CN116043558A - 一种生物基柔软凉感抗菌整理剂及其制备方法和应用 - Google Patents
一种生物基柔软凉感抗菌整理剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于纺织工业印染生产中纺织品印染技术领域,尤其是涉及一种生物基柔软凉感抗菌整理剂及其制备方法和应用。在反应中加入生物基有机脂肪酸、催化剂和有机胺混合,进行脱水反应,再加入季铵化试剂,进行季铵化反应,再与生物基乳化剂、消泡剂复配成阳离子型柔软剂;加入天然植物抗菌剂,对织物进行抗菌整理,水洗后,对金黄色葡萄菌、肺炎菌、大肠杆菌的抗菌率均能达到95%以上,有很好的广谱抗菌耐洗性;最后产品中加入了天然凉感整理剂,赋予面料柔滑冰爽的效果。用该整理剂利用非离子表面活性剂和阴离子表面活性剂的协同效应和增效作用,应用效果好,织物色变小,亲水性能和抗静电性能好,且无细胞毒性耐药性,对皮肤无刺激。
Description
技术领域
本发明属于纺织工业印染生产中纺织品印染技术领域,尤其是涉及一种生物基柔软凉感抗菌整理剂及其制备方法和应用。
背景技术
随着生活质量的不断提高,人们对服装的穿着舒适度和特种功能的要求越来越高,纺织品在加工或日常使用中,经多次加工、洗涤处理后手感会变得粗糙,一般合成纤维织物手感更差。为了使织物具有柔软、凉爽、顺滑、舒适的手感,和抗菌功能,就需要对其进行整理,目前应用广泛的是用柔软剂、凉感剂和抗菌剂进行整理。因此后整理是纺织印染加工中提高产品质量,增加产品附加价值必不可少的一种重要工序。
阳离子型柔软剂是使用范围最广泛的一类,包含季铵盐型、有机硅树脂型、酯季铵盐型等。此外,具有良好手感的有机硅整理剂由于使用原料中含有硅氧烷环体,其在使用时存在一定的安全风险,同时对印染厂使用过程中回收造成一定困难,故现在市场上需要不含硅且手感较好的柔软剂;而同时,常见的无硅柔软剂的生物降解性差并且黄变严重,随着公共意识及环保质量的要求的提高,此类产品也逐渐不能满足社会发展的需求。
纤维属于多孔性材料,叠加编织后又会形成无数空隙的多层体,因此织物较容易吸附菌类,并会迅速繁殖。抗菌整理是指在纤维制品上用具有抗菌防臭作用的试剂进行处理,赋予抗菌防毒性能以防止纤维因微生物引起的恶化,色素的附着,袜子和内衣发生恶臭等。理想的抗菌剂必须是安全、低毒的,具有广谱抗菌性,抗菌作用大,用量小,不引起皮肤过敏反应或损伤,不能影响织物的服用性能,对纺织品性能和外观影响小,不影响通常的纺织品染整加工。
很多纺织品直接接触人体皮肤,因而抗菌剂务必具有安全性、无毒性,对身体无刺激性。现阶段,在纺织品抗菌剂的选用中,仍以有机抗菌剂为主导、季铵盐类、聚六甲基双胍盐酸盐等有机抗菌剂,其效果优良,但毒副作用比较大,耐用性较弱,而且非常容易造成微生物的抗药性等,限制了其在直接接触人体皮肤的纺织品上的应用。
发明内容
本发明的目的在于提供一种生物基柔软凉感抗菌整理剂及其制备方法和应用,以解决上述问题,将该织物整理剂按照设定的整理工艺作用在织物上,可达到良好的柔软平滑性、凉爽的触感、广谱抗菌性和耐洗性,对纺织品的损伤小,且织物的颜色、状态等几乎无变化;同时该织物整理剂来源天然,可降解对环境无污染,整理后的织物可直接接触人体,无细胞毒性,对皮肤无刺激,无耐药性,适合广泛应用。
为达此目的,本发明采用以下技术方案:
一种生物基柔软凉感抗菌整理剂,该柔软凉感抗菌整理剂的原料包括生物基有机脂肪酸、催化剂、有机胺、季铵化试剂、生物基乳化剂、天然油脂磺化油、天然植物抗菌剂、多元醇、聚氨酯、天然凉感整理剂、消泡剂和水;
以该柔软凉感抗菌整理剂的原料的总质量为100%计算,各组份的质量百分含量为:
其中,所述的生物基有机脂肪酸为C12-C18的饱和脂肪酸、妥尔油脂肪酸、精制妥尔油中的任意一种或任意组合;
所述催化剂为次亚磷酸、对甲苯磺酸中的任意一种或任意组合;
所述的有机胺为二乙烯三胺、三乙醇胺和N,N-双(3-氨丙基)甲胺中的任意一种或任意组合;
所述的季铵化试剂为碳酸二甲酯、硫酸二甲酯、碳酸二乙酯和硫酸二乙酯中的任意一种或任意组合;
