CN114908571B - 一种蒸汽凝聚复合制备水性聚氨酯超纤革的方法 - Google Patents

一种蒸汽凝聚复合制备水性聚氨酯超纤革的方法 Download PDF

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CN114908571B
CN114908571B CN202210535527.9A CN202210535527A CN114908571B CN 114908571 B CN114908571 B CN 114908571B CN 202210535527 A CN202210535527 A CN 202210535527A CN 114908571 B CN114908571 B CN 114908571B
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林鹭
李志鹏
李仁杰
王旭
焦森
晁宣琦
陈益嘉
张政楠
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Shaanxi University of Science and Technology
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Abstract

本发明公开了一种蒸汽凝聚复合制备水性聚氨酯超纤革的方法，采用预聚体法将聚酯纤维无纺布浸入固含量为20％的水性聚氨酯溶液的浸渍槽中，在水中实现乳化，在破乳过程中，通过蒸汽凝聚符合技术，使用减压冷凝设备，真空脱水，将水汽化、蒸发，从而对树脂进行干燥，后采用高温回火的方式来加强超纤革的力学性能与强度提高水性超纤革的力学性能，其中强度提高了18.63％、拉伸负荷高达140N、撕裂强度达到38N，生产过程安全，无污染，具有绿色环保、无毒、无害、低VOC等环保方面的优点，实现了绿色生产；本发明的水性聚氨酯超细纤维，获得柔软丰满的革体，经测试透气透湿性能是传统溶剂型超纤革的两倍，综合性能优异，可以广泛的应用于汽车内饰、高档鞋包。

