CN106337155B - 抗菌能力较好的生物医用金属材料 - Google Patents
抗菌能力较好的生物医用金属材料 Download PDFInfo
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- CN106337155B CN106337155B CN201610741939.2A CN201610741939A CN106337155B CN 106337155 B CN106337155 B CN 106337155B CN 201610741939 A CN201610741939 A CN 201610741939A CN 106337155 B CN106337155 B CN 106337155B
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 16
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 15
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- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims abstract description 8
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- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 14
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- KWUZCAVKPCRJPO-UHFFFAOYSA-N n-ethyl-4-(6-methyl-1,3-benzothiazol-2-yl)aniline Chemical compound C1=CC(NCC)=CC=C1C1=NC2=CC=C(C)C=C2S1 KWUZCAVKPCRJPO-UHFFFAOYSA-N 0.000 claims description 7
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- 239000011575 calcium Substances 0.000 claims 1
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- 230000007797 corrosion Effects 0.000 abstract description 11
- 238000005260 corrosion Methods 0.000 abstract description 11
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
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- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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Classifications
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Abstract
本发明提供了一种抗菌能力较好的生物医用金属材料，所述金属材料原料包括铌粉、铂粉、钛粉、钼粉、纤维素硝酸酯、磷酸三苯酯、抗氧剂、辅助抗氧剂、硅灰石纤维、二丁基硫醇锡、邻苯二甲酸二丁酯、亚磷酸三苯酯、玻璃酸、淀粉、硅酸钙和2‑乙基‑4‑甲基咪唑。其制备方法为先将各组分加至混合搅拌机中，搅拌混合均匀，将所得混合物料加入到反应釜中，在氮气氛围中加热搅拌反应，将所得反应物送入双螺杆挤出机中经挤出、水冷、风干、切粒，得到生物医用金属材料。本发明所得生物医用金属材料不仅硬度和耐腐性能都有不同程度的提高，而且对大肠杆菌和金黄色葡萄球菌均具有良好的抗菌能力，其抗菌率分别可达到99.5%和98.45%。
