CN109529105A - 仿生人工骨材料的制备方法 - Google Patents
仿生人工骨材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种仿生人工骨材料的制备方法，该方法包括以下步骤：步骤一，将过氧化氢溶液和螃蟹壳粉混合均匀，超声分散，备用；步骤二，将植物纤维、碳酸钙、壳聚糖、羟基磷灰石混合，加入去离子水，混合均匀；加入红霉素、硫酸钙和磺酸钠，超声分散，备用；步骤三，将步骤一和步骤二备用的混合物混合，升温至70～80℃，搅拌至糊状；步骤四，将糊状混合物放入模具中，‑100～‑80℃条件下快速冷冻成型；降温至‑20～‑15℃，再次冷冻1～5h；步骤五，烘干，灭菌，即可。本发明添加了螃蟹壳粉，可以促进人体骨骼修复，增强人工骨的强度。
Description
技术领域
本发明属于复合材料领域，尤其涉及一种仿生人工骨材料的制备方法。
背景技术
骨骼之所以能成为理想的生物体支架，是因为它同时具备了硬度和弹性。从电子显微镜下观察，骨骼有一套非常精巧的结构：一束束的有机胶原蛋白基质中“镶嵌”着一层层无机羟基磷灰石(HAP)晶体，这种多层复合的结构让骨骼的硬度和抗弯能力兼备。骨骼中的HAP晶体是已知生物材料中最薄的晶体，厚度仅为1.5到2纳米左右。
在骨科领域,由于严重创伤、骨肿瘤、骨髓炎等多种原因所致的骨缺损十分常见。目前常用的骨修复材料包括自体骨和金属假体。自体骨增加了患者的创伤和痛苦；金属假体存在松动、断裂等问题。因此,人工骨替代材料移植修复骨缺损成为医学重点。人工骨(Artificail Bone)是指可以替代人体骨或者修复骨组织缺损的人工生物材料。当需替换关节或治疗骨断裂时，最理想的方式是通过组织再生功能实现骨的自身修复。然而在许多情形下，人体骨并不能实现自身修复，例如骨组织坏死，骨关节创伤，这时就需要人工骨的帮助，理想人工骨材料的研制是医学和生物材料科学领域的一个重要课题。
发明内容
本发明为了解决现有技术的不足，提供了一种仿生人工骨材料的制备方法，方法简单，且具有一定的人工骨作用。
为了解决上述技术问题，本发明采用以下技术方案：
仿生人工骨材料的制备方法，包括以下步骤：
步骤一，将过氧化氢溶液和螃蟹壳粉混合均匀，超声分散，备用；
步骤二，将植物纤维、碳酸钙、壳聚糖、羟基磷灰石混合，加入去离子水，混合均匀；加入红霉素、硫酸钙和磺酸钠，超声分散，备用；
步骤三，将步骤一和步骤二备用的混合物混合，升温至70～80℃，搅拌至糊状；
步骤四，将糊状混合物放入模具中，-100～-80℃条件下快速冷冻成型；降温至-20～-15℃，再次冷冻1～5h；
步骤五，烘干，灭菌，即可。
作为优选，所述各原料的重量份比为：过氧化氢溶液40～60份、螃蟹壳粉30～80份、植物纤维10～20份、碳酸钙40～80份、壳聚糖1～3份、羟基磷灰石40～90份、红霉素4～8份、硫酸钙30～40份、磺酸钠20～30份和去离子水50～90份。
作为优选，所述各原料的重量份比为：过氧化氢溶液50份、螃蟹壳粉50份、植物纤维15份、碳酸钙60份、壳聚糖2份、羟基磷灰石50份、红霉素6份、硫酸钙35份、磺酸钠25份和去离子水70份。
作为优选，所述各原料的重量份比为：过氧化氢溶液46份、螃蟹壳粉40份、植物纤维16份、碳酸钙45份、壳聚糖3份、羟基磷灰石60份、红霉素7份、硫酸钙33份、磺酸钠23份和去离子水80份。
作为优选，所述过氧化氢溶液的质量浓度为5％。
作为优选，所述去离子水中含有氯化钠，氯化钠的质量浓度为0.5％。
作为优选，步骤一中，超声分散频率为60～80kHz，分散时间为20～30min。
作为优选，步骤二中，超声分散频率为420～500kHz，分散时间为1～2h。
作为优选，步骤四快速冷冻成型阶段，降温速率为40～60℃/min。
