CN108385391B - 一种非均相氧化壳聚糖接枝羊绒制备抗菌羊绒纱线的方法 - Google Patents
一种非均相氧化壳聚糖接枝羊绒制备抗菌羊绒纱线的方法 Download PDFInfo
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Abstract
本发明公开了本发明涉及一种非均相氧化壳聚糖接枝羊绒制备抗菌羊绒纱线的方法。首先是将大分子壳聚糖溶解在离子液体中,加入无水甲醇析出离子液体中的壳聚糖,以无水甲醇浸渍和超声波振荡充分置换出沉淀中的离子液体后得到多孔壳聚糖,再将多孔壳聚糖在离子液体中进行润涨,形成一定粘度的半固态凝胶,然后采用浓硝酸‑浓磷酸‑亚硝酸钠体系在离子液体介质中将壳聚糖吡喃糖环中C6位的部分或全部羟基选择性氧化成羧基而获得非均相氧化壳聚糖,再将非均相氧化壳聚糖制成溶液,接枝在羊绒纱线上,利用氧化壳聚糖上的羧基与羊绒蛋白质中的氨基结合形成酰胺交联键,使羊绒纱线具备抗菌性能。
Description
技术领域
本发明涉及一种非均相氧化壳聚糖接枝羊绒制备抗菌羊绒纱线的方法。
背景技术
羊绒纤维是一种天然珍贵的纺织材料,近年来,羊绒服饰制品在激烈的服装市场竞争中以其手感舒适、质地轻薄、保暖透气性好等特点越来越受到消费者青睐。但随着生态环境对生活用品绿色有好的要求,健康、舒适、环保、安全已经成为人们的消费主题。羊绒制品多作贴身衣物,与人体皮肤接触紧密,人体分泌的汗液体液等物质容易渗透进羊绒纤维的微孔结构和角蛋白,为细菌滋生提供水及营养。因此开发具有亲肤性和抗菌性等特点的、可提升其产品附加值的高档羊绒面料是值得研究的方向。
壳聚糖具有抗炎、抗过敏、杀菌等功效,对金黄色葡萄球菌、链球菌和白喉、枯草、炭疽、副伤寒及痢疾等杆菌均有很强的抑制作用。但壳聚糖分子内和分子间极强的氢键作用使其难溶于水、碱及多数有机溶剂中, 只能溶于醋酸、盐酸、多元羧酸等酸性溶液,极大限制了壳聚糖的应用,且这些酸具有易挥发、难回收、腐蚀性强、污染环境等缺点,难以符合绿色环保要求。因此开发出水溶性壳聚糖对抗菌羊绒纤维制备具有重要作用。
近年来,离子液体作为一种新型的绿色溶剂体系,用于溶解和润涨壳聚糖的离子液体为1-乙基-3-甲基咪唑醋酸盐、1-丁基-3-甲基咪唑醋酸盐、1-烯丙基-3-甲基咪唑氯盐、1-丁基-3-甲基咪唑氯盐、1-氢-3-甲基咪唑氯盐。因其稳定的物理、化学性质,无毒无污染,不挥发,溶解性强,易与产物分离,易回收及可循环使用等优点,在化学合成、生物催化、萃取分离和生物质溶解等领域被视为传统挥发性溶剂的理想替代品,为天然壳聚糖的溶解与应用开辟了新途径。
C6位选择性氧化壳聚糖是壳聚糖衍生物的一种,具有良好的生物相容、生物降解、水溶性、反应性、环境友好和无毒等特性,已被广泛应用。由于壳聚糖是一种易结晶的天然高聚物,分子间存在强烈的氢键作用,反应过程中氧化剂很难进入壳聚糖内部,多数反应只能在聚合物表面无定形区进行,导致氧化反应时间长、壳聚糖氧化度低,且氧化中释放出的大量水分子易使酸性氧化剂降解壳聚糖,羧基壳聚糖产物收率少;同时,用于溶解壳聚糖的无机酸和有机酸存在易挥发、难回收和环境污染等问题。因此,探究绿色环保、高收率的选择性氧化壳聚糖制备的新方法具有重要意义。
发明内容
本发明的目的是提供一种非均相氧化壳聚糖接枝羊绒制备抗菌羊绒纱线的方法,以解决现有技术中的不足,它能够解决传统羊绒制品中抗菌性能、壳聚糖抗菌剂制备工艺等问题。
