CN111607969B - 一种用于棉织物的亲水有机硅整理剂及其制备方法 - Google Patents
一种用于棉织物的亲水有机硅整理剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种用于棉织物的亲水有机硅整理剂及其制备方法,涉及纺织助剂的技术领域,所述有机硅整理剂由包括以下重量百分比的组分制备得到:一氯单体15%~25%、二氯单体5%~10%、三氯单体2.5%~5%、交联性单体0.5%~1%、环保溶剂5%~10%、混合乳化剂2.5%~5%、pH=4~4.5的去离子水余量。本发明具有提供一种亲水性能更好的纺织整理剂优点。
Description
技术领域
本发明涉及纺织助剂的技术领域,尤其是涉及一种用于棉织物的亲水有机硅整理剂及其制备方法。
背景技术
纺织助剂是纺织品生产加工过程中必须的化学品。纺织助剂对提高纺织品的产品质量和附加价值具有不可或缺的重要作用,它不仅能赋予纺织品各种特殊功能和风格,如柔软、防皱、防缩、防水、抗菌、抗静电、阻燃等,还可以改进染整工艺,起到节约能源和降低加工成本的作用。纺织助剂对提升纺织工业的整体水平以及在纺织产业链中的作用是至关重要的。
有机硅整理剂作为织物面料的特殊功能整理,越来越受到广大消费者的喜爱,随着消费者消费水平的不断提高,消费需求的不断加大,作为面料加工单位,也越来越重视织物的手感研究,并不断推出符合广大消费者要求的手感特点,市面上的有机硅整理剂可以显著改善织物的手感,具有柔软、滑爽、蓬松等特点,大大的满足消费者需求。
但目前用于棉织物的有机硅整理剂存在的一个普遍的缺点是耐洗性不佳和亲水性因为客户追求手感而失去过多,这主要是有机硅整理剂与棉纤维的反应基团不够牢固,常规经过十次洗涤之后手感明显下降,另外棉织物本身的亲水基团又被有机硅整理剂封闭而失去了作用导致。
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用于棉织物的亲水有机硅整理剂及其制备方法,要求整理剂在棉织物上吸附量高且耐洗性好,在赋予织物很好的柔软、滑爽、蓬松等手感的同时,不失去棉织物本身的高亲水性能。
本发明的上述目的是通过以下技术方案得以实现的:
一种用于棉织物的亲水有机硅整理剂,所述有机硅整理剂由包括以下重量百分比的组分制备得到:
其中,一氯单体的结构式为式(a);
二氯单体的结构式为式(b);
三氯单体的结构式为式(c);
其中,
R为:
4≤a≤6,8≤b≤10,8≤n≤10,5≤x≤10,30≤y≤60。
通过采用上述技术方案,配制得到的有机硅整理剂一方面由于具有三聚氯氰的桥架结构,具有极佳的平面构型,所以具有更为优异的平滑性能;另一方面由于此有机硅结构中含有多种反应基团,特别是含有氯反应基团,可以更好的与棉织物反应,同时,由于一氯单体、二氯单体、三氯单体分子量差别较大,所以可以在棉织物的内、中、外不同层面起作用,又由于此有机硅整理剂不单独作用于织物表面,而是采用氯反应基团与织物反应,如此一来可以更多的保留有机硅整理剂中的氨基和羟基,而并不完全封闭亲水基团,最终起到持久整理效果的同时,又可以兼顾手感和亲水性,另外混合乳化剂中的成分,又可以进一步保证亲水性效果。
本发明进一步设置为:交联性单体为分子量为1000~2000的乙烯基硅油,所述环保溶剂为1,4-戊二醇。
