CN106521986A - 一种水性双面绒面超纤pu合成革及其制备方法 - Google Patents

一种水性双面绒面超纤pu合成革及其制备方法 Download PDF

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CN106521986A
CN106521986A CN201611096305.2A CN201611096305A CN106521986A CN 106521986 A CN106521986 A CN 106521986A CN 201611096305 A CN201611096305 A CN 201611096305A CN 106521986 A CN106521986 A CN 106521986A
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aqueous
mass parts
water
woven fabric
finished product
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CN106521986B (zh
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李桂军
向以俊
杨运波
张锋
王桦
卢海峰
倪伶俐
高晓燕
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Jiangsu Huayuan High Tech Co.,Ltd.
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Abstract

本发明公开了一种水性双面绒面超纤PU合成革及其制备方法，所述水性双面绒面超纤PU合成革以定岛超纤无纺布为基布，以水性PU浆料为含浸浆料，经过含浸、轧出、干燥、碱减量、再烘干、染色、双面水磨、再烘干工艺制得。发明不仅工艺简单、生产流程短、能耗低、生产效率高，且生产过程完全没有使用有机溶剂，安全环保。所制备的水性绒面PU超纤合成革产品不仅质优价廉，生产过程安全环保，而且经检测各项指标皆基本达到国外产品标准。

Description

一种水性双面绒面超纤PU合成革及其制备方法
技术领域
本发明涉及合成革制造领域，具体涉及一种水性双面绒面超纤PU合成革及其制备方法。
背景技术
合成革行业已有几十年的发展历史，随着各种新材料的不断出现，其产品也在不断更新。革用基布从机织到非织造布，所用树脂从聚氯乙烯，丙烯酸树脂到聚氨酯，底布基材纤维也已发展到超细纤维等。在产品风格上，人造革经历了从低档到高档，从仿真皮到超载真皮的发展过程，其部分特性已经实现了超越天然皮革。目前聚氨酯(PU)合成革的加工技术已相当成熟，而且人们仍在不断地开发运用新技术、新工艺、新材料来持续提高产品的性能和价值。
超纤皮革与真皮结构极为相似，均为束状超细纤维三维立体结构。超细纤维合成皮革是在充分剖析天然皮革的基础上发展起来的。超细纤维合成革是由束状超细纤维与聚氨酯经过特殊工艺加工而成。它是采用与天然皮革中束状胶原纤维结构和性能相似的尼龙超细纤维，制成具有三维网络结构的非织造布，再填充性能优异具有开式微孔结构的聚氨酯经后处理工艺通过含浸、减量抽出，整染、磨皮、揉制形成可用于后加工的超纤贝斯。
由于超纤皮革不仅外在表观和内在结构上都具有真皮的特性，而且又有工业化生产和加工方便，使得超纤皮革产品的物理性能达到甚至超越真皮革。其在防霉、防蛀、拉伸强度、撕裂强度、透气性等方面都优于普通PU革而接近甚至超过天然皮革，同时其产品的厚薄均匀性、撕裂强度、色彩鲜艳度及革面利用率等方面明显优于天然皮革，被广大消费者予以广泛应用，特别在制鞋、箱包、服装、家具、家居装饰、汽车内饰等领域，因此超纤皮革已经成为当代合成革的发展方向。
