TW202306928A - 一種從含鈣生物廢棄物製備雙相磷酸鈣多孔陶瓷的兩階段燒結方法 - Google Patents
一種從含鈣生物廢棄物製備雙相磷酸鈣多孔陶瓷的兩階段燒結方法 Download PDFInfo
- Publication number
- TW202306928A TW202306928A TW110129795A TW110129795A TW202306928A TW 202306928 A TW202306928 A TW 202306928A TW 110129795 A TW110129795 A TW 110129795A TW 110129795 A TW110129795 A TW 110129795A TW 202306928 A TW202306928 A TW 202306928A
- Authority
- TW
- Taiwan
- Prior art keywords
- calcium phosphate
- shells
- biphasic calcium
- foaming agent
- phosphate porous
- Prior art date
Links
- 230000002051 biphasic effect Effects 0.000 title claims abstract description 40
- 238000005245 sintering Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 20
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 239000011575 calcium Substances 0.000 title claims abstract description 12
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 12
- 239000010796 biological waste Substances 0.000 title claims description 8
- 239000004068 calcium phosphate ceramic Substances 0.000 title 1
- 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 claims abstract description 52
- 229910000389 calcium phosphate Inorganic materials 0.000 claims abstract description 40
- 239000001506 calcium phosphate Substances 0.000 claims abstract description 40
- 235000011010 calcium phosphates Nutrition 0.000 claims abstract description 40
- 239000000919 ceramic Substances 0.000 claims abstract description 35
- 239000004088 foaming agent Substances 0.000 claims abstract description 22
- 210000000988 bone and bone Anatomy 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000011049 filling Methods 0.000 claims abstract description 7
- 239000011148 porous material Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- 241000237502 Ostreidae Species 0.000 claims description 10
- 235000020636 oyster Nutrition 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 6
- 229910052586 apatite Inorganic materials 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[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 VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 claims description 5
- 235000019864 coconut oil Nutrition 0.000 claims description 4
- 239000003240 coconut oil Substances 0.000 claims description 4
- 241000238565 lobster Species 0.000 claims description 4
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 241000238424 Crustacea Species 0.000 claims description 2
- 241000238557 Decapoda Species 0.000 claims description 2
- 241000239366 Euphausiacea Species 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 150000001413 amino acids Chemical class 0.000 claims description 2
- 210000003278 egg shell Anatomy 0.000 claims description 2
- 239000006260 foam Substances 0.000 claims description 2
- 239000013505 freshwater Substances 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 229940079862 sodium lauryl sarcosinate Drugs 0.000 claims description 2