Description

一种蒸汽凝聚复合制备水性聚氨酯超纤革的方法
技术领域
本发明属于合成革技术领域，涉及聚氨酯超纤革的制备方法，具体涉及一种蒸汽凝聚复合制备水性聚氨酯超纤革的方法。
背景技术
现阶段我国皮革行业原料短缺，合成革行业污染严重，所用的树脂几乎全部为溶剂型聚氨酯，需要大量的溶剂，使得其环境污染问题严重，增加了处理环境污染成本，然而随着国际、国内限用或禁用物质法规不断出台，合成革行业面临着更加严峻的挑战，具有优良性能的仿真合成革的开发成为人类的追求。
水性聚氨酯是以水为分散介质，减少了VOC与DMF以及MEK等污染物的排放，具有绿色环保、无毒、无害、低VOC等环保方面的优点，实现了绿色生产，已成为合成革行业传统溶剂型聚氨酯的理想替代品。水性超纤革一般由两部分组成：一部分为非织造革基布，另一部分为WPU涂层，WPU涂层一般包括面层、发泡层和粘合层。水性聚氨酯具有耐低温的特点，WPU在成膜过程中，随着温度的升高，膜的断面上出现的泡孔数目就会越多且密度增大，在温度过高时，WPU上面就会出现很多不均匀的泡孔结构，粘合层表面出现严重的裂纹，为了使得粘结层的树脂与基布贴合更加牢固，则需要对树脂进行充分的干燥，然而水性聚氨酯的分散相为水，如果要水分完全被干燥则需要对水性聚氨酯进行破乳，以便在升温后水分子可以快速逸出。
目前现有的水性聚氨酯破乳方法为离心分离的机械破乳或加入乙酸、氢氧化钠等酸碱的化学方法进行破乳成膜，这些方法存在使成本增加并且所加入的酸碱等化学物质影响基布的性能，过程中产生大量废水、对环境有污染的缺陷有悖于国家现在所提倡的绿色环保生产。
发明内容
针对现有技术存在的不足，本发明的目的在于提供一种蒸汽凝聚复合制备水性聚氨酯超纤革的方法，提高产品的抵抗性能、提高复合效率、降低成本、减少污染。
为了实现上述目的，本发明采用以下技术方案予以实现：
一种蒸汽凝聚复合制备水性聚氨酯超纤革的方法，包括以下步骤：
步骤一、将100g聚乙二醇、30g异佛尔酮二异氰酸酯和3g 1,4-丁二醇加入到带有搅拌器的反应釜中，控制温度在70～80℃，搅拌反应3小时后，降温到25℃～35℃加入532g去离子水，搅拌乳化分散2小时，得到固含量为20％的水性聚氨酯溶液，即WPU-20；
步骤二、按浸渍量300％，用聚酯纤维无纺布在30～50℃的条件下含浸40～60min步骤一制备的WPU-20；
步骤三、在真空度为-0.1MPa温度为80℃的真空箱中，真空脱水50min，然后在70℃～90℃、31.16kpa～47.38kpa条件下在减压冷凝干燥设备中减压干燥30～60min，然后在100℃～120℃的烘箱中进行高温干燥30min，得到干燥的聚酯纤维无纺布/WPU复合材料；
步骤四、将干燥的聚酯纤维无纺布/WPU复合材料进行碱减量，减量结束后清洗，最后在100℃～140℃的烘箱中高温回火处理30min，制得水性聚氨酯超纤维革。
本发明还具有以下技术特征：
优选的，步骤一中所述的聚乙二醇的平均分子量为2000。
优选的，步骤一中所述的搅拌反应和搅拌乳化分散过程中搅拌器转速为300r/min。
优选的，步骤二中所述的聚酯纤维无纺布为PA6/COPET海岛纤维无纺布或PET/COPET海岛纤维无纺布。
优选的，所述的步骤二中浸渍完成后升温至50℃～65℃加入WPU-20质量的3wt％～5wt％的聚乙二醇进行扩链。
优选的，步骤四中所述的碱减量为用质量分数为2％的NaOH溶液进行碱减量，减量时间为50min，减量温度为95℃。
优选的，步骤四中所述的清洗为用大量的温水进行水洗，并用PH试纸进行检测，直至中性。
本发明与现有技术相比，具有如下技术效果：
本发明用水性聚氨酯替代了原有的溶剂型聚氨酯，在破乳过程中，通过蒸汽凝聚技术，使用减压冷凝设备，降低水的沸点，带出WPU-20浸渍聚酯纤维无纺布中的水分，使水分在蒸发后遇冷又凝结成水珠覆于浸渍无纺布的表面，降低浸渍聚酯纤维无纺布中水蒸发的速度，从而形成孔径大小一致，分布均匀的泡孔结构，在聚酯纤维无纺布间形成微孔水性聚氨酯填充体；破乳过程未使用任何溶剂，水性聚氨酯是以水为分散介质，生产过程安全，无污染，具有绿色环保、无毒、无害、低VOC等环保方面的优点，实现了绿色生产；
进一步的，本发明采用干法移膜技术制备水性聚氨酯超细纤维，利用真空脱水、降压、升温的方式对水性聚氨酯进行破乳，并且去除水，实现完全干燥，采用高温回火的方式来加强超纤革的力学性能与强度，提高水性超纤革的力学性能，其中强度提高了18.63％、拉伸负荷高达140N、撕裂强度达到38N；
本发明采用水性聚氨酯代替原有的溶剂型聚氨酯，降低溶剂的使用量，采用预聚体混合法能够减少有机溶剂使用量，降低成本，利用预聚体黏度严重影响乳化效果的缺点来帮助经过湿法浸渍后使用蒸汽凝聚的复合技术进行破乳成膜代替原有的物理—机械—化学的破乳方法；达到提高产品的抵抗性能、提高复合效率、降低成本、减少污染以及改良国内水性超纤革的生产技术与提升生产水平；
本发明中制备固含量为20％的水性聚氨酯溶液时升温至温度50℃～65℃时引入聚乙二醇进行扩链，得到密度小，柔软度高，吸水性好，透气性透湿性好的材料；
本发明的水性聚氨酯超细纤维，获得柔软丰满的革体，经测试透气透湿性能是传统溶剂型超纤革的两倍，综合性能优异，可以广泛的应用于汽车内饰、高档鞋包。
附图说明
图1为实施例1中进行蒸汽凝聚后的泡孔电镜扫描图；
图2为实施例1进行蒸汽凝聚前的泡孔电镜扫描图。
具体实施方式
以下结合实施例对本发明的具体内容做进一步详细解释说明。
以下各个实施例中聚乙二醇的平均分子量为2000。
实施例1：
