CN105237725B - 一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂及其制备方法 - Google Patents

一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂及其制备方法 Download PDF

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CN105237725B
CN105237725B CN201510581307.XA CN201510581307A CN105237725B CN 105237725 B CN105237725 B CN 105237725B CN 201510581307 A CN201510581307 A CN 201510581307A CN 105237725 B CN105237725 B CN 105237725B
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田海英
姚克俭
武春余
吴兴保
张彪
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HEFEI ANLI POLYURETHANE NEW MATERIAL CO Ltd
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Abstract

本发明公开了一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂及其制备方法，聚氨酯树脂主要是由以下组分按重量份比制备而成：异氰酸酯9‑11份；有机硅油0.5‑5份；多元醇化合物13‑20份；二元醇扩链剂1‑4份；抗氧剂0‑0.3份；反应终止剂0‑0.05份；有机锡类或有机铋类催化剂，添加量为多元醇化合物重量的0.001‑0.05%。本发明制备的聚氨酯树脂较大改善和提高了中硬质镜面面层聚氨酯树脂的耐寒性能和抗热粘连性能，制造的合成革鞋革经久耐用，具有市场竞争力。

Description

一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂及其 制备方法
技术领域
本发明涉及合成革加工领域，具体是一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂及其制备方法。
背景技术
由于聚氨酯合成革鞋革市场的不断扩大，人们对鞋革物性的要求越来越高，尤其是运动休闲鞋的使用环境，使得提高聚氨酯的耐曲挠性能尤为关键，既要求柔软舒适，耐曲挠性能好，又要手感滑爽，防止粘连，防尘防涂鸦。然而，现有聚氨酯树脂很难兼顾柔韧性，耐寒性，防止粘连以及革面的滑爽度。
发明内容
本发明要解决的技术问题是提供一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂及其制备方法，解决了现有的聚氨酯树脂很难兼顾柔韧性，耐寒性，防止粘连以及革面滑爽度的问题。
本发明的技术方案为：
一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂，主要是由以下组分按重量份比制备而成：
有机锡类或有机铋类催化剂，添加量为多元醇化合物重量的0.001-0.05％；所述的有机硅油的分子量为2000；所述的多元醇化合物包括有聚酯多元醇和聚醚多元醇，其中，聚酯多元醇和聚醚多元醇的质量比为1:2—3；所述的多元醇化合物的平均分子量为1000-3000。
所述的异氰酸酯为4,4′-二苯基甲烷二异氰酸酯。
所述的二元醇扩链剂为乙二醇、1,4-丁二醇、1,6-己二醇中的一种或两种的混合物，当乙二醇和1,4-丁二醇两种醇混合使用时，两种醇的摩尔比例为0.1—10：1。
所述的反应终止剂为甲醇。
所述的聚酯多元醇选用己二酸系聚酯多元醇；所述的聚醚多元醇选用聚四氢呋喃醚多元醇。
所述的有机硅油的官能度为2；所述的聚酯多元醇的官能度为2；所述的聚醚多元醇的官能度为2。
一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂的制备方法，具体包括有以下步骤：
(1)、将多元醇化合物、抗氧剂、有机硅油加在一起，搅拌混合均匀后加入有机锡类或有机铋类催化剂以及占异氰酸酯总重量40％的异氰酸酯，于65—75℃反应60分钟，生成聚酯聚醚多元醇和有机硅油二元醇共聚的异氰酸酯封端的预聚体；
(2)、向步骤1)合成的预聚体中加入有机溶剂，稀释成固含40-50％的有机体系，再加入二元醇扩链剂，搅拌均匀后逐步加入余量的异氰酸酯，在65—75℃下每步反应30—40分钟，共增黏反应3-5h，在反应的过程中随着体系粘度的增加不断补充有机溶剂使得最终粘度控制在80-120Pa·s/25℃，固含量控制在29—31％，反应完成后加入反应终止剂甲醇即可。
所述的有机溶剂选用N,N-二甲基甲酰胺；所述的多元醇化合物、异氰酸酯、二元醇扩链剂、溶剂的含水率均小于500ppm。
本发明的优点：
本发明制备的聚氨酯树脂解决了现有的聚氨酯树脂很难兼顾柔韧性，耐寒性，防止粘连以及革面滑爽度的问题。使用本发明的中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂制成的合成革鞋革具有耐寒性高、抗热粘连性好、革面滑爽度好等特点，产品经久耐用，产品档次高，具有市场竞争力。
具体实施方式
下面给出实施例以对本发明进行具体的描述，有必要在此指出的是以下实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，该领域的技术熟练人员根据本发明内容对本发明做出的一些非本质的改进和调整仍属于本发明的保护范围。
实施例1
一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂，主要是由以下组分按重量比制备而成：
一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂的制备方法，具体包括有以下步骤:
(1)、将SP-1、PTMG-2、抗氧剂I-1010、有机硅油加在一起，搅拌混合均匀后加入有机铋类催化剂(8106，美国领先化学品公司生产)以及占MDI总重量39％的MDI，于65—75℃反应60分钟，生成聚酯聚醚多元醇和有机硅油二元醇共聚的异氰酸酯封端的预聚体；
(2)、向步骤1)合成的预聚体中加入DMF溶剂，稀释成固含40-50％的有机体系，再加入二元醇扩链剂，搅拌均匀后逐步加入余量的MDI，在65—75℃下每步反应30—40分钟，共增黏反应3-5h，在反应的过程中随着体系粘度的增加不断补充DMF溶剂使得最终粘度控制在80-120Pa·s/25℃，固含量控制在29—31％，反应完成后加入反应终止剂甲醇即可。
其中，上述的SP-1、PTMG-2、MDI、二元醇扩链剂、DMF溶剂的含水率均小于500ppm。
实施例2
一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂，主要是由以下组分按重量比制备而成：
一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂的制备方法，具体包括有以下步骤:
(1)、将SP-1、PTMG-2、抗氧剂I-1010、有机硅油加在一起，搅拌混合均匀后加入有机铋类催化剂(8106，美国领先化学品公司生产)以及占MDI总重量41％的MDI，于65—75℃反应60分钟，生成聚酯聚醚多元醇和有机硅油二元醇共聚的异氰酸酯封端的预聚体；
(2)、向步骤1)合成的预聚体中加入DMF溶剂，稀释成固含40-50％的有机体系，再加入二元醇扩链剂，搅拌均匀后逐步加入余量的MDI，在65—75℃下每步反应30—40分钟，共增黏反应3-5h，在反应的过程中随着体系粘度的增加不断补充DMF溶剂使得最终粘度控制在80-120Pa·s/25℃，固含量控制在29—31％，反应完成后加入反应终止剂甲醇即可。
其中，上述的SP-1、PTMG-2、MDI、二元醇扩链剂、DMF溶剂的含水率均小于500ppm。
验证效果方案：
为了验证本发明所述的中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂具有更高的耐寒性，具有较好的抗热粘连性，把上述实施方案1—2所制备的树脂和普通耐寒性镜面树脂对比，按如下配方制成合成革，具体制革配方如下：
面层：树脂 90；
N,N-二甲基甲酰胺(DMF) 70；
1A70色粉 1；
粘结层：SA-3635无色涂料 150；
IA70色粉 1；
底坯：黑色无纺布高剥离16小时耐水解贴镜面革用湿法坯革；
其中，1A70色粉为佛山市顺德区宝斯特颜料有限公司的产品。
SA-3635无色涂料为合肥安利聚氨酯新材料有限公司的产品。
生产工艺：两刀厚度均涂15丝，烘干温度130-135℃
用上述配方制成的聚氨酯合成革，在-20℃耐寒机中挠曲8万次，发现该产品革面未开裂，由此可见镜面面层耐寒性能得到了提高。将革样裁剪成10×10㎝方块两个，革面对贴后，在其上面压3㎏重的正方铁块，在100℃烘箱，恒温放置1小时后拿出，在室温放置30分钟，再用拉力机将两块革撕开，与普通耐寒性镜面树脂生产的合成革产品相比，本发明用力小，说明该镜面面层的抗热粘连性提高，革面较滑爽。
本说明书及本申请的权利要求书中，所谓体系，是指整个反应体系，就是所有物质的总量。上述实施方案和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其同物界定。