所述的生物基乳化剂为腰果酚聚氧乙烯醚NSS 1305、NSS 1305A、NSS1308中的任意一种或任意组合;
所述的天然油脂磺化油为天然磺化菜籽油、天然磺化蓖麻油、硫酸化天然牛蹄油中的至少一种或任意组合;
所述的天然植物抗菌剂为除虫菊酯、柠檬桉叶油、日本扁柏提取物、香叶天竺葵提取物中的至少一种或任意组合;
所述的多元醇为1,3-丁二醇、乙二醇、丙二醇中的至少一种或任意组合;
所述聚氨酯为乙烯基聚氨酯乳液、多异氰酸酯乳液、封闭型聚氨酯乳液中的至少一种或任意组合;
所述天然凉感整理剂木糖醇、薄荷油、赤糖醇、蚕丝素蛋白、红色线反射陶瓷的至少一种或任意组合;
所述的消泡剂为聚氧丙基聚氧乙基甘油醚、聚醚改性聚硅氧烷类中的任意一种或任意组合。
一种生物基柔软凉感抗菌整理剂的制备方法,其中包括以下步骤:
步骤一、在反应釜1中加入生物基有机酸,催化剂和有机胺,开始脱水反应,反应得到初始产物;
步骤二、向步骤一得到的初始产物中加入季铵化试剂,开始季铵化反应;
步骤三、待步骤二所述季铵化反应结束后,加入生物基乳化剂,得到所述生物基阳离子整理剂;
步骤四、将天然植物抗菌剂、多元醇和天然油脂磺化油加入混合罐1中,搅拌至混合均匀;
步骤五、将水和聚氨酯加入混合罐1中,搅拌至混合均匀,得到所述生物基抗菌剂;
步骤六、将混合罐1的物料加入到反应釜1中,搅拌至混合均匀;
步骤七、随后将天然凉感整理剂加入反应釜1中,搅拌至混合均匀;
步骤八、最后将消泡剂投入到反应釜1中,搅拌均匀即可,过滤得到生物基柔软凉感抗菌整理剂。
所述的步骤一中,在N2氛围下,先将生物基有机酸加热熔融,温度为120-180℃,搅拌速度为20-40rpm;熔融后加入催化剂,搅拌均匀;随后加入有机胺,升温至180-230℃开始脱水反应,反应时间为3-10小时;在真空条件下继续反应0.5-3小时,得到初始产物,所述初始产物是单酯和双酯的混合物;
通过生物基有机酸和有机胺的脱水反应,生成带有亲水链段结构长碳链酯胺,确保了所制备得到的生物基柔软凉感抗菌整理剂的柔软性能,从而增强聚合物的亲水性能和抗静电性能;
通入N2气体可以将脱水反应产生的水带走,有利于反应的进行,同时由于N2气体的通入,能使原料在高温下不被空气氧化,从而确保了产品的色泽;
所述的步骤二中,降温至70-90℃,缓慢加入季铵化试剂,控制加料时间为1-3小时,需开启冷却水控制反应温度,加完后继续持温反应1-3小时;
发生季铵化反应,生成酯基季铵盐,提高了产物的稳定性和抗黄变效果,同时其亲水性得到进一步提升;
所述的步骤三中,降温至70-80℃,加入生物基乳化剂,搅拌均匀,降温至45℃以下;
所述步骤四中,将天然植物抗菌剂、多元醇和天然油脂磺化油混合,搅拌10-45min,搅拌速度为20-40rpm;
所述步骤五中,在步骤四得到的混合物中加入水和聚氨酯,搅拌10-45min;
所述步骤六中,将步骤三得到的混合物和步骤五得到的混合物进行混合,搅拌30-60min,搅拌速度为20-40rpm;
所述步骤七中,将步骤六得到的混合物中加入天然凉感整理剂,搅拌10-45min;
所述步骤八中,将步骤七得到的混合物中加入消泡剂,搅拌10-30min,过滤得到所述生物基柔软凉感抗菌整理剂;
优选地,所述的生物基有机脂肪酸为C12-C18的饱和脂肪酸;
优选地,所述妥尔油脂肪酸为ALTAPYNE 1483、HARTALL FA-1和L1-C中的任意一种或任意组合,优选ALTAPYNE 1483;
优选地,所述催化剂为次亚磷酸、对甲苯磺酸中的任意一种或任意组合,优选次亚磷酸;
所述的催化剂为0.02%-0.2%,当催化剂低于0.02%时,反应速度缓慢,升温保温时间加长,容易发生爆聚;当催化剂大于0.2%时,反应速度太快,不好控制,反应时容易产生爆聚。
优选地,所述有机胺为所述的有机胺为二乙烯三胺、三乙醇胺和N,N-双(3-氨丙基)甲胺中的任意一种或任意组合;
所述生物基有机酸与所述有机胺的摩尔比为(1-3)∶1。在该摩尔比范围内,生物基有机酸上的羧基能和足量的有机胺上的氨基或羟基发生脱水反应,合成了不含三酯的酯铵,保证合成长碳链结构的单酯和双酯混合物,这使后续生成的酯基季铵盐的活性更强。