- ADWNFGORSPBALY-UHFFFAOYSA-M sodium;2-[dodecyl(methyl)amino]acetate Chemical compound [Na+].CCCCCCCCCCCCN(C)CC([O-])=O ADWNFGORSPBALY-UHFFFAOYSA-M 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 241000237858 Gastropoda Species 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 241000237536 Mytilus edulis Species 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229940094506 lauryl betaine Drugs 0.000 claims 1
- 235000020638 mussel Nutrition 0.000 claims 1
- DVEKCXOJTLDBFE-UHFFFAOYSA-N n-dodecyl-n,n-dimethylglycinate Chemical compound CCCCCCCCCCCC[N+](C)(C)CC([O-])=O DVEKCXOJTLDBFE-UHFFFAOYSA-N 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 abstract description 28
- 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 abstract description 28
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000012071 phase Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- 210000004027 cell Anatomy 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 210000000130 stem cell Anatomy 0.000 description 6
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 4
- 239000012890 simulated body fluid Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000005187 foaming Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 230000004071 biological effect Effects 0.000 description 2
- 229940036811 bone meal Drugs 0.000 description 2
- 239000002374 bone meal Substances 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000004069 differentiation Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 230000000399 orthopedic effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- TUBPSFQENHCYBW-HVDRVSQOSA-N (2s)-2-aminopentanedioic acid;2-[bis(2-hydroxyethyl)amino]ethanol Chemical compound OC(=O)[C@@H](N)CCC(O)=O.OCCN(CCO)CCO TUBPSFQENHCYBW-HVDRVSQOSA-N 0.000 description 1
- AZKSAVLVSZKNRD-UHFFFAOYSA-M 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide Chemical compound [Br-].S1C(C)=C(C)N=C1[N+]1=NC(C=2C=CC=CC=2)=NN1C1=CC=CC=C1 AZKSAVLVSZKNRD-UHFFFAOYSA-M 0.000 description 1
- 102000002260 Alkaline Phosphatase Human genes 0.000 description 1
- 108020004774 Alkaline Phosphatase Proteins 0.000 description 1
- 238000008940 Alkaline Phosphatase assay kit Methods 0.000 description 1
- 229910014497 Ca10(PO4)6(OH)2 Inorganic materials 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- JDRSMPFHFNXQRB-CMTNHCDUSA-N Decyl beta-D-threo-hexopyranoside Chemical compound CCCCCCCCCCO[C@@H]1O[C@H](CO)C(O)[C@H](O)C1O JDRSMPFHFNXQRB-CMTNHCDUSA-N 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- ZQBZAOZWBKABNC-UHFFFAOYSA-N [P].[Ca] Chemical compound [P].[Ca] ZQBZAOZWBKABNC-UHFFFAOYSA-N 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 description 1
