CN114887557A - 一种co2-温度双重响应型壳聚糖复合微胶囊的制备方法及其应用 - Google Patents
一种co2-温度双重响应型壳聚糖复合微胶囊的制备方法及其应用 Download PDFInfo
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Abstract
本发明提供了一种CO2‑温度双重响应型壳聚糖复合微胶囊的制备方法及其应用,属于纺织加工技术领域。本发明以壳聚糖和二氧化硅作为壁材,同时分别加入CO2响应低聚物和温度响应低聚物,以植物精油作为芯材,并通过单凝聚‑溶胶凝胶法制得壳聚糖复合微胶囊;再将所得微胶囊配置成微胶囊整理液,以浸渍法对无纺布进行微胶囊整理,最终得到微胶囊整理织物。本发明采用的材料具有生物降解性、无毒性、抑菌等多种生理功能以及较好的机械强度与韧性,由于微胶囊在CO2和温度响应下可释放内部精油,整理的无纺布在受到外界环境条件影响时达到缓释香味的功效,具有优异抗菌、抗病毒等作用。
Description
技术领域
本发明属于纺织加工制备技术领域,具体涉及一种CO2-温度双重响应型壳聚糖复合微胶囊的制备方法及其在应用。
背景技术
随着生活质量的改善,人们对于香味保健纺织品的需求也在提高。但植物精油易于挥发且有效成分不稳定,随着环境条件的变化,释放香味的速度不稳定,难以达到长久释香的效果,且由于贮藏、运输不便限制了其应用范围。此外,对于纺织品的附加价值,例如洁净空气、杀菌消毒、舒缓情绪等功能也在不断完善。因此,设计具有CO2-O2双气体响应、温敏响应的壳聚糖复合微胶囊,一方面使用微胶囊技术将植物精油包封起来,降低植物精油的挥发损失,保护植物精油免受光、氧、热的影响,并且能通过CO2-O2双气体响应、温敏响应控制其缓慢释放,达到持久留香的目的;另一方面使之随环境变化缓慢释放香味进入外界,还能满足抗菌除臭、改善情绪的特性。
目前,专利CN113712144A公开了一种抗菌的玫瑰天竺葵精油微胶囊的制备方法,以多糖和蛋白质为壁材与芯材乳化,通过复凝聚法制备微胶囊,精油包裹在微胶囊中,提高稳定性,具有抗氧化作用和抑菌作用;专利CN113854464A公开了一种柑橘精油微胶囊制备方法,将壳聚糖季铵盐与海藻酸钠、醋酸和水混合,得到壁材溶液,乳化后进行复凝聚反应,再与氯化钙混合,交联固化得到柑橘精油微胶囊,这种微胶囊包埋率较高,能缓慢释放芯材,延长香味。这两种胶囊都可使织物具有抗菌或释放香味的能力,但单一的微胶囊功能有限制,不能满足可控释放的需求,因此,合成既具CO2-O2双气体响应、温敏响应缓释香精功能,还具抗菌作用的复合微胶囊具有重大意义。
发明内容
针对现有技术的不足,本发明提供了一种CO2-温度双重响应型壳聚糖复合微胶囊的制备方法及其在应用,该壳聚糖复合微胶囊的表面接枝CO2-O2双气体响应低聚物和温度响应低聚物,赋予微胶囊在CO2和温度响应下可缓慢释放内部精油的性能,使得纺织品具有香味长效性,同时采用的材料具有生物降解性、无毒性、抑菌等多种生理功能以及较好的机械强度与韧性,用此壳聚糖微胶囊制备的纺织品不仅具有香味缓释性还具有优异的抗菌、抗病毒等性能。
为解决现有技术问题,本发明采取的技术方案为:
一种CO2-温度双重响应型壳聚糖复合微胶囊的制备方法,以壳聚糖和二氧化硅作为壁材,同时加入CO2-O2双气体响应低聚物和温度响应低聚物,以植物精油作为芯材,并通过单凝聚-溶胶凝胶法制得壳聚糖复合微胶囊。