作为优选，所述螃蟹壳粉的制备方法如下：将螃蟹壳洗净，干燥，粉碎后加入乙酸溶液，一边搅拌一边加入氧化铜粉末和磷酸三钙，升温至60～100℃反应2～3h，冷冻成型后，粉碎。
作为优选，所述的螃蟹壳、乙酸溶液、氧化铜粉末和磷酸三钙的质量比为9:12:3:4。
本发明添加了螃蟹壳粉，螃蟹的外壳是由高度矿化的几丁质-蛋白质纤维组成的，硬度较高，断裂韧性好，还可以促进人体骨骼修复，增强人工骨的强度。过氧化氢溶液加热产生的气体，使骨内部形成孔隙，提高骨的孔隙率。植物纤维有利于成骨细胞的生长。
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介绍。
实施例1
仿生人工骨材料的制备方法，包括以下步骤：
步骤一，将质量浓度为5％的过氧化氢溶液和螃蟹壳粉混合均匀，超声分散，超声分散频率为60～80kHz，分散时间为20～30min，备用；
步骤二，将植物纤维、碳酸钙、壳聚糖、羟基磷灰石混合，加入去离子水，混合均匀；加入红霉素、硫酸钙和磺酸钠，超声分散，超声分散频率为420～500kHz，分散时间为1～2h，备用；
步骤三，将步骤一和步骤二备用的混合物混合，升温至70～80℃，搅拌至糊状；
步骤四，将糊状混合物放入模具中，以40～60℃/min的降温速率降至-100～-80℃，冷冻成型；降温至-20～-15℃，再次冷冻1～5h；
步骤五，烘干，灭菌，即可。
所述各原料的重量份比为：过氧化氢溶液50份、螃蟹壳粉50份、植物纤维15份、碳酸钙60份、壳聚糖2份、羟基磷灰石50份、红霉素6份、硫酸钙35份、磺酸钠25份和去离子水70份。
所述去离子水中含有氯化钠，氯化钠的质量浓度为0.5％。
所述螃蟹壳粉的制备方法如下：将螃蟹壳洗净，干燥，粉碎后加入乙酸溶液，一边搅拌一边加入氧化铜粉末和磷酸三钙，升温至60～100℃反应2～3h，冷冻成型后，粉碎。所述的螃蟹壳、乙酸溶液、氧化铜粉末和磷酸三钙的质量比为9:12:3:4。
实施例2
仿生人工骨材料的制备方法，包括以下步骤：
步骤一，将质量浓度为5％的过氧化氢溶液和螃蟹壳粉混合均匀，超声分散，超声分散频率为60～80kHz，分散时间为20～30min，备用；
步骤二，将植物纤维、碳酸钙、壳聚糖、羟基磷灰石混合，加入去离子水，混合均匀；加入红霉素、硫酸钙和磺酸钠，超声分散，超声分散频率为420～500kHz，分散时间为1～2h，备用；
步骤三，将步骤一和步骤二备用的混合物混合，升温至70～80℃，搅拌至糊状；
步骤四，将糊状混合物放入模具中，以40～60℃/min的降温速率降至-100～-80℃，冷冻成型；降温至-20～-15℃，再次冷冻1～5h；
步骤五，烘干，灭菌，即可。
所述各原料的重量份比为：过氧化氢溶液40份、螃蟹壳粉80份、植物纤维20份、碳酸钙80份、壳聚糖3份、羟基磷灰石90份、红霉素8份、硫酸钙40份、磺酸钠30份和去离子水90份。
所述去离子水中含有氯化钠，氯化钠的质量浓度为0.5％。
所述螃蟹壳粉的制备方法如下：将螃蟹壳洗净，干燥，粉碎后加入乙酸溶液，一边搅拌一边加入氧化铜粉末和磷酸三钙，升温至60～100℃反应2～3h，冷冻成型后，粉碎。所述的螃蟹壳、乙酸溶液、氧化铜粉末和磷酸三钙的质量比为9:12:3:4。
实施例3
仿生人工骨材料的制备方法，包括以下步骤：
步骤一，将质量浓度为5％的过氧化氢溶液和螃蟹壳粉混合均匀，超声分散，超声分散频率为60～80kHz，分散时间为20～30min，备用；
步骤二，将植物纤维、碳酸钙、壳聚糖、羟基磷灰石混合，加入去离子水，混合均匀；加入红霉素、硫酸钙和磺酸钠，超声分散，超声分散频率为420～500kHz，分散时间为1～2h，备用；
步骤三，将步骤一和步骤二备用的混合物混合，升温至70～80℃，搅拌至糊状；
