CN105879110A - 一种天然透辉石矿物多孔生物陶瓷骨修复材料 - Google Patents
一种天然透辉石矿物多孔生物陶瓷骨修复材料 Download PDFInfo
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- NWXHSRDXUJENGJ-UHFFFAOYSA-N calcium;magnesium;dioxido(oxo)silane Chemical compound [Mg+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O NWXHSRDXUJENGJ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052637 diopside Inorganic materials 0.000 title claims abstract description 41
- 210000000988 bone and bone Anatomy 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 title claims abstract description 31
- 239000003462 bioceramic Substances 0.000 title claims abstract description 28
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 27
- 239000011707 mineral Substances 0.000 title claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000007710 freezing Methods 0.000 claims abstract description 5
- 230000008014 freezing Effects 0.000 claims abstract description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910020489 SiO3 Inorganic materials 0.000 claims abstract description 4
- 239000011575 calcium Substances 0.000 claims abstract description 4
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 4
- 239000011777 magnesium Substances 0.000 claims abstract description 4
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims abstract description 4
- 239000011148 porous material Substances 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
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- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
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- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 230000007547 defect Effects 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000001746 injection moulding Methods 0.000 claims description 2
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000498 ball milling Methods 0.000 abstract description 2
- 238000002316 cosmetic surgery Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 210000000130 stem cell Anatomy 0.000 abstract description 2
- 238000001356 surgical procedure Methods 0.000 abstract description 2
- 230000033558 biomineral tissue development Effects 0.000 abstract 1
- FGZBFIYFJUAETR-UHFFFAOYSA-N calcium;magnesium;silicate Chemical compound [Mg+2].[Ca+2].[O-][Si]([O-])([O-])[O-] FGZBFIYFJUAETR-UHFFFAOYSA-N 0.000 abstract 1
- 238000005266 casting Methods 0.000 abstract 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 230000000399 orthopedic effect Effects 0.000 abstract 1
- 230000009818 osteogenic differentiation Effects 0.000 abstract 1
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- 238000004537 pulping Methods 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
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- 108010010803 Gelatin Proteins 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019322 gelatine Nutrition 0.000 description 2
- 235000011852 gelatine desserts Nutrition 0.000 description 2
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 210000000963 osteoblast Anatomy 0.000 description 1
- 230000004072 osteoblast differentiation Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229940078499 tricalcium phosphate Drugs 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/10—Ceramics or glasses
- A61L27/105—Ceramics or glasses containing Al2O3
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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- A61L27/56—Porous materials, e.g. foams or sponges
