CN106883592A - 一种超耐磨耐黄变易染色超纤革用聚氨酯树脂 - Google Patents

一种超耐磨耐黄变易染色超纤革用聚氨酯树脂 Download PDF

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CN106883592A
CN106883592A CN201710155243.6A CN201710155243A CN106883592A CN 106883592 A CN106883592 A CN 106883592A CN 201710155243 A CN201710155243 A CN 201710155243A CN 106883592 A CN106883592 A CN 106883592A
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polyurethane resin
super
solvent
color inhibition
nano
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胡水仙
朱张林
张亚楠
王娟
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JIANDE CITY SHUNFA CHEMICAL ADDITIVE CO Ltd
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JIANDE CITY SHUNFA CHEMICAL ADDITIVE CO Ltd
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Abstract

本发明公开了一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，按重量百分比计，由以下原料组分混合制成：聚醚多元醇1‑15％，聚酯多元醇1‑15％，异氰酸酯5‑10％，小分子多元醇0.5‑1％，扩链剂2‑4％，封端剂1‑2％，催化剂0.02‑0.5％，抗氧化剂0.1‑1％，硅油0.5‑1％，改性纳米粉体2‑4％，溶剂余量。本发明不仅具有优异的染色性能，而且具有耐黄变、耐磨、耐水洗等良好的特性。

Description

一种超耐磨耐黄变易染色超纤革用聚氨酯树脂
技术领域
本发明涉及一种合成革用树脂，特别涉及一种超耐磨耐黄变易染色超纤革用聚氨酯树脂。
背景技术
目前，合成革已大量取代资源不足的天然皮革，用以制作箱包、服装、沙发、汽车内饰、鞋革等，具有广阔的发展前景。然而，随着人们生活水平和审美需求的提高，消费者对皮革的外观、物性和手感的要求也越来越高。
超纤合成革在外观质感、物理特性以及穿着舒适性等方面，都能与高级天然皮革相媲美。但是由于超纤合成革中的锦纶超细纤维和聚氨酯树脂，结构不同、染色差异大，从而造成了超纤革难于染色的问题；而且普通合成革不耐黄变、不耐磨，这也限制了合成革的使用。因此，超纤合成革用超耐磨耐黄变染色树脂成了发展的必要趋势。
发明内容
本发明的目的在于提供一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，不仅具有优异的染色性能(易染色、固色强、上色率高、上色均匀)，而且具有耐黄变、耐磨、耐水洗等良好的特性。
本发明解决其技术问题所采用的技术方案是：
一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，按重量百分比计，由以下原料组分混合制成：聚醚多元醇1-15％，聚酯多元醇1-15％，异氰酸酯5-10％，小分子多元醇0.5-1％，扩链剂2-4％，封端剂1-2％，催化剂0.02-0.5％，抗氧化剂0.1-1％，硅油0.5-1％，改性纳米粉体2-4％，溶剂余量。
本发明通过向聚氨酯树脂中引入纳米粉体、有机硅以及可与染料结合的基团，使产品在满足普通合成革性能的基础上，提高了合成革的耐磨性能和染色性能。本发明以聚醚多元醇和聚酯多元醇为羟基的主要供体，经过纳米粉体改性，与异氰酸酯预聚，再经扩链反应，合成一种新型的聚氨酯树脂。