步骤四，将糊状混合物放入模具中，以40～60℃/min的降温速率降至-100～-80℃，冷冻成型；降温至-20～-15℃，再次冷冻1～5h；
步骤五，烘干，灭菌，即可。
所述各原料的重量份比为：过氧化氢溶液60份、螃蟹壳粉30份、植物纤维10份、碳酸钙40份、壳聚糖1份、羟基磷灰石40份、红霉素4份、硫酸钙30份、磺酸钠20份和去离子水50份。
所述去离子水中含有氯化钠，氯化钠的质量浓度为0.5％。
所述螃蟹壳粉的制备方法如下：将螃蟹壳洗净，干燥，粉碎后加入乙酸溶液，一边搅拌一边加入氧化铜粉末和磷酸三钙，升温至60～100℃反应2～3h，冷冻成型后，粉碎。所述的螃蟹壳、乙酸溶液、氧化铜粉末和磷酸三钙的质量比为9:12:3:4。
实施例4
仿生人工骨材料的制备方法，包括以下步骤：
步骤一，将质量浓度为5％的过氧化氢溶液和螃蟹壳粉混合均匀，超声分散，超声分散频率为60～80kHz，分散时间为20～30min，备用；
步骤二，将植物纤维、碳酸钙、壳聚糖、羟基磷灰石混合，加入去离子水，混合均匀；加入红霉素、硫酸钙和磺酸钠，超声分散，超声分散频率为420～500kHz，分散时间为1～2h，备用；
步骤三，将步骤一和步骤二备用的混合物混合，升温至70～80℃，搅拌至糊状；
步骤四，将糊状混合物放入模具中，以40～60℃/min的降温速率降至-100～-80℃，冷冻成型；降温至-20～-15℃，再次冷冻1～5h；
步骤五，烘干，灭菌，即可。
所述各原料的重量份比为：过氧化氢溶液46份、螃蟹壳粉40份、植物纤维16份、碳酸钙45份、壳聚糖3份、羟基磷灰石60份、红霉素7份、硫酸钙33份、磺酸钠23份和去离子水80份。
所述去离子水中含有氯化钠，氯化钠的质量浓度为0.5％。
所述螃蟹壳粉的制备方法如下：将螃蟹壳洗净，干燥，粉碎后加入乙酸溶液，一边搅拌一边加入氧化铜粉末和磷酸三钙，升温至60～100℃反应2～3h，冷冻成型后，粉碎。所述的螃蟹壳、乙酸溶液、氧化铜粉末和磷酸三钙的质量比为9:12:3:4。
对照例1
与实施例1的区别在于：用虾壳粉代替螃蟹壳粉。
仿生人工骨材料的制备方法，包括以下步骤：
步骤一，将质量浓度为5％的过氧化氢溶液和虾壳粉混合均匀，超声分散，超声分散频率为60～80kHz，分散时间为20～30min，备用；
步骤二，将植物纤维、碳酸钙、壳聚糖、羟基磷灰石混合，加入去离子水，混合均匀；加入红霉素、硫酸钙和磺酸钠，超声分散，超声分散频率为420～500kHz，分散时间为1～2h，备用；
步骤三，将步骤一和步骤二备用的混合物混合，升温至70～80℃，搅拌至糊状；
步骤四，将糊状混合物放入模具中，以40～60℃/min的降温速率降至-100～-80℃，冷冻成型；降温至-20～-15℃，再次冷冻1～5h；
步骤五，烘干，灭菌，即可。
所述各原料的重量份比为：过氧化氢溶液50份、虾壳粉50份、植物纤维15份、碳酸钙60份、壳聚糖2份、羟基磷灰石50份、红霉素6份、硫酸钙35份、磺酸钠25份和去离子水70份。
所述去离子水中含有氯化钠，氯化钠的质量浓度为0.5％。
所述虾壳粉的制备方法如下：将螃蟹壳洗净，干燥，粉碎后加入乙酸溶液，一边搅拌一边加入氧化铜粉末和磷酸三钙，升温至60～100℃反应2～3h，冷冻成型后，粉碎。所述的虾壳粉、乙酸溶液、氧化铜粉末和磷酸三钙的质量比为9:12:3:4。
对照例2
与实施例2的区别在于：未加植物纤维。
仿生人工骨材料的制备方法，包括以下步骤：
步骤一，将质量浓度为5％的过氧化氢溶液和螃蟹壳粉混合均匀，超声分散，超声分散频率为60～80kHz，分散时间为20～30min，备用；
步骤二，将碳酸钙、壳聚糖、羟基磷灰石混合，加入去离子水，混合均匀；加入红霉素、硫酸钙和磺酸钠，超声分散，超声分散频率为420～500kHz，分散时间为1～2h，备用；
步骤三，将步骤一和步骤二备用的混合物混合，升温至70～80℃，搅拌至糊状；
