CN108691213B - 一种偏蓝相干法聚氨酯合成革的制备工艺 - Google Patents

一种偏蓝相干法聚氨酯合成革的制备工艺 Download PDF

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CN108691213B
CN108691213B CN201810566518.XA CN201810566518A CN108691213B CN 108691213 B CN108691213 B CN 108691213B CN 201810566518 A CN201810566518 A CN 201810566518A CN 108691213 B CN108691213 B CN 108691213B
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舒适
徐洁
王元有
金党琴
毛云飞
陈锁金
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Yangzhou Polytechnic Institute
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Abstract

本发明涉及一种偏蓝相干法聚氨酯合成革的制备工艺，具体包括如下步骤：取本发明上述PU树脂、炭黑、DMF、BYK‑130分散剂，在高速搅拌下分散20‑30分钟后，再进行离心脱泡1‑3分钟，静置1‑1.5小时后得料浆，并将料浆刮涂于离型纸上，于110℃烘箱中烘干即得黑色面层，用粘结剂将黑色面层树脂与基布贴合，通过滚轮压合再烘干，然后从离型纸上剥离，即可制得偏蓝相聚氨酯合成革成品。

Description

一种偏蓝相干法聚氨酯合成革的制备工艺
技术领域
本发明属于聚氨酯合成革领域，具体涉及一种偏蓝相干法聚氨酯合成革的制备工艺。
背景技术
随着环境保护观念的日益加深、动物保护主义观念的广泛流行，当今的皮革工业面临着严峻的挑战，但这为合成革工业的发展提供了良好的契机。由于聚氨酯合成革(PU革)具有优异的耐磨性、可着色性、价格低廉、容易保养及低温柔韧性，被广泛应用于服装、运动鞋、箱包、汽车坐椅及体育器材中。与真皮相比PU革存在着展色性差的缺点，这限制了其在高质量产品中的应用。PU革中，干法树脂作为PU的面层树脂，它的展色性能对合成革产品质量具有决定性作用。干法PU树脂主要由如下几部分组成：即异氰酸酯、聚酯多元醇、扩链剂及溶剂等，其中的组成或者比例不同，均会对干法PU的展色性能产生重要的影响。本发明提供一种以邻苯二甲酸缩二乙二醇酯作为扩链剂制备PU树脂，并进一步制备展色性良好的偏蓝相PU合成革，其拉伸强度、耐磨性及透气性能优良。
发明内容
本发明提供一种PU树脂，其特征在于所述PU树脂的制备方法包括如下步骤：
(1)聚酯多元醇的制备：
将己二酸与乙二醇、1,4-丁二醇混匀，加入催化量的钛酸四异丙酯，并升温至200-210℃，反应10小时得到聚酯多元醇；
(2)PU树脂的制备：
以DMF为溶剂，加入步骤(1)制备的聚酯多元醇与扩链剂搅拌20分钟后，加入4,4-二苯基甲烷二异氰酸酯(MDI)升温至70-75℃，反应至粘度为20万时出料，即得PU树脂。
步骤(1)中已二酸、乙二醇、1,4-丁二醇的摩尔比为2:1:1；
步骤(2)中聚酯多元醇、扩链剂、4,4-二苯基甲烷二异氰酸酯的质量比为10:2.5:1，所述扩链剂选自式A、式B、式C所示结构的邻苯二甲酸二乙二醇酯中的一种或几种，式A、式B、式C所示结构如下：
Figure BDA0001682986480000021
其中扩链剂优选式A、式B、式C以质量比1:1:0.5的组合。
本发明提供一种偏蓝相聚氨酯合成革，所述偏蓝相聚氨酯合成革的制备方法包括如下步骤：
取本发明上述PU树脂、炭黑、DMF、BYK-130分散剂，在高速搅拌下分散20-30分钟后，再进行离心脱泡1-3分钟，静置1-1.5小时后得料浆，并将料浆刮涂于离型纸上，于110℃烘箱中烘干即得黑色面层，用粘结剂将黑色面层树脂与基布贴合，通过滚轮压合再烘干，然后从离型纸上剥离，即可制得偏蓝相聚氨酯合成革成品。所述高速搅拌速度为1000-1200转/分钟；料浆的刮涂厚度为0.2-0.3mm；以重量份计，每100份PU树脂、使用5份炭黑、80份DMF、3份BYK-130分散剂。所述粘结剂优选UNKPU-350A或UNKPU-380贴布胶。
本发明的另一实施方案提供上述PU树脂的制备方法，其特征在于包括如下步骤：
(1)聚酯多元醇的制备：
将己二酸与乙二醇、1,4-丁二醇混匀，加入催化量的钛酸四异丙酯，并升温至200-210℃，反应10小时得到聚酯多元醇；
(2)PU树脂的制备：
以DMF为溶剂，加入步骤(1)制备的聚酯多元醇与扩链剂搅拌20分钟后，加入4,4-二苯基甲烷二异氰酸酯(MDI)升温至70-75℃，反应至粘度为20万时出料，即得PU树脂。
步骤(1)中已二酸、乙二醇、1,4-丁二醇的摩尔比为2:1:1；
