CN111334236A - 一种双组份水性聚氨酯耐水煮胶粘剂的制备方法 - Google Patents

一种双组份水性聚氨酯耐水煮胶粘剂的制备方法 Download PDF

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CN111334236A
CN111334236A CN202010189130.XA CN202010189130A CN111334236A CN 111334236 A CN111334236 A CN 111334236A CN 202010189130 A CN202010189130 A CN 202010189130A CN 111334236 A CN111334236 A CN 111334236A
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欧华新
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Abstract

本发明公开了一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,属于化工胶粘剂技术领域。本发明的双组份水性聚氨酯耐水煮胶粘剂包括预聚物的制备,本发明主要以聚己二酸丁二醇酯、聚四氢呋喃醚二醇、甲苯二异氰酸酯、二羟甲基丙酸、丙二醇甲醚醋酸酯、碳酸丙烯酯和脱水剂等为原料,合成了一种双组份水性聚氨酯耐水煮胶粘剂。该双组份水性聚氨酯胶粘剂具有溶剂用量少,固含量高,高粘结强度,价格低廉,尤其是具有较好的拉伸强度,较好的抗扭折性以及耐高温等性能,可用在织物、泡沫、塑料、皮革等基材上,具有广泛的应用前景。

Description

一种双组份水性聚氨酯耐水煮胶粘剂的制备方法
技术领域
本发明属于化工胶粘剂技术领域,尤其涉及一种双组份水性聚氨酯耐水煮胶粘剂的制备方法。
背景技术
复合薄膜软包装具有屏蔽、可印刷和热封等功能,已广泛应用于食品、医药、化妆品等领域。随着用途的不同,对软包装性能的要求各异,但总的要求是包装材料具有良好的柔韧性、较高的拉伸强度、较好的抗扭折性以及能耐高温(如巴氏消毒、沸煮和蒸煮等)、能印刷等。
目前,在水性胶粘剂领域,双组分WPU以其对各种薄膜适应性强、初粘性高、无任何添加剂、保质时间久、耐高低温等优异性能备受人们关注。
首先,国内已工业化的聚氨酯耐水煮胶粘剂产品较少,性能不稳定。本发明是一种可满足普通塑料薄膜的复合、耐水煮的双组份水性聚氨酯耐水煮胶粘剂的制备,该胶可耐100℃水煮40min,对各种塑料薄膜具有较高的粘接强度。双组份水性聚氨酯耐水煮胶粘剂,是一种可替代溶剂型双组份聚氨酯黏合剂产品。是一种真正的绿色环保型,生产环境友好型及产品安全型的产品。
双组份水性聚氨酯耐水煮胶粘剂的研发成功,是对传统的溶剂型胶粘剂的一次突破性的变革。本发明的双组份水性聚氨酯耐水煮胶粘剂与溶剂型胶粘剂相比:在复合设备不变、工艺条件基本相同的情况下,使软包装复合制品没有了溶剂残留,且彻底改善车间生产环境。
并且,水性聚氨酯的固体材料部分同是聚氨酯系列,故具备了溶剂型聚氨酯胶粘剂所具备的性能。水性聚氨酯胶粘剂在对材料结构、油墨的适应性、耐温和冷冻等复合材料制品上,都能具备或优于溶剂型聚氨酯胶粘剂所具备的性能。另外,有较明显的成本优势。一般的,复合产品有更好的初粘接力和抗低温性,还可大大降低操作工的劳动强度或节省用工人数。
本发明的双组份水性聚氨酯耐水煮胶粘剂与水性丙烯酸胶粘剂相比较,本发明的双组份水性聚氨酯耐水煮胶粘剂同样具备了目前市场上水性丙烯酸胶粘剂的安全环保,复合成本低,无溶剂残留的优点,并且弥补了水性丙烯酸胶粘剂功能单一,只能做轻包装和卷料及制袋效果不佳的局限性和耐高低温性能差的不足。
水性聚氨酯胶粘剂与水性丙烯酸胶粘剂相比,不会出现后期复合强度衰减的现象。因丙烯酸乳液是使用乳化剂将不溶于水的物质乳化后分散在水中的,属不均一相。而一般乳化剂是不参加反映的。为了使水性丙烯酸类复合胶粘剂获得较好的粘接效果,要求对被粘接材料有较好的润湿性,又要加入润湿剂。由于乳化剂的存在,在使用中又会产生大量气泡,所以又要加入消泡剂等等。也就是说在水性丙烯酸类复合胶粘剂体系中至少含有乳化剂,润湿剂,消泡剂等多种添加剂,当复合粘接完成后,随着时间的推移,这些添加剂会或多或少的向复合粘接界面迁移,导致粘接强度衰减,而双组份水性聚氨酯耐水煮胶粘剂则从根本上解决了上述一系列问题。
发明内容
首先,本发明人通过一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,具体步骤为,以重量份数计,将混合聚合物聚己二酸丁二醇酯18-22份、聚四氢呋喃醚二醇9-11份升温使其溶解,降温,加入2,2-二羟甲基丙酸1-3份、甲苯二异氰酸酯9-11份以及丙酮1-3份到反应釜中,加热下搅拌反应1-5小时后,降温再加入三乙胺,高速搅拌去离子水、乙二胺0.4-0.6份和二乙烯三胺1-3份,加热下搅拌反应5-15min,成功得到了一种水性聚氨酯耐水煮胶粘剂主剂;将丙二醇甲醚醋酸酯1-3份、碳酸丙烯酯7-9份和脱水剂0.1-0.5份混合得到水性固化剂;将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂混合得到一种双组份水性聚氨酯耐水煮胶粘剂。
