CN104436310B - A kind of biomedical metallic material and preparation method thereof - Google Patents
A kind of biomedical metallic material and preparation method thereof Download PDFInfo
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- CN104436310B CN104436310B CN201410623911.XA CN201410623911A CN104436310B CN 104436310 B CN104436310 B CN 104436310B CN 201410623911 A CN201410623911 A CN 201410623911A CN 104436310 B CN104436310 B CN 104436310B
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- 239000007769 metal material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 30
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 28
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 28
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 18
- 239000010936 titanium Substances 0.000 claims abstract description 18
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 16
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 15
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 15
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000376 reactant Substances 0.000 claims abstract description 15
- 239000000020 Nitrocellulose Substances 0.000 claims abstract description 9
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 claims abstract description 9
- 229920001220 nitrocellulos Polymers 0.000 claims abstract description 9
- 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
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920002472 Starch Polymers 0.000 claims abstract description 8
- 235000012241 calcium silicate Nutrition 0.000 claims abstract description 8
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000835 fiber Substances 0.000 claims abstract description 8
- 229920002674 hyaluronan Polymers 0.000 claims abstract description 8
- 229960003160 hyaluronic acid Drugs 0.000 claims abstract description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 8
- 238000005453 pelletization Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000008107 starch Substances 0.000 claims abstract description 8
- 235000019698 starch Nutrition 0.000 claims abstract description 8
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000010456 wollastonite Substances 0.000 claims abstract description 8
- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 8
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 14
- 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
- 239000000203 mixture Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 7
- 238000001125 extrusion Methods 0.000 claims description 7
- 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
- 238000003756 stirring Methods 0.000 claims description 7
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical group CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 9
- 238000005260 corrosion Methods 0.000 abstract description 9
- 230000003115 biocidal effect Effects 0.000 abstract description 6
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 5
- 241000588724 Escherichia coli Species 0.000 abstract description 3
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 9
- 229920001817 Agar Polymers 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 3
- 239000008272 agar Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000003462 bioceramic Substances 0.000 description 2
- 239000003519 biomedical and dental material Substances 0.000 description 2
- 239000012567 medical material Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 206010060872 Transplant failure Diseases 0.000 description 1
- 208000030961 allergic reaction Diseases 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000000680 avirulence Effects 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000002308 calcification Effects 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 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
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 230000008076 immune mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
-
- 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
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
-
- 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
- A61L27/04—Metals or alloys
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
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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
- A61L27/14—Macromolecular materials
- A61L27/20—Polysaccharides
-
- 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
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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
- A61L27/50—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
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- A—HUMAN NECESSITIES
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- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/02—Inorganic materials
- A61L31/022—Metals or alloys
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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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/02—Inorganic materials
- A61L31/028—Other inorganic materials not covered by A61L31/022 - A61L31/026
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/04—Macromolecular materials
- A61L31/042—Polysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A—HUMAN NECESSITIES
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- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L31/16—Biologically active materials, e.g. therapeutic substances
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
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- A—HUMAN NECESSITIES
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- 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
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- A—HUMAN NECESSITIES
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- 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
Abstract
The invention provides a kind of biomedical metallic material and preparation method thereof, described metal material raw material includes niobium powder, platinum powder, titanium valve, molybdenum powder, cellulose nitrate, triphenyl phosphate, antioxidant, auxiliary antioxidant, wollastonite fibre, dibutyl tin mercaptides, dibutyl phthalate, triphenyl phosphite, Hyaluronic Acid, starch, calcium silicates and 2 ethyl 4 Methylimidazole .s.Its preparation method is for first to add in mixing and blending machine by each component, it is uniformly mixed, gained mixed material is joined in reactor, heated and stirred reaction in nitrogen atmosphere, by extruded in gained reactant feeding double screw extruder, water-cooled, air-dried, pelletizing, obtain biomedical metallic material.Gained biomedical metallic material not only hardness of the present invention and corrosion resistant performance have raising in various degree, and escherichia coli and staphylococcus aureus are respectively provided with good antibacterial ability, and its antibiotic rate respectively reaches 99.5% and 98.45%.
Description
Technical field
The invention belongs to biology medical material technical field, be specifically related to a kind of biomedical metallic material and preparation method thereof.
