CN105330815B - 高回弹高绒感服装革用聚氨酯牛巴树脂及制备方法 - Google Patents

高回弹高绒感服装革用聚氨酯牛巴树脂及制备方法 Download PDF

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CN105330815B
CN105330815B CN201510778203.8A CN201510778203A CN105330815B CN 105330815 B CN105330815 B CN 105330815B CN 201510778203 A CN201510778203 A CN 201510778203A CN 105330815 B CN105330815 B CN 105330815B
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杨信实
彭峰
于吉鹏
郝智平
张初银
俞杰
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ZHEJIANG HUAFENG SYNTHETIC RESIN CO Ltd
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Abstract

本发明提供了一种高回弹高绒感服装革用聚氨酯牛巴树脂及制备方法，高回弹高绒感服装革用聚氨酯牛巴树脂，是采用包括如下重量百分比的组分制备的：异氰酸酯4.0％～12％，混合聚多元醇16％～22％，扩链剂1.0％～2.5％，N,N‑二甲基甲酰胺65％～80％，助剂0.1％～0.5％，聚氧化丙烯二醇(PPG)1.0％～2.0％，甲醇0.05％～0.5％。本发明运用聚己二酸丁二醇‑一缩二乙二醇酯二醇、聚碳酸酯二醇、双端羟基聚醚改性硅油和二异氰酸酯等反应物及两种中间体单独链增长方式合成工艺制得的树脂用于聚氨酯牛巴革，制得的牛巴革具有回弹性高、泡孔细竖均匀、绒感强、耐候性好等优点。

