CN108310469A - 一种高性能聚乙烯醇水凝胶人工软骨替代材料的制备方法 - Google Patents
一种高性能聚乙烯醇水凝胶人工软骨替代材料的制备方法 Download PDFInfo
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Abstract
本发明公开一种高性能聚乙烯醇(PVA)水凝胶人工软骨替代材料的制备方法,其特点是利用碳纳米材料的高强度、优异的耐磨自润滑性及易于功能化修饰的特性,采用带有活性官能基、且自润滑性优异的聚氧化乙烯醚、聚硅氧烷等功能偶联剂对碳纳米材料表面进行偶联处理,研究制备PVA/碳纳米材料纳米复合凝胶,实现碳纳米粒子在PVA基体中的良好分散,发挥功能偶联剂偶联增容及其与碳纳米材料协同增强、减摩作用;在此基础上,对复合凝胶进行拉伸取向,形成分子取向结构,进一步提升其力学强韧性,延长其使用寿命。
Description
技术领域
本发明涉及一种高性能聚乙烯醇水凝胶人工软骨替代材料的制备方法,属于高分子材料制备领域。
背景技术
关节是人体骨骼肌肉系统的重要组成部分,是人体维持正常生活及运动的基础;关节软骨在关节活动中起重要作用,因承受较高压应力而具有较好的力学强韧性;同时关节软骨又具有优良的润滑系统,可保护软骨下的骨骼不受破坏。
具有类似天然软骨组织的多孔状聚乙烯醇(PVA)水凝胶被认为是软骨替代的较理想材料,具有无毒、无副作用,生物相容性优良,化学性质稳定,良好的柔韧性和高弹性能够减少对周围细胞和组织的机械刺激,润滑性优良等特点。但PVA水凝胶缺乏足够的力学强度,尤其作为软骨替代材料,缺乏足够的抗压和抗剪切性能以承受施加于人体关节表面严峻的负荷条件;同时其自润滑性不足。在人工软骨替代材料研发方面,Lei Cao等人,J.Photoch.Photobio.B,2018,178:440-460,通过将棒状TiO2纳米粒子引入PVA/聚乙烯吡咯烷酮(PVP)复合物理水凝胶中,从而提高其对细胞黏附性能;Gang Wu等人,Mater.Chem.Phys.,2008,107:364-369,通过冷冻解冻法制备了PVA/羟基磷灰石(HA)复合水凝胶,结果发现HA加入使得材料可在模拟人体溶液中诱导形成磷灰石,表明其具有很好的骨诱导性能,同时材料的弹性模量达23MPa;Jiongrun Chen等人,Carbon,2017,111:18-27,通过将环糊精接枝交联到氨基改性的石墨烯上,并将其引入PVA基体中,制备石墨烯/PVA有机/无机互穿水凝胶,结果表明其拉伸强度、断裂伸长率、压缩模量分别提高到2.0MPa、875%、0.9MPa,且材料同时具备较好的细胞相容性;Mohammad Sabzi等人,Mat.Sci.Eng.C-Mater.,2017,74:374-381,通过冷冻解冻法制备PVA/琼脂物理交联水凝胶,结果表明其内部分别形成了PVA及琼脂的双网络结构,从而使得其拉伸强度达到1400kPa。然而,所报道文献对PVA力学强度提升幅度较小,仍不能满足人体对软骨力学强度的要求。
发明内容
本发明的目的是针对现有技术的不足而提供一种高性能PVA水凝胶人工软骨替代材料的制备方法,其特点是利用碳纳米材料的高强度、优异的耐磨自润滑性及易于功能化修饰的特性,利用碳纳米材料的高强度、优异的耐磨自润滑性及易于功能化修饰的特性,采用带有活性官能基、且自润滑性优异的聚氧化乙烯醚、聚硅氧烷等功能偶联剂对碳纳米材料表面进行偶联处理,研究制备PVA/碳纳米材料纳米复合凝胶,实现碳纳米粒子在PVA基体中的良好分散,发挥功能偶联剂偶联增容及其与碳纳米材料协同增强、减摩作用,以低含量碳纳米粒子大幅提高PVA凝胶的力学强韧性、耐磨自润滑性;在此基础上,对复合凝胶进行拉伸取向,形成分子取向结构,进一步提升其综合性能,延长其使用寿命。