- 229940063953 ammonium lauryl sulfate Drugs 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- -1 calcium phosphorus compound Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002361 compost Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000263 cytotoxicity test Toxicity 0.000 description 1
- 229940073499 decyl glucoside Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000004053 dental implant Substances 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 210000002950 fibroblast Anatomy 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000003703 image analysis method Methods 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 239000013642 negative control Substances 0.000 description 1
- 231100001083 no cytotoxicity Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000004818 osteo-differentiation Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000013641 positive control Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- BOLDJAUMGUJJKM-LSDHHAIUSA-N renifolin D Natural products CC(=C)[C@@H]1Cc2c(O)c(O)ccc2[C@H]1CC(=O)c3ccc(O)cc3O BOLDJAUMGUJJKM-LSDHHAIUSA-N 0.000 description 1
- 108700004121 sarkosyl Proteins 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229940045885 sodium lauroyl sarcosinate Drugs 0.000 description 1
- KSAVQLQVUXSOCR-UHFFFAOYSA-M sodium lauroyl sarcosinate Chemical compound [Na+].CCCCCCCCCCCC(=O)N(C)CC([O-])=O KSAVQLQVUXSOCR-UHFFFAOYSA-M 0.000 description 1
- 210000004872 soft tissue Anatomy 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000017423 tissue regeneration Effects 0.000 description 1
- 229940048912 triethanolamine cocoyl glutamate Drugs 0.000 description 1
- 239000013026 undiluted sample Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
- A61K6/838—Phosphorus compounds, e.g. apatite
-
- 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
- A61L27/12—Phosphorus-containing materials, e.g. apatite
-
- 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
-
- 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
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
-
- 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
- C04B35/62625—Wet mixtures
- C04B35/62635—Mixing details
-
- 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
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
-
- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
-
- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/638—Removal thereof
-
- 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
- C04B35/64—Burning or sintering processes
-
- 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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0051—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
- C04B38/0054—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity the pores being microsized or nanosized
-
- 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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
-
