CN111166001B - 一种能抑制真菌的保温鞋垫及其制备方法 - Google Patents
一种能抑制真菌的保温鞋垫及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种具有抑制真菌功能的新型隔热保温鞋垫及其制备方法,所述保温鞋垫包括依次层叠设置的底层、除菌隔热层和表面透气层,所述除菌隔热层的材料为绝热材料,所述绝热材料的基材为二氧化硅气凝胶,所述二氧化硅气凝胶上负载有药物。本发明的新型保温鞋垫,在底层和表面透气层之间增加了除菌隔热层,通过在隔热层基材—二氧化硅气凝胶制作过程中加入纳米级药物粉末,使除菌隔热层具备吸附净化级保温功能,保证了在热量不会通过鞋垫散失。
Description
技术领域
本发明涉及一种新型保温鞋垫,特别是涉及一种具有抑制真菌功能的新型隔热保温鞋垫及其制备方法。
背景技术
鞋垫是生活中很常见的一种服饰品类,主要功能是保温及减震。传统的鞋垫主要以棉、亚麻或乳胶等材料编织而成,保温性能与如今的新型材料相比相差甚远,且舒适度一般,较差的透气性也会让使用者在长时间穿着后产生真菌感染的症状。如今广泛使用的鞋垫无法满足在极寒等特殊条件下的防寒及舒适需求,因此,开发一种保温效果好且更加舒适的鞋垫尤为必要。
发明内容
本发明为解决传统鞋垫中,保温效果及舒适度不佳,且在穿着过程中易产生真菌感染的问题,而提供一种制备能够有效抑制真菌滋生、增加舒适度、提高保温效果的鞋垫的方法。
本发明包括一种能有效抑制真菌的保温鞋垫的制备方法,所述保温鞋垫包括依次层叠设置的底层、除菌隔热层和表面透气层,所述除菌隔热层的材料为绝热材料,所述绝热材料的基材为二氧化硅气凝胶,所述二氧化硅气凝胶上负载有药物。
进一步地,所述绝热材料的制备方法按如下:
步骤一、纳米级药物粉末的制备:选取硝酸咪康唑、联苯苄唑、醋酸地塞米松、咪康唑氯倍他索、糠酸莫米松、醋酸泼尼松龙或吲哚美辛研磨至纳米级,得到纳米级药物粉末;
步骤二、负载纳米级药物粉体的二氧化硅气凝胶的制备:将纳米级药物粉末加入到甲醇中,再依次加入水和稀盐酸,搅拌3~10min后,加入正硅酸甲酯,得到混合物;将混合物放在温度为70~100℃的油浴中回流搅拌2~8h,自然冷却至室温,加入浓度为0.5~5mol/L的稀氨水调节pH=8~13,然后转移至高压反应釜中,将高压反应釜放入烘箱中,在温度为225~255℃的条件下静置直至凝胶,最后降温至150~170℃持续陈化12~36h,得到湿凝胶;
步骤三、老化:向步骤二中得到的湿凝胶中加入老化液,在温度为70~90℃的条件下老化12~36h;
步骤四、换液:将经步骤三处理的湿凝胶放入等体积量甲醇中进行换液处理,共换液 2~4次,每次换液处理的持续时间为6~24h;换液处理是在温度为70-90℃的恒温鼓风干燥箱中进行的;
步骤五、表面修饰:将催化剂加入到改性剂六甲基二硅胺烷中,得到混合液;再将经步骤四处理的湿凝胶加入到混合液中,在温度为60~80℃条件下静置48~72h;
步骤六、清洗:将经步骤五处理的湿凝胶用醇清洗,直至洗涤液呈中性且醇洗废液中水含量小于2%,以去除其中残留的改性剂、水分及催化剂;
步骤七、干燥:将经步骤六中处理后的湿凝胶梯度升温进行干燥处理,得到负载药物的二氧化硅气凝胶粉体。
进一步地,步骤二中,所述纳米级药物粉末、甲醇、水和浓度为0.5~3.0mol/L的稀盐酸的质量比为1:(35~40):(2.5~3.5):(0.05~0.1);纳米级药物粉末与正硅酸甲酯的质量比为1:(15~20)。
进一步地,步骤二中,使用水热釜,在160℃—255℃的条件下对水溶胶进行凝胶处理。
