CN116970174A - 一种亲水蓬松树枝状嵌段硅油及其制备方法 - Google Patents
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Abstract
本发明涉及纺织助剂领域,尤其涉及一种亲水蓬松树枝状嵌段硅油及其制备方法,先由丙三醇三缩水甘油醚、一乙醇胺制得Y型结构中间体,再以异丙醇为溶剂,用Y型结构中间体与双端环氧聚醚硅油反应,制得亲水蓬松树枝状嵌段硅油。制得的亲水蓬松树枝状嵌段硅油不仅具有优异自乳化性,而且能够赋予棉、涤、涤棉织物优异的蓬松手感、抗静电性以及亲水性能。
Description
技术领域
本发明涉及纺织助剂领域,尤其是涉及一种亲水蓬松树枝状嵌段硅油及其制备方法。
背景技术
随着生活水平的提高,人们对多样化织物的需求量也越来越大,使用舒适性要求也越来越高,往往整理后的织物不仅要求具有优异的亲水,而且同时还需要优异的抗静电、蓬松、柔软等性能。
近年来,硅油领域发展迅速,各种功能型硅油如雨后春笋般涌现,尤其在手感亲水硅油方面可谓日新月异。传统亲水硅油主要分为:(1)侧链含氢硅油与烯丙醇聚醚制得侧链型聚醚改性硅油(CJF);(2)环氧硅油与亲水聚醚胺交替排列直链型共聚亲水硅油;(3)环氧硅油与叔胺交替排列直链型共聚,然后加入烷基化试剂进行改性制得亲水硅油;(4)聚氨酯改性有机硅制备的亲水硅油。专利CN201610632480.2《一种三元共聚嵌段亲水性氨基硅油及其制备方法和应用》、专利CN201210134514.7《一种超柔软亲水嵌段硅油化合物和制备方法》就是通过上述合成工艺制得。
侧链型聚醚改性硅油(CJF)虽能够赋予整理后的织物优异亲水性,但存在整理后织物手感欠佳、织物使用面较窄等问题;环氧硅油与亲水聚醚胺或环氧硅油与叔胺交替排列直链型共聚亲水硅油虽能够赋予整理后织物优异的亲水性和手感,但是其结构为直链型聚合物,从结构上分析其手感主要体现为柔软、滑爽等特点;聚氨酯改性有机硅亲水硅油虽然也能体现整理后织物优异的亲水性,因其结构中软硬链段的存在,其主要体现的风格为滑弹型。综合分析,上述结构产物,其主要体现的性能为亲水、柔软、滑爽,而蓬松性能次之。因此,本发明通过使用自制的Y型结构中间体与双端环氧聚醚硅油反应,制备出一种亲水蓬松树枝状嵌段硅油,其树枝状结构中含大量的硅氧烷链段、胺基链段、亲水聚醚链段和羟基链段,从而可赋硅油优异的自乳化性,且赋予整理后的织物优异的蓬松性、抗静电性以及亲水性。
发明内容
本发明所要解决的技术问题是克服上述现有技术存在的缺陷,提供一种亲水蓬松树枝状嵌段硅油的制备方法。
为了实现上述目的,本发明采用以下技术方案:
一种亲水蓬松树枝状嵌段硅油的制备方法,其特征在于按如下合成方法进行,按质量份数计算:
将190~200份一乙醇胺加入到装有冷凝回流装置的反应容器中,开启搅拌,升温至60~80℃,然后将260份丙三醇三缩水甘油醚通过恒压滴液漏斗匀速滴加到反应容器中,滴加完成后,保温反应2~4小时,制得Y型结构中间体,其反应式如下;
将1000份双端环氧聚醚硅油、70~160份Y型结构中间体、300~500份溶剂加入到装有冷凝回流装置的反应容器中,开启搅拌,反应容器升温至80~83℃,在此温度范围内保温反应6~9小时,制得亲水蓬松树枝状嵌段硅油,其反应式如下;
式中m为27~80之间的整数,n为20~25之间的整数。
作为优选,所述的双端环氧聚醚硅油的数均分子量为4000~9000中的一种,且其结构中的聚醚链段为环氧乙烷(EO)链段。
作为优选,所述溶剂为异丙醇。
由于上述技术方案的运用,本发明具有如下优点:
本发明通过用自制的Y型结构中间体与双端环氧聚醚硅油反应制得了一种亲水蓬松树枝状嵌段硅油,自制的中间体结构中含有三个仲胺基,能与双端环氧基硅油反应制得树枝状结构,产物不仅具有高度支化、低粘度、高溶解性以及高反应性等特点,而且能够赋予整理后织物优异的蓬松性能。此外,Y型结构中间体相比传统的烷基叔胺和聚醚叔胺(EA结构系列),其反应后聚合物结构中含有大量的羟基,能够使聚合物实现自乳化的同时,也赋予织物优异的亲水性和抗静电性。
实施方式
下面通过具体实施方式对本发明做进一步描述。
实施例1
1、将190份一乙醇胺加入到装有冷凝回流装置的反应容器中,开启搅拌,升温至65℃,然后将260份丙三醇三缩水甘油醚通过恒压滴液漏斗匀速滴加到反应容器中,滴加完成后,保温反应2小时,制得Y型结构中间体。
