CN107441558A - A kind of porous SiO of bone tissue engineer2The preparation method of/biphasic calcium phosphate compound rest - Google Patents
A kind of porous SiO of bone tissue engineer2The preparation method of/biphasic calcium phosphate compound rest Download PDFInfo
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- CN107441558A CN107441558A CN201710759772.7A CN201710759772A CN107441558A CN 107441558 A CN107441558 A CN 107441558A CN 201710759772 A CN201710759772 A CN 201710759772A CN 107441558 A CN107441558 A CN 107441558A
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- calcium phosphate
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- 239000001506 calcium phosphate Substances 0.000 title claims abstract description 70
- 230000002051 biphasic effect Effects 0.000 title claims abstract description 59
- 229910000389 calcium phosphate Inorganic materials 0.000 title claims abstract description 59
- 235000011010 calcium phosphates Nutrition 0.000 title claims abstract description 59
- -1 calcium phosphate compound Chemical class 0.000 title claims abstract description 29
- 210000000988 bone and bone Anatomy 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 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 44
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000000741 silica gel Substances 0.000 claims abstract description 21
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 21
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- 238000007598 dipping method Methods 0.000 claims abstract description 18
- 239000006260 foam Substances 0.000 claims abstract description 18
- 229920002635 polyurethane Polymers 0.000 claims abstract description 17
- 239000004814 polyurethane Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 15
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 15
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 239000004068 calcium phosphate ceramic Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000011148 porous material Substances 0.000 claims abstract description 10
- 238000004513 sizing Methods 0.000 claims abstract description 10
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- 238000012545 processing Methods 0.000 claims abstract description 6
- 239000011575 calcium Substances 0.000 claims description 20
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 13
- 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 claims description 13
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims description 11
- 229940078499 tricalcium phosphate Drugs 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 238000005470 impregnation Methods 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 13
- 239000002585 base Substances 0.000 description 10
- 229910052791 calcium Inorganic materials 0.000 description 7
- 210000004027 cell Anatomy 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 210000001519 tissue Anatomy 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000012010 growth Effects 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 230000003013 cytotoxicity Effects 0.000 description 3
- 231100000135 cytotoxicity Toxicity 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229940123373 Adenovirus E1A gene Drugs 0.000 description 1
- 229910014497 Ca10(PO4)6(OH)2 Inorganic materials 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 108010087230 Sincalide Proteins 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- ZQBZAOZWBKABNC-UHFFFAOYSA-N [P].[Ca] Chemical compound [P].[Ca] ZQBZAOZWBKABNC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000003462 bioceramic Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 230000008468 bone growth Effects 0.000 description 1
- 210000002805 bone matrix Anatomy 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- UUVBYOGFRMMMQL-UHFFFAOYSA-N calcium;phosphoric acid Chemical compound [Ca].OP(O)(O)=O UUVBYOGFRMMMQL-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000010609 cell counting kit-8 assay Methods 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 231100000263 cytotoxicity test Toxicity 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 210000002919 epithelial cell Anatomy 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000006651 lactation Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 231100001083 no cytotoxicity Toxicity 0.000 description 1
- 230000011164 ossification Effects 0.000 description 1
- 230000004072 osteoblast differentiation Effects 0.000 description 1
- 230000000278 osteoconductive effect Effects 0.000 description 1
- 210000004409 osteocyte Anatomy 0.000 description 1
- 210000005009 osteogenic cell Anatomy 0.000 description 1
- 230000002188 osteogenic effect Effects 0.000 description 1
- 230000002138 osteoinductive effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000007170 pathology Effects 0.000 description 1
- 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 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- IZTQOLKUZKXIRV-YRVFCXMDSA-N sincalide Chemical compound C([C@@H](C(=O)N[C@@H](CCSC)C(=O)NCC(=O)N[C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)N[C@@H](CCSC)C(=O)N[C@@H](CC(O)=O)C(=O)N[C@@H](CC=1C=CC=CC=1)C(N)=O)NC(=O)[C@@H](N)CC(O)=O)C1=CC=C(OS(O)(=O)=O)C=C1 IZTQOLKUZKXIRV-YRVFCXMDSA-N 0.000 description 1
- 239000002993 sponge (artificial) Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 210000005065 subchondral bone plate Anatomy 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
Classifications
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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
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/42—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix
- A61L27/425—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix of phosphorus containing material, 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
