CN106117509A - 一种耐增塑剂单组份水性聚氨酯树脂及其制备方法 - Google Patents

一种耐增塑剂单组份水性聚氨酯树脂及其制备方法 Download PDF

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CN106117509A
CN106117509A CN201610615361.6A CN201610615361A CN106117509A CN 106117509 A CN106117509 A CN 106117509A CN 201610615361 A CN201610615361 A CN 201610615361A CN 106117509 A CN106117509 A CN 106117509A
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颜志鸿
吕华波
江平
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XUCHUAN CHEMICAL (SUZHOU) CO Ltd
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Abstract

本发明公开了一种耐增塑剂单组份水性聚氨酯树脂，属于聚氨酯树脂技术领域，除水以外包括以下重量百分比的组分：30％‑80％的多羟基化合物、0.5％‑15％的离子或潜力型亲水化合物、5％‑45％的异氰酸酯化合物、0.5％‑10％的含有羟基或氨基的低分子量化合物；其中，多羟基化合物分子量为400‑6000，含有羟基或氨基的低分子量化合物分子量为40‑500。本发明还公开了其制备方法；本发明一种耐增塑剂单组份水性聚氨酯树脂，使用葵二酸、丁二酸为原料的多羟基化合物，具有粘结力强、耐增塑剂、耐热性好的优点；本发明的制备方法，制备方法简便、用现有设备可以生产。

