CN110924143A - 一种拒水拒油整理剂的制备方法 - Google Patents

一种拒水拒油整理剂的制备方法 Download PDF

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CN110924143A
CN110924143A CN201911250372.9A CN201911250372A CN110924143A CN 110924143 A CN110924143 A CN 110924143A CN 201911250372 A CN201911250372 A CN 201911250372A CN 110924143 A CN110924143 A CN 110924143A
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repellent
water
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许磊
张蓉
虞琳
张振雄
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Suzhou Institute of Trade and Commerce
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Abstract

本发明提供了一种拒水拒油整理剂的制备方法，包括以下步骤：（1）将纳米SiO2和ZnO用硅烷偶联剂处理；（2）将步骤（1）制得的沉淀颗粒、聚氧乙烯烷基醇酰胺、十二烷基醇聚氧乙烯醚硫酸钠加入水溶液中搅拌混合，再加入三异丙基硅烷基甲基丙烯酸酯、三羟甲基丙烷三丙烯酸酯、乙二醇二甲基丙烯酸酯、甲基丙烯酸缩水甘油酯、三氟甲基三氟乙烯基醚、N‑甲基全氟辛基磺酰基胺基丙烯酸乙酯、水性聚氨酯，制得预乳液；（3）将预乳液使用过硫酸铵引发聚合；（4）再加入醋酸锌、2,5,二甲基‑2,5‑双（叔丁过氧基）己烷、乙醇胺2‑5份继续搅拌反应，制得拒水拒油整理剂。该整理剂作为拒水拒油功能剂具有良好的应用价值和市场前景。

Description

一种拒水拒油整理剂的制备方法
技术领域
本发明属于纺织技术领域，具体涉及一种拒水拒油整理剂的制备方法。
背景技术
纺织品由天然或合成纤维构成，纤维具有多孔性且纤维与纤维之间存在一定的空隙，因此由纤维构成的织物特别容易被液体润湿。随着生产和生活水平的提高，人们对纺织品的要求也在不断提高，对于一些特殊应用环境的纺织品，需要具有拒水拒油的性能，从而满足纺织品的防水防油性，适应人们生活生产的需要。现有对纺织品进行拒水拒油的处理方法通常是在织物表面通过浸渍、浸轧或涂覆手段施加一种分子结构特殊的化合物，经与纤维发生结合，改变纤维表面结构，降低织物临界表面张力，使其不被水或者油润湿。虽然现有的整理方法能够实现一定的拒水拒油整理效果，然而对于更高要求的拒水拒油需求，现有的整理方法还不能满足，因此，有必要进一步开发具有更高性能的拒水拒油整理剂。
发明内容
为了解决以上现有技术存在的问题，本发明的目的在于提供一种拒水拒油整理剂的制备方法。
为了实现上述目的，本发明提供以下技术方案：
一种拒水拒油整理剂的制备方法，包括以下步骤：
（1）将纳米SiO2和ZnO加入含有聚乙烯吡咯烷酮的水溶液中，使得纳米颗粒的质量分数为20-40%，将溶液pH调节到7.5-8.0，在搅拌的条件下将温度缓慢升至40-50℃，在搅拌的过程中加入浓度为5-10%的硅烷偶联剂，继续搅拌反应1-2h后，通过抽滤收集沉淀颗粒，并将其置于烘箱中烘干；