优选的是,上述CO2-温度双重响应型壳聚糖复合微胶囊的制备方法,具体步骤如下:称取植物精油1-30份、正硅酸乙酯0.5-5份、CO2-O2双气体响应低聚物0.1-5份,温度响应低聚物0.1-5份,去离子水10-150份,曲拉通X-100 0.5-10份,质量分数为1%-5%的壳聚糖醋酸溶液5-50份;将植物精油、正硅酸乙酯、CO2-O2双气体响应低聚物和温度响应低聚物加入到去离子水中,并加入曲拉通X-100,搅拌形成稳定乳液;再将乳液置于30-80℃恒温水浴锅中,再加入1%-5%的壳聚糖醋酸溶液,调节pH值至8,在搅拌速度500rpm下反应3-8小时,反应结束后,对微胶囊悬浮液进行抽滤,并用无水乙醇多次淋洗去除表面杂质,在0-5℃下真空干燥,即得粒径为1-100μm的壳聚糖复合微胶囊。
进一步优选的是,所述CO2-O2双气体响应低聚物的装备方法为:按重量份数称取2-(二甲基胺基)甲基丙烯酸乙酯1-10份,3-(五氟苯基)五氟-1-丙烯1-10份,γ-甲基丙烯酰氧基丙基三甲氧基硅烷1-5份,偶氮二异丁腈0.1-1份;将2-(二甲基胺基)甲基丙烯酸乙酯与3-(五氟苯基)五氟-1-丙烯加入到聚合管中,抽真空充氮气3次,再往聚合管中加入γ-甲基丙烯酰氧基丙基三甲氧基硅烷和偶氮二异丁腈,密封聚合管,在30-80℃下聚合反应3-8小时,经终止、沉降、干燥、纯化后得到含硅烷偶联剂的CO2-O2双气体响应低聚物。
进一步改进的是,所述温度响应低聚物的制备方法为:按重量份数称取以下组分:N-异丙基丙烯酰胺1-10份,γ-甲基丙烯酰氧基丙基三甲氧基硅烷1-5份,偶氮二异丁腈0.1-1份,甲醇10-50份;将N-异丙基丙烯酰胺、γ-甲基丙烯酰氧基丙基三甲氧基硅烷和偶氮二异丁腈溶解到甲醇中,在30-80℃反应3-8小时后,经过离心、水洗、烘干得到含硅烷偶联剂的温敏响应低聚物。
优选的是,所述植物精油为艾草、柠檬、薄荷、百里香、葡萄柚、丁香、肉桂、茶树精油中的一种或几种的混合物。
基于方法制备的壳聚糖复合微胶囊在整理无纺布上的应用。
优选的是,具体步骤如下:将无纺布放入去离子水中浸泡30-35min,以去除其表面的杂质,取出晾干后备用。预处理后的无纺布浸入到复合微胶囊整理液中,浴比为1:30-50,浸渍时间0.5-3小时,浸渍温度20-50℃,随后将整理后的无纺布高温80-120℃下烘焙1-5分钟,最后得到微胶囊整理的无纺布。
进一步改进的是,所述复合微胶囊整理液由壳聚糖微胶囊与粘合剂按照质量比为1-5:1。
进一步改进的是,所述粘合剂为丝胶蛋白、阿拉伯树胶、聚氨酯、或聚酰亚胺中的一种或几种的混合物。
上述无纺布在制备医用防护用品或家纺用品上的应用。
有益效果
与现有技术相比,本发明一种CO2-温度双重响应型壳聚糖复合微胶囊的制备方法及其在应用,具有如下优势:
(1)壳聚糖复合微胶囊中CO2-O2双气体响应、温敏响应的聚合物赋予微胶囊气体触发与温度响应控释香味的性能;
(2)壳聚糖具有生物降解性、无毒性、抑菌等多种生理功能,具有低成本、可持续和绿色环保的优点,且材料来源广泛;
(3)植物精油具有优异的抗氧化、抗病毒、抗菌、抗炎等作用,还起到放松情绪、改善睡眠的实质性作用;
(4)经过微胶囊后整理的无纺布具有良好的香味缓释和抗菌抗病毒性能。
附图说明