步骤四，将糊状混合物放入模具中，以40～60℃/min的降温速率降至-100～-80℃，冷冻成型；降温至-20～-15℃，再次冷冻1～5h；
步骤五，烘干，灭菌，即可。
所述各原料的重量份比为：过氧化氢溶液40份、螃蟹壳粉80份、碳酸钙80份、壳聚糖3份、羟基磷灰石90份、红霉素8份、硫酸钙40份、磺酸钠30份和去离子水90份。
所述去离子水中含有氯化钠，氯化钠的质量浓度为0.5％。
所述螃蟹壳粉的制备方法如下：将螃蟹壳洗净，干燥，粉碎后加入乙酸溶液，一边搅拌一边加入氧化铜粉末和磷酸三钙，升温至60～100℃反应2～3h，冷冻成型后，粉碎。所述的螃蟹壳、乙酸溶液、氧化铜粉末和磷酸三钙的质量比为9:12:3:4。
性能测试：
螃蟹外壳由高度矿化的几丁质-蛋白质纤维组成的，硬度较高，断裂韧性好，还可以促进人体骨骼修复，增强人工骨的强度。植物纤维有利于成骨细胞的生长，提高孔隙率。
以上所述，仅为本发明较佳的具体实施方案，本发明的保护范围不限于此，任何熟悉本技术领域的技术人员在本发明披露的技术范围内，可显而易见地得到的技术方案的简单变化或等效替换均落入本发明的保护范围内。
Claims (9)
1.仿生人工骨材料的制备方法，其特征在于，包括以下步骤：
步骤一，将过氧化氢溶液和螃蟹壳粉混合均匀，超声分散，备用；
步骤二，将植物纤维、碳酸钙、壳聚糖、羟基磷灰石混合，加入去离子水，混合均匀；加入红霉素、硫酸钙和磺酸钠，超声分散，备用；
步骤三，将步骤一和步骤二备用的混合物混合，升温至70～80℃，搅拌至糊状；
步骤四，将糊状混合物放入模具中，-100～-80℃条件下快速冷冻成型；降温至-20～-15℃，再次冷冻1～5h；
步骤五，烘干，灭菌，即可。
2.根据权利要求1所述的仿生人工骨材料的制备方法，其特征在于，所述各原料的重量份比为：过氧化氢溶液40～60份、螃蟹壳粉30～80份、植物纤维10～20份、碳酸钙40～80份、壳聚糖1～3份、羟基磷灰石40～90份、红霉素4～8份、硫酸钙30～40份、磺酸钠20～30份和去离子水50～90份。
3.根据权利要求1所述的仿生人工骨材料的制备方法，其特征在于，所述过氧化氢溶液的质量浓度为5％。
4.根据权利要求1所述的仿生人工骨材料的制备方法，其特征在于，所述去离子水中含有氯化钠，氯化钠的质量浓度为0.5％。
5.根据权利要求1所述的仿生人工骨材料的制备方法，其特征在于，步骤一中，超声分散频率为60～80kHz，分散时间为20～30min。
6.根据权利要求1所述的仿生人工骨材料的制备方法，其特征在于，步骤二中，超声分散频率为420～500kHz，分散时间为1～2h。
7.根据权利要求1所述的仿生人工骨材料的制备方法，其特征在于，步骤四快速冷冻成型阶段，降温速率为40～60℃/min。
8.根据权利要求1所述的仿生人工骨材料的制备方法，其特征在于，所述螃蟹壳粉的制备方法如下：将螃蟹壳洗净，干燥，粉碎后加入乙酸溶液，一边搅拌一边加入氧化铜粉末和磷酸三钙，升温至60～100℃反应2～3h，冷冻成型后，粉碎。
9.根据权利要求8所述的仿生人工骨材料的制备方法，其特征在于，所述的螃蟹壳、乙酸溶液、氧化铜粉末和磷酸三钙的质量比为9:12:3:4。
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| CN111068121A (zh) * | 2019-12-30 | 2020-04-28 | 浙江农林大学 | 一种木质基仿生骨支架材料的制备方法 |
| CN112354016A (zh) * | 2020-11-24 | 2021-02-12 | 重庆工程职业技术学院 | 一种仿生人工骨材料及其生产方法 |
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