步骤一、将100g聚乙二醇、30g异佛尔酮二异氰酸酯和3g 1,4-丁二醇加入到带有搅拌器的反应釜中，控制温度在80℃，搅拌反应3小时后，降温到30℃加入532g去离子水，搅拌乳化分散2小时，得到固含量为20％的水性聚氨酯溶液，即WPU-20；搅拌器搅拌转速为300r/min；
步骤二、按浸渍量300％用尼龙6(PA6)/碱溶性聚氨酯(COPET)海岛纤维无纺布含浸步骤一制备的WPU-20(以PA6/COPET的质量为基准)，50℃的条件下含浸40min，浸渍完成后升温至65℃加入WPU-20质量的3wt％的聚乙二醇进行扩链；
步骤三、在真空度为-0.1MPa温度为80℃的真空箱中，真空脱水50min，然后在70℃、31.16kpa条件下在减压冷凝干燥设备中减压干燥60min，然后在120℃的烘箱中进行高温干燥30min，得到干燥的PA6/COPET海岛纤维无纺布/WPU复合材料；
步骤四、将干燥的PA6/COPET海岛纤维无纺布/WPU复合材料用质量分数为2％的NaOH溶液进行碱减量，减量时间为50min，减量温度为95℃；减量结束后用大量的温水进行水洗，用PH试纸进行检测，直至中性最后在140℃的烘箱中高温回火处理30min，制得水性聚氨酯超纤维革。
实施例2：
步骤一、将100g聚乙二醇、30g异佛尔酮二异氰酸酯和3g 1,4-丁二醇加入到带有搅拌器的反应釜中，控制温度在70℃，搅拌反应3小时后，降温到25℃加入532g去离子水，搅拌乳化分散2小时，得到固含量为20％的水性聚氨酯溶液，即WPU-20；搅拌器搅拌转速为300r/min；
步骤二、按浸渍量300％用PET/COPET海岛纤维无纺布含浸步骤一制备的WPU-20，30℃的条件下含浸60min，浸渍完成后升温至50℃加入WPU-20质量的5wt％的聚乙二醇进行扩链；
步骤三、浸渍结束后，在真空度为-0.1MPa温度为80℃的真空箱中，真空脱水50min，然后在90℃、47.38kpa条件下在减压冷凝干燥设备中减压干燥50min，然后在100℃的烘箱中进行高温干燥30min，得到干燥的PET/COPET海岛纤维无纺布/WPU复合材料；
步骤四、将干燥的PET/COPET海岛纤维无纺布/WPU复合材料用质量分数为2％的NaOH溶液进行碱减量，减量时间为50min，减量温度为95℃；减量结束后用大量的温水进行水洗，用PH试纸进行检测，直至中性最后在100℃的烘箱中高温回火处理30min，制得水性聚氨酯超纤维革。
实施例3：
步骤一、将100g聚乙二醇、30g异佛尔酮二异氰酸酯和3g 1,4-丁二醇加入到带有搅拌器的反应釜中，控制温度在75℃，搅拌反应3小时后，降温到35℃加入532g去离子水，搅拌乳化分散2小时，得到固含量为20％的水性聚氨酯溶液，即WPU-20；搅拌器搅拌转速为300r/min；
步骤二、按浸渍量300％用尼龙6(PA6)/碱溶性聚氨酯(COPET)海岛纤维无纺布含浸步骤一制备的WPU-20，40℃的条件下含浸50min，浸渍完成后升温至55℃加入WPU-20质量的4wt％的聚乙二醇进行扩链；
步骤三、在真空度为-0.1MPa温度为80℃的真空箱中，真空脱水50min，然后在80℃、45kpa条件下在减压冷凝干燥设备中减压干燥50min，然后在110℃的烘箱中进行高温干燥30min，得到干燥的PA6/COPET海岛纤维无纺布/WPU复合材料；
步骤四、将干燥的PA6/COPET海岛纤维无纺布/WPU复合材料用质量分数为2％的NaOH溶液进行碱减量，减量时间为50min，减量温度为95℃；减量结束后用大量的温水进行水洗，用PH试纸进行检测，直至中性最后在120℃的烘箱中高温回火处理30min，制得水性聚氨酯超纤维革。
实施例4：
步骤一、将100g聚乙二醇、30g异佛尔酮二异氰酸酯和3g 1,4-丁二醇加入到带有搅拌器的反应釜中，控制温度在80℃，搅拌反应3小时后，降温到30℃加入532g去离子水，搅拌乳化分散2小时，得到固含量为20％的水性聚氨酯溶液，即WPU-20；搅拌器搅拌转速为300r/min；
步骤二、按浸渍量300％用尼龙6(PA6)/碱溶性聚氨酯(COPET)海岛纤维无纺布含浸步骤一制备的WPU-20，50℃的条件下含浸40min，浸渍完成后升温至65℃加入WPU-20质量的5wt％的聚乙二醇进行扩链；
步骤三、在真空度为-0.1MPa温度为80℃的真空箱中，真空脱水50min，然后在75℃、35kpa条件下在减压冷凝干燥设备中减压干燥60min，然后在110℃的烘箱中进行高温干燥30min，得到干燥的PA6/COPET海岛纤维无纺布/WPU复合材料；
步骤四、将干燥的PA6/COPET海岛纤维无纺布/WPU复合材料用质量分数为2％的NaOH溶液进行碱减量，减量时间为50min，减量温度为95℃；减量结束后用大量的温水进行水洗，用PH试纸进行检测，直至中性最后在140℃的烘箱中高温回火处理30min，制得水性聚氨酯超纤维革。
将实施例1中进行蒸汽凝聚前后的泡孔电镜扫描图对比，如图1所示，对比于图2，纤维束之间的PU，形成立体网状的通透“离型结构”填充，赋予成革良好的透气透湿性能和压缩弹性，获得柔软丰满的革体，经测试透气透湿性能是传统溶剂型超纤革的两倍；测试实施例1进行高温回火处理前后的水性超纤革的力学性能与强度，结果显示经过高温回火处理加强了水性超纤革的力学性能与强度，强度提高了18.63％。
参照上述实施例对本发明进行了详细说明，所属领域的普通技术人员在未脱离本发明精神和范围内对本发明技术方案所做出的任何修改或者等同替换，其均应涵盖在本发明权利要求保护范围当中。