Description

高回弹高绒感服装革用聚氨酯牛巴树脂及制备方法
技术领域
本发明涉及聚氨酯牛巴树脂及制备方法。
背景技术
聚氨酯合成革具有力学性能优良、质地柔软、外观漂亮等优点，既有仿天然革结构，又有天然真皮的手感，是真皮的最佳代用品，在鞋、箱包、服装、家具等领域有相当广泛的应用，尤其在服装领域。用聚氨酯树脂制成的服装革由于具有手感柔软细腻、透湿透气性好、穿着舒适、耐折耐磨等优点，深受市场的欢迎，在皮革类服装中占据了半壁江山。特别是用聚氨酯牛巴树脂制成的服装革经磨砂后具有其它产品所无法比拟的手感，细腻柔软绒感强，因此也深受消费者的喜爱。但近几年随着生活水平的提高，人民对消费的要求越来越高，国内的聚氨酯牛巴树脂渐渐暴露出弹性差、绒感不够的问题，极大限制了其在服装领域的应用。
发明内容
本发明所要解决的技术问题是克服现有技术的不足，提供一种高回弹高绒感服装革用聚氨酯牛巴树脂及制备方法。
所述高回弹高绒感服装革用聚氨酯牛巴树脂，是采用包括如下重量百分比的组分制备的：
各个组分的百分比之和为100％。
优选的，所述高回弹高绒感服装革用聚氨酯牛巴树脂，是采用包括如下重量百分比的组分制备的：
各个组分的百分比之和为100％。
所述的二异氰酸酯为4,4-二苯基甲烷二异氰酸酯；
所述混合聚多元醇为聚己二酸丁二醇-一缩二乙二醇酯二醇、聚碳酸酯二醇(PCD)和双端羟基聚醚改性硅油的混合物，重量百分比如下：
聚己二酸丁二醇-一缩二乙二醇酯二醇 50％～78％
聚碳酸酯二醇(PCD) 18％～42％
双端羟基聚醚改性硅油 4％～8％；
所述聚己二酸丁二醇-一缩二乙二醇酯二醇数均分子量为2000～4000，所述聚碳酸酯二醇数均分子量为2000～3000，所述双端羟基聚醚改性硅油数均分子量为4000；
所述的扩链剂为乙二醇或1，4-丁二醇；
所述的助剂为展色助剂，如不饱和多元羧酸的多元胺酰胺溶液，可采用商业化产品，如毅克化学科技有限公司牌号YCK-2560的产品；
所述高回弹高绒感服装革用聚氨酯牛巴树脂的制备方法，包括如下步骤：
1)预聚反应：将聚己二酸丁二醇-一缩二乙二醇酯二醇、部分扩链剂、二甲基甲酰胺和部分4,4-二苯基甲烷二异氰酸酯加入反应釜中进行预聚反应，控制反应液中异氰酸酯基和羟基的摩尔比为1～1.09:1，固含量控制在60％，并在70℃～80℃下反应2.0～3.0h，测反应液粘度达到(60～80)Pa·s/70℃，预聚反应结束；
所述的部分扩链剂，指的是扩链剂总重量的35～45％；
所述的部分4,4-二苯基甲烷二异氰酸酯，指的是4,4-二苯基甲烷二异氰酸酯总重量的35～45％；
2)链增长反应：加入聚碳酸酯二醇(PCD)、双端羟基聚醚改性硅油、剩余扩链剂和剩余溶剂，反应20～40min后加入剩余4,4-二苯基甲烷二异氰酸酯进行链增长反应，测反应液粘度达到(200～280)Pa·s/25℃，加入甲醇封端，并加入展色剂和聚氧化丙烯二醇(PPG)，得到高回弹高绒感服装革用聚氨酯牛巴树脂。
本发明与现有技术相比，具有以下优点：
本发明运用聚己二酸丁二醇-一缩二乙二醇酯二醇、聚碳酸酯二醇、双端羟基聚醚改性硅油和二异氰酸酯等反应物及两种中间体单独链增长方式合成工艺制得的树脂用于聚氨酯牛巴革，制得的牛巴革具有回弹性高、泡孔细竖均匀、绒感强、耐候性好等优点。
具体实施方式
下面通过实施例对本发明进行具体的描述，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定。实施例中采用的实施条件可以根据具体厂家的条件和要求做一些非本质的改进和调整。
,实施例1
将聚己二酸丁二醇-一缩二乙二醇酯二醇900kg、1，4-丁二醇64kg、二甲基甲酰胺798.7kg和4,4-二苯基甲烷二异氰酸酯234kg加入反应釜中进行预聚反应，反应温度控制在70℃，反应3.0h后，取样测反应液粘度达到60Pa·s/70℃时加入聚碳酸酯二醇(PCD)756kg、双端羟基聚醚改性硅油144kg、1，4-丁二醇64kg和N,N-二甲基甲酰胺6401.3kg，反应40min后加入4,4-二苯基甲烷二异氰酸酯336kg进行链增长反应，测反应液粘度达到200Pa·s/25℃时加入甲醇30kg封端，同时加入展色剂40kg和聚氧化丙烯二醇(PPG)200kg，得到高回弹高绒感服装革用聚氨酯牛巴树脂。。
实施例2
将聚己二酸丁二醇-一缩二乙二醇酯二醇1560kg、乙二醇76kg、二甲基甲酰胺1425kg和4,4-二苯基甲烷二异氰酸酯501.5kg加入反应釜中进行预聚反应，反应温度控制在80℃，反应2.0h后，取样测反应液粘度达到80Pa·s/70℃时加入聚碳酸酯二醇(PCD)360kg、双端羟基聚醚改性硅油80kg、乙二醇114kg和N,N-二甲基甲酰胺5245kg，反应20min后加入4,4-二苯基甲烷二异氰酸酯508.5kg进行链增长反应，测反应液粘度达到280Pa·s/25℃时加入甲醇10kg封端，同时加入展色剂20kg和聚氧化丙烯二醇(PPG)100kg，得到高回弹高绒感服装革用聚氨酯牛巴树脂。
实施例3
将聚己二酸丁二醇-一缩二乙二醇酯二醇1200kg、乙二醇68kg、二甲基甲酰胺1078.1kg和4,4-二苯基甲烷二异氰酸酯349.2kg加入反应釜中进行预聚反应，反应温度控制在70℃，反应3.0h后，取样测反应液粘度达到70Pa·s/70℃时加入聚碳酸酯二醇(PCD)720kg、双端羟基聚醚改性硅油80kg、乙二醇102kg和N,N-二甲基甲酰胺5706.9kg，反应30min后加入4,4-二苯基甲烷二异氰酸酯505.8kg进行链增长反应，测反应液粘度达到240Pa·s/25℃时加入甲醇10kg封端，同时加入展色剂30kg和聚氧化丙烯二醇(PPG)150kg，，得到高回弹高绒感服装革用聚氨酯牛巴树脂。
实施例4
将聚己二酸丁二醇-一缩二乙二醇酯二醇1400kg、乙二醇72kg、二甲基甲酰胺1233.2kg和4,4-二苯基甲烷二异氰酸酯377.8kg加入反应釜中进行预聚反应，反应温度控制在80℃，反应2.0h后，取样测反应液粘度达到70Pa·s/70℃时加入聚碳酸酯二醇(PCD)480kg、双端羟基聚醚改性硅油120kg、乙二醇108kg和N,N-二甲基甲酰胺5475.8kg，反应30min后加入4,4-二苯基甲烷二异氰酸酯483.2kg进行链增长反应，测反应液粘度达到260Pa·s/25℃时加入甲醇10kg封端，同时加入展色剂40kg和聚氧化丙烯二醇(PPG)200kg，得到高回弹高绒感服装革用聚氨酯牛巴树脂。
对比例1
将聚己二酸丁二醇酯二醇1000kg、聚己二酸乙二醇-丁二醇酯二醇1000kg、二甲基甲酰胺1472.2kg和4,4-二苯基甲烷二异氰酸酯208.3kg加入反应釜中进行预聚反应，反应温度控制在80℃，反应2.0h后，取样测反应液粘度达到60Pa·s/70℃时加入乙二醇180kg和N,N-二甲基甲酰胺5167.8kg，反应半小时后加入4,4-二苯基甲烷二异氰酸酯721.7kg进行链增长反应，测反应液粘度达到200Pa·s/25℃时加入甲醇10kg封端，同时加入展色剂40kg和聚氧化丙烯二醇(PPG)200kg，反应结束。
实施例1～4中所用双端羟基聚醚改性硅油为道康宁公司的型号为SF8427产品。
检测试验
现将实施例1～4和对比例1所制备的服装革用聚氨酯牛巴树脂进行检测试验，测量制备湿法base过程所需的凝固时间，观察湿法base的泡孔结构，测试湿法base的手感、回弹性，以及湿法base在恒温恒湿测试前后的剥离强度，以判断其耐候性。
实验步骤
(1)将上述实施例1-4及对比例1所制备的树脂与常规公知的泡孔调节剂、渗透剂按照一定比例稀释配成涂刮液；
(2)以1.4mm的刀距在处理好的弹力布上进行涂刮，涂刮完后进入凝固槽，测量凝固时间(以完全凝固为准)，凝固结束后水洗、烘干，得到湿法base；
(3)将上述制备所得湿法base放入恒温恒湿试验仪中在75℃×95％RH的条件下分别进行2周和3周的测试，并检测放入恒温恒湿试验仪前后湿法base的剥离强度。
实验结果
实施例1～4及对比例1所制备的聚氨酯湿法base的凝固时间、泡孔结构、手感、回弹性等性能对比如表1所示；75℃×95％RH恒温恒湿试验2周和3周前后剥离强度对比如表2所示。
表1
表2
从表1中可知，实施例1～4所制湿法base整体凝固速度快，泡孔细竖分布均匀，绒感强，还略带滑感，弹性好，指压后恢复快，各方性能均较对比例1所制湿法base要好。
从表2中可知，实施例1～4所制湿法base，经2周恒温恒湿试验后，剥离强度衰减不超过5％，经3周恒温恒湿试验后，剥离强度衰减不超过10％，而对比例1所制湿法base，经2周恒温恒湿试验后，剥离强度衰减已超过35％，经3周恒温恒湿试验后，剥离强度衰减已接近90％。综上可知，本发明制备的服装革用聚氨酯牛巴树脂绒感强，弹性好，而且耐侯性好，弥补了传统服装革用聚氨酯牛巴树脂的不足。
以上对本发明做了详尽的描述，其目的在于让熟悉此领域技术的人士能够了解本发明的内容并加以实施，并不能以此限制本发明的保护范围，凡根据本发明的精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围内。

