CN113813447B - 一种具有抗菌性能的硅钙磷基生物活性材料及其制备方法 - Google Patents
一种具有抗菌性能的硅钙磷基生物活性材料及其制备方法 Download PDFInfo
- Publication number
- CN113813447B CN113813447B CN202111324112.9A CN202111324112A CN113813447B CN 113813447 B CN113813447 B CN 113813447B CN 202111324112 A CN202111324112 A CN 202111324112A CN 113813447 B CN113813447 B CN 113813447B
- Authority
- CN
- China
- Prior art keywords
- calcium
- phosphorus
- source
- silicon
- bioactive material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000463 material Substances 0.000 title claims abstract description 57
- 230000000975 bioactive effect Effects 0.000 title claims abstract description 49
- BXYHXVIURNMBJM-UHFFFAOYSA-N [P].[Si].[Ca] Chemical compound [P].[Si].[Ca] BXYHXVIURNMBJM-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 12
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011574 phosphorus Substances 0.000 claims abstract description 10
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 10
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 10
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011701 zinc Substances 0.000 claims abstract description 10
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 9
- 239000011575 calcium Substances 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 12
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 8
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical group CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- KQAGKTURZUKUCH-UHFFFAOYSA-L strontium oxalate Chemical compound [Sr+2].[O-]C(=O)C([O-])=O KQAGKTURZUKUCH-UHFFFAOYSA-L 0.000 claims description 4
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- ZQBZAOZWBKABNC-UHFFFAOYSA-N [P].[Ca] Chemical compound [P].[Ca] ZQBZAOZWBKABNC-UHFFFAOYSA-N 0.000 claims 1
- 239000000378 calcium silicate Substances 0.000 claims 1
- 229910052918 calcium silicate Inorganic materials 0.000 claims 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 4
- 230000003013 cytotoxicity Effects 0.000 abstract description 3
- 231100000135 cytotoxicity Toxicity 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 150000004703 alkoxides Chemical class 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 210000001519 tissue Anatomy 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 208000015181 infectious disease Diseases 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001356 surgical procedure Methods 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 241000699670 Mus sp. Species 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000005313 bioactive glass Substances 0.000 description 1
- 239000005312 bioglass Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000030833 cell death Effects 0.000 description 1