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/42—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix
- A61L27/427—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix of other specific inorganic materials not covered by A61L27/422 or A61L27/425
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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
-
- 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
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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
- A61L27/58—Materials at least partially resorbable by the body
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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
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Transplantation (AREA)
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- Medicinal Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- General Health & Medical Sciences (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
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Abstract
The present invention relates to a kind of bone tissue engineer with porous SiO2The preparation method of/biphasic calcium phosphate compound rest, belongs to technical field of biomedical materials.Biphasic calcium phosphate presoma powder is prepared by the precipitation method first；Biphasic calcium phosphate presoma powder calcination is obtained into biophasic calcium phosphate ceramic powder；Biophasic calcium phosphate ceramic powder is well mixed with egg binding agent to obtain slurry A, is added in distilled water and is uniformly mixing to obtain dipping sizing agent；Polyurethane organic foam carrier with regular through hole is prepared using Laser Processing forming technique；In the dipping sizing agent that polyurethane organic foam carrier is placed in, obtain impregnating base substrate B after drying；Dipping base substrate B is thermally treated resulting in porous biphasic calcium phosphate support C；Silica gel is well mixed with distilled water to obtain aqueous solution of silica gel, porous biphasic calcium phosphate support C is placed in aqueous solution of silica gel and soaked；Finally it is thermally treated resulting in porous SiO2/ biphasic calcium phosphate compound rest.This method technique is simple, and the porosity of porous material of preparation is high.
Description
Technical field
The present invention relates to a kind of bone tissue engineer with porous SiO2The preparation method of/biphasic calcium phosphate compound rest, belongs to
Technical field of biomedical materials.
Background technology
Organizational project (Tissue Engineering, TE) is a kind of emerging interdisciplinary fields, and it is related to application project
Learn with the principle of life science and method to understand the histioid structure-function relationship of lactation of normal and pathology, and research
Biological substitution product are to recover, maintain or improve its function.Nineteen ninety-five, Crane systems propose the bone tissue engineer of concept, turn into group
Focus in weaver's journey research field.The content of bone tissue engineer research is mainly seed cell, timbering material and activator three
Individual part, wherein timbering material are most important parts, and it refers to be combined and be implanted into organism with seed cell
Material, it is possible to increase the attachment of that cell and the place as its metabolism, while the form of the timbering material and function are straight
Connect the form and function for affecting formed tissue.Natural material can be divided into by studying more bone tissue engineering stent material at present
Material, synthesis high polymer material and biological active ceramic material three parts.Wherein, bioceramic material is due to its excellent biology
Compatibility, there is to bone similar constituent, there is osteoconductive, forming the biology performances such as chemical bonds with bone tissue,
Obtain the favor of increasing investigation of materials person and Medical Technologist.Conventional biological active ceramic material mainly has hydroxy-apatite
Stone（Hydroxyapatite, HAP), tricalcium phosphates of β mono- (β-tricalcium phosphate, β-TCP) etc..
Hydroxyapatite（HAP）, molecular formula Ca10(PO4)6(OH)2, it is that one kind is soluble in acid, is insoluble in alkali, and slightly soluble
Yu Shui, be in weakly alkaline fragile material in water, its Ca/P ratio is 1.67, be human body bone with the host inorganic of animal skeleton into
Point.Calcium and phosphorus in HAP can dissociate material surface, absorbed by body tissue and cause to degrade, and will not be in people after degrading
Leave foreign matter in vivo.Because can with bon e formation is stronger is bonded, produce bone matrix collagen, promote bone growth, form stable, hydroxyl
Base apatite is considered as the bone tissue engineer biomaterial of current better performances.Bata-tricalcium phosphate, molecular formula Ca3
(PO4)2, abbreviation β-TCP, the ratio of calcium atom and phosphorus atoms is 1.5, is close with the calcium-phosphorus ratio of bone tissue, and porous beta-TCP
Material can provide larger specific surface area, be advantageous to growth, breeding and differentiation of the cell on material.Its constituent
Ca, P, O are similar to the inorganic constituents in natural bone, good biocompatibility, are easy to degrade in viable organism after implanting,
The Elements C a, P of degraded can enter in living body fluids and participate in circulating, and have facilitation to New born formation.Therefore, β-tricresyl phosphate
Calcium turns into a kind of tissue engineering bracket material of potential high comprehensive performance.