（2）将步骤（1）制得的沉淀颗粒15-30份、聚氧乙烯烷基醇酰胺4-8份、十二烷基醇聚氧乙烯醚硫酸钠5-10份加入60-80份水溶液中搅拌混合，在搅拌的条件下依次加入三异丙基硅烷基甲基丙烯酸酯10-15份、三羟甲基丙烷三丙烯酸酯8-16份、乙二醇二甲基丙烯酸酯10-16份、甲基丙烯酸缩水甘油酯9-14份、三氟甲基三氟乙烯基醚10-20份、N-甲基全氟辛基磺酰基胺基丙烯酸乙酯6-12份、水性聚氨酯7-14份，在室温下搅拌反应1-2h，再将反应物置于剪切乳化机上乳化20-30min，制得预乳液；
（3）将步骤（2）制得的预乳液转移至搅拌器中，在搅拌的条件下升温至50-80℃，缓慢滴加过硫酸铵2-4份并于1h内滴完，滴加完后于60-70℃的温度下保温反应2-4h，反应结束后将反应体系降至30-40℃；
（4）向步骤（3）的反应体系中加入醋酸锌3-6份、2,5,二甲基-2,5-双（叔丁过氧基）己烷4-9份、乙醇胺2-5份继续搅拌反应1-3h，将反应体系降至室温，即制得拒水拒油整理剂。
进一步的，所述步骤（1）中SiO2和ZnO的质量比为（1-4）：（1-3）。
进一步的，所述步骤（1）中硅烷偶联剂为γ-氨丙基三乙氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷或γ-(甲基丙烯酰氧)丙基三甲氧基硅烷。
进一步的，所述步骤（2）中各原料的重量份为：步骤（1）制得的沉淀颗粒22份、聚氧乙烯烷基醇酰胺6份、十二烷基醇聚氧乙烯醚硫酸钠8份、水溶液70份、三异丙基硅烷基甲基丙烯酸酯12份、三羟甲基丙烷三丙烯酸酯12份、乙二醇二甲基丙烯酸酯13份、甲基丙烯酸缩水甘油酯12份、三氟甲基三氟乙烯基醚15份、N-甲基全氟辛基磺酰基胺基丙烯酸乙酯9份、水性聚氨酯10份。
以上所述的制备方法制得的拒水拒油整理剂。
有益效果：本发明提供了一种拒水拒油整理剂的制备方法，经本发明所述制备方法制备的整理剂处理的面料具有良好的拒水拒油性能，并且本发明所述整理剂的拒水拒油效果明显优于市售整理剂的使用效果。并且通过对比例得知，纳米SiO2和ZnO对拒水拒油性能的提高起到重要的作用，醋酸锌、2,5,二甲基-2,5-双（叔丁过氧基）己烷和乙醇胺与其它原料协同作用，共同发挥整理剂的拒水拒油性能。因此，该整理剂在纺织领域具有良好的应用价值和市场前景。
具体实施方式
下面结合具体实施例来进一步描述本发明，但实施例仅是范例性的，并不对本发明的范围构成任何限制。本领域技术人员应该理解的是，在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换，但这些修改和替换均落入本发明的保护范围内。
实施例1
一种拒水拒油整理剂的制备方法，包括以下步骤：
（1）将纳米SiO2和ZnO加入含有聚乙烯吡咯烷酮的水溶液中，使得纳米颗粒的质量分数为30%，将溶液pH调节到7.5，在搅拌的条件下将温度缓慢升至45℃，在搅拌的过程中加入浓度为8%的硅烷偶联剂，继续搅拌反应1.5h后，通过抽滤收集沉淀颗粒，并将其置于烘箱中烘干；
（2）将步骤（1）制得的沉淀颗粒22份、聚氧乙烯烷基醇酰胺6份、十二烷基醇聚氧乙烯醚硫酸钠8份加入70份水溶液中搅拌混合，在搅拌的条件下依次加入三异丙基硅烷基甲基丙烯酸酯12份、三羟甲基丙烷三丙烯酸酯12份、乙二醇二甲基丙烯酸酯13份、甲基丙烯酸缩水甘油酯12份、三氟甲基三氟乙烯基醚15份、N-甲基全氟辛基磺酰基胺基丙烯酸乙酯9份、水性聚氨酯10份，在室温下搅拌反应1.5h，再将反应物置于剪切乳化机上乳化25min，制得预乳液；
（3）将步骤（2）制得的预乳液转移至搅拌器中，在搅拌的条件下升温至50-80℃，缓慢滴加过硫酸铵3份并于1h内滴完，滴加完后于65℃的温度下保温反应3h，反应结束后将反应体系降至35℃；
