CN105948731A - 一种仿骨生物陶瓷的制备方法 - Google Patents

一种仿骨生物陶瓷的制备方法 Download PDF

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CN105948731A
CN105948731A CN201610278072.1A CN201610278072A CN105948731A CN 105948731 A CN105948731 A CN 105948731A CN 201610278072 A CN201610278072 A CN 201610278072A CN 105948731 A CN105948731 A CN 105948731A
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金仲恩
全春兰
张帆
喻国贞
欧阳智琨
陈晋纳
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Abstract

本发明提供了一种仿骨生物陶瓷的制备方法，先将硝酸钙、2‑膦酸丁烷‑1，2，4‑三羧酸、磺基丁二酸酯淀粉、蔗糖、水份混合，在70～90℃条件下反应，再将所得反应物在180～210℃脱水、900～1100℃烧结，得到改性磷酸三钙粉末，最后将所得改性磷酸三钙粉末、钛酸四丁酯、磷酸二氢铵、聚乙烯吡咯烷酮、聚丁二酸丁二醇酯、石蜡、聚乙烯、四乙氧基硅烷、硬脂酸、大豆卵磷脂混合分散，球磨，先在200～380℃下烧结60～80min，再在850～1000℃下烧结40～60min℃，冷却，即得。本发明的生物陶瓷孔隙率78%～87%，压缩强度在209MPa，14天降解率在5.15%，28天降解率8.72%，具有很好的力学强度和降解性能。

Description

一种仿骨生物陶瓷的制备方法
技术领域
本发明属于生物医用材料的技术领域，具体涉及一种仿骨生物陶瓷的制备方法。
背景技术
骨骼作为人体重要的组成部分，其对人体的各个脏器起着不可替代的保护和支持作用，同时还担负着支撑躯干、造血、储钙、代谢等功能，是人体生命的基础。人体含有大小共计206块骨骼，一旦骨骼出现损伤，会对人体造成极大的损害，而且大部分骨缺损不能自愈，需要进行骨移植治疗，于是仿骨材料被广泛应用起来。可用于骨移植治疗的仿骨材料多种多样，一般包括金属材料、非金属材料以及高分子材料等，每种材料根据其性质及特点还可以继续分类，目前非金属材料中的磷酸三钙基生物陶瓷材料的应用十分广泛，由于其成分与骨质中的无机相成分十分相似，所以其降解性、相容性以及在诱导骨生长方面具有特殊的优势，一直都是研究的热点。
发明内容
本发明的目的是克服现有技术的不足而提供一种仿骨生物陶瓷的制备方法，所得生物陶瓷具有很好的力学强度和降解性能。
一种仿骨生物陶瓷的制备方法，包括以下步骤：
步骤1，以重量份计，将硝酸钙5～12份、2-膦酸丁烷-1，2，4-三羧酸4～12份、磺基丁二酸酯淀粉1～5份、蔗糖3～6份、水2～8份混合，在70～90℃条件下反应，得到反应物；
步骤2，将步骤1所得反应物在180～210℃脱水、900～1100℃烧结，得到改性磷酸三钙粉末；
步骤3，以重量份计，将步骤2所得改性磷酸三钙粉末10～20份、钛酸四丁酯1～5份、磷酸二氢铵2～6份、聚乙烯吡咯烷酮3～7份、聚丁二酸丁二醇酯1～4份、石蜡3～5份、聚乙烯2～6份、四乙氧基硅烷1～6份、硬脂酸3～6份、大豆卵磷脂1～5份混合分散，球磨，先在200～380℃下烧结60～80min，再在850～1000℃下烧结40～60min℃，冷却，即得。
进一步地，步骤1中反应时间为1～3h。
进一步地，步骤1中反应过程在CO2气氛中进行。
进一步地，步骤3中分散条件为2000～3000rpm、20～30min。
进一步地，步骤3中球磨在氮气或氩气氛围中进行。
进一步地，步骤1中还需要加入色拉油1～4份。
本发明的生物陶瓷孔隙率78％～87％，压缩强度在209MPa，14天降解率在5.15％，28天降解率8.72％，具有很好的力学强度和降解性能。
具体实施方式
实施例1
一种仿骨生物陶瓷的制备方法，包括以下步骤：
步骤1，以重量份计，将硝酸钙5份、2-膦酸丁烷-1，2，4-三羧酸4份、磺基丁二酸酯淀粉1份、蔗糖3份、水2份混合，在70℃条件下反应，得到反应物；
步骤2，将步骤1所得反应物在180℃脱水、1100℃烧结，得到改性磷酸三钙粉末；
步骤3，以重量份计，将步骤2所得改性磷酸三钙粉末10份、钛酸四丁酯1份、磷酸二氢铵2份、聚乙烯吡咯烷酮3份、聚丁二酸丁二醇酯1份、石蜡3份、聚乙烯2份、四乙氧基硅烷1份、硬脂酸3份、大豆卵磷脂1份混合分散，球磨，先在200℃下烧结60min，再在850℃下烧结60min℃，冷却，即得。
其中，步骤1中反应时间为1h，反应过程在CO2气氛中进行；步骤3中分散条件为2000rpm、30min，球磨在氮气氛围中进行。
实施例2
一种仿骨生物陶瓷的制备方法，包括以下步骤：
步骤1，以重量份计，将硝酸钙8份、2-膦酸丁烷-1，2，4-三羧酸7份、磺基丁二酸酯淀粉2份、蔗糖5份、水7份混合，在80℃条件下反应，得到反应物；
步骤2，将步骤1所得反应物在200℃脱水、1000℃烧结，得到改性磷酸三钙粉末；
步骤3，以重量份计，将步骤2所得改性磷酸三钙粉末15份、钛酸四丁酯4份、磷酸二氢铵4份、聚乙烯吡咯烷酮5份、聚丁二酸丁二醇酯2份、石蜡4份、聚乙烯5份、四乙氧基硅烷3份、硬脂酸4份、大豆卵磷脂3份混合分散，球磨，先在250℃下烧结65min，再在900℃下烧结50min℃，冷却，即得。
其中，步骤1中反应时间为2h，反应过程在CO2气氛中进行；步骤3中分散条件为2400rpm、25min，球磨在氮气氛围中进行。
实施例3
一种仿骨生物陶瓷的制备方法，包括以下步骤：
步骤1，以重量份计，将硝酸钙12份、2-膦酸丁烷-1，2，4-三羧酸12份、磺基丁二酸酯淀粉5份、蔗糖6份、水8份混合，在90℃条件下反应，得到反应物；
步骤2，将步骤1所得反应物在210℃脱水、900℃烧结，得到改性磷酸三钙粉末；
步骤3，以重量份计，将步骤2所得改性磷酸三钙粉末20份、钛酸四丁酯5份、磷酸二氢铵6份、聚乙烯吡咯烷酮7份、聚丁二酸丁二醇酯4份、石蜡5份、聚乙烯6份、四乙氧基硅烷6份、硬脂酸6份、大豆卵磷脂5份混合分散，球磨，先在380℃下烧结80min，再在100℃下烧结40min℃，冷却，即得。
其中，步骤1中反应时间为3h，反应过程在CO2气氛中进行；步骤3中分散条件为3000rpm、20min，球磨在氮气氛围中进行。
实施例4
本实施例与实施例3的区别在于：步骤1中还需要加入色拉油1～4份。
一种仿骨生物陶瓷的制备方法，包括以下步骤：
步骤1，以重量份计，将硝酸钙12份、2-膦酸丁烷-1，2，4-三羧酸12份、磺基丁二酸酯淀粉5份、蔗糖6份、色拉油4份、水8份混合，在90℃条件下反应，得到反应物；
步骤2，将步骤1所得反应物在210℃脱水、900℃烧结，得到改性磷酸三钙粉末；
步骤3，以重量份计，将步骤2所得改性磷酸三钙粉末20份、钛酸四丁酯5份、磷酸二氢铵6份、聚乙烯吡咯烷酮7份、聚丁二酸丁二醇酯4份、石蜡5份、聚乙烯6份、四乙氧基硅烷6份、硬脂酸6份、大豆卵磷脂5份混合分散，球磨，先在380℃下烧结80min，再在100℃下烧结40min℃，冷却，即得。
其中，步骤1中反应时间为3h，反应过程在CO2气氛中进行；步骤3中分散条件为3000rpm、20min，球磨在氮气氛围中进行。
将实施例1至4所得生物陶瓷进行性能测试，结果如下：
本发明的生物陶瓷孔隙率78％～87％，压缩强度在209MPa，14天降解率在5.15％，28天降解率8.72％，具有很好的力学强度和降解性能。

