CN113968936A - 一种强韧壳聚糖水凝胶及其制备方法与应用 - Google Patents
一种强韧壳聚糖水凝胶及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种强韧壳聚糖水凝胶及其制备方法与应用。本发明将壳聚糖溶解与凝胶化特性联系起来,采用紫外光交联法使壳聚糖溶液形成稳定的共价键交联网络。方法是选用含不饱和双键的丙烯酸或甲基丙烯酸充当壳聚糖的溶剂,并且为壳聚糖接枝丙烯酸类光交联剂提供反应环境,所得的壳聚糖溶液可直接或透析后进行紫外光交联,残留的丙烯酸会发生光聚合并与壳聚糖大分子交联,从而形成强韧的壳聚糖水凝胶。该方法可以原位添加其他天然高分子、功能性添加剂或者生物活性物质,扩大壳聚糖水凝胶的应用领域,本发明的强韧壳聚糖水凝胶可应用于组织支架、传感器和药物缓释领域。
Description
技术领域
本发明属于天然高分子材料领域,具体涉及一种强韧壳聚糖水凝胶及其制备方法与应用。
背景技术
水凝胶是三维聚合物网络,具有吸液膨胀性,同时保持其机械稳定性。水凝胶具有良好的亲水性、生物相容性和柔韧性,已被用于多种生物医学应用,如药物载体、可吸收缝线和可注射生物材料。许多天然高分子被用于水凝胶材料中,其中,壳聚糖因有良好的生物相容性、生物降解性、天然抗菌性、成型加工性以及高的交联率而成为制备水凝胶的优选材料。
壳聚糖水凝胶可以通过物理交联和化学交联两种方式制备。物理交联法是通过形成大量的分子间氢键网络、疏水键作用以及范德华力等非共价键力而构建的凝胶网络,这种结构稳定性较差,容易受到温度、水、pH值的影响而发生结构坍塌,承受外力作用的耐受性差。化学交联法通常引入交联剂,如戊二醛、京尼平、多巴胺等,并引入其他高分子发生化学交联形成水凝胶,这种方法可得到结构性能稳定的水凝胶,但是结构形态不具备原位成型性,可控适应性欠佳。而光交联法则通过紫外光辐照使壳聚糖衍生物激发交联反应,壳聚糖衍生物以液体流动,可塑性强且可原位凝胶化,因此能以更匹配的形态粘附在被粘物上。从现有技术来看,光交联法适合原位凝胶化强韧水凝胶的制备,而现有光交联法制备壳聚糖水凝胶并没有很好地将壳聚糖的溶解及其光交联反应联合起来考虑,因此本发明结合两者的特性,提出新的解决方案。
发明内容
本发明的目的在于提供一种强韧的壳聚糖水凝胶及其制备方法,其特点是选择丙烯酸或者甲基丙烯酸作为壳聚糖的溶剂,同时又具有光聚合反应性。在壳聚糖大分子上引入甲基丙烯酸酐或者甲基丙烯酸缩水甘油酯,使得壳聚糖大分子之间以及大分子与溶剂分子间在紫外光辐照下形成共价键交联,从而得到强韧的壳聚糖水凝胶。为了达到上述目的,本发明采取的技术方案为:
一种强韧壳聚糖水凝胶的制备方法,其特征在于,包括如下步骤:
S1.将壳聚糖粉末溶于丙烯酸或甲基丙烯酸溶液,得到纯壳聚糖溶液;进一步地,所得的纯壳聚糖溶液还可与其他高分子溶液混合,所述其他高分子为明胶、聚乙烯醇、水溶性纤维素衍生物中的任何一种;
S2.将丙烯酸衍生物滴加入S1所得的壳聚糖溶液中并加热反应,所述丙烯酸衍生物为甲基丙烯酸缩水甘油酯、甲基丙烯酸酐中的任何一种;
S3.将S2所得的壳聚糖溶液直接或者透析后加入光引发剂,搅拌溶解均匀,真空脱泡,然后经紫外光辐照,即得强韧壳聚糖水凝胶。
进一步地,S1中所述壳聚糖溶液的组分质量浓度为:壳聚糖2%~5%,丙烯酸或甲基丙烯酸3%~20%,其他高分子0%~10%,其余为水。