（4）向步骤（3）的反应体系中加入醋酸锌4份、2,5,二甲基-2,5-双（叔丁过氧基）己烷7份、乙醇胺4份继续搅拌反应2h，将反应体系降至室温，即制得拒水拒油整理剂。
所述步骤（1）中SiO2和ZnO的质量比为1：1。
所述步骤（1）中硅烷偶联剂为γ-氨丙基三乙氧基硅烷。
实施例2
一种拒水拒油整理剂的制备方法，包括以下步骤：
（1）将纳米SiO2和ZnO加入含有聚乙烯吡咯烷酮的水溶液中，使得纳米颗粒的质量分数为20%，将溶液pH调节到7.5，在搅拌的条件下将温度缓慢升至40℃，在搅拌的过程中加入浓度为5%的硅烷偶联剂，继续搅拌反应1h后，通过抽滤收集沉淀颗粒，并将其置于烘箱中烘干；
（2）将步骤（1）制得的沉淀颗粒15份、聚氧乙烯烷基醇酰胺4份、十二烷基醇聚氧乙烯醚硫酸钠5份加入60份水溶液中搅拌混合，在搅拌的条件下依次加入三异丙基硅烷基甲基丙烯酸酯10份、三羟甲基丙烷三丙烯酸酯8份、乙二醇二甲基丙烯酸酯10份、甲基丙烯酸缩水甘油酯9份、三氟甲基三氟乙烯基醚10份、N-甲基全氟辛基磺酰基胺基丙烯酸乙酯6份、水性聚氨酯7份，在室温下搅拌反应1h，再将反应物置于剪切乳化机上乳化20min，制得预乳液；
（3）将步骤（2）制得的预乳液转移至搅拌器中，在搅拌的条件下升温至50℃，缓慢滴加过硫酸铵2份并于1h内滴完，滴加完后于60℃的温度下保温反应2h，反应结束后将反应体系降至30℃；
（4）向步骤（3）的反应体系中加入醋酸锌3份、2,5,二甲基-2,5-双（叔丁过氧基）己烷4份、乙醇胺2份继续搅拌反应1h，将反应体系降至室温，即制得拒水拒油整理剂。
所述步骤（1）中SiO2和ZnO的质量比为1：2。
所述步骤（1）中硅烷偶联剂为γ-缩水甘油醚氧丙基三甲氧基硅烷。
实施例3
一种拒水拒油整理剂的制备方法，包括以下步骤：
（1）将纳米SiO2和ZnO加入含有聚乙烯吡咯烷酮的水溶液中，使得纳米颗粒的质量分数为25%，将溶液pH调节到7.8，在搅拌的条件下将温度缓慢升至45℃，在搅拌的过程中加入浓度为7%的硅烷偶联剂，继续搅拌反应1.2h后，通过抽滤收集沉淀颗粒，并将其置于烘箱中烘干；
（2）将步骤（1）制得的沉淀颗粒20份、聚氧乙烯烷基醇酰胺5份、十二烷基醇聚氧乙烯醚硫酸钠6份加入65份水溶液中搅拌混合，在搅拌的条件下依次加入三异丙基硅烷基甲基丙烯酸酯12份、三羟甲基丙烷三丙烯酸酯10份、乙二醇二甲基丙烯酸酯12份、甲基丙烯酸缩水甘油酯10份、三氟甲基三氟乙烯基醚12份、N-甲基全氟辛基磺酰基胺基丙烯酸乙酯8份、水性聚氨酯9份，在室温下搅拌反应1.2h，再将反应物置于剪切乳化机上乳化22min，制得预乳液；
（3）将步骤（2）制得的预乳液转移至搅拌器中，在搅拌的条件下升温至60℃，缓慢滴加过硫酸铵2.5份并于1h内滴完，滴加完后于62℃的温度下保温反应2.5h，反应结束后将反应体系降至33℃；
（4）向步骤（3）的反应体系中加入醋酸锌4份、2,5,二甲基-2,5-双（叔丁过氧基）己烷6份、乙醇胺3份继续搅拌反应1.5h，将反应体系降至室温，即制得拒水拒油整理剂。
所述步骤（1）中SiO2和ZnO的质量比为1：3。
所述步骤（1）中硅烷偶联剂为γ-(甲基丙烯酰氧)丙基三甲氧基硅烷。
实施例4
一种拒水拒油整理剂的制备方法，包括以下步骤：
（1）将纳米SiO2和ZnO加入含有聚乙烯吡咯烷酮的水溶液中，使得纳米颗粒的质量分数为40%，将溶液pH调节到8.0，在搅拌的条件下将温度缓慢升至50℃，在搅拌的过程中加入浓度为10%的硅烷偶联剂，继续搅拌反应2h后，通过抽滤收集沉淀颗粒，并将其置于烘箱中烘干；