本发明提供了一种非均相氧化壳聚糖接枝羊绒制备抗菌羊绒纱线的方法, 包括以下步骤:
(1)采用分子量70万脱乙酰度大于95%的壳聚糖与离子液体按1:15~20溶解1~2小时,溶解温度为90~100℃,再加入等体积2~3倍的无水甲醇,进行超声波震荡1~2小时,过滤后再倒入无水甲醇反复过滤清洗3~5次;
(2)将多次过滤清洗后的壳聚糖放入烘箱在90~100℃下烘1~2小时,通过高温使甲醇挥发使壳聚糖表面产生大量孔洞,再将烘干后制得的多孔壳聚糖粉碎至粉末,将干燥的多孔壳聚糖粉末置于离子液体中在30~45℃下进行润胀1~8小时形成半凝胶状态;
(3)向步骤(2)中润胀后的溶液中加入由浓硝酸和浓磷酸按体积比1:0.5~4构成的混合酸和亚硝酸钠,于室温下避光密闭、持续搅拌、非均相氧化反应0.5~6h,生成羧基壳聚糖,所述多孔壳聚糖的质量与所述混合酸的体积的比为1:2~4.5g/mL,所述亚硝酸钠的质量与所述混合酸的体积的比为0.005~0.016g/mL;
(4)等体积2~3倍的无水甲醇终止氧化反应,再将过滤后的壳聚糖产物浸渍在无水甲醇中进行超声波震荡清洗1~2小时 ,如此反复3~5次;
(5)经丙酮洗净、过滤、真空干燥和球磨粉碎后得到选择性氧化壳聚糖;
(6)取氧化壳聚糖溶解成质量浓度为2~4%的溶液,取羊绒纱线与溶液按浴比1:40~60进行浸泡接枝,加入乙酸调节溶液pH=4~5,60℃下接枝2~3小时;
(7)将接枝后的羊绒纱线在80~90℃下烘1~2小时,烘干后使用纯水洗净晾干。
与现有技术相比,本发明的有益效果为:利用离子液体制备非均相选择性氧化壳聚糖,再将选择性氧化壳聚糖溶解对羊绒纱线进行接枝反应,制得具备抗菌性能的羊绒纱线,为制备高品质功能性羊绒面料提供一种技术可实施性,在羊绒抗菌面料应用前景广泛。
具体实施方式
本发明提供了一种非均相氧化壳聚糖接枝羊绒制备抗菌羊绒纱线的方法, 包括以下步骤:
(1)采用分子量70万脱乙酰度大于95%的壳聚糖与离子液体按1:15~20溶解1~2小时,溶解温度为90~100℃,再加入等体积2~3倍的无水甲醇,由于甲醇挥发性强,表面张力小,在干燥时挥发过程可减小壳聚糖分子间的氢键力,使壳聚糖结晶度减小,内部结构疏松,在壳聚糖中形成蓬松的空隙。进行超声波震荡1~2小时,过滤后再倒入无水甲醇反复过滤清洗3~5次;
(2)将多次过滤清洗后的壳聚糖放入烘箱在90~100℃下烘1~2小时,通过高温使甲醇挥发使壳聚糖表面产生大量孔洞,再将烘干后制得的多孔壳聚糖粉碎至粉末,将干燥的多孔壳聚糖粉末置于离子液体中在30~45℃下进行润胀1~8小时形成半凝胶状态;
(3)向步骤(2)中润胀后的溶液中加入由浓硝酸和浓磷酸按体积比1:0.5~4构成的混合酸和亚硝酸钠,采用浓硝酸-浓磷酸-亚硝酸钠体系在离子液体介质中将壳聚糖吡喃糖环中C6位的部分或全部羟基选择性氧化成羧基,于室温下避光密闭、持续搅拌、非均相氧化反应0.5~6h,生成羧基壳聚糖,所述多孔壳聚糖的质量与所述混合酸的体积的比为1:2~4.5g/mL,所述亚硝酸钠的质量与所述混合酸的体积的比为0.005~0.016g/mL;
(4)等体积2~3倍的无水甲醇终止氧化反应,再将过滤后的壳聚糖产物浸渍在无水甲醇中进行超声波震荡清洗1~2小时 ,如此反复3~5次;
(5)经丙酮洗净、过滤、真空干燥和球磨粉碎后得到选择性氧化壳聚糖;
