CN109137512A - 一种羊毛抗菌除臭整理剂的制备方法 - Google Patents
一种羊毛抗菌除臭整理剂的制备方法 Download PDFInfo
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Abstract
本发明提供了一种羊毛抗菌除臭整理剂的制备方法,包括以下步骤:S1.制备多孔陈皮粉;S2.制备炭化蚕沙;S3.制备活化蚕沙;S4.制备改性多孔蚕沙;S5.用1‑2%的乙酸溶液溶解壳聚糖,得到浓度为2‑5%的壳聚糖溶液,然后壳聚糖溶液依次加入45‑80g/L的1,2,3,4‑四羧酸丁烷,1‑8g/L十二烷基硫酸钠,25‑90g/L多孔陈皮粉,45‑70g/L改性多孔蚕沙和15‑30g/L次亚磷酸钠,在30‑50℃的恒温搅拌2h‑4h,得到羊毛整理剂。
Description
技术领域
本发明涉及羊毛整理剂领域,具体涉及一种羊毛抗菌除臭整理剂的制备方法。
背景技术
羊毛作为一种天然蛋白质纤维,具有其他纤维无法比拟的优点,因而由其织成的产品备受国内外消费者青睐。但近年来羊毛及其混纺服装正向着轻薄夏季、休闲系列和卫生保健方向发展,市场对清新防臭面料的需求增大,而目前的化学防臭整理剂对皮肤的刺激性和生物毒性一直是人们有争议的话题。 在蚕桑资源中,蚕沙占单位面积桑园干物质含量的22%,是蚕桑业主要副产物之一。据统计仅全国五大蚕区干蚕沙的年产量可达百万吨以上。长期以来,蚕沙一般直接用作农田肥料或被丢弃,不仅浪费了大量宝贵的资源,而且直接影响到蚕区蚕病的防疫,不利于蚕桑业的可持续发展。蚕沙资源丰富、营养价值高、成本低、产品多样、市场广阔,开发蚕沙资源具有可观的经济效益和社会效益,是一种具有广阔应用前景的农副产物。桔皮是常用的药引和食物调料。在本研究的目的是有效利用天然物资源,开发低成本、高效、简单、新的整理剂,解决织物抗菌除臭的问题,同时解决资源大量丢弃浪费的现状,促进资源、环境的协调。
发明内容
要解决的技术问题:本发明的目的是提供一种羊毛抗菌除臭整理剂,本发明的抗菌除臭整理剂对羊毛具有很好抗菌除臭的效果。
技术方案:一种羊毛抗菌除臭整理剂的制备方法,包括以下步骤:
S1. 将陈皮粉末加入蒸馏水中,然后滴加盐酸调节溶液至pH4-6,66-85℃水浴加热15-30min,所得混合物趁热用纱布过滤,冷至室温,洗涤自然阴干,然后将陈皮置于-25℃条件下冷冻2-4 h,然后,再将冷冻样品放入台式冷冻干燥机中,于-50--80℃冷冻干燥12-24 h后,取出并研磨成400-800目粉末,得到多孔陈皮粉;
S2. 选用二龄蚕沙,将蚕沙用去离子水洗净,于100℃下烘干,然后将蚕沙放入管式炉中,通入N2以3℃/min升温至300℃,然后以5℃/min升温600℃,再保温炭化2 h,研磨过100-150目筛,得到炭化蚕沙;
S3. 将步骤S2制备得到的炭化蚕沙通入CO2进行二次活化,10℃/min升温400-600℃,得到活化蚕沙;
S4. 将步骤S3制备得到活化蚕沙加入至双氧水溶液中,活化蚕沙和双氧水的质量比为5:3-4,然后在65-80℃下回流反应3-6h,反应结束后将蚕沙洗涤至中性,干燥得到改性多孔蚕沙;
S5. 用1-2%的乙酸溶液溶解壳聚糖,得到浓度为2-5%的壳聚糖溶液,然后壳聚糖溶液依次加入45-80g/L的1,2,3,4-四羧酸丁烷,1-8g/L十二烷基硫酸钠,25-90g/L多孔陈皮粉,45-70g/L改性多孔蚕沙和15-30g/L次亚磷酸钠,在30-50℃的恒温搅拌2h-4h,得到羊毛整理剂。
