CN106075601A - 一种竹纤维/羟基磷灰石/聚乳酸类三元复合可降解多孔材料及其制备方法 - Google Patents
一种竹纤维/羟基磷灰石/聚乳酸类三元复合可降解多孔材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种竹纤维/羟基磷灰石/聚乳酸类多孔材料及其制备方法。该竹纤维/羟基磷灰石/聚乳酸类多孔材料是指将羟基磷灰石分散液滴加到竹纤维和聚乳酸类复合的1,4二氧六环分散液中，超声搅拌后置于培养皿中，冷冻干燥得三元复合多孔材料。本发明制得的三元复合多孔材料其力学性能比羟基磷灰石/聚乳酸类二元复合多孔材料明显提高，其孔径变大，且能完全降解，制备方法简单，多孔材料结构可控，有望用做新型骨组织工程支架材料。
Description
技术领域
本发明涉及一种竹纤维/羟基磷灰石/聚乳酸类三元复合可降解多孔材料及其制备方法，属于生物医用材料领域。
背景技术
骨缺损修复问题一直是骨科医生面临的难题。随着组织工程学的迅速发展，利用组织工程学的方法修复骨缺损已成为一种全新的治疗模式。在骨组织工程的研究中，主要包含以下三个方面的关键因素：信号分子(骨生长因子、骨诱导因子)、支架材料和靶细胞。其中支架材料在骨组织工程中扮演着极为重要的角色，一方面作为信号因子的载体，将其运送到缺损位置；另一方面可提供新骨生长的框架。故研制理想的支架材料则是骨组织工程研究的关键问题。要获得理想的支架材料，若仅靠单一材料，显然很难满足以上各项性能的要求，因此人们通常模仿天然骨的成分和结构特征进行仿生制备无机/有机杂化支架。纳米羟基磷灰石/聚乳酸类支架材料综合了聚乳酸的可降解性和生物相容性，以及纳米羟基磷灰石的骨传导性及弱碱性，因而是骨组织工程支架材料研究的热点。但研究表明该纳米羟基磷灰石/聚乳酸类复合支架其力学性能及降解性仍有待提高。
纤维作为增强体在复合材料中能起到传递载荷作用，因而是增强材料的研究热点。碳纤维作为增强材料具有以下优势：强度高，吸附能力高，表面有很多亲水性基团。浙江大学沈烈等将碳纤维用浓硝酸处理后，采用溶液共混法制备了炭碳纤维/羟基磷灰石/聚乳酸复合生物材料(复合材料学报，2007,24（5）：61-65)。通过模压成型获得的CF/HA/PLA 复合材料具有优异的力学性能，与HA/PLA 复合材料相比，剪切强度提高了4~5倍。但碳纤维不降解，留在体内可能成为永久的异物，显然无法满足骨组织工程支架材料的降解性要求。
天然植物纤维具有低成本、低密度、良好的比强度、易于分离以及可降解性等优点，是聚合物的绿色增强材料。竹纤维是天然植物纤维中的一种，不仅资源丰富、有优异的力学性能，还具有天然抗菌、除臭、吸湿放湿、抗紫外线等优点，被誉为增强聚合物的“天然玻璃纤维”。目前已经用于增强的聚合物，并实现商业化生产的主要有聚乳酸(PLA)、聚丁二酸丁二醇酯(PBS)、聚羟基丁酸酯(PHB)、聚已内酰胺(PCL)等。这些塑料大多具有优良的可塑性、易加工成型等特点，主要应用于汽车部件、装饰装修、电器产品、包装、纺织业和医疗保健等领域。但用于增强羟基磷灰石/聚乳酸复合的多孔材料至今未见报道。
发明内容
针对上述情况，本发明的目的在于提供一种竹纤维/羟基磷灰石/聚乳酸类(BF/HA/PLGA) 三元复合可降解多孔材料及其制备方法。本发明制备的竹纤维/羟基磷灰石/聚乳酸类三元复合可降解多孔材料具有较高的力学性能、降解性能及生物相容性，是一种新型可降解多孔材料，能满足骨组织工程支架材料性能的基本要求。
本发明采用以下技术方案：竹纤维是指经表面处理后的竹纤维；羟基磷灰石
是指经表面接枝少量聚乳酸后的改性羟基磷灰石；聚乳酸类高聚物L-乳酸（L-LA）与乙醇酸（GA）共聚物，摩尔比为92 : 8～98 : 2，粘均分子量在30~60万。
本发明所涉竹纤维的制备方法可以参照Li Ye等人报道的竹纤维的处理的方
法（Industrial & Engineering Chemistry Research，2015; 54: 12017−12024）。聚-L-乳酸/乙醇酸共聚物(L-PLGA)的制备方法可以参照Wang Liansong等人报道的PLGA的制备方法（Journal of polymer rerearch, 2010, 17:77–82），羟基磷灰石的制备方法可以参照Jiang Liuyun等人报道的方法（Applied Surface Science, 2012; 259:72-78）。
本发明的竹纤维/羟基磷灰石/聚乳酸类三元复合可降解多孔材料由下述技术方案实现的，其特征在于采用如下工艺步骤：
（1）称取一定量的PLGA溶解于1,4-二氧六环，加入改性的BF搅拌至均匀分散。同时将n-HA超声分散于1,4二氧六环的分散液滴加到BF/PLGA混合溶液中，继续超声磁力搅拌后转移到表面皿中。
（2）将上述混合的复合材料放入冰箱中冷冻或液氮中冷冻，再用冷冻干燥机冷冻干燥至恒重，放入40℃真空烘箱中烘干。
