CN115354417A - 一种含抗静电剂的化纤纺丝油剂的制备方法 - Google Patents
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Abstract
本发明公开了一种含抗静电剂的化纤纺丝油剂的制备方法。本发明以乙二醇丁醚、环氧氯丙烷及十六烷基二甲基叔胺为原料,合成了抗静电剂脂肪醇醚季铵盐。季铵盐表面活性剂的亲脂基团面向纤维表面,亲水基团面向空气,可以与水缔合提高表面电导率,迅速泄漏电荷,达到抗静电效果。同时正电荷的脂肪醇醚季铵盐,对带负电荷的化纤纤维有很强的吸附能力,具有优良的抗静电性能和一定的耐洗涤性能。本发明的化纤纺丝油剂可以很好地调剂化学纤维的摩擦,保护纤维、防止纤维对设备的磨损和锈蚀,克服油剂对高速纺丝的丝素表面光滑度不够等问题。
Description
技术领域
本发明涉及一种含抗静电剂的化纤纺丝油剂的制备方法。
背景技术
纺丝油剂是合成纤维织造和加工过程中必要的添加剂,可以减小纤维与纤维之间、纤维与金属之间的摩擦系数,减少摩擦产生的静电,使纤维呈簇状、光滑且细密,满足纤维加工后的相关工艺的需要。在纺丝过程中,较低表面张力的油剂能快速均匀地分布在纤维表面。一般纺丝油剂的主要作用是使纤维能顺利卷绕,丝筒成型,在拉伸过程中保证拉伸的正常。所以助剂还必须具有良好的抗静电性能和适度的润湿性及平滑性、耐热性及防结焦等性能。近年来,随着高速纺丝、细旦纤维等的发展,对纺丝油剂提出了更高的要求。目前的季铵盐型抗静电剂一般采用季铵盐型阳离子表面活性剂,季铵盐型阳离子表面活性剂具有高表面活性、强协同效应、良好的去污和抗菌能力等多种优点,被用于新材料制造、生命科学和生物技术、纳米材料等高新技术领域。与传统的单体(单链)季铵盐相比,多阳离子表面活性剂由多个单链离子表面活性剂通过间隔基连接组成,表现出更高的表面活性,被广泛用作有效的乳化剂、杀菌剂、分散剂和消泡剂;季铵盐抗静电剂的活性离子带正电荷,对带负电荷的化纤有很强的吸附能力,具有优良的抗静电性能和一定的耐洗涤性能。其结构式如下:
其中R为十六烷基二甲基叔胺。
但是这种材料存在效果不能满足要求,亲油性过强的缺陷。
因此,生产出一种高效抗静电纺丝油剂有很大的市场需求。
发明内容
发明目的:针对上述现有技术的不足,本发明提供了一种抗静电效果好的化纤纺丝油剂的制备方法。
本发明所述的化纤纺丝油剂的制备包括以下步骤:
S10、以乙二醇丁醚和环氧氯丙烷为原料,加入催化剂,在50~100℃下、反应1~5小时后,得到含有烷氧基氯代甘油醚的混合物A;
S20、取混合物A加入去离子水洗涤分液,将下层液体加入无水硫酸钠去除水分,得到烷氧基氯代甘油醚;
S30、将得到的烷氧基氯代甘油醚与十六烷基二甲基叔胺混合,以水作溶剂,在50~100℃下反应3~9小时,得到含有脂肪醇醚季铵盐的混合物B;
S40、取混合物B用氯仿溶解,加入无水硫酸钠除水,过滤后将滤液旋蒸去除氯仿,用乙酸乙酯-丙酮混合溶剂重结晶,干燥后得到脂肪醇醚季铵盐;
S50、将天然油脂、合成油酯与脂肪醇醚季铵盐,在40-70℃时混合均匀;缓慢加入水,得到乳液状液体;加入聚乙二醇脂肪酸酯,搅拌均匀,乳液状液体变为透明状,继续搅拌20-30min;加入微乳平衡调节剂、杀菌防腐剂,搅拌均匀即可得到浅黄色澄清透明的油液。
进一步的,在步骤S10中,所述乙二醇丁醚与环氧氯丙烷的摩尔比为1:1~3。
进一步的,在步骤S10中,所述催化剂与乙二醇丁醚的摩尔比为1:100~500。
进一步的,在步骤S30中,所述烷氧基氯代甘油醚与十六烷基二甲基叔胺的摩尔比为3~1:1。
进一步的,在步骤S30中,所述溶剂水的用量为1~5毫升/克烷氧基氯代甘油醚。