Biphasic calcium phosphate is bone tissue engineering stent material the most frequently used at present, and it is β-TCP and HAP mixture, is
A kind of bioactive materials with network structure, wherein, β-TCP and HAP can be mixed by different proportion.Biphasic calcium phosphate material
Cell adherence and propagation can be promoted, there is good biocompatibility, also, it has β-TCP and HAP characteristic simultaneously, makes
β-TCP easy absorbability and HAP support effect produce cooperative effect, so, its controllable degradation property and bone formation performance ratio list
One Ca-P ceramic material is more preferable.Moreover, the osteogenic of biphasic calcium phosphate can be obtained by the crystal microstructure of controlled material
Improve.Research shows, has the biophasic calcium phosphate ceramic support of three-dimensional porous structure, can be by adjusting HAP/ β-TCP ratio
So that the timbering material has osteoinductive under certain condition.
Ludox is the gel rubber system of silica for being disperseed to be formed in water by unbodied silica colloidal particles,
Its particle size is several nanometers to few tens of nanometers.Its top layer is covered by silanol group (- Si-OH) and hydroxyl (- OH), and
Inside is siloxanes (- Si-O-Si-) network.Ludox can improve the mechanical strength of support as binding agent, and to more
The pore space structure of hole support influences little.Research shows that nano grain surface coating silicon dioxide coating can significantly reduce base
The cytotoxicity of body material；Porous silica support has good bioactivity and osteoblast differentiation performance.
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of bone tissue engineer porous SiO2/
The preparation method of biphasic calcium phosphate compound rest.For this method using biphasic calcium phosphate porous support as matrix, silica gel is the second material
Compound obtained porous SiO2/ biphasic calcium phosphate compound rest, the porous compound support frame have irregular through hole and rule straight
The pore space structure that through hole is combined, there is good connectivity and bioactivity.Pass through laser forming technology and foam impregnation method
Biphasic calcium phosphate biological scaffold is prepared.The present invention is achieved through the following technical solutions.
A kind of porous SiO of bone tissue engineer2The preparation method of/biphasic calcium phosphate compound rest, it is comprised the following steps that：
Step 1, calcium carbonate and phosphoric acid are mixed according to stoichiometry Ca/P=1.5 and stoichiometry Ca/P=1.67 respectively first
Bata-tricalcium phosphate and hydroxyapatite is prepared in precipitation respectively, according to mass ratio is 70 by bata-tricalcium phosphate and hydroxyapatite
~85：15~30 well mixed obtain biphasic calcium phosphate presoma powder；
Step 2, by biphasic calcium phosphate presoma powder that step 1 obtains be 1000~1200 DEG C in temperature at calcine 8-10h, obtain
To biophasic calcium phosphate ceramic powder；
Step 3, by the biophasic calcium phosphate ceramic powder that step 2 obtains according to mass ratio be 1:3~1:7 mix with egg binding agent
Conjunction uniformly obtain slurry A, by slurry A according to volume ratio be 2:1~2:7 are added in distilled water, are uniformly mixing to obtain dipping slurry
Material；
Step 4, the polyurethane organic foam carrier with regular through hole is prepared using Laser Processing forming technique；