优选地,所述的季铵化试剂为碳酸二甲酯、硫酸二甲酯、碳酸二乙酯和硫酸二乙酯中的任意一种或任意组合,优选硫酸二甲酯;
所述季铵化反应,聚合物上氨基的氢离子被取代,季铵结构上没有氢,形成了阳离子表面活性剂,从而可以进一步提高纺织物的亲水性和渗透性;而且所述酯基季铵盐的稳定性好,具有良好的抗黄变性能和优异的生物降解性
优选地,所述的生物基乳化剂为腰果酚聚氧乙烯醚NSS 1305、NSS 1305A、NSS1308中的任意一种或任意组合;
优选地,所述的天然油脂磺化油为天然磺化菜籽油、天然磺化蓖麻油、硫酸化天然牛蹄油中的至少一种或任意组合,优选天然磺化菜籽油;
所述天然油脂磺化油选择5%-10%的加入量,在此范围内,柔软凉感抗菌整理剂的稳定性不会受到明显影响。
优选地,所述的天然植物抗菌剂为除虫菊酯、柠檬桉叶油、日本扁柏提取物、香叶天竺葵提取物的至少一种或任意组合,优选除虫菊酯和柠檬桉叶油组合;
所述除虫菊酯为质量百分含量为50%的油溶性除虫菊酯;
所述柠檬桉叶油为澄清液体,柠檬桉叶油中含有的含有香茅醛、香茅醇、牻牛儿醇、异胡薄荷醇、1,8-桉油素和愈创木醇成分中,香茅醛的质量百分含量为65%-80%;
优选地,所述的多元醇为1,3-丁二醇、乙二醇、丙二醇中的至少一种或任意组合,优选1,3-丁二醇;
优选地,所述聚氨酯为乙烯基聚氨酯乳液、多异氰酸酯乳液、封闭型聚氨酯乳液中的至少一种或任意组合,优选封闭型异氰酸酯;
所述封闭型异氰酸酯用量0.1%-3%,优选范围为0.5%-2%;其可与纤维发生反应,生成共价键结合,使抗菌剂和凉感剂更好与织物结合,提高整理后织物的耐洗性能;
优选地,所述天然凉感整理剂为木糖醇、薄荷油、赤糖醇、蚕丝素蛋白、红色线反射陶瓷的至少一种或任意组合,优选木糖醇和薄荷油组合FINFOCECCL;
所述的FINFOCE CCL是一种含有木糖醇和薄荷油的纳米微胶凉感整理剂,可通过摩擦等方式释放清凉感觉,有效成分质量百分含量为10%-20%;
优选地,所述的消泡剂为聚氧丙基聚氧乙基甘油醚、聚醚改性聚硅氧烷类中的任意一种或任意组合,优选聚醚改性聚硅氧烷CD-1116M。
所述CD-1116M能够在高温起泡体系中快速的渗透到泡沫内部,破坏泡沫的稳定性,从而达到消泡的效果;
优选地,所述步骤一中,脱水反应温度为180-200℃,反应时间为3-5小时。
一种生物基柔软凉感抗菌整理剂的应用,将生物基柔软凉感抗菌整理剂用于纺织物的后整理,使用的工艺为一浴两步法,包括如下步骤:
S1.织物柔软凉感抗菌整理液的调配:柔软凉感抗菌整理剂溶液浓度为50-100g/L,加水溶解均匀配成工作液;
S2.浸轧工作液:将织物在上述工作液中浸轧处理,带液率为60-80%;
S3.烘干:在100-110℃温度条件下60-120秒;
S4.定型:在130-140℃温度条件下60-90秒;
优选地,所述S2中,浸轧处理为三浸三轧,轧辊压力为0.15-0.25Mpa。
优选地,所述织物为全棉织物、棉及聚酰胺纤维的混织物、棉及聚酯纤维的混织物、天丝的至少一种,优选全棉梭织布。
一种生物基柔软凉感抗菌整理剂,采用本发明所述的原料和制备方法制备而成。
一种生物基柔软凉感抗菌整理剂的应用,其中,将本发明所述的生物基柔软凉感抗菌整理剂或者本发明任意方法制备得到的生物基柔软凉感抗菌整理剂用于纺织物的后整理。
有益效果
(1)本发明先采用生物基有机酸为主体进行反应,极大降低了化石原料的消耗,提高产品的生物降解性及产品附加价值。首先,采用的饱和脂肪酸为硬脂酸,即C12-C18的饱和脂肪酸,是自然界广泛存在的一种脂肪酸,目前国内生产的硬脂酸绝大多数企业都是从国外进口棕榈油,进行加氢变成硬化油,然后水解蒸馏得到硬脂酸,来源天然;其次,采用的妥尔油脂肪酸源于妥尔油,其加工利用是循环经济的重要组成部分,涉及到森林资源的可持续循环利用,对生态环境有较大的联动关系,具有较大的经济效益和社会效益。将其通过改性,制成性能合适的纺织助剂原料,此类纺织原材料的低碳化及循环利用,为纺织产业绿色低碳可持续发展提供了强有力的支撑。
