CN113968993A - 一种多孔海藻酸盐膜的制备方法及应用 - Google Patents

一种多孔海藻酸盐膜的制备方法及应用 Download PDF

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CN113968993A
CN113968993A CN202111350513.1A CN202111350513A CN113968993A CN 113968993 A CN113968993 A CN 113968993A CN 202111350513 A CN202111350513 A CN 202111350513A CN 113968993 A CN113968993 A CN 113968993A
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汪涛
肖晓蝶
刘子逸
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Southwest University
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Abstract

本发明公开了一种多孔海藻酸盐膜的制备方法及应用，该方法是将海藻酸钠溶液低温冷冻凝固后，再将低熔点的解冻凝固剂注入其中，所述解冻凝固剂由组分质量分数分别为无水乙醇50%~94%、无水氯化钙5%~25%、甘油0.5%~2%和水组成，利用乙醇渗透将其冰晶结构逐渐溶化，同时液化钙离子将解冻中的海藻酸钠大分子迅速交联固化，保留住海藻酸钠大分子冰冻状态的空间结构，从而形成多孔海藻酸盐膜。本发明的制备方法设备工艺条件简单，极大地提高了成孔效率，改善了多孔海藻酸盐膜的机械性能，适合规模化加工。本发明制得的多孔海藻酸盐膜可用于面膜、创伤敷料、止血海绵或细胞支架。