Description
技术领域
本发明属于生物医用材料技术领域，具体涉及一种生物医用金属材料及其制备方法。
背景技术
生物医用材料是指用于医疗上能够植入生物体或与生物组织相结合的材料，可用于诊断、治疗，以及替换生物机体中的组织、器官或增进其功能。目前用于临床的生物医用材料主要包括生物医用金属材料、生物医用有机材料(主要指有机高分子材料)、生物医用无机非金属材料(主要指生物陶瓷)、生物玻璃和碳素材料以及生物医用复合材料等。与生物陶瓷及生物高分子材料相比，生物医用金属材料，如不锈钢、钴基合金、钛和钛合金以及贵金属等具有高的强度、良好的韧性及抗弯曲疲劳强度、优异的加工性能等许多其他医用材料不可替代的优良性能。
生物医用金属材料在应用中面临的主要问题，是由于生理环境的腐蚀而造成的金属离子向周围组织扩散以及植入材料自身性质的退变，前者可能导致毒副作用，后者可能导致植入失败。医用金属材料作为生物材料的一类，其研究和发展要严格满足如下从的生物学要求：良好的组织相容性，包括无毒性、无热源反应、不致畸、不致癌、不引起过敏反应或干扰机体的免疫机理、不破坏临近组织，也不发生材料表面的钙化沉着等；良好的物理、化学稳定性，包括强度、弹性、尺寸稳定性、耐腐蚀性、耐磨性以及界面稳定性等；易于加工成型，材料易于制造；价格适当。
因此，研究和开发性能更优，生物相容性更好的新型生物医用金属材料是材料工作者和医务工作者共同关心的课题。
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生物医用金属材料及其制备方法，该材料具有良好的抗菌性、力学性能和耐腐蚀性能。
一种生物医用金属材料，原料以重量份计包括：铌粉3～9份，铂粉2～8份，钛粉1～7份，钼粉2～7份，纤维素硝酸酯1～6份，磷酸三苯酯3～8份，抗氧剂1～7份，辅助抗氧剂2～8份，硅灰石纤维1～5份，二丁基硫醇锡2～7份，邻苯二甲酸二丁酯3～9份，亚磷酸三苯酯3～8份，玻璃酸2～7份，淀粉1～8份，硅酸钙2～9份，2-乙基-4-甲基咪唑1～6份。
作为上述发明的进一步改进，所述铌粉、铂粉、钛粉和钼粉的粒度为100～200目。
作为上述发明的进一步改进，所述抗氧剂为抗氧剂1010和抗氧剂1076的混合物，其中，抗氧剂1010和抗氧剂1076的重量比为3:2。
作为上述发明的进一步改进，所述辅助抗氧剂为硫代二丙酸双月桂酯。
上述生物医用金属材料的制备方法，包括以下步骤：
步骤1，将各组分加至混合搅拌机中，搅拌混合均匀，得到混合物料；
步骤2，将步骤1所得混合物料加入到反应釜中，在氮气氛围中加热到65～80℃，搅拌反应30～40min，得到反应物；
步骤3，将步骤2所得反应物送入双螺杆挤出机中经挤出、水冷、风干、切粒，得到生物医用金属材料。
作为上述发明的进一步改进，步骤1中搅拌混合均匀的搅拌速度为300～400rpm，搅拌时间为20～40min。
作为上述发明的进一步改进，步骤3中双螺杆挤出机的挤出条件为：一区温度180～200℃、二区温度200～220℃、三区温度210～230℃、四区温度230～250℃，螺杆转速为160～180rpm。
本发明的生物医用金属材料不仅硬度和耐腐性能都有不同程度的提高，而且对大肠杆菌和金黄色葡萄球菌均具有良好的抗菌能力，其抗菌率分别可达到99.5％和98.45％，能满足生物医用金属材料所需的抗菌性、力学性能和耐腐蚀性能的要求。
具体实施方式
实施例1
一种生物医用金属材料，原料以重量份计包括：铌粉3份，铂粉2份，钛粉1份，钼粉2份，纤维素硝酸酯1份，磷酸三苯酯3份，抗氧剂1份，辅助抗氧剂2份，硅灰石纤维1份，二丁基硫醇锡2份，邻苯二甲酸二丁酯3份，亚磷酸三苯酯3份，玻璃酸2份，淀粉1份，硅酸钙2份，2-乙基-4-甲基咪唑1份。
上述铌粉、铂粉、钛粉和钼粉的粒度为100目。
上述抗氧剂为抗氧剂1010和抗氧剂1076的混合物，其中，抗氧剂1010和抗氧剂1076的重量比为3:2。
上述辅助抗氧剂为硫代二丙酸双月桂酯。