进一步地,步骤三中,所述老化液是用浓度为0.2mol/L的氨水与水按质量比为(0.3~1.0):100配制而成的。
进一步地,,步骤五中,所述催化剂为盐酸、硫酸、磷酸、醋酸、氨水、亚硫酸、磷酸一氢盐、磷酸二氢盐或焦磷酸;催化剂的浓度为1mol/L。
进一步地,步骤七中,所述梯度升温为:升温至60~62℃保持4~4.2h,然后以4~4.5℃ /min的速度升温至80~82℃保持4~4.2h,接着以4~4.5℃/min的速度升温至100~105℃保持2~2.2h,最后以4~4.5℃/min的速度升温至120~130℃保持2~2.2h。
进一步地,所述底层、所述除菌隔热层和所述表面透气层使用热压法封装设置。
本发明还涉及一种根据上述方法制备的能有效抑制真菌的保温鞋垫,所述除菌隔热层的厚度为1mm—2mm。
进一步地,所述面层为亚麻层或织布层,所述底层的材料为聚氨酯橡胶。
本发明的新型保温鞋垫,在底层和表面透气层之间增加了除菌隔热层,通过在隔热层基材—二氧化硅气凝胶制作过程中加入纳米级药物粉末,使除菌隔热层具备吸附净化级保温功能,保证了在热量不会通过鞋垫散失,长期穿着不会导致真菌滋生,且提高了鞋垫整体的柔软度,达到健康、舒适及保温的效果。利用二氧化硅气凝胶优异的吸附性能,可以在制备二氧化硅气凝胶过程中加入一定量的球磨至纳米级的药物,使其附着在气凝胶骨架上,在使用过程中抑制鞋内的真菌繁殖,在保证隔热性及舒适性的同时,更能够避免脚气等其他真菌感染类疾病的发生,适合长时间穿着。
具体实施方式
本发明的能有效抑制真菌的保温鞋垫包括三层。底层为橡胶层,与鞋底直接接触,为层;最上层为表面透气层,与脚底直接接触;两层之间为除菌隔热层,其存在可避免脚部热量的散失,同时避免长期穿着鞋内气体不流通加之温度过高,导致真菌滋生引发足部疾病,二氧化硅气凝胶粉末基材也提升了鞋垫的柔软程度,使穿着更加舒适。
将底层,除菌隔热层以及表面透气层使用热压法依次层叠封装。热压成型时,均匀涂布于除菌隔热层上下表面的环保热熔胶受热熔化,热压后鞋垫一体成型,使得鞋垫的三个部分连接成为一个整体,不会因为脚步用力踩踏碾压是出现打滑或褶皱移位等情况,确保其稳定舒适耐用。此外,还可以采用缝制,黏贴等方法连接固定。
除菌隔热层的材料为绝热材料。在整体中,除菌隔热层起主要作用,包括提高舒适度,抑制鞋内真菌滋生,防止鞋内部热量散失。所选绝热材料为经过溶胶-凝胶法制备得到的二氧化硅气凝胶。在制备气凝胶前驱体的过程中,加入经过球磨至纳米级别的药物粉体,使其附着在二氧化硅气凝胶骨架上,最终形成用于此产品中的特制二氧化硅气凝胶。特制二氧化硅气凝胶具有极大的比表面积,良好的吸附性,耐高温,优异的绝热性能,密度极低,柔软。这一系列的特性使做成的气凝胶鞋垫具有非常高的实用价值。
所述除菌隔热层厚度为1-2mm。除菌隔热层厚度不宜过薄或过厚,会影响产品的舒适性及保温性能。除菌隔热层中气凝胶材料的厚度优选为1.5mm,成本适中且在该厚度下既保证了鞋垫的舒适度,又使得保暖效果明显。
底层使用聚氨酯,但不限于聚氨酯材料。底层与鞋之间应具有较高的摩擦系数,避免穿着过程中出现打滑移位等现象,降低危险系数,提高舒适度。
表面透气层为亚麻材质或纤维棉材质。该层使用透气性良好的材料,确保脚底与除菌隔热层之间良好的通畅性,使鞋内气体顺畅的被吸附到除菌隔热层中,起到抑制真菌滋生的作用。亚麻或棉纤维也保证了鞋垫的舒适性。
此外,表面透气层也可以使用带孔毛皮等材质,但不限于该类型材料,主要保证其透气性和舒适性。
本发明中,绝热材料的制备方法如下:
步骤一、纳米级药物粉末的制备:选取硝酸咪康唑、联苯苄唑、醋酸地塞米松、咪康唑氯倍他索、糠酸莫米松、醋酸泼尼松龙或吲哚美辛研磨至纳米级,得到纳米级药物粉末;
步骤二、负载纳米级药物粉体的二氧化硅气凝胶的制备:将纳米级药物粉末加入到甲醇中,再依次加入水和稀盐酸,搅拌3~10min后,加入正硅酸甲酯,得到混合物;将混合物放在温度为70~100℃的油浴中回流搅拌2~8h,自然冷却至室温,加入浓度为0.5~5mol/L的稀氨水调节pH=8~13,然后转移至高压反应釜中,将高压反应釜放入烘箱中,在温度为225~255℃的条件下静置直至凝胶,最后降温至150~170℃持续陈化12~36h,得到湿凝胶;所述纳米级药物粉末、甲醇、水和浓度为0.5~3.0mol/L的稀盐酸的质量比为1: (35~40):(2.5~3.5):(0.05~0.1);纳米级药物粉末与正硅酸甲酯的质量比为1:(15~20)。
使用水热釜,在160℃—255℃的条件下对水溶胶进行凝胶处理。相对于常压法,抑菌类药物在体系中溶解更充分,更利于凝胶骨架形成后药物粉末的在体系中的均匀分布,且凝胶后的气凝胶骨架更加稳定。
步骤三、老化:向步骤二中得到的湿凝胶中加入老化液,在温度为70~90℃的条件下老化12~36h;所述老化液是用浓度为0.2mol/L的氨水与水按质量比为(0.3~1.0):100配制而成的。
步骤四、换液:将经步骤三处理的湿凝胶放入等体积量甲醇中进行换液处理,共换液 2~4次,每次换液处理的持续时间为6~24h;换液处理是在温度为70-90℃的恒温鼓风干燥箱中进行的;
步骤五、表面修饰:将催化剂加入到改性剂六甲基二硅胺烷中,得到混合液;再将经步骤四处理的湿凝胶加入到混合液中,在温度为60~80℃条件下静置48~72h;所述催化剂为盐酸、硫酸、磷酸、醋酸、氨水、亚硫酸、磷酸一氢盐、磷酸二氢盐或焦磷酸;催化剂的浓度为1mol/L。
步骤六、清洗:将经步骤五处理的湿凝胶用醇清洗,直至洗涤液呈中性且醇洗废液中水含量小于2%,以去除其中残留的改性剂、水分及催化剂;
步骤七、干燥:将经步骤六中处理后的湿凝胶梯度升温进行干燥处理,得到负载药物的二氧化硅气凝胶粉体。梯度升温为:升温至60~62℃保持4~4.2h,然后以4~4.5℃/min 的速度升温至80~82℃保持4~4.2h,接着以4~4.5℃/min的速度升温至100~105℃保持 2~2.2h,最后以4~4.5℃/min的速度升温至120~130℃保持2~2.2h。
具体实施方式一、绝热材料的制备方法如下:
步骤一、纳米级药物粉末的制备:选取硝酸咪康唑研磨至纳米级,得到纳米级药物粉末;
步骤二、负载纳米级药物粉体的二氧化硅气凝胶的制备:将纳米级药物粉末加入到甲醇中,再依次加入水和稀盐酸,搅拌3min后,加入正硅酸甲酯,得到混合物;将混合物放在温度为70℃的油浴中回流搅拌2h,自然冷却至室温,加入浓度为0.5mol/L的稀氨水调节pH=8,然后转移至高压反应釜中,将高压反应釜放入烘箱中,在温度为225℃的条件下静置直至凝胶,最后降温至150℃持续陈化12h,得到湿凝胶;所述纳米级药物粉末、甲醇、水和浓度为0.5mol/L的稀盐酸的质量比为1:35:2.5:0.05;纳米级药物粉末与正硅酸甲酯的质量比为1:15。
使用水热釜,在160℃℃的条件下对水溶胶进行凝胶处理。相对于常压法,抑菌类药物在体系中溶解更充分,更利于凝胶骨架形成后药物粉末的在体系中的均匀分布,且凝胶后的气凝胶骨架更加稳定。
步骤三、老化:向步骤二中得到的湿凝胶中加入老化液,在温度为70℃的条件下老化12h;所述老化液是用浓度为0.2mol/L的氨水与水按质量比为0.3:100配制而成的。