本发明在聚氨酯主体结构上引入可与染料结合的基团，使产品在满足合成革基本性能要求的同时，还提高了合成革的染色性能。在聚氨酯主体结构上引入了α-活泼氢特殊处理过的纳米粉体，大大提高了树脂的耐磨性能。采用脂肪族异氰酸酯作为原料，而且在聚氨酯树脂合成过程中加入了抗氧剂，提高了树脂的耐黄变性能。
作为优选，所述的聚醚多元醇选自聚四氢呋喃二醇、聚氧化丙烯二醇、四氢呋喃-氧化丙烯共聚二醇中的一种或几种，所述的聚酯多元醇选自聚己内酯多元醇、聚碳酸酯多元醇、聚碳酸亚丙酯多元醇、聚己二酸醇酯多元醇中的一种或几种，所述聚醚多元醇以及聚酯多元醇化合物的数均分子量为1000-4000g/mol。
作为优选，所述脂肪族异氰酸酯为异佛尔酮二异氰酸酯、氢化苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯中的一种或几种。
作为优选，所述小分子多元醇选自乙二醇、丙二醇、1，4-丁二醇、1，6-己二醇中的一种或几种；所述扩链剂为二苯基甲烷二胺和N-甲基二乙醇胺按1∶0.5-2的质量比的组合。小分子多元醇作为多元醇扩链剂使用，可以提高树脂的分子量，增加树脂的硬段含量，改善树脂成膜后的力学性能与手感。扩链剂选用二苯基甲烷二胺和N-甲基二乙醇胺的组合，是因为这两种扩链剂组合后，在扩链的同时，还能提高树脂的染色性能。二苯基甲烷二胺扩链剂能与异氰酸酯形成脲键，脲键的极性比氨酯基强，与染料分子结合力强；N-甲基二乙醇胺具有叔胺结构，在酸性染液中，它可以作为结合酸性染料阴离子的染座，因此，这两种扩链剂的组合，可以大大提高树脂的染色性能。
作为优选，所述封端剂为甲醇；所述溶剂为N’N-二甲基甲酰胺。
作为优选，所述催化剂为有机铋催化剂；所述抗氧化剂为抗氧剂1010；所述硅油为端羟基聚醚改性有机硅。抗氧剂1010具有光稳定性，能保证制品的透明性及颜色稳定性；所述硅油为端羟基聚醚改性聚硅氧烷化合物，通过端羟基与异氰酸酯的反应，可在聚氨酯材料中引入有机硅组分，从而改善树脂的流平性、柔韧性、耐水性、滑爽性、耐候性和手感等。
作为优选，所述改性纳米粉体由纳米粉体经α-活泼氢改性处理而得，纳米粉体选自纳米二氧化硅、纳米二氧化钛、纳米氧化锌、纳米氧化铝中的一种或几种。纳米粉体能够在一定程度上提高有机聚合物复合材料的强度和模量。但是普通的纳米粉体在提高强度和模量的同时，因为与有机聚合物的亲和力较弱，会导致其他性能的降低。为了增加纳米粉体与聚氨酯树脂的分散性以及相容性，在提高树脂强度的同时不降低其他性能，本项目选用α-活泼氢特殊处理过的纳米粉体，其与聚氨酯树脂有很好的结合力，在聚氨酯树脂中可以得到很好的分散。引入α-活泼氢特殊处理过的纳米粉体，可以大大提高聚氨酯树脂的耐磨性能。
作为优选，所述α-活泼氢改性处理方法为：将油酸与纳米粉体按照1∶1的摩尔比配比后充分分散在水中，采用钴60辐照源的γ射线辐照处理1小时，辐照剂量率为9kGy/h，然后离心分离，用去离子水洗涤，烘干。
一种超耐磨耐黄变易染色超纤革用聚氨酯树脂的制备方法，包括以下步骤：
(1)将聚酯多元醇、聚醚多元醇、硅油加入反应釜，在110℃进行真空脱水，使其含水率小于0.03％；
(2)降温至60℃，向反应釜中加入抗氧剂、改性纳米粉体和第一次部分溶剂，搅拌混合均匀；
(3)在50℃，加入异氰酸酯、催化剂后自由升温，然后控温在80℃预聚反应3h；
(4)预聚完成后，降温至60℃，加入第二次部分溶剂以及小分子多元醇，控温在65℃反应2h；
(5)降温至55℃，加入第三次部分溶剂以及扩链剂N-甲基二乙醇胺，控温在60℃反应1h；
(6)降温至50℃，加入剩余量溶剂以及扩链剂二苯基甲烷二胺，控温在55℃反应1h；
(7)加入封端剂，反应控温在50-55℃，搅拌1h，得产品。
作为优选，第一次部分溶剂用量为溶剂总重量的10％，第二次部分溶剂用量为溶剂总重量的40％，第三次部分溶剂用量为溶剂总重量的30％。
本发明的有益效果是：
1、本发明产品制革后具有耐黄变、耐寒、耐磨、耐水洗等特性，耐黄变等级可达4以上，1.5kg压力下耐磨耗值可达1000次以上，而且易染色、上色率高、固色强，K/S值可达8.5以上。
2、本发明产品的生产工艺简单，对设备、环境无严格要求。
3、该染色树脂具有很好的耐磨性，用此树脂制成的革具有很强的真皮感，可将其应用领域由普通的服装革扩展到鞋革、箱包革上。
具体实施方式
下面通过具体实施例，对本发明的技术方案作进一步的具体说明。