(6)取氧化壳聚糖溶解成质量浓度为2~4%的溶液,取羊绒纱线与溶液按浴比1:40~60进行浸泡接枝,加入乙酸调节溶液pH=4~5,60℃下接枝2~3小时;
(7)将接枝后的羊绒纱线在80~90℃下烘1~2小时,烘干后使用纯水洗净晾干。
本方法是利用选择性氧化壳聚糖的抗菌性,将氧化壳聚糖接枝到羊绒纱线上,使羊绒纤维上蛋白质上的氨基与壳聚糖分子结合,使其具有抗菌性。
本发明的实施例一:
一种非均相氧化壳聚糖接枝羊绒制备抗菌羊绒纱线的方法,包括以下步骤:
(1)称取粘均分子量70w、脱乙酰度大于95%的壳聚糖2.0g与离子液体1-乙基-3-甲基咪唑醋酸盐按1:15进行溶解1小时,溶解温度90℃,再加入100ml的无水甲醇,进行超声波振荡1小时,振荡后过滤使用无水乙醇反复过滤清洗3次;
(2)将步骤(1)中的壳聚糖放入烘箱90℃烘1小时,将烘干后的多孔壳聚糖粉碎研磨成粉末状,置于离子液体1-烯丙基-3-甲基咪唑氯盐中润胀4小时,温度为40℃;
(3)在步骤(2)中的润胀溶液中,加入由浓硝酸和浓磷酸按体积比1:0.5~4构成的混合酸和亚硝酸钠,于室温下避光密闭、持续搅拌、非均相氧化反应2h,所述多孔壳聚糖的质量与所述混合酸的体积的比为1:4g/mL,所述亚硝酸钠的质量与所述混合酸的体积的比为0.014g/mL;
(4)在步骤(3)中加入150ml的无水乙醇,过滤后再浸渍在150ml无水乙醇中采用超声波振荡1小时;
(5)将步骤(4)重复3次后,经丙酮洗净、过滤、真空干燥和球磨粉碎后得到选择性氧化壳聚糖;
(6)将步骤(5)制得的选择性氧化壳聚糖取1g加入50ml纯水中,加入纯羊绒纱线1g,进行接枝反应,接枝温度60℃,调节pH=4.5,接枝时间为2小时;
(7)将步骤(6)中羊绒纱线取出在烘箱中90℃烘1小时,烘干后用纯水洗净晾干。
Claims (1)
1.一种非均相氧化壳聚糖接枝羊绒制备抗菌羊绒纱线的方法,其特征在于:包括以下步骤:
(1)采用分子量70万脱乙酰度大于95%的壳聚糖与离子液体按1:15~20溶解1~2小时,溶解温度为90~100℃,再加入等体积2~3倍的无水甲醇,进行超声波震荡1~2小时,过滤后再倒入无水甲醇反复过滤清洗3~5次;
(2)将多次过滤清洗后的壳聚糖放入烘箱在90~100℃下烘1~2小时,通过高温使甲醇挥发使壳聚糖表面产生大量孔洞,再将烘干后制得的多孔壳聚糖粉碎至粉末,将干燥的多孔壳聚糖粉末置于离子液体中在30~45℃下进行润胀1~8小时形成半凝胶状态;
(3)向步骤(2)中润胀后的溶液中加入由浓硝酸和浓磷酸按体积比1:0.5~4构成的混合酸和亚硝酸钠,于室温下避光密闭、持续搅拌、非均相氧化反应0.5~6h,生成羧基壳聚糖,所述多孔壳聚糖的质量与所述混合酸的体积的比为1:2~4.5g/mL,所述亚硝酸钠的质量与所述混合酸的体积的比为0.005~0.016g/mL;
(4)等体积2~3倍的无水甲醇终止氧化反应,再将过滤后的壳聚糖产物浸渍在无水甲醇中进行超声波震荡清洗1~2小时,如此反复3~5次;
(5)经丙酮洗净、过滤、真空干燥和球磨粉碎后得到选择性氧化壳聚糖;
(6)取氧化壳聚糖溶解成质量浓度为2~4%的溶液,取羊绒纱线与溶液按浴比1:40~60进行浸泡接枝,加入乙酸调节溶液pH=4~5,60℃下接枝2~3小时;
(7)将接枝后的羊绒纱线在80~90℃下烘1~2小时,烘干后使用纯水洗净晾干。
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