- 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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/10—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by using foaming agents or by using mechanical means, e.g. adding preformed foam
-
- 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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/08—Methods for forming porous structures using a negative form which is filled and then removed by pyrolysis or dissolution
-
- 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
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00836—Uses not provided for elsewhere in C04B2111/00 for medical or dental applications
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/447—Phosphates or phosphites, e.g. orthophosphate or hypophosphite
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/781—Nanograined materials, i.e. having grain sizes below 100 nm
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/785—Submicron sized grains, i.e. from 0,1 to 1 micron
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Inorganic Chemistry (AREA)
- Epidemiology (AREA)
- Public Health (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Transplantation (AREA)
- Dermatology (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Nanotechnology (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Materials For Medical Uses (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
本發明係關於一種從含鈣生物廢棄物製備雙相磷酸鈣多孔陶瓷的兩階段燒結方法，利用含鈣廢棄物所製備的氫氧基磷灰石和起泡劑混合，經過兩階段燒結，製成具有醫藥用途之骨填補材料。
Description
本發明係關於一種從含鈣生物廢棄物製備雙相磷酸鈣多孔陶瓷的兩階段燒結方法，透過將氫氧基磷灰石材料和起泡劑預混拌，並利用發泡法及兩階段不同溫度及不同時間的加熱，使得具備孔洞之雙相磷酸鈣。
氫氧基磷灰石(Hydroxyapatite,HA)化學式為Ca10(PO4)6(OH)2，理想鈣磷比為1.67，具有優良生物活性、生物相容性及骨傳導性，可與骨組織形成鍵結，且HA不具毒性，在體內不會產生發炎反應，因此廣泛應用於骨缺損修復及替代材料、整形外科填充材料、組織工程支架及藥物載體等。
氫氧基磷灰石的合成技術已有許多不同的方法被發展，主要可分為液相合成法與固相合成法，其中固相合成法包含固相燒結法及球磨法；液相合成法則包含溶膠凝膠法、微乳液法、化學沉澱法、水熱法、微波輻射法等。
與傳統化學藥劑所合成之磷灰石相較下，天然牡蠣殼具有多種微量元素，如鈉、鎂、鍶等，而這些微量元素為人體骨骼成長所必要之元素。
目前台灣合成氫氧基磷灰石仍以化學合成方式為主，然而，以天然廢棄物所合成的氫氧基磷灰石比化學合成的更具有優良的生物相容性，可降低與人體軟組織如皮膚、肌肉和牙齦的排斥性，使其成為骨科和牙科植入材料之理想成分，近年來已被廣泛應用於硬組織修復和運用在包括骨增強、骨修復以及表面塗層應用。
根據農委會廢棄物統計資料顯示，2007至2017年，臺灣每年平均產生約19萬公噸的廢棄牡蠣殼。
廢棄牡蠣殼不僅占空間，且殼上的殘肉容易孳生蒼蠅，在高溫日照下產生惡臭，造成環境汙染問題。
過去牡蠣殼主要用於飼料、堆肥及栽培介質上，其整體的附加價值並不高。
本發明係以廢棄牡蠣殼為原料製備氫氧基磷灰石，製備過程透過使其相變為具雙相氫氧基磷灰石/β-三鈣磷酸鹽的骨填補材料，故除可更進一步提升廢棄牡蠣殼之附加價值外，亦能降低其所造成之環境汙染問題。
根據本發明的目的，使用生物性含鈣原料牡蠣殼所合成之氫氧基磷灰石結晶結構之成分更類似於人骨，故生物相容性較高。
依據本發明之實施方式，包含以下步驟：混合轉動步驟、烘乾步驟、第一段燒結步驟及第二段燒結步驟。
混合轉動步驟，將氫氧基磷灰石和起泡劑，以10%比90%至90%比10%的比例混合成混合體，並將該混合體以250至3000rpm的高速攪拌成泡沫狀，其中較佳之混合比例為15%比85%至85%比15%。
烘乾步驟，將該經過上述混合轉動步驟之泡沫狀混合體，以50-200℃烘乾成定型混合體。
第一段燒結步驟，將該定型混合體以300℃至900℃下持溫加熱1至5小時，其中較佳燒結效果之持溫條件為溫度500℃至800℃加熱2至4小時。
第二段燒結步驟，延續該經過第一段燒結之該定型混合體，以900℃至1400℃下持溫加熱0.1至30小時，得含有雙相磷酸鈣多孔陶瓷之骨填充材料，其中較佳燒結效果之持溫條件為溫度1000℃至1200℃加熱15至30小時。
依照本發明實施方式，製備的雙相磷酸鈣具有孔隙率40-95%及孔洞尺寸50~700μm的物理表徵。
依照本發明實施方式，製備的雙相磷酸鈣含有氫氧基磷灰石及β-三鈣磷酸鹽成分，該氫氧基磷灰石含量(體積百分比)為20%至80%，該β-三鈣磷酸鹽含量(體積百分比)為20%至80%。