然后,本发明人将一种双组份水性聚氨酯耐水煮胶粘剂主剂与水性固化剂的质量比为(10-20):(0.1-5),得到了一种双组份水性聚氨酯耐水煮胶粘剂。特别说明,在一种双组份水性聚氨酯耐水煮胶粘剂的制备方法中,混合聚合物二醇,以重量份数计,由聚己二酸丁二醇酯18-22份以及相对分子量为2000的聚四氢呋喃醚二醇9-11份混合而成。
另外,聚己二酸丁二醇酯和聚四氢呋喃醚二醇的相对分子量均为2000。控制加热的温度在100-160℃之间,110℃为最优。降温到30-50℃,40℃最优。搅拌乳化的时间为1-5小时,4小时最优。混合聚合物聚己二酸丁二醇酯和聚四氢呋喃醚二醇使用前应进行真空脱水。
最后得到一种性能优越的耐100℃水煮复合软包装用胶粘剂。应用时,按重量比m主制:m固化剂=16:1,控制涂布量为1.2-2.5g/m2,熟化:50℃/4小时,热封:160℃,压力0.2MPa/s,杀菌蒸煮条件:100℃/40min。
将产品涂于标签并在试验条件下置于试验炉中,并令其互不接触(。将对照组标签的温度各湿度分别保持在90℃±10℃和50%RH下72小时。试验结束时,将被测试标签从试验炉中取出,目视检测粘结程度。电子剥离试验机测试3次,检测其粘结程度。
具体实施方式
实施例1.一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,以重量份数计,将混合聚合物聚己二酸丁二醇酯18-22份、聚四氢呋喃醚二醇9-11份升温使其溶解,降温,加入2,2-二羟甲基丙酸1-3份、甲苯二异氰酸酯9-11份以及丙酮1-3份到反应釜中,加热下搅拌反应1-5小时后,降温再加入三乙胺,高速搅拌去离子水、乙二胺0.4-0.6份和二乙烯三胺1-3份,加热下搅拌反应5-15min,即为水性聚氨酯耐水煮胶粘剂主剂;将丙二醇甲醚醋酸酯1-3份、碳酸丙烯酯7-9份和脱水剂0.1-0.5份混合得到水性固化剂;将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂混合得到一种双组份水性聚氨酯耐水煮胶粘剂。将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂的质量比为(10-20):(0.1-5)配合,得到双组分水性聚氨酯耐水煮胶粘剂。按重量比m主制:m固化剂=16:1,控制涂布量为1.2-2.5g/m2,熟化:50℃/4小时,热封:160℃,压力0.2MPa/s,杀菌蒸煮条件:100℃/40min进行制备测试条件。将产品涂于标签并在试验条件下置于试验炉中,并令其互不接触。将对照组标签的温度各湿度分别保持在85℃和50%RH下72小时。试验结束时,将被测试标签从试验炉中取出,目视检测,粘结完好。电子剥离试验机测试3次,检测其粘结程度,粘结完好。
实施例2.一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,以重量份数计,将混合聚合物聚己二酸丁二醇酯18-22份、聚四氢呋喃醚二醇9-11份升温使其溶解,降温,加入2,2-二羟甲基丙酸1-3份、甲苯二异氰酸酯9-11份以及丙酮1-3份到反应釜中,加热下搅拌反应1-5小时后,降温再加入三乙胺,高速搅拌去离子水、乙二胺0.4-0.6份和二乙烯三胺1-3份,加热下搅拌反应5-15min,即为水性聚氨酯耐水煮胶粘剂主剂;将丙二醇甲醚醋酸酯1-3份、碳酸丙烯酯7-9份和脱水剂0.1-0.5份混合得到水性固化剂;将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂混合得到一种双组份水性聚氨酯耐水煮胶粘剂。将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂的质量比为(10-20):(0.1-5)配合,得到双组分水性聚氨酯耐水煮胶粘剂。按重量比m主制:m固化剂=16:1,控制涂布量为1.2-2.5g/m2,熟化:50℃/4小时,热封:160℃,压力0.2MPa/s,杀菌蒸煮条件:100℃/40min进行制备测试条件。将产品涂于标签并在试验条件下置于试验炉中,并令其互不接触。将对照组标签的温度各湿度分别保持在90℃和50%RH下72小时。试验结束时,将被测试标签从试验炉中取出,目视检测,粘结完好。电子剥离试验机测试3次,检测其粘结程度,粘结完好。
实施例3.一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,以重量份数计,将混合聚合物聚己二酸丁二醇酯18-22份、聚四氢呋喃醚二醇9-11份升温使其溶解,降温,加入2,2-二羟甲基丙酸1-3份、甲苯二异氰酸酯9-11份以及丙酮1-3份到反应釜中,加热下搅拌反应1-5小时后,降温再加入三乙胺,高速搅拌去离子水、乙二胺0.4-0.6份和二乙烯三胺1-3份,加热下搅拌反应5-15min,即为水性聚氨酯耐水煮胶粘剂主剂;将丙二醇甲醚醋酸酯1-3份、碳酸丙烯酯7-9份和脱水剂0.1-0.5份混合得到水性固化剂;将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂混合得到一种双组份水性聚氨酯耐水煮胶粘剂。将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂的质量比为(10-20):(0.1-5)配合,得到双组分水性聚氨酯耐水煮胶粘剂。按重量比m主制:m固化剂=16:1,控制涂布量为1.2-2.5g/m2,熟化:50℃/4小时,热封:160℃,压力0.2MPa/s,杀菌蒸煮条件:100℃/40min进行制备测试条件。将产品涂于标签并在试验条件下置于试验炉中,并令其互不接触。将对照组标签的温度各湿度分别保持在95℃和50%RH下72小时。试验结束时,将被测试标签从试验炉中取出,目视检测,粘结完好。电子剥离试验机测试3次,检测其粘结程度,粘结完好。