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- A61L2430/00—Materials or treatment for tissue regeneration
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Abstract
本发明涉及一种天然透辉石矿物多孔生物陶瓷骨修复材料，属于先进陶瓷材料和生物医用材料技术领域。该生物陶瓷骨修复材料以高纯天然钙镁质硅酸盐矿物透辉石CaMg(SiO3)2为主要原料，经过球磨，过筛，制浆，海绵浸渍或者凝胶/冷冻注模，干燥和高温烧结造孔制备得到，具有高连通性孔道结构，孔径介于20μm到1000μm之间，孔隙率大于50％。透辉石具有良好的生物降解性和生物矿化能力，在生理环境中能够释放钙、硅和镁等离子，促进干细胞成骨分化。本发明优点在于，该多孔生物陶瓷不仅满足骨组织工程支架材料对孔道结构的要求，同时具有突出的力学性能和优良的骨诱导性能，制备工艺简单，原料来源广泛，生产成本低廉，可广泛应用骨科、口腔外科、整形外科等领域。
Description
技术领域
本发明涉及一种天然透辉石矿物多孔生物陶瓷骨修复材料，属于先进陶瓷材料和生物医用材料技术领域。
背景技术
多孔生物活性陶瓷骨修复材料作为自体骨和异体骨替代材料广泛应用于骨组织缺损重建。传统磷酸盐体系多孔生物陶瓷包括羟基磷灰石、磷酸三钙和二者复合材料，具有良好的生物相容性和骨传导性，但其力学性能差，骨诱导和血管诱导性能差，难以用于修复大尺寸承重骨缺损。人工合成硅酸盐体系新型生物活性陶瓷包括透辉石表现出优异的骨诱导和血管诱导性能，在生理环境中能够释放钙、硅和镁等离子，促进干细胞成骨分化，提高成骨细胞活力，进而增强骨再生。Scientific Report 6(2016)22005,Acta Biomaterialia 6(2010)2797–2807,Journal of Biomedical Materials Research Part B:Applied Biomaterials83B(2007)153–160,Acta Biomaterialia 9(2013)8004–8014,PLoS ONE 10(2015):e0143713and Ceramics International41(2015)12355–12363等论文证实了人工合成透辉石陶瓷具有优异的骨诱导和血管诱导性能，同时具有很好的力学性能，尤其适合应用于大尺寸承重骨缺损修复和重建。发明专利CN201410480213.9公开了一种人工合成透辉石复合氧化铝致密生物陶瓷。发明专利CN200710113907.9公开了一种人工合成透辉石复合羟基磷灰石致密生物陶瓷及其制备方法。
目前，尚未发现以天然透辉石矿物为原料制备多孔生物陶瓷骨修复材料的专利和论文报道。并且，人工合成透辉石生物陶瓷制备成本高，在很大程度上限制了其作为骨修复材料的广泛应用。天然透辉石矿物与人工合成透辉石主要化学成分和主晶相相同，原料来源更广泛，成本低廉，含有微量铁和钾等有益元素。本发明提出一种高纯天然硅灰石矿物多孔生物陶瓷修复材料，与现有多孔生物陶相比，具有成本低，强度高和生物学性能更好的技术优势，尤其适合修复大尺寸承重骨缺损，可广泛应用于骨科、整形外科和口腔外科等领域。
发明内容
本发明是针对传统磷酸钙基多孔生物活性陶瓷力学性能差和骨诱导性能差，人工合成透辉石硅酸盐生物陶瓷生产成本高等问题，提出一种低成本高性能的以天然透辉石矿物为主要原料制备的新型多孔生物陶瓷骨修复材料。
本发明提出的一种天然透辉石矿物多孔生物陶瓷骨修复材料，其特征在于，所述的生物陶瓷骨修复材料以高纯天然透辉石CaMg(SiO3)2为主要原料制备得到。主要物相为钙镁透辉石CaMg(SiO3)2,其化学组成(wt.％)为CaO 25.9，MgO 18.5，SiO255.6。主要原料天然透辉石的纯度大于90wt.％，化学组成(wt.％)为CaO≥20；MgO≥18；SiO2≥55；CO2≤6；Al2O3≤0.8；Fe2O3≤0.1；K2O≤0.1。该天然透辉石矿物多孔生物陶瓷骨修复材料具有高连通性孔道结构，孔径介于20μm到1000μm之间，孔隙率大于50％。该多孔生物陶瓷骨修复材料采用以下工艺制备：将天然透辉石矿物粉体干法或湿法球磨6到24小时进一步磨细；5000目筛过筛；与水混合制备料浆，外加0.2-1wt.％羧甲基纤维素或三聚磷酸钠作为减水剂，固相含量10-85wt.％，湿混6到12小时；海绵浸渍料浆至充分挂浆或者凝胶/冷冻注模；普通干燥或冷冻干燥24到48小时；1000℃到1300℃空气气氛烧结2－6小时即制备得到所述的天然透辉石矿物多孔生物陶瓷骨修复材料。
具体实施方式
下面结合实施例对本发明的技术方案做进一步说明：
实施例1
原料：
天然透辉石矿物粉体，粒径(d97)4μm，化学成分(wt.％)为CaO 25；MgO 18；SiO255；CO21.3；Al2O30.5；Fe2O30.1；K2O 0.1。
制备步骤：
将天然透辉石矿物粉体干法或者湿法球磨18小时，过5000目筛。将筛下粉体与水混合制备料浆，固相含量为65％，外加0.5wt.％羧甲基纤维素作为减水剂，湿磨8小时。将料浆外加10wt.％明胶，加热至70℃，继续搅拌，直到料浆和明胶混合均匀。将料浆－明胶混合液倒入模具中成型，将注模试样放入冰箱，－20℃冷冻24小时。将预冷冻注模试样用冷冻干燥机在0℃以下充分干燥5天。将冷冻干燥试样在1200℃空气气氛烧结2小时即制备得到所述的天然透辉石矿物多孔生物陶瓷骨修复材料。
理化性能：
所制备天然透辉石矿物多孔生物陶瓷骨支架试样气孔率为65.3％，耐压强度28.2MPa。
实施例2
天然透辉石矿物粉体，粒径(d97)8μm，化学成分(wt.％)为CaO 25；MgO 18；SiO255；CO21.3；Al2O30.5；Fe2O30.1；K2O 0.1。
制备步骤：
将天然透辉石矿物粉体干法或者湿法球磨24小时，过5000目筛。将筛下粉体与水混合制备料浆，固相含量为55％，外加0.5wt.％羧甲基纤维素作为减水剂，湿磨10小时。用海绵多次浸渍料浆至完全挂浆，将挂浆试样自然干燥24小时，60℃干燥12小时，900℃空气气氛烧结1小时，将预烧多孔试样再次浸渍料浆，干燥，1250℃空气气氛烧结2小时，即制备得到所述的天然透辉石矿物多孔生物陶瓷骨修复材料。
理化性能：
所制备天然透辉石矿物多孔生物陶瓷骨支架试样气孔率为70.8％，耐压强度23.5MPa。
Claims (5)
1.一种天然透辉石矿物多孔生物陶瓷骨修复材料，其特征在于，所述的生物陶瓷骨修复材料以高纯天然透辉石CaMg(SiO3)2为主要原料制备得到。
2.根据权利要求书1所述的天然透辉石矿物多孔生物陶瓷骨修复材料，其特征在于，主要物相为钙镁透辉石CaMg(SiO3)2,其化学组成(wt.％)为CaO 25.9，MgO 18.5，SiO2 55.6。
3.根据权利要求书1所述的天然透辉石矿物多孔生物陶瓷骨修复材料，其特征在于，主要原料天然透辉石的纯度大于90wt.％，化学组成(wt.％)为CaO≥20；MgO≥18；SiO2≥55；CO2≤6；Al2O3≤0.8；Fe2O3≤0.1；K2O≤0.1。
4.根据权利要求书1所述的天然透辉石矿物多孔生物陶瓷骨修复材料，其特征在于，具有高连通性孔道结构，孔径介于20μm到1000μm之间，孔隙率大于50％。
5.根据权利要求书1所述的一种天然透辉石矿物多孔生物陶瓷骨修复材料，采用以下工艺制备：将天然透辉石矿物粉体干法或者湿法球磨6到24小时进一步磨细；5000目筛过筛；与水混合制备料浆，外加0.2-1wt.％羧甲基纤维素或三聚磷酸钠作为减水剂，固相含量10-85wt.％，湿混6到12小时；海绵浸渍料浆至充分挂浆或者凝胶/冷冻注模；普通干燥或冷冻干燥24到48小时；1000℃到1300℃空气气氛烧结2－6小时即制备得到所述的天然透辉石矿物多孔生物陶瓷骨修复材料。
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