但是，我国目前的超纤皮革制备却由于技术受限、原料依赖进口等方面的困扰，发展相当缓慢，而纯水性、生态环保的超纤皮革更是少之又少，常规工艺大多是先在离型纸上涂敷面层、粘结层，再与超纤基布贴合等（如果需要双面花纹，还需要重复上述工艺），不仅工艺繁琐，而且成本特高。因此目前市场上主要的水性生态超纤PU皮革产品主要还是依赖进口。
发明内容
为了解决上述现有技术的缺陷，本发明的目的在于提供一种水性双面绒面超纤PU合成革及其制备方法，以克服目前超纤PU合成革的现有加工工艺复杂、成本高、主要依赖进口等问题。
本发明是通过以下技术方案实现的：
一种水性双面绒面超纤PU合成革，以定岛超纤无纺布为基布，以水性PU浆料为含浸浆料，经过含浸、轧出、干燥、碱减量、再烘干、染色、双面水磨、再烘干工艺制得。
具体包括如下步骤：
步骤一：制备含浸水性PU浆料
称取水性PU树脂60-80质量份，水溶性粉8-20质量份，水性增稠剂0.2-0.6质量份，有机硅手感剂0.5-1质量份，有机硅柔软剂1-5质量份，填料10-20质量份，水性消泡剂0.2-0.6质量份混合制备成乳白色均一粘稠液体待用；
步骤二：定岛超纤无纺布含浸
将步骤一制备的含浸浆料加入含浸槽中，将定岛超纤无纺布以300-600m/h的速度匀速经过含浸槽，使其充分浸润水性PU浆料；
步骤三：轧出
将浸透了水性PU浆料的超纤基布通过一对轧辊，挤出其中的部分浸渍液，通过调整轧辊间隙为基布厚度的三分之二，保证基布中含浸水性PU浆料的质量为基布质量的60%-120%；
步骤四：烘箱烘干
经挤压好的含有含浸水性PU浆料的基布以300-600m/h的速度进入温度为100-150℃的烘箱进行干燥固化得半成品一；
步骤五：碱减量
将半成品一在碱减量机中进行碱减量处理，其中碱为氢氧化钠，浓度为3-5%，水温为90℃，时间为30-50分钟；
步骤六：水洗及烘干
经碱减量好的半成品一用清水清洗后，再用20%的柠檬酸溶液常温浸泡20分钟进行中和，再用清水洗至PH为7后进入温度为100-150℃的烘箱进行干燥得半成品二；
步骤七：染色
将半成品二放入染色机，加入重量份300%-1000%的水，2%-6%的强酸性染料，1%-3%的弱酸性染料，在90-95℃的温度下染色60-120分钟，染色后进行水洗得半成品三；
步骤八：双面水磨
利用通过式磨革机对半成品三进行双面水磨1-3遍，再用毛刷辊起绒机进行双面起绒；
步骤九：烘干定型
经双面水磨的半成品以300-600m/h的速度进入温度为100-150℃的烘箱进行干燥并定型后即得成品水性双面绒面超纤PU合成革。
本发明的进一步改进方案为：
所述水性PU树脂的制备方法包括如下步骤：
步骤1：制备羟基聚醚封端的烷基聚硅氧烷中间体
取丙烯醇聚氧乙烯醚、双硅氢基封端的甲基长链烷基聚二甲基硅氧烷和铂金speier催化剂置入反应釜中搅拌升温至80～160℃反应3～5h, 得羟基聚醚封端的长链烷聚硅氧烷中间体；丙烯醇聚氧乙烯醚和双硅氢基封端的甲基长链烷基聚二甲基硅氧烷物质的量的比为1:0.5，铂金speier催化剂投料量占体系总质量的10-20ppm；
步骤2：制备长链烷基聚硅氧烷改性水性PU树脂预聚体
取150质量份的羟基聚醚封端的长链烷聚硅氧烷中间体、290质量份的PTMG2000、120质量份的TDI、10质量份的乙二醇、50质量份的二羟甲基丙酸（DMPA）和0.4质量份有机铋催化剂, 80～90℃下反应至预聚体粘度增为8000～10000mPa.S时,添加50质量份的丙酮，80～90℃下保持丙酮回流反应3小时,冷却到50℃以下，加入38质量份的三乙胺进行中和反应0.5-1小时，得长链烷基聚硅氧烷改性水性PU树脂预聚体；