Description

一种多孔海藻酸盐膜的制备方法及应用
技术领域
本发明属于天然高分子材料领域，具体涉及一种多孔海藻酸盐膜的制备方法及应用。
背景技术
海藻酸钠是一种天然多糖类高分子化合物，与人体细胞外基质中的蛋白多糖结构相似，具有良好的生物相容性，生物降解性和安全无毒性。这些优良特性使得海藻酸钠广泛应用于美容保健产品、医疗卫生用品以及组织工程支架等领域。
现有技术中，海藻酸盐膜的制备方法主要有水凝胶法、冷冻干燥法和静电纺丝法，其中冷冻干燥法和静电纺丝法制得多孔海藻酸盐膜。专利CN109675089A 公布了将海藻酸盐、明胶和纳米纤维素共混后，经流延干燥成膜，再用氯化钙溶液交联，然后干燥成膜，用作生物支架材料。专利CN107519535A公布了一种可降解海藻酸钠/丝素双层皮肤组织工程支架材料，以海藻酸钠膜和海藻酸钠/丝素共混溶液复合后，经冷冻干燥处理而成。专利CN107737366A公布了一种改性海藻酸钠电纺纤维止血膜及其制备方法，以巯基化海藻酸钠和聚乙烯醇混合，经静电纺丝方法制备而成。但上述这些方法的多孔成膜技术往往效率低下，膜的机械性能差，且不适于大规模加工。
发明内容
本发明的目的在于解决上述技术问题而提出一种多孔海藻酸盐膜的制备方法及应用。本发明使海藻酸钠溶液冷冻凝固，形成临时稳定的空间结构。通过向其中注入含乙醇和氯化钙的解冻凝固剂，利用乙醇（熔点-114.1℃）渗透使冰晶结构逐渐溶化，与此同时液化钙离子进入海藻酸钠溶液解冻空间，并使海藻酸钠大分子迅速发生离子交联固化，保留住海藻酸钠大分子原有空间框架结构而不塌陷，从而形成多孔结构的海藻酸盐膜。
为达到上述目的，本发明采取的技术方案为：
一种多孔海藻酸盐膜的制备方法，包括如下步骤：
S1.将海藻酸钠溶于纯水中，静置或真空脱泡；
S2.将S1所得海藻酸钠溶液在平板容器上流延铺平后，放入-20℃~-80℃冷柜中冷冻；
S3.配制解冻凝固剂，所述解冻凝固剂由无水乙醇、无水氯化钙、甘油和水混合而成；
S4.向S2所得冰冻态海藻酸钠溶液注入S3所得解冻凝固剂，继续在冷柜中放置处理，使海藻酸钠溶液一边解冻，一边交联固化；
S5.将S4所得的海藻酸盐膜取出，用纯水漂洗后干燥，即得多孔海藻酸盐膜。
进一步地，S1中所述海藻酸钠溶液浓度为0.02~0.07g/mL。
进一步地，S2中所述海藻酸钠溶液流延厚度2mm以下，冷冻时间为1-5h。
进一步地，S3中所述解冻凝固剂中各组分质量分数分别为无水乙醇50%~94%，无水氯化钙5%~25%，甘油0.5%~2%，其余为水。
进一步地，S4中注入S3所述解冻凝固剂的体积用量为海藻酸钠溶液体积的3~10倍，并在-20℃~-80℃冷柜中解冻凝固时间为2~12h。
进一步地，S5中干燥方法为鼓风干燥或真空干燥，温度为20~50℃。
另一方面，本发明提供了上述所述的多孔海藻酸盐膜的制备方法制备得到的多孔海藻酸盐膜。
再一方面，本发明提供了一种上述所述的多孔海藻酸盐膜的应用，多孔海藻酸盐膜能用于面膜、创伤敷料、止血海绵或细胞支架。
本发明的有益效果在于：
1）本发明所公开的多孔海藻酸盐膜的制备方法简单有效。相比冷冻干燥法而言，本发明的方法无需真空环境，而是利用乙醇溶液的低熔点性将冰晶升华致孔改变为冰晶溶化致孔，极大地提高了成孔效率。
2）本发明所公开的方法使海藻酸钠大分子在冻结状态下逐渐被液化钙离子交联固化，保持了良好的多孔框架结构，并且极大地改善了多孔海藻酸盐膜的机械性能。
3）本发明所公开的方法所需设备工艺条件简单，且成膜取膜极为方便，适合于规模化加工。
附图说明
图1和图2为本发明实施例1制备的多孔海藻酸盐膜表面SEM照片（图1放大500x，图2放大5000x）；
图3和图4为本发明实施例2制备的多孔海藻酸盐膜表面SEM照片（图3放大500x，图4放大5000x）。
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
将0.3g海藻酸钠溶于10mL纯水中，静置脱泡12h。取0.5mL海藻酸钠溶液注入平底试样皿，使其流延铺平，厚度为0.5mm，然后将试样皿放入冷柜中-80℃下冷冻2h。另外，配制解冻凝固剂，将94g无水乙醇，5g无水氯化钙，0.5g甘油，0.5g水混合，室温下搅拌溶解。然后，向冰冻态海藻酸钠溶液中注入2.5mL解冻凝固剂，使其在-20℃下解冻和交联固化，时间6h。之后，将多孔海藻酸盐膜取出，用纯水漂洗后，在20℃鼓风干燥即可。所得多孔海藻酸盐膜厚度0.5mm左右，柔软多孔（见图1和图2）。从图1可以看出，海藻酸盐膜孔隙率高且分布均匀。由放大5000倍的图2可以看出，海藻酸盐膜孔壁上还分布着许多更小的微孔。该多孔海藻酸盐膜吸水率达到自重的15倍以上，吸液保湿效果好，可用于面膜。
实施例2
将0.5g海藻酸钠溶于10mL纯水中，真空脱泡6h。取1mL海藻酸钠溶液注入平底试样皿，使其流延铺平，厚度为1mm，然后将试样皿放入冷柜中-20℃下冷冻5h。另外，配制解冻凝固剂，将75g无水乙醇，20g无水氯化钙，2g甘油，3g水混合，室温下搅拌溶解。然后，向冰冻态海藻酸钠溶液中注入3mL解冻凝固剂，使其在-20℃下解冻和交联固化，时间8h。之后，将多孔海藻酸盐膜取出，用纯水漂洗后，在50℃真空干燥即可。所得多孔海藻酸盐膜厚度1mm左右，柔软多孔。本实施例所得多孔海藻酸盐膜的孔隙结构特点与实施例1相似（见图3和图4）。该多孔海藻酸盐膜的吸水率达到自重的20倍以上，吸液保湿效果好，可用于创伤敷料、止血海绵或细胞支架。
实施例3
将0.7g海藻酸钠溶于10mL纯水中，真空脱泡12h。取2mL海藻酸钠溶液注入平底试样皿，使其流延铺平，厚度为2mm，然后将试样皿放入冷柜中-80℃下冷冻3h。另外，配制解冻凝固剂，将85g无水乙醇，10g无水氯化钙，2g甘油，3g水混合，室温下搅拌溶解。然后，向冰冻态海藻酸钠溶液中注入20mL解冻凝固剂，使其在-80℃下解冻和交联固化，时间12h。之后，将多孔海藻酸盐膜取出，用纯水漂洗后，在25℃真空干燥即可。所得多孔海藻酸盐膜厚度2mm左右，柔软多孔，吸液保湿效果好，可用于创伤敷料、止血海绵或细胞支架。
实施例4
将0.2g海藻酸钠溶于10mL纯水中，静置脱泡12h。取0.2mL海藻酸钠溶液注入平底试样皿，使其流延铺平，厚度为0.2mm，然后将试样皿放入冷柜中-20℃下冷冻1h。另外，配制解冻凝固剂，将50g无水乙醇，25g无水氯化钙，2g甘油，23g水混合，室温下搅拌溶解。然后，向冰冻态海藻酸钠溶液中注入2mL解冻凝固剂，使其在-20℃下解冻和交联固化，时间2h。之后，将多孔海藻酸盐膜取出，用纯水漂洗后，在37℃鼓风干燥即可。所得多孔海藻酸盐膜厚度0.2mm左右，柔软多孔，吸液保湿效果好，可用于面膜或人工皮肤。