图1为实施例1制备的薄荷精油微胶囊在(a)×1.3k倍和(b)×3k倍下的扫描电镜SEM图;
图2为实施例5制备的柠檬精油微胶囊在不同温度下的释放曲线;
图3为实施例2制备的艾草精油微胶囊在正常大气和CO2环境下的释放曲线;
图4为本发明复合微胶囊CO2-温度双重响应释放机理。
具体实施方式
下面结合实施例对本发明作进一步详细的描述,但本发明的实施方式不限于此。
实施例1
(1)将2份的2-(二甲基胺基)甲基丙烯酸乙酯、2份3-(五氟苯基)五氟-1-丙烯加入到聚合管中,抽真空充氮气3次,再往聚合管中加入1份的γ-甲基丙烯酰氧基丙基三甲氧基硅烷和0.2份偶氮二异丁腈,密封聚合管,在30℃下聚合反应3小时,经终止、沉降、干燥、纯化后得到含硅烷偶联剂的CO2-O2双气体响应低聚物;
(2)将2份的N-异丙基丙烯酰胺、1份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和0.2份偶氮二异丁腈溶解到10份甲醇中,在30℃反应3小时后,经过离心、水洗、烘干得到含硅烷偶联剂的温敏响应低聚物;
(3)将5份薄荷精油、1份正硅酸乙酯、1份CO2-O2双气体响应低聚物和1份温度响应低聚物加入到30份去离子水中,并加入2份曲拉通X-100,搅拌形成稳定乳液,将上述乳液置于30℃恒温水浴锅中,然后将10份1%的壳聚糖醋酸溶液加入其中,最后将溶液pH值调节至8,在搅拌速度500rpm下反应3小时,反应结束后,将微胶囊悬浮液进行抽滤,并用无水乙醇多次淋洗去除表面杂质,在0℃下真空干燥,即可得到粒径为20μm的壳聚糖复合微胶囊。
对上述方法制备的壳聚糖复合微胶囊进行表征,具体如图1所示,从图中可以看出,微胶囊球形较为规整,部分微胶囊表面存在粘结,这是因为壳聚糖分子质量较大,且具有较好的吸附性,溶液粘度相对较高,在发生单凝聚反应时容易发生粘结。
(4)将无纺布放入去离子水中浸泡30min,以去除其表面的杂质,取出晾干后备用;预处理后的无纺布浸入到壳聚糖复合微胶囊整理液(壳聚糖微胶囊与粘合剂按照质量比为1:1)中,浴比为1:30,浸渍时间1小时,浸渍温度20℃,随后将整理后的无纺布高温80℃下烘焙3分钟,得到微胶囊整理的无纺布。
对步骤(4)制备的微胶囊整理的无纺布进行抗菌性能测试,测试方法参照GB-T20944.3—2008《纺织品抗菌性能的评价第3部分:振荡法》。
表1薄荷精油微胶囊处理无纺布的抗菌性能
其中,表中1、2、3号样是实施例1中未经微胶囊处理的无纺布的空白样品,4、5、6号样是实施例1中经薄荷精油微胶囊处理后的无纺布的样品,为同一参数下的三块样品。
从表1可以看出,薄荷精油微胶囊整理的无纺布对大肠杆菌的抗菌率是92.4%,对金黄色葡萄球菌的抗菌率是87.9%。相较于未经处理的空白无纺布,复合微胶囊整理后的无纺布细菌数量明显减少。复合微胶囊整理的无纺布的抗菌性能一方面来自微胶囊中包裹的薄荷精油,另一方面来自作为壁材的壳聚糖的天然抗菌性能,从而使整理后的无纺布具有良好的抗菌性。
实施例2
(1)将4份的2-(二甲基胺基)甲基丙烯酸乙酯、3份3-(五氟苯基)五氟-1-丙烯加入到聚合管中,抽真空充氮气3次,再往聚合管中加入2份的γ-甲基丙烯酰氧基丙基三甲氧基硅烷和0.4份偶氮二异丁腈,密封聚合管,在40℃温度下聚合反应4小时,经终止、沉降、干燥、纯化后得到含硅烷偶联剂的CO2-O2双气体响应低聚物;