Claims (6)

1.高回弹高绒感服装革用聚氨酯牛巴树脂，其特征在于，是采用包括如下重量百分比的组分制备的：
所述混合聚多元醇为聚己二酸丁二醇-一缩二乙二醇酯二醇、聚碳酸酯二醇(PCD)和双端羟基聚醚改性硅油的混合物；
所述混合聚多元醇各个组分的重量百分比如下：
聚己二酸丁二醇-一缩二乙二醇酯二醇 50％～78％
聚碳酸酯二醇(PCD) 18％～42％
双端羟基聚醚改性硅油 4％～8％。
所述聚己二酸丁二醇-一缩二乙二醇酯二醇数均分子量为2000～4000，所述聚碳酸酯二醇数均分子量为2000～3000，所述双端羟基聚醚改性硅油数均分子量为4000。
2.根据权利要求1所述的高回弹高绒感服装革用聚氨酯牛巴树脂，其特征在于，是采用包括如下重量百分比的组分制备的：
3.根据权利要求1所述的高回弹高绒感服装革用聚氨酯牛巴树脂，其特征在于，所述的二异氰酸酯为4,4-二苯基甲烷二异氰酸酯。
4.根据权利要求1所述的高回弹高绒感服装革用聚氨酯牛巴树脂，其特征在于，所述的扩链剂为乙二醇或1，4-丁二醇。
5.根据权利要求1所述的高回弹高绒感服装革用聚氨酯牛巴树脂，其特征在于，所述的助剂为展色助剂。
6.根据权利要求1～5任一项所述的高回弹高绒感服装革用聚氨酯牛巴树脂的制备方法，其特征在于，包括如下步骤：
1)预聚反应：将聚己二酸丁二醇-一缩二乙二醇酯二醇、部分扩链剂、二甲基甲酰胺和部分4,4-二苯基甲烷二异氰酸酯加入反应釜中进行预聚反应，控制反应液中异氰酸酯基和羟基的摩尔比为1～1.09:1，固含量控制在60％，并在70℃～80℃下反应2.0～3.0h，测反应液粘度达到(60～80)Pa·s/70℃，预聚反应结束；
所述的部分扩链剂，指的是扩链剂总重量的35～45％；
所述的部分4,4-二苯基甲烷二异氰酸酯，指的是4,4-二苯基甲烷二异氰酸酯总重量的35～45％；
2)链增长反应：加入聚碳酸酯二醇(PCD)、双端羟基聚醚改性硅油、剩余扩链剂和剩余溶剂，反应20～40min后加入剩余4,4-二苯基甲烷二异氰酸酯进行链增长反应，测反应液粘度达到(200～280)Pa·s/25℃，加入甲醇封端，并加入展色剂和聚氧化丙烯二醇(PPG)，得到高回弹高绒感服装革用聚氨酯牛巴树脂。
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