进一步地,S2中所述的丙烯酸衍生物的加入量为壳聚糖摩尔当量的20%~100%,反应温度为25~60℃,反应时间为3~24h。
进一步地,S3中所述的光引发剂为水溶性紫外光引发剂,光引发剂的加入量为丙烯酸衍生物用量的2%~5%。
进一步地,S3中紫外线的波长为265~395nm,辐照时间为60~600s。
本发明提供了一种强韧壳聚糖水凝胶,由上述的制备方法制备得到。
进一步地,本发明还提供了一种强韧壳聚糖水凝胶,在上述制备方法制备的壳聚糖水凝胶中引入功能性添加剂或者生物活性物质。
进一步地,所述引入的功能性添加剂包括金属或金属盐纳米粒子、碳纳米管及其衍生物、石墨烯及其衍生物、小分子药物粉末等,所述引入的生物活性物质包括细胞、酶、生长因子等。
进一步地,本发明提供了一种强韧壳聚糖水凝胶的应用,所述强韧壳聚糖水凝胶用于组织支架、传感器、药物缓释等领域。
与现有技术相比,本发明具有以下有益效果:
1)本发明中壳聚糖的溶剂本身又是光交联剂,因此经紫外光引发聚合反应并与壳聚糖交联,从而形成稳定的分子间共价键交联网络,极大地提高了壳聚糖水凝胶的机械性能。
2)本发明制备的壳聚糖溶液可原位凝胶化,通过将壳聚糖溶液流延在不同形态的模具上,再进行紫外光交联固化,可制备具有特定形状的强韧水凝胶材料,也可用于3D打印,扩大了其应用领域。
附图说明
图1为实施例1中制备的壳聚糖溶液经紫外光辐照后得到强韧的壳聚糖水凝胶。
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,所提供的实施例仅是对本发明方法的说明,而不以任何方式限制本发明。
实施例1
将2.5g壳聚糖,2.5g丙烯酸加入到45g纯水中,室温搅拌溶解。将2.2g甲基丙烯酸酐滴加到壳聚糖溶液中,50℃加热搅拌反应6h。壳聚糖溶液在光交联之前具有较高的粘度,但是仍能较好地流动(见图1的左图)。向接枝反应后的壳聚糖溶液中加入110mg光引发剂2-羟基-4’-(2-羟乙氧基)-2-甲基苯丙酮,搅拌溶解均匀,真空脱泡。将脱泡后的壳聚糖溶液置于365nm的紫外光下辐照600s,即得强韧的壳聚糖水凝胶(见图1的右图)。
实施例2
将1g壳聚糖,1.5g丙烯酸加入到47.5g纯水中,室温搅拌溶解。将0.18g甲基丙烯酸缩水甘油酯滴加到壳聚糖溶液中,60℃加热搅拌反应3h,透析72h。向透析后的壳聚糖溶液中加入10mg光引发剂2-羟基-4’-(2-羟乙氧基)-2-甲基苯丙酮,搅拌溶解均匀,真空脱泡。将脱泡后的壳聚糖溶液置于365nm的紫外光下辐照200s,即得强韧的壳聚糖水凝胶,可用于组织支架领域。
实施例3
将1g壳聚糖,1g明胶,1.5g丙烯酸加入到46.5g纯水中,50℃搅拌溶解。将0.5g甲基丙烯酸缩水甘油酯滴加到壳聚糖溶液中,25℃加热搅拌反应24h,透析72h。向透析后的壳聚糖溶液中加入20mg光引发剂苯基(2,4,6-三甲基苯甲酰基)磷酸锂,搅拌溶解均匀,真空脱泡。将脱泡后的壳聚糖溶液置于395nm的紫外光下辐照300s,即得强韧的壳聚糖水凝胶,可用于组织支架领域。
实施例4