进一步的,步骤S1中所述冷冻干燥的温度为-55--70℃,干燥时间为15-20 h。
进一步的,步骤S4中回流反应的温度为70-75℃,时间为4-5h。
进一步的,步骤S5中在壳聚糖溶液中加入1,2,3,4-四羧酸丁烷,十二烷基硫酸钠,多孔陈皮粉,改性多孔蚕沙和次亚磷酸钠的浓度分别为55-70g/L,2-5g/L,45-60g/L,52-65g/L和15-25g/L。
有益效果:本发明的的整理剂具有以下优点:本身陈皮就具有很好的吸附效果,通过冻干处理后得到多孔的陈皮,其吸附效果得到提成,而多孔蚕沙也具有相同的作用,将两种物质混合具有协同的吸附作用,得到的整理剂具有抗菌除臭的效果。
具体实施方式
实施例1
一种羊毛抗菌除臭整理剂的制备方法,包括以下步骤:
S1. 将陈皮粉末加入蒸馏水中,然后滴加盐酸调节溶液至pH=4,66℃水浴加热15min,所得混合物趁热用纱布过滤,冷至室温,洗涤自然阴干,然后将陈皮置于-25℃条件下冷冻2h,然后,再将冷冻样品放入台式冷冻干燥机中,于-80℃冷冻干燥24 h后,取出并研磨成400目粉末,得到多孔陈皮粉;
S2. 选用二龄蚕沙,将蚕沙用去离子水洗净,于100℃下烘干,然后将蚕沙放入管式炉中,通入N2以3℃/min升温至300℃,然后以5℃/min升温600℃,再保温炭化2 h,研磨过100目筛,得到炭化蚕沙;
S3. 将步骤S2制备得到的炭化蚕沙通入CO2进行二次活化,10℃/min升温400℃,得到活化蚕沙;
S4. 将步骤S3制备得到活化蚕沙加入至双氧水溶液中,活化蚕沙和双氧水的质量比为5:3,然后在65℃下回流反应6h,反应结束后将蚕沙洗涤至中性,干燥得到改性多孔蚕沙;
S5. 用1%的乙酸溶液溶解壳聚糖,得到浓度为5%的壳聚糖溶液,然后壳聚糖溶液依次加入45g/L的1,2,3,4-四羧酸丁烷,1g/L十二烷基硫酸钠,90g/L多孔陈皮粉,45g/L改性多孔蚕沙和15g/L次亚磷酸钠,在30℃的恒温搅拌2h,得到羊毛整理剂。
实施例2
一种羊毛抗菌除臭整理剂的制备方法,包括以下步骤:
S1. 将陈皮粉末加入蒸馏水中,然后滴加盐酸调节溶液至pH=6,85℃水浴加热30min,所得混合物趁热用纱布过滤,冷至室温,洗涤自然阴干,然后将陈皮置于-25℃条件下冷冻4h,然后,再将冷冻样品放入台式冷冻干燥机中,于-50℃冷冻干燥12-h后,取出并研磨成800目粉末,得到多孔陈皮粉;
S2. 选用二龄蚕沙,将蚕沙用去离子水洗净,于100℃下烘干,然后将蚕沙放入管式炉中,通入N2以3℃/min升温至300℃,然后以5℃/min升温600℃,再保温炭化2 h,研磨过150目筛,得到炭化蚕沙;
S3. 将步骤S2制备得到的炭化蚕沙通入CO2进行二次活化,10℃/min升温600℃,得到活化蚕沙;
S4. 将步骤S3制备得到活化蚕沙加入至双氧水溶液中,活化蚕沙和双氧水的质量比为5:4,然后在80℃下回流反应3h,反应结束后将蚕沙洗涤至中性,干燥得到改性多孔蚕沙;
S5. 用2%的乙酸溶液溶解壳聚糖,得到浓度为2%的壳聚糖溶液,然后壳聚糖溶液依次加入80g/L的1,2,3,4-四羧酸丁烷,8g/L十二烷基硫酸钠,25g/L多孔陈皮粉,70g/L改性多孔蚕沙和30g/L次亚磷酸钠,在50℃的恒温搅拌4h,得到羊毛整理剂。
实施例3
一种羊毛抗菌除臭整理剂的制备方法,包括以下步骤:
S1. 将陈皮粉末加入蒸馏水中,然后滴加盐酸调节溶液至pH=4,80℃水浴加热15min,所得混合物趁热用纱布过滤,冷至室温,洗涤自然阴干,然后将陈皮置于-25℃条件下冷冻4h,然后,再将冷冻样品放入台式冷冻干燥机中,于-55℃冷冻干燥15 h后,取出并研磨成400目粉末,得到多孔陈皮粉;
S2. 选用二龄蚕沙,将蚕沙用去离子水洗净,于100℃下烘干,然后将蚕沙放入管式炉中,通入N2以3℃/min升温至300℃,然后以5℃/min升温600℃,再保温炭化2 h,研磨过120目筛,得到炭化蚕沙;
S3. 将步骤S2制备得到的炭化蚕沙通入CO2进行二次活化,10℃/min升温550℃,得到活化蚕沙;
S4. 将步骤S3制备得到活化蚕沙加入至双氧水溶液中,活化蚕沙和双氧水的质量比为5:3然后在70℃下回流反应4h,反应结束后将蚕沙洗涤至中性,干燥得到改性多孔蚕沙;
S5. 用1%的乙酸溶液溶解壳聚糖,得到浓度为3%的壳聚糖溶液,然后壳聚糖溶液依次加入55g/L的1,2,3,4-四羧酸丁烷,5g/L十二烷基硫酸钠,60g/L多孔陈皮粉,65g/L改性多孔蚕沙和15g/L次亚磷酸钠,在30℃的恒温搅拌3h,得到羊毛整理剂。
实施例4
一种羊毛抗菌除臭整理剂的制备方法,包括以下步骤:
S1. 将陈皮粉末加入蒸馏水中,然后滴加盐酸调节溶液至pH=6,70℃水浴加热30min,所得混合物趁热用纱布过滤,冷至室温,洗涤自然阴干,然后将陈皮置于-25℃条件下冷冻2h,然后,再将冷冻样品放入台式冷冻干燥机中,于-70℃冷冻干燥20 h后,取出并研磨成800目粉末,得到多孔陈皮粉;
S2. 选用二龄蚕沙,将蚕沙用去离子水洗净,于100℃下烘干,然后将蚕沙放入管式炉中,通入N2以3℃/min升温至300℃,然后以5℃/min升温600℃,再保温炭化2 h,研磨过150目筛,得到炭化蚕沙;
S3. 将步骤S2制备得到的炭化蚕沙通入CO2进行二次活化,10℃/min升温450℃,得到活化蚕沙;
S4. 将步骤S3制备得到活化蚕沙加入至双氧水溶液中,活化蚕沙和双氧水的质量比为5:4,然后在75℃下回流反应5h,反应结束后将蚕沙洗涤至中性,干燥得到改性多孔蚕沙;
S5. 用2%的乙酸溶液溶解壳聚糖,得到浓度为4%的壳聚糖溶液,然后壳聚糖溶液依次加入70g/L的1,2,3,4-四羧酸丁烷,4g/L十二烷基硫酸钠,60g/L多孔陈皮粉,52g/L改性多孔蚕沙和30g/L次亚磷酸钠,在50℃的恒温搅拌3h,得到羊毛整理剂。
实施例5
一种羊毛抗菌除臭整理剂的制备方法,包括以下步骤:
S1. 将陈皮粉末加入蒸馏水中,然后滴加盐酸调节溶液至pH=5,75℃水浴加热20min,所得混合物趁热用纱布过滤,冷至室温,洗涤自然阴干,然后将陈皮置于-25℃条件下冷冻3h,然后,再将冷冻样品放入台式冷冻干燥机中,于-55℃冷冻干燥20 h后,取出并研磨成400-800目粉末,得到多孔陈皮粉;
S2. 选用二龄蚕沙,将蚕沙用去离子水洗净,于100℃下烘干,然后将蚕沙放入管式炉中,通入N2以3℃/min升温至300℃,然后以5℃/min升温600℃,再保温炭化2 h,研磨过150目筛,得到炭化蚕沙;
S3. 将步骤S2制备得到的炭化蚕沙通入CO2进行二次活化,10℃/min升温500℃,得到活化蚕沙;
S4. 将步骤S3制备得到活化蚕沙加入至双氧水溶液中,活化蚕沙和双氧水的质量比为5:4,然后在75℃下回流反应4h,反应结束后将蚕沙洗涤至中性,干燥得到改性多孔蚕沙;
S5. 用2%的乙酸溶液溶解壳聚糖,得到浓度为4%的壳聚糖溶液,然后壳聚糖溶液依次加入65g/L的1,2,3,4-四羧酸丁烷,4g/L十二烷基硫酸钠,55g/L多孔陈皮粉,60g/L改性多孔蚕沙和20g/L次亚磷酸钠,在40℃的恒温搅拌3h,得到羊毛整理剂。