Background technology
Bio-medical material refers to, for medically implanting organism or the material combined with biological tissue, can be used for diagnosing, treating, and replaces tissue, the organ in living organism or promote its function.The bio-medical material being currently used for clinic mainly includes biomedical metallic material, bio-medical organic material (referring mainly to high-molecular organic material), bio-medical Inorganic Non-metallic Materials (referring mainly to bioceramic), bio-vitric and carbon materials and bio-medical composition etc..Compared with bioceramic and bioabsorbable polymer material, biomedical metallic material, as rustless steel, cobalt-base alloys, titanium and titanium alloy and noble metal etc. have many irreplaceable premium properties of other medical materials such as high intensity, good toughness and counter-bending fatigue strength, excellent processing characteristics.
The subject matter that biomedical metallic material faces in the application, is that the metal ion caused due to the corrosion of physiological environment spreads and the regression of embedded material self property to surrounding tissue, and the former may cause toxic and side effects, and the latter may cause graft failure.Medical metal material is as a class of biomaterial, its research and development strictly to meet as follows from biological requirement: good histocompatibility, including avirulence, without heat source response, not teratogenesis, the most carcinogenic, do not cause allergic reaction or the immune mechanism of interference body, do not destroy adjacent tissue, the most the calcification on generating material surface is calm etc.；Good physics, chemical stability, including intensity, elasticity, dimensional stability, corrosion resistance, wearability and interface stability etc.；Easily processed into type, material is easily fabricated；Price is suitable.
Therefore, research and development performance is more excellent, and biocompatibility more preferable new bio medical metal material is material supplier author and the problem of medical personnel's common concern.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art to provide a kind of biomedical metallic material and preparation method thereof, this material has good antibiotic property, mechanical property and decay resistance.
A kind of biomedical metallic material, raw material includes in parts by weight: niobium powder 3～9 parts, platinum powder 2～8 parts, titanium valve 1～7 parts, molybdenum powder 2～7 parts, cellulose nitrate 1～6 parts, triphenyl phosphate 3～8 parts, antioxidant 1～7 parts, auxiliary antioxidant 2～8 parts, wollastonite fibre 1～5 parts, dibutyl tin mercaptides 2～7 parts, dibutyl phthalate 3～9 parts, triphenyl phosphite 3～8 parts, Hyaluronic Acid 2～7 parts, starch 1～8 parts, calcium silicates 2～9 parts, 2-ethyl-4-methylimidazole 1～6 parts.
As the further improvement of foregoing invention, the granularity of described niobium powder, platinum powder, titanium valve and molybdenum powder is 100～200 mesh.
As the further improvement of foregoing invention, described antioxidant is the mixture of antioxidant 1010 and antioxidant 1076, and wherein, the weight ratio of antioxidant 1010 and antioxidant 1076 is 3:2.
As the further improvement of foregoing invention, described auxiliary antioxidant is the double lauryl of thio-2 acid.
The preparation method of above-mentioned biomedical metallic material, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 65～80 DEG C in nitrogen atmosphere, stirring reaction 30～40min, obtains reactant；
Step 3, by extruded in step 2 gained reactant feeding double screw extruder, water-cooled, air-dried, pelletizing, obtains biomedical metallic material.
As the further improvement of foregoing invention, the mixing speed being uniformly mixed in step 1 is 300～400rpm, and mixing time is 20～40min.
As the further improvement of foregoing invention, in step 3, the extrusion condition of double screw extruder is: district's temperature 180～200 DEG C, two district's temperature 200～220 DEG C, three district's temperature 210～230 DEG C, four district's temperature 230～250 DEG C, screw speed is 160～180rpm.
The biomedical metallic material of the present invention not only hardness and corrosion resistant performance have raising in various degree, and escherichia coli and staphylococcus aureus are respectively provided with good antibacterial ability, its antibiotic rate respectively reaches 99.5% and 98.45%, can meet the requirement of the antibiotic property needed for biomedical metallic material, mechanical property and decay resistance.
