CN110029443B - 一种山茶籽油纤维膜料的应用 - Google Patents

一种山茶籽油纤维膜料的应用 Download PDF

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CN110029443B
CN110029443B CN201910440044.9A CN201910440044A CN110029443B CN 110029443 B CN110029443 B CN 110029443B CN 201910440044 A CN201910440044 A CN 201910440044A CN 110029443 B CN110029443 B CN 110029443B
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camellia
membrane material
mixed solution
oil
spinning
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CN110029443A (zh
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周心慧
程建华
武士川
于翔
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Guangdong Baohua Agricultural Technology Co., Ltd
South China Institute of Collaborative Innovation
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Guangzhou Chagan Biotechnology Co ltd
South China Institute of Collaborative Innovation
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Abstract

本发明属于膜材料及护肤品领域，公开了一种山茶籽油纤维膜料及其制备方法与应用。所述方法：将茶籽油与助溶剂或增溶剂均匀混合，形成混合液A；将抗氧化剂和溶剂均匀混合，形成混合液B；将混合液A和混合液B互混均匀，形成混合液C；向混合液C中加入高分子聚合物，搅拌溶解，得到纺丝液；所述茶籽油为山茶籽油和或改性山茶籽油；将纺丝液通过静电纺丝制备山茶籽油纤维膜料。本发明的方法能够将山茶籽油均匀附着在纤维内部和表面，茶油缓释过程更长，效果更持久；在使用过程中，山茶籽油能更加充分的利用，而且皮肤更易吸收。本发明的纤维膜料增强了山茶籽油的功效。本发明制备的山茶籽油纤维膜料用于化妆品、卫生用品和/或医疗用品。

Description

一种山茶籽油纤维膜料的应用
技术领域
本发明属于纺织科学与功效护肤品领域，具体涉及一种山茶籽油纤维膜料及其制备方法与应用。
背景技术
山茶籽油、橄榄油、棕榈油、椰子油是世界四大木本植物油，其中山茶籽油是从野生木本油料植物油茶树的果实中提取而成。山茶籽油在中国具有悠久的历史，素有“贡品油”、“月子油”，“东方橄榄油”之称。山茶籽油营养丰富，可恢复皮肤弹性，是皮肤和头皮的保湿剂；同时，对皮肤具有抗敏消炎、抗氧化、抗衰老的作用；此外，还具有促渗透和易渗透的功效。但是山茶籽油中的山茶甙、皂甙、鞣质以及具有抗氧化和消炎功效的角鲨烯与黄酮类等功效物质易被氧化，而山茶籽油作为功效护肤品直接涂抹，油腻感极重。因此解决上述山茶籽油在应用过程中的难题对山茶籽油的功效开发具有重要意义。