步骤四、换液:将经步骤三处理的湿凝胶放入等体积量甲醇中进行换液处理,共换液 2次,每次换液处理的持续时间为6h;换液处理是在温度为70℃的恒温鼓风干燥箱中进行的;
步骤五、表面修饰:将催化剂加入到改性剂六甲基二硅胺烷中,得到混合液;再将经步骤四处理的湿凝胶加入到混合液中,在温度为60℃条件下静置48h;所述催化剂为盐酸;催化剂的浓度为1mol/L。
步骤六、清洗:将经步骤五处理的湿凝胶用醇清洗,直至洗涤液呈中性且醇洗废液中水含量小于2%,以去除其中残留的改性剂、水分及催化剂;
步骤七、干燥:将经步骤六中处理后的湿凝胶梯度升温进行干燥处理,得到负载药物的二氧化硅气凝胶粉体。梯度升温为:升温至60℃保持4h,然后以4℃/min的速度升温至80℃保持4h,接着以4℃/min的速度升温至100℃保持2h,最后以4℃/min的速度升温至120℃保持2h。
具体实施方式二、绝热材料的制备方法如下:
步骤一、纳米级药物粉末的制备:选取联苯苄唑研磨至纳米级,得到纳米级药物粉末;
步骤二、负载纳米级药物粉体的二氧化硅气凝胶的制备:将纳米级药物粉末加入到甲醇中,再依次加入水和稀盐酸,搅拌10min后,加入正硅酸甲酯,得到混合物;将混合物放在温度为100℃的油浴中回流搅拌8h,自然冷却至室温,加入浓度为5mol/L的稀氨水调节pH=13,然后转移至高压反应釜中,将高压反应釜放入烘箱中,在温度为255℃的条件下静置直至凝胶,最后降温至170℃持续陈化36h,得到湿凝胶;所述纳米级药物粉末、甲醇、水和浓度为3.0mol/L的稀盐酸的质量比为1:40:3.5:0.1;纳米级药物粉末与正硅酸甲酯的质量比为1:20。
使用水热釜,在255℃的条件下对水溶胶进行凝胶处理。相对于常压法,抑菌类药物在体系中溶解更充分,更利于凝胶骨架形成后药物粉末的在体系中的均匀分布,且凝胶后的气凝胶骨架更加稳定。
步骤三、老化:向步骤二中得到的湿凝胶中加入老化液,在温度为90℃的条件下老化36h;所述老化液是用浓度为0.2mol/L的氨水与水按质量比为1.0:100配制而成的。
步骤四、换液:将经步骤三处理的湿凝胶放入等体积量甲醇中进行换液处理,共换液 4次,每次换液处理的持续时间为24h;换液处理是在温度为90℃的恒温鼓风干燥箱中进行的;
步骤五、表面修饰:将催化剂加入到改性剂六甲基二硅胺烷中,得到混合液;再将经步骤四处理的湿凝胶加入到混合液中,在温度为80℃条件下静置72h;所述催化剂为磷酸;催化剂的浓度为1mol/L。
步骤六、清洗:将经步骤五处理的湿凝胶用醇清洗,直至洗涤液呈中性且醇洗废液中水含量小于2%,以去除其中残留的改性剂、水分及催化剂;
步骤七、干燥:将经步骤六中处理后的湿凝胶梯度升温进行干燥处理,得到负载药物的二氧化硅气凝胶粉体。梯度升温为:升温至62℃保持4.2h,然后以4.5℃/min的速度升温至82℃保持4.2h,接着以4.5℃/min的速度升温至105℃保持2.2h,最后以4.5℃/min 的速度升温至130℃保持2.2h。
有益效果:
本发明的鞋垫厚度适中且质量超轻,提升舒适度,降低鞋整体质量,在徒步或极寒地区使用时减轻使用者负担,适用广泛。
气凝胶的柔软度可以适应各种脚型的需求,在穿着过程中保证脚掌最大程度的与鞋垫贴合,降低脚掌所受压强,在徒步或其他长时间穿着情况下令使用者减少疲劳感。气凝胶材料优异的保温性能更大程度上保护鞋内温度不会从鞋底部流失,起到了极佳的保温效果。除菌隔热层中特制气凝胶的使用,对鞋内空气起到了吸附净化的作用,有效抑制了真菌滋生,避免使用者因长时间穿着而导致的脚部真菌感染等疾病。