上述生物医用金属材料的制备方法，包括以下步骤：
步骤1，将各组分加至混合搅拌机中，搅拌混合均匀，搅拌速度为300rpm，搅拌时间为40min，得到混合物料；
步骤2，将步骤1所得混合物料加入到反应釜中，在氮气氛围中加热到65℃，搅拌反应40min，得到反应物；
步骤3，将步骤2所得反应物送入双螺杆挤出机中经挤出、水冷、风干、切粒，得到生物医用金属材料，其中双螺杆挤出机的挤出条件为：一区温度180℃、二区温度200℃、三区温度210℃、四区温度230℃，螺杆转速为160rpm。
实施例2
一种生物医用金属材料，原料以重量份计包括：铌粉4份，铂粉6份，钛粉2份，钼粉3份，纤维素硝酸酯5份，磷酸三苯酯6份，抗氧剂2份，辅助抗氧剂5份，硅灰石纤维4份，二丁基硫醇锡5份，邻苯二甲酸二丁酯8份，亚磷酸三苯酯7份，玻璃酸5份，淀粉3份，硅酸钙5份，2-乙基-4-甲基咪唑3份。
上述铌粉、铂粉、钛粉和钼粉的粒度为140目。
上述抗氧剂为抗氧剂1010和抗氧剂1076的混合物，其中，抗氧剂1010和抗氧剂1076的重量比为3:2。
上述辅助抗氧剂为硫代二丙酸双月桂酯。
上述生物医用金属材料的制备方法，包括以下步骤：
步骤1，将各组分加至混合搅拌机中，搅拌混合均匀，搅拌速度为350rpm，搅拌时间为30min，得到混合物料；
步骤2，将步骤1所得混合物料加入到反应釜中，在氮气氛围中加热到75℃，搅拌反应35min，得到反应物；
步骤3，将步骤2所得反应物送入双螺杆挤出机中经挤出、水冷、风干、切粒，得到生物医用金属材料，其中双螺杆挤出机的挤出条件为：一区温度190℃、二区温度210℃、三区温度220℃、四区温度240℃，螺杆转速为170rpm。
实施例3
一种生物医用金属材料，原料以重量份计包括：铌粉7份，铂粉3份，钛粉2份，钼粉3份，纤维素硝酸酯5份，磷酸三苯酯6份，抗氧剂2份，辅助抗氧剂3份，硅灰石纤维4份，二丁基硫醇锡6份，邻苯二甲酸二丁酯8份，亚磷酸三苯酯5份，玻璃酸4份，淀粉3份，硅酸钙7份，2-乙基-4-甲基咪唑2份。
上述铌粉、铂粉、钛粉和钼粉的粒度为160目。
上述抗氧剂为抗氧剂1010和抗氧剂1076的混合物，其中，抗氧剂1010和抗氧剂1076的重量比为3:2。
上述辅助抗氧剂为硫代二丙酸双月桂酯。
上述生物医用金属材料的制备方法，包括以下步骤：
步骤1，将各组分加至混合搅拌机中，搅拌混合均匀，搅拌速度为400rpm，搅拌时间为20min，得到混合物料；
步骤2，将步骤1所得混合物料加入到反应釜中，在氮气氛围中加热到80℃，搅拌反应30min，得到反应物；
步骤3，将步骤2所得反应物送入双螺杆挤出机中经挤出、水冷、风干、切粒，得到生物医用金属材料，其中双螺杆挤出机的挤出条件为：一区温度200℃、二区温度220℃、三区温度230℃、四区温度250℃，螺杆转速为180rpm。
实施例4
一种生物医用金属材料，原料以重量份计包括：铌粉5份，铂粉3份，钛粉6份，钼粉4份，纤维素硝酸酯2份，磷酸三苯酯6份，抗氧剂4份，辅助抗氧剂7份，硅灰石纤维3份，二丁基硫醇锡5份，邻苯二甲酸二丁酯8份，亚磷酸三苯酯4份，玻璃酸3份，淀粉6份，硅酸钙7份，2-乙基-4-甲基咪唑5份。
上述铌粉、铂粉、钛粉和钼粉的粒度为120目。
上述抗氧剂为抗氧剂1010和抗氧剂1076的混合物，其中，抗氧剂1010和抗氧剂1076的重量比为3:2。
上述辅助抗氧剂为硫代二丙酸双月桂酯。
上述生物医用金属材料的制备方法，包括以下步骤：
步骤1，将各组分加至混合搅拌机中，搅拌混合均匀，搅拌速度为300rpm，搅拌时间为40min，得到混合物料；
步骤2，将步骤1所得混合物料加入到反应釜中，在氮气氛围中加热到65℃，搅拌反应40min，得到反应物；
步骤3，将步骤2所得反应物送入双螺杆挤出机中经挤出、水冷、风干、切粒，得到生物医用金属材料，其中双螺杆挤出机的挤出条件为：一区温度180℃、二区温度200℃、三区温度210℃、四区温度230℃，螺杆转速为160rpm。
实施例5
一种生物医用金属材料，原料以重量份计包括：铌粉9份，铂粉8份，钛粉7份，钼粉7份，纤维素硝酸酯6份，磷酸三苯酯8份，抗氧剂7份，辅助抗氧剂8份，硅灰石纤维5份，二丁基硫醇锡7份，邻苯二甲酸二丁酯9份，亚磷酸三苯酯8份，玻璃酸7份， 淀粉8份，硅酸钙9份，2-乙基-4-甲基咪唑6份。