依照本發明實施方式，可產生大於100μm和小於100μm的孔洞，故滿足多孔植入物的應用性，大於100μm的孔洞可使骨組織向內生長，另外氫氧基磷灰石粉末經過燒結形成頸(necking)互相連接，顯示粉體已
經互相鍵結，可提供手術操作所需要強度。
依照本發明實施方式，該氫氧基磷灰石晶粒尺寸皆介於32-146nm。
依照本發明實施方式，該β-三鈣磷酸鹽晶粒尺寸皆介於37-49nm。
依照本發明實施方式，該氫氧基磷灰石的結晶度高於62%。
本發明之廢棄原料包含但不限於蛋殼、甲殼亞門動物之螃蟹殼、蝦殼、龍蝦殼、淡水龍蝦殼與磷蝦殼、雙殼綱動物之牡蠣殼、蛤蠣殼、文蛤殼、腹足綱動物之鮑魚殼。
本發明之另一樣態提供一種生醫材料及製備方法，其包含但不限於骨材料、牙科材料。
本發明之另一樣態提供一種含鈉、鎂、鍶之鈣磷化合物及其製備方法。
第一圖為雙相磷酸鈣多孔陶瓷於不同持溫時間燒結之(X-Ray Diffractometer,XRD)繞射圖。
第二圖為雙相磷酸鈣多孔陶瓷於不同持溫溫度燒結之繞射圖。
第三圖為雙相磷酸鈣多孔陶瓷於不同持溫時間燒結之繞射圖。
第四圖為雙相磷酸鈣多孔陶瓷之傅立葉轉換紅外光譜
(Fourier-transform infrared spectroscopy,FTIR)分析。
第五圖為雙相磷酸鈣多孔陶瓷之掃描式電子顯微鏡(Field Emission Scanning Electron Microscope,FESEM)照片。
第六圖為雙相磷酸鈣多孔陶瓷的孔徑分佈。
第七圖為雙相磷酸鈣多孔陶瓷浸泡於人工模擬體液(Simulated body fluid,SBF)溶液中的pH變化。
第八圖為雙相磷酸鈣多孔陶瓷浸泡於SBF中7天後之FESEM照片。
第九圖為MTT細胞活性試驗。
第十圖為第1、7、14天D1小鼠前驅幹細胞之WST-8細胞活性試驗。
第十一圖為第1、7、14天D1小鼠前驅幹細胞之ALP骨分化試驗。
依照本發明較佳實施例，將1公克氫氧基磷灰石與1.5ml起泡劑混合，其中該起泡劑包含但不限於椰子油起泡劑、葡萄糖起泡劑(癸基葡萄糖甘)、氨基酸起泡劑(TEA Cocoyl Glutamate)、弱酸性起泡劑(Ammonium Lauryl Sulfate)、月桂醯肌氨酸鈉(Sodium Lauroyl Sarcosinate)、脂肪醇界面活性劑(Fatty Alcohol Ethoxylate)。
參閱圖一，為本發明之雙相磷酸鈣多孔陶瓷於不同持溫時間燒結之XRD繞射圖，透過繞射圖可得知氫氧基磷灰石及β-三鈣磷酸鹽之兩
相比例、兩階段燒結溫度和時間如下表表一所示。
表一 雙相磷酸鈣多孔陶瓷於不同持溫時間燒結後之相比例、晶粒尺寸及結晶度。
依照本發明較佳實施例，將1公克氫氧基磷灰石與1.5ml起泡劑混合，其中該起泡劑為椰子油起泡劑。
參閱圖二，為本發明之雙相磷酸鈣多孔陶瓷於不同持溫時間燒結之XRD繞射圖，透過繞射圖可得知氫氧基磷灰石及β-三鈣磷酸鹽之兩相比例、兩階段燒結溫度和時間如下表表二所示。
表二 雙相磷酸鈣多孔陶瓷於不同持溫溫度燒結後之相比例、晶粒尺寸及結晶度。
依照本發明較佳實施例，將1公克氫氧基磷灰石與1.5ml起泡劑混合，其中該起泡劑為椰子油起泡劑。
參閱圖三，為本發明之雙相磷酸鈣多孔陶瓷於不同持溫時間燒結之XRD繞射圖，透過繞射圖可得知氫氧基磷灰石及β-三鈣磷酸鹽之兩相比例、兩階段燒結溫度和時間如下表表三所示。
表三 雙相磷酸鈣多孔陶瓷於不同持溫時間燒結後之相比例、晶粒尺寸及結晶度。
依照本發明實施方式，該氫氧基磷灰石含量(體積百分比)為20%至80%，該β-三鈣磷酸鹽含量(體積百分比)為20%至80%，其中較佳分別為62%與38%。
依照本發明實施方式，該氫氧基磷灰石的晶粒尺寸皆介於32-146nm，其中較佳為38、49、50nm。
依照本發明實施方式，該β-三鈣磷酸鹽的晶粒尺寸皆介於37-49nm，其中較佳為37、38、49nm。
依照本發明實施方式，第一階段燒結溫度和時間為700℃持溫2小時、其中較佳第二階段燒結溫度為1000℃，較佳持溫燒結時間為25小時，以該條件進行後續分析。
參閱圖四，為本發明之雙相磷酸鈣多孔陶瓷之FTIR分析結果圖。透過官能基比對發現，經過本發明燒結之結果具有雙相磷酸鈣的化學官能基團，包含OH-和PO4 3-基團。
參閱圖五，為本發明雙相磷酸鈣多孔陶瓷之FESEM照片，可發現經過本發明燒結之結晶顆粒存在多孔性，且許多孔洞大於100μm，另外可從照片發現，孔洞之間具有連通性，可以從一邊之孔洞觀察到另一側
的孔洞。
參閱圖六，為雙相磷酸鈣多孔陶瓷的孔徑分佈。透過圖像分析方法，以平均直徑表示經本發明製備之多孔陶瓷顆粒的孔徑分佈，本發明製備之多孔陶瓷顆粒有超過60%的孔洞之平均孔徑大於100μm。
參閱圖七，為雙相磷酸鈣多孔陶瓷浸泡於模擬體液的pH變化圖，模擬人體環境，本發明製備之多孔陶瓷顆粒在80小時後的pH變化趨向穩定，表示降解和沉積達到平衡。
參閱圖八，為雙相磷酸鈣多孔陶瓷浸泡於SBF中7天後之FESEM照片，本發明製備之多孔陶瓷顆粒在浸泡模擬體液7天後，表面有磷灰石沉積，可為骨組織形成鍵結之用，本發明製備之材料具有生物活性。
參閱圖九，為細胞活性試驗(3-(4,5-Dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide,MTT)結果圖，用以評估細胞毒性。
該試驗中的樣品為H、H/B、商用骨粉，其中H樣品為水溶解牡蠣殼，經沈澱法反應30min合成之氫氧基磷灰石，經過發泡及1300℃燒結20min後，得到的單相多孔氫氧基磷灰石顆粒；H/B樣品為醋酸溶解牡蠣殼，經沈澱法反應12小時合成之氫氧基磷灰石，經過發泡及1000℃燒結25小時後，得到的雙相多孔磷灰石顆粒(氫氧基磷灰石/：β-三鈣磷酸鹽)；正控制為苯酚；負控制組為三氧化二鋁。
將的0.2g/mL比例將樣品(H、H/B、商用骨粉)浸泡在培養基中24小時萃取，並稀釋成100、50、25、12.5%比例，與L929纖維母細胞在37℃下培養1天。
本發明製備雙相磷酸鈣多孔陶瓷的細胞毒性試驗結果顯示，除無稀釋之樣品，其餘稀釋之50、25、12.5%比例皆無細胞毒性。
參閱圖十，為第1、7、14天小鼠前驅幹細胞之WST-8細胞活性試驗。
試驗組材料以25%培養基萃取24小時後，相當於50mg/mL濃度，與D1細胞培養1、7、14天，並以WST試劑培養2小時後測量450nm之吸光度。
本發明製備雙相磷酸鈣多孔陶瓷對小鼠前驅幹細胞之細胞活性，在第14天優於商用套組。
參閱圖十一，為第1、7、14天D1小鼠前驅幹細胞之鹼性磷酸酶螢光活性(Alkaline Phosphatase Assay Kit,ALP)之骨分化試驗。