本发明的目的由以下技术措施实现,其中所述原料分数除特殊说明外,均为重量份数。
高性能PVA水凝胶人工软骨替代材料制备主要原料配方组分为:
聚乙烯醇 100份
碳纳米材料 0.1-20份
功能偶联剂 0.05-10份
其中,聚乙烯醇聚合度为400~3000,醇解度为75~99%;
碳纳米材料为碳纳米管、石墨、石墨烯中的任一种;
功能偶联剂为分子量200~50000g/mol的端羟基聚氧化乙烯醚、分子量200~50000g/mol的端氨基聚氧化乙烯醚、分子量200~50000g/mol的端羟基聚二甲基硅氧烷、分子量200~50000g/mol的端氨丙基聚二甲基硅氧烷、分子量200~50000g/mol氨乙基氨丙基聚二甲基硅氧烷中的任一种;
碳纳米材料的偶联处理:
将0.1-20份碳纳米材料分散在400-3000份去离子水中,加入0.05-10份功能偶联剂于室温搅拌均匀,采用超声波分散10-200min,超声波功率为100-5000w、频率为10000-100000HZ,超声温度为40-95℃,获得偶联处理碳纳米材料分散液;PVA水凝胶人工软骨替代材料制备:
称取聚乙烯醇100份加入上述制备的偶联处理碳纳米材料分散液中,于80-95℃加热搅拌2-5小时配制成均匀的复合溶液;将溶液倒入模具中,置于-50--10℃冷冻6-20小时,然后置于室温解冻2-8h,循环冷冻-解冻2-8次;当循环冷冻-解冻一次后,将试样两端固定于拉伸夹具上,施加拉伸应力进行拉伸取向,制备不同取向倍率取向复合水凝胶,封袋包装,置4℃冰箱保存备用。
本发明具有如下优点
本发明旨在制备一种高性能PVA水凝胶人工软骨替代材料。针对关节软骨性能要求,利用碳纳米材料的高强度、优异的耐磨自润滑性及易于功能化修饰的特性,通过对反应性偶联增容技术、原位交联技术的探索,采用带有活性官能基、且自润滑性优异的聚氧化乙烯醚、聚硅氧烷等功能偶联剂对碳纳米材料表面进行偶联处理,二者间可形成化学键作用或氢键作用,同时功能偶联剂可与PVA分子上的羟基形成氢键作用,从而增强各组分界面作用,有利于碳纳米材料在PVA基体中的均匀分散;另一方面,采用原位交联技术,使碳纳米材料更均匀分散于PVA水溶液中,有利于增强界面相互作用;并发挥功能偶联剂与碳纳米材料协同减摩作用,以低含量碳纳米粒子大幅提高PVA凝胶的力学强韧性、耐磨自润滑性;在此基础上,对复合凝胶试样进行拉伸取向,使PVA分子及碳纳米材料分子形成分子取向结构,进一步显著提升其生物力学强度、生物摩擦学性能及耐疲劳稳定性,延长其使用寿命。
具体实施方式
下面通过实施例对本发明进行具体的描述,有必要在此指出的是本实施例只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限制,该领域的技术熟练人员可以根据上述本发明的内容对本发明作出一些非本质的改进和调整。
实施例1
将0.05g石墨分散在50g去离子水中,加入0.05g分子量2000g/mol的端氨基聚氧化乙烯醚于室温搅拌均匀,采用超声波分散30min,超声波功率为500w、频率为20000HZ,超声温度为50℃,获得偶联处理石墨分散液。
称取聚合度为1300、醇解度为99%的聚乙烯醇10g加入上述制备的偶联处理石墨分散液中,于85℃加热搅拌5小时配制成均匀的复合溶液;将溶液倒入模具中,置于-10℃冷冻8小时,然后置于恒温恒湿箱解冻2h,循环冷冻-解冻4次;当循环冷冻-解冻一次后,将试样两端固定于拉伸夹具上,施加拉伸应力进行拉伸取向,制备取向倍率为150%的取向复合水凝胶,封袋包装,置4℃冰箱保存备用;其拉伸强度为5.1MPa,压缩模量为1.2MPa。