步骤3：长链烷基聚硅氧烷改性水性PU树脂扩链反应
将500长链烷基聚硅氧烷改性水性PU树脂预聚体流加入搅拌速度为1000～1500转/分的1300质量份的纯水中，加入10质量份的扩链剂，进行扩链反应4-6小时，得长链烷基聚硅氧烷改性水性PU树脂；所述扩链剂为乙二胺或联肼；
步骤4：脱除丙酮
长链烷基聚硅氧烷改性水性PU树脂在50～60℃、10～30KPa下减压蒸馏脱除丙酮，添加纯水使得到的长链烷基聚硅氧烷改性水性PU树脂固含量为30-35%。
本发明的更进一步改进方案为：
所述水性PU树脂的制备方法步骤1中丙烯醇聚氧乙烯醚的分子式为CH2=CH-CH2O(C2H4O)nH，其中n为8-12的整数；
双硅氢基封端的甲基长链烷基聚二甲基硅氧烷的分子式为H-Si（CH3）2-O-[ Si（CH3）2]a-[ Si（CH3）（CmH2m+1）O]b-（CH3）2 Si-H，其中m为10-20的整数，a为5-20的整数，b为5-10的整数；
羟基聚醚封端的长链烷聚硅氧烷中间体的分子式为H(OH4C2)nOH6C3-Si（CH3）2-O-[ Si（CH3）2]a-[ Si（CH3）（CmH2m+1）O]b-（CH3）2 Si- C3 H6O(C2 H4O)nH，其中m为10-20的整数，n为8-12的整数，a为5-20的整数，b为5-10的整数。
本发明再进一步改进方案为：
所述水溶性粉包括醇解度为85-100的聚乙烯醇细粉，有机硅手感剂为超高分子量聚二甲基硅油乳液，有机硅柔软剂为非离子氨基硅油乳液，填料为凹凸棒土、高岭土微粉中的一种，水性消泡剂为有机硅消泡剂
本发明的有益效果为：
1.本发明制备含浸浆料的原料中用水溶性粉代替传统的起泡剂，水溶性粉在经过步骤五碱减量和步骤六的水洗和烘干会被洗去，在产品内部留下大小均一、分布均匀的小气孔，使材料富有良好的弹性。
2. 本发明制备含浸浆料时采用水性添加剂，减少了有机物质的残留，制备出更加纯净的水性的PU合成革；且整个制备过程中没有使用有机溶剂，生产过程安全环保。
3.本发明工艺简单、生产流程短、能耗低、生产效率高，所制备的水性绒面PU超纤合成革产品质优价廉，生产过程安全环保，而且经检测各项指标皆基本达到国外产品标准。
具体实施方式
实施例1
水性PU树脂的制备
步骤1：制备羟基聚醚封端的烷基聚硅氧烷中间体
在2000ml四口玻璃反应釜中，加入1mol分子式为CH2=CH-CH2O(C2H4O)nH的丙烯醇聚氧乙烯醚，其中n为8-12的整数，0.5mol分子式为H-Si（CH3）2-O-[ Si（CH3）2]a-[ Si（CH3）（CmH2m+1）O]b-（CH3）2 Si-H 的双硅氢基封端的甲基长链烷基聚二甲基硅氧烷，其中m为10-20的整数，a为5-20的整数，b为5-10的整数，开动搅拌并加入占体系总质量的10-20ppm的铂金speier催化剂搅拌升温至80～160℃反应3～5h,得分子式为H(OH4C2)nOH6C3-Si（CH3）2-O-[Si（CH3）2]a-[ Si（CH3）（CmH2m+1）O]b-（CH3）2 Si- C3 H6O(C2 H4O)nH的羟基聚醚封端的长链烷聚硅氧烷中间体，其中m为10-20的整数，n为8-12的整数，a为5-20的整数，b为5-10的整数。
步骤2：制备长链烷基聚硅氧烷改性水性聚氨酯树脂预聚体