(2)本发明制备方法中进行季铵化反应,提高了产品的亲水性和渗透性;采用生物基乳化剂,提升产品的亲水性和渗透性的同时,不产生有毒有害物质,以免增加污水处理压力。本发明制备的生物基柔软凉感抗菌整理剂用于纺织物整理时,可有效提升纺织物的手感、柔软性能、色牢性能以及抗黄效果;同时还可在纺织物上形成分子通道,使得静电可以迅速转移,从而提升纺织物的抗静电性能。
(3)本发明加入了天然油脂磺化油,这是一种以天然油脂为主要原料,采用三氧化硫气体磺化工艺进行改性,再与其他必要组分复配而成的阴离子型磺化油加脂剂,是一种优良的阴离子表面活性剂,提高亲水性能和抗静电性能;可减少织物间,织物与机器之间的摩擦作用,防止织物在浴中造成绳状皱纹,或受到擦伤形成色斑及发毛和“鸡爪花”现象。
(4)本发明纺织抗菌整理剂创新性地将天然原料作用于织物整理中,抗菌效果优良,具有良好的广谱抗菌性,经过本发明所述的织物抗菌整理剂的抗菌处理后,对各类常见菌种的抗菌率均能达95%以上。
(5)本发明纺织抗菌整理剂采用水性聚氨酯,通过其与纤维发生反应,生成共价键结合,使织物的抗菌凉感整理具有较好的耐洗性,且不影响后续的防水防油整理效果,具有广泛的应用性。
(6)本发明选用的凉感整理剂FINFOCE CCL是一种含有木糖醇和薄荷油的纳米微胶囊,可通过摩擦等方式释放清凉感觉,香味纯正,芬芳宜人,保香性强,留香持久,对人体无害,对皮肤无刺激,无过敏反应。
(7)本发明中采用的生物基有机脂肪酸、生物基乳化剂、天然油脂磺化油、天然植物抗菌剂和天然凉感整理剂均是来源于天然,无毒无害,生物降解迅速彻底的产品,对环境无污染,减少了印染前处理工艺的污水排放;同时,产品作用温和,纺织品经处理后损伤小。实现产业的绿色可持续发展。
(8)本发明的生物基柔软凉感抗菌整理剂及其应用,采用了一浴两步法一道工序实现了柔软抗菌凉感三种后整理效果,缩短了传统工艺流程,降低了生产能耗和成本。
(9)本发明属于纺织工业印染生产中纺织品印染技术领域,尤其是涉及一种生物基柔软凉感抗菌整理剂及其制备方法和应用。在本发明中,首先,在反应中加入生物基有机脂肪酸、催化剂和有机胺混合,进行脱水反应,再加入季铵化试剂,进行季铵化反应,再与生物基乳化剂、消泡剂复配成阳离子型柔软剂;加入天然植物抗菌剂,对织物进行抗菌整理,水洗50次后,对金黄色葡萄菌、肺炎菌、大肠杆菌的抗菌率均能达到95%以上,有很好的广谱抗菌耐洗性;最后产品中加入了天然凉感整理剂,赋予面料柔滑冰爽的效果。通过特殊的后整理应用工艺,一浴两步法一道工序实现了柔软抗菌凉感三种效果,减少工艺流程,节约了生产能耗。天然生物基产品,自然环境中可以完全生物降解,环保安全,提升了产品的可再生及环境友好价值;用本发明制成的整理剂利用非离子表面活性剂和阴离子表面活性剂的协同效应和增效作用,应用效果好,织物色变小,亲水性能和抗静电性能好,且无细胞毒性耐药性,对皮肤无刺激,满足市场需求提高产品质量,具有显著的社会效益和广阔的市场前景。
具体实施方式
为使本发明的目的、技术方案及优点更加清楚、明确,以下列举实施例对本发明进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。
下面通过具体实施例对本发明进行详细说明。
实施例1
(1)在反应釜1中加入50gALTAPYNE 1483,30g C12-C18的饱和脂肪酸,开启搅拌加热,转速为20rpm,温控140℃加热熔融,通氮气,加入0.5g次亚磷酸50%;升温至140℃左右加入14.1g二乙烯三胺,加完后开始升温,转速调整为40-50rpm,温度达到186±3℃时,持温反应3.5小时,关氮气,抽真空,继续保温反应30分钟;
(2)破真空,通氮气,降温至80-85℃,缓慢加入17.4g硫酸二甲酯,开启冷却盘管,控制温度不超过90℃,加入时间控制为1小时左右,加完后控温80℃反应80分钟;
(3)降温至70℃,加入50g NSS 1305、30g NSS 1308,搅拌30分钟至乳化均匀;降温至45℃;