实施例2
将0.5g石墨烯分散在800g去离子水中,加入0.38g分子量为20000g/mol的端羟基聚二甲基硅氧烷于室温搅拌均匀,采用超声波分散90min,超声波功率为1000w、频率为40000HZ,超声温度为75℃,获得偶联处理石墨烯分散液。
称取聚合度为1700,醇解度为88%的聚乙烯醇10g加入上述制备的偶联处理石墨烯分散液中,于90℃加热搅拌3.5小时配制成均匀的复合溶液;将溶液倒入模具中,置于-30℃冷冻12小时,然后置于恒温恒湿箱解冻6h,循环冷冻-解冻6次;当循环冷冻-解冻一次后,将试样两端固定于拉伸夹具上,施加拉伸应力进行拉伸取向,制备取向倍率为300%的取向复合水凝胶,封袋包装,置4℃冰箱保存备用;其拉伸强度为9.5MPa,压缩模量为2.3MPa。
实施例3
将1.5g碳纳米管分散在2000g去离子水中,加入0.8g分子量为40000g/mol氨乙基氨丙基聚二甲基硅氧烷于室温搅拌均匀,采用超声波分散150min,超声波功率为2000w、频率为60000HZ,超声温度为90℃,获得偶联处理碳纳米管分散液。
称取聚合度为2000、醇解度为99%的聚乙烯醇10g加入上述制备的偶联处理碳纳米管分散液中,于95℃加热搅拌3小时配制成均匀的复合溶液;将溶液倒入模具中,置于-50℃冷冻16小时,然后置于恒温恒湿箱解冻8h,循环冷冻-解冻8次;当循环冷冻-解冻一次后,将试样两端固定于拉伸夹具上,施加拉伸应力进行拉伸取向,制备取向倍率为350%的取向复合水凝胶,封袋包装,置4℃冰箱保存备用;其拉伸强度为11.5MPa,压缩模量为2.9MPa。
Claims (1)
1.一种高性能聚乙烯醇水凝胶人工软骨替代材料,其特征在于该水凝胶主要原料由以下组分组成,按重量计为:
聚乙烯醇(PVA) 100份
碳纳米材料 0.1-20份
功能偶联剂 0.05-10份
其中,聚乙烯醇聚合度为400~3000,醇解度为75~99%;
碳纳米材料为碳纳米管、石墨、石墨烯中的任一种;
功能偶联剂为分子量200~50000g/mol的端羟基聚氧化乙烯醚、分子量200~50000g/mol的端氨基聚氧化乙烯醚、分子量200~50000g/mol的端羟基聚二甲基硅氧烷、分子量200~50000g/mol的端氨丙基聚二甲基硅氧烷、分子量200~50000g/mol氨乙基氨丙基聚二甲基硅氧烷中的任一种;
该高性能聚乙烯醇水凝胶人工软骨替代材料的制备方法包括以下步骤:
碳纳米材料的偶联处理:
将0.1-20份碳纳米材料分散在400-3000份去离子水中,加入0.05-10份功能偶联剂于室温搅拌均匀,采用超声波分散10-200min,超声波功率为100-5000w、频率为10000-100000HZ,超声温度为40-95℃,获得偶联处理碳纳米材料分散液;
PVA水凝胶人工软骨替代材料制备:
称取聚乙烯醇100份加入上述制备的偶联处理碳纳米材料分散液中,于80-95℃加热搅拌2-5小时配制成均匀的复合溶液;将溶液倒入模具中,置于-50--10℃冷冻6-20小时,然后置于室温解冻2-8h,循环冷冻-解冻2-8次;当循环冷冻-解冻一次后,将试样两端固定于拉伸夹具上,施加拉伸应力进行拉伸取向,制备取向倍率为0.5-5的取向复合水凝胶,封袋包装,置4℃冰箱保存备用。
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