将1.5g壳聚糖,5g羟丙基纤维素,10g丙烯酸加入到33.5g纯水中,室温搅拌溶解。将0.6g甲基丙烯酸缩水甘油酯滴加到壳聚糖溶液中,60℃加热搅拌反应3h。向接枝反应后的壳聚糖溶液中加入18mg光引发剂苯基(2,4,6-三甲基苯甲酰基)磷酸锂,搅拌溶解均匀,真空脱泡。将脱泡后的壳聚糖溶液置于365nm的紫外光下辐照600s,即得强韧的壳聚糖水凝胶。
实施例5
将1.5g壳聚糖,0.5g聚乙烯醇,2g丙烯酸加入到46g纯水中,80℃搅拌溶解。将1g甲基丙烯酸酐滴加到壳聚糖溶液中,60℃加热搅拌反应3h,然后透析72h。向透析后的壳聚糖溶液中加入18mg光引发剂苯基(2,4,6-三甲基苯甲酰基)磷酸锂,搅拌溶解均匀,再加入50mg牛血清蛋白和真空脱泡。将脱泡后的壳聚糖溶液置于365nm的紫外光下辐照100s,即得具有载药性的强韧壳聚糖水凝胶,可用于药物缓释领域。
实施例6
将2g壳聚糖,1.5g丙烯酸加入到46.5g纯水中,50℃搅拌溶解。将1g甲基丙烯酸缩水甘油酯滴加到壳聚糖溶液中,45℃加热搅拌反应6h。向接枝反应后的壳聚糖溶液中加入20mg单层石墨烯和10mg光引发剂苯基(2,4,6-三甲基苯甲酰基)磷酸锂,搅拌溶解均匀,真空脱泡。将脱泡后的壳聚糖溶液置于265nm的紫外光下辐照60s,即得具有导电性的强韧壳聚糖水凝胶,可用于传感器领域。
Claims (9)
1.一种强韧壳聚糖水凝胶的制备方法,其特征在于,包括如下步骤:
S1.将壳聚糖粉末溶于丙烯酸或甲基丙烯酸溶液,得到纯壳聚糖溶液;进一步地,所得的纯壳聚糖溶液还可与其他高分子溶液混合,所述其他高分子为明胶、聚乙烯醇、水溶性纤维素衍生物中的任何一种;
S2.将丙烯酸衍生物滴加入S1所得的壳聚糖溶液中并加热反应,所述丙烯酸衍生物为甲基丙烯酸缩水甘油酯、甲基丙烯酸酐中的任何一种;
S3.将S2所得的壳聚糖溶液直接或者透析后加入光引发剂,搅拌溶解均匀,真空脱泡,然后经紫外光辐照,即得强韧壳聚糖水凝胶。
2.根据权利要求1所述的一种强韧壳聚糖水凝胶的制备方法,其特征在于,S1中所述壳聚糖溶液的组分质量浓度为:壳聚糖2%~5%,丙烯酸或甲基丙烯酸3%~20%,其他高分子0%~10%,其余为水。
3.根据权利要求1所述的一种强韧壳聚糖水凝胶的制备方法,其特征在于,S2中所述的丙烯酸衍生物的加入量为壳聚糖摩尔当量的20%~100%,反应温度为25~60℃,反应时间为3~24h。
4.根据权利要求1所述的一种强韧壳聚糖水凝胶的制备方法,其特征在于,S3中所述的光引发剂为水溶性紫外光引发剂,光引发剂的加入量为丙烯酸衍生物用量的2%~5%。
5.根据权利要求1所述的一种强韧壳聚糖水凝胶的制备方法,其特征在于,S3中紫外线的波长为265~395nm,辐照时间为60~600s。
6.一种强韧壳聚糖水凝胶,其特征在于,根据权利要求1-5所述的制备方法制备得到。
7.一种强韧壳聚糖水凝胶,其特征在于,在权利要求1-5任意一项所述的方法制备的壳聚糖水凝胶中引入功能性添加剂或者生物活性物质。
8.根据权利要求7所述的制备方法,其特征在于,所述的功能性添加剂包括金属或金属盐纳米粒子、碳纳米管及其衍生物、石墨烯及其衍生物、小分子药物粉末等,所述的生物活性物质包括细胞、酶、生长因子等。
9.根据权利要求6-7所述的一种强韧壳聚糖水凝胶的应用,其特征在于,所述强韧壳聚糖水凝胶用于组织支架、传感器、药物缓释等领域。
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