CN111411522A - 一种羊毛织物防毡缩整理工艺 - Google Patents
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Abstract
本发明涉及羊毛织物技术领域,公开了一种羊毛织物防毡缩整理工艺。包括以下步骤:S1、将羊毛织物放入氧化处理液中进行氧化处理,得到预处理羊毛织物;S2、将复合蛋白酶加入Tris‑HCl缓冲溶液中,进行超声振荡分散,得到复合蛋白酶分散液,将预处理羊毛织物放入复合蛋白酶分散液中进行酶解,得到酶解羊毛织物;S3、向聚醋酸乙烯酯溶液中加入氢氧化钠,搅拌醇解得到醇解液,将步骤S2得到的酶解羊毛织物放入醇解液中浸泡,取出后放入戊二醛溶液中进行交联反应,然后经过醇洗、干燥,即得。本发明羊毛织物经过酶解液整理后保持较高的断裂强力,且具有优良的防毡缩性能。
Description
技术领域
本发明涉及羊毛织物技术领域,尤其是涉及一种羊毛织物防毡缩整理工艺。
背景技术
羊毛织物具有许多优良特性,如弹性好、吸湿性强、保暖性好、光泽柔和等。羊毛织物以其高贵风格、优雅的服用性能而深受消费者喜爱。羊毛纤维主要由包覆于纤维外部的鳞片层、组成羊毛实体主要部分的皮质层、处于纤维中心因含空气而不透明的髓质层和鳞片内层构成,羊毛鳞片层含有大量的二硫键,结构致密,可以保护羊毛内层组织,抵抗外界机械、化学等的侵蚀,羊毛鳞片层结构使的羊毛纤维在水洗时经不断挤压、揉搓容易发生毡缩,从而引起织物尺寸缩小,导致羊毛织物的柔软性能和弹性变差,尺寸稳定性受到影响,严重影响了羊毛织物的外观和服用性能。蛋白酶可作用于羊毛或者蚕丝等纤维,能够催化肽键水解,被认为是替代羊毛氯化防毡缩方法最优潜力的方法。现有常规技术是将羊毛织物浸入蛋白酶溶液中,蛋白酶酶解羊毛纤维表面的鳞片,从而提高羊毛织物的防毡缩性能,但是由于蛋白酶分子体积较小,很容易从羊毛纤维纤维表面的鳞片间渗入纤维内部,对羊毛纤维内部实体皮质层造成酶损伤,导致羊毛的断裂强力下降,服用性能变差。
中国专利公开号CN110468594A公开了一种粗纺羊毛织物的防毡缩整理工艺,将粗纺羊毛织物浸渍于含有枯草杆菌蛋白酶、SZ蛋白酶和纤维素酶的复合酶工作液中整理,然后将酶解后的羊毛织物浸渍在含有双氧水和双氧水稳定剂的剥磷处理液中,从而使羊毛织物具有防毡缩性能。
中国专利公开号CN102965955A公开了一种角质酶、角蛋白酶和蛋白酶一浴法羊毛防毡缩工艺,羊毛试样经萃取去除游离性杂质后在含有一定浓度的角质酶、角蛋白酶和蛋白酶溶液中一浴法处理,通过三种酶的协同作用,提高了纤维鳞片表面的亲水性和处理浴中角蛋白酶和蛋白酶的作用效率。
中国专利公开号CN103924439A公开了一种应用超声波技术进行蛋白酶羊毛防毡缩处理的方法,在超声波条件下对羊毛织物进行防毡缩整理,提高蛋白酶催化水解的速率,加快羊毛鳞片的脱落,缩短酶法防毡缩处理时间,通过超声波和蛋白酶的协同作用,可替代传统的氯化法或单一蛋白酶防毡缩整理方法,提高羊毛织物的防毡缩性能。
以上技术方案中均采用将羊毛织物浸泡在蛋白酶处理液中的方式利用蛋白酶的酶解作用去除羊毛织物表面的鳞片结构,减小羊毛织物表面的摩擦,从而达到防毡缩的目的。但是由于蛋白酶分子体积较小,蛋白酶能够从羊毛纤维表面的鳞片间隙渗入羊毛纤维内部的皮质层,从而对纤维内部结构造成损伤,导致羊毛织物的断裂强力下降。
发明内容
本发明是为了克服现有以上技术问题,提供一种羊毛织物防毡缩整理工艺。