以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (4)
1.一种能抑制真菌的保温鞋垫的制备方法,其特征在于,所述保温鞋垫包括依次层叠设置的底层、除菌隔热层和表面透气层,所述除菌隔热层的材料为绝热材料,所述绝热材料的基材为二氧化硅气凝胶,所述二氧化硅气凝胶上负载有药物;
其中,所述绝热材料的制备方法按如下:
步骤一、纳米级药物粉末的制备:选取硝酸咪康唑、联苯苄唑、醋酸地塞米松、咪康唑氯倍他索、糠酸莫米松、醋酸泼尼松龙或吲哚美辛研磨至纳米级,得到纳米级药物粉末;
步骤二、负载纳米级药物粉体的二氧化硅气凝胶的制备:将纳米级药物粉末加入到甲醇中,再依次加入水和稀盐酸,搅拌3~10min后,加入正硅酸甲酯,得到混合物;将混合物放在温度为70~100℃的油浴中回流搅拌2~8 h,自然冷却至室温,加入浓度为0.5~5 mol/L的稀氨水调节pH=8~13,然后转移至高压反应釜中,将高压反应釜放入烘箱中,在温度为225~255℃的条件下静置直至凝胶,最后降温至150~170℃持续陈化12~36 h,得到湿凝胶;其中所述纳米级药物粉末、甲醇、水和浓度为0.5~3.0 mol/L的稀盐酸的质量比为1:(35~40):(2.5~3.5):(0.05~0.1);纳米级药物粉末与正硅酸甲酯的质量比为1:(15~20);
步骤三、老化:向步骤二中得到的湿凝胶中加入老化液,在温度为70~90℃的条件下老化12~36 h;其中所述老化液是用浓度为0.2 mol/L的氨水与水按质量比为(0.3~1.0):100配制而成;
步骤四、换液:将经步骤三处理的湿凝胶放入等体积量甲醇中进行换液处理,共换液2~4次,每次换液处理的持续时间为6~24 h;换液处理是在温度为70-90℃的恒温鼓风干燥箱中进行的;
步骤五、表面修饰:将催化剂加入到改性剂六甲基二硅胺烷中,得到混合液;再将经步骤四处理的湿凝胶加入到混合液中,在温度为60~80℃条件下静置48~72 h;其中所述催化剂为盐酸、硫酸、磷酸、醋酸、氨水、亚硫酸、磷酸一氢盐、磷酸二氢盐或焦磷酸;催化剂的浓度为1mol/L;
步骤六、清洗:将经步骤五处理的湿凝胶用醇清洗,直至洗涤液呈中性且醇洗废液中水含量小于2%,以去除其中残留的改性剂、水分及催化剂;
步骤七、干燥:将经步骤六中处理后的湿凝胶梯度升温进行干燥处理,得到负载药物的二氧化硅气凝胶粉体,即得到绝热材料;其中所述梯度升温为:升温至60~62℃保持4~4.2h,然后以4~4.5℃/ min的速度升温至80~82℃保持4~4.2 h,接着以4~4.5℃/ min的速度升温至100~105℃保持2~2.2 h,最后以4~4.5℃/ min的速度升温至120~130℃保持2~2.2 h;
所述底层、所述除菌隔热层和所述表面透气层使用热压法封装。
2.根据权利要求1所述的能抑制真菌的保温鞋垫的制备方法,其特征在于,步骤二中,使用水热釜,在160℃—255℃的条件下对水溶胶进行凝胶处理。
3.一种根据权利要求1所述方法制备的能抑制真菌的保温鞋垫,其特征在于,保温鞋垫包括依次层叠设置的底层、除菌隔热层和表面透气层,所述除菌隔热层的材料为绝热材料,所述绝热材料的基材为二氧化硅气凝胶,所述二氧化硅气凝胶上负载有药物;所述除菌隔热层的厚度为1 mm~2 mm。
4.根据权利要求3所述的能抑制真菌的保温鞋垫,其特征在于,所述表面透气层为亚麻层或织布层,所述底层的材料为聚氨酯橡胶。
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