上述铌粉、铂粉、钛粉和钼粉的粒度为200目。
上述抗氧剂为抗氧剂1010和抗氧剂1076的混合物，其中，抗氧剂1010和抗氧剂1076的重量比为3:2。
上述辅助抗氧剂为硫代二丙酸双月桂酯。
上述生物医用金属材料的制备方法，包括以下步骤：
步骤1，将各组分加至混合搅拌机中，搅拌混合均匀，搅拌速度为400rpm，搅拌时间为20min，得到混合物料；
步骤2，将步骤1所得混合物料加入到反应釜中，在氮气氛围中加热到80℃，搅拌反应30min，得到反应物；
步骤3，将步骤2所得反应物送入双螺杆挤出机中经挤出、水冷、风干、切粒，得到生物医用金属材料，其中双螺杆挤出机的挤出条件为：一区温度200℃、二区温度220℃、三区温度230℃、四区温度250℃，螺杆转速为180rpm。
试验例1
将实施例1至5所得材料进行耐腐性能测试：测试样品为工作电极、石墨棒为对电极、甘汞电极为参比电极，利用电化学工作站(上海辰华CHI760C)测试材料的耐腐性能，测试电压为-2V～2V。
结果显示，本发明的材料相对于纯钛而言，腐蚀电位均向正方向偏移，表明本发明的材料耐腐能力得到增强，这可能是纤维素硝酸酯的存在使其耐腐能力得到了改善。
试验例2
将实施例1至5所得材料进行纳米硬度测试：利用纳米压痕仪(美国美特斯工艺系统有限公司)，用连续硬度测试法对材料进行纳米硬度测试，三角金刚锥压头在荷载力为1mN的推动下在材料表面压入深度为70nm，电脑软件同时记录相应的数据。样品的硬度值通过测量样品五个不同区域获得。
结果显示，本发明的材料相对于纯钛而言，纳米硬度值均提高了15％以上。
试验例3
将实施例1至5所得材料进行抗菌实验：所有样品在121℃高压灭菌40min，将浓度为107CFU/mL的菌液滴在灭菌过的样品表面(0.06mL/cm2)，然后将滴有菌液的样品放入37℃恒温培养箱培养24h。取出24h培养的样品，将菌液倍比稀释后接种在含有培养基的琼脂板上。接种后的琼脂板放入37℃恒温培养箱培养24h，经过24h的培养后取出琼脂板计算活的细菌数(参照国家标准GB/T4789.2)。
结果显示，本发明的材料对大肠杆菌具有明显的抗菌能力，其抗菌率达到99.5％；对金黄色葡萄球菌也具有明显的抗菌能力，抗菌率达到98.45％。
Claims (1)
1.一种生物医用金属材料，其特征在于：原料以重量份计包括：铌粉7份，铂粉3份，钛粉2份，钼粉3份，纤维素硝酸酯5份，磷酸三苯酯6份，抗氧剂2份，辅助抗氧剂3份，硅灰石纤维4份，二丁基硫醇锡6份，邻苯二甲酸二丁酯8份，亚磷酸三苯酯5份，玻璃酸4份，淀粉3份，硅酸钙7份，2-乙基-4-甲基咪唑2份；
上述铌粉、铂粉、钛粉和钼粉的粒度为160目；
上述抗氧剂为抗氧剂1010和抗氧剂1076的混合物，其中，抗氧剂1010和抗氧剂1076的重量比为3:2；
上述辅助抗氧剂为硫代二丙酸双月桂酯；
上述生物医用金属材料的制备方法，包括以下步骤：
步骤1，将各组分加至混合搅拌机中，搅拌混合均匀，搅拌速度为400rpm，搅拌时间为20min，得到混合物料；
步骤2，将步骤1所得混合物料加入到反应釜中，在氮气氛围中加热到80℃，搅拌反应30min，得到反应物；
步骤3，将步骤2所得反应物送入双螺杆挤出机中经挤出、水冷、风干、切粒，得到生物医用金属材料，其中双螺杆挤出机的挤出条件为：一区温度200℃、二区温度220℃、三区温度230℃、四区温度250℃，螺杆转速为180rpm。
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| CN201610730219.6A Withdrawn CN106267333A (zh) | 2014-11-07 | 2014-11-07 | 一种抗菌能力和耐腐蚀性能较好的生物医用金属材料 |
| CN201610725898.8A Pending CN106267372A (zh) | 2014-11-07 | 2014-11-07 | 一种生物医用金属材料 |