为了实现上述目的,本发明采用以下技术方案:一种羊毛织物防毡缩整理工艺,包括以下步骤:
S1、将双氧水和氢氧化钠加入去离子水中,搅拌均匀,得到氧化处理液,水浴加热至30-35℃,将羊毛织物放入氧化处理液中进行氧化处理20-30min,水洗,烘干,得到预处理羊毛织物;
S2、将复合蛋白酶加入Tris-HCl缓冲溶液中,进行超声振荡分散,得到复合蛋白酶分散液,将预处理羊毛织物放入复合蛋白酶分散液中,调节pH至8-9,水浴加热至40-50℃,进行酶解30-50min,水洗,干燥,得到酶解羊毛织物;
S3、将聚醋酸乙烯酯加入无水乙醇中搅拌溶解得到聚醋酸乙烯酯溶液,向聚醋酸乙烯酯溶液中加入氢氧化钠,搅拌醇解,得到醇解液,将步骤S2得到的酶解羊毛织物放入醇解液中浸泡20-30min,取出后放入戊二醛溶液中,调节pH至3-5,水浴加热至40-45℃,进行交联反应1-3h,然后经过醇洗、干燥,即得。
本发明先使用双氧水在碱性条件下对羊毛织物进行氧化处理,破坏羊毛纤维鳞片层的二硫键,生成具有亲水作用的羧基、羟基亲水性官能团,使羊毛纤维表面具有亲水性能,提高后续复合蛋白酶对羊毛鳞片的酶解作用,使用复合蛋白酶酶解羊毛纤维表面的鳞片后,然后利用聚醋酸乙烯酯水解生成的聚乙烯醇在羊羊毛纤维表面通过交联剂戊二醛的作用发生分子间的交联,从而在羊毛纤维表面包覆一层高分子聚合物层,降低羊毛纤维表面的定向摩擦作用,从而提高羊毛织物的防毡缩性能;另一方面,步骤S1中使用双氧水氧化羊毛纤维,使羊毛纤维表面负载有羟基官能团,羊毛纤维表面的羟基参与到聚乙烯醇分子之间的交联反应,从而将羊毛纤维与纤维之间连接,减小羊毛纤维的收缩作用力,从而进一步提高羊毛纤维的防毡缩性能。
作为优选,所述步骤S2中复合蛋白酶与Tris-HCl缓冲溶液的质量比为1:30-50。
作为优选,所述步骤S3中酶解羊毛织物与醇解液的浴比为1:20-30。
作为优选,所述步骤S3中戊二醛质量为聚醋酸乙烯酯的5-10wt%。
作为优选,所述步骤S2中复合蛋白酶的制备方法包括以下步骤:
将3-缩水甘油醚氧基丙基三乙氧基硅烷加入去离子水中,调节pH至5-6,水浴加热至40-50℃,搅拌水解30-50min,得水解液,将二氧化硅微米颗粒加入水解液中,在45-55℃下保温反应1-2h,洗涤,干燥,得偶联剂改性二氧化硅微米颗粒;向羧甲基纤维素溶液中加入氢氧化钠,搅拌溶解,然后加入偶联剂改性二氧化硅微米颗粒,在50-60℃下反应10-15h,将反应得到的产物加入蛋白酶溶液中,然后添加戊二醛交联剂,调节pH至4-5,在35-40℃下进行反应2-3h,水洗,室温晾干,得到复合蛋白酶。
本发明复合蛋白酶制备方法为先将3-缩水甘油醚氧基丙基三乙氧基硅烷接枝在二氧化硅微米颗粒表面,使二氧化硅微米颗粒表面负载环氧基团,然后利用环氧基与羧甲基纤维素分子上的羟基发生开环反应,从而将羧甲基纤维素接枝在二氧化硅微米颗粒表面,然后将表面接枝有羧甲基纤维素的二氧化硅微米颗粒放入含有交联剂的蛋白酶溶液中,二氧化硅微米颗粒表面的羧甲基纤维素分子在交联剂的作用下发生分子间的交联,从而将蛋白酶固定负载在二氧化硅微米颗粒表面,从而制备得到以二氧化硅为载体的复合蛋白酶,利用二氧化硅微米颗粒作为蛋白酶的载体,由于二氧化硅微米颗粒粒径大小在微米级,体积大于羊毛纤维表面鳞片间的间距空隙,蛋白酶不能进入到羊毛纤维的内部皮质层结构中,从而避免蛋白酶渗入羊毛纤维内部造成羊毛纤维的损伤,增强羊毛织物的断裂强力,提高羊毛织物的服用性能。