Detailed description of the invention
Embodiment 1
A kind of biomedical metallic material, raw material includes in parts by weight: 3 parts of niobium powder, platinum powder 2 parts, titanium valve 1 part, molybdenum powder 2 parts, cellulose nitrate 1 part, triphenyl phosphate 3 parts, 1 part of antioxidant, auxiliary antioxidant 2 parts, wollastonite fibre 1 part, dibutyl tin mercaptides 2 parts, dibutyl phthalate 3 parts, triphenyl phosphite 3 parts, Hyaluronic Acid 2 parts, starch 1 part, calcium silicates 2 parts, 2-ethyl-4-methylimidazole 1 part.
The granularity of above-mentioned niobium powder, platinum powder, titanium valve and molybdenum powder is 100 mesh.
Above-mentioned antioxidant is the mixture of antioxidant 1010 and antioxidant 1076, and wherein, the weight ratio of antioxidant 1010 and antioxidant 1076 is 3:2.
Above-mentioned auxiliary antioxidant is the double lauryl of thio-2 acid.
The preparation method of above-mentioned biomedical metallic material, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, and mixing speed is 300rpm, and mixing time is 40min, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 65 DEG C in nitrogen atmosphere, stirring reaction 40min, obtains reactant；
Step 3, by extruded in step 2 gained reactant feeding double screw extruder, water-cooled, air-dried, pelletizing, obtain biomedical metallic material, wherein the extrusion condition of double screw extruder is: district's temperature 180 DEG C, two district's temperature 200 DEG C, three district's temperature 210 DEG C, four district's temperature 230 DEG C, and screw speed is 160rpm.
Embodiment 2
A kind of biomedical metallic material, raw material includes in parts by weight: 4 parts of niobium powder, platinum powder 6 parts, titanium valve 2 parts, molybdenum powder 3 parts, cellulose nitrate 5 parts, triphenyl phosphate 6 parts, 2 parts of antioxidant, auxiliary antioxidant 5 parts, wollastonite fibre 4 parts, dibutyl tin mercaptides 5 parts, dibutyl phthalate 8 parts, triphenyl phosphite 7 parts, Hyaluronic Acid 5 parts, starch 3 parts, calcium silicates 5 parts, 2-ethyl-4-methylimidazole 3 parts.
The granularity of above-mentioned niobium powder, platinum powder, titanium valve and molybdenum powder is 140 mesh.
Above-mentioned antioxidant is the mixture of antioxidant 1010 and antioxidant 1076, and wherein, the weight ratio of antioxidant 1010 and antioxidant 1076 is 3:2.
Above-mentioned auxiliary antioxidant is the double lauryl of thio-2 acid.
The preparation method of above-mentioned biomedical metallic material, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, and mixing speed is 350rpm, and mixing time is 30min, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 75 DEG C in nitrogen atmosphere, stirring reaction 35min, obtains reactant；
Step 3, by extruded in step 2 gained reactant feeding double screw extruder, water-cooled, air-dried, pelletizing, obtain biomedical metallic material, wherein the extrusion condition of double screw extruder is: district's temperature 190 DEG C, two district's temperature 210 DEG C, three district's temperature 220 DEG C, four district's temperature 240 DEG C, and screw speed is 170rpm.
Embodiment 3
A kind of biomedical metallic material, raw material includes in parts by weight: 7 parts of niobium powder, platinum powder 3 parts, titanium valve 2 parts, molybdenum powder 3 parts, cellulose nitrate 5 parts, triphenyl phosphate 6 parts, 2 parts of antioxidant, auxiliary antioxidant 3 parts, wollastonite fibre 4 parts, dibutyl tin mercaptides 6 parts, dibutyl phthalate 8 parts, triphenyl phosphite 5 parts, Hyaluronic Acid 4 parts, starch 3 parts, calcium silicates 7 parts, 2-ethyl-4-methylimidazole 2 parts.
The granularity of above-mentioned niobium powder, platinum powder, titanium valve and molybdenum powder is 160 mesh.
Above-mentioned antioxidant is the mixture of antioxidant 1010 and antioxidant 1076, and wherein, the weight ratio of antioxidant 1010 and antioxidant 1076 is 3:2.
Above-mentioned auxiliary antioxidant is the double lauryl of thio-2 acid.