对比例1
对比例1在实施例1的基础上中直接加入常规的陈皮粉,不进行冻干处理。
对比例2
对比例2在实施例1的基础上中直接加入常规的蚕沙,不进行炭化和活化。
将实施例和空白对比例的织物,分别悬挂于10L真空干燥器中,每个干燥器中加入0.05ml氨标液,把干燥器置于恒温培养箱中,25℃放置12h,用大气 采样器以0.4L/min速率采样2.5min,吸收液为20ml蒸馏水。采样结束后,把吸收液用水稀释至100ml容量瓶中。用可见分光光度计在420nm处,以空白溶液为参比,测其吸光度,然后代入氨-吸光度工作曲线,计算干燥器中氨气浓度。
采用振荡烧瓶法测抗菌效果,在盛有稀释液的具塞三角 烧瓶中,投入整理后的织物后加入菌液,37℃条件下在摇床上振荡1 h,取出1mL试验液,置于固体培养基,用稀释平板计数法培养计数,按下式计算抑菌率。
抑菌率=(整理织物浸渍振荡前烧瓶中的平均活菌数-整理织物浸渍振荡后烧瓶中的平均活菌数)/整理织物浸渍振荡前烧瓶中的平均活菌数*100%;
按标准皂洗方法:皂片4g/L,纯碱2g/L,40℃, 浴比1:30,20 min(前、中、后各搅拌1次),作为洗涤1 次.经20次洗涤后,用大肠杆菌进行抗菌效果测试。
。
Claims (4)
1.一种羊毛抗菌除臭整理剂的制备方法,其特征在于,包括以下步骤:
S1. 将陈皮粉末加入蒸馏水中,然后滴加盐酸调节溶液至pH4-6,66-85℃水浴加热15-30min,所得混合物趁热用纱布过滤,冷至室温,洗涤自然阴干,然后将陈皮置于-25℃条件下冷冻2-4 h,然后,再将冷冻样品放入台式冷冻干燥机中,于-50--80℃冷冻干燥12-24 h后,取出并研磨成400-800目粉末,得到多孔陈皮粉;
S2. 选用二龄蚕沙,将蚕沙用去离子水洗净,于100℃下烘干,然后将蚕沙放入管式炉中,通入N2以3℃/min升温至300℃,然后以5℃/min升温600℃,再保温炭化2 h,研磨过100-150目筛,得到炭化蚕沙;
S3. 将步骤S2制备得到的炭化蚕沙通入CO2进行二次活化,10℃/min升温400-600℃,得到活化蚕沙;
S4. 将步骤S3制备得到活化蚕沙加入至双氧水溶液中,活化蚕沙和双氧水的质量比为5:3-4,然后在65-80℃下回流反应3-6h,反应结束后将蚕沙洗涤至中性,干燥得到改性多孔蚕沙;
S5. 用1-2%的乙酸溶液溶解壳聚糖,得到浓度为2-5%的壳聚糖溶液,然后壳聚糖溶液依次加入45-80g/L的1,2,3,4-四羧酸丁烷,1-8g/L十二烷基硫酸钠,25-90g/L多孔陈皮粉,45-70g/L改性多孔蚕沙和15-30g/L次亚磷酸钠,在30-50℃的恒温搅拌2h-4h,得到羊毛整理剂。
2.根据权利要求1所述的羊毛抗菌除臭整理剂的制备方法,其特征在于:步骤S1中所述冷冻干燥的温度为-55--70℃,干燥时间为15-20 h。
3.根据权利要求1所述的羊毛抗菌除臭整理剂的制备方法,其特征在于:步骤S4中回流反应的温度为70-75℃,时间为4-5h。
4.根据权利要求1所述的羊毛抗菌除臭整理剂的制备方法,其特征在于:步骤S5中在壳聚糖溶液中加入1,2,3,4-四羧酸丁烷,十二烷基硫酸钠,多孔陈皮粉,改性多孔蚕沙和次亚磷酸钠的浓度分别为55-70g/L,2-5g/L,45-60g/L,52-65g/L和15-25g/L。
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