CN108486882A - 一种抗菌防皱丝绸整理剂的制备方法 - Google Patents
一种抗菌防皱丝绸整理剂的制备方法 Download PDFInfo
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Abstract
本发明提供了一种抗菌防皱丝绸整理剂的制备方法,包括以下步骤:(1)将蚕丝与碳酸钠溶液混合,煮沸,清洗得处理后的蚕丝;(2)将处理后的蚕丝、氯化钙、无水乙醇和去离子水加热搅拌;(3)透析,离心分离取上清液A;(4)取鱼皮,加入氢氧化钙悬浊液,浸泡;(5)冲洗,调节pH,水浴反应;(6)离心后取上清液B;(7)将马来酸单体、衣康酸单体和去离子水加热,缓慢滴加过硫酸钾水溶液;(8)继续搅拌,得溶液C;(9)将上清液A、上清液B、溶液C、表面活性剂、樟树叶提取物、载银壳聚糖和三乙醇胺混合搅拌,脱泡即得。本方法所制备的整理剂具有很好的防皱效果,耐洗性好,稳定性佳,且整理剂的抗菌效果也非常好。
Description
技术领域
本发明涉及一种抗菌防皱丝绸整理剂的制备方法。
背景技术
丝绸是一种纺织品,用蚕丝或合成纤维、人造纤维、短丝等织成;用蚕丝或人造丝纯织或交织而成的织品的总称。在古代,丝绸就是蚕丝(以桑蚕丝为主,也包括少量的柞蚕丝和木薯蚕丝)织造的纺织品。现代由于纺织品原料的扩展,凡是经线采用了人造或天然长丝纤维织造的纺织品,都可以称为广义的丝绸。丝绸作为服装面料,由于存在易折皱、弹性回复差等先天缺陷,因此无法广泛以及更好的应用,另一方面,丝绸很多时候作为一种贴身衣物,其抗菌性也显得尤为重要。因此,研究开发防皱性好,抗菌性佳的整理剂来提高丝绸的性能具有重要的意义。
发明内容
要解决的技术问题:本发明的目的是提供一种抗菌防皱丝绸整理剂的制备方法,所制备的整理剂具有很好的防皱效果,耐洗性好,稳定性佳,且整理剂的抗菌效果也非常好。
技术方案:一种抗菌防皱丝绸整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将10份蚕丝与500-600份碳酸钠溶液混合,煮沸30-40min,用60℃热水清洗,重复2-3次得处理后的蚕丝,其中,碳酸钠溶液中碳酸钠的含量为0.5wt%-0.7wt%;
(2)将1份处理后的蚕丝、10份氯化钙、20份无水乙醇和80份去离子水混合,加热至75-80℃,搅拌2-3h;
(3)转移至透析袋中,在4℃下用去离子水透析2-3天,离心分离取上清液A;
(4)取鱼皮5-7份,加入40-50份氢氧化钙悬浊液,放入冰箱中,在7-8℃下浸泡80-100h,其中,氢氧化钙悬浊液的浓度为1.6g/L;
(5)用蒸馏水冲洗至溶液pH值为9-10,调节pH值至5.0-5.5,在40-60℃水浴下反应6-8h;
(6)离心后取上清液B;
(7)将5-10份马来酸单体、5-10份衣康酸单体和80-100去离子水加入四口烧瓶中,通入氮气,加热70-80℃,缓慢滴加10-15份过硫酸钾水溶液,其中过硫酸钾水溶液的浓度为 2-4mmol/L;
(8)继续搅拌4-5h,得溶液C;
(9)将上清液A、上清液B、溶液C、2-5份表面活性剂、0.5-0.8份樟树叶提取物、1-1.5份载银壳聚糖和1-3份三乙醇胺混合搅拌,脱泡即得。
进一步的,所述表面活性剂包括脂肪醇聚氧乙烯醚硫酸钠、月桂醇硫酸钠、木质素磺酸钠和月桂酸二乙醇酰胺。
进一步的,所述樟树叶提取物的提取方法为:
第一步:将80-100份樟树叶冷冻干燥后粉碎,过40-60目筛;
第二步:加入蒸馏水,使其料液比为1:12,搅拌均匀,在室温下静置3h;
第三步:转移至微波萃取釜中,萃取条件为:功率500W,温度70℃,时间15min;
第四步:过滤后将滤液减压蒸馏干燥即得。
进一步的,所述载银壳聚糖的制备方法为:
第一步:用1%的乙酸溶液配制1.5%的壳聚糖乙酸溶液,边搅拌边加入1.0mol/L AgNO3溶液,继续搅拌15-20 min;
第二步:加入过量的硼氢化钠溶液,即得混合液A;