（2）将步骤（1）制得的沉淀颗粒30份、聚氧乙烯烷基醇酰胺8份、十二烷基醇聚氧乙烯醚硫酸钠10份加入80份水溶液中搅拌混合，在搅拌的条件下依次加入三异丙基硅烷基甲基丙烯酸酯15份、三羟甲基丙烷三丙烯酸酯16份、乙二醇二甲基丙烯酸酯16份、甲基丙烯酸缩水甘油酯14份、三氟甲基三氟乙烯基醚20份、N-甲基全氟辛基磺酰基胺基丙烯酸乙酯12份、水性聚氨酯14份，在室温下搅拌反应2h，再将反应物置于剪切乳化机上乳化30min，制得预乳液；
（3）将步骤（2）制得的预乳液转移至搅拌器中，在搅拌的条件下升温至80℃，缓慢滴加过硫酸铵4份并于1h内滴完，滴加完后于70℃的温度下保温反应4h，反应结束后将反应体系降至40℃；
（4）向步骤（3）的反应体系中加入醋酸锌6份、2,5,二甲基-2,5-双（叔丁过氧基）己烷9份、乙醇胺5份继续搅拌反应3h，将反应体系降至室温，即制得拒水拒油整理剂。
所述步骤（1）中SiO2和ZnO的质量比为2：1。
所述步骤（1）中硅烷偶联剂为γ-缩水甘油醚氧丙基三甲氧基硅烷。
对比例1
对比例1与实施例1的区别在于，对比例1中未添加纳米SiO2和ZnO。
对比例2
对比例2与实施例1的区别在于，对比例2中未进行步骤（4）的操作。
将实施例1-4、对比例1-2、市售整理剂整理后的纯棉面料进行以下性能测试：
（1）拒水性能测试：使用OCA40型视频接触角测量仪进行接触角测定，同一样品在不同位置测量5次，取其平均值。
（2）防油性能测试：参照AATCC-118，在试验布上的三个地方滴加数滴测试液，观察30s后的浸透状态，以未出现浸透的测试液所赋予的防油性的最高点作为防油等级。
（3）拒水等级测试：参照AATCC22-2005纺织品拒水性测试喷淋法进行拒水等级测试。
从表1和表2中得出，经本发明整理剂处理的面料具有良好的拒水拒油性能，并且本发明所述整理剂的拒水拒油效果明显优于市售整理剂的使用效果，因此，该整理剂具有良好的市场前景。并且通过对比例得知，纳米SiO2和ZnO对拒水拒油性能的提高起到重要的作用，纳米SiO2和ZnO可以大幅提升醋酸锌、2,5,二甲基-2,5-双（叔丁过氧基）己烷和乙醇胺与其它原料协同作用，共同发挥整理剂的拒水拒油性能，其纳米化粒子的小尺寸效应及表面效应大大提升了拒水性能。
表1
Figure 808575DEST_PATH_IMAGE002
表2
Figure 912666DEST_PATH_IMAGE004

Claims (5)

1.一种拒水拒油整理剂的制备方法，其特征在于，包括以下步骤：
（1）将纳米SiO2和ZnO加入含有聚乙烯吡咯烷酮的水溶液中，使得纳米颗粒的质量分数为20-40%，将溶液pH调节到7.5-8.0，在搅拌的条件下将温度缓慢升至40-50℃，在搅拌的过程中加入浓度为5-10%的硅烷偶联剂，继续搅拌反应1-2h后，通过抽滤收集沉淀颗粒，并将其置于烘箱中烘干；
（2）将步骤（1）制得的沉淀颗粒15-30份、聚氧乙烯烷基醇酰胺4-8份、十二烷基醇聚氧乙烯醚硫酸钠5-10份加入60-80份水溶液中搅拌混合，在搅拌的条件下依次加入三异丙基硅烷基甲基丙烯酸酯10-15份、三羟甲基丙烷三丙烯酸酯8-16份、乙二醇二甲基丙烯酸酯10-16份、甲基丙烯酸缩水甘油酯9-14份、三氟甲基三氟乙烯基醚10-20份、N-甲基全氟辛基磺酰基胺基丙烯酸乙酯6-12份、水性聚氨酯7-14份，在室温下搅拌反应1-2h，再将反应物置于剪切乳化机上乳化20-30min，制得预乳液；
（3）将步骤（2）制得的预乳液转移至搅拌器中，在搅拌的条件下升温至50-80℃，缓慢滴加过硫酸铵2-4份并于1h内滴完，滴加完后于60-70℃的温度下保温反应2-4h，反应结束后将反应体系降至30-40℃；
（4）向步骤（3）的反应体系中加入醋酸锌3-6份、2,5,二甲基-2,5-双（叔丁过氧基）己烷4-9份、乙醇胺2-5份继续搅拌反应1-3h，将反应体系降至室温，即制得拒水拒油整理剂。
