CN110152072B - 降低钛合金人工关节材料磨损的关节滑液制备方法 - Google Patents
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Abstract
本发明公开了一种降低钛合金人工关节材料磨损的关节滑液制备方法，该方法包括了纳米润滑颗粒聚N‑异丙基丙烯酰胺的制备及其在关节滑液中的分散。本发明方法简单有效，可以提高人工关节滑液润滑性能，显著降低钛合金人工关节材料的磨损，在人工关节、生物医药、智能材料等领域具有较大的应用潜力。
Description
技术领域
本发明涉及人工关节润滑领域，具体涉及一种通过添加润滑剂降低钛合金人工关节材料磨损的关节滑液制备方法。
背景技术
我国有超过3600万人存在关节疾病，其中每年大约有200万人需要进行关节置换手术，并且这个数字仍在不断上升。经过关节置换手术的病人经常会因为人工关节材料的摩擦磨损而导致无菌性松动问题，此外，磨损带来的磨粒也会在关节处造成炎症，严重时会给病人带来疼痛，甚至会让病人彻底丧失行动能力，因此，降低人工关节材料磨损是至关重要的。
目前解决人工关节置换材料无菌性松动问题和磨粒问题最常用的方式是选择力学性能和生物相容性更优异的材料作为关节置换材料。从高分子量聚乙烯到不锈钢材料、陶瓷和钴铬钼合金，再到钛合金材料，人工关节置换材料的综合性能得到了一定的提高，然而，随着人工置换关节病人年轻化趋势的发展以及活动量需求的提升，人们对人工关节材料的服役寿命提出了更高的要求。如何从提高关节滑液润滑性角度提高人工关节材料减摩耐磨性能，实现人工关节摩擦副延寿成为研究热点。王莹莹等[王莹莹,郁惠敏,刘蕾,等.含石墨烯仿生滑液对ZrO2陶瓷人工关节材料的润滑作用研究[J].摩擦学学报,2018,38(3):319-326.]利用良好生物相容性的透明质酸修饰具有良好润滑性能的氧化石墨烯制备了水分散性较好的氧化石墨烯透明质酸纳米复合材料，并且将复合材料作为仿生关节润滑液添加剂，研究发现复合材料添加在仿生关节液可以明显提高滑液的润滑性能。李稳稳[李稳稳.含牛血清蛋白纳米粒的仿生关节润滑液的制备与性能[D].河南大学,2016.]通过制备牛血清蛋白纳米粒并将其作为关节模拟润滑液的润滑添加剂，研究发现添加牛血清蛋白纳米粒可以很好的改善关节润滑液的润滑性能，延长ZrO2/ZrO2关节材料的使用寿命。
研究表明，通过在关节滑液中添加良好生物相容性的润滑颗粒可以增强陶瓷类人工关节材料的减摩抗磨性能，延长关节材料寿命，然而，润滑颗粒在关节滑液中的分散性一直没有很好的解决，此外，通过添加润滑颗粒来提高钛合金关节材料的报道较少，而钛合金作为目前人工关节摩擦副主要材料，其耐磨性有待进一步提高，此外，由于摩擦副材质的差别，现有的人工关节抗磨效果提升方法并不具有迁移性。
发明内容
本发明针对现有技术的不足，就是要提供一种关节滑液的制备方法，用以显著降低钛合金人工关节材料磨损。
本发明通过以下技术方案实施，具体步骤包括：
(1)纳米润滑颗粒聚N-异丙基丙烯酰胺的制备：
将0.5～1g N-异丙基丙烯酰胺，12～18mg N,N'-亚甲基双丙烯酰胺，8～12mg十二烷基磺酸钠依次加入含50～65mL去离子水的烧杯中，磁力搅拌20min得到混合溶液，再将混合溶液加入到三口烧瓶中，将烧瓶密闭抽真空后，通入高纯氮气至烧瓶内压力恢复至1atm，最后将5mL 0.006～0.01g/mL的过硫酸铵溶液通过注射器加入到烧瓶中，在65～75℃进行反应4.8～5.2h，将所得样品使用透析袋透析9～12d，每隔12h换一次去离子水，即得纳米润滑颗粒聚(N-异丙基丙烯酰胺)；并将其配成1-5wt％的聚N-异丙基丙烯酰胺溶液备用；
(2)纳米润滑颗粒聚N-异丙基丙烯酰胺的分散：
1)pH调节：将3～5mL 0.5mol/L叠氮酸钠溶液加入20～30mL小牛血清中，再加入0.2mol/L的磷酸盐控制溶液pH在7.4～7.6；其中所述的磷酸盐为磷酸钠、磷酸钾或二者任意比例的混合物。
