高。目前市场上耐蒸煮接着剂的销售量在一年 2000吨左右,市场前景广阔。
发明内容
本发明为了解决现有技术的问题,提供了一种耐蒸煮二液型接着剂的制备方法,采用多耐蒸煮型高分子量多元醇与脂肪族异氰酸酯聚合制备聚氨酯树脂,其具备软硬相分离的聚集态合金结构,在保证抗老化、耐蒸煮性等综合性能不降低的条件下增加牢度,使用时间等性能。本发明生产出的接着剂耐蒸煮性能优异,在60度下可以在50个小时内保持牢度不降低。
本发明包括以下步骤:
1)合成耐蒸煮型高分子量多元醇:采用二元醇与多元异氰酸酯加成聚合制备大分子聚氨酯预聚体,再通过耐蒸煮型多元醇封端该大分子聚氨酯预聚体,从而得到耐蒸煮型高分子量多元醇,具体过程如下:
把己二酸,1,3-苯二甲酸,苯二甲酸,乙二醇,二甘醇,丙二醇加到反应釜升温,先在140度进行 2个小时酯化反应,然后升温至 180度反应2个小时,然后升温至220度反应1个小时, 再升温至 240度反应 1个小时,最后加催化剂反应1个小时,真空脱水1~2小时,达到羟值32-112时反应结束。
常用多元醇的平均分子量一般在1000~4000之间,其中以分子量为2000、3000 应用最为广泛,多元醇的稳定性非常关键,尤其是1,3-苯二甲酸,苯二甲酸这两种酸的反应稳定性很难控制。该技术方案中结合了有多年来的经验和大量实验,得到酸和醇的优化组合比例。
2)用耐蒸煮型高分子量多元醇与多异氰酸酯加成聚合制备聚氨酯树脂,反应过程中加入流平剂、界面剂、复合抗老化剂以及助剂对聚氨酯树脂进行改性,得到耐蒸煮二液型接着剂,具体过程如下:
2.1)将步骤1)得到的耐蒸煮型高分子量多元醇加热至110℃,真空脱水2h;
2.2)加入适量IPDI(异佛尔酮二异氰酸酯)后降温至60~70℃;
2.3)添加复合抗老化剂及助剂,在氮气保护下反应1h;
2.4)加入催化剂在100℃下反应2h;
2.4)降温至70℃,加如醋酸乙酯和异佛尔酮二胺继续反应,确认没有NCO(红外线分析)后加液体MDI反应1个小时;
2.5)加乙二醇,当粘度达到30,000-40,000/25度时加二正丁胺和硅烷反应至少40分钟,确认没有异氰酸酯时终止反应。
催化剂对于反应速度影响很大, Bismuth系类催化剂常温保管性很好,可是反应速度太慢。有机锡系类反应速度很快,可是环保上有问题。Amine系类在影响适用期常温稳定性差。我们采用了稳定性和反应速度比较好的钛酸四丁酯作为催化剂。
本发明有益效果在于:
1、生产出的接着剂耐蒸煮性能优异,在60度下可以在50个小时内保持牢度不降低。
2、采用多耐蒸煮型高分子量多元醇与脂肪族异氰酸酯聚合制备聚氨酯树脂,其具备软硬相分离的聚集态合金结构,在保证抗老化、耐蒸煮性等综合性能不降低的条件下增加牢度,使用时间等性能。
3、采用了稳定性和反应速度比较好的钛酸四丁酯作为催化剂,同时保证了稳定性和反应速度。
附图说明
图1为耐蒸煮型高分子量多元醇合成过程示意图。
图2为本发明一种具体实施例操作过程示意图。
图3为本发明生产流程图。
图4为本发明应用流程图。
具体实施方式
下面结合附图对本发明作进一步说明。
本发明包括以下步骤:
1)合成耐蒸煮型高分子量多元醇过程如图1所示:采用二元醇与多元异氰酸酯加成聚合制备大分子聚氨酯预聚体,再通过耐蒸煮型多元醇封端该大分子聚氨酯预聚体,从而得到耐蒸煮型高分子量多元醇,具体过程如下:
把己二酸,1,3-苯二甲酸,苯二甲酸,乙二醇,二甘醇,丙二醇加到反应釜升温,先在140度进行 2个小时酯化反应,然后升温至 180度反应2个小时,然后升温至220度反应1个小时, 再升温至 240度反应 1个小时,最后加催化剂反应1个小时,真空脱水1~2小时,达到羟值32-112时反应结束。
常用多元醇的平均分子量一般在1000~4000之间,其中以分子量为2000、3000 应用最为广泛,多元醇的稳定性非常关键,尤其是1,3-苯二甲酸,苯二甲酸这两种酸的反应稳定性很难控制。该技术方案中结合了有多年来的经验和大量实验,得到酸和醇的优化组合比例。
2)用耐蒸煮型高分子量多元醇与多异氰酸酯加成聚合制备聚氨酯树脂,反应过程中加入流平剂、界面剂、复合抗老化剂以及助剂对聚氨酯树脂进行改性,得到耐蒸煮二液型接着剂,具体过程如下:
2.1)将步骤1)得到的耐蒸煮型高分子量多元醇加热至110℃,真空脱水2h;
2.2)加入适量IPDI(异佛尔酮二异氰酸酯)后降温至60~70℃;