Step 5, the polyurethane organic foam carrier that step 4 obtains is placed in the dipping sizing agent of step 3, is 30~60 in temperature
1~7min is impregnated under the conditions of DEG C, repeated impregnations 1~7 time, obtains impregnating base substrate B after drying；
Step 6, dipping base substrate B that step 3 obtains is raised to 130~160 DEG C with 1~4 DEG C/min from room temperature, 4~7 DEG C/min from
130~160 DEG C rise to 280~320 DEG C, and 0.5~2.5 DEG C/min rises to 550~650 DEG C from 280~320 DEG C, with 4~8
DEG C/min rises to 800~850 DEG C, 3~6h is incubated, last furnace cooling obtains porous biphasic calcium phosphate support C；
Step 7, the silica gel that step 6 is obtained and distilled water are 1 in mass ratio:1~1:3 it is well mixed obtain aqueous solution of silica gel,
The porous biphasic calcium phosphate support C that step 6 is obtained is placed in aqueous solution of silica gel, soaks 4~10h, taking-up filter at room temperature
The abundant adsorption surface redundant solution of paper, then drying bracket；
Step 8, the support handled through step 7 is raised to 150~180 DEG C with 1~4 DEG C/min from room temperature, 4~7 DEG C/min is from 150
~180 DEG C rise to 300~330 DEG C, are incubated 3~6h, last furnace cooling to room temperature, obtain porous SiO2/ biphasic calcium phosphate
Compound rest.
0.6~2mm of polyurethane organic foam carrier clear opening pore diameter range in the step 4.
The beneficial effects of the invention are as follows：
（1）This experiment prepares porous biophasic calcium phosphate ceramic support using laser forming technology and Polymeric sponge method, uses
The method that immersion silica gel solution re-sinters prepares porous SiO2/ biphasic calcium phosphate biological scaffold.Its preparation technology is simple, preparation
Porosity of porous material is high, and aperture is controllable and is three-dimensional open pores network structure, can preferably meet bone tissue engineering stent material
Requirement to loose structure.
（2）Ca, P composition contained in biphasic calcium phosphate can produce slight dissolving in body, Ca after dissolving first,
P is combined with the calcium ion and phosphonium ion of surrounding tissue in the form of chemical bonds, next subchondral bone around of combining closely
Archaeocyte, last osteogenic cell enter support and developed to osteocyte, finally progressively substitute carrier, promote the growth of bone tissue.
（3）Because of the addition of silica gel, its mechanical property is improved the complex stephanoporate bracket of gained.
Brief description of the drawings
Fig. 1 is the porous SiO that the embodiment of the present invention 1 is prepared2/ biphasic calcium phosphate compound rest XRD；
Fig. 2 is the porous SiO that the embodiment of the present invention 1 is prepared2/ biphasic calcium phosphate compound rest FTIR schemes；
Fig. 3 is the porous SiO that the embodiment of the present invention 1 is prepared2/ biphasic calcium phosphate compound rest different parts SEM schemes.
Embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
The porous SiO of the bone tissue engineer2The preparation method of/biphasic calcium phosphate compound rest, it is comprised the following steps that：
Step 1, first at room temperature by calcium carbonate and phosphoric acid respectively according to stoichiometry Ca/P=1.5 and stoichiometry Ca/P=
Bata-tricalcium phosphate and hydroxyapatite is prepared in 1.67 mixed precipitations respectively, by bata-tricalcium phosphate and hydroxyapatite according to matter