Claims (8)

1.一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂，其特征在于：主要是由以下组分按重量份比制备而成：
异氰酸酯 9-11份；
有机硅油 0.5-5份；
多元醇化合物 13-20份；
二元醇扩链剂 1-4份；
抗氧剂 0-0.3份；
反应终止剂 0-0.05份；
有机锡类或有机铋类催化剂，添加量为多元醇化合物重量的0.001-0.05%；所述的有机硅油的分子量为2000；所述的多元醇化合物包括有聚酯多元醇和聚醚多元醇，其中，聚酯多元醇和聚醚多元醇的质量比为1:2—3；所述的多元醇化合物的平均分子量为1000-3000。
2.根据权利要求1所述的一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂，其特征在于：所述的异氰酸酯为4,4′-二苯基甲烷二异氰酸酯。
3.根据权利要求1所述的一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂，其特征在于：所述的二元醇扩链剂为乙二醇、1,4-丁二醇、1,6-己二醇中的一种或两种的混合物，当乙二醇和1,4-丁二醇两种醇混合使用时，两种醇的摩尔比例为0.1—10：1。
4.根据权利要求1所述的一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂，其特征在于：所述的反应终止剂为甲醇。
5.根据权利要求1所述的一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂，其特征在于：所述的聚酯多元醇选用己二酸系聚酯多元醇；所述的聚醚多元醇选用聚四氢呋喃醚多元醇。
6.根据权利要求1所述的一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂，其特征在于：所述的有机硅油的官能度为2；所述的聚酯多元醇的官能度为2；所述的聚醚多元醇的官能度为2。
7.根据权利要求1所述的一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂的制备方法，其特征在于：具体包括有以下步骤：
（1）、将多元醇化合物、抗氧剂、有机硅油加在一起，搅拌混合均匀后加入有机锡类或有机铋类催化剂以及占异氰酸酯总重量40%的异氰酸酯，于65—75℃反应60分钟，生成聚酯聚醚多元醇和有机硅油二元醇共聚的异氰酸酯封端的预聚体；
（2）、向步骤1）合成的预聚体中加入有机溶剂，稀释成固含40-50%的有机体系，再加入二元醇扩链剂，搅拌均匀后逐步加入余量的异氰酸酯，在65—75℃下每步反应30—40分钟，共增黏反应3-5h，在反应的过程中随着体系粘度的增加不断补充有机溶剂使得最终粘度控制在80-120Pa·s/25℃，固含量控制在29—31%，反应完成后加入反应终止剂甲醇即可。
8.根据权利要求7所述的一种中硬质高耐寒抗热粘连滑爽型镜面面层聚氨酯树脂的制备方法，其特征在于：所述的有机溶剂选用N,N-二甲基甲酰胺；所述的多元醇化合物、异氰酸酯、二元醇扩链剂、溶剂的含水率均小于500ppm。
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