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| CN101107067A (zh) * | 2005-01-24 | 2008-01-16 | 金文申有限公司 | 含金属的复合材料 |
| CN101724764A (zh) * | 2009-12-10 | 2010-06-09 | 中南大学 | 一种生物医用β-钛合金的制备工艺 |
| CN103788581A (zh) * | 2014-02-08 | 2014-05-14 | 常州华森三维打印研究院有限公司 | 3d打印人骨模型医用材料及其制备方法 |
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| CN1735562A (zh) * | 2003-01-17 | 2006-02-15 | 西巴特殊化学品控股有限公司 | 制备含纳米颗粒的多孔无机材料或基体材料的方法 |
| CN100544776C (zh) * | 2006-05-18 | 2009-09-30 | 上海交通大学 | 具有中空结构的泡沫生物钛合金人造骨骼制造方法 |
| CN101165087B (zh) * | 2006-10-17 | 2010-12-01 | 路德石油化工（北京）有限公司 | 纳米复合生物降解塑料及其制备方法 |
| EP2240213B1 (en) * | 2008-01-04 | 2019-03-13 | Smith & Nephew, Inc. | Surface alloyed medical implant |
| KR101324170B1 (ko) * | 2010-09-16 | 2013-11-05 | 한국과학기술연구원 | 표면 개질된 금속 입자 및 생분해성 고분자를 포함하는 생체 이식물, 이의 염증 억제용으로서의 용도 및 그 제조 방법 |
| CN103028146B (zh) * | 2011-09-29 | 2015-06-03 | 深圳兰度生物材料有限公司 | 增强型医用复合材料及其制备方法 |
| CN102964790A (zh) * | 2012-11-19 | 2013-03-13 | 贵州鸿顺发建材科技有限公司 | 一种人造石盆及其制作方法 |
| CN103113129A (zh) * | 2013-01-31 | 2013-05-22 | 华南理工大学 | 一种多级孔生物活性陶瓷的制备方法和应用 |
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| CN101107067A (zh) * | 2005-01-24 | 2008-01-16 | 金文申有限公司 | 含金属的复合材料 |
| CN101724764A (zh) * | 2009-12-10 | 2010-06-09 | 中南大学 | 一种生物医用β-钛合金的制备工艺 |
| CN103788581A (zh) * | 2014-02-08 | 2014-05-14 | 常州华森三维打印研究院有限公司 | 3d打印人骨模型医用材料及其制备方法 |
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| CN106267372A (zh) | 2017-01-04 |
| CN106267333A (zh) | 2017-01-04 |
| CN106237377A (zh) | 2016-12-21 |
| CN106178097A (zh) | 2016-12-07 |
| CN104436310A (zh) | 2015-03-25 |
| CN106334216A (zh) | 2017-01-18 |
| CN106337155A (zh) | 2017-01-18 |
| CN104436310B (zh) | 2016-11-16 |
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