本发明的优越性在于：（1）本发明所用的原材料来源广泛，尤其是竹纤维资源丰富，价格便宜。
（2）本发明制备的竹纤维/羟基磷灰石/聚乳酸类三元复合可降解多孔材料，与羟基磷灰石/聚乳酸类二元复合多孔材料相比，可利用其中的竹纤维改善其多孔结构，并能提高其力学性能，同时可改善其降解性能，从而获得理想的骨组织工程支架材料。
（3）该新型竹纤维/羟基磷灰石/聚乳酸类三元复合可降解多孔材料其制备方法简单易行，成本低，绿色环保，适合大规模生产，有望用于骨组织工程支架材料。
附图说明
图1为羟基磷灰石/聚乳酸类二元复合多孔材料及竹纤维/羟基磷灰石/聚乳酸类三元复合多孔材料的SEM照片。(a) 30%HA/PLGA复合材料; (b) 20%BF/30%HA/PLGA复合材料。
具体实施方式
实施例1：称取3.0 g PLGA（LA : GA摩尔比为92 : 08，分子量为40万）溶解于100ml 1,4-二氧六环，加入5.0 g长径为1 mm，直径为0.2 mm的改性竹纤维搅拌至均匀分散。同时将2.0 g 纳米羟基磷灰石超声分散于100 ml 1,4二氧六环，超声1 h后，将n-HA分散液滴加到上述BF/PLGA混合液中。继续超声磁力搅拌4 h后转移到表面皿中。放入-20 ℃的冰箱中冷冻48 h。用冷冻干燥机冷冻干燥至恒重，放入40℃真空烘箱中烘干。将其切割成10 mm×10 mm×10 mm的块状材料，测得抗压强度为2.53 MPa, 孔隙率为88 %，平均孔径为450um。
实施例2：称取4.0 g PLGA（LA : GA摩尔比为95 : 05，分子量为35万）溶解于150ml 1,4-二氧六环，加入3.0 g长径为5 mm，直径为0.1 mm的改性竹纤维搅拌至均匀分散。同时将3.0 g 纳米羟基磷灰石超声分散于50 ml 1,4二氧六环，超声1 h后，将n-HA分散液滴加到上述BF/PLGA混合液中。继续超声磁力搅拌4 h后转移到表面皿中。放入-40℃的冰箱中冷冻48 h。用冷冻干燥机冷冻干燥至恒重，放入40 ℃真空烘箱中烘干。将其切割成10 mm×10 mm×10 mm的块状材料，测得抗压强度为3.45 MPa, 孔隙率为85 %，平均孔径为250 um。
实施例3：称取2.0 g PLGA（LA : GA摩尔比为95 : 05，分子量为45万）溶解于100ml 1,4-二氧六环，加入4.0 g长径为8 mm，直径为0.2 mm的改性竹纤维搅拌至均匀分散。同时将4.0 g 纳米羟基磷灰石超声分散于100 ml 1,4二氧六环，超声2 h后，将n-HA分散液滴加到上述BF/PLGA混合液中。继续超声磁力搅拌5 h后转移到表面皿中。放入-196 ℃的冰箱中冷冻48 h。用冷冻干燥机冷冻干燥至恒重，放入40℃真空烘箱中烘干。将其切割成10 mm×10 mm×10 mm的块状材料，测得抗压强度为3.45 MPa, 孔隙率为83 %，平均孔径为200um。
对比实施例1：称取6.0 g PLGA（LA : GA摩尔比为95 : 05，分子量为45万）溶解于100 ml 1,4-二氧六环。将4.0 g 纳米羟基磷灰石超声分散于100 ml 1,4二氧六环，超声2h后，将n-HA分散液滴加到上述BF/PLGA混合液中。继续超声磁力搅拌5 h后转移到表面皿中。放入-40 ℃的冰箱中冷冻48 h。用冷冻干燥机冷冻干燥至恒重，放入40℃真空烘箱中烘干。将其切割成10 mm×10 mm×10 mm的块状材料，测得抗压强度为0.82 MPa, 孔隙率为75%，平均孔径为100 um。
抗压强度测试条件：将切好的10 mm×10 mm×10 mm块状材料用万能材料试验机（SANSCMT4503，中国深圳SANS公司）测试其压缩变形为40 %时的压缩性能。测试温度为20℃±2℃，加载速度为1 mm/min。每组测试五个平行样，结果取平均值。
孔隙率的测定：向量筒中加入适量无水乙醇，将切好的10 mm×10 mm×10 mm块状材料称干重记为m1，放入无水乙醇中，称乙醇和样品初始重量记为V1。在室温下浸泡1周后将材料取出称材料湿重为m2，剩余乙醇重量为V2。则孔隙率θ=[ (m2-m1)/ρ]/(V1-V2)。每个样品测三个平行样，取平均值。
Claims (4)
1.一种竹纤维/羟基磷灰石/聚乳酸类多孔材料，其特征为竹纤维、羟基磷灰石及聚乳酸类三元复合物在1,4二氧六环溶剂中超声搅拌后，置于培养皿中预冷后冷冻干燥 。
2.按照权利要求1所述的竹纤维，其特征是指经表面处理后的竹纤维长度3~10mm，直径0.05~0.3mm。
3.按照权利要求1所述的三元复合物其组分比例，其特征是指质量比为：竹纤维占为5%~40%，羟基磷灰石含量为10~40%，聚乳酸为20%~85%。
4.按照权利要求1所述的在1,4二氧六环溶剂中超声搅拌，其特征是指浓度为物料干重在1,4二氧六环中占2 %~8% (w/v)。
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