静电纺丝技术是利用高压静电场产生纳米级喷丝，形成密度可控、表面均匀的薄膜，静电纺丝技术也是迄今最为有效的制备连续纳米纤维的方法之一。通过这种方法制备的纳米微米纤维膜具有比表面积大、孔隙率高、质量轻等优点。采用与功能性纳米粒子或功能性溶液进一步复合的方法可以使电纺纤维膜材料充分发挥其独特的优势并在众多领域拥有广阔的应用前景。
目前，功能性山茶籽油膜料大都是通过机械喷涂或者浸渍的方法将山茶籽油附着在膜料上，而这些方法只能将茶籽油附着在膜料表面，并且存在茶籽油分布不均、附着力不强、易氧化变质、肤感油腻等缺点。现有的茶籽油膜料功效较弱、稳定性较差，并且不能满足山茶籽油膜料的社会需求。
发明内容
为了克服现有技术的缺点和不足，本发明的目的在于提供一种山茶籽油纤维膜料及其制备方法。
本发明的另一目的在于提供上述山茶籽油纤维膜料的应用。所述山茶籽油纤维膜料在化妆品、卫生用品和/或医疗用品中的应用。
本发明的目的通过以下技术方案实现：
一种山茶籽油纤维膜料的制备方法，具体包括以下步骤：
(1)纺丝液的配置
首先将茶籽油与助溶剂或增溶剂均匀混合，形成混合液A；其次将抗氧化剂和溶剂均匀混合，形成混合液B；再次，将混合液A和混合液B互混均匀，形成混合液C；最后，向混合液C中加入高分子聚合物，搅拌溶解，得到纺丝液；所述茶籽油为山茶籽油和或改性山茶籽油；
(2)静电纺丝制备山茶籽油纤维膜料
将纺丝液通过静电纺丝技术进行纺丝成膜，获得山茶籽油纤维膜料。
步骤(2)中纺丝液在进行纺丝前需静置，去除纺丝液中的气泡。
步骤(1)中所述改性山茶籽油购自广州潮徽生物科技有限公司， RunmoistTMCE。
步骤(1)中所述助溶剂或增溶剂为PEG-40氢化蓖麻油、癸基葡糖苷、椰油基葡糖苷、吐温-20中的一种或几种；所述助溶剂或增溶剂在混合液C中的质量浓度为0.02％～3％。
步骤(1)中所述抗氧化剂为维生素E、迷迭香提取物、茶多酚、丁羟甲苯中的一种或几种；所述抗氧化剂在混合液C中质量浓度为0.01％～3％。
步骤(1)中所述溶剂为水、乙醇、N,N-二甲基甲酰胺、四氢呋喃、甲酸中的一种或几种。
步骤(1)中所述高分子聚合物为聚乙烯醇(PVA)、聚丙烯腈(PAN)、聚丙烯(PP)、聚氧化乙烯(PEO)、聚氨酯(PU)、尼龙(PA6)、聚乙烯吡咯烷酮(PVP)中的一种或几种；
所述PVA的分子量为5-20W；PAN的分子量为7-30W；PEO的分子量为 20-100W；PVP的分子量大于100W。
所述高分子聚合物在纺丝液中的质量浓度为2％～15％。
步骤(1)中山茶籽油在混合液C中的质量浓度为0.05％～3％。
步骤(2)中所述静电纺丝技术为针筒静电纺丝技术或金属丝静电纺丝技术。其中针头式静电纺丝条件为：纺丝电压：10～25KV；湿度30％～50％；温度：20～25℃；接收距离16～22cm。钢丝式静电纺丝条件为：纺丝电压：12～50KV；湿度30～50％；温度：20～25℃；接收距离18～25cm。
步骤(2)中所述纺丝成膜中纤维接收基底为无纺布、金箔、铝箔、喷金膜、碳纤维、果浆纤维、蚕丝和天然纤维素中的一种或多种衬底。
上述山茶籽油纤维膜料在化妆品、卫生用品和/或医疗用品中的应用，尤其是在面膜、尿不湿膜料、姨妈巾、创口贴膜料方面的应用。
与现有技术相比，本发明具有如下优点及有益效果：
(1)本发明采用静电纺丝技术将山茶籽油均匀附着在纤维内部和表面，附着量高，茶油缓释过程更长，效果更持久。