The preparation method of above-mentioned biomedical metallic material, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, and mixing speed is 400rpm, and mixing time is 20min, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 80 DEG C in nitrogen atmosphere, stirring reaction 30min, obtains reactant；
Step 3, by extruded in step 2 gained reactant feeding double screw extruder, water-cooled, air-dried, pelletizing, obtain biomedical metallic material, wherein the extrusion condition of double screw extruder is: district's temperature 200 DEG C, two district's temperature 220 DEG C, three district's temperature 230 DEG C, four district's temperature 250 DEG C, and screw speed is 180rpm.
Embodiment 4
A kind of biomedical metallic material, raw material includes in parts by weight: 5 parts of niobium powder, platinum powder 3 parts, titanium valve 6 parts, molybdenum powder 4 parts, cellulose nitrate 2 parts, triphenyl phosphate 6 parts, 4 parts of antioxidant, auxiliary antioxidant 7 parts, wollastonite fibre 3 parts, dibutyl tin mercaptides 5 parts, dibutyl phthalate 8 parts, triphenyl phosphite 4 parts, Hyaluronic Acid 3 parts, starch 6 parts, calcium silicates 7 parts, 2-ethyl-4-methylimidazole 5 parts.
The granularity of above-mentioned niobium powder, platinum powder, titanium valve and molybdenum powder is 120 mesh.
Above-mentioned antioxidant is the mixture of antioxidant 1010 and antioxidant 1076, and wherein, the weight ratio of antioxidant 1010 and antioxidant 1076 is 3:2.
Above-mentioned auxiliary antioxidant is the double lauryl of thio-2 acid.
The preparation method of above-mentioned biomedical metallic material, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, and mixing speed is 300rpm, and mixing time is 40min, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 65 DEG C in nitrogen atmosphere, stirring reaction 40min, obtains reactant；
Step 3, by extruded in step 2 gained reactant feeding double screw extruder, water-cooled, air-dried, pelletizing, obtain biomedical metallic material, wherein the extrusion condition of double screw extruder is: district's temperature 180 DEG C, two district's temperature 200 DEG C, three district's temperature 210 DEG C, four district's temperature 230 DEG C, and screw speed is 160rpm.
Embodiment 5
A kind of biomedical metallic material, raw material includes in parts by weight: 9 parts of niobium powder, platinum powder 8 parts, titanium valve 7 parts, molybdenum powder 7 parts, cellulose nitrate 6 parts, triphenyl phosphate 8 parts, 7 parts of antioxidant, auxiliary antioxidant 8 parts, wollastonite fibre 5 parts, dibutyl tin mercaptides 7 parts, dibutyl phthalate 9 parts, triphenyl phosphite 8 parts, Hyaluronic Acid 7 parts, starch 8 parts, calcium silicates 9 parts, 2-ethyl-4-methylimidazole 6 parts.
The granularity of above-mentioned niobium powder, platinum powder, titanium valve and molybdenum powder is 200 mesh.
Above-mentioned antioxidant is the mixture of antioxidant 1010 and antioxidant 1076, and wherein, the weight ratio of antioxidant 1010 and antioxidant 1076 is 3:2.
Above-mentioned auxiliary antioxidant is the double lauryl of thio-2 acid.
The preparation method of above-mentioned biomedical metallic material, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, and mixing speed is 400rpm, and mixing time is 20min, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 80 DEG C in nitrogen atmosphere, stirring reaction 30min, obtains reactant；
Step 3, by extruded in step 2 gained reactant feeding double screw extruder, water-cooled, air-dried, pelletizing, obtain biomedical metallic material, wherein the extrusion condition of double screw extruder is: district's temperature 200 DEG C, two district's temperature 220 DEG C, three district's temperature 230 DEG C, four district's temperature 250 DEG C, and screw speed is 180rpm.
Test example 1
Embodiment 1 to 5 resulting materials is carried out corrosion resistant performance test: test sample is that working electrode, graphite rod are for being reference electrode to electrode, calomel electrode, utilizing the corrosion resistant performance of electrochemical workstation (Shanghai occasion China CHI760C) test material, test voltage is-2V～2V.
Result shows, the material of the present invention is for pure titanium, and corrosion potential all offsets to positive direction, shows that the material corrosion resistant ability of the present invention is strengthened, and this existence being probably cellulose nitrate makes its corrosion resistant ability be improved.