- 230000024245 cell differentiation Effects 0.000 description 1
- 230000004663 cell proliferation Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 210000002901 mesenchymal stem cell Anatomy 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000003170 nutritional factors Nutrition 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Images
Classifications
-
- 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
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
-
- 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
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/446—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with other specific inorganic fillers other than those covered by A61L27/443 or A61L27/46
-
- 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
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/46—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with phosphorus-containing inorganic fillers
-
- 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
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/22—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in calcium oxide, e.g. wollastonite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/447—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on phosphates, e.g. hydroxyapatite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/112—Phosphorus-containing compounds, e.g. phosphates, phosphonates
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
-
- 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
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
-
- 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
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Ceramic Engineering (AREA)
- Medicinal Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Dermatology (AREA)
- Manufacturing & Machinery (AREA)
- Transplantation (AREA)
- Epidemiology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Composite Materials (AREA)
- Dispersion Chemistry (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Catalysts (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Silicon Compounds (AREA)
Abstract
本发明公开了一种具有抗菌性能的硅钙磷基生物活性材料及其制备方法，该生物活性材料由前驱体凝胶经洗涤干燥后高温烧结而成；其中，前驱体凝胶由前驱体溶胶制备得到，前驱体溶胶由硅源、钙源、磷源、锶源、锌源、模板剂、催化剂、乙醇和去离子水制备得到。本发明制备的硅钙磷基生物活性材料的化学成分均匀，具有大的比表面积。本发明公开的硅钙磷基生物活性材料制备过程中通过参数的调控使得材料的粒径尺寸从几十纳米到几十微米；本发明制备的硅钙磷基生物活性材料既具有良好的抗菌效果又细胞毒性低。
Description
技术领域
本发明涉及生物活性材料技术领域，具体涉及一种具有抗菌性能的硅钙磷基生物活性材料及其制备方法。
背景技术
生物活性材料属于第三代组织诱导类生物材料，同样用于人体组织或器官的诊断、修复。目前，生物活性玻璃在生物医学领域有着广泛的应用，尤其是骨齿科方面。
然而因骨外科手术、齿科手术中往往存在感染问题，许多治疗手段都是为了防止进一步感染，但是也会带来某些组织功能的丧失，给患者带来二次伤害。因此同时具有高抗菌能力又能促进细胞增殖分化功能的新型硅钙磷体系材料可以弥补传统生物玻璃抗菌能力的不足。