Claims (8)

1.一种多孔海藻酸盐膜的制备方法，包括如下步骤：
S1.将海藻酸钠溶于纯水中，静置或真空脱泡；
S2.将S1所得海藻酸钠溶液在平板容器上流延铺平后，放入-20℃~-80℃冷柜中冷冻；
S3.配制解冻凝固剂，所述解冻凝固剂由无水乙醇、无水氯化钙、甘油和水组成；
S4.向S2所得冰冻态海藻酸钠溶液注入S3所得解冻凝固剂，继续在冷柜中放置处理，使海藻酸钠溶液一边解冻，一边交联固化；
S5.将S4所得的海藻酸盐膜取出，用纯水漂洗后干燥，即得多孔海藻酸盐膜。
2.根据权利要求1所述的一种多孔海藻酸盐膜的制备方法，其特征在于，S1中海藻酸钠溶液浓度为0.02~0.07g/mL。
3.根据权利要求1所述的一种多孔海藻酸盐膜的制备方法，其特征在于，S2中海藻酸钠溶液流延厚度2mm以下，冷冻时间为1~5h。
4.根据权利要求1所述的一种多孔海藻酸盐膜的制备方法，其特征在于，S3中解冻凝固剂各组分质量分数分别为无水乙醇50%~94%，无水氯化钙5%~25%，甘油0.5%~2%，其余为水。
5.根据权利要求1所述的一种多孔海藻酸盐膜的制备方法，其特征在于，S4中注入S3所述解冻凝固剂的体积用量为海藻酸钠溶液体积的3~10倍，并在-20℃~-80℃冷柜中解冻凝固时间为2~12h。
6.根据权利要求1所述的一种多孔海藻酸盐膜的制备方法，其特征在于，S5中干燥方法为鼓风干燥或真空干燥，温度为20~50℃。
7.根据权利要求1-6制备得到的多孔海藻酸盐膜。
8.根据权利要求7所述的多孔海藻酸盐膜的应用，其特征在于，多孔海藻酸盐膜能用于面膜、创伤敷料、止血海绵或细胞支架。
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