CN113336987A - 一种天然高强度海藻酸钠双交联水凝胶膜的制备方法 - Google Patents
一种天然高强度海藻酸钠双交联水凝胶膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种天然高强度海藻酸钠双交联水凝胶膜的制备方法。该双交联水凝胶膜以海藻酸钠作基体,脱乙酰基蟹壳粉作交联剂,并用葡萄糖酸内酯作为蟹壳粉中的钙离子释放剂促进海藻酸钠凝胶的交联。同时蟹壳粉中的甲壳素经脱乙酰基作用后暴露出的氨基可以与海藻酸钠的羧基发生聚电解质相互作用,最终得到双交联水凝胶膜。本发明制备的双交联水凝胶膜具有制备方法简便,溶胀性能好,机械强度大且绿色环保等优点。该水凝胶膜可用于医疗卫生、生物工程、食品保鲜等领域。
Description
技术领域
本发明涉及一种天然高强度海藻酸钠双交联水凝胶膜的制备方法,属于绿色生物高分子材料领域。
背景技术
水凝胶膜是一种新型高分子材料,具有良好的封闭性、溶胀性以及可降解性等优点,并被广泛应用于生物医疗、组织工程以及食品包装等领域。在应用过程中水凝胶膜通常负载一些活性物质,以起到传感、递送、释放等作用。然而,传统水凝胶膜也存在一定的缺点,如制备原料来源非天然、制备过程复杂、力学性能差与溶胀率低等。因此,目前关于水凝胶的研究主要集中于制备方法和提高机械强度等方面。
水凝胶的形成机制主要为离子交联、化学交联和物理交联。离子交联是指离子间相互作用形成三维网状水凝胶。化学交联水凝胶是基质材料在外加交联剂或催化剂的作用下形成稳定的共价键构建高度交联结构形成的水凝胶,具有良好的性能,但也存在交联剂的细胞毒性问题,不利于其应用。物理交联水凝胶通常通过物理相互作用(如氢键、链缠结、配位作用或聚电解质相互作用)形成的水凝胶,易于使用且毒性低,但是有一定的可逆性且形成的水凝胶机械强度不够。
海藻酸钠是一种安全的天然阴离子多糖,具有良好的成模性,可与二价金属阳离子交联形成水凝胶膜。与其他水凝胶材料相比,海藻酸钠水凝胶膜无毒且生物相容性高,被广泛应用于人造骨和皮肤的凝胶组织工程、药物传递、创面敷料、包装等多种生物技术领域。海藻酸钠水凝胶的制备通常以离子交联为主,常用碳酸钙或氯化钙溶液等来源于非天然的原料作为钙源,其中的Ca2+可以与海藻酸钠的羧基形成“蛋盒”结构状水凝胶,通过这种方法制备的水凝胶的交联不够均匀,易出现局部过度交联的情况,力学性能差、溶胀率较低且形成的水凝胶强度较低,在水合状态下很难保持固有形状,且易破裂,这些缺点严重限制了其应用。因此,亟需开发高交联强度的海藻酸钠水凝胶,以扩大其进一步应用。
蟹壳是一种天然废弃物,其主要成分为80%的碳酸钙与20%的甲壳素,经粉碎、脱乙酰基处理和葡萄糖酸内酯改性后,一方面被释放的Ca2+可与海藻酸钠交联,另一方面其中的甲壳素经脱乙酰基处理后暴露的氨基可以海藻酸钠形成聚电解质相互作用,进而得到一种制备简单、绿色、均一、溶胀性好且强度高的海藻酸钠水凝胶膜,该发明具有非常重要的现实意义。
发明内容
本发明的目的是提供一种绿色、高强度、高溶胀性的海藻酸钠双交联水凝胶膜,以天然废弃蟹壳为交联引发剂,旨在利用葡萄糖酸内酯作为Ca2+释放剂,将蟹壳粉中Ca2+释放出来与海藻酸钠交联,同时蟹壳粉经脱乙酰基处理后可与海藻酸钠形成聚电解质复合物,进而形成双交联水凝胶膜,可改善传统水凝胶膜交联不均匀、溶胀性低和力学性能差等缺点,为其在医疗卫生、生物工程、食品保鲜等领域的研究奠定基础。
为实现上述目的,包括以下步骤:
(1)将蟹壳粉进行超微粉碎,加入低浓度的氢氧化钠溶液在60℃搅拌6h进行脱蛋白,将得到的蟹壳粉过滤水洗至ph为7,加入无水乙醇在室温条件下搅拌6h进行脱色,过滤烘干后加入高质量分数的氢氧化钠溶液并在100℃搅拌3h进行脱乙酰基处理,最后水洗至ph 为中性,干燥后得到脱乙酰基蟹壳粉。
(2)配置质量分数为2%的海藻酸钠水溶液,完全溶解后加入一定量的脱乙酰基蟹壳粉,混合均匀后加入甘油增塑,室温下搅拌6h。
(3)在海藻酸钠与部分脱乙酰基蟹壳粉混合液中一定量的葡萄糖酸内酯,搅拌3min后将混合物倒入培养皿中,室温下干燥7天,并在恒温恒湿箱中平衡48h,平衡条件为20℃、 50%相对湿度,得到天然高强度海藻酸钠双交联水凝胶膜。
本发明还包括这样一些特征:
所述(1)中用于脱蛋白浓度的氢氧化钠质量分数为5%,脱乙酰基处理过程中的氢氧化钠质量分数为33.7%。最终得到的脱乙酰基蟹壳粉的粒径范围在0.125μm-33.95μm,平均粒径为7.45μm。
所述(2)加入的脱乙酰基蟹壳粉、甘油与海藻酸钠的质量比为1:1:2。
所述(3)中加入的葡萄糖酸内酯的质量分数分别为0.5%、0.7%、0.9%。
采用激光粒度仪、傅里叶红外光谱、溶胀率与溶胀损失、以及凝胶强度来对本发明的海藻酸钠双交联水凝胶膜性能进行表征。
从上述步骤看本发明有益效果:一、本发明制备双交联水凝胶膜选用的基体海藻酸钠是生物可降解材料,具有无毒、生物相容性高、安全性高等优点。二、本发明使用来源于天然的蟹壳粉作为双交联剂,并对其进行脱乙酰基处理,为海藻酸钠水凝胶的离子交联提供钙源的同时促进海藻酸钠与氨基形成聚电解质复合物,增加了农副产物综合利用率。三、本发明使用葡萄糖酸内酯作为Ca2+释放剂,葡萄糖酸内酯溶于水后解离出的H+可以缓慢的将蟹壳中的Ca2+释放出来,进而与海藻酸钠均匀交联形成“蛋盒”结构,效果优于其他有机酸。四、本发明中脱乙酰基蟹壳粉与海藻酸钠之间形成了双重交联网络结构,使其机械强度远高于传统用于生物医疗、组织工程以及食品包装等领域海藻酸钠水凝胶膜。五、本发明海藻酸钠双交联水凝胶膜制备简单且具有非常高的溶胀能力,优于传统海藻酸钠水凝胶膜。
附图说明
附图1脱乙酰基蟹壳粉的平均粒径图
附图2海藻酸钠双交联水凝胶膜的傅里叶红外光谱图
附图3双交联海藻酸钠水凝胶膜水合后的凝胶强度
附图4是水凝胶膜的凝胶含量与溶胀率
具体实施方式
实施例1
一种天然高强度海藻酸钠双交联水凝胶膜的制备方法,包括以下步骤:
步骤一:将废弃蟹壳用超微粉碎机粉碎粉碎(平均粒径为7.45μm),加入5%的氢氧化钠溶液在60℃搅拌6h进行脱蛋白处理,将蟹壳粉过滤水洗至pH为中性,加入无水乙醇在室温条件下搅拌6h进行脱色处理,过滤、干燥后得到未脱乙酰基蟹壳粉。傅里叶红外光谱结果:3698cm-1(蟹壳粉中甲壳素的氢键特征峰),3428cm-1(-OH振动峰),2517cm-1 (CaCO3的特征峰),1425cm-1(-C=O不对称伸缩峰),873cm-1(CO3 2-的面内弯曲振动峰),与713cm-1(CO3 2-的面外弯曲振动峰)。
将净化处理后的蟹壳粉加入到质量分数为33.7%的氢氧化钠溶液中并在100℃反应3h 进行脱乙酰基处理,水洗至ph为中性,干燥得到脱乙酰基蟹壳粉,其平均粒径为7.45μm。如傅里叶红外光谱所示,在3642cm-1出现了新峰,这是由于脱乙酰基处理后暴露的氨基形成了新的氢键。
步骤二:将一定量的海藻酸钠溶于去离子水中得到质量分数为2%的海藻酸钠水溶液。然后加入一定量的脱乙酰基蟹壳粉和甘油(m海藻酸钠:m甘油:m蟹壳粉=2:2:1),搅拌得均匀混合液。