发明内容
本发明的第一个目的是为了解决现有技术中的上述缺陷，提供一种具有抗菌性能的硅钙磷基生物活性材料，该生物活性材料的抗菌性能好且细胞毒性低。
本发明的另一个目的是为了解决现有技术中的上述缺陷，提供一种具有抗菌性能的硅钙磷基生物活性材料的制备方法
本发明的第一个目的可以通过采取如下技术方案达到：
一种具有抗菌性能的硅钙磷基生物活性材料，所述生物活性材料由前驱体凝胶经洗涤干燥后高温烧结而成；
所述前驱体凝胶由前驱体溶胶制备得到，所述前驱体溶胶由硅源、钙源、磷源、锶源、锌源、模板剂、催化剂、乙醇和去离子水制备得到。
进一步优选的实施方式中，所述硅源为正硅酸乙酯，属于一种醇盐，与磷酸三乙酯构成醇盐体系，与其他原料形成醇盐-醇-水体系，进行水解和缩聚反应；
所述钙源为草酸钙、硝酸钙中的一种或两种的组合，可为硅钙磷基生物活性材料的合成提供不同程度的酸性环境，为钙元素的释放与细胞相互作用提供基础；
所述磷源为磷酸三乙酯，属于一种醇盐，与正硅酸乙酯构成醇盐体系与其他原料形成醇盐-醇-水体系，进行水解和缩聚反应；
所述锶源为硝酸锶、乙酸锶、草酸锶中的一种或两种以上的组合，锶元素的引入可调控细胞行为；
所述锌源为乙酸锌、硝酸锌中的一种或两种的组合，锌元素的引入可有利于实现高抗菌效果；
所述催化剂为硝酸、盐酸、乙酸、醋酸、柠檬酸中的一种或两种以上的组合，含有催化剂的去离子水可催化正硅酸乙酯的充分水解；
所述模板剂为聚乙二醇、聚乙烯吡咯烷酮中的一种或两种的组合，作为硅钙磷基生物活性材料成球形的模板剂。
本发明的另一个目的可以通过采取如下技术方案达到：
一种具有抗菌性能的硅钙磷基生物活性材料的制备方法，所述制备方法包括以下步骤：
S1、用去离子水溶解催化剂，配成溶液待用，催化剂和去离子水的质量比为(0.5～2)：(50～250)；
S2、将硅源、磷源、乙醇按照体积比为(6～12)：(1～3)：(20～30)量取并将其混合搅拌10～60min；
S3、将步骤S2中制备的混合溶液缓慢倒入步骤S1中制备的溶液中，搅拌1～2h；
S4、按照钙源、锶源、锌源与催化剂质量比为(25～50)：(0.2～2.5)：(0.2～2.5)：1称量加入步骤S3中制备的混合液中，搅拌2h；
S5、按照模板剂与催化剂质量比为(1.5～20)：1称量模板剂加入步骤S4中制备的混合溶液中，搅拌2～4h；
S6、将步骤S5中制备的混合溶液置于25℃～75℃温度下静置陈化24h～96h得到凝胶；
S7、将步骤S6中的凝胶用去离子水和无水乙醇交替清洗凝胶后，将凝胶置于烘箱中干燥；
S8、将步骤S7中干燥的凝胶打散，并进行研磨过筛收集粉体；
S9、将步骤S8中粉体置于高温烧结炉中在600～900℃的煅烧温度下煅烧1～4h，得到硅钙磷基生物活性材料。
进一步优选的实施方式中，所述硅源为正硅酸乙酯。
进一步优选的实施方式中，所述钙源为草酸钙、硝酸钙中的一种或两种的组合。
进一步优选的实施方式中，所述磷源为磷酸三乙酯。
进一步优选的实施方式中，所述锶源为硝酸锶、乙酸锶、草酸锶中的一种或两种以上的组合。
进一步优选的实施方式中，所述锌源为乙酸锌、硝酸锌中的一种或两种的组合。
进一步优选的实施方式中，所述催化剂为硝酸、盐酸、乙酸、醋酸、柠檬酸中的一种或两种以上的组合。
进一步优选的实施方式中，所述模板剂为聚乙二醇、聚乙烯吡咯烷酮中的一种或两种的组合。
本发明相对于现有技术具有如下的优点及效果：
1、本发明制备得到的硅钙磷基生物活性材料的化学成分均匀；
2、本发明制备得到的硅钙磷基生物活性材料具有大的比表面积；
3、本发明制备得到的硅钙磷基生物活性材料制备过程中通过参数的调控使得材料的粒径尺寸可从几十纳米到几十微米；
4、本发明制备得到的硅钙磷基生物活性材料既具有良好的抗菌效果又细胞毒性低。
附图说明
图1是本发明实施例一中制备的纳米基硅钙磷基生物活性材料的形貌图；
图2是本发明实施例二中制备的微米级硅钙磷基生物活性材料的形貌图；
图3是本发明实施例二中制备的微米级硅钙磷基生物活性材料的抗菌效果图；
图4是本发明实施例2制备的微米级硅钙磷基生物活性材料的细胞死活图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例一
本实施例提供一种具有抗菌性能的硅钙磷基生物活性材料的制备方法，包括以下步骤：
S1、量取5mL催化剂硝酸溶液，加入到1000mL去离子水中，搅拌混匀待用；
S2、分别量取正硅酸乙酯100mL、磷酸三乙酯20mL和乙醇300mL，将其搅拌30min混匀待用；
S3、将步骤S2中制备的混合溶液缓慢倒入步骤S1中制备的溶液中，搅拌2h；
S4、分别称取草酸钙150g、硝酸锶5g和硝酸锌5g加入步骤S3中制备的混合液，搅拌2h；
S5、称量25g模板剂加入步骤S4中制备的混合溶液，搅拌2h；
S6、将步骤S5中制备的混合溶液置于50℃温度下静置陈化48h得到凝胶；
S7、将步骤S6中制备的凝胶用去离子水和无水乙醇交替分别清洗2次后，将凝胶置于烘箱中干燥；
S8、将步骤S7中干燥的凝胶打散，并进行研磨过筛收集粉体；
S9、将步骤S8中粉体置于高温烧结炉中在750℃的煅烧温度下煅烧2h，得到硅钙磷基生物活性材料。
实施例二
本实施例提供一种具有抗菌性能的硅钙磷基生物活性材料的制备方法，包括以下步骤：
S1、量取6g催化剂乙酸溶液，加入到1000mL去离子水中，搅拌混匀待用；
S2、分别量取正硅酸乙酯100mL、磷酸三乙酯20mL和乙醇500mL，将其搅拌30min混匀待用；
S3、将步骤S2中制备的混合溶液缓慢倒入步骤S1中制备的溶液中，搅拌2h；
S4、分别称取草酸钙180g、硝酸锶8g和硝酸锌8g加入步骤S3中制备的混合液，搅拌2h；
S5、称量15g模板剂加入步骤S4中制备的混合溶液，搅拌2h；
S6、将步骤S5中制备的混合溶液置于50℃温度下静置陈化72h得到凝胶；
S7、将步骤S6中制备的凝胶用去离子水和无水乙醇交替分别清洗2次后，将凝胶置于烘箱中干燥；
S8、将步骤S7中干燥的凝胶打散，并进行研磨过筛收集粉体；
S9、将步骤S8中粉体置于高温烧结炉中在850℃的煅烧温度下煅烧2h，得到硅钙磷基生物活性材料。
下面进一步结合附图对实施例一和实施例二制备的生物活性材料进行性能测试，其中，