进一步的,在步骤S50中,所述天然油脂为椰子油、棕榈油、大豆油、花生油、玉米油、蓖麻油、菜籽油中的一种或几种。
进一步的,在步骤S50中,所述合成油酯为:季戊四醇四油酸酯、聚甘油-2硬脂酸酯、聚甘油-2异硬脂酸酯、聚甘油-2月桂酸酯、三羟甲基丙烷油酸酯、新戊二醇油酸酯中的一种或几种。
进一步的,在步骤S50中,所述聚乙二醇脂肪酸酯是PEG200ML、PEG400ML、PEG600ML、EL-10、EL-20、EL-40、EL-60、EL-90、HEL-10、HEL-20、HEL-90、PEG600DS中的两种或几种。
进一步的,在步骤S50中,所述微乳平衡调节剂是三乙醇胺、二乙醇胺、单乙醇胺、二甲基乙醇胺、二乙基乙醇胺、二丁基胺、二己基乙醇胺、三正丁胺、异丁醇胺中的一种或几种。
进一步的,在步骤S50中,所述杀菌防腐剂是1,2-苯并异噻唑啉-3-酮、5-氯-2-甲基-4-异噻唑啉-3-酮、2-甲基-4-异噻唑啉-3-酮中的一种。
本发明的有益效果:本发明与现有技术相比,本发明以乙二醇丁醚、环氧氯丙烷及十六烷基二甲基叔胺为原料,合成了抗静电剂脂肪醇醚季铵盐。季铵盐表面活性剂的亲脂基团面向纤维表面,亲水基团面向空气,可以与水缔合提高表面电导率,迅速泄漏电荷,达到抗静电效果。同时正电荷的脂肪醇醚季铵盐,对带负电荷的化纤纤维有很强的吸附能力,具有优良的抗静电性能和一定的耐洗涤性能。本发明的化纤纺丝油剂可以很好地调剂化学纤维的摩擦,保护纤维、防止纤维对设备的磨损和锈蚀,克服油剂对高速纺丝的丝素表面光滑度不够等问题。
附图说明
图1是本发明实施例中制备的脂肪醇醚季铵盐的红外光谱图。
图2是本发明实施例中制备的脂肪醇醚季铵盐的质谱图;其中,m/z=444是[M+H]+的峰,为产物峰。
图3是本发明实施例中制备的脂肪醇醚季铵盐与十二烷基三甲基氯化铵(DTAC)的质量分数对静电压的影响。
图4是本发明实施例中制备的脂肪醇醚季铵盐与DTAC的质量分数对静态半周期的影响。
具体实施方式
为了更清楚地说明本发明的技术方案,下面结合附图对本发明的技术方案做进一步的详细说明:
一种含抗静电剂的化纤纺丝油剂的制备方法,具体操作步骤如下:
S10、以乙二醇丁醚和环氧氯丙烷为原料,加入催化剂,在70~90℃下、反应2~4小时后,得到包括烷氧基氯代甘油醚和催化剂的混合物A;
S20、取混合物A加入去离子水洗涤分液,将下层液体加入无水硫酸钠去除水分,得到烷氧基氯代甘油醚;
S30、将得到的烷氧基氯代甘油醚与十六烷基二甲基叔胺混合,以水作溶剂,在70~90℃下反应5~7小时,得到包括脂肪醇醚季铵盐和少量没有反应完全的烷氧基氯代甘油醚与十六烷基二甲基叔胺的混合物B;
S40、取混合物B用氯仿溶解,加入无水硫酸钠除水,过滤后将滤液旋蒸去除氯仿,用乙酸乙酯-丙酮混合溶剂重结晶,干燥后得到脂肪醇醚季铵盐;
S50、将天然油脂、合成油脂与脂肪醇醚季铵盐,在50℃时混合均匀;缓慢加入水,得到乳液状液体;加入聚乙二醇脂肪酸酯,搅拌均匀,乳液状液体变为透明状,继续搅拌20min;加入微乳平衡调节剂、杀菌防腐剂,搅拌均匀即可得到浅黄色澄清透明的油液。
其中,在步骤S10中,所述乙二醇丁醚与环氧氯丙烷的摩尔比为1:1~2。
其中,在步骤S10中,所述催化剂与乙二醇丁醚的摩尔比为1:100~300。
其中,在步骤S30中,所述烷氧基氯代甘油醚与十六烷基二甲基叔胺的摩尔比为2~1:1。
其中,在步骤S30中,所述溶剂水的用量为2~4毫升/克烷氧基氯代甘油醚。
其中,在步骤S50中,所述天然油脂为椰子油、棕榈油、大豆油、花生油、玉米油、蓖麻油、菜籽油中的一种或几种。