Test example 2
Embodiment 1 to 5 resulting materials is carried out nano hardness test: utilize nano-hardness tester (Mei Tesi process system company limited of the U.S.), with continuous hardness test, material is carried out nano hardness test, triangle Buddha's warrior attendant cone pressure head is 70nm at material surface compression distance under the promotion that load force is 1mN, and computer software records corresponding data simultaneously.The hardness number of sample is obtained by five zoness of different of measuring samples.
Result shows, the material of the present invention is for pure titanium, and nano-hardness value all improves more than 15%.
Test example 3
Embodiment 1 to 5 resulting materials is carried out antibacterial experiment: the bacterium solution that concentration is 107CFU/mL, at 121 DEG C of autoclaving 40min, is dropped in the sample surfaces (0.06mL/cm of sterilizing by all samples2), then there is the sample of bacterium solution to put into 37 DEG C of constant incubators cultivation 24h by dripping.Take out the sample that 24h cultivates, be seeded in after bacterium solution doubling dilution on the agar plate containing culture medium.Postvaccinal agar plate is put into 37 DEG C of constant incubators and is cultivated 24h, takes out agar plate and calculate the bacterial population (with reference to standard GB/T/T4789.2) lived after the cultivation of 24h.
Result shows, the material of the present invention has obvious antibacterial ability to escherichia coli, and its antibiotic rate reaches 99.5%；Also have obvious antibacterial ability to staphylococcus aureus, antibiotic rate reaches 98.45%.
Claims (4)
1. a biomedical metallic material, it is characterized in that: raw material includes in parts by weight: niobium powder 3～9 parts, platinum powder 2～8 parts, titanium valve 1～7 parts, molybdenum powder 2～7 parts, cellulose nitrate 1～6 parts, triphenyl phosphate 3～8 parts, antioxidant 1～7 parts, auxiliary antioxidant 2～8 parts, wollastonite fibre 1～5 parts, dibutyl tin mercaptides 2～7 parts, dibutyl phthalate 3～9 parts, triphenyl phosphite 3～8 parts, Hyaluronic Acid 2～7 parts, starch 1～8 parts, calcium silicates 2～9 parts, 2-ethyl-4-methylimidazole 1～6 parts；
Wherein, the granularity of described niobium powder, platinum powder, titanium valve and molybdenum powder is 100～200 mesh；Described antioxidant is the mixture of antioxidant 1010 and antioxidant 1076, and wherein, the weight ratio of antioxidant 1010 and antioxidant 1076 is 3:2；Described auxiliary antioxidant is the double lauryl of thio-2 acid.
2. the preparation method of the biomedical metallic material described in claim 1, it is characterised in that: comprise the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 65～80 DEG C in nitrogen atmosphere, stirring reaction 30～40min, obtains reactant；
Step 3, by extruded in step 2 gained reactant feeding double screw extruder, water-cooled, air-dried, pelletizing, obtains biomedical metallic material.
The preparation method of biomedical metallic material the most according to claim 2, it is characterised in that: the mixing speed being uniformly mixed in step 1 is 300～400rpm, and mixing time is 20～40min.
The preparation method of biomedical metallic material the most according to claim 2, it is characterized in that: in step 3, the extrusion condition of double screw extruder is: district's temperature 180～200 DEG C, two district's temperature 200～220 DEG C, three district's temperature 210～230 DEG C, four district's temperature 230～250 DEG C, screw speed is 160～180rpm.