作为优选,所述羧甲基纤维素溶液的质量浓度为3-6%。
作为优选,所述戊二醛交联剂添加量为蛋白酶溶液的2-5wt%。
作为优选,所述二氧化硅微米颗粒经过预处理,包括以下步骤:将去离子水与无水乙醇混合均匀,滴加醋酸调节pH至2-3,得到溶液a,备用;将钛酸四丁酯与二氧化硅微米颗粒加入无水乙醇中,搅拌均匀,得悬浮液,将溶液a滴加到悬浮液中,滴加完毕后静置3-6h,离心分离,水洗,干燥,送入马弗炉中进行煅烧处理,冷却,即得。
使用二氧化硅微米颗粒负载蛋白酶虽然能够避免蛋白酶进入羊毛纤维的内部对羊毛纤维造成强力损伤,但是采用二氧化硅颗粒负载蛋白酶与羊毛纤维表面的接触面积小,蛋白酶对羊毛纤维表面鳞片的酶解作用降低,造成羊毛织物的防毡缩性能不佳,所以本发明对二氧化硅微米颗粒进行预处理,在二氧化硅微米颗粒表面沉积纳米二氧化钛颗粒,在二氧化硅颗粒表面形成纳米二氧化钛凸起结构,从而增加二氧化硅微米颗粒的表面积,提高复合蛋白酶与羊毛织物纤维的接触面积,从而提高对羊毛纤维表面鳞片的酶解作用,进而提高羊毛织物的防毡缩性能。
作为优选,所述去离子水与无水乙醇的体积比为1:3-5。
作为优选,所述钛酸四丁酯与二氧化硅微米颗粒的质量比为1:4-8。
因此,本发明具有如下有益效果:(1)利用聚醋酸乙烯酯水解生成的聚乙烯醇在羊羊毛纤维表面通过交联剂戊二醛的作用发生分子间的交联,从而在羊毛纤维表面包覆一层高分子聚合物层,降低羊毛纤维表面的定向摩擦作用,从而提高羊毛织物的防毡缩性能;(2)避免蛋白酶渗入羊毛纤维内部造成羊毛纤维的损伤,增强羊毛织物的断裂强力,提高羊毛织物的服用性能。
附图说明
图1为本发明羊毛织物经过整理后扫描电镜SEM图。
具体实施方式
下面通过具体实施例,对本发明的技术方案做进一步说明。
若非特指,所采用的原料和设备等均可从市场购得或是本领域常用的,实施例中的方法,如无特别说明,均为本领域的常规方法。
羊毛织物:190g/m2美利奴羊毛平纹织物,金百盛纺织科技有限公司;蛋白酶:型号Esperase8L,诺维信生物科技有限公司;聚醋酸乙烯酯:分子量12000-25000,银洋胶基材料有限公司;二氧化硅微米颗粒:粒径0.5-1μm,上海晶炼新材料有限公司。
实施例1
复合蛋白酶的制备方法包括以下步骤:
将去离子水与无水乙醇按照体积比1:5混合均匀,滴加醋酸调节pH至2,得到溶液a,备用;将钛酸四丁酯与二氧化硅微米颗粒加入无水乙醇中,钛酸四丁酯与二氧化硅微末颗粒的质量比为1:7,二氧化硅微米颗粒与无水乙醇的质量体积比为1g/30mL,搅拌均匀,得悬浮液,按照溶液a与悬浮液的体积比1:5的比例将溶液a以3滴/秒的速率滴加到悬浮液中,滴加完毕后静置5h,离心分离,水洗,置于烘箱中在50℃下干燥3h,然后送入马弗炉中在500℃下进行煅烧3h,冷却,得到预处理二氧化硅微米颗粒;
按照3-缩水甘油醚氧基丙基三乙氧基硅烷与去离子水的质量比1:50的比例,将3-缩水甘油醚氧基丙基三乙氧基硅烷加入去离子水中,调节pH至6,水浴加热至50℃,搅拌水解40min,得水解液,将预处理二氧化硅微米颗粒按照质量体积比1g/60mL的比例加入水解液中,在55℃下保温反应1.5h,洗涤,干燥,得偶联剂改性二氧化硅微米颗粒;将羧甲基纤维素加入去离子水中配制成浓度为5%的羧甲基纤维溶液,向羧甲基纤维素溶液中加入氢氧化钠,氢氧化钠添加量为羧甲基纤维素溶液的0.5wt%,搅拌溶解,然后加入偶联剂改性二氧化硅微米颗粒,偶联剂改性二氧化硅微米颗粒与羧甲基纤维素的质量比为1:0.5,在55℃下反应13h,将反应得到的产物按照质量体积比1g/50mL的比例加入质量浓度为3%的蛋白酶溶液中,然后添加戊二醛交联剂,戊二醛交联剂添加量为蛋白酶溶液的5wt%,调节pH至4.5,在37℃下进行反应2.5h,水洗,室温晾干,得到复合蛋白酶。