2)升温搅拌分散：将上述溶液按体积比1:1与上述聚N-异丙基丙烯酰胺溶液混合，在32～36℃条件下，磁力搅拌20～25min，得到混合溶液；
3)温度梯度冷却：将混合溶液以2℃/5min的速度冷却到室温，即得用于降低钛合金人工关节材料磨损的关节滑液。
和现有技术相比，本发明方法的工艺流程简单有效，材料生物相容性与安全性好，不会对人体产生毒副作用；本发明方法所制备的纳米润滑颗粒聚N-异丙基丙烯酰胺在关节滑液中分散性好，稳定时间长达30天以上；本发明方法所制备的滑液润滑性能好，可显著降低钛合金关节材料的磨损，相较于常规人工关节滑液，钛合金人工关节材料的磨损量降低幅度可达95％以上。
具体实施方式
下面结合具体实施例来对本发明进行详细说明：
将0.8g N-异丙基丙烯酰胺，15mg N,N'-亚甲基双丙烯酰胺,10mg十二烷基磺酸钠放入含60mL去离子水的烧杯中，磁力搅拌20min得到混合溶液，再将混合溶液加入到三口烧瓶中，将烧瓶密闭抽真空后，通入高纯氮气至烧瓶内压力恢复至1atm，接下来将5mL0.008g/mL的过硫酸铵溶液通过注射器加入到烧瓶中，在70℃进行反应5h，制备得的样品透析10d，每隔12h更换一次去离子水，并将其配成1.35wt％的聚N-异丙基丙烯酰胺溶液备用。接着将4mL 0.5mol/L叠氮酸钠溶液加入20mL小牛血清中，再加入0.2mol/L的磷酸钠控制溶液pH在7.5。将上述溶液按体积比1:1与上述聚N-异丙基丙烯酰胺溶液混合，在32℃条件下，磁力搅拌20min，得到混合溶液。最后让混合溶液以2℃/5min的速度冷却到室温，即得用于降低钛合金人工关节材料磨损的关节滑液。稳定性实验表明，滑液稳定时间超过35天。
将上述得到的人工关节滑液在以下的摩擦试验条件下(摩擦副材料：超高分子量聚乙烯销/Ti6Al4V盘，滑动速度：67mm/s，接触应力：4MPa)得到的钛合金人工关节材料的磨损量如表1所示。从表中数据可以看出，采用本发明方法和常规人工关节滑液小牛血清相比，钛合金磨损可降低95.8％，显示了本发明突出的降低钛合金人工关节材料磨损效果。
表1小牛血清与本发明关节滑液润滑后钛合金人工关节材料磨损量对比
Claims (2)
1.一种降低钛合金人工关节材料磨损的关节滑液制备方法，其特征在于，包括以下步骤：
(1)纳米润滑颗粒聚N-异丙基丙烯酰胺的制备：
将0.5～1g N-异丙基丙烯酰胺，12～18mg N,N'-亚甲基双丙烯酰胺，8～12mg十二烷基磺酸钠依次加入含50～65mL去离子水的烧杯中，磁力搅拌20min得到混合溶液，再将混合溶液加入到三口烧瓶中，将烧瓶密闭抽真空后，通入高纯氮气至烧瓶内压力恢复至1atm，最后将5mL0.006～0.01g/mL的过硫酸铵溶液通过注射器加入到烧瓶中，在65～75℃进行反应4.8～5.2h，将所得样品使用透析袋透析9～12d，每隔12h换一次去离子水，即得纳米润滑颗粒聚N-异丙基丙烯酰胺；并将其配成1-5wt％的聚N-异丙基丙烯酰胺溶液备用；
(2)纳米润滑颗粒聚N-异丙基丙烯酰胺的分散：
1)pH调节：将3～5mL0.5mol/L叠氮酸钠溶液加入20～30mL小牛血清中，再加入0.2mol/L的磷酸盐控制溶液pH在7.4～7.6；
2)升温搅拌分散：将上述溶液按体积比1:1与上述聚N-异丙基丙烯酰胺溶液混合，在32～36℃条件下，磁力搅拌20～25min，得到混合溶液；
3)温度梯度冷却：将混合溶液以2℃/5min的速度冷却到室温，即得用于降低钛合金人工关节材料磨损的关节滑液。
2.根据权利要求1所述的一种降低钛合金人工关节材料磨损的关节滑液制备方法，其特征在于，步骤(2)中所述的磷酸盐为磷酸钠、磷酸钾或二者任意比例的混合物。
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