步骤三:在上述成膜液中加入质量分数为0.5%的葡萄糖酸内酯。搅拌2min后倒入培养皿中,室温下干燥7天,并在20℃,相对湿度50%的条件下平衡48h,得到天然高溶胀双交联水凝胶膜。本实施例在傅里叶红外光谱结果:3249cm-1对应-OH的振动峰,1725cm-1对应海藻酸钠特征峰,1598cm-1与1409cm-1对应-COO–的对称与不对称的伸缩振动峰。
实施例1的傅里叶红外光谱表征见图2,凝胶强度见图3,溶胀率和凝胶含量见图4。
实施例2
本实施例与实施例1所述的方法基本一致,不同之处为步骤三中的葡萄糖酸内酯的质量分数为0.7%。傅里叶红外光谱结果:1596cm-1与1410cm-1对应-COO–的对称与不对称的伸缩振动峰,3235cm-1对应的是-OH的振动峰。
实施例2的傅里叶红外光谱表征见图2,凝胶强度见图3,溶胀率和凝胶含量见图4。
实施例3
本实施例与实施例1所述的方法基本一致,不同之处为步骤三中葡萄糖酸内酯的质量分数为0.9%。傅里叶红外光谱结果:1595cm-1与1410cm-1对应-COO–的对称与不对称的伸缩振动峰,3204cm-1对应的是-OH的振动峰。
实施例3的傅里叶红外光谱表征见图2,凝胶强度见图3,溶胀率和凝胶含量见图4。
Claims (5)
1.本发明以天然废弃蟹壳为双交联引发剂,其主要成分为碳酸钙和甲壳素。一方面用葡萄糖酸内酯作为钙离子释放剂,促进蟹壳粉中钙离子与海藻酸钠的交联,另一方面通过经脱乙酰基处理后的蟹壳粉中暴露出的氨基与海藻酸钠之间形成的聚电解质复合物改善其疏水性和凝胶强度,进而形成海藻酸钠双交联水凝胶膜。该水凝胶膜可用于医疗卫生、生物工程、食品保鲜等领域。
2.根据权利要求1,一种天然高强度海藻酸钠双交联水凝胶膜的制备方法,其特征在于,包括以下步骤:
S1:将废弃蟹壳用超微粉碎机粉碎,收集备用并于60℃下在低浓度氢氧化钠溶液中搅拌6h脱蛋白,然后过滤、水洗至pH呈中性,加入无水乙醇并在室温条件下搅拌6h进行脱色,过滤、干燥后加入高浓度的氢氧化钠溶液并在100℃搅拌3h进行脱乙酰基处理,最后水洗至pH为中性,干燥后得到脱乙酰基蟹壳粉。
S2:配置质量分数为2%的海藻酸钠水溶液,搅拌至完全溶解后加入一定量的脱乙酰基蟹壳粉,混合均匀后加入适量的甘油增塑,室温下搅拌6h。
S3:在海藻酸钠与脱乙酰基蟹壳粉混合液中加入一定量的的葡萄糖酸内酯,室温下搅拌3min后倒入培养皿中,并在室温下干燥7天,然后在恒温恒湿箱中平衡48h,平衡条件为20℃、50%相对湿度,得到天然高强度海藻酸钠双交联水凝胶膜。
3.根据权利要求2所述的天然高强度海藻酸钠双交联水凝胶膜的制备方法,其特征是,所述S1中用于脱蛋白的氢氧化钠质量分数为5%,脱乙酰基过程使用的氢氧化钠的质量分数为33.7%。
4.根据权利要求2所述的天然高强度海藻酸钠双交联水凝胶膜的制备方法,其特征是,所述S2中加入的海藻酸钠、甘油与脱乙酰基蟹壳粉的质量比为2:2:1。
5.根据权利要求2所述的天然高强度海藻酸钠双交联水凝胶膜的制备方法,其特征是,所述S3中加入的葡萄糖酸内酯的质量分数分别为0.5%、0.7%、0.9%。
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WO2024102491A1 (en) * | 2022-11-13 | 2024-05-16 | Steakholder Foods Ltd. | Multilayered seafood-emulating consumable |
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