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| CN201410623911.XA CN104436310B (en) | 2014-11-07 | 2014-11-07 | A kind of biomedical metallic material and preparation method thereof |
| CN201610723368.XA CN106178097A (en) | 2014-11-07 | 2014-11-07 | Preferable biomedical metallic material of antibacterial ability and preparation method thereof |
| CN201610724630.2A CN106334216A (en) | 2014-11-07 | 2014-11-07 | Biomedical metal material with good antibacterial ability |
| CN201610730219.6A CN106267333A (en) | 2014-11-07 | 2014-11-07 | A kind of antibacterial ability and the preferable biomedical metallic material of decay resistance |
| CN201610741939.2A CN106337155B (en) | 2014-11-07 | 2014-11-07 | The preferable biomedical metallic material of antibacterial ability |
| CN201610725898.8A CN106267372A (en) | 2014-11-07 | 2014-11-07 | A kind of biomedical metallic material |
| CN201610725174.3A CN106237377A (en) | 2014-11-07 | 2014-11-07 | Antibacterial ability and the preferable biomedical metallic material of decay resistance |
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| CN201610730219.6A Division CN106267333A (en) | 2014-11-07 | 2014-11-07 | A kind of antibacterial ability and the preferable biomedical metallic material of decay resistance |
| CN201610725174.3A Division CN106237377A (en) | 2014-11-07 | 2014-11-07 | Antibacterial ability and the preferable biomedical metallic material of decay resistance |
| CN201610741939.2A Division CN106337155B (en) | 2014-11-07 | 2014-11-07 | The preferable biomedical metallic material of antibacterial ability |
| CN201610724630.2A Division CN106334216A (en) | 2014-11-07 | 2014-11-07 | Biomedical metal material with good antibacterial ability |
| CN201610725898.8A Division CN106267372A (en) | 2014-11-07 | 2014-11-07 | A kind of biomedical metallic material |
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| CN201610725174.3A Withdrawn CN106237377A (en) | 2014-11-07 | 2014-11-07 | Antibacterial ability and the preferable biomedical metallic material of decay resistance |
| CN201610741939.2A Expired - Fee Related CN106337155B (en) | 2014-11-07 | 2014-11-07 | The preferable biomedical metallic material of antibacterial ability |
| CN201610730219.6A Withdrawn CN106267333A (en) | 2014-11-07 | 2014-11-07 | A kind of antibacterial ability and the preferable biomedical metallic material of decay resistance |
| CN201410623911.XA Active CN104436310B (en) | 2014-11-07 | 2014-11-07 | A kind of biomedical metallic material and preparation method thereof |
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| CN201610725174.3A Withdrawn CN106237377A (en) | 2014-11-07 | 2014-11-07 | Antibacterial ability and the preferable biomedical metallic material of decay resistance |
| CN201610741939.2A Expired - Fee Related CN106337155B (en) | 2014-11-07 | 2014-11-07 | The preferable biomedical metallic material of antibacterial ability |
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| CN101107067A (en) * | 2005-01-24 | 2008-01-16 | 金文申有限公司 | Metal-containing composite materials |
| CN103028146A (en) * | 2011-09-29 | 2013-04-10 | 深圳兰度生物材料有限公司 | Reinforcement medical composite material and method for preparing same |
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| CN1735562A (en) * | 2003-01-17 | 2006-02-15 | 西巴特殊化学品控股有限公司 | A process for the production of porous inorganic materials or a matrix material containing nanoparticles |
| CN100544776C (en) * | 2006-05-18 | 2009-09-30 | 上海交通大学 | Method for making foam biological titanium alloy artificial skelecton with hollow structure |
| CN101165087B (en) * | 2006-10-17 | 2010-12-01 | 路德石油化工（北京）有限公司 | Nano composite biological degradation plastic and preparing method thereof |
| KR20100112586A (en) * | 2008-01-04 | 2010-10-19 | 스미스 앤드 네퓨, 인크. | Surface alloyed medical implant |
| CN101724764B (en) * | 2009-12-10 | 2011-07-20 | 中南大学 | Process for preparing biomedical beta-titanium alloy |
| KR101324170B1 (en) * | 2010-09-16 | 2013-11-05 | 한국과학기술연구원 | Biomedical implants comprising surface-modified metal particles and biodegradable polymers, its use for suppressing inflammation, and preparation method thereof |
| CN102964790A (en) * | 2012-11-19 | 2013-03-13 | 贵州鸿顺发建材科技有限公司 | Man-made stone basin and preparation method thereof |
| CN103113129A (en) * | 2013-01-31 | 2013-05-22 | 华南理工大学 | Preparation method and application of hierarchical porous bioactive ceramic |
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| CN106267372A (en) | 2017-01-04 |
| CN104436310A (en) | 2015-03-25 |
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| CN106267333A (en) | 2017-01-04 |
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