2.根据权利要求1所述的一种拒水拒油整理剂的制备方法，其特征在于，所述步骤（1）中SiO2和ZnO的质量比为（1-4）：（1-3）。
3.根据权利要求1所述的一种拒水拒油整理剂的制备方法，其特征在于，所述步骤（1）中硅烷偶联剂为γ-氨丙基三乙氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷或γ-(甲基丙烯酰氧)丙基三甲氧基硅烷。
4.根据权利要求1所述的一种拒水拒油整理剂的制备方法，其特征在于，所述步骤（2）中各原料的重量份为：步骤（1）制得的沉淀颗粒22份、聚氧乙烯烷基醇酰胺6份、十二烷基醇聚氧乙烯醚硫酸钠8份、水溶液70份、三异丙基硅烷基甲基丙烯酸酯12份、三羟甲基丙烷三丙烯酸酯12份、乙二醇二甲基丙烯酸酯13份、甲基丙烯酸缩水甘油酯12份、三氟甲基三氟乙烯基醚15份、N-甲基全氟辛基磺酰基胺基丙烯酸乙酯9份、水性聚氨酯10份。
5.权利要求1-4任一项所述的制备方法制得的拒水拒油整理剂。
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102002128A (zh) * 2010-10-22 2011-04-06 东华大学 一种有机－无机复合乳液拒水拒油整理剂及其应用
CN102041681A (zh) * 2009-10-14 2011-05-04 江南大学 一种含有改性纳米氧化物短支链含氟拒水拒油整理剂的制备方法
CN103289010A (zh) * 2013-05-23 2013-09-11 陕西科技大学 核壳型纳米SiO2/含氟聚丙烯酸酯无皂乳液的制备方法
CN103938451A (zh) * 2014-03-25 2014-07-23 福州大学 一种含氟硅核-壳型织物整理剂及其制备方法
CN104831540A (zh) * 2015-05-20 2015-08-12 丹东优耐特纺织品有限公司 纺织品用拒水、拒油、耐晒、抗扭曲弯挠、耐寒、无光皮膜水性涂层胶及制备方法
CN109371679A (zh) * 2018-09-20 2019-02-22 黄勇 一种易去污型织物拒水拒油整理剂的制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102041681A (zh) * 2009-10-14 2011-05-04 江南大学 一种含有改性纳米氧化物短支链含氟拒水拒油整理剂的制备方法
CN102002128A (zh) * 2010-10-22 2011-04-06 东华大学 一种有机－无机复合乳液拒水拒油整理剂及其应用
CN103289010A (zh) * 2013-05-23 2013-09-11 陕西科技大学 核壳型纳米SiO2/含氟聚丙烯酸酯无皂乳液的制备方法
CN103938451A (zh) * 2014-03-25 2014-07-23 福州大学 一种含氟硅核-壳型织物整理剂及其制备方法
CN104831540A (zh) * 2015-05-20 2015-08-12 丹东优耐特纺织品有限公司 纺织品用拒水、拒油、耐晒、抗扭曲弯挠、耐寒、无光皮膜水性涂层胶及制备方法
CN109371679A (zh) * 2018-09-20 2019-02-22 黄勇 一种易去污型织物拒水拒油整理剂的制备方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
安秋凤 等: ""氟代聚丙烯酸酯乳液的制备及应用"", 《纺织学报》 *

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