(2)将4份的N-异丙基丙烯酰胺、2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和0.4份偶氮二异丁腈溶解到20份甲醇中,在40℃反应4小时后,经过离心、水洗、烘干得到含硅烷偶联剂的温敏响应低聚物;
(3)将10份艾草精油、2份正硅酸乙酯、2份CO2-O2双气体响应低聚物和2份温度响应低聚物加入到50份去离子水中,并加入3份曲拉通X-100,搅拌形成稳定乳液,将上述乳液置于40℃恒温水浴锅中,然后将20份2%的壳聚糖醋酸溶液加入其中,最后将溶液pH值调节至8,在搅拌速度500rpm下反应4小时。反应结束后,将微胶囊悬浮液抽滤,并用无水乙醇多次淋洗去除表面杂质,在1℃下真空干燥,即可得到壳聚糖复合微胶囊;
对上述壳聚糖复合微胶囊进行性能检测,检测方法参照紫外分光光度计法进行。
结果如图3所示,从图中可以看出,艾草精油在CO2作用下,释放速率大大增加,而大气条件下CO2浓度较低时释放率较低,达到了CO2控制释放的效果。
(4)将无纺布放入去离子水中浸泡30min,以去除其表面的杂质,取出晾干后备用;预处理后的无纺布浸入到壳聚糖复合微胶囊整理液(壳聚糖微胶囊与粘合剂按照质量比为2:1)中,浴比为1:35,浸渍时间1.5小时,浸渍温度30℃,随后将整理后的无纺布高温90℃下烘焙3分钟,得到微胶囊整理的无纺布。
实施例3
(1)将6份的2-(二甲基胺基)甲基丙烯酸乙酯、6份3-(五氟苯基)五氟-1-丙烯加入到聚合管中,抽真空充氮气3次,再往聚合管中加入3份的γ-甲基丙烯酰氧基丙基三甲氧基硅烷和0.6份偶氮二异丁腈,密封聚合管,在50℃温度下聚合反应5小时,经终止、沉降、干燥、纯化后得到含硅烷偶联剂的CO2-O2双气体响应低聚物。
(2)将6份的N-异丙基丙烯酰胺、3份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和0.1-1份偶氮二异丁腈溶解到10-50份甲醇中,在50℃反应5小时后,经过离心、水洗、烘干得到含硅烷偶联剂的的温敏响应低聚物。
(3)将15份丁香精油、3份正硅酸乙酯、3份CO2-O2双气和3份温度响应低聚物加入到80份去离子水中,并加入3份曲拉通X-100,搅拌形成稳定乳液,将上述乳液置于50℃恒温水浴锅中,然后将30份3%的壳聚糖醋酸溶液加入其中,最后将溶液pH值调节至8,在搅拌速度500rpm下反应5小时。反应结束后,将微胶囊悬浮液抽滤,并用无水乙醇多次淋洗去除表面杂质,在2℃下真空干燥,即可得到壳聚糖复合微胶囊。
(4)将无纺布放入去离子水中浸泡30min,以去除其表面的杂质,取出晾干后备用。预处理后的无纺布浸入到壳聚糖复合微胶囊整理液(壳聚糖微胶囊与粘合剂按照质量比为3:1)中,浴比为1:40,浸渍时间2小时,浸渍温度40℃,随后将整理后的无纺布高温100℃下烘焙3分钟,得到微胶囊整理的无纺布。
实施例4
(1)将8份的2-(二甲基胺基)甲基丙烯酸乙酯、8份3-(五氟苯基)五氟-1-丙烯加入到聚合管中,抽真空充氮气3次,再往聚合管中加入4份的γ-甲基丙烯酰氧基丙基三甲氧基硅烷和0.8份偶氮二异丁腈,密封聚合管,在60℃温度下聚合反应6小时。经终止、沉降、干燥、纯化后得到含硅烷偶联剂的CO2-O2双气体响应低聚物。