通过采用上述技术方案,采用分子量为1000~2000的乙烯基硅油与其他各组分的兼容性好,交联后得到的产物分子量更加合适,更加有利于得到的有机硅整理剂布料的整理效果。
本发明进一步设置为:所述一氯单体、二氯单体、三氯单体由包括以下重量百分比的组分制备得到:
所述碱性催化剂选用碳酸氢钠、碳酸钠或单乙醇胺中的一种或多种;
所述端环氧基硅油的结构简式为:
所述聚醚胺的结构简式为:
本发明进一步设置为:所述端环氧基硅油选用分子量为2218-2774的端环氧基硅油,聚醚胺选用分子量为364-654的聚醚胺。
通过采用上述技术方案,控制端环氧基硅油和聚醚胺的分子量,以控制最终产物的分子量适宜,分子量太大容易失去亲水效果,分子量太小又严重影响手感。
本发明进一步设置为:所述一氯单体、二氯单体、三氯单体通过以下步骤制备得到:
步骤a:制备分子量为5000~7000的中间体A;
步骤b:将中间体A在0~10℃温度下,用碱性催化剂控制pH在8~8.5,与三聚氯氰反应,得到粗品一氯单体;将中间体A在30~40℃温度下,用碱性催化剂控制pH在8.6~9.0,与三聚氯氰反应,得到粗品二氯单体;将中间体A在70~80℃温度下,用碱性催化剂控制pH在9.5~10.5,与三聚氯氰反应,得到粗品三氯单体;
步骤c:然后将得到的粗品一氯单体、二氯单体、三氯单体多次在乙醇和水的溶液中提纯,去除杂质,最后经过蒸馏得到纯品一氯单体、二氯单体、三氯单体。
通过采用上述技术方案,三聚氯氰中含有活性氯离子,而中间体A两端含有可反应的氨基,在碱性条件下三聚氯氰的氯离子和端氨基聚醚硅油的氨基很容易发生缩合反应,反应过程中掉下一个氯化氢,用碱中和而起到正向反应,促进达到所需要的产物。反应在不同碱度和不同温度下,得到不同的取代缩合物。而三聚氯氰的桥架结构,具有极佳的平面构型,所以具有更为优异的平滑性能。一氯单体、二氯单体、三氯单体分子量差别较大,所以可以在棉织物的内、中、外不同层面起作用,起到对棉织物更加优异的平滑柔软作用。
本发明进一步设置为:所述中间体A的制备方法包括以下步骤:
步骤a:将端环氧基硅油和聚醚胺按比例加入异丙醇中,搅拌混合均匀;
步骤b:控制温度在80~90℃下,回流反应5~7h,即得到端氨基嵌段硅油;
步骤c:将步骤b得到的端氨基嵌段硅油中按比例加入八甲基环四硅氧烷和催化剂氯铂酸,搅拌均匀;
步骤d:控制温度为90~100℃,进行扩链反应4~6h,得到中间体A;
步骤e:向步骤d中的中间体A中加入聚乙二醇,并在50~60℃下蒸馏出溶剂异丙醇。
通过采用上述技术方案,端环氧硅油和聚醚胺反应发生环氧基团和氨基的缩合反应,加入八甲基环四硅氧烷在溶剂和催化剂作用下进行扩链,反应如下:
分子结构中硅半结构基团增加,达到更滑软的作用。
一种用于棉织物的亲水有机硅整理剂的制备方法,包括以下步骤:
将纯品一氯产物、两氯产物、三氯产物按照比例混合后,再加入交联性单体、环保溶剂1,4-戊二醇和混合乳化剂,搅拌均匀后制得性能优异的高亲水有机硅整理剂。
与现有技术相比,本发明的有益效果是:
1、通过制备既含有氨基聚硅氧烷链段的有机硅整理剂,能赋予棉织物优异的耐洗性能、柔软、平滑、蓬松等手感,又含有氯基团,优先与棉织物反应,从而可以保留更多氨基和羟基,使得聚氧乙烯醚链段、氨基、羟基更多的暴露在织物表面起到高亲水作用。
2、通过一氯、二氯、三氯和交联剂单体的不同比例的复配可以满足不同颜色面料和不同染色深度的要求,可衍生出不同风格的织物手感整理效果。