实施例4.一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,以重量份数计,将混合聚合物聚己二酸丁二醇酯18-22份、聚四氢呋喃醚二醇9-11份升温使其溶解,降温,加入2,2-二羟甲基丙酸1-3份、甲苯二异氰酸酯9-11份以及丙酮1-3份到反应釜中,加热下搅拌反应1-5小时后,降温再加入三乙胺,高速搅拌去离子水、乙二胺0.4-0.6份和二乙烯三胺1-3份,加热下搅拌反应5-15min,即为水性聚氨酯耐水煮胶粘剂主剂;将丙二醇甲醚醋酸酯1-3份、碳酸丙烯酯7-9份和脱水剂0.1-0.5份混合得到水性固化剂;将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂混合得到一种双组份水性聚氨酯耐水煮胶粘剂。将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂的质量比为(10-20):(0.1-5)配合,得到双组分水性聚氨酯耐水煮胶粘剂。按重量比m主制:m固化剂=16:1,控制涂布量为1.2-2.5g/m2,熟化:50℃/4小时,热封:160℃,压力0.2MPa/s,杀菌蒸煮条件:100℃/40min进行制备测试条件。将产品涂于标签并在试验条件下置于试验炉中,并令其互不接触。将对照组标签的温度各湿度分别保持在100℃和50%RH下72小时。试验结束时,将被测试标签从试验炉中取出,目视检测,粘结完好。电子剥离试验机测试3次,检测其粘结程度,粘结完好。
实施例5.一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,以重量份数计,将混合聚合物聚己二酸丁二醇酯18-22份、聚四氢呋喃醚二醇9-11份升温使其溶解,降温,加入2,2-二羟甲基丙酸1-3份、甲苯二异氰酸酯9-11份以及丙酮1-3份到反应釜中,加热下搅拌反应1-5小时后,降温再加入三乙胺,高速搅拌去离子水、乙二胺0.4-0.6份和二乙烯三胺1-3份,加热下搅拌反应5-15min,即为水性聚氨酯耐水煮胶粘剂主剂;将丙二醇甲醚醋酸酯1-3份、碳酸丙烯酯7-9份和脱水剂0.1-0.5份混合得到水性固化剂;将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂混合得到一种双组份水性聚氨酯耐水煮胶粘剂。将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂的质量比为(10-20):(0.1-5)配合,得到双组分水性聚氨酯耐水煮胶粘剂。按重量比m主制:m固化剂=16:1,控制涂布量为1.2-2.5g/m2,熟化:50℃/4小时,热封:160℃,压力0.2MPa/s,杀菌蒸煮条件:100℃/40min进行制备测试条件。将产品涂于标签并在试验条件下置于试验炉中,并令其互不接触。将对照组标签的温度各湿度分别保持在105℃和50%RH下72小时。试验结束时,将被测试标签从试验炉中取出,目视检测,粘结完好。电子剥离试验机测试3次,检测其粘结程度,粘结完好。
实施例6.一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,以重量份数计,将混合聚合物聚己二酸丁二醇酯18-22份、聚四氢呋喃醚二醇9-11份升温使其溶解,降温,加入2,2-二羟甲基丙酸1-3份、甲苯二异氰酸酯9-11份以及丙酮1-3份到反应釜中,加热下搅拌反应1-5小时后,降温再加入三乙胺,高速搅拌去离子水、乙二胺0.4-0.6份和二乙烯三胺1-3份,加热下搅拌反应5-15min,即为水性聚氨酯耐水煮胶粘剂主剂;将丙二醇甲醚醋酸酯1-3份、碳酸丙烯酯7-9份和脱水剂0.1-0.5份混合得到水性固化剂;将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂混合得到一种双组份水性聚氨酯耐水煮胶粘剂。将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂的质量比为(10-20):(0.1-5)配合,得到双组分水性聚氨酯耐水煮胶粘剂。按重量比m主制:m固化剂=16:1,控制涂布量为1.2-2.5g/m2,熟化:50℃/4小时,热封:160℃,压力0.2MPa/s,杀菌蒸煮条件:100℃/40min进行制备测试条件。将产品涂于标签并在试验条件下置于试验炉中,并令其互不接触。将对照组标签的温度各湿度分别保持在110℃和50%RH下72小时。试验结束时,将被测试标签从试验炉中取出,目视检测,产品与标签分离。电子剥离试验机测试3次,检测其粘结程度,产品与标签分离。