(2)将10份的N-异丙基丙烯酰胺、5份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和1份偶氮二异丁腈溶解到50份甲醇中,在60℃反应6小时后,经过离心、水洗、烘干得到含硅烷偶联剂的的温敏响应低聚物。
(3)将20份百里香精油、4份正硅酸乙酯、4份CO2-O2双气和4份温度响应低聚物加入到120份去离子水中,并加入10份曲拉通X-100,搅拌形成稳定乳液,将上述乳液置于60℃恒温水浴锅中,然后将40份4%的壳聚糖醋酸溶液加入其中,最后将溶液pH值调节至8,在搅拌速度500rpm下反应6小时。反应结束后,将微胶囊悬浮液抽滤,并用无水乙醇多次淋洗去除表面杂质,在4℃下真空干燥,即可得到壳聚糖复合微胶囊。
(4)将无纺布放入去离子水中浸泡30min,以去除其表面的杂质,取出晾干后备用;预处理后的无纺布浸入到壳聚糖复合微胶囊整理液(壳聚糖微胶囊与粘合剂按照质量比为4:1)中,浴比为1:45,浸渍时间2.5小时,浸渍温度45℃,随后将整理后的无纺布高温110℃下烘焙3分钟,得到微胶囊整理的无纺布。
实施例5
(1)将10份的2-(二甲基胺基)甲基丙烯酸乙酯、10份3-(五氟苯基)五氟-1-丙烯加入到聚合管中,抽真空充氮气3次,再往聚合管中加入5份的γ-甲基丙烯酰氧基丙基三甲氧基硅烷和1份偶氮二异丁腈,密封聚合管,在70℃温度下聚合反应7小时,经终止、沉降、干燥、纯化后得到含硅烷偶联剂的CO2-O2双气体响应低聚物。
(2)将10份的N-异丙基丙烯酰胺、5份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和1份偶氮二异丁腈溶解到50份甲醇中,在80℃反应8小时后,经过离心、水洗、烘干得到含硅烷偶联剂的温敏响应低聚物。
(3)将30份柠檬精油、5份正硅酸乙酯、5份CO2-O2双气和5份温度响应低聚物加入到150份去离子水中,并加入10份曲拉通X-100,搅拌形成稳定乳液,将上述乳液置于80℃恒温水浴锅中,然后将50份5%的壳聚糖醋酸溶液加入其中,最后将溶液pH值调节至8,在搅拌速度500rpm下反应8小时。反应结束后,将微胶囊悬浮液抽滤,并用无水乙醇多次淋洗去除表面杂质,在5℃下真空干燥,即可得到壳聚糖复合微胶囊。
对上述壳聚糖复合微胶囊进行性能检测,检测方法参照紫外分光光度计法进行。
结果如图2所示,从图中可以看出,无纺布在不同温度下柠檬精油的释放效率不同,柠檬精油在较高温度下释放速率大大增加,而在低温下速率较慢,可以达到温度控制的效果。
(4)将无纺布放入去离子水中浸泡30min,以去除其表面的杂质,取出晾干后备用;预处理后的无纺布浸入到壳聚糖复合微胶囊整理液(壳聚糖微胶囊与粘合剂按照质量比为5:1)中,浴比为1:50,浸渍时间3小时,浸渍温度50℃,随后将整理后的无纺布高温120℃下烘焙3分钟,得到微胶囊整理的无纺布。
本发明一种CO2-温度双重响应型壳聚糖复合微胶囊的制备方法及其在应用,该壳聚糖复合微胶囊的表面接枝CO2-O2双气体响应低聚物和温度响应低聚物,赋予微胶囊在CO2和温度响应下可缓慢释放内部精油的性能,使得纺织品具有香味长效性,同时采用的材料具有生物降解性、无毒性、抑菌等多种生理功能以及较好的机械强度与韧性,用此壳聚糖微胶囊制备的纺织品不仅具有香味缓释性还具有优异的抗菌、抗病毒等性能。
Claims (10)