Amount is than being 85：15 well mixed obtain biphasic calcium phosphate presoma powder；
Step 2, by biphasic calcium phosphate presoma powder that step 1 obtains be 1200 DEG C in temperature at calcine 10h, obtain two-phase phosphorus
Sour calcium ceramic powder；
Step 3, by the biophasic calcium phosphate ceramic powder that step 2 obtains according to mass ratio be 1:3 mix with egg binding agent
It is even to obtain slurry A, by slurry A according to volume ratio be 2:1 is added in distilled water, is uniformly mixing to obtain dipping sizing agent；
Step 4, the polyurethane organic foam carrier with regular through hole, wherein polyurethane are prepared using Laser Processing forming technique
Organic foam carrier clear opening pore diameter range 0.6mm；
Step 5, the polyurethane organic foam carrier that step 4 obtains is placed in the dipping sizing agent of step 3, is 30 DEG C of bars in temperature
Impregnate 1min under part, repeated impregnations 1 time, obtain impregnating base substrate B after 40 DEG C of drying 6h；
Step 6, the dipping base substrate B that step 3 obtains is raised to 130 DEG C with 1 DEG C/min from room temperature, 4 DEG C/min rises to from 130 DEG C
280 DEG C, 0.5 DEG C/min rises to 550 DEG C from 280 DEG C, rises to 800 DEG C with 4 DEG C/min, is incubated 3h, last furnace cooling obtains
To porous biphasic calcium phosphate support C；
Step 7, the silica gel that step 6 is obtained and distilled water are 1 in mass ratio:1 it is well mixed obtain aqueous solution of silica gel, by step
6 obtained porous biphasic calcium phosphate support C are placed in aqueous solution of silica gel, soak 4h at room temperature, taking-up is fully drawn with filter paper
Excess surface solution, then 30 DEG C of drying bracket 4h；
Step 8, the support handled through step 7 is raised to 150 DEG C with 1 DEG C/min from room temperature, 4 DEG C/min rises to 300 from 150 DEG C
DEG C, 3h is incubated, last furnace cooling to room temperature, obtains porous SiO2/ biphasic calcium phosphate compound rest.
The porous SiO that the present embodiment is prepared2/ biphasic calcium phosphate compound rest XRD, as shown in figure 1, from Fig. 1
It can be seen that porous SiO2/ biphasic calcium phosphate compound rest composition is β-TCP and HAP two-phases, and wherein β-TCP are principal phase.It is porous
SiO2/ biphasic calcium phosphate compound rest FTIR is schemed as shown in Fig. 2 3571cm-1The absworption peak at place corresponds to the not right of O-H in the crystallization water
Claim the flexible peak that shakes, 1637cm-1The peak at place is the H-O-H flexural vibrations peaks of water, and the two infrared absorption peaks are due in Ludox
Constitution water caused by.1065cm-1It is PO to locate strong and wide peak4 3-Asymmetric stretching vibration peak, 605cm-1Absworption peak pair
Answer PO4 3-Flexural vibrations peak, 553cm-1Absworption peak correspond to HPO4 2-Flexural vibrations peak, this shows two-phase in the porous support
The presence of phosphoric acid calcium component；472cm-1There are Si-O deformation vibrations in silicon-oxy tetrahedron, it was demonstrated that SiO after compound2Presence.
Porous SiO2/ biphasic calcium phosphate compound rest SEM schemes the support as shown in figure 3, after as can be seen from Figure 3 compound
Rough surface, and have micro-crack generation, in addition, compared with non-compound rest, its aperture diminishes, and has part aperture to be blocked.Figure
In as can be seen that irregular clear opening aperture be 100~500um, regular clear opening aperture is 700~900um.