(4)在混合罐1中加入24g除虫菊酯、12g柠檬桉叶油、25g1,3-丁二醇、60g天然磺化菜籽油,搅拌25分钟至乳化均匀;
(5)在混合罐1中继续加入473g水和14g封闭型聚氨酯,搅拌25分钟至乳化均匀;
(6)将混合罐1中的物料加入反应釜1中,搅拌45分钟至乳化均匀;
(7)在反应釜1中加入200g FINFOCE CCL,搅拌30分钟至乳化均匀;
(8)在反应釜1中加入0.2g CD-1116M搅拌20分钟至乳化均匀,过滤出料,制得整理剂1。
实施例2
(1)在反应釜中加入50g ALTAPYNE 1483,31g C12-C18的饱和脂肪酸,开启搅拌加热,转速为20rpm,温控140℃加热熔融,通氮气,加入0.5g次亚磷酸50%;升温至140℃左右加入20.8g三乙醇胺,加完后开始升温,转速调整为40-50rpm,温度达到190℃时,持温反应3.5小时,关氮气,抽真空,继续保温反应30分钟;
(2)破真空,通氮气,降温至70℃,缓慢加入17.4g硫酸二甲酯,开启冷却盘管,控制温度不超过90℃,加入时间控制为1小时左右,加完后控温70℃反应80分钟;
(3)加入50g NSS 1305、30g NSS 1308,搅拌30分钟至乳化均匀;降温至45℃;
(4)在混合罐1中加入30g除虫菊酯、10g柠檬桉叶油、26g1,3-丁二醇、60g天然磺化菜籽油,搅拌25分钟至乳化均匀;
(5)在混合罐1中继续加入410g水和15g封闭型聚氨酯,搅拌25分钟至乳化均匀;
(6)将混合罐1中的物料加入反应釜1中,搅拌45分钟至乳化均匀;
(7)在反应釜1中加入250g FINFOCE CCL,搅拌30分钟至乳化均匀;
(8)在反应釜1中加入0.2g CD-1116M搅拌20分钟至乳化均匀,过滤出料,制得整理剂2。
实施例3
(1)在反应釜中加入50g ALTAPYNE 1483,31g C12-C18的饱和脂肪酸,开启搅拌加热,转速为20rpm,温控140℃加热熔融,通氮气,加入0.5g次亚磷酸50%;升温至140℃左右加入20.3g N,N-双(3-氨丙基)甲胺,加完后开始升温,转速调整为40-50rpm,温度达到190℃时,持温反应3.5小时,关氮气,抽真空,继续保温反应30分钟;
(2)破真空,通氮气,降温至70℃,缓慢加入17.4g硫酸二甲酯,开启冷却盘管,控制温度不超过90℃,加入时间控制为1小时左右,加完后控温70℃反应80分钟;
(3)加入50gNSS 1305、30gNSS 1308,搅拌30分钟至乳化均匀;降温至45℃;
(4)在混合罐1中加入30g除虫菊酯、15g柠檬桉叶油、27g1,3-丁二醇、60g天然磺化菜籽油,搅拌25分钟至乳化均匀;
(5)在混合罐1中继续加入403g水和16g封闭型聚氨酯,搅拌25分钟至乳化均匀;
(6)将混合罐1中的物料加入反应釜1中,搅拌45分钟至乳化均匀;
(7)在反应釜1中加入250g FINFOCE CCL,搅拌30分钟至乳化均匀;
(8)在反应釜1中加入0.2g CD-1116M搅拌20分钟至乳化均匀,过滤出料,制得整理剂3。
实施例4
(1)在反应釜中加入86g ALTAPYNE 1483,开启搅拌加热,转速为20rpm,温控140℃加热熔融,通氮气,加入0.6g次亚磷酸50%;升温至140℃左右加入21.7g三乙醇胺,加完后开始升温,转速调整为40-50rpm,温度达到200±3℃时,持温反应3小时,
(2)关氮气,抽真空,继续保温反应30分钟;破真空,通氮气,降温至75-80℃,缓慢加入10.4g硫酸二甲酯,开启冷却盘管,控制温度不超过90℃,加入时间控制为1小时左右,加完后控温80℃反应60分钟;
(3)降温至70℃,加入80g NSS 1305A,搅拌30分钟至乳化均匀;降温至45℃;
(4)在混合罐1中加入25g除虫菊酯、15g柠檬桉叶油、28g1,3-丁二醇、60g天然磺化菜籽油,搅拌25分钟至乳化均匀;
(5)在混合罐1中继续加入387g水和17g封闭型聚氨酯,搅拌25分钟至乳化均匀;