第三步:取30-50份液体石蜡,加入0.6-1份丙二醇脂肪酸酯,搅拌混合均匀;
第四步:采用恒压漏斗缓慢滴加混合液A,在50℃恒温水浴中继续搅拌30 min;
第五步:用冰水浴骤冷所得混合液体10 min加入体积分数为1.5-2%的戊二醛,交联固化2h;
第六步:离心洗涤,真空冷冻干燥即得。
进一步的,所述鱼皮为草鱼鱼皮、青鱼鱼皮、鲢鱼鱼皮或鳙鱼鱼皮中的一种或几种。
有益效果:
1. 本发明整理剂能与与丝绸纤维形成较长的柔性链,外力作用时,负荷能较均匀分配,使丝绸强力损伤下降。经50次水洗后,丝绸仍保持较高的急弹、缓弹和断裂强力保留率,是因为多羧酸的邻基效应使整理剂与丝绸之间形成的交链不易水解,提高丝绸的防皱性和耐洗性。
2. 本发明整理剂具有很好的防皱效果,丝绸整理后急弹、缓弹和断裂强力保留率分别最高可达264°、299.9°和100.94%,同时经过50次水洗后,其各项性能指标依然很好,具有很好的耐洗性,稳定性佳,且整理剂的抗菌效果也非常好。
具体实施方式
实施例1
一种抗菌防皱丝绸整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将10份蚕丝与500份碳酸钠溶液混合,煮沸30min,用60℃热水清洗,重复2次得处理后的蚕丝,其中,碳酸钠溶液中碳酸钠的含量为0.5wt%;
(2)将1份处理后的蚕丝、10份氯化钙、20份无水乙醇和80份去离子水混合,加热至75℃,搅拌2h;
(3)转移至透析袋中,在4℃下用去离子水透析2天,离心分离取上清液A;
(4)取青鱼鱼皮5份,加入40份氢氧化钙悬浊液,放入冰箱中,在7℃下浸泡80h,其中,氢氧化钙悬浊液的浓度为1.6g/L;
(5)用蒸馏水冲洗至溶液pH值为9,调节pH值至5.0,在40℃水浴下反应6h;
(6)离心后取上清液B;
(7)将5份马来酸单体、5份衣康酸单体和80去离子水加入四口烧瓶中,通入氮气,加热70℃,缓慢滴加10份过硫酸钾水溶液,其中过硫酸钾水溶液的浓度为 2mmol/L;
(8)继续搅拌4h,得溶液C;
(9)将上清液A、上清液B、溶液C、2份脂肪醇聚氧乙烯醚硫酸钠、0.5份樟树叶提取物、1份载银壳聚糖和1份三乙醇胺混合搅拌,脱泡即得。
实施例2
一种抗菌防皱丝绸整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将10份蚕丝与550份碳酸钠溶液混合,煮沸35min,用60℃热水清洗,重复2次得处理后的蚕丝,其中,碳酸钠溶液中碳酸钠的含量为0.6wt%;
(2)将1份处理后的蚕丝、10份氯化钙、20份无水乙醇和80份去离子水混合,加热至75℃,搅拌2.5h;
(3)转移至透析袋中,在4℃下用去离子水透析2天,离心分离取上清液A;
(4)取草鱼鱼皮6份,加入45份氢氧化钙悬浊液,放入冰箱中,在7℃下浸泡85h,其中,氢氧化钙悬浊液的浓度为1.6g/L;
(5)用蒸馏水冲洗至溶液pH值为9.5,调节pH值至5.0,在45℃水浴下反应7h;
(6)离心后取上清液B;
(7)将7份马来酸单体、6份衣康酸单体和90去离子水加入四口烧瓶中,通入氮气,加热75℃,缓慢滴加12份过硫酸钾水溶液,其中过硫酸钾水溶液的浓度为3mmol/L;
(8)继续搅拌4.5h,得溶液C;
(9)将上清液A、上清液B、溶液C、3份月桂醇硫酸钠、1.2份载银壳聚糖和2份三乙醇胺混合搅拌,脱泡即得。
实施例3
一种抗菌防皱丝绸整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将10份蚕丝与550份碳酸钠溶液混合,煮沸35min,用60℃热水清洗,重复3次得处理后的蚕丝,其中,碳酸钠溶液中碳酸钠的含量为0.6wt%;
(2)将1份处理后的蚕丝、10份氯化钙、20份无水乙醇和80份去离子水混合,加热至80℃,搅拌2.5h;
(3)转移至透析袋中,在4℃下用去离子水透析3天,离心分离取上清液A;
(4)取鲢鱼鱼皮6份,加入45份氢氧化钙悬浊液,放入冰箱中,在8℃下浸泡90h,其中,氢氧化钙悬浊液的浓度为1.6g/L;