Embodiment 2
The porous SiO of the bone tissue engineer2The preparation method of/biphasic calcium phosphate compound rest, it is comprised the following steps that：
Step 1, first at room temperature by calcium carbonate and phosphoric acid respectively according to stoichiometry Ca/P=1.5 and stoichiometry Ca/P=
Bata-tricalcium phosphate and hydroxyapatite is prepared in 1.67 mixed precipitations respectively, by bata-tricalcium phosphate and hydroxyapatite according to matter
Amount is than being 80：20 well mixed obtain biphasic calcium phosphate presoma powder；
Step 2, by biphasic calcium phosphate presoma powder that step 1 obtains be 1100 DEG C in temperature at calcine 9h, obtain two-phase phosphorus
Sour calcium ceramic powder；
Step 3, by the biophasic calcium phosphate ceramic powder that step 2 obtains according to mass ratio be 1:4 mix with egg binding agent
It is even to obtain slurry A, by slurry A according to volume ratio be 2:3 are added in distilled water, are uniformly mixing to obtain dipping sizing agent；
Step 4, the polyurethane organic foam carrier with regular through hole, wherein polyurethane are prepared using Laser Processing forming technique
Organic foam carrier clear opening pore diameter range 2mm；
Step 5, the polyurethane organic foam carrier that step 4 obtains is placed in the dipping sizing agent of step 3, is 40 DEG C of bars in temperature
Impregnate 3min under part, repeated impregnations 3 times, obtain impregnating base substrate B after 40 DEG C of drying 6h；
Step 6, the dipping base substrate B that step 3 obtains is raised to 140 DEG C with 2 DEG C/min from room temperature, 5 DEG C/min rises to from 140 DEG C
300 DEG C, 1 DEG C/min rises to 580 DEG C from 300 DEG C, rises to 810 DEG C with 5 DEG C/min, is incubated 4h, last furnace cooling obtains
Porous biphasic calcium phosphate support C；
Step 7, the silica gel that step 6 is obtained and distilled water are 1 in mass ratio:2 it is well mixed obtain aqueous solution of silica gel, by step
6 obtained porous biphasic calcium phosphate support C are placed in aqueous solution of silica gel, soak 6h at room temperature, taking-up is fully drawn with filter paper
Excess surface solution, then 30 DEG C of drying bracket 4h；
Step 8, the support handled through step 7 is raised to 160 DEG C with 2 DEG C/min from room temperature, 5 DEG C/min rises to 310 from 160 DEG C
DEG C, 4h is incubated, last furnace cooling to room temperature, obtains porous SiO2/ biphasic calcium phosphate compound rest.
From 293T cells（Transfect people's renal epithelial cell of Adenovirus E1A gene）, CCK-8 methods foundation standard GB/T/
T14233.3-2005, to the porous SiO being prepared2/ biphasic calcium phosphate compound rest, row cytotoxicity test.Its result is such as
Shown in table 1, with reference to standard GB/T/T14233.3-2005 relevant regulations, cytotoxicity result shows：（1）Support concentration exists
During 0.05-0.3g/ml, relative growth rate（RGR）Between 90-110, cytotoxicity is 0 or 1 grade；As a result prepared by explanation
SiO2/ biphasic calcium phosphate timbering material no cytotoxicity.
1 porous SiO of table2The relative growth rate of/biphasic calcium phosphate compound rest
Embodiment 3
The porous SiO of the bone tissue engineer2The preparation method of/biphasic calcium phosphate compound rest, it is comprised the following steps that：
Step 1, first at room temperature by calcium carbonate and phosphoric acid respectively according to stoichiometry Ca/P=1.5 and stoichiometry Ca/P=
Bata-tricalcium phosphate and hydroxyapatite is prepared in 1.67 mixed precipitations respectively, by bata-tricalcium phosphate and hydroxyapatite according to matter
Amount is than being 70：30 well mixed obtain biphasic calcium phosphate presoma powder；
Step 2, by biphasic calcium phosphate presoma powder that step 1 obtains be 1000 DEG C in temperature at calcine 8h, obtain two-phase phosphorus
Sour calcium ceramic powder；
Step 3, by the biophasic calcium phosphate ceramic powder that step 2 obtains according to mass ratio be 1:7 mix with egg binding agent
It is even to obtain slurry A, by slurry A according to volume ratio be 2:7 are added in distilled water, are uniformly mixing to obtain dipping sizing agent；
Step 4, the polyurethane organic foam carrier with regular through hole, wherein polyurethane are prepared using Laser Processing forming technique
Organic foam carrier clear opening pore diameter range 1.5mm；
Step 5, the polyurethane organic foam carrier that step 4 obtains is placed in the dipping sizing agent of step 3, is 60 DEG C of bars in temperature
Impregnate 7min under part, repeated impregnations 7 times, obtain impregnating base substrate B after 40 DEG C of drying 6h；
Step 6, the dipping base substrate B that step 3 obtains is raised to 160 DEG C with 4 DEG C/min from room temperature, 7 DEG C/min rises to from 160 DEG C
320 DEG C, 2.5 DEG C/min rises to 650 DEG C from 320 DEG C, rises to 850 DEG C with 8 DEG C/min, is incubated 6h, last furnace cooling obtains
To porous biphasic calcium phosphate support C；
Step 7, the silica gel that step 6 is obtained and distilled water are 1 in mass ratio:3 it is well mixed obtain aqueous solution of silica gel, by step
6 obtained porous biphasic calcium phosphate support C are placed in aqueous solution of silica gel, soak 10h at room temperature, taking-up is fully drawn with filter paper
Excess surface solution, then 30 DEG C of drying bracket 4h；
Step 8, the support handled through step 7 is raised to 180 DEG C with 4 DEG C/min from room temperature, 7 DEG C/min rises to 330 from 180 DEG C
DEG C, 6h is incubated, last furnace cooling to room temperature, obtains porous SiO2/ biphasic calcium phosphate compound rest.