Description

一种耐增塑剂单组份水性聚氨酯树脂及其制备方法
技术领域
本发明属于聚氨酯树脂技术领域，具体涉及一种耐增塑剂单组份水性聚氨酯树脂及其制备方法。
背景技术
目前，溶剂型聚氨酯树脂作为传统合成革制品的基本原料，其生产过程大多采用二甲基甲酸胺(DMF)、甲苯等作为溶剂。在溶剂型的干法生产中溶剂很少，这不仅造成了有机溶剂和能源的大量浪费，还势必会严重影响生态环境。欧共体最新生态标准也将有毒有害的溶剂可使用范围有了新的界定，同时我国环保部门对皮革行业的污水排放规定DMF含量在2mg/L以下。
水性聚氨酯树脂以水为分散介质，具有不燃、无毒、安全、环保等优点，水性聚氨酯树脂的开发应用成为国内外研究的热点，几乎所有的大的化学公司、中小型的化学公司和大学的研究中心都投入了大量的人力和物力进行了水性聚氨酯树脂的研究和开发。
普通单组份水性聚氨酯耐增塑剂、耐热性差；溶剂型聚氨酯污染较严重，耐增塑剂一般。目前耐增塑剂单组份水性聚氨酯树脂，鲜见公开报道。
发明内容
发明目的：本发明的目的在于提供一种耐增塑剂单组份水性聚氨酯树脂，不但耐增塑剂、耐热好，而且耐久性好，应用于半PU合成革的服装革、沙发革、汽车革等领域。
技术方案：为实现上述发明目的，本发明采用如下技术方案：
一种耐增塑剂单组份水性聚氨酯树脂，除水以外包括以下重量百分比的组分：30％-80％的多羟基化合物、0.5％-15％的离子或潜力型亲水化合物、5％-45％的异氰酸酯化合物、0.5％-10％的含有羟基或氨基的低分子量化合物；其中，多羟基化合物分子量为400-6000，含有羟基或氨基的低分子量化合物分子量为40-500。
所述的多羟基化合物包括以下重量百分比的组分：40％-90％的聚酯多元醇、10％-30％聚醚多元醇和5％-25％聚碳酸酯多元醇。
所述的聚酯多元醇选自使用葵二酸、丁二酸为原料的多羟基化合物，包括聚葵二酸己二酸丁二酸与己二醇丁二醇酯二醇、聚葵二酸己二酸与己二醇酯二醇、聚葵二酸己二酸与丁二醇酯二醇、聚己二酸乙二醇己二醇酯二醇、聚己二酸新戊二醇己二醇酯二醇和聚己二酸新戊二醇丁二醇酯二醇；所述的聚醚多元醇选自聚氧化丙烯二醇、聚四氢呋喃二元醇和聚氧化乙烯二醇。
所述的离子或潜力型亲水化合物是指带有-COOY、SO3Y、-PO(OY)2、-NR2、-NR3+基团的化合物，其中Y选自H、NH4+和金属阳离子，R选自H、烷基和芳基。包括二氨基磺酸盐、二羟甲基丙酸、二羟甲基丁酸、羟基新戊酸、2-(2-氨基乙基氨基)乙磺酸、和环己基氨基丙磺酸等。
所述的异氰酸酯化合物包括以下重量百分比的组分：10％-90％脂肪族异氰酸酯化合物和不超过50％芳香族多异氰酸酯化合物。
所述的含有羟基或氨基的低分子量化合物选自醇胺类、胺类、二元胺、二元醇、三元醇和三元胺。
所述的高耐磨单组份软质水性聚氨酯树脂的制备方法，包括如下步骤：
1)向反应釜中加入5％-45％的异氰酸酯化合物、30％-80％的多羟基化合物、控温80-90℃，常压下反应5h，得到多元醇与异氰酸酯的预聚体；
2)向步骤1)预聚体中再加入加入0.5％-15％的离子或潜力型亲水化合物、0.5％-10％的含有羟基或氨基的低分子量化合物，控温80-100℃，常压下反应2h；待体系NCO含量达到理论值后，降温至40-70℃，加入适量溶剂丙酮和二甲基乙醇胺反应45分钟，在高速搅拌的条件下加入去离子水，乳化45分钟后加入乙二胺和二乙烯三胺，控温30-50℃，常压下反应2h，加入适量消泡剂在一定条件下抽除溶剂丙酮，反应得到水性聚氨酯乳液；
3)向步骤2)水性聚氨酯乳液中最后加入增稠剂、润湿流平剂，常温搅拌1h，制得耐增塑剂单组份水性聚氨酯。
8、根据权利要求7所述的耐增塑剂单组份水性聚氨酯树脂的制备方法，其特征在于：步骤3)中，所述的润湿流平剂为改性聚硅氧烷或聚醚改性聚二甲基硅氧烷；增稠剂为缔合型水性聚氨酯。
有益效果：现有水性树脂粘结牢度不够，只能做要求不高的产品；或者为双组份树脂，需要使用时再加入架桥剂；与现有技术相比，本发明的耐增塑剂单组份水性聚氨酯树脂，具备以下优势：首次使用含有葵二酸、丁二酸为原料的多羟基化合物，制备的水性聚氨酯树脂具有粘结牢度高、耐增塑剂、耐久性好的特点；本发明的耐增塑剂单组份水性聚氨酯树脂制备方法简便、用现有设备可以生产。
具体实施方式
下面结合具体实施方式，进一步阐明本发明。
一种耐增塑剂单组份水性聚氨酯树脂，除水以外包括以下重量百分比的组分：30％-80％的多羟基化合物、0.5％-15％的离子或潜力型亲水化合物、5％-45％的异氰酸酯化合物、0.5％-10％的含有羟基或氨基的低分子量化合物；其中，多羟基化合物分子量为400-6000，含有羟基或氨基的低分子量化合物分子量为40-500。
多羟基化合物包括以下重量百分比的组分：40％-90％的聚酯多元醇、10％-30％聚醚多元醇和5％-25％聚碳酸酯多元醇。
所述的多羟基化合物包括以下重量百分比的组分：40％-90％的聚酯多元醇、10％-30％聚醚多元醇和5％-25％聚碳酸酯多元醇。
所述的聚酯多元醇选自使用葵二酸、丁二酸为原料的多羟基化合物，包括聚葵二酸己二酸丁二酸与己二醇丁二醇酯二醇、聚葵二酸己二酸与己二醇酯二醇、聚葵二酸己二酸与丁二醇酯二醇、聚己二酸乙二醇己二醇酯二醇、聚己二酸新戊二醇己二醇酯二醇和聚己二酸新戊二醇丁二醇酯二醇；所述的聚醚多元醇选自聚氧化丙烯二醇、聚四氢呋喃二元醇和聚氧化乙烯二醇。
所述的离子或潜力型亲水化合物是指带有-COOY、SO3Y、-PO(OY)2、-NR2、-NR3+基团的化合物，其中Y选自H、NH4+和金属阳离子，R选自H、烷基和芳基。包括二氨基磺酸盐、二羟甲基丙酸、二羟甲基丁酸、羟基新戊酸、2-(2-氨基乙基氨基)乙磺酸、和环己基氨基丙磺酸等。
所述的异氰酸酯化合物包括以下重量百分比的组分：10％-90％脂肪族异氰酸酯化合物和不超过50％芳香族多异氰酸酯化合物。
10％-90％脂肪族异氰酸酯化合物，包括二环己基甲烷二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HDI)、异氟尔酮二异氰酸酯(IPDI)；不超过50％芳香族多异氰酸酯化合物，包括甲苯二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯(MDI)。
含有羟基或氨基的低分子量化合物选自醇胺类、胺类、二元胺、二元醇、三元醇和三元胺。包括乙二醇、丙二醇、二甘醇、丁二醇、三甘醇、三羟甲基丙烷、乙二胺、二乙烯三胺以及三乙胺、N-甲基二乙醇胺。
高耐磨单组份软质水性聚氨酯树脂，制备方法如下：
1)向反应釜中加入，22.3kg二环己基甲烷二异氰酸酯(HMDI)、0.8kg甲苯二异氰酸酯(TDI)、25.2kg聚葵二酸己二酸丁二酸与己二醇丁二醇酯二醇(分子量3000)、8.1kg四氢呋喃共聚二醇(分子量2000)，2.1kg聚己二酸新戊二醇己二醇酯二醇(分子量1000)控温80-90℃，常压下反应5h；得预聚体
2)再加入1.5kg二羟甲基丙酸、1.2kg丁二醇、0.35kg三羟甲基丙烷，控温80-100℃，常压下反应2h；待体系NCO含量达到理论值后，降温至40-70℃，加入适量溶剂丙酮和1.3kg二甲基乙醇胺反应45分钟，在高速搅拌的条件下加入去离子水，乳化45分钟后加入0.6kg乙二胺和0.1kg二乙烯三胺，控温30-50℃，常压下反应2h，加入0.1kg消泡剂在一定条件下抽除溶剂丙酮，
3)最后加入1kg增稠剂、0.1kg润湿流平剂，常温搅拌1h，制得高耐磨单组份软质水性聚氨酯树脂。
润湿流平剂为改性聚硅氧烷，如Levaslip 455(商用名)；或为聚醚改性聚二甲基硅氧烷，如Wet-250(商用名)。消泡剂为聚醚改性有机硅类化合物，如BYK-020(商用名)；消泡剂为二炔类化合物，如Surfynol DF-75(商用名)；增稠剂为缔合型水性聚氨酯，如UH-420(商用名)或为碱溶胀型聚丙烯酸乳液，如ASE-60(商用名)。
高耐磨单组份软质水性聚氨酯树脂制革应用，将水性聚氨酯树脂刮涂在PVC发泡层上，贴基布，烘干，做成革。测试剥离强度并做耐久性测试。