(6)将混合罐1中的物料加入反应釜1中,搅拌45分钟至乳化均匀;
(7)在反应釜1中加入270g FINFOCE CCL,搅拌30分钟至乳化均匀;
(8)在反应釜1中加入0.3g CD-1116M搅拌20分钟至乳化均匀,过滤出料,制得整理剂4。
柔软剂是指一种能够吸附于纺织品纤维表面并使纤维平滑,以改变手感,使产品更有舒适感的纺织助剂。柔软整理是纺织印染加工中的重要后整理工序。纺织品在加工过程中,经多次处理后手感会变得粗糙,一般合成纤维织物更差,尤其是超细纤维织物,为了使织物具有柔软、滑爽、舒适的手感,就需要对其染色后进行柔软手感整理,目前应用广泛的是用柔软整理剂进行整理。整理剂优劣评价除了带给织物的柔软性能外,还需要产品稳定、对织物色光影响、亲水性能和抗静电性能等做综合评价。
抗菌剂是一种用于织物整理的具有广谱抗菌活性的整理剂,主要对金黄色葡萄菌、肺炎菌、大肠杆菌的抗菌率和耐洗能力做综合评价。
凉感剂是一种织物整理的具有顺滑凉爽触感的整理剂,主要对织物大热流失量Q-max值和耐洗能力做综合评价。
下面结合对比例对本发明做进一步说明,所述实施例和对比例仅为帮助理解本发明,不应视为对本发明的具体限制。
对比例1
市售凉感整理剂HB-100C,抗菌剂XC-980、柔软剂JL-206,此为市面常用整理剂,效果良好。
一、物理特性测试
对通过本发明实施例1-4制得的生物基柔软凉感抗菌整理剂进行物理特性测试,结果如表1所示:
表1
由表1可知,通过本发明制备出来的生物基柔软凉感抗菌整理剂产品稳定,含量高,安全性好,是一种可用于纺织品加工和纺织品日常洗护整理的整理剂,安全性高,具有良好的应用前景。
二、整理剂应用性能测试
将上述实施例1-4所制得的生物基柔软凉感抗菌整理剂和市面常用的整理剂对比例1进行对比测试。
2.1整理剂应用工艺:
织物:全棉梭织布
工艺:浸轧法
2.1.1生物基柔软凉感抗菌整理剂实施例1-4的应用,织物柔软凉感抗菌后整理一浴两步法工艺:
配制60g/L工作液→0.2MPa三浸三轧(带液率为60-80%)→烘干(105℃×120s)→定型(135℃×80s)→回潮评价。
2.1.2常规柔软凉感抗菌后整理工艺,凉感整理→抗菌整理→柔软整理三步法:
(1)HB-100C凉感整理
配制40g/L工作液→0.2MPa浸轧一遍(带液率为80%)→定型(100℃×120s);
(2)XC-980抗菌整理
配制80g/L工作液→0.2MPa浸轧一遍(带液率为65-70%%)→定型(130℃×90s);
(3)JL-206柔软整理
配制20g/L工作液→0.2MPa浸轧一遍(带液率为65-70%%)→定型(150℃×90s)→回潮评价。
2.2将实施例和对比例分别对其柔软性能、黄变、亲水性能、抗静电性能、抗菌性能和凉感性能进行测试:
(1)柔软性能评价方法
手感评价:对两种布样进行手触摸法进行评价,将原布手感评定为1级,手感评定最好的定位为5级。由3人以上的奇数位测试人员进行评定打分,取平均值,数值越大,表示手感越好,测试结果见表2。
(2)白度、色光评价方法
用Datacolor测色仪进行测试。与未处理布样进行白度对比,白度变化越大,即黄变越大,测试结果见表2。
(3)亲水性能评价方法
将水滴滴在整理后的织物上,测定水珠在织物上完全铺展开的时间,时间越短,表示亲水性能越好,测试结果见表2。
(4)抗静电性能评价方法
用表面电阻测试仪测定布面电阻率,电阻率越小,说明抗静电性能越好,测试结果见表2。
表2
整理剂 | 手感等级 | 白度 | 亲水性能(s) | 电阻率 |
原布 | 1 | 77.02 | 1-2 | <![CDATA[10<sup>9</sup><!-- 9 -->]]> |
实施例1 | 4 | 74.18 | 5 | <![CDATA[10<sup>9</sup>]]> |
实施例2 | 4 | 75.37 | 1-2 | <![CDATA[10<sup>8</sup>]]> |
实施例3 | 4 | 73.25 | 3 | <![CDATA[10<sup>9</sup>]]> |