(2)本发明采用静电纺丝技术制备的山茶籽油纤维膜料，能够通过高压电场将山茶籽油随高分子聚合物劈裂成纳米微球，同时不破坏山茶籽油中的功效成分，并且能使山茶籽油均匀分布在纤维内部、表面及整个膜料上。在使用过程中，山茶籽油能更加充分的利用，而且皮肤更易吸收。
(3)本发明制备的山茶籽油纤维膜料不仅可以更加充分的发挥山茶籽油的功效，而且纤维对山茶籽油本身具有保护作用，提升山茶籽油的抗氧化性能。
附图说明
图1为实施例1所制备山茶籽油纤维膜料A的扫描电镜图；
图2为实施例2所制备山茶籽油纤维膜料B的扫描电镜图；
图3为实施例3所制备山茶籽油纤维膜料C的扫描电镜图；
图4为实施例4所制备山茶籽油纤维膜料D的扫描电镜图；
图5为喷涂膜料的扫描电镜图；
图6为实施例1制备的膜料A和实施例2制备的膜料B以及喷涂膜料的受损皮肤水分流失变化趋势图；
图7为实施例1制备的膜料A和实施例2制备的膜料B以及喷涂膜料的受损皮肤红血丝变化趋势图；
图8为实施例1制备的膜料A和实施例2制备的膜料B以及喷涂膜料的使用者调查问卷结果柱状图。
具体实施方式
下面结合具体实施例对本发明作进一步详细地描述，但本发明的实施方式不限于此。
实施例1
(1)将10g PEG-40氢化蓖麻油与10g癸基葡糖苷混合均匀，配置成增溶剂；将0.50g山茶籽油与0.50g增溶剂混合均匀，形成混合液A；然后将0.80g 茶多酚和48.20g蒸馏水在超声条件下混合均匀，形成混合液B；将混合液A和混合液B互混，充分搅拌，形成混合液C；最后，向混合液C中缓慢2.0g PVA (PVA的分子量为85000)，90℃水浴条件下搅拌5h，得到纺丝液A；
(2)使用步骤(1)所得的纺丝液A进行静电纺丝，纺丝设备为针筒式静电纺丝机，纤维接收基底为铝箔；纺丝电压17.6KV，针头与纤维接收基底距离为21.8cm，温度为常温，空气湿度40％，纺丝时间30min后，揭下膜料于45℃条件下真空干燥10小时，得到山茶籽油纤维膜料A。
实施例2
(1)将0.50g改性山茶籽油(广州潮徽生物科技有限公司，RunmoistTMCE) 与0.50gPEG-40氢化蓖麻油混合均匀，形成混合液A；然后将0.75g维生素E、 0.05g迷迭香提取物和48.20g乙醇在超声条件下混合均匀，形成混合液B；将混合液A和混合液B互混，充分搅拌，形成混合液C；最后，向混合液C中缓慢 2.0g PVP(分子量1300000)，70℃水浴条件下搅拌5h，得到纺丝液B；
(2)使用步骤(1)所得的纺丝液B进行静电纺丝，纺丝设备为钢丝式静电纺丝机，纤维接收基底为无纺布；纺丝电压17.6KV，针头与纤维接收基底距离为22.1cm，温度为常温，空气湿度低于40％，纺丝时间30min后，揭下膜料于55℃条件下真空干燥10小时，得到山茶籽油纤维膜料B。
实施例3
(1)将1.50g改性山茶籽油(广州潮徽生物科技有限公司，RunmoistTMCE) 与1.00g椰油基葡糖苷混合均匀，形成混合液A；然后将1.50g迷迭香提取物和 46.0g去离子水在超声条件下混合均匀，形成混合液B；将混合液A和混合液B 互混，充分搅拌，形成混合液C；最后，向混合液C中缓慢2.0g PEO(分子量 600000)，50℃水浴条件下搅拌5h，得到纺丝液C；
(2)使用步骤(1)所得的纺丝液C进行静电纺丝，纺丝设备为钢丝式静电纺丝机，纤维接收基底为无纺布；纺丝电压15.0KV，针头与纤维接收基底距离为21cm，温度为常温，空气湿度低于40％，纺丝时间30min后，揭下膜料于 55℃条件下真空干燥10小时，得到山茶籽油纤维膜料C。
实施例4