在装有搅拌器、温度计、回流冷凝器的500ml玻璃聚合反应瓶中加入150质量份上述步骤1的羟基聚醚封端的长链烷聚硅氧烷中间体,290质量份的PTMG2000, 120质量份的TDI,10质量份的乙二醇, 50质量份的二羟甲基丙酸（DMPA）,0.4质量份有机铋催化剂,常温混合搅拌均匀，逐步加热升温到80～90℃，随着反应的进行粘度逐步增加，预聚体粘度增至8000～10000mPa.S时,添加50g丙酮，保持丙酮回流温度反应3小时,取样检测异氰酸根含量合格后停止加热,将反应体系冷却到50℃以下，加入38g三乙胺进行中和反应0.5-1小时，得长链烷基聚硅氧烷改性水性聚氨酯树脂预聚体。
步骤3：长链烷基聚硅氧烷改性水性聚氨酯树脂扩链反应
将上述步骤2的长链烷基聚硅氧烷改性水性聚氨酯树脂预聚体，缓慢流加入高速搅拌（1000～1500转/分）下的1300质量份的纯水中，然后加入10质量份的乙二胺或联肼等后扩链剂，进行扩链反应4-6小时。
步骤4：脱除丙酮
在具有冷凝回收装置的2000ml减压蒸馏釜中，加入1500g上述步骤4制备的长链烷基聚硅氧烷改性水性聚氨酯树脂,加热至50～60℃后在真空度10～30KPa下减压蒸馏脱除丙酮，并适当补充纯水，即得固体份为30-35%的长链烷基聚硅氧烷改性水性聚氨酯树脂。
实施例2
步骤一：制备含浸水性PU浆料
称取水性PU树脂60质量份，水溶性粉20质量份，水性增稠剂0.2质量份，有机硅手感剂1质量份，有机硅柔软剂1质量份，填料20质量份，水性消泡剂0.2质量份混合制备成乳白色均一粘稠液体待用；
步骤二：定岛超纤无纺布含浸
将步骤一制备的含浸浆料加入含浸槽中，将定岛超纤无纺布以300m/h的速度匀速经过含浸槽，使其充分浸润水性PU浆料；
步骤三：轧出
将浸透了水性PU浆料的超纤基布通过一对轧辊，挤出其中的部分浸渍液，通过调整轧辊间隙为基布厚度的三分之二，保证基布中含浸水性PU浆料的质量为基布质量的60%；
步骤四：烘箱烘干
经挤压好的含有含浸水性PU浆料的基布以300m/h的速度进入温度为100-150℃的烘箱进行干燥固化得半成品一；
步骤五：碱减量
将半成品一在碱减量机中进行碱减量处理，其中碱为氢氧化钠，浓度为3%，水温为90℃，时间为30分钟；
步骤六：水洗及烘干
经碱减量好的半成品一用清水清洗后，再用20%的柠檬酸溶液常温浸泡20分钟进行中和，再用清水洗至PH为7后进入温度为100-150℃的烘箱进行干燥得半成品二；
步骤七：染色
将半成品二放入染色机，加入重量份300%的水，2%-6%的强酸性染料，1%-3%的弱酸性染料，在90-95℃的温度下染色60分钟，染色后进行水洗得半成品三；
步骤八：双面水磨
利用通过式磨革机对半成品三进行双面水磨，再用毛刷辊起绒机进行双面起绒；
步骤九：烘干定型
经双面水磨的半成品以300m/h的速度进入温度为100-150℃的烘箱进行干燥并定型后即得成品水性双面绒面超纤PU合成革。
实施例3
步骤一：制备含浸水性PU浆料
称取水性PU树脂70质量份，水溶性粉15质量份，水性增稠剂0.6质量份，有机硅手感剂0.5质量份，有机硅柔软剂3质量份，填料10质量份，水性消泡剂0.6质量份混合制备成乳白色均一粘稠液体待用；
步骤二：定岛超纤无纺布含浸
将步骤一制备的含浸浆料加入含浸槽中，将定岛超纤无纺布以600m/h的速度匀速经过含浸槽，使其充分浸润水性PU浆料；
步骤三：轧出
将浸透了水性PU浆料的超纤基布通过一对轧辊，挤出其中的部分浸渍液，通过调整轧辊间隙为基布厚度的三分之二，保证基布中含浸水性PU浆料的质量为基布质量的90%；
步骤四：烘箱烘干
经挤压好的含有含浸水性PU浆料的基布以600m/h的速度进入温度为100-150℃的烘箱进行干燥固化得半成品一；
步骤五：碱减量
将半成品一在碱减量机中进行碱减量处理，其中碱为氢氧化钠，浓度为5%，水温为90℃，时间为45分钟；
步骤六：水洗及烘干
