CN115584635B - 一种耐水洗的涤纶整理剂及其合成方法 - Google Patents
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Abstract
本发明公开了一种耐水洗的涤纶整理剂包括具有环氧基团的阳离子型水溶性聚酯。水溶性聚酯的合成包括以下步骤：在四口烧瓶内加入聚酯，然后加入酯交换多元醇，充分搅拌，通氮气驱赶空气；待空气驱赶完毕，加入酯交换催化剂，打开真空泵，缓慢升温至130‑200℃，保温2‑5h；关闭真空泵，加入亲水聚醚，充分搅拌后加入聚酯缩合催化剂，然后打开真空泵，缓慢升温至200‑280℃，保温3‑8h；关闭真空泵，缓慢降温至80‑120℃，加入亲核取代催化剂，然后缓慢滴加季铵化试剂，并保温2‑5h；然后加入溶剂，充分搅拌后，降温到常温，得到水溶性聚酯。本发明采用上述水溶性聚酯作为涤纶整理剂，具有持久的亲水性、抗静电效果，能够解决传统的涤纶整理剂耐水洗性较差的问题。
Description
技术领域
本发明涉及涤纶整理剂技术领域，尤其是涉及一种耐水洗的涤纶整理剂及其合成方法。
背景技术
水溶性聚酯作为涤纶整理剂的应用方向近几年尤为热门，其通过聚醚长链可以有效的改善涤纶的亲水性，提升涤纶织物的手感，以及改善其抗静电效果，赋予其如丝质般的手感。通常而言这类水溶性聚酯是由对苯二甲酸酯，间苯二甲酸酯，聚乙二醇，间苯二甲酸酯磺酸盐这四类物质缩合而成。
水溶性聚酯在涤纶面料上的应用极大程度的提升了面料品质及附加值。随着其大规模的应用，面料终端客户对其品质要求越来越高，其中最核心的一点就是耐洗性。通常在合成水溶性聚酯时我们需要加入间苯二甲酸酯磺酸盐来提升聚合物的溶解度以及水溶性聚酯溶液的分散稳定性，但极性较强的磺酸基与聚乙二醇无法在非极性的涤纶表面形成较好的共平面吸附，遇到清水洗涤时会不断的溶解到水溶液中，造成其耐洗性能较差。因此解决其耐洗性是水性聚酯作为涤纶整理剂的核心突破。
发明内容
本发明的目的是提供一种耐水洗的涤纶整理剂及其合成方法，以水溶性聚酯作为涤纶整理剂，具有持久的亲水性、抗静电效果，能够解决传统的涤纶整理剂耐水洗性较差的问题。
为实现上述目的，本发明提供了一种耐水洗的涤纶整理剂，包括具有环氧基团的阳离子型水溶性聚酯。
上述的具有环氧基团的阳离子型水溶性聚酯的结构式如下：
其中a，b，c，d，e的值均大于2。
上述的一种耐水洗的涤纶整理剂的合成方法，包括以下步骤：
S1、在搭有温度计，搅拌器，恒压滴加器和真空泵的四口烧瓶内加入聚酯，然后加入酯交换多元醇，充分搅拌，通氮气驱赶空气；
S2、待空气驱赶完毕，加入酯交换催化剂，打开真空泵，缓慢升温，升温至130-200℃，保温2-5h；
S3、关闭真空泵，加入亲水聚醚，充分搅拌后加入聚酯缩合催化剂，然后打开真空泵，缓慢升温至200-280℃，保温3-8h；
S4、关闭真空泵，缓慢降温至80-120℃，加入亲核取代催化剂，然后缓慢滴加季铵化试剂，并保温2-5h；然后加入溶剂，充分搅拌后，降温到常温，得到水溶性聚酯。
优选的，所述步骤S1中聚酯为间苯二甲酸二甲酯磺酸钠和对苯二甲酸二甲酯，酯交换多元醇为三乙醇胺。
优选的，所述步骤S2中酯交换催化剂为醋酸锌或醋酸锰。