2、将1000份数均分子量为5000的双端环氧聚醚硅油、130份Y型结构中间体、350份异丙醇加入到装有冷凝回流装置的反应容器中,开启搅拌,反应容器升温至80℃,在此温度范围内保温反应7小时,制得亲水蓬松树枝状嵌段硅油。
实施例2
1、将195份一乙醇胺加入到装有冷凝回流装置的反应容器中,开启搅拌,升温至70℃,然后将260份丙三醇三缩水甘油醚通过恒压滴液漏斗匀速滴加到反应容器中,滴加完成后,保温反应3小时,制得Y型结构中间体。
2、将1000份数均分子量为6000的双端环氧聚醚硅油、110份Y型结构中间体、400份异丙醇加入到装有冷凝回流装置的反应容器中,开启搅拌,反应容器升温至82℃,在此温度范围内保温反应8小时,制得亲水蓬松树枝状嵌段硅油。
实施例3
1、将200份一乙醇胺加入到装有冷凝回流装置的反应容器中,开启搅拌,升温至75℃,然后将260份丙三醇三缩水甘油醚通过恒压滴液漏斗匀速滴加到反应容器中,滴加完成后,保温反应4小时,制得Y型结构中间体。
2、将1000份数均分子量为8000的双端环氧聚醚硅油、80份Y型结构中间体、450份异丙醇加入到装有冷凝回流装置的反应容器中,开启搅拌,反应容器升温至83℃,在此温度范围内保温反应9小时,制得亲水蓬松树枝状嵌段硅油。
硅油应用评价工艺:
硅油的乳液配制
将实施例样品与市售同类型风格的对比样按同样乳化工艺乳化,得到含固量为14% ~15%的乳液,最后用冰醋酸调pH至3 ~ 6。
2.整理工艺
所用织物:白色纯棉针织布、黑色涤纶针织布、黑色涤棉针织布。
整理工艺流程:浸轧工作液(亲水蓬松树枝状嵌段硅油乳液40g/L,一浸一轧,轧余率(白色纯棉针织布80%~90%、黑色涤纶针织布60%~80%、黑色涤棉针织布70%~80%)→焙烘(白色纯棉针织布165oC×50s、黑色涤纶针织布190oC×60s、黑色涤棉针织布170oC×80s)→冷却回潮24 小时→测试性能。
3.应用性能测试
3.1蓬松性评价
用KES-FB3风格仪测试织物的压缩比功(N﹒cm/cm2),数值越大,蓬松性越好。
3.2亲水性评价
亲水性评价:用标准滴管从离织物10cm高度处向水平铺展的织物表面滴1滴水,从静态情况下测定水滴在织物表面上完全润湿、扩散、渗透所用的时间,时间越短,亲水效果越好。
3.3抗静电性评价
将整理后的织物在25℃,RH 30%条件下平衡24小时,然后在YG(B)342D型织物静电测试仪按标准测试峰值电压、半衰期。
本发明的一种亲水蓬松树枝状嵌段硅油乳液与对比样硅油乳液的蓬松性应用性能评价结果如表1所示:
表1实施例样品与对比样品的蓬松性对比
由表1可以看出,经本发明的一种亲水蓬松树枝状嵌段硅油制成的乳液对织物进行整理后,相比于对比样,蓬松性明显优于对比样。
本发明的一种亲水蓬松树枝状嵌段硅油乳液与对比样硅油乳液的亲水性能评价结果如表2所示:
表2实施例样品与对比样品的亲水性对比
由表2可以看出,经本发明的一种亲水蓬松树枝状嵌段硅油制成的乳液对织物进行整理后,相比于对比样,亲水性明显优于对比样。
本发明的一种亲水蓬松树枝状嵌段硅油乳液与对比例硅油乳液的抗静电性能测对比果如表3所示:
表3实施例样品与对比样品的抗静电性对比
由表3可以看出,经本发明的一种亲水蓬松树枝状嵌段硅油制成的乳液对织物进行整理后,峰值电压和半衰期均低于原布与对比例。
Claims (4)
1.一种亲水蓬松树枝状嵌段硅油及其制备方法,其特征在于包括如下步骤:
A: 按质量份进行配比,将190~200份一乙醇胺加入到装有冷凝回流装置的反应容器中,开启搅拌,升温至60~80℃,然后将260份丙三醇三缩水甘油醚通过恒压滴液漏斗匀速滴加到反应容器中,滴加完成后,保温反应2~4小时,制得Y型结构中间体,
B: 将1000份双端环氧聚醚硅油、70~160份Y型结构中间体、300~500份溶剂加入到装有冷凝回流装置的反应容器中,开启搅拌,反应容器升温至80~83℃,在此温度范围内保温反应6~9小时,制得亲水蓬松树枝状嵌段硅油。
2.根据权利要求1所述的一种亲水蓬松树枝状嵌段硅油及其制备方法,其特征在于:所述双端环氧聚醚硅油的数均分子量为4000~9000,且其结构中的聚醚链段为环氧乙烷(EO)链段。
3.根据权利要求1所述的一种亲水蓬松树枝状嵌段硅油及其制备方法,其特征在于:所述溶剂为异丙醇、乙二醇丁醚、二乙二醇丁醚中的一种。
4.一种亲水蓬松树枝状嵌段硅油,其特征在于:通过权利要求1-3中任一项所述的制备方法获得。
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