本发明中，若非特指，所采用的原料和设备等均可从市场购得或是本领域常用的。下述实施例中的方法，如无特别说明，均为本领域的常规方法。
总实施方案：
一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，按重量百分比计，由以下原料组分混合制成：聚醚多元醇1-15％，聚酯多元醇1-15％，异氰酸酯5-10％，小分子多元醇0.5-1％，扩链剂2-4％，封端剂1-2％，催化剂0.02-0.5％，抗氧化剂0.1-1％，硅油0.5-1％，改性纳米粉体2-4％，溶剂余量。
所述的聚醚多元醇选自聚四氢呋喃二醇、聚氧化丙烯二醇、四氢呋喃-氧化丙烯共聚二醇中的一种或几种，所述的聚酯多元醇选自聚己内酯多元醇、聚碳酸酯多元醇、聚碳酸亚丙酯多元醇、聚己二酸醇酯多元醇中的一种或几种，所述聚醚多元醇以及聚酯多元醇化合物的数均分子量为1000-4000g/mol。所述脂肪族异氰酸酯为异佛尔酮二异氰酸酯、氢化苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯中的一种或几种。所述小分子多元醇选自乙二醇、丙二醇、1，4-丁二醇、1，6-己二醇中的一种或几种；所述扩链剂为二苯基甲烷二胺和N-甲基二乙醇胺按1∶0.5-2的质量比的组合。所述封端剂为甲醇；所述溶剂为N’N-二甲基甲酰胺。所述催化剂为有机铋催化剂(市售，美国气体化工的有机铋催化剂Dabco MB20)；所述抗氧化剂为抗氧剂1010；所述硅油为端羟基聚醚改性有机硅(市售，上海泰格聚合物技术有限公司的有机硅改性剂Tech-2127)。
所述改性纳米粉体由纳米粉体经α-活泼氢改性处理而得，纳米粉体选自纳米二氧化硅、纳米二氧化钛、纳米氧化锌、纳米氧化铝中的一种或几种。所述α-活泼氢改性处理方法为：将油酸与纳米粉体按照1∶1的摩尔比配比后充分分散在水中，采用钴60辐照源的γ射线辐照处理1小时，辐照剂量率为9kGy/h，然后离心分离，用去离子水洗涤，烘干。
制备方法，包括以下步骤：
(1)将聚酯多元醇、聚醚多元醇、硅油加入反应釜，在110℃进行真空脱水，使其含水率小于0.03％；
(2)降温至60℃，向反应釜中加入抗氧剂、改性纳米粉体和第一次部分溶剂(溶剂总重量的10％)，搅拌混合均匀；
(3)在50℃，加入异氰酸酯、催化剂后自由升温，然后控温在80℃预聚反应3h；
(4)预聚完成后，降温至60℃，加入第二次部分溶剂(溶剂总重量的40％)以及小分子多元醇，控温在65℃反应2h；
(5)降温至55℃，加入第三次部分溶剂(溶剂总重量的30％)以及扩链剂N-甲基二乙醇胺，控温在60℃反应1h；
(6)降温至50℃，加入剩余量溶剂(溶剂总重量的20％)以及扩链剂二苯基甲烷二胺，控温在55℃反应1h；
(7)加入封端剂，反应控温在50-55℃，搅拌1h，得产品。
以下具体实施例中：催化剂为有机铋催化剂(市售，美国气体化工的有机铋催化剂Dabco MB20)所述抗氧化剂为抗氧剂1010；所述硅油为端羟基聚醚改性有机硅(市售，上海泰格聚合物技术有限公司的有机硅改性剂Tech-2127)。封端剂为甲醇；所述溶剂为N’N-二甲基甲酰胺。
具体实施例1：
一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，由以下重量百分比计的组分制成：聚醚多元醇4％，聚酯多元醇8％，异氰酸酯8.6％，小分子多元醇0.8％，扩链剂2.2％，封端剂1.5％，催化剂0.1％，抗氧化剂0.5％，硅油0.5％、改性纳米粉体3.5％，其余为溶剂。
本实施例中：聚醚多元醇为聚四氢呋喃二醇，且数均分子量为2000g/mol；聚酯多元醇为聚酯多元醇HP3020，且数均分子量为2000g/mol；异氰酸酯为氢化苯基甲烷二异氰酸酯；小分子多元醇为1，4丁二醇；扩链剂为二苯基甲烷二胺和N-甲基二乙醇胺的混合物，且质量比为1∶1；改性纳米粉体为纳米二氧化硅与纳米二氧化钛的混合物(质量比为5∶2)经α-活泼氢改性处理而得。α-活泼氢改性处理方法为：将油酸与纳米二氧化硅与纳米二氧化钛的混合物按照1∶1的摩尔比配比后充分分散在水中，采用钴60辐照源的γ射线辐照处理1小时，辐照剂量率为9kGy/h，然后离心分离，用去离子水洗涤，烘干。
制备方法，依次包括以下步骤：
(1)将聚酯多元醇、聚醚多元醇、硅油加入反应釜，在110℃进行真空脱水，使其含水率小于0.03％；