优选的，所述步骤S3中亲水聚醚为PEG6000或PEG8000，聚酯缩合催化剂为二氧化钛或草酸钛钾。
优选的，所述步骤S4中亲核取代催化剂为四丁基溴化铵，季铵化试剂为环氧氯丙烷，溶剂为纯水和乙二醇。
上述的一种耐水洗的涤纶整理剂应用于涤纶纤维后整理。
本发明所述的一种耐水洗的涤纶整理剂及其合成方法的优点和积极效果是：
1、本发明所合成的水溶性聚酯含有阳离子基团与环氧基团，通过阳离子基团与涤纶表层的弱阴离子通过电荷吸引，在通过浸轧整理液时加入胺类固化剂后定型形成交联成膜，提升了吸附性能，有效的解决了涤纶整理的耐洗性问题。
2、连续状态的膜有效地改善涤纶亲水柔软的问题，阳离子的加入大大提升了其抗静电效果，使得涤纶织物的亲水、柔软、抗静电效果更加持久，提升了面料的服用性能与档次，具有极佳的推广价值。
下面通过实施例，对本发明的技术方案做进一步的详细描述。
具体实施方式
以下通过实施例对本发明的技术方案作进一步说明。除非另外定义，本发明使用的技术术语或者科学术语应当为本发明所属领域内具有一般技能的人士所理解的通常意义。
实施例1
具有环氧基团的阳离子型水溶性聚酯合成组分包括
酯交换催化剂：醋酸锌2份，
亲核取代催化剂：四丁基溴化铵3份，
季铵化试剂：环氧氯丙烷5份，
酯交换多元醇：三乙醇胺12份，
亲水聚醚：PEG6000 30份，
聚酯：间苯二甲酸二甲酯磺酸钠8份，对苯二甲酸二甲酯10份，
聚酯缩合催化剂：二氧化钛2份，
胺类固化剂：乙二胺3份，
溶剂：纯水20份，乙二醇10份，
合成步骤如下：
S1、在搭有温度计，搅拌器，恒压滴加器和真空泵的四口烧瓶内加入间苯二甲酸二甲酯磺酸钠和对苯二甲酸二甲酯，然后加入三乙醇胺，充分搅拌，通氮气驱赶空气；
S2、待空气驱赶完毕，加入醋酸锌，打开真空泵，缓慢升温，升温至150-200℃，保温3-5h；
S3、关闭真空泵，加入PEG6000，充分搅拌后加入二氧化钛，然后打开真空泵，缓慢升温至220-280℃，保温3-8h；
S4、关闭真空泵，缓慢降温至80-120℃，加入四丁基溴化铵，然后缓慢滴加环氧氯丙烷，并保温2-4h；然后加入纯水和乙二醇，充分搅拌后，降温到常温，得到水溶性聚酯。
浸轧合成的水溶性聚酯(浓度为50g/L)，并加入乙二胺，然后于160℃烘干定性40S，得到3块布料样品A。
实施例2
具有环氧基团的阳离子型水溶性聚酯合成组分包括
酯交换催化剂：醋酸锰2份，
亲核取代催化剂：四丁基溴化铵3份，
季铵化试剂：环氧氯丙烷4份，
酯交换多元醇：三乙醇胺14份，
亲水聚醚：PEG8000 18份，
聚酯：间苯二甲酸二甲酯磺酸钠6份，对苯二甲酸二甲酯8份，
聚酯缩合催化剂：草酸钛钾2份，
胺类固化剂：二乙烯三胺2份，
溶剂：纯水18份，乙二醇10份，
合成步骤如下：
S1、在搭有温度计，搅拌器，恒压滴加器和真空泵的四口烧瓶内加入间苯二甲酸二甲酯磺酸钠和对苯二甲酸二甲酯，然后加入三乙醇胺，充分搅拌，通氮气驱赶空气；
S2、待空气驱赶完毕，加入醋酸锰，打开真空泵，缓慢升温，升温至170-200℃，保温3-4h；
S3、关闭真空泵，加入PEG8000，充分搅拌后加入草酸钛钾，然后打开真空泵，缓慢升温至240-280℃，保温3-8h；