实施例4 | 5 | 73.35 | 1-2 | <![CDATA[10<sup>8</sup>]]> |
对比例1 | 3-4 | 60.21 | >60 | <![CDATA[>10<sup>12</sup>]]> |
(5)抗菌性能评价方法
按照GB/T 17596-1998进行水洗50次后;按GB/T 20944.2-2007测试抑菌率结果,测试结果见表3。
表3
(6)凉爽性能评价方法
按照GB35263-2017《纺织品接触瞬间凉感性能的检测与评价》标准测试:
S1将ThermoLaboII设备电源启动,确认参数后热机约15分钟;
S2将主热板加热器(Heater)开关切入启始位置(ON),同时亦设定热板(Temperature-Box)之温度为35±0.1℃,当达到35℃时再将护环加热器(Guard Heater)开关切入启始位置(ON);
S3将冷板(Water-Box)设定于所需温度(模拟外界环境)一般为25℃,待温度(25℃)达到后,再将样布放置于冷板上(织物贴身侧朝上),当热板(Temperature-Box)之温度达到设定之温度(35℃)时按下qm键,同时并快速将热板(Temperature-Box)置于样布上(注意放置角度需垂直),记录显示幕上之qm值,此数值即为织物接触凉感(瞬间热流失量最大值),亦即实验结果,单位为W/cm2;
S4取5块样品测试,记录数据,求平均值,测试结果见表4。
表4
由表2可以看出,织物经过三次后整理工艺高温定型,白度值变化很大,但是经过采用本发明所制备的生物质整理剂一浴两步法整理后,白度值变化小,白度好,具备优异的手感,不易色变,具有良好的抗黄变效果。同时,处理后的织物还具有极佳的亲水性和抗静电性能。
由表3和表4的结果可以看出,采用本发明所制备的生物质整理剂处理后,通过封闭型聚氨酯乳液的交联作用,提高了织物的抗菌和凉感效果,特别是耐洗后的抗菌和凉感效果表现优异。
综上所述,本发明提供一种生物基柔软凉感抗菌整理剂及其制备方法,先将生物基有机酸和有机胺的脱水反应,生成带亲水链段结构的长链酯铵,确保了所制备得到的生物基柔软凉感抗菌整理剂的柔软性能,从而增强聚合物的亲水抗静电性能;最后将所述聚合物与季铵化试剂混合,发生季铵化反应,生成酯基季铵盐,提高了产物的稳定性和抗黄变效果,同时其亲水性得到进一步提升。加入天然油脂磺化油,这是一种以天然油脂为主要原料,采用三氧化硫气体磺化工艺进行改性,再与其他必要组分复配而成的阴离子型磺化油加脂剂,是一种优良的阴离子表面活性剂,有很强的亲水性能,该亲水链段在织物上会形成分子通道,使纺织物表面上的静电迅速转移,实现降低织物间的静摩擦系数和动摩擦系数。加入天然植物抗菌剂和天然凉感整理剂,增加了织物的抗菌性能和赋予面料柔滑冰爽的触感。通过特殊的后整理应用工艺,一浴两步法实现了一道工序达到柔软抗菌凉感三种后整理效果,减少了传统工艺流程,节约了生产能耗。
采用本发明的制备方法,可以得到一种亲水性能和柔软性能好,抗静电,抗黄变效果好,抗菌效果好,凉感效果好的生物基柔软凉感抗菌整理剂,以提高纺织品的品质和附加值。
申请人声明,本发明通过上述实施例来说明本发明的生物基柔软凉感抗菌整理剂及制备方法和应用,但本发明并不局限于上述详细方法,即不意味着本发明必须依赖上述详细方法才能实施。所属技术领域的技术人员应该明了,对本发明的任何改进,对本发明产品各原料的等效替换及辅助成分的添加、具体方式的选择等,均落在本发明的保护范围和公开范围之内。
Claims (10)
2.根据权利要求1所述的一种生物基柔软凉感抗菌整理剂,其特征在于:
所述的生物基有机酸为C12-C18的饱和脂肪酸、妥尔油脂肪酸、精制妥尔油中的任意一种或任意组合;
所述催化剂为次亚磷酸、对甲苯磺酸中的任意一种或任意组合;
所述的有机胺为二乙烯三胺、三乙醇胺和N,N-双(3-氨丙基)甲胺中的任意一种或任意组合;
所述的季铵化试剂为碳酸二甲酯、硫酸二甲酯、碳酸二乙酯和硫酸二乙酯中的任意一种或任意组合;