本發明製備雙相磷酸鈣多孔陶瓷對小鼠前驅幹細胞骨分化活性，在第7天優於商用套組。
Claims (9)
- 一種從含鈣生物廢棄物製備雙相磷酸鈣多孔陶瓷的兩階段燒結方法，其包含：混合轉動步驟，將氫氧基磷灰石和起泡劑混合成混合體，將該混合體高速攪拌成泡沫狀；烘乾步驟，將該泡沫狀混合體烘乾成定型混合體；第一段燒結步驟，將該定型混合體以300度至900度下加熱1至5小時；以及第二段燒結步驟，接續將經過第一段燒結之該定型混合體以900度至1400度下加熱0.1至30小時，得含有雙相磷酸鈣多孔陶瓷之骨填充材料。
- 如申請專利範圍第1項所述之含鈣生物廢棄物製備雙相磷酸鈣多孔材料的兩階段燒結方法，其中該含鈣生物廢棄物係為蛋殼、甲殼亞門動物之螃蟹殼、蝦殼、龍蝦殼、淡水龍蝦殼與磷蝦殼、雙殼綱動物之牡蠣殼、蛤蠣殼、文蛤殼、貽貝殼、腹足綱動物之鮑魚殼。
- 如申請專利範圍第1項所述之含鈣生物廢棄物製備雙相磷酸鈣多孔材料的兩階段燒結方法，其中該混合轉動步驟之起泡劑為椰子油起泡劑、葡萄糖起泡劑、氨基酸起泡劑、弱酸性起泡劑、月桂醯肌氨酸鈉、月桂基甜菜鹼、脂肪醇界面活性劑或其組合。
- 如申請專利範圍第1項所述之含鈣生物廢棄物製備雙相磷酸鈣多孔材料的兩階段燒結方法，其中該混合轉動步驟之該氫氧基磷灰石和該起泡劑混合比例為10%比90%至90%比10%。
- 如申請專利範圍第1項所述之含鈣生物廢棄物製備雙相磷酸鈣多孔材料的兩階段燒結方法，其中該混合轉動步驟之該高速轉速為250至3000rpm。
- 如申請專利範圍第1項所述之含鈣生物廢棄物製備雙相鈣磷酸鹽材料的兩階段燒結方法，其中該烘乾步驟之烘乾溫度為50至200度。
- 一種如專利申請範圍第1項至第5項中任一項所述之方法製成的雙相磷酸鈣多孔陶瓷，其包含：氫氧基磷灰石及β-三鈣磷酸鹽，其中該氫氧基磷灰石體積百分比為20%至80%，該β-三鈣磷酸鹽體積百分比為20%至80%。
- 如申請專利範圍第6項所述之雙相磷酸鈣多孔陶瓷，該雙相磷酸鈣多孔陶瓷的孔洞尺寸介於50μm至700μm。
- 一種如專利申請範圍第1項至第5項中任一項所述之方法製成的雙相磷酸鈣多孔陶瓷之用途，其可用於骨填充、牙填充材料。
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW110129795A TWI791260B (zh) | 2021-08-12 | 2021-08-12 | 一種從含鈣生物廢棄物製備雙相磷酸鈣多孔陶瓷的兩階段燒結方法 |
| CN202210883374.7A CN115703685A (zh) | 2021-08-12 | 2022-07-26 | 一种从含钙生物废弃物制备双相磷酸钙多孔陶瓷的两阶段烧结方法 |
| US17/815,218 US20230062742A1 (en) | 2021-08-12 | 2022-07-27 | Two-stage sintering method for preparing porous biphasic calcium phosphate ceramic from calcium-containing biological waste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW110129795A TWI791260B (zh) | 2021-08-12 | 2021-08-12 | 一種從含鈣生物廢棄物製備雙相磷酸鈣多孔陶瓷的兩階段燒結方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| TWI791260B TWI791260B (zh) | 2023-02-01 |
| TW202306928A true TW202306928A (zh) | 2023-02-16 |
Family
ID=85181413
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| TW110129795A TWI791260B (zh) | 2021-08-12 | 2021-08-12 | 一種從含鈣生物廢棄物製備雙相磷酸鈣多孔陶瓷的兩階段燒結方法 |
Country Status (3)
| Country | Link |
|---|---|
| US (1) | US20230062742A1 (zh) |
| CN (1) | CN115703685A (zh) |
| TW (1) | TWI791260B (zh) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116813328A (zh) * | 2023-05-15 | 2023-09-29 | 四川大学 | 一种用于牙槽骨缺损修复的多孔白磷钙石复相陶瓷及制备方法 |
| CN118206089A (zh) * | 2024-03-20 | 2024-06-18 | 上海倍尔康生物医学科技有限公司 | 一种羟基磷灰石微球及其制备方法和应用 |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6713420B2 (en) * | 2000-10-13 | 2004-03-30 | Toshiba Ceramics Co., Ltd. | Porous ceramics body for in vivo or in vitro use |
| CN100491288C (zh) * | 2005-09-06 | 2009-05-27 | 四川大学 | 一种纳米多孔生物陶瓷的制备方法 |
| TWI382852B (zh) * | 2009-12-22 | 2013-01-21 | Univ Taipei Medical | 一種口腔保健用磷酸鈣複合物及其製法與組合物 |
| CN101983728B (zh) * | 2010-11-09 | 2013-12-04 | 厦门大学 | 贝壳多孔羟基磷灰石基骨修复材料及其制备方法 |
| CN102107020B (zh) * | 2011-02-14 | 2014-08-27 | 温宁 | 三维类骨结构人工骨的制备方法及其产品 |
| EP2865791A4 (en) * | 2012-06-20 | 2016-02-24 | Jnc Corp | PROCESS FOR PRODUCING POROUS CALCIUM PHOSPHATE BODY AND POROUS CALCIUM PHOSPHATE BODY PRODUCED THEREBY |