Above in association with accompanying drawing to the present invention embodiment be explained in detail, but the present invention be not limited to it is above-mentioned
Embodiment, can also be before present inventive concept not be departed from those of ordinary skill in the art's possessed knowledge
Put that various changes can be made.
Claims (2)
- A kind of 1. porous SiO of bone tissue engineer2The preparation method of/biphasic calcium phosphate compound rest, it is characterised in that specific steps It is as follows：Step 1, calcium carbonate and phosphoric acid are mixed according to stoichiometry Ca/P=1.5 and stoichiometry Ca/P=1.67 respectively first Bata-tricalcium phosphate and hydroxyapatite is prepared in precipitation respectively, according to mass ratio is 70 by bata-tricalcium phosphate and hydroxyapatite ~85：15~30 well mixed obtain biphasic calcium phosphate presoma powder；Step 2, by biphasic calcium phosphate presoma powder that step 1 obtains be 1000~1200 DEG C in temperature at calcine 8-10h, obtain To biophasic calcium phosphate ceramic powder；Step 3, by the biophasic calcium phosphate ceramic powder that step 2 obtains according to mass ratio be 1:3~1:7 mix with egg binding agent Conjunction uniformly obtain slurry A, by slurry A according to volume ratio be 2:1~2:7 are added in distilled water, are uniformly mixing to obtain dipping slurry Material；Step 4, the polyurethane organic foam carrier with regular through hole is prepared using Laser Processing forming technique；Step 5, the polyurethane organic foam carrier that step 4 obtains is placed in the dipping sizing agent of step 3, is 30~60 in temperature 1~7min is impregnated under the conditions of DEG C, repeated impregnations 1~7 time, obtains impregnating base substrate B after drying；Step 6, dipping base substrate B that step 3 obtains is raised to 130~160 DEG C with 1~4 DEG C/min from room temperature, 4~7 DEG C/min from 130~160 DEG C rise to 280~320 DEG C, and 0.5~2.5 DEG C/min rises to 550~650 DEG C from 280~320 DEG C, with 4~8 DEG C/min rises to 800~850 DEG C, 3~6h is incubated, last furnace cooling obtains porous biphasic calcium phosphate support C；Step 7, the silica gel that step 6 is obtained and distilled water are 1 in mass ratio:1~1:3 it is well mixed obtain aqueous solution of silica gel, The porous biphasic calcium phosphate support C that step 6 is obtained is placed in aqueous solution of silica gel, soaks 4~10h, taking-up filter at room temperature The abundant adsorption surface redundant solution of paper, then drying bracket；Step 8, the support handled through step 7 is raised to 150~180 DEG C with 1~4 DEG C/min from room temperature, 4~7 DEG C/min is from 150 ~180 DEG C rise to 300~330 DEG C, are incubated 3~6h, last furnace cooling to room temperature, obtain porous SiO2/ biphasic calcium phosphate Compound rest.
- 2. the porous SiO of bone tissue engineer according to claim 12The preparation method of/biphasic calcium phosphate compound rest, its It is characterised by：0.6~2mm of polyurethane organic foam carrier clear opening pore diameter range in the step 4.
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