羊毛织物防毡缩整理工艺,包括以下步骤:
S1、将质量浓度为20%的双氧水和氢氧化钠加入去离子水中,双氧水添加量为去离子水的体积的0.5倍,氢氧化钠与去离子水的质量体积比为0.3g/L,搅拌均匀,得到氧化处理液,水浴加热至35℃,将羊毛织物按浴比1:20放入氧化处理液中进行氧化处理25min,水洗,烘干,得到预处理羊毛织物;
S2、按照复合蛋白酶与Tris-HCl缓冲溶液的质量比为1:35比例将复合蛋白酶加入0.1mol/L的Tris-HCl缓冲溶液中,进行超声振荡分散,得到复合蛋白酶分散液,将预处理羊毛织物按照浴比1:30的比例放入复合蛋白酶分散液中,调节pH至9,水浴加热至50℃,进行酶解45min,水洗,置于烘箱中80℃下干燥1h,得到酶解羊毛织物;
S3、将聚醋酸乙烯酯加入无水乙醇中搅拌溶解配制成质量浓度为5%的聚醋酸乙烯酯溶液,向聚醋酸乙烯酯溶液中加入氢氧化钠,氢氧化钠添加量为聚醋酸乙烯酯的2wt%,搅拌醇解,得到醇解液,将步骤S2得到的酶解羊毛织物按照浴比1:25的比例放入醇解液中浸泡25min,取出后放入质量浓度为5%的戊二醛溶液中,戊二醛质量为聚醋酸乙烯酯的8wt%,调节pH至3,水浴加热至43℃,进行交联反应2.5h,然后经过醇洗,转入烘箱中在60℃下干燥2h,即得。
实施例2
复合蛋白酶的制备方法包括以下步骤:
将去离子水与无水乙醇按照体积比1:3混合均匀,滴加醋酸调节pH至3,得到溶液a,备用;将钛酸四丁酯与二氧化硅微米颗粒加入无水乙醇中,钛酸四丁酯与二氧化硅微末颗粒的质量比为1:5,二氧化硅微米颗粒与无水乙醇的质量体积比为1g/30mL,搅拌均匀,得悬浮液,按照溶液a与悬浮液的体积比1:5的比例将溶液a以3滴/秒的速率滴加到悬浮液中,滴加完毕后静置4h,离心分离,水洗,置于烘箱中在50℃下干燥3h,然后送入马弗炉中在500℃下进行煅烧3h,冷却,得到预处理二氧化硅微米颗粒;
按照3-缩水甘油醚氧基丙基三乙氧基硅烷与去离子水的质量比1:50的比例,将3-缩水甘油醚氧基丙基三乙氧基硅烷加入去离子水中,调节pH至5,水浴加热至40℃,搅拌水解35min,得水解液,将预处理二氧化硅微米颗粒按照质量体积比1g/60mL的比例加入水解液中,在45℃下保温反应1.5h,洗涤,干燥,得偶联剂改性二氧化硅微米颗粒;将羧甲基纤维素加入去离子水中配制成浓度为4%的羧甲基纤维溶液,向羧甲基纤维素溶液中加入氢氧化钠,氢氧化钠添加量为羧甲基纤维素溶液的0.5wt%,搅拌溶解,然后加入偶联剂改性二氧化硅微米颗粒,偶联剂改性二氧化硅微米颗粒与羧甲基纤维素的质量比为1:0.5,在55℃下反应12h,将反应得到的产物按照质量体积比1g/50mL的比例加入质量浓度为3%的蛋白酶溶液中,然后添加戊二醛交联剂,戊二醛交联剂添加量为蛋白酶溶液的2wt%,调节pH至4.5,在37℃下进行反应2.5h,水洗,室温晾干,得到复合蛋白酶。
羊毛织物防毡缩整理工艺,包括以下步骤:
S1、将质量浓度为20%的双氧水和氢氧化钠加入去离子水中,双氧水添加量为去离子水的体积的0.5倍,氢氧化钠与去离子水的质量体积比为0.3g/L,搅拌均匀,得到氧化处理液,水浴加热至30℃,将羊毛织物按浴比1:20放入氧化处理液中进行氧化处理22min,水洗,烘干,得到预处理羊毛织物;