| ES2555235B1 (es) * | 2014-06-25 | 2016-10-05 | Universitat Politècnica De Catalunya | Nuevo proceso de fabricación en un solo paso de biomateriales espumados |
| CN105347322B (zh) * | 2015-12-08 | 2017-05-03 | 浙江理工大学 | 一种利用贝壳制备的球状纳米多孔性羟基磷灰石及其制备方法 |
| CN108159497A (zh) * | 2018-01-22 | 2018-06-15 | 福建吉特瑞生物科技有限公司 | 一种牡蛎壳羟基磷灰石多孔骨修复材料及其制备方法 |
-
2021
- 2021-08-12 TW TW110129795A patent/TWI791260B/zh active
-
2022
- 2022-07-26 CN CN202210883374.7A patent/CN115703685A/zh active Pending
- 2022-07-27 US US17/815,218 patent/US20230062742A1/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| US20230062742A1 (en) | 2023-03-02 |
| CN115703685A (zh) | 2023-02-17 |
| TWI791260B (zh) | 2023-02-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Waheed et al. | Channelling eggshell waste to valuable and utilizable products: a comprehensive review | |
| TWI791260B (zh) | 一種從含鈣生物廢棄物製備雙相磷酸鈣多孔陶瓷的兩階段燒結方法 | |
| Clarke et al. | Designs from the deep: Marine organisms for bone tissue engineering | |
| Mondal et al. | Physico-chemical characterization and biological response of Labeo rohita-derived hydroxyapatite scaffold | |
| Kumar et al. | Hydroxyapatite: a versatile bioceramic for tissue engineering application | |
| WO2007011172A1 (en) | Preparation method of porous beta tricalcium phosphate granules | |
| CN114452439B (zh) | 一种仿生天然骨矿组成的羟基磷灰石/白磷钙石生物活性陶瓷支架及其制备方法 | |
| CN107032775B (zh) | 一种纳米羟基磷灰石、硅酸二钙复合生物陶瓷及其制备方法和应用 | |
| JP6318282B1 (ja) | リン酸四カルシウムを調製する方法 | |
| CN109453430B (zh) | 一种羟基磷灰石涂层的胶原蛋白-氧化石墨烯仿生材料及其制备方法 | |
| CN102145193A (zh) | 墨鱼骨转化系列多孔生物陶瓷 | |
| Malau et al. | Synthesis of hydrokxyapatite based duck egg shells using precipitation method | |
| Oktar et al. | Marine-derived bioceramics for orthopedic, reconstructive and dental surgery applications | |
| CN107596453A (zh) | 一种3d打印复合磁性金属支架及其应用 | |
| Akyol et al. | Morphology, characterization, and conversion of the corals Goniopora spp. and Porites cylindrica to hydroxyapatite | |
| Manchinasetty et al. | Preparation of flexible bone tissue scaffold utilizing sea urchin test and collagen | |
| Siddiqi et al. | FABRICATION OF BIOCOMPATIBLE NANO-CARBONATED HYDROXYAPATITE/POLYMER SPONGY SCAFFOLDS. | |
| Hanan et al. | Fabrication of poly (Lactic-co-glycolic acid)/calcium phosphate bone cement composite: Synthesization of calcium phosphate from crab shells | |
| Malau et al. | Hydroxyapatite Preparation from Crab Shell Waste by Precipitation Method | |
| TWI769746B (zh) | 天然含鈣廢棄物製備之骨填補物及其製備方法 | |
| US20230001050A1 (en) | Bone void filler and method for manufacturing the same by natural calcium-containing waste | |
| Hiray et al. | Invertebrate-derived bioceramics: An effective alternative source for biomedical applications | |
| CN115572177A (zh) | 天然含钙废弃物制备的骨填补物及其制备方法 | |
| CN103977454A (zh) | 磷酸镁/小麦蛋白复合材料及其制备方法和应用 | |
| CN114348981B (zh) | 一种仿生生物矿化的三斜钙磷石的制备方法和应用 |