经碱减量好的半成品一用清水清洗后，再用20%的柠檬酸溶液常温浸泡20分钟进行中和，再用清水洗至PH为7后进入温度为100-150℃的烘箱进行干燥得半成品二；
步骤七：染色
将半成品二放入染色机，加入重量份600%的水，2%-6%的强酸性染料，1%-3%的弱酸性染料，在90-95℃的温度下染色60-120分钟，染色后进行水洗得半成品三；
步骤八：双面水磨
利用通过式磨革机对半成品三进行双面水磨，再用毛刷辊起绒机进行双面起绒；
步骤九：烘干定型
经双面水磨的半成品以600m/h的速度进入温度为100-150℃的烘箱进行干燥并定型后即得成品水性双面绒面超纤PU合成革。
实施例4
步骤一：制备含浸水性PU浆料
称取水性PU树脂80质量份，水溶性粉8质量份，水性增稠剂0.4质量份，有机硅手感剂0.7质量份，有机硅柔软剂5质量份，填料15质量份，水性消泡剂0.4质量份混合制备成乳白色均一粘稠液体待用；
步骤二：定岛超纤无纺布含浸
将步骤一制备的含浸浆料加入含浸槽中，将定岛超纤无纺布以450m/h的速度匀速经过含浸槽，使其充分浸润水性PU浆料；
步骤三：轧出
将浸透了水性PU浆料的超纤基布通过一对轧辊，挤出其中的部分浸渍液，通过调整轧辊间隙为基布厚度的三分之二，保证基布中含浸水性PU浆料的质量为基布质量的120%；
步骤四：烘箱烘干
经挤压好的含有含浸水性PU浆料的基布以450m/h的速度进入温度为100-150℃的烘箱进行干燥固化得半成品一；
步骤五：碱减量
将半成品一在碱减量机中进行碱减量处理，其中碱为氢氧化钠，浓度为4%，水温为90℃，时间为50分钟；
步骤六：水洗及烘干
经碱减量好的半成品一用清水清洗后，再用20%的柠檬酸溶液常温浸泡20分钟进行中和，再用清水洗至PH为7后进入温度为100-150℃的烘箱进行干燥得半成品二；
步骤七：染色
将半成品二放入染色机，加入重量份1000%的水，2%-6%的强酸性染料，1%-3%的弱酸性染料，在90-95℃的温度下染色60-120分钟，染色后进行水洗得半成品三；
步骤八：双面水磨
利用通过式磨革机对半成品三进行双面水磨，再用毛刷辊起绒机进行双面起绒；
步骤九：烘干定型
经双面水磨的半成品以450m/h的速度进入温度为100-150℃的烘箱进行干燥并定型后即得成品水性双面绒面超纤PU合成革。
下表是实施例1-3制得的水性双面绒面超纤PU合成革主要性能参数。

Claims (5)

1.一种水性双面绒面超纤PU合成革，其特征在于，以定岛超纤无纺布为基布，以水性PU浆料为含浸浆料，经过含浸、轧出、干燥、碱减量、再烘干、染色、双面水磨、再烘干工艺制得。
2.制备权利要求1所述一种水性双面绒面超纤PU合成革的方法，其特征在于包括如下步骤：
步骤一：制备含浸水性PU浆料
称取水性PU树脂60-80质量份，水溶性粉8-20质量份，水性增稠剂0.2-0.6质量份，有机硅手感剂0.5-1质量份，有机硅柔软剂1-5质量份，填料10-20质量份，水性消泡剂0.2-0.6质量份混合制备成乳白色均一粘稠液体待用；
步骤二：定岛超纤无纺布含浸
将步骤一制备的含浸浆料加入含浸槽中，将定岛超纤无纺布以300-600m/h的速度匀速经过含浸槽，使其充分浸润水性PU浆料；
步骤三：轧出
将浸透了水性PU浆料的超纤基布通过一对轧辊，挤出其中的部分浸渍液，通过调整轧辊间隙为基布厚度的三分之二，保证基布中含浸水性PU浆料的质量为基布质量的60%-120%；
步骤四：烘箱烘干
经挤压好的含有含浸水性PU浆料的基布以300-600m/h的速度进入温度为100-150℃的烘箱进行干燥固化得半成品一；
步骤五：碱减量
将半成品一在碱减量机中进行碱减量处理，其中碱为氢氧化钠，浓度为3-5%，水温为90℃，时间为30-50分钟；
步骤六：水洗及烘干