Claims (8)

1.一种耐增塑剂单组份水性聚氨酯树脂，其特征在于：除水以外包括以下重量百分比的组分：30％-80％的多羟基化合物、0.5％-15％的离子或潜力型亲水化合物、5％-45％的异氰酸酯化合物、0.5％-10％的含有羟基或氨基的低分子量化合物；其中，多羟基化合物分子量为400-6000，含有羟基或氨基的低分子量化合物分子量为40-500。
2.根据权利要求1所述的一种耐增塑剂单组份水性聚氨酯树脂，其特征在于：所述的多羟基化合物包括以下重量百分比的组分：40％-90％的聚酯多元醇、10％-30％聚醚多元醇和5％-25％聚碳酸酯多元醇。
3.根据权利要求1所述的一种耐增塑剂单组份水性聚氨酯树脂，其特征在于：所述的聚酯多元醇选自使用葵二酸、丁二酸为原料的多羟基化合物，包括聚葵二酸己二酸丁二酸与己二醇丁二醇酯二醇、聚葵二酸己二酸与己二醇酯二醇、聚葵二酸己二酸与丁二醇酯二醇、聚己二酸乙二醇己二醇酯二醇、聚己二酸新戊二醇己二醇酯二醇和聚己二酸新戊二醇丁二醇酯二醇；所述的聚醚多元醇选自聚氧化丙烯二醇、聚四氢呋喃二元醇和聚氧化乙烯二醇。
4.根据权利要求1所述的一种耐增塑剂单组份水性聚氨酯树脂，其特征在于：所述的离子或潜力型亲水化合物是指带有-COOY、SO3Y、-PO(OY)2、-NR2、-NR3+基团的化合物，其中Y选自H、NH4+和金属阳离子，R选自H、烷基和芳基。包括二氨基磺酸盐、二羟甲基丙酸、二羟甲基丁酸、羟基新戊酸、2-(2-氨基乙基氨基)乙磺酸、和环己基氨基丙磺酸等。
5.根据权利要求1所述的一种耐增塑剂单组份水性聚氨酯树脂，其特征在于：所述的异氰酸酯化合物包括以下重量百分比的组分：10％-90％脂肪族异氰酸酯化合物和不超过50％芳香族多异氰酸酯化合物。
6.根据权利要求1所述的一种耐增塑剂单组份水性聚氨酯树脂，其特征在于：所述的含有羟基或氨基的低分子量化合物选自醇胺类、胺类、二元胺、二元醇、三元醇和三元胺。
7.权利要求1～6中任意一项所述的高耐磨单组份软质水性聚氨酯树脂的制备方法，其特征在于：包括如下步骤：
1)向反应釜中加入5％-45％的异氰酸酯化合物、30％-80％的多羟基化合物、控温80-90℃，常压下反应5h，得到多元醇与异氰酸酯的预聚体；
2)向步骤1)预聚体中再加入加入0.5％-15％的离子或潜力型亲水化合物、0.5％-10％的含有羟基或氨基的低分子量化合物，控温80-100℃，常压下反应2h；待体系NCO含量达到理论值后，降温至40-70℃，加入适量溶剂丙酮和二甲基乙醇胺反应45分钟，在高速搅拌的条件下加入去离子水，乳化45分钟后加入乙二胺和二乙烯三胺，控温30-50℃，常压下反应2h，加入适量消泡剂在一定条件下抽除溶剂丙酮，反应得到水性聚氨酯乳液；
3)向步骤2)水性聚氨酯乳液中最后加入增稠剂、润湿流平剂，常温搅拌1h，制得耐增塑剂单组份水性聚氨酯。
8.根据权利要求7所述的耐增塑剂单组份水性聚氨酯树脂的制备方法，其特征在于：步骤3)中，所述的润湿流平剂为改性聚硅氧烷或聚醚改性聚二甲基硅氧烷；增稠剂为缔合型水性聚氨酯。
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