1.一种CO2-温度双重响应型壳聚糖复合微胶囊的制备方法,其特征在于:以壳聚糖和二氧化硅作为壁材,同时加入CO2-O2双气体响应低聚物和温度响应低聚物,以植物精油作为芯材,并通过单凝聚-溶胶凝胶法制得壳聚糖复合微胶囊。
2.根据权利要求1所述的CO2-温度双重响应型壳聚糖复合微胶囊的制备方法,其特征在于,具体步骤如下:称取植物精油1-30份、正硅酸乙酯0.5-5份、CO2-O2双气体响应低聚物0.1-5份,温度响应低聚物0.1-5份,去离子水10-150份,曲拉通X-100 0.5-10份,质量分数为1%-5%的壳聚糖醋酸溶液5-50份;将植物精油、正硅酸乙酯、CO2-O2双气体响应低聚物和温度响应低聚物加入到去离子水中,并加入曲拉通X-100,搅拌形成稳定乳液;再将乳液置于30-80℃恒温水浴锅中,再加入1%-5%的壳聚糖醋酸溶液,调节pH值至8,在搅拌速度500rpm下反应3-8小时,反应结束后,对微胶囊悬浮液进行抽滤,并用无水乙醇多次淋洗去除表面杂质,在0-5℃下真空干燥,即得粒径为1-100 µm的壳聚糖复合微胶囊。
3.根据权利要求2所述的一种CO2-温度双重响应型壳聚糖复合微胶囊的制备方法,其特征在于,所述CO2-O2双气体响应低聚物的装备方法为:按重量份数称取2-(二甲基胺基)甲基丙烯酸乙酯 1-10份,3-(五氟苯基)五氟-1-丙烯 1-10份,γ-甲基丙烯酰氧基丙基三甲氧基硅烷 1-5份,偶氮二异丁腈 0.1-1份;将2-(二甲基胺基)甲基丙烯酸乙酯与3-(五氟苯基)五氟-1-丙烯加入到聚合管中,抽真空充氮气 3次,再往聚合管中加入γ-甲基丙烯酰氧基丙基三甲氧基硅烷和偶氮二异丁腈,密封聚合管,在30-80℃下聚合反应3-8小时,经终止、沉降、干燥、纯化后得到含硅烷偶联剂的CO2-O2双气体响应低聚物。
4.根据权利要求2所述的一种CO2-温度双重响应型壳聚糖复合微胶囊的制备方法,其特征在于,所述温度响应低聚物的制备方法为:按重量份数称取以下组分: N-异丙基丙烯酰胺 1-10份,γ-甲基丙烯酰氧基丙基三甲氧基硅烷1-5份,偶氮二异丁腈0.1-1份,甲醇10-50份;将N-异丙基丙烯酰胺、γ-甲基丙烯酰氧基丙基三甲氧基硅烷和偶氮二异丁腈溶解到甲醇中,在30-80℃反应3-8小时后,经过离心、水洗、烘干得到含硅烷偶联剂的温敏响应低聚物。
5.根据权利要求2所述的一种CO2-温度双重响应型壳聚糖复合微胶囊的制备方法,其特征在于,所述植物精油为艾草、柠檬、薄荷、百里香、葡萄柚、丁香、肉桂、茶树精油中的一种或几种的混合物。
6.基于权利要求1所述方法制备的壳聚糖复合微胶囊在整理无纺布上的应用。
7.根据权利要求6所述的应用,其特征在于,具体步骤如下:将无纺布放入去离子水中浸泡30-35min,以去除其表面的杂质,取出晾干后备用;预处理后的无纺布浸入到复合微胶囊整理液中,浴比为1:30-50,浸渍时间0.5-3小时,浸渍温度20-50℃,随后将整理后的无纺布高温80-120℃下烘焙1-5分钟,最后得到微胶囊整理的无纺布。
8.根据权利要求7所述的应用,其特征在于,所述复合微胶囊整理液由壳聚糖微胶囊与粘合剂按照质量比为1-5:1。
9.根据权利要求7所述的应用,其特征在于,所述粘合剂为丝胶蛋白、阿拉伯树胶、聚氨酯、或聚酰亚胺中的一种或几种的混合物。
10.基于权利要求6-9所述的无纺布在制备医用防护用品或家纺用品上的应用。
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