经碱减量好的半成品一用清水清洗后，再用20%的柠檬酸溶液常温浸泡20分钟进行中和，再用清水洗至PH为7后进入温度为100-150℃的烘箱进行干燥得半成品二；
步骤七：染色
将半成品二放入染色机，加入重量份300%-1000%的水，2%-6%的强酸性染料，1%-3%的弱酸性染料，在90-95℃的温度下染色60-120分钟，染色后进行水洗得半成品三；
步骤八：双面水磨
利用通过式磨革机对半成品三进行双面水磨1-3遍，再用毛刷辊起绒机进行双面起绒；
步骤九：烘干定型
经双面水磨的半成品以300-600m/h的速度进入温度为100-150℃的烘箱进行干燥并定型后即得成品水性双面绒面超纤PU合成革。
3.根据权利要求2所述的一种水性双面绒面超纤PU合成革的制备方法，其特征在于：所述水性PU树脂的制备方法包括如下步骤：
步骤1：制备羟基聚醚封端的烷基聚硅氧烷中间体
取丙烯醇聚氧乙烯醚、双硅氢基封端的甲基长链烷基聚二甲基硅氧烷和铂金speier催化剂置入反应釜中搅拌升温至80～160℃反应3～5h, 得羟基聚醚封端的长链烷聚硅氧烷中间体；丙烯醇聚氧乙烯醚和双硅氢基封端的甲基长链烷基聚二甲基硅氧烷物质的量的比为1:0.5，铂金speier催化剂投料量占体系总质量的10-20ppm；
步骤2：制备长链烷基聚硅氧烷改性水性PU树脂预聚体
取150质量份的羟基聚醚封端的长链烷聚硅氧烷中间体、290质量份的PTMG2000、120质量份的TDI、10质量份的乙二醇、50质量份的二羟甲基丙酸和0.4质量份有机铋催化剂, 80～90℃下反应至预聚体粘度增为8000～10000mPa.S时,添加50质量份的丙酮，80～90℃下保持丙酮回流反应3小时,冷却到50℃以下，加入38质量份的三乙胺进行中和反应0.5-1小时，得长链烷基聚硅氧烷改性水性PU树脂预聚体；
步骤3：长链烷基聚硅氧烷改性水性PU树脂扩链反应
将500长链烷基聚硅氧烷改性水性PU树脂预聚体流加入搅拌速度为1000～1500转/分的1300质量份的纯水中，加入10质量份的扩链剂，进行扩链反应4-6小时，得长链烷基聚硅氧烷改性水性PU树脂；所述扩链剂为乙二胺或联肼；
步骤4：脱除丙酮
长链烷基聚硅氧烷改性水性PU树脂在50～60℃、10～30KPa下减压蒸馏脱除丙酮，添加纯水使得到的长链烷基聚硅氧烷改性水性PU树脂固含量为30-35%。
4.根据权利要求3所述的一种水性双面绒面超纤PU合成革的制备方法，其特征在于：所述水性PU树脂的制备方法步骤1中丙烯醇聚氧乙烯醚的分子式为CH2=CH-CH2O(C2H4O)nH，其中n为8-12的整数；双硅氢基封端的甲基长链烷基聚二甲基硅氧烷的分子式为H-Si（CH3）2-O-[ Si（CH3）2]a-[ Si（CH3）（CmH2m+1）O]b-（CH3）2 Si-H，其中m为10-20的整数，a为5-20的整数，b为5-10的整数；羟基聚醚封端的长链烷聚硅氧烷中间体的分子式为H(OH4C2)nOH6C3-Si（CH3）2-O-[ Si（CH3）2]a-[ Si（CH3）（CmH2m+1）O]b-（CH3）2 Si- C3 H6O(C2 H4O)nH，其中m为10-20的整数，n为8-12的整数，a为5-20的整数，b为5-10的整数。
5.根据权利要求2所述的一种水性双面绒面超纤PU合成革的制备方法，其特征在于：所述水溶性粉包括醇解度为85-100的聚乙烯醇细粉，有机硅手感剂为超高分子量聚二甲基硅油乳液，有机硅柔软剂为非离子氨基硅油乳液，填料为凹凸棒土、高岭土、碳酸钙、木质素、钛白粉中的一种或两种以上混合，水性消泡剂为有机硅消泡剂。
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