将0.05g改性山茶籽油(广州潮徽生物科技有限公司，RunmoistTMCE)与 0.05g吐温20混合均匀，形成混合液A；然后将0.10g丁羟甲苯和49.80g甲酸在超声条件下混合均匀，形成混合液B；将混合液A和混合液B互混，充分搅拌，形成混合液C；最后，向混合液C中缓慢2.0g尼龙6(73G30HSL，美国杜邦)，常温下搅拌5h，得到纺丝液D；
(2)使用步骤(1)所得的纺丝液D进行纺丝，纺丝设备为钢丝式静电纺丝机，纤维接收基底为无纺布；纺丝电压12.6KV，针头与纤维接收基底距离为 22.1cm，温度为常温，空气湿度低于40％，纺丝时间30min后，揭下膜料于55℃条件下真空干燥10小时，得到山茶籽油纤维膜料D。
表征测试：
SEM表征分析：采用MERLIN场发射扫描电子显微镜(Carl Zeiss公司，德国)分别对实施例1～5制备的山茶籽油纤维膜料A～D和喷涂膜料(喷涂所用的液体为实施例2中纺丝液B，喷涂量与单张纺丝面膜用量相同，接收基材为无纺布)的表面形貌进行表征。结果分别如图1～5所示。图1为实施例1所制备山茶籽油纤维膜料A的扫描电镜图；图2为实施例2所制备山茶籽油纤维膜料 B的扫描电镜图；图3为实施例3所制备山茶籽油纤维膜料C的扫描电镜图；图4为实施例4所制备山茶籽油纤维膜料D的扫描电镜图；图5为喷涂膜料的扫描电镜图。
图1～4可知，从膜料A、B、C和D中的纳米纤维十分均匀，说明茶油在纺丝液中溶解或者分散均匀，同时也表明茶油在纤维内部和表面分布均匀，而图5 显示，喷涂后的膜料呈有沟壑的块状。
效果测试：
(1)选择合适的受试者(10人次)，测量皮肤损伤前的皮肤经皮水分流失量和皮肤血红素值。然后把3％SLS水溶液置于斑试器中，在受试者手臂上贴敷 24小时以刺激皮肤；揭下斑试器30分钟后，测量皮肤损伤后的皮肤经皮水分流失量和皮肤血红素值；然后在相应区域分别使用喷涂茶油膜料(喷涂所用的液体为实施例2中纺丝液B，喷涂量与单张纺丝面膜用量相同，接收基材为无纺布)、实施例1中膜料A、实施例2中膜料B进行膜敷，3小时后测量皮肤经皮水分流失量和皮肤血红素值；连续使用待测样品2天，每天使用2次，每天均测量皮肤经皮水分流失量和皮肤血红素值。0.9％NaCl溶液为空白对照。利用软件SPSS 19.0对数据进行统计分析。测试结果如图6和7所示。图6为实施例1制备的膜料A和实施例2制备的膜料B以及喷涂膜料的受损皮肤水分流失变化趋势图；图7为实施例1制备的膜料A和实施例2制备的膜料B以及喷涂膜料的受损皮肤红血丝变化趋势图。
抗敏修复效果分析：抗敏修复效果由受损皮肤水分流失变化和红血丝含量变化体现。结果如图6和图7，由图6可知，皮肤受损后，随着时间的推移，水分流失变化量先增加后降低，这是因为皮肤受损后，组织在一定时间内发生水肿，然后才开始恢复。另外，从图中可知，在皮肤损伤后，经膜料A、膜料B 和喷涂膜料敷过的皮肤的水分流失量均下降了，表明三种膜料均可以缓解组织水肿，但是膜料A和膜料B的效果更佳。证明了由本发明方法制备的膜料相比于传统喷涂法制备的膜料具有明显的效果优势。从图7可以得出，皮肤损伤后红血丝随着时间的推移逐渐减少，经三种膜料敷过的皮肤红血丝减少的速率明显更快，其中膜料A和膜料B的降低速率更快，表明膜料A和膜料B具有加快皮肤修复的功效，同时修复功效要强于喷涂型膜料。