图1是实施例一中制备的纳米级硅钙磷基生物活性材料的形貌图，从图中可以看出，粉体材料的形貌呈现纳米絮状，尺寸均一，处于纳米级；
图2是实施例二中制备的纳米级硅钙磷基生物活性材料的形貌图，从图中可以看出，提高调控参数，可调控粉体材料的形貌，呈现球形颗粒，尺寸处于8-12μm范围；
图3是实施例二中制备的微米级硅钙磷基生物活性材料的抗菌效果图，从图中可以看出，与空白组对比，实验组的抗菌率可达到97.5％，具有良好的抗菌效果；
图4是实施例二中制备的微米级硅钙磷基生物活性材料的细胞死活荧光图，从图中可以看出，与空白组对比，实验组的材料本身对小鼠骨髓间充质干细胞的毒性较低，故该类材料在具有良好抗菌性能的同时，也能保持良好的细胞相容性。
表1.实施例二中制备的微米级硅钙磷基生物活性材料的吸附脱附的孔径、孔体积、比表面积数据表
从表1中可以看出，该类制备得到的微米级硅钙磷基生物活性材料具有较大的比表面积，且表面有很多介孔，可为应用于药物及其他一些营养因子的输送有很好载体作用。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (9)
1.一种具有抗菌性能的硅钙磷基生物活性材料，其特征在于，所述生物活性材料由前驱体凝胶经洗涤干燥后高温烧结而成；
所述前驱体凝胶由前驱体溶胶制备得到，所述前驱体溶胶由硅源、钙源、磷源、锶源、锌源、模板剂、催化剂、乙醇和去离子水制备得到；
其中，所述硅源为正硅酸乙酯；
所述钙源为草酸钙、硝酸钙中的一种或两种的组合；
所述磷源为磷酸三乙酯；
所述锶源为硝酸锶、乙酸锶、草酸锶中的一种或两种以上的组合；
所述锌源为乙酸锌、硝酸锌中的一种或两种的组合；
所述的具有抗菌性能的硅钙磷基生物活性材料的制备方法包括以下步骤：
S1、用去离子水溶解催化剂，配成溶液待用，催化剂和去离子水的质量比为(0.5～2)：(50～250)；
S2、将硅源、磷源、乙醇按照体积比为(6～12)：(1～3)：(20～30)量取并将其混合搅拌10～60min；
S3、将步骤S2中制备的混合溶液缓慢倒入步骤S1中制备的溶液中，搅拌1～2h；
S4、按照钙源、锶源、锌源与催化剂质量比为(25～50)：(0.2～2.5)：
(0.2～2.5)：1称量加入步骤S3中制备的混合液中，搅拌2h；
S5、按照模板剂与催化剂质量比为(1.5～20)：1称量模板剂加入步骤S4中制备的混合溶液中，搅拌2～4h；
S6、将步骤S5中制备的混合溶液置于25℃～75℃温度下静置陈化24h～96h得到凝胶；
S7、将步骤S6中的凝胶用去离子水和无水乙醇交替清洗凝胶后，将凝胶置于烘箱中干燥；
S8、将步骤S7中干燥的凝胶打散，并进行研磨过筛收集粉体；
S9、将步骤S8中粉体置于高温烧结炉中在600～900℃的煅烧温度下煅烧1～4h，得到硅钙磷基生物活性材料。
2.根据权利要求1所述的一种具有抗菌性能的硅钙磷基生物活性材料，其特征在于，
所述催化剂为硝酸、盐酸、乙酸、醋酸、柠檬酸中的一种或两种以上的组合；
所述模板剂为聚乙二醇、聚乙烯吡咯烷酮中的一种或两种的组合。
3.根据权利要求1所述的一种具有抗菌性能的硅钙磷基生物活性材料，其特征在于，所述硅源为正硅酸乙酯。
4.根据权利要求1所述的一种具有抗菌性能的硅钙磷基生物活性材料，其特征在于，所述钙源为草酸钙、硝酸钙中的一种或两种的组合。
5.根据权利要求1所述的一种具有抗菌性能的硅钙磷基生物活性材料，其特征在于，所述磷源为磷酸三乙酯。
6.根据权利要求1所述的一种具有抗菌性能的硅钙磷基生物活性材料，其特征在于，所述锶源为硝酸锶、乙酸锶、草酸锶中的一种或两种以上的组合。
7.根据权利要求1所述的一种具有抗菌性能的硅钙磷基生物活性材料，其特征在于，所述锌源为乙酸锌、硝酸锌中的一种或两种的组合。
8.根据权利要求1所述的一种具有抗菌性能的硅钙磷基生物活性材料，其特征在于，所述催化剂为硝酸、盐酸、乙酸、醋酸、柠檬酸中的一种或两种以上的组合。
9.根据权利要求1所述的一种具有抗菌性能的硅钙磷基生物活性材料，其特征在于，所述模板剂为聚乙二醇、聚乙烯吡咯烷酮中的一种或两种的组合。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111324112.9A CN113813447B (zh) | 2021-11-10 | 2021-11-10 | 一种具有抗菌性能的硅钙磷基生物活性材料及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111324112.9A CN113813447B (zh) | 2021-11-10 | 2021-11-10 | 一种具有抗菌性能的硅钙磷基生物活性材料及其制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113813447A CN113813447A (zh) | 2021-12-21 |
| CN113813447B true CN113813447B (zh) | 2023-05-02 |
Family
ID=78919458
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111324112.9A Active CN113813447B (zh) | 2021-11-10 | 2021-11-10 | 一种具有抗菌性能的硅钙磷基生物活性材料及其制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113813447B (zh) |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314039B (zh) * | 2008-07-03 | 2011-05-18 | 华南理工大学 | 一种生物活性玻璃介孔微球及其制备方法 |
| CN102923946B (zh) * | 2012-11-30 | 2015-08-12 | 浙江理工大学 | 具有磷灰石纳米晶的介孔生物活性玻璃材料及其制备方法 |
| ES2899774T3 (es) * | 2013-03-14 | 2022-03-14 | Prosidyan Inc | Implantes de injerto óseo de compuesto poroso bioactivo |
