CN110201224A - A kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite and preparation method thereof - Google Patents
A kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite and preparation method thereof Download PDFInfo
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- CN110201224A CN110201224A CN201910441305.9A CN201910441305A CN110201224A CN 110201224 A CN110201224 A CN 110201224A CN 201910441305 A CN201910441305 A CN 201910441305A CN 110201224 A CN110201224 A CN 110201224A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 63
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 63
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000004696 Poly ether ether ketone Substances 0.000 title claims abstract description 60
- 229920002530 polyetherether ketone Polymers 0.000 title claims abstract description 60
- 239000011350 dental composite resin Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims description 12
- 239000002131 composite material Substances 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 24
- 238000004140 cleaning Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 7
- 239000000835 fiber Substances 0.000 claims description 7
- 238000001746 injection moulding Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- -1 Ether ether ketone Chemical class 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000010981 drying operation Methods 0.000 claims description 5
- 239000010410 layer Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 239000002356 single layer Substances 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000007306 functionalization reaction Methods 0.000 abstract description 7
- 239000002346 layers by function Substances 0.000 abstract description 5
- 238000006277 sulfonation reaction Methods 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 3
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 239000012567 medical material Substances 0.000 abstract description 3
- 230000002188 osteogenic effect Effects 0.000 abstract description 3
- 238000012876 topography Methods 0.000 abstract description 3
- 238000005253 cladding Methods 0.000 abstract description 2
- 238000011017 operating method Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 11
- 244000137852 Petrea volubilis Species 0.000 description 9
- 210000000988 bone and bone Anatomy 0.000 description 9
- 238000005498 polishing Methods 0.000 description 8
- 230000009286 beneficial effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 229920000570 polyether Polymers 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000011164 ossification Effects 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
- 210000001519 tissue Anatomy 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 239000004053 dental implant Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 230000010148 water-pollination Effects 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002138 osteoinductive effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002023 wood Substances 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
- A61L27/02—Inorganic materials
- A61L27/08—Carbon ; Graphite
-
- 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
- A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/303—Carbon
-
- 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
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
-
- 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
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/02—Methods for coating medical devices
-
- 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
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Transplantation (AREA)
- Dermatology (AREA)
- Medicinal Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention provides a kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composites, carbon fiber reinforced polyetheretherketonecomposite composite material is surface-treated by sulfonation and the functionalization of graphene oxide to obtain the surface-functionalized carbon fiber reinforced polyetheretherketonecomposite composite material of cladding graphene oxide functional layer, functional layer is strong with basal body binding force, it is not easily to fall off, and it can effectively change the surface geometry and surface functional group composition of carbon fiber reinforced polyetheretherketonecomposite composite material, assign carbon fiber reinforced polyetheretherketonecomposite composite material completely new surface topography and surface characteristic, promote its biocompatibility and osteogenic, and then promote its application in terms of medical material, it is important that operating method of the invention is simple and easy, it is surface-treated mild condition, suitable for large-scale promotion and application, medical value with higher.
Description
Technical field
The present invention relates to medical material tech fields, in particular to dental material technical field, more particularly to
A kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite and preparation method thereof.
Background technique
It is non-renewable due to tooth, once damage can only select planting body material to be repaired or substituted, existing skill
The dental implant materials clinically used in art are mostly titanium metal implants material, but elasticity modulus between titanium and bone tissue
Differ greatly, and there is metal sensitization, influences normal use.
Polyether-ether-ketone is the thermoplastic special engineering plastic of a kind of all aromatic hemicrystalline, with excellent resistance to height
The performances such as warm, wear-resistant, hydrolysis, resistant to chemical etching, are readily extruded and are injection moulded, and processing performance is excellent, shaping efficiency compared with
Height, so that this quasi polymer has widely in fields such as aerospace, automobile manufacture, electric, medical and food processings
Using, it is very wide in dental field prospect, although the more other high molecular materials of its mechanical strength are good, in order to more preferably meet
The practical application of many complex environments and harsh conditions, carbon fiber are usually used to as a kind of common fibre reinforced materials
Polyetheretherketonepolymer polymer is enhanced, the high purity carbon fiberreinforced polyether-ether-ketone composite material with excellent mechanical performance is obtained.
Technology of the high purity carbon fiberreinforced polyether-ether-ketone composite material as medical planting body is proposed in the prior art, due to its springform
Amount is slightly above bone, more preferably with the matching of bone tissue, does not easily cause stress shielding.But high purity carbon fiberreinforced polyether-ether-ketone composite wood
Material is a kind of inert material, and surface-active is low, and bioconjugation performance, bone formation performance are poor, it is difficult to which it is special that satisfaction has surface property
It is required that medical-dental implant field.
Therefore how to provide a kind of high show activity, bioconjugation ability and the strong high purity carbon fiberreinforced polyethers ether of bone formation performance
Ketone composite material is those skilled in the art's urgent problem to be solved.
Summary of the invention
In view of this, leading to the present invention provides a kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite
The functionalization for crossing sulfonation and graphene oxide is surface-treated to obtain carbon fiber reinforced polyetheretherketonecomposite composite material
The surface-functionalized carbon fiber reinforced polyetheretherketonecomposite composite material for coating graphene oxide functional layer, improves its overall performance.
In order to achieve the above object, the present invention adopts the following technical scheme:
Firstly, the present invention provides a kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite, including carbon
Fiber reinforcement polyether-ether-ketone forming composite and graphene oxide layer, the graphene oxide layer are uniformly wrapped on the carbon fiber
Tie up reinforced polyether ether ketone forming composite surface.
Preferably, carbon fiber content is 0wt%~60wt% in the carbon fiber reinforced polyether-ether-ketone forming composite.
The beneficial effect of above-mentioned optimal technical scheme is: carbon fiber is in the content range, obtained enhanced polyether-ether-ketone
Composite material has excellent mechanical property, and elasticity modulus is slightly above bone, best with the matching of bone tissue, does not easily cause and answers
Power shielding.It is easy to generate damage to surrounding bone higher than the content.Insufficient lower than the content material intensity, mechanical property is bad.
Preferably, the carbon fiber reinforced polyether-ether-ketone forming composite is injection molding, forming temperature 350 ± 40
℃。
The beneficial effect of above-mentioned optimal technical scheme is: the excessively high one side of temperature influences mode of appearance, generates gas under high temperature
Body, plastic generate bubble, overlap, coking etc.；On the other hand, it affects the mechanical properties, high temperature makes plastic elasticity modulus become smaller, plastic
Become fragile；The too low then plastic surface of temperature generates defect, and pit, crack influences performance.
Preferably, the polymer beads partial size of the polyether-ether-ketone in the carbon fiber reinforced polyether-ether-ketone forming composite
It is 10~100 μm.
The beneficial effect of above-mentioned optimal technical scheme is: the polymer beads in the particle size range are conducive to injection molding,