具体实施方式
下面结合实施例,对本发明进行详细描述。
实施例1:
本发明公开的一种用于棉织物的亲水有机硅整理剂,包括以下重量百分比的组分制备得到:
交联性单体为分子量为1000的乙烯基硅油;
环保溶剂为1,4-戊二醇;
混合乳化剂为烷氧基化的聚乙烯亚胺和异构十醇聚氧乙烯醚,其中重量比为1.5∶1。
其中,一氯单体的结构式为式(a);
二氯单体的结构式为式(b);
三氯单体的结构式为式(c);
其中,
R为:
4≤a≤6,8≤b≤10,8≤n≤10,5≤x≤10,30≤y≤60。
一氯单体、二氯单体、三氯单体由包括以下重量百分比的组分制备得到:
所述碱性催化剂选用碳酸氢钠、碳酸钠或单乙醇胺中的一种或多种;
所述催化剂选用氯铂酸;
所述端环氧基硅油的结构简式为:
所述聚醚胺的结构简式为:
所述端环氧基硅油选用分子量为2218的端环氧基硅油,聚醚胺选用分子量为364的聚醚胺。
一种用于棉织物的亲水有机硅整理剂的制备方法,包括以下步骤:
S1:制备中间体A,包括以下步骤:
步骤a:将端环氧基硅油和聚醚胺按比例加入异丙醇中,搅拌混合均匀;
步骤b:控制温度在80℃下,回流反应5h,即得到端氨基嵌段硅油;
步骤c:将步骤b得到的端氨基嵌段硅油中按比例加入八甲基环四硅氧烷和催化剂氯铂酸,搅拌均匀;
步骤d:控制温度为100℃,进行扩链反应6h,得到中间体A;
步骤e:向步骤d中的中间体A中加入聚乙二醇,并在50℃下蒸馏出溶剂异丙醇;
S2:制备一氯单体、二氯单体、三氯单体,包括以下步骤:
步骤a:将中间体A在0℃温度下,用碳酸氢钠控制pH在8,与三聚氯氰反应,得到粗品一氯单体;将中间体A在30℃温度下,用碳酸钠控制pH在8.6,与三聚氯氰反应,得到粗品二氯单体;将中间体A在70℃温度下,用碳酸钠和单乙醇胺控制pH在9.5,与三聚氯氰反应,得到粗品三氯单体;
步骤b:然后将得到的粗品一氯单体、二氯单体、三氯单体在乙醇和水的溶液中进行5次提纯,去除杂质,最后经过蒸馏得到纯品一氯单体、二氯单体、三氯单体。
S3:将纯品一氯产物、两氯产物、三氯产物按照比例混合后,再添加乙烯基硅油、环保溶剂1,4-戊二醇和混合乳化剂,搅拌均匀后制得性能优异的高亲水有机硅整理剂。
实施例2~5与实施例1的区别在于整理剂中各组分按重量百分比计为下表。
实施例6~9与实施例1的区别在于制备一氯单体、二氯单体、三氯单体的原料按重量百分比计为下表。
实施例10~13与实施例1的区别在于乙烯基硅油、端环氧基硅油、聚醚胺的分子量计为下表。
实施例14~17与实施例1的区别在于步骤S1中的各个参数计为下表。
实施例18~21与实施例1的区别在于步骤S2中的各个参数计为下表。
对比例
对比例1为绍兴海成化工有限公司的型号为739B市售硅油;
对比例2为绍兴海成化工有限公司的型号为739H市售硅油。
检测方法
1.整理工艺:
所用织物:棉及其涤棉混纺织物
应用工艺流程:浸轧工作液(有机整理剂50g/L,轧余率70%)→焙烘(165℃×30s)→回潮24h→评价
将同一块布样剪开,然后经过水洗处理10次后→焙烘(165℃×30s)→回潮24h→再评价
2.应用性能测试
2.1手感评价:采用主观评定方法,主要通过手对织物的揉、挤、压、掐等,将织物的力学性能反应给大脑,大脑感知后的心理反应即为织物的基本手感,每块布样选用5名专业的人员评定感知分数,最终确认综合得分。10分表示手感最好,1分表示手感最差。