S2、按照复合蛋白酶与Tris-HCl缓冲溶液的质量比为1:45比例将复合蛋白酶加入0.1mol/L的Tris-HCl缓冲溶液中,进行超声振荡分散,得到复合蛋白酶分散液,将预处理羊毛织物按照浴比1:30的比例放入复合蛋白酶分散液中,调节pH至8,水浴加热至40℃,进行酶解35min,水洗,置于烘箱中80℃下干燥1h,得到酶解羊毛织物;
S3、将聚醋酸乙烯酯加入无水乙醇中搅拌溶解配制成质量浓度为5%的聚醋酸乙烯酯溶液,向聚醋酸乙烯酯溶液中加入氢氧化钠,氢氧化钠添加量为聚醋酸乙烯酯的2wt%,搅拌醇解,得到醇解液,将步骤S2得到的酶解羊毛织物按照浴比1:25的比例放入醇解液中浸泡25min,取出后放入质量浓度为5%的戊二醛溶液中,戊二醛质量为聚醋酸乙烯酯的6wt%,调节pH至5,水浴加热至42℃,进行交联反应1.5h,然后经过醇洗,转入烘箱中在60℃下干燥2h,即得。
实施例3
复合蛋白酶的制备方法包括以下步骤:
将去离子水与无水乙醇按照体积比1:4混合均匀,滴加醋酸调节pH至2.5,得到溶液a,备用;将钛酸四丁酯与二氧化硅微米颗粒加入无水乙醇中,钛酸四丁酯与二氧化硅微末颗粒的质量比为1:8,二氧化硅微米颗粒与无水乙醇的质量体积比为1g/30mL,搅拌均匀,得悬浮液,按照溶液a与悬浮液的体积比1:5的比例将溶液a以3滴/秒的速率滴加到悬浮液中,滴加完毕后静置6h,离心分离,水洗,置于烘箱中在50℃下干燥3h,然后送入马弗炉中在500℃下进行煅烧3h,冷却,得到预处理二氧化硅微米颗粒;
按照3-缩水甘油醚氧基丙基三乙氧基硅烷与去离子水的质量比1:50的比例,将3-缩水甘油醚氧基丙基三乙氧基硅烷加入去离子水中,调节pH至5.5,水浴加热至45℃,搅拌水解50min,得水解液,将预处理二氧化硅微米颗粒按照质量体积比1g/60mL的比例加入水解液中,在50℃下保温反应2h,洗涤,干燥,得偶联剂改性二氧化硅微米颗粒;将羧甲基纤维素加入去离子水中配制成浓度为6%的羧甲基纤维溶液,向羧甲基纤维素溶液中加入氢氧化钠,氢氧化钠添加量为羧甲基纤维素溶液的0.5wt%,搅拌溶解,然后加入偶联剂改性二氧化硅微米颗粒,偶联剂改性二氧化硅微米颗粒与羧甲基纤维素的质量比为1:0.5,在60℃下反应15h,将反应得到的产物按照质量体积比1g/50mL的比例加入质量浓度为3%的蛋白酶溶液中,然后添加戊二醛交联剂,戊二醛交联剂添加量为蛋白酶溶液的3wt%,调节pH至5,在40℃下进行反应3h,水洗,室温晾干,得到复合蛋白酶。
羊毛织物防毡缩整理工艺,包括以下步骤:
S1、将质量浓度为20%的双氧水和氢氧化钠加入去离子水中,双氧水添加量为去离子水的体积的0.5倍,氢氧化钠与去离子水的质量体积比为0.3g/L,搅拌均匀,得到氧化处理液,水浴加热至32℃,将羊毛织物按浴比1:20放入氧化处理液中进行氧化处理30min,水洗,烘干,得到预处理羊毛织物;
S2、按照复合蛋白酶与Tris-HCl缓冲溶液的质量比为1:30比例将复合蛋白酶加入0.1mol/L的Tris-HCl缓冲溶液中,进行超声振荡分散,得到复合蛋白酶分散液,将预处理羊毛织物按照浴比1:30的比例放入复合蛋白酶分散液中,调节pH至8.5,水浴加热至45℃,进行酶解50min,水洗,置于烘箱中80℃下干燥1h,得到酶解羊毛织物;