S4、关闭真空泵，缓慢降温至80-120℃，加入四丁基溴化铵，然后缓慢滴加环氧氯丙烷，并保温3-5h；然后加入纯水和乙二醇，充分搅拌后，降温到常温，得到水溶性聚酯。
浸轧合成的水溶性聚酯(浓度为50g/L)，并加入二乙烯三胺，然后于160℃烘干定性40S，得到3块布料样品B。
耐水洗性测试
将布料样品A(3块)、布料样品B(3块)和未扎染涤纶整理剂的空白布料(3块)分别用洗衣机进行洗涤0，1，2，3，4，5次。分别测试其亲水性来表征其表层水性聚酯的残留，结果取平均值。结果如表1所示：
表1样布洗涤后水在样布表面爬升的高度
| 洗涤0次 | 洗涤1次 | 洗涤2次 | 洗涤3次 | 洗涤4次 | 洗涤5次 | |
| 实施例1 | 21 | 23 | 19 | 20 | 18 | 19 |
| 实施例2 | 20 | 19 | 21 | 18 | 20 | 23 |
| 空白布料 | 6 | 5 | 7 | 5 | 4 | 4 |
水在样布表面爬升的高度越高，亲水性越好。
由表1可知，洗涤五次后浸轧水性聚酯的布料表面水爬升的高度没有太大变化，说明其亲水性并未有明显的衰减。表明本发明所述的水溶性聚酯作为涤纶整理剂具有优异的耐水洗性能。
因此，本发明采用上述水溶性聚酯作为涤纶整理剂，具有持久的亲水性、抗静电效果，能够解决传统的涤纶整理剂耐水洗性较差的问题。
最后应说明的是：以上实施例仅用以说明本发明的技术方案而非对其进行限制，尽管参照较佳实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对本发明的技术方案进行修改或者等同替换，而这些修改或者等同替换亦不能使修改后的技术方案脱离本发明技术方案的精神和范围。
Claims (3)
1.一种耐水洗的涤纶整理剂，其特征在于：包括具有环氧基团的阳离子型水溶性聚酯，结构式为：
其中a，b，c，d，e的值均大于2。
2.一种如权利要求1所述的耐水洗的涤纶整理剂的合成方法，其特征在于，包括以下步骤：
S1、在搭有温度计，搅拌器，恒压滴加器和真空泵的四口烧瓶内加入聚酯，然后加入酯交换多元醇，充分搅拌，通氮气驱赶空气；
S2、待空气驱赶完毕，加入酯交换催化剂，打开真空泵，缓慢升温，升温至130-200℃，保温2-5h；
S3、关闭真空泵，加入亲水聚醚，充分搅拌后加入聚酯缩合催化剂，然后打开真空泵，缓慢升温至200-280℃，保温3-8h；
S4、关闭真空泵，缓慢降温至80-120℃，加入亲核取代催化剂，然后缓慢滴加季铵化试剂，并保温2-5h；然后加入溶剂，充分搅拌后，降温到常温，得到水溶性聚酯；
其中步骤S1中聚酯为间苯二甲酸二甲酯磺酸钠和对苯二甲酸二甲酯，酯交换多元醇为三乙醇胺；步骤S2中酯交换催化剂为醋酸锌或醋酸锰；步骤S3中亲水聚醚为PEG6000或PEG8000，聚酯缩合催化剂为二氧化钛或草酸钛钾；步骤S4中亲核取代催化剂为四丁基溴化铵，季铵化试剂为环氧氯丙烷，溶剂为纯水和乙二醇。
3.一种如权利要求1所述的耐水洗的涤纶整理剂应用于涤纶纤维后整理。
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