| CN104288830B (zh) * | 2014-09-12 | 2017-10-20 | 华南理工大学 | 一种微纳米棒状生物活性玻璃及其制备方法与应用 |
| CN109336371A (zh) * | 2018-09-03 | 2019-02-15 | 中国科学院深圳先进技术研究院 | 微纳米硼硅酸盐生物活性玻璃的制备方法 |
| CN111888519A (zh) * | 2020-08-13 | 2020-11-06 | 江西理工大学 | 一种含锶介孔生物玻璃-镁复合材料及其制备方法和应用 |
| CN113461019A (zh) * | 2021-06-15 | 2021-10-01 | 华南理工大学 | 一种元素掺杂硅基微纳米球颗粒的制备方法 |
-
2021
- 2021-11-10 CN CN202111324112.9A patent/CN113813447B/zh active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN113813447A (zh) | 2021-12-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Izquierdo-Barba et al. | High-performance mesoporous bioceramics mimicking bone mineralization | |
| Zheng et al. | Toward highly dispersed mesoporous bioactive glass nanoparticles with high Cu concentration using Cu/ascorbic acid complex as precursor | |
| Arcos et al. | Ordered mesoporous microspheres for bone grafting and drug delivery | |
| WO2018072679A1 (zh) | 一种仿生生物矿化人工骨修复材料及其制备方法与应用 | |
| CN101314039B (zh) | 一种生物活性玻璃介孔微球及其制备方法 | |
| CN107522389B (zh) | 一种具有表面纳米孔隙结构的微纳米生物活性玻璃微球及其制备方法 | |
| Padilla et al. | High specific surface area in nanometric carbonated hydroxyapatite | |
| CN1785862A (zh) | 一种钙硅基有序介孔生物活性玻璃及其制备方法和应用 | |
| CN108083618A (zh) | 一种利用微乳液技术制备的微纳米生物活性玻璃微球及其制备方法 | |
| CN101401965B (zh) | 一种复合骨修复生物活性材料的合成方法 | |
| CN101401950A (zh) | 含二氧化硅的纳米磷酸钙生物活性陶瓷材料及其制备方法 | |
| CN101401964A (zh) | 一种有机无机复合的骨修复生物活性材料 | |
| CN111908798A (zh) | 一种掺杂Sr/Mg/Zn/Cu的硅基溶胶-凝胶生物活性玻璃粉体及其制备方法与应用 | |
| CN111905151A (zh) | 一种介孔生物活性玻璃/聚乳酸-羟基乙酸共聚物复合微球及其制备方法与应用 | |
| CN102936141A (zh) | 一种含银抗菌生物陶瓷,制备方法及其应用 | |
| CN101921061B (zh) | 磷硅酸基玻璃的制备方法 | |
| CN104192817A (zh) | 利用模板法制备高比表面积介孔羟基磷灰石纳米粒子的方法 | |
| CN110420357A (zh) | 适用于3d打印的载药改性介孔羟基磷灰石生物医用复合材料、制备方法及其应用 | |
| CN112079572B (zh) | 一种锶掺杂中空介孔生物活性玻璃微球的制备方法及其制得的产品 | |
| CN101401966A (zh) | 一种复合骨修复生物活性材料的制备方法 | |
| KR20090044858A (ko) | 생체의료용 실리카 제로겔 키토산 유무기 하이브리드복합체 및 그 제조방법 | |
| CN103848574A (zh) | 一种含锶生物玻璃粉体制备、及含锶多孔生物玻璃支架的制备方法 | |
| CN101293112A (zh) | 一种生物活性玻璃纳米纤维簇的制备方法 | |
| El-Naggar et al. | Facile modification of polycaprolactone nanofibers with hydroxyapatite doped with thallium ions for wound and mucosal healing applications | |
| CN113813447B (zh) | 一种具有抗菌性能的硅钙磷基生物活性材料及其制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240511 Address after: Room 1103, No. 7, Zhongxin Wisdom 1st Street, Huangpu District, Guangzhou, Guangdong 510700 Patentee after: Guangzhou Baimai Technology Co.,Ltd. Country or region after: China Address before: Room 1018, No.2, Tengfei 1st Street, Tengfei Science Park, Guangzhou, Guangdong 510000 Patentee before: SINO-SINGAPORE INTERNATIONAL JOINT Research Institute Country or region before: China |