S3、将聚醋酸乙烯酯加入无水乙醇中搅拌溶解配制成质量浓度为5%的聚醋酸乙烯酯溶液,向聚醋酸乙烯酯溶液中加入氢氧化钠,氢氧化钠添加量为聚醋酸乙烯酯的2wt%,搅拌醇解,得到醇解液,将步骤S2得到的酶解羊毛织物按照浴比1:30的比例放入醇解液中浸泡30min,取出后放入质量浓度为5%的戊二醛溶液中,戊二醛质量为聚醋酸乙烯酯的10wt%,调节pH至4,水浴加热至45℃,进行交联反应3h,然后经过醇洗,转入烘箱中在60℃下干燥2h,即得。
实施例4
复合蛋白酶的制备方法包括以下步骤:
将去离子水与无水乙醇按照体积比1:4混合均匀,滴加醋酸调节pH至2.5,得到溶液a,备用;将钛酸四丁酯与二氧化硅微米颗粒加入无水乙醇中,钛酸四丁酯与二氧化硅微末颗粒的质量比为1:4,二氧化硅微米颗粒与无水乙醇的质量体积比为1g/30mL,搅拌均匀,得悬浮液,按照溶液a与悬浮液的体积比1:5的比例将溶液a以3滴/秒的速率滴加到悬浮液中,滴加完毕后静置3h,离心分离,水洗,置于烘箱中在50℃下干燥3h,然后送入马弗炉中在500℃下进行煅烧3h,冷却,得到预处理二氧化硅微米颗粒;
按照3-缩水甘油醚氧基丙基三乙氧基硅烷与去离子水的质量比1:50的比例,将3-缩水甘油醚氧基丙基三乙氧基硅烷加入去离子水中,调节pH至5.5,水浴加热至45℃,搅拌水解30min,得水解液,将预处理二氧化硅微米颗粒按照质量体积比1g/60mL的比例加入水解液中,在50℃下保温反应1h,洗涤,干燥,得偶联剂改性二氧化硅微米颗粒;将羧甲基纤维素加入去离子水中配制成浓度为3%的羧甲基纤维溶液,向羧甲基纤维素溶液中加入氢氧化钠,氢氧化钠添加量为羧甲基纤维素溶液的0.5wt%,搅拌溶解,然后加入偶联剂改性二氧化硅微米颗粒,偶联剂改性二氧化硅微米颗粒与羧甲基纤维素的质量比为1:0.5,在50℃下反应10h,将反应得到的产物按照质量体积比1g/50mL的比例加入质量浓度为3%的蛋白酶溶液中,然后添加戊二醛交联剂,戊二醛交联剂添加量为蛋白酶溶液的3wt%,调节pH至4,在35℃下进行反应2h,水洗,室温晾干,得到复合蛋白酶。
羊毛织物防毡缩整理工艺,包括以下步骤:
S1、将质量浓度为20%的双氧水和氢氧化钠加入去离子水中,双氧水添加量为去离子水的体积的0.5倍,氢氧化钠与去离子水的质量体积比为0.3g/L,搅拌均匀,得到氧化处理液,水浴加热至32℃,将羊毛织物按浴比1:20放入氧化处理液中进行氧化处理20min,水洗,烘干,得到预处理羊毛织物;
S2、按照复合蛋白酶与Tris-HCl缓冲溶液的质量比为1:50比例将复合蛋白酶加入0.1mol/L的Tris-HCl缓冲溶液中,进行超声振荡分散,得到复合蛋白酶分散液,将预处理羊毛织物按照浴比1:30的比例放入复合蛋白酶分散液中,调节pH至8.5,水浴加热至45℃,进行酶解30min,水洗,置于烘箱中80℃下干燥1h,得到酶解羊毛织物;
S3、将聚醋酸乙烯酯加入无水乙醇中搅拌溶解配制成质量浓度为5%的聚醋酸乙烯酯溶液,向聚醋酸乙烯酯溶液中加入氢氧化钠,氢氧化钠添加量为聚醋酸乙烯酯的2wt%,搅拌醇解,得到醇解液,将步骤S2得到的酶解羊毛织物按照浴比1:20的比例放入醇解液中浸泡20min,取出后放入质量浓度为5%的戊二醛溶液中,戊二醛质量为聚醋酸乙烯酯的5wt%,调节pH至4,水浴加热至40℃,进行交联反应1h,然后经过醇洗,转入烘箱中在60℃下干燥2h,即得。
对比例1:
对比例1与实施例1的不同之处在于将复合蛋白酶替换为市售没有经过处理的蛋白酶。
对比例2:
对比例2与实施例1的不同之处在于二氧化硅微米颗粒没有经过预处理。
对比例3:
对比例3与实施例1的不同之处在于没有经过步骤S3处理。
羊毛织物性能检测:
1.羊毛织物面积毡缩率:
根据FZ/T 70009-1999《毛纺织产品经机洗后的松弛及毡化收缩试验方法》和GB/T8629-2001《纺织品试验用家庭洗涤和干燥程序》,采用5A程序,在(40±3)℃条件下循环水洗,浴比控制在1:50,洗衣粉添加量为3g/L,皂片添加量为0.5g/L,脱水烘干后进行吸湿平衡,测定羊毛织物尺寸面积大小,计算出羊毛织物的面积毡缩率,羊毛织物面积毡缩率的计算公式为:
羊毛织物面积毡缩率=(S1-S2)/S1×100%;其中S1表示整理前羊毛织物的面积,S2表示整理后羊毛织物的面积。
经检测羊毛织物整理前面积毡缩率为15.74%。
2.采用织物风格测试仪对羊毛织物柔软程度进行测定,柔软程度分为Ⅰ-Ⅴ级,其中Ⅰ柔软程度最柔;采用测色配色仪对羊毛织物泛黄指数进行检测,泛黄指数越大证明织物泛黄越严重。
由测试上述测试结果可以得到本发明羊毛织物经过整理后面积毡缩率达到3%以下,相比之前为整理过的羊毛织物抗毡缩性能得到大幅提升,由实施例和对比例3对比可以得到经过步骤S3高分子聚合物包覆处理的羊毛织物的抗毡缩性能优于未经过步骤S3高分子聚合物包覆处理的羊毛织物的抗毡缩性能。由实施例和对比例2对比得到实施例羊毛织物的抗毡缩性能由于对比例2,这是由于本发明实施例中对二氧化硅微米颗粒进行预处理,在二氧化硅微米颗粒表面沉积纳米二氧化钛颗粒,在二氧化硅颗粒表面形成纳米二氧化钛凸起结构,从而增加二氧化硅微米颗粒的表面积,提高复合蛋白酶与羊毛织物纤维的接触面积,从而提高对羊毛纤维表面鳞片的酶解作用,进而提高羊毛织物的抗毡缩性能,通过图1可以观察得到本发明羊毛纤维经过整理后羊毛纤维表面光滑,羊毛纤维表面的鳞片结构基本消失。另外本发明实施例中羊毛织物的柔软程度达到Ⅱ级,泛黄指数控制在28附近,达到羊毛织物的可服用标准。
3.羊毛织物力学性能:
根据GB/T3923.1-1997《织物拉伸性能第一部分:断裂强力和断裂伸长率测定条样法》,测定羊毛的断裂强力,然后根据测定的羊毛织物的断裂强力计算得出羊毛织物的断裂强力保留率。羊毛织物的断裂强力测定方法为将羊毛织物剪切为大小20mm×70mm的条状羊毛织物,然后放置于等速拉伸实验仪中测试条状羊毛织物试样的断裂强力,间距长度为200mm,以20mm/min的拉伸速率进行拉伸,直至试样条发生断裂,记录羊毛织物的断裂强力,然后根据测定羊毛织物整理前后试样的断裂强力,计算出羊毛织物试样的强力损失率。羊毛织物的强力损失率按照下式进行计算:
羊毛织物强力损失率=(1-T1/T2)×100%;其中T1代表整理后羊毛织物的断裂强力,T2代表整理前羊毛织物的断裂强力。
经测试美利奴羊毛平纹织物未整理前断裂强力为255.7N。
由本发明实施例1-4羊毛织物的断裂强力和强力损失率与对比例1对比得到:实施例1-4中经过酶处理后的羊毛织物的强力损失明显低于对比例1羊毛织物,这是因为本发明实施例中利用二氧化硅微米颗粒作为蛋白酶的载体,由于二氧化硅微米颗粒粒径大小在微米级,体积大于羊毛纤维表面鳞片间的间距空隙,蛋白酶不能进入到羊毛纤维的内部皮质层结构中,从而避免蛋白酶渗入羊毛纤维内部造成羊毛纤维的损伤,增强羊毛织物的断裂强力,降低羊毛织物的强力损失。