(5)用蒸馏水冲洗至溶液pH值为9.5,调节pH值至5.5,在50℃水浴下反应7h;
(6)离心后取上清液B;
(7)将8份马来酸单体、8份衣康酸单体和90去离子水加入四口烧瓶中,通入氮气,加热75℃,缓慢滴加13份过硫酸钾水溶液,其中过硫酸钾水溶液的浓度为 3mmol/L;
(8)继续搅拌4.5h,得溶液C;
(9)将上清液A、上清液B、溶液C、4份木质素磺酸钠、0.7份樟树叶提取物、1.3份载银壳聚糖和2份三乙醇胺混合搅拌,脱泡即得。
实施例4
一种抗菌防皱丝绸整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将10份蚕丝与600份碳酸钠溶液混合,煮沸40min,用60℃热水清洗,重复3次得处理后的蚕丝,其中,碳酸钠溶液中碳酸钠的含量为0.7wt%;
(2)将1份处理后的蚕丝、10份氯化钙、20份无水乙醇和80份去离子水混合,加热至80℃,搅拌3h;
(3)转移至透析袋中,在4℃下用去离子水透析3天,离心分离取上清液A;
(4)取鳙鱼鱼皮7份,加入50份氢氧化钙悬浊液,放入冰箱中,在8℃下浸泡100h,其中,氢氧化钙悬浊液的浓度为1.6g/L;
(5)用蒸馏水冲洗至溶液pH值为10,调节pH值至5.5,在40℃-60℃水浴下反应8h;
(6)离心后取上清液B;
(7)将10份马来酸单体、10份衣康酸单体和100去离子水加入四口烧瓶中,通入氮气,加热80℃,缓慢滴加15份过硫酸钾水溶液,其中过硫酸钾水溶液的浓度为 4mmol/L;
(8)继续搅拌5h,得溶液C;
(9)将上清液A、上清液B、溶液C、5份月桂酸二乙醇酰胺、0.8份樟树叶提取物、1.5份载银壳聚糖和3份三乙醇胺混合搅拌,脱泡即得。
对比例1
一种抗菌防皱丝绸整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)取青鱼鱼皮5份,加入40份氢氧化钙悬浊液,放入冰箱中,在7℃下浸泡80h,其中,氢氧化钙悬浊液的浓度为1.6g/L;
(2)用蒸馏水冲洗至溶液pH值为9,调节pH值至5.0,在40℃水浴下反应6h;
(3)离心后取上清液B;
(4)将5份马来酸单体、5份衣康酸单体和80去离子水加入四口烧瓶中,通入氮气,加热70℃,缓慢滴加10份过硫酸钾水溶液,其中过硫酸钾水溶液的浓度为 2mmol/L;
(5)继续搅拌4h,得溶液C;
(6)将上清液B、溶液C、2份脂肪醇聚氧乙烯醚硫酸钠、0.5份樟树叶提取物、1份载银壳聚糖和1份三乙醇胺混合搅拌,脱泡即得。
对比例2
一种抗菌防皱丝绸整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将10份蚕丝与500份碳酸钠溶液混合,煮沸30min,用60℃热水清洗,重复2次得处理后的蚕丝,其中,碳酸钠溶液中碳酸钠的含量为0.5wt%;
(2)将1份处理后的蚕丝、10份氯化钙、20份无水乙醇和80份去离子水混合,加热至75℃,搅拌2h;
(3)转移至透析袋中,在4℃下用去离子水透析2天,离心分离取上清液A;
(4)将5份马来酸单体、5份衣康酸单体和80去离子水加入四口烧瓶中,通入氮气,加热70℃,缓慢滴加10份过硫酸钾水溶液,其中过硫酸钾水溶液的浓度为 2mmol/L;
(5)继续搅拌4h,得溶液C;
(6)将上清液A、溶液C、2份脂肪醇聚氧乙烯醚硫酸钠、0.5份樟树叶提取物、1份载银壳聚糖和1份三乙醇胺混合搅拌,脱泡即得。
对比例3
一种抗菌防皱丝绸整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将10份蚕丝与500份碳酸钠溶液混合,煮沸30min,用60℃热水清洗,重复2次得处理后的蚕丝,其中,碳酸钠溶液中碳酸钠的含量为0.5wt%;
(2)将1份处理后的蚕丝、10份氯化钙、20份无水乙醇和80份去离子水混合,加热至75℃,搅拌2h;
(3)转移至透析袋中,在4℃下用去离子水透析2天,离心分离取上清液A;