(2)选择合适的受试者(10人次)，年龄分布为22-45岁之间，分别使用喷涂茶油膜料(喷涂所用的液体为实施例2中纺丝液B，喷涂量与单张纺丝面膜用量相同，接收基材为无纺布)、实施例1中膜料A、实施例2中膜料B进行膜敷，膜敷前，用清水清洗皮肤并保持皮肤湿润，膜料统一为3*3cm，膜敷20分钟后，取下膜料，10分钟后，让使用者填写调查问卷，调查项目包括膜料的外观感、柔软感，使用后的油腻感、服帖感、滋润感、清爽感、光滑感、保湿感和刺激性，其中膜料的外观感、柔软感，使用后的油腻感、服帖感、滋润感、清爽感、光滑感、保湿感、刺激性分值分布为0-10分，最终结果去10人每项得分的平均值。测试结果如图8所示。图8为实施例1制备的膜料A和实施例2 制备的膜料B以及喷涂膜料的使用者调查问卷结果柱状图。
调查结果如图8所示，由图8可以明显的看到，本发明制备的膜料A和B 油腻感大大降低，对皮肤的刺激性较低，同时在服帖感、滋润感、清爽感、光滑感和保湿感等方面也有不同程度的提升，这是因为使用静电纺丝技术制备的茶油膜更佳均匀，更易吸收。根据使用者调查结果，本发明制备的膜料A和B 相对于喷涂膜料更能得到使用者的肯定。
本发明采用静电纺丝技术将山茶籽油均匀附着在纤维内部和表面，附着量高，茶油缓释过程更长，效果更持久。本发明采用静电纺丝技术制备的山茶籽油纤维膜料，能够通过高压电场将山茶籽油随高分子聚合物劈裂成纳米微球，同时不破坏山茶籽油中的功效成分，并且能使山茶籽油均匀分布在纤维内部、表面及整个膜料上。在使用过程中，山茶籽油能更加充分的利用，而且皮肤更易吸收。而且本发明制备的山茶籽油纤维膜料不仅可以更加充分的发挥山茶籽油的功效，而且纤维对山茶籽油本身具有保护作用，提升山茶籽油的抗氧化性能。

Claims (3)

1.一种山茶籽油纤维膜料的应用，其特征在于：所述山茶籽油纤维膜料用于制备面膜、尿不湿膜料、姨妈巾、创口贴膜料；所述山茶籽油纤维膜料为具有抗敏修复和抗氧化功效的膜料；所述山茶籽油纤维膜料包括通过高压电场形成的山茶籽油纳米微球；
所述山茶籽油纤维膜料通过以下制备方法得到：
（1）纺丝液的配置
首先将茶籽油与助溶剂或增溶剂均匀混合，形成混合液A；其次将抗氧化剂和溶剂均匀混合，形成混合液B；再次，将混合液A和混合液B互混均匀，形成混合液C；最后，向混合液C中加入高分子聚合物，搅拌溶解，得到纺丝液；所述茶籽油为山茶籽油和或改性山茶籽油；
（2）静电纺丝制备山茶籽油纤维膜料
将纺丝液通过静电纺丝技术进行纺丝成膜，获得山茶籽油纤维膜料；
步骤（1）中所述助溶剂或增溶剂为PEG-40氢化蓖麻油、癸基葡糖苷、椰油基葡糖苷中的一种或几种；
步骤（1）中所述高分子聚合物为聚乙烯醇、聚丙烯腈、聚丙烯、聚氧化乙烯、聚氨酯、尼龙、聚乙烯吡咯烷酮中的一种或几种；
所述助溶剂或增溶剂在混合液C中的质量浓度为0.02%~3%；
所述高分子聚合物在纺丝液中的质量浓度为2%~15%；
步骤（1）中茶籽油在混合液C中的质量浓度为0.05%~3%；
步骤（2）中所述静电纺丝技术为针筒静电纺丝技术或金属丝静电纺丝技术；针筒静电纺丝技术中静电纺丝条件为：纺丝电压：10~25KV；湿度30%~50%；温度：20~25℃；接收距离16~22cm；
金属丝静电纺丝技术中静电纺丝条件为：纺丝电压：12~50KV；湿度30~50%；温度：20~25℃；接收距离18~25cm；
步骤（1）中所述抗氧化剂为维生素E、迷迭香提取物、茶多酚、丁羟甲苯中的一种或几种；
步骤（1）中所述溶剂为水、乙醇、N,N-二甲基甲酰胺、四氢呋喃、甲酸中的一种或几种。
2.根据权利要求1所述的应用，其特征在于：
步骤（2）中所述纺丝成膜中纤维接收基底为无纺布、金箔、铝箔、喷金膜、碳纤维、果浆纤维、蚕丝和天然纤维素中的一种或多种衬底。
3.根据权利要求1所述的应用，其特征在于：所述抗氧化剂在混合液C中质量浓度为0.01%~3%。
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