表1浸轧有机硅整理剂后烘干定型回潮后的手感评定表
表2经过洗涤10次后再烘干定型回潮后的手感评定表
从上述表格来看,实施例的各配方有机硅整理剂在初始阶段的手感可以达到甚至超越市售有机硅整理剂手感,并且经过10次洗涤以后的手感明显比市售有机硅整理剂相同处理后手感优异,说明实施例的有机硅整理剂的处理效果更长效,与织物的结合更牢固。
2.2亲水性评价:用滴管吸取清水后滴于有机硅整理后的布面上,测定多次水滴被完全吸收的过程时间的平均值来判定,时间越短亲水效果越好,时间越长亲水效果越差。
表1浸轧有机硅整理剂后烘干定型回潮后的亲水性能评定表
从上述表格来看,实施例的各配方有机硅整理剂比市售有机硅整理剂的亲水能力明显要好,和未处理的空白布样依旧存在差距,不过差距也较小,属于近似亲水效果。
以上所述仅是本发明的优选实施方式,本发明的保护范围并不仅局限于上述实施例,凡属于本发明思路下的技术方案均属于本发明的保护范围。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理前提下的若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (6)
3.根据权利要求2所述的一种用于棉织物的亲水有机硅整理剂,其特征在于:所述端环氧基硅油选用分子量为2218-2774的端环氧基硅油,聚醚胺选用分子量为364-654的聚醚胺。
4.根据权利要求2所述的一种用于棉织物的亲水有机硅整理剂,其特征在于:所述一氯单体、二氯单体、三氯单体通过以下步骤制备得到:
步骤a:制备分子量为5000~7000的中间体A;
步骤b:将中间体A在0~10℃温度下,用碱性催化剂控制pH在8~8.5,与三聚氯氰反应,得到粗品一氯单体;将中间体A在30~40℃温度下,用碱性催化剂控制pH在8.6~9.0,与三聚氯氰反应,得到粗品二氯单体;将中间体A在70~80℃温度下,用碱性催化剂控制pH在9.5~10.5,与三聚氯氰反应,得到粗品三氯单体;
步骤c:然后将得到的粗品一氯单体、粗品二氯单体、粗品三氯单体多次在乙醇和水的溶液中提纯,去除杂质,最后经过蒸馏得到纯品一氯单体、纯品二氯单体、纯品三氯单体。
5.根据权利要求4所述的一种用于棉织物的亲水有机硅整理剂,其特征在于:所述中间体A的制备方法包括以下步骤:
步骤a:将端环氧基硅油和聚醚胺按比例加入异丙醇中,搅拌混合均匀;
步骤b:控制温度在80~90℃下,回流反应5~7h,即得到端氨基嵌段硅油;
步骤c:将步骤b得到的端氨基嵌段硅油中按比例加入八甲基环四硅氧烷和6~8ppm氯铂酸,搅拌均匀;
步骤d:控制温度为90~100℃,进行扩链反应4~6h,得到中间体A;
步骤e:向步骤d中的中间体A中加入聚乙二醇,并在50~60℃下蒸馏出溶剂异丙醇。
6.一种根据权利要求1所述的用于棉织物的亲水有机硅整理剂的制备方法,其特征在于:包括以下步骤:
将纯品一氯单体、纯品二氯单体、纯品三氯单体按照比例混合后,再添加分子量为1000~2000的乙烯基硅油、环保溶剂1,4-戊二醇和混合乳化剂,搅拌均匀后制得性能优异的高亲水有机硅整理剂。
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