(4)取青鱼鱼皮5份,加入40份氢氧化钙悬浊液,放入冰箱中,在7℃下浸泡80h,其中,氢氧化钙悬浊液的浓度为1.6g/L;
(5)用蒸馏水冲洗至溶液pH值为9,调节pH值至5.0,在40℃水浴下反应6h;
(6)离心后取上清液B;
(7)将上清液A、上清液B、2份脂肪醇聚氧乙烯醚硫酸钠、0.5份樟树叶提取物、1份载银壳聚糖和1份三乙醇胺混合搅拌,脱泡即得。
室温浸轧整理液(二浸二轧,轧余率 100%)→预烘(80℃,5min)→焙烘(170-180℃,1-3min)→水洗(60℃,15min)→烘干(80-85℃)。
整理液中本发明整理剂的用量为6%。
表1 抗菌防皱丝绸整理剂的防皱性能
表2 抗菌防皱丝绸整理剂的抗菌性
本发明方法所制备的抗菌防皱丝绸整理剂的防皱性能指标见上表1,我们可以看到本发明整理剂具有很好的防皱效果,丝绸整理后急弹、缓弹和断裂强力保留率分别最高可达264°、299.9°和100.94%,同时经过50次水洗后,其各项性能指标依然很好,具有很好的耐洗性,稳定性佳,且我们可以从表2中看到,整理剂的抗菌效果也非常好。
Claims (5)
1.一种抗菌防皱丝绸整理剂的制备方法,其特征在于:成分按重量份计,包括以下步骤:
(1)将10份蚕丝与500-600份碳酸钠溶液混合,煮沸30-40min,用60℃热水清洗,重复2-3次得处理后的蚕丝,其中,碳酸钠溶液中碳酸钠的含量为0.5wt%-0.7wt%;
(2)将1份处理后的蚕丝、10份氯化钙、20份无水乙醇和80份去离子水混合,加热至75-80℃,搅拌2-3h;
(3)转移至透析袋中,在4℃下用去离子水透析2-3天,离心分离取上清液A;
(4)取鱼皮5-7份,加入40-50份氢氧化钙悬浊液,放入冰箱中,在7-8℃下浸泡80-100h,其中,氢氧化钙悬浊液的浓度为1.6g/L;
(5)用蒸馏水冲洗至溶液pH值为9-10,调节pH值至5.0-5.5,在40-60℃水浴下反应6-8h;
(6)离心后取上清液B;
(7)将5-10份马来酸单体、5-10份衣康酸单体和80-100去离子水加入四口烧瓶中,通入氮气,加热70-80℃,缓慢滴加10-15份过硫酸钾水溶液,其中过硫酸钾水溶液的浓度为 2-4mmol/L;
(8)继续搅拌4-5h,得溶液C;
(9)将上清液A、上清液B、溶液C、2-5份表面活性剂、0.5-0.8份樟树叶提取物、1-1.5份载银壳聚糖和1-3份三乙醇胺混合搅拌,脱泡即得。
2.根据权利要求 1所述的一种抗菌防皱丝绸整理剂的制备方法,其特征在于:所述表面活性剂包括脂肪醇聚氧乙烯醚硫酸钠、月桂醇硫酸钠、木质素磺酸钠和月桂酸二乙醇酰胺。
3.根据权利要求 1所述的一种抗菌防皱丝绸整理剂的制备方法,其特征在于:所述樟树叶提取物的提取方法为:
第一步:将80-100份樟树叶冷冻干燥后粉碎,过40-60目筛;
第二步:加入蒸馏水,使其料液比为1:12,搅拌均匀,在室温下静置3h;
第三步:转移至微波萃取釜中,萃取条件为:功率500W,温度70℃,时间15min;
第四步:过滤后将滤液减压蒸馏干燥即得。
4.根据权利要求 1所述的一种抗菌防皱丝绸整理剂的制备方法,其特征在于:所述载银壳聚糖的制备方法为:
第一步:用1%的乙酸溶液配制1.5%的壳聚糖乙酸溶液,边搅拌边加入1.0mol/L AgNO3溶液,继续搅拌15-20 min;
第二步:加入过量的硼氢化钠溶液,即得混合液A;
第三步:取30-50份液体石蜡,加入0.6-1份丙二醇脂肪酸酯,搅拌混合均匀;
第四步:采用恒压漏斗缓慢滴加混合液A,在50℃恒温水浴中继续搅拌30 min;
第五步:用冰水浴骤冷所得混合液体10 min加入体积分数为1.5-2%的戊二醛,交联固化2h;
第六步:离心洗涤,真空冷冻干燥即得。
5.根据权利要求 1所述的一种抗菌防皱丝绸整理剂的制备方法,其特征在于:所述鱼皮为草鱼鱼皮、青鱼鱼皮、鲢鱼鱼皮或鳙鱼鱼皮中的一种或几种。。
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