Claims (5)

1.一种蒸汽凝聚复合制备水性聚氨酯超纤革的方法，其特征在于，包括以下步骤：
步骤一、将100g聚乙二醇、30g异佛尔酮二异氰酸酯和3g 1,4-丁二醇加入到带有搅拌器的反应釜中，控制温度在70～80℃，搅拌反应3小时后，降温到25℃～35℃加入532g去离子水，搅拌乳化分散2小时，得到固含量为20%的水性聚氨酯溶液，即WPU-20；
步骤二、按浸渍量300%，用聚酯纤维无纺布在30~50℃的条件下含浸40~60min步骤一制备的WPU-20；
所述的步骤二中浸渍完成后升温至50℃~65℃加入WPU-20质量的3wt%~5wt%的聚乙二醇进行扩链；
步骤三、在真空度为-0.1MPa温度为80℃的真空箱中，真空脱水50min，然后在70℃~90℃、31.16kpa~47.38kpa条件下在减压冷凝干燥设备中减压干燥30~60min，然后在100℃~120℃的烘箱中进行高温干燥30min，得到干燥的聚酯纤维无纺布/WPU复合材料；
步骤四、将干燥的聚酯纤维无纺布/WPU复合材料进行碱减量，减量结束后清洗，最后在100℃~140℃的烘箱中高温回火处理30min，制得水性聚氨酯超纤维革；
所述的聚乙二醇的平均分子量为2000。
2.如权利要求1所述的蒸汽凝聚复合制备水性聚氨酯超纤革的方法，其特征在于，步骤一中所述的搅拌反应和搅拌乳化分散过程中搅拌器转速为300r/min。
3.如权利要求1所述的蒸汽凝聚复合制备水性聚氨酯超纤革的方法，其特征在于，步骤二中所述的聚酯纤维无纺布为PA6/COPET海岛纤维无纺布或PET/COPET海岛纤维无纺布。
4.如权利要求1所述的蒸汽凝聚复合制备水性聚氨酯超纤革的方法，其特征在于，步骤四中所述的碱减量为用质量分数为2%的NaOH溶液进行碱减量，减量时间为50 min，减量温度为95℃。
5.如权利要求1所述的蒸汽凝聚复合制备水性聚氨酯超纤革的方法，其特征在于，步骤四中所述的清洗为用大量的温水进行水洗，并用PH试纸进行检测，直至中性。
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