步骤(2)中聚酯多元醇、扩链剂、4,4-二苯基甲烷二异氰酸酯的质量比为10:2.5:1，所述扩链剂选自式A、式B、式C所示结构的邻苯二甲酸二乙二醇酯中的一种或几种，式A、式B、式C所示结构如下：
Figure BDA0001682986480000031
其中扩链剂优选式A、式B、式C以质量比1:1:0.5的组合。
本发明提供上述偏蓝相聚氨酯合成革的制备方法，其特征在于包括如下步骤：
取本发明上述PU树脂、炭黑、DMF、BYK-130分散剂，在高速搅拌下分散20-30分钟后，再进行离心脱泡1-3分钟，静置1-1.5小时后得料浆，并将料浆刮涂于离型纸上，于110℃烘箱中烘干即得黑色面层，用粘结剂将黑色面层树脂与基布贴合，通过滚轮压合再烘干，然后从离型纸上剥离，即可制得偏蓝相聚氨酯合成革成品。所述高速搅拌速度为1000-1200转/分钟；料浆的刮涂厚度为0.2-0.3mm；以重量份计，每100份PU树脂、使用5份炭黑、80份DMF、3份BYK-130分散剂。所述粘结剂优选UNKPU-350A或UNKPU-380贴布胶。
本发明的另一实施方案提供上述PU树脂在制备聚氨酯合成革中的应用。
与现有技术相比，本发明的优点在于本发明通过使用分子量较大的邻苯二甲酸二乙二醇酯式A、式B、式C的组合作为扩链剂，制备得到的PU树脂硬段与软段比例恰当，具有良好的展色性，制备得到偏蓝相聚氨酯合成革；该偏蓝相聚氨酯合成革拉伸强度大、耐磨性与透气性良好。
具体实施方式
为了便于对本发明的进一步理解，下面提供的实施例对其做了更详细的说明。但是这些实施例仅供更好的理解发明而并非用来限定本发明的范围或实施原则，本发明的实施方式不限于以下内容。
实施例1
(1)聚酯多元醇的制备：
将己二酸(2mol)与乙二醇(1mol)、1,4-丁二醇(1mol)混匀，加入催化量的钛酸四异丙酯，并升温至200-210℃，反应10小时得到聚酯多元醇；
(2)PU树脂的制备：
以DMF为溶剂，加入步骤(1)制备的聚酯多元醇(100g)与扩链剂(25g，式A:式B：式C＝1:1:0.5)，搅拌20分钟后，加入4,4-二苯基甲烷二异氰酸酯(10g)升温至70-75℃，反应至粘度为20万时出料，即得PU树脂(以下简称产品A)。
实施例2
PU树脂的制备：
以DMF为溶剂(与实施例1用量相同)，加入实施例1步骤(1)制备的聚酯多元醇(100g)与式A(25g)，搅拌20分钟后，加入4,4-二苯基甲烷二异氰酸酯(10g)升温至70-75℃，反应至粘度为20万时出料，即得PU树脂(以下简称产品B)。
以DMF为溶剂(与实施例1用量相同)，加入实施例1步骤(1)制备的聚酯多元醇(100g)与式B(25g)，搅拌20分钟后，加入4,4-二苯基甲烷二异氰酸酯(10g)升温至70-75℃，反应至粘度为20万时出料，即得PU树脂(以下简称产品C)。
以DMF为溶剂(与实施例1用量相同)，加入实施例1步骤(1)制备的聚酯多元醇(100g)与式C(25g)，搅拌20分钟后，加入4,4-二苯基甲烷二异氰酸酯(10g)升温至70-75℃，反应至粘度为20万时出料，即得PU树脂(以下简称产品D)。
以DMF为溶剂(与实施例1用量相同)，加入实施例1步骤(1)制备的聚酯多元醇(100g)与乙二醇(25g)，搅拌20分钟后，加入4,4-二苯基甲烷二异氰酸酯(10g)升温至70-75℃，反应至粘度为20万时出料，即得PU树脂(以下简称产品E)。
以DMF为溶剂，加入步骤(1)制备的聚酯多元醇(100g)与扩链剂(25g，式A:式B：式C＝0.5:1:1)，搅拌20分钟后，加入4,4-二苯基甲烷二异氰酸酯(10g)升温至70-75℃，反应至粘度为20万时出料，即得PU树脂(以下简称产品F)。
实施例3
取产品A(100g)、炭黑(5g)、DMF(80g)、BYK-130分散剂(3g)，在高速搅拌(1200转/分钟)下分散20分钟后，再进行离心脱泡1分钟，静置1小时后得料浆，并将料浆刮涂于离型纸上(料浆的刮涂厚度为0.2mm)，于110℃烘箱中烘干即得黑色面层，用UNKPU-380贴布胶将黑色面层树脂与无纺布基布贴合，通过滚轮压合再烘干，然后从离型纸上剥离，即可制得偏蓝相聚氨酯合成革成品(以下简称产品a)。
实施例4
取产品A(100g)、炭黑(5g)、DMF(80g)、BYK-130分散剂(3g)，在高速搅拌(1000转/分钟)下分散30分钟后，再进行离心脱泡3分钟，静置1.5小时后得料浆，并将料浆刮涂于离型纸上(料浆的刮涂厚度为0.3mm)，于110℃烘箱中烘干即得黑色面层，用UNKPU-350A贴布胶将黑色面层树脂与无纺布基布贴合，通过滚轮压合再烘干，然后从离型纸上剥离，即可制得偏蓝相聚氨酯合成革成品(以下简称产品a-1)。
实施例5
分别以产品B、C、D、E、F替换产品A，按照实施例3中的操作分别得到相应的合成革b、c、d、e、f。
实施例6产品a-f性能测试
按照QB/T4194-2011、GB/T 4689.2-1984规定的测试产品a-f的拉伸强度、耐磨性、透气性。
Figure BDA0001682986480000051