其中,在步骤S50中,所述合成油脂为:季戊四醇四油酸酯、聚甘油-2硬脂酸酯、聚甘油-2月桂酸酯、三羟甲基丙烷油酸酯、新戊二醇油酸酯中的一种或几种。
其中,在步骤S50中,所述聚乙二醇脂肪酸酯是PEG200ML、PEG400ML、PEG600ML、EL-10、EL-20、EL-40、EL-90、HEL-20、HEL-90、PEG600DS中的两种或几种。
其中,在步骤S50中,所述微乳平衡调节剂是三乙醇胺、二乙醇胺、单乙醇胺、二甲基乙醇胺、二乙基乙醇胺、二己基乙醇胺、异丁醇胺中的一种或几种。
其中,在步骤S50中,所述杀菌防腐剂是1,2-苯并异噻唑啉-3-酮、5-氯-2-甲基-4-异噻唑啉-3-酮、2-甲基-4-异噻唑啉-3-酮中的一种。
实施例1:
将乙二醇丁醚和环氧氯丙烷按摩尔比1:1加入催化剂,在70℃下、反应2小时后,得到含有烷氧基氯代甘油醚的混合物A。取混合物A加入去离子水洗涤分液,将下层液体加入无水硫酸钠去除水分,得到烷氧基氯代甘油醚。
将得到的烷氧基氯代甘油醚与十六烷基二甲基叔胺按摩尔比2:1混合,加入30mL水,在70℃下反应5小时,得到含有脂肪醇醚季铵盐的混合物B。取混合物B用氯仿溶解,加入无水硫酸钠除水,过滤后将滤液旋蒸去除氯仿,用乙酸乙酯-丙酮混合溶剂重结晶,干燥后得到脂肪醇醚季铵盐。
将质量百分比12%的椰子油、17%的季戊四醇四油酸酯、10%的三羟甲基丙烷硬脂酸酯与3%的脂肪醇醚季铵盐,在50℃时混合均匀;缓慢加入水,得到乳液状液体;加入15%的PEG400DO与15%的PEG600ML,搅拌均匀,乳液状液体变为透明状,继续搅拌20min;加入2%的三乙醇胺、1%的2-甲基-4-异噻唑啉-3-酮,搅拌均匀即可得到浅黄色澄清透明的油液。
用上述油剂浸泡涤纶布12h并烘干,测得涤纶布的静电压为11V,静态半周期为0.08s。
实施例2:
将乙二醇丁醚和环氧氯丙烷按摩尔比1:1.5加入催化剂,在80℃下、反应3小时后,得到含有烷氧基氯代甘油醚的混合物A。取混合物A加入去离子水洗涤分液,将下层液体加入无水硫酸钠去除水分,得到烷氧基氯代甘油醚。
将得到的烷氧基氯代甘油醚与十六烷基二甲基叔胺按摩尔比1.5:1混合,加入30mL水,在80℃下反应6小时,得到含有脂肪醇醚季铵盐的混合物B。取混合物B用氯仿溶解,加入无水硫酸钠除水,过滤后将滤液旋蒸去除氯仿,用乙酸乙酯-丙酮混合溶剂重结晶,干燥后得到脂肪醇醚季铵盐。
将质量百分比12%的棕榈油、17%的季戊四醇四油酸酯、10%的聚甘油-2硬脂酸酯与3%的脂肪醇醚季铵盐,在50℃时混合均匀;缓慢加入水,得到乳液状液体;加入15%的PEG200ML与15%的EL-10,搅拌均匀,乳液状液体变为透明状,继续搅拌20min;加入2%的二乙醇胺、1%的1,2-苯并异噻唑啉-3-酮,搅拌均匀即可得到浅黄色澄清透明的油液。
用上述油剂浸泡涤纶布12h并烘干,测得涤纶布的静电压为9V,静态半周期为0.07s。
实施例3:
将乙二醇丁醚和环氧氯丙烷按摩尔比1:2加入催化剂,在90℃下、反应4小时后,得到含有烷氧基氯代甘油醚的混合物A。取混合物A加入去离子水洗涤分液,将下层液体加入无水硫酸钠去除水分,得到烷氧基氯代甘油醚。
将得到的烷氧基氯代甘油醚与十六烷基二甲基叔胺按摩尔比1:1混合,加入30mL水,在90℃下反应7小时,得到含有脂肪醇醚季铵盐的混合物B。取混合物B用氯仿溶解,加入无水硫酸钠除水,过滤后将滤液旋蒸去除氯仿,用乙酸乙酯-丙酮混合溶剂重结晶,干燥后得到脂肪醇醚季铵盐。
将质量百分比12%的玉米油、17%的新戊二醇油酸酯、10%的聚甘油-2硬脂酸酯与3%的脂肪醇醚季铵盐,在50℃时混合均匀;缓慢加入水,得到乳液状液体;加入15%的PEG600DS与15%的HEL-20,搅拌均匀,乳液状液体变为透明状,继续搅拌20min;加入2%的二甲基乙醇胺、1%的5-氯-2-甲基-4-异噻唑啉-3-酮,搅拌均匀即可得到浅黄色澄清透明的油液。