以上所述仅是本发明的优选实施例方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以作出若干改进和润饰,这些改进和润饰也应该视为本发明的保护范围。
Claims (10)
1.一种羊毛织物防毡缩整理工艺,其特征在于,包括以下步骤:
S1、将双氧水和氢氧化钠加入去离子水中,搅拌均匀,得到氧化处理液,水浴加热至30-35℃,将羊毛织物放入氧化处理液中进行氧化处理20-30min,水洗,烘干,得到预处理羊毛织物;
S2、将复合蛋白酶加入Tris-HCl缓冲溶液中,进行超声振荡分散,得到复合蛋白酶分散液,将预处理羊毛织物放入复合蛋白酶分散液中,调节pH至8-9,水浴加热至40-50℃,进行酶解30-50min,水洗,干燥,得到酶解羊毛织物;
S3、将聚醋酸乙烯酯加入无水乙醇中搅拌溶解得到聚醋酸乙烯酯溶液,向聚醋酸乙烯酯溶液中加入氢氧化钠,搅拌醇解,得到醇解液,将步骤S2得到的酶解羊毛织物放入醇解液中浸泡20-30min,取出后放入戊二醛溶液中,调节pH至3-5,水浴加热至40-45℃,进行交联反应1-3h,然后经过醇洗、干燥,即得。
2.根据权利要求1所述的一种羊毛织物防毡缩整理工艺,其特征在于,其特征在于,所述步骤S2中复合蛋白酶与Tris-HCl缓冲溶液的质量比为1:30-50。
3.根据权利要求1所述的一种羊毛织物防毡缩整理工艺,其特征在于,其特征在于,所述步骤S3中酶解羊毛织物与醇解液的浴比为1:20-30。
4.根据权利要求1所述的一种羊毛织物防毡缩整理工艺,其特征在于,其特征在于,所述步骤S3中戊二醛质量为聚醋酸乙烯酯的5-10wt%。
5.根据权利要求1所述的一种羊毛织物防毡缩整理工艺,其特征在于,其特征在于,所述步骤S2中复合蛋白酶的制备方法包括以下步骤:
将3-缩水甘油醚氧基丙基三乙氧基硅烷加入去离子水中,调节pH至5-6,水浴加热至40-50℃,搅拌水解30-50min,得水解液,将二氧化硅微米颗粒加入水解液中,在45-55℃下保温反应1-2h,洗涤,干燥,得偶联剂改性二氧化硅微米颗粒;向羧甲基纤维素溶液中加入氢氧化钠,搅拌溶解,然后加入偶联剂改性二氧化硅微米颗粒,在50-60℃下反应10-15h,将反应得到的产物加入蛋白酶溶液中,然后添加戊二醛交联剂,调节pH至4-5,在35-40℃下进行反应2-3h,水洗,室温晾干,得到复合蛋白酶。
6.根据权利要求5所述的一种羊毛织物防毡缩整理工艺,其特征在于,其特征在于,所述羧甲基纤维素溶液的质量浓度为3-6%。
7.根据权利要求5所述的一种羊毛织物防毡缩整理工艺,其特征在于,其特征在于,所述戊二醛交联剂添加量为蛋白酶溶液的2-5wt%。
8.根据权利要求5所述的一种羊毛织物防毡缩整理工艺,其特征在于,其特征在于,所述二氧化硅微米颗粒经过预处理,包括以下步骤:将去离子水与无水乙醇混合均匀,滴加醋酸调节pH至2-3,得到溶液a,备用;将钛酸四丁酯与二氧化硅微米颗粒加入无水乙醇中,搅拌均匀,得悬浮液,将溶液a滴加到悬浮液中,滴加完毕后静置3-6h,离心分离,水洗,干燥,送入马弗炉中进行煅烧处理,冷却,即得。
9.根据权利要求8所述的一种羊毛织物防毡缩整理工艺,其特征在于,其特征在于,所述去离子水与无水乙醇的体积比为1:3-5。
10.根据权利要求8所述的一种羊毛织物防毡缩整理工艺,其特征在于,其特征在于,所述钛酸四丁酯与二氧化硅微米颗粒的质量比为1:4-8。
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