Claims (7)

1.一种PU树脂，其特征在于所述PU树脂的制备方法包括如下步骤：
(1)聚酯多元醇的制备：
将己二酸与乙二醇、1,4-丁二醇混匀，加入催化量的钛酸四异丙酯，并升温至200-210℃，反应10小时得到聚酯多元醇；
(2)PU树脂的制备：
以DMF为溶剂，加入步骤(1)制备的聚酯多元醇与扩链剂搅拌20分钟后，加入4,4-二苯基甲烷二异氰酸酯(MDI)升温至70-75℃，反应至粘度为20万时出料，即得PU树脂；步骤(1)中已二酸、乙二醇、1,4-丁二醇的摩尔比为2:1:1；
所述步骤(2)中聚酯多元醇、扩链剂、4,4-二苯基甲烷二异氰酸酯的质量比为10:2.5:1，所述扩链剂选自式A、式B、式C所示结构的邻苯二甲酸二乙二醇酯中的一种或几种，式A、式B、式C所示结构如下：
Figure DEST_PATH_IMAGE001
。
2.权利要求1所述的PU树脂，其特征在于所述扩链剂优选式A、式B、式C以质量比1:1:0.5的组合。
3.一种偏蓝相聚氨酯合成革，其特征在于所述偏蓝相聚氨酯合成革的制备方法包括如下步骤：
取权利要求1-2任一项所述的PU树脂、炭黑、DMF、BYK-130分散剂，在高速搅拌下分散20-30分钟后，再进行离心脱泡1-3分钟，静置1-1.5小时后得料浆，并将料浆刮涂于离型纸上，于110℃烘箱中烘干即得黑色面层，用粘结剂将黑色面层树脂与基布贴合，通过滚轮压合再烘干，然后从离型纸上剥离，即可制得偏蓝相聚氨酯合成革成品。
4.权利要求3所述的偏蓝相聚氨酯合成革，其特征在于所述高速搅拌速度为1000-1200转/分钟。
5.权利要求3-4任一项所述的偏蓝相聚氨酯合成革，其特征在于料浆的刮涂厚度为0.2-0.3mm。
6.权利要求5所述的偏蓝相聚氨酯合成革，其特征在于以重量份计，每100份PU树脂、使用5份炭黑、80份DMF、3份BYK-130分散剂。
7.权利要求6所述的偏蓝相聚氨酯合成革，其特征在于所述粘结剂优选UNKPU-350A或UNKPU-380贴布胶。
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