所述的生物基乳化剂为腰果酚聚氧乙烯醚NSS 1305、NSS 1305A、NSS 1308中的任意一种或任意组合;
所述的天然油脂磺化油为天然磺化菜籽油、天然磺化蓖麻油、硫酸化天然牛蹄油中的至少一种或任意组合;
所述的天然植物抗菌剂为除虫菊酯、柠檬桉叶油、日本扁柏提取物、香叶天竺葵提取物的至少一种或任意组合;
所述的多元醇为1,3-丁二醇、乙二醇、丙二醇中的至少一种或任意组合;
所述聚氨酯为乙烯基聚氨酯乳液、多异氰酸酯乳液、封闭型聚氨酯乳液中的至少一种或任意组合;
所述天然凉感整理剂木糖醇、薄荷油、赤糖醇、蚕丝素蛋白、红色线反射陶瓷的至少一种或任意组合;
所述的消泡剂为聚氧丙基聚氧乙基甘油醚、聚醚改性聚硅氧烷类中的任意一种或任意组合。
3.一种生物基柔软凉感抗菌整理剂的制备方法,其特征在于步骤包括:
步骤一、将生物基有机酸、催化剂和有机胺混合进行脱水反应,得到初始产物;
步骤二、向步骤一得到的初始产物中加入季铵化试剂进行季铵化反应;
步骤三、待步骤二所述季铵化反应结束后,加入生物基乳化剂,得到所述生物基阳离子柔软剂A;
步骤四、将天然植物抗菌剂、多元醇和天然油脂磺化油进行混合,得到混合物B;
步骤五、将步骤四得到的混合物B中加入水和聚氨酯,搅拌混合,得到混合物生物基抗菌剂C;
步骤六、将步骤三得到的生物基阳离子柔软剂A和步骤五得到的生物基抗菌剂C进行混合,得到混合物D;
步骤七、在步骤六得到的混合物D中加入天然凉感整理剂,搅拌,得到混合物E;
步骤八、将消泡剂投入到步骤七得到的混合物E中,搅拌,过滤得到生物基柔软凉感抗菌整理剂。
4.根据权利要求3所述的生物基柔软凉感抗菌整理剂的制备方法,其特征在于:
所述步骤一中,进行脱水反应时的具体步骤为:
在N2氛围下,先将生物基有机酸加热熔融,温度为120-180℃,搅拌速度为20-40rpm;熔融后加入催化剂,搅拌均匀;随后加入有机胺,升温至180-230℃开始脱水反应,反应时间为3-10小时;在真空条件下继续反应0.5-3小时,得到初始产物。
5.根据权利要求4所述的生物基柔软凉感抗菌整理剂的制备方法,其特征在于:
所述步骤二中,进行季铵化反应时,初始产物的温度为70-90℃,加入季铵化试剂的时间为1-3h,季铵化反应时间为1-3h。
6.根据权利要求4或5所述的生物基柔软凉感抗菌整理剂的制备方法,其特征在于:
所述步骤三中,加入生物基乳化剂后搅拌时间为10-30min,搅拌完成后降温至45℃以下,得到生物基阳离子柔软剂。
7.根据权利要求6所述的生物基柔软凉感抗菌整理剂的制备方法,其特征在于:
所述步骤四中,混合时进行搅拌,搅拌时间为10-45min,搅拌速度为20-40rpm;
所述步骤五中,混合时进行搅拌,搅拌时间为10-45min;
所述步骤六中,混合时进行搅拌,搅拌时间为30-60min,搅拌速度为20-40rpm;
所述步骤七中,混合时进行搅拌,搅拌时间为10-45min;
所述步骤八中,混合时进行搅拌,搅拌时间为10-30min。
8.一种生物基柔软凉感抗菌整理剂的应用,其特征在于:将生物基柔软凉感抗菌整理剂应用到织物的后整理中,包括如下步骤:
S1,将权利要求1-2任一所述的生物基柔软凉感抗菌整理剂或者是权利要求3-7任一方法制备得到的生物基柔软凉感抗菌整理剂与水进行混合,得到工作液,工作液的浓度为50-100g/L;
S2,将织物在步骤S1得到的工作液中进行浸轧处理,带液率为60-80%,然后进行烘干和定型。
9.根据权利要求8所述的生物基柔软凉感抗菌整理剂的应用,其特征在于:
所述的步骤S2中,浸轧处理为三浸三轧,轧辊压力为0.15-0.25Mpa,烘干温度为100-110℃,烘干时间为60-120s,定型温度为130-140℃,定型时间为60-90s。
10.根据权利要求8所述的生物基柔软凉感抗菌整理剂的应用,其特征在于:
所述的步骤S2中,所述织物为全棉织物、棉及聚酰胺纤维的混织物、棉及聚酯纤维的混织物、天丝中的至少一种。
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