用上述油剂浸泡涤纶布12h并烘干,测得涤纶布的静电压为13V,静态半周期为0.11s。
最后,应当理解的是,本发明中所述实施例仅用以说明本发明实施例的原则;其他的变形也可能属于本发明的范围;因此,作为示例而非限制,本发明实施例的替代配置可视为与本发明的教导一致;相应地,本发明的实施例不限于本发明明确介绍和描述的实施例。
Claims (10)
1.一种含抗静电剂的化纤纺丝油剂的制备方法,其特征在于,具体操作步骤如下:
S10、以乙二醇丁醚和环氧氯丙烷为原料,加入催化剂,在50~100℃下、反应1~5小时后,得到含有烷氧基氯代甘油醚的混合物A;
S20、取混合物A加入去离子水洗涤分液,将下层液体加入无水硫酸钠去除水分,得到烷氧基氯代甘油醚;
S30、将得到的烷氧基氯代甘油醚与十六烷基二甲基叔胺混合,以水作溶剂,在50~100℃下反应3~9小时,得到含有脂肪醇醚季铵盐的混合物B;
S40、取混合物B用氯仿溶解,加入无水硫酸钠除水,过滤后将滤液旋蒸去除氯仿,用乙酸乙酯-丙酮混合溶剂重结晶,干燥后得到脂肪醇醚季铵盐;
S50、将天然油脂与合成油脂与脂肪醇醚季铵盐,在40-70℃时混合均匀;缓慢加入水,得到乳液状液体;加入聚乙二醇脂肪酸酯,搅拌均匀,乳液状液体变为透明状,继续搅拌20-30min;加入微乳平衡调节剂、杀菌防腐剂,搅拌均匀即可得到浅黄色澄清透明的油液。
2.根据权利要求1所述的一种脂肪醇醚季铵盐的制备方法,其特征在于,在步骤S10中,所述乙二醇丁醚与环氧氯丙烷的摩尔比为1:1~3。
3.根据权利要求1所述的一种脂肪醇醚季铵盐的制备方法,其特征在于,在步骤S10中,所述催化剂与乙二醇丁醚的摩尔比为1:100~500。
4.根据权利要求1所述的一种脂肪醇醚季铵盐的制备方法,其特征在于,在步骤S30中,所述烷氧基氯代甘油醚与十六烷基二甲基叔胺的摩尔比为3~1:1。
5.根据权利要求1所述的一种脂肪醇醚季铵盐的制备方法,其特征在于,在步骤S30中,所述溶剂水的用量为1~5毫升/克烷氧基氯代甘油醚。
6.根据权利要求1所述的一种脂肪醇醚季铵盐的制备方法,其特征在于,在步骤S50中,所述天然油脂为椰子油、棕榈油、大豆油、花生油、玉米油、蓖麻油、菜籽油中的一种或几种。
7.根据权利要求1所述的一种脂肪醇醚季铵盐的制备方法,其特征在于,在步骤S50中,所述合成油脂为:季戊四醇四油酸酯、聚甘油-2硬脂酸酯、聚甘油-2异硬脂酸酯、聚甘油-2月桂酸酯、三羟甲基丙烷油酸酯、新戊二醇油酸酯中的一种或几种。
8.根据权利要求1所述的一种脂肪醇醚季铵盐的制备方法,其特征在于,在步骤S50中,所述聚乙二醇脂肪酸酯是PEG200ML、PEG400ML、PEG600ML、EL-10、EL-20、EL-40、EL-60、EL-90、HEL-10、HEL-20、HEL-90、PEG600DS中的两种或几种。
9.根据权利要求1所述的一种脂肪醇醚季铵盐的制备方法,其特征在于,在步骤S50中,所述微乳平衡调节剂是三乙醇胺、二乙醇胺、单乙醇胺、二甲基乙醇胺、二乙基乙醇胺、二丁基胺、二己基乙醇胺、三正丁胺、异丁醇胺中的一种或几种。
10.根据权利要求1所述的一种脂肪醇醚季铵盐的制备方法,其特征在于,在步骤S50中,所述杀菌防腐剂是1,2-苯并异噻唑啉-3-酮、5-氯-2-甲基-4-异噻唑啉-3-酮、2-甲基-4-异噻唑啉-3-酮中的一种。
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