Claims (10)

1.一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,其特征在于,以重量份数计,将混合聚合物聚己二酸丁二醇酯、聚四氢呋喃醚二醇升温使其溶解,降温,加入2,2-二羟甲基丙酸、甲苯二异氰酸酯以及丙酮到反应釜中,加热下搅拌反应,降温再加入三乙胺,高速搅拌去离子水、乙二胺和二乙烯三胺,加热下搅拌反应,即为水性聚氨酯耐水煮胶粘剂主剂;将丙二醇甲醚醋酸酯、碳酸丙烯酯和脱水剂混合得到水性固化剂;将水性聚氨酯耐水煮胶粘剂主剂与水性固化剂混合得到一种双组份水性聚氨酯耐水煮胶粘剂。
2.根据权利要求1所述的一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,其特征在于:水性聚氨酯耐水煮胶粘剂主剂与水性固化剂的质量比为(10-20):(0.1-5)。
3.根据权利要求1所述的一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,其特征在于:混合聚合物二醇,以重量份数计,由聚己二酸丁二醇酯18-22份、2,2-二羟甲基丙酸1-3份、甲苯二异氰酸酯9-11份以及丙酮1-3份以及相对分子量为2000的聚四氢呋喃醚二醇9-11份、乙二胺0.4-0.6份和二乙烯三胺1-3份混合而成。
4.根据权利要求3所述的一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,其特征在于:聚己二酸丁二醇酯和聚四氢呋喃醚二醇的相对分子量均为2000。
5.根据权利要求1所述的一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,其特征在于:加热的温度均为100-160℃。
6.根据权利要求1所述的一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,其特征在于:降温到30-50℃。
7.根据权利要求1所述的一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,其特征在于:搅拌乳化的时间为1-5小时。
8.根据权利要求1所述的一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,其特征在于:混合聚合物聚己二酸丁二醇酯和聚四氢呋喃醚二醇使用前进行真空脱水。
9.根据权利要求1所述的一种双组份水性聚氨酯耐水煮胶粘剂的制备方法,其特征在于:丙二醇甲醚醋酸酯1-3份、碳酸丙烯酯7-9份和脱水剂0.1-0.5份。
10.一种根据权利要求1所述的双组份水性聚氨酯耐水煮胶粘剂的制备方法,其特征在于:按重量比m主制:m固化剂=16:1,控制涂布量为1.2-2.5g/m2,熟化:50℃/12小时,热封:160℃,压力0.2MPa/s,水煮条件:100℃/40min。
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Application publication date: 20200626