2.3)添加复合抗老化剂及助剂,在氮气保护下反应1h;
2.4)加入催化剂在100℃下反应2h;
2.4)降温至70℃,加如醋酸乙酯和异佛尔酮二胺继续反应,确认没有NCO(红外线分析)后加液体MDI反应1个小时;
2.5)加乙二醇,当粘度达到30,000-40,000/25度时加二正丁胺和硅烷反应至少40分钟,确认没有异氰酸酯时终止反应。
催化剂对于反应速度影响很大, Bismuth系类催化剂常温保管性很好,可是反应速度太慢。有机锡系类反应速度很快,可是环保上有问题。Amine系类在影响适用期常温稳定性差。我们采用了稳定性和反应速度比较好的钛酸四丁酯作为催化剂。
图2和图3为步骤2)的一种具体实施例制备过程示意图,该实施例具体操作过程如下:
先准备除去水分的DP-7025(耐蒸煮型高分子量多元醇) 440g, 升温到60度,然后放入75.7g的 IPDI(异佛尔酮二异氰酸酯)和1.6g 抗氧剂,0.1g反应延迟剂,搅拌60分钟(均匀分散反应)。加催化剂(bismuth)0.18g. 催化剂加后,反应温度自然地上升,直到90℃左右。加点热使反应温度保持95℃,进行2个小时。降温至60度。 加285.37g醋酸乙酯和异佛尔酮二胺 18.64g继续反应,确认没有NCO(红外线分析)加液体MDI27.7g,反应 1个小时,再加6.9g乙二醇,保持反应温度在60度。达到目标粘度 30,000-40,000的时候加 2.62g二正丁胺和200.15g醋酸乙酯,进行40分钟,再次确认没有剩下的NCO,最后加3.8g硅烷和85.78g醋酸乙酯,进行30分钟后反应终止。该实施例制备出的接着剂测试效果如下:
外观 (无色透明):现在,淡黄色半透明 ;改善, 淡黄色透明;
干洗:现在, 300 lux/m2 ;改善,50 lux/m2;
水洗(60度50回):现在, 300 lux/m2 80 lux/m2 ;改善,100 lux/m2 ;
固含量 (%):现在, 55% ;改善,50%;
粘度(cps/25度):现在, 10,000-20,000;改善,30,000-40,000。
本发明制备的接着剂应用过程如图4所示,与现有接着剂相同,不需要增加新设备,可用原来的设备节省费用。
本发明具体应用途径很多,以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以作出若干改进,这些改进也应视为本发明的保护范围。
Claims (4)
1.一种耐蒸煮二液型接着剂的制备方法,其特征在于包括以下步骤:
1)合成耐蒸煮型高分子量多元醇:采用二元醇与多元异氰酸酯加成聚合制备大分子聚氨酯预聚体,再通过耐蒸煮型多元醇封端该大分子聚氨酯预聚体,从而得到耐蒸煮型高分子量多元醇;
2)用耐蒸煮型高分子量多元醇与多异氰酸酯加成聚合制备聚氨酯树脂,反应过程中加入流平剂、界面剂、复合抗老化剂以及助剂对聚氨酯树脂进行改性,得到耐蒸煮二液型接着剂。
2.根据权利要求1所述的耐蒸煮二液型接着剂的制备方法,其特征在于,所述步骤1)具体过程如下:把己二酸,1,3-苯二甲酸,苯二甲酸,乙二醇,二甘醇,丙二醇加到反应釜升温,先在140度进行 2个小时酯化反应,然后升温至 180度反应2个小时,然后升温至220度反应1个小时,再升温至 240度反应 1个小时,最后加催化剂反应1个小时,真空脱水1~2小时,达到羟值32-112时反应结束。
3.根据权利要求1所述的耐蒸煮二液型接着剂的制备方法,其特征在于,所述的所述步骤2)具体过程如下:
2.1)将步骤1)得到的耐蒸煮型高分子量多元醇加热至110℃,真空脱水2h;
2.2)加入适量IPDI(异佛尔酮二异氰酸酯)后降温至60~70℃;
2.3)添加复合抗老化剂及助剂,在氮气保护下反应1h;
2.4)加入催化剂在100℃下反应2h;
2.4)降温至70℃,加如醋酸乙酯和异佛尔酮二胺继续反应,确认没有NCO(红外线分析)后加液体MDI反应1个小时;
2.5)加乙二醇,当粘度达到30,000-40,000/25度时加二正丁胺和硅烷反应至少40分钟,确认没有异氰酸酯时终止反应。
4.根据权利要求2或3所述的耐蒸煮二液型接着剂的制备方法,其特征在于:所述的催化剂为钛酸四丁酯。
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