Claims (6)

1.一种仿骨生物陶瓷的制备方法，其特征在于：包括以下步骤：
步骤1，以重量份计，将硝酸钙5～12份、2-膦酸丁烷-1，2，4-三羧酸4～12份、磺基丁二酸酯淀粉1～5份、蔗糖3～6份、水2～8份混合，在70～90℃条件下反应，得到反应物；
步骤2，将步骤1所得反应物在180～210℃脱水、900～1100℃烧结，得到改性磷酸三钙粉末；
步骤3，以重量份计，将步骤2所得改性磷酸三钙粉末10～20份、钛酸四丁酯1～5份、磷酸二氢铵2～6份、聚乙烯吡咯烷酮3～7份、聚丁二酸丁二醇酯1～4份、石蜡3～5份、聚乙烯2～6份、四乙氧基硅烷1～6份、硬脂酸3～6份、大豆卵磷脂1～5份混合分散，球磨，先在200～380℃下烧结60～80min，再在850～1000℃下烧结40～60min℃，冷却，即得。
2.根据权利要求1所述的仿骨生物陶瓷的制备方法，其特征在于：步骤1中反应时间为1～3h。
3.根据权利要求1所述的仿骨生物陶瓷的制备方法，其特征在于：步骤1中反应过程在CO2气氛中进行。
4.根据权利要求1所述的仿骨生物陶瓷的制备方法，其特征在于：步骤3中分散条件为2000～3000rpm、20～30min。
5.根据权利要求1所述的仿骨生物陶瓷的制备方法，其特征在于：步骤3中球磨在氮气或氩气氛围中进行。
6.根据权利要求1所述的仿骨生物陶瓷的制备方法，其特征在于：步骤1中还需要加入色拉油1～4份。
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FR3065645A1 (fr) * 2017-04-27 2018-11-02 Lifco Industrie Elaboration d'un biomateriau pour le comblement osseux par frittage de poudres composites

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