(2)降温至60℃，向反应釜中加入抗氧剂、改性纳米粉体和部分溶剂(溶剂总量的10％)，搅拌混合均匀；
(3)在50℃，加入异氰酸酯、催化剂后自由升温，然后控温在80℃预聚反应3h；
(4)预聚完成后，降温至60℃，加入部分溶剂(溶剂总量的40％)以及小分子多元醇扩链剂，控温在65℃反应2h；
(5)降温至55℃，加入部分溶剂(溶剂总量的30％)以及N-甲基二乙醇胺，控温在60℃反应1h；
(6)降温至50℃，加入部分溶剂(溶剂总量的20％)以及二苯基甲烷二胺，控温在55℃反应1h；
(7)加入甲醇终止，反应控温在50-55℃，搅拌1h，得产品。
具体实施例2：
一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，由以下重量百分比计的组分制成：聚醚多元醇2％，聚酯多元醇10％，异氰酸酯9％，小分子多元醇0.6％，扩链剂3％，封端剂2％，催化剂0.05％，抗氧化剂0.25％，硅油0.5％、改性纳米粉体3％，其余为溶剂。
本实施例中：聚醚多元醇为聚氧化丙烯二醇，且数均分子量为2000g/mol；聚酯多元醇为聚己内酯多元醇与聚碳酸酯多元醇的混合物，且数均分子量均为2000g/mol，其质量比4∶1；异氰酸酯为异佛尔酮二异氰酸酯与氢化苯基甲烷二异氰酸酯的混合物，且质量比为2∶1；小分子多元醇为丙二醇；扩链剂为二苯基甲烷二胺和N-甲基二乙醇胺的混合物，且质量比为2∶1；改性纳米粉体为纳米二氧化硅与纳米氧化铝的混合物(质量比为2∶1)经α-活泼氢改性处理而得。α-活泼氢改性处理方法为：将油酸与纳米二氧化硅与纳米氧化铝的混合物按照1∶1的摩尔比配比后充分分散在水中，采用钴60辐照源的γ射线辐照处理1小时，辐照剂量率为9kGy/h，然后离心分离，用去离子水洗涤，烘干。
制备方法，依次包括以下步骤：
(1)将聚酯多元醇、聚醚多元醇、硅油加入反应釜，在110℃进行真空脱水，使其含水率小于0.03％；
(2)降温至60℃，向反应釜中加入抗氧剂、改性纳米粉体和部分溶剂(溶剂总量的10％)，搅拌混合均匀；
(3)在50℃，加入异氰酸酯、催化剂后自由升温，然后控温在80℃预聚反应3h；
(4)预聚完成后，降温至60℃，加入部分溶剂(溶剂总量的40％)以及小分子多元醇扩链剂，控温在65℃反应2h；
(5)降温至55℃，加入部分溶剂(溶剂总量的30％)以及N-甲基二乙醇胺，控温在60℃反应1h；
(6)降温至50℃，加入部分溶剂(溶剂总量的20％)以及二苯基甲烷二胺，控温在55℃反应1h；
(7)加入甲醇终止，反应控温在50-55℃，搅拌1h，得产品。
具体实施例3：
一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，由以下重量百分比计的组分制成：聚醚多元醇10％，聚酯多元醇3％，异氰酸酯6.2％，小分子多元醇0.7％，扩链剂2.4％，封端剂1.8％，催化剂0.2％，抗氧化剂0.6％，硅油0.8％、纳米粉体2.5％，其余为溶剂。
本实施例中：聚醚多元醇为四氢呋喃-氧化丙烯共聚二醇，且数均分子量为1000g/mol；聚酯多元醇为聚己二酸1，4-丁二醇酯，且数均分子量为2000g/mol；异氰酸酯为六亚甲基二异氰酸酯；小分子多元醇为1，6-己二醇；扩链剂为二苯基甲烷二胺和N-甲基二乙醇胺的混合物(质量比为1∶2)；改性纳米粉体为纳米氧化锌经α-活泼氢改性处理而得。α-活泼氢改性处理方法为：将油酸与纳米氧化锌按照1∶1的摩尔比配比后充分分散在水中，采用钴60辐照源的γ射线辐照处理1小时，辐照剂量率为9kGy/h，然后离心分离，用去离子水洗涤，烘干。。
超耐磨耐黄变易染色超纤革用聚氨酯树脂的制备方法，依次包括以下步骤：
(1)将聚酯多元醇、聚醚多元醇、硅油加入反应釜，在110℃进行真空脱水，使其含水率小于0.03％；
(2)降温至60℃，向反应釜中加入抗氧剂、改性纳米粉体和部分溶剂(溶剂总量的10％)，搅拌混合均匀；
(3)在50℃，加入异氰酸酯、催化剂后自由升温，然后控温在80℃预聚反应3h；
(4)预聚完成后，降温至60℃，加入部分溶剂(溶剂总量的40％)以及小分子多元醇扩链剂，控温在65℃反应2h；
(5)降温至55℃，加入部分溶剂(溶剂总量的30％)以及N-甲基二乙醇胺，控温在60℃反应1h；
(6)降温至50℃，加入部分溶剂(溶剂总量的20％)以及二苯基甲烷二胺，控温在55℃反应1h；
(7)加入甲醇终止，反应控温在50-55℃，搅拌1h，得产品。
以上所述的实施例只是本发明的一种较佳的方案，并非对本发明作任何形式上的限制，在不超出权利要求所记载的技术方案的前提下还有其它的变体及改型。

Claims (10)

1.一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，其特征在于，按重量百分比计，由以下原料组分混合制成：聚醚多元醇1-15％，聚酯多元醇1-15％，异氰酸酯5-10％，小分子多元醇0.5-1％，扩链剂2-4％，封端剂1-2％，催化剂0.02-0.5％，抗氧化剂0.1-1％，硅油0.5-1％，改性纳米粉体2-4％，溶剂余量。
2.根据权利要求1所述的一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，其特征在于，所述的聚醚多元醇选自聚四氢呋喃二醇、聚氧化丙烯二醇、四氢呋喃-氧化丙烯共聚二醇中的一种或几种，所述的聚酯多元醇选自聚己内酯多元醇、聚碳酸酯多元醇、聚碳酸亚丙酯多元醇、聚己二酸醇酯多元醇中的一种或几种，所述聚醚多元醇以及聚酯多元醇化合物的数均分子量为1000-4000g/mol。
3.根据权利要求1所述的一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，其特征在于，所述脂肪族异氰酸酯为异佛尔酮二异氰酸酯、氢化苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯中的一种或几种。
4.根据权利要求1所述的一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，其特征在于，所述小分子多元醇选自乙二醇、丙二醇、1，4-丁二醇、1，6-已二醇中的一种或几种；所述扩链剂为二苯基甲烷二胺和N-甲基二乙醇胺按1∶0.5-2的质量比的组合。
5.根据权利要求1所述的一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，其特征在于，所述封端剂为甲醇；所述溶剂为N’N-二甲基甲酰胺。
6.根据权利要求1所述的一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，其特征在于，所述催化剂为有机铋催化剂；所述抗氧化剂为抗氧剂1010；所述硅油为端羟基聚醚改性有机硅。
7.根据权利要求1所述的一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，其特征在于，所述改性纳米粉体由纳米粉体经α-活泼氢改性处理而得，纳米粉体选自纳米二氧化硅、纳米二氧化钛、纳米氧化锌、纳米氧化铝中的一种或几种。
8.根据权利要求1所述的一种超耐磨耐黄变易染色超纤革用聚氨酯树脂，其特征在于，所述α-活泼氢改性处理方法为：将油酸与纳米粉体按照1∶1的摩尔比配比后充分分散在水中，采用钴60辐照源的γ射线辐照处理1小时，辐照剂量率为9kGy/h，然后离心分离，用去离子水洗涤，烘干。
9.如权利要求1所述的一种超耐磨耐黄变易染色超纤革用聚氨酯树脂的制备方法，其特征在于，包括以下步骤：
(1)将聚酯多元醇、聚醚多元醇、硅油加入反应釜，在110℃进行真空脱水，使其含水率小于0.03％；
(2)降温至60℃，向反应釜中加入抗氧剂、改性纳米粉体和第一次部分溶剂，搅拌混合均匀；
(3)在50℃，加入异氰酸酯、催化剂后自由升温，然后控温在80℃预聚反应3h；
(4)预聚完成后，降温至60℃，加入第二次部分溶剂以及小分子多元醇，控温在65℃反应2h；
(5)降温至55℃，加入第三次部分溶剂以及扩链剂N-甲基二乙醇胺，控温在60℃反应1h；
(6)降温至50℃，加入剩余量溶剂以及扩链剂二苯基甲烷二胺，控温在55℃反应1h；
(7)加入封端剂，反应控温在50-55℃，搅拌1h，得产品。
10.根据权利要求9所述的制备方法，其特征在于，第一次部分溶剂用量为溶剂总重量的10％，第二次部分溶剂用量为溶剂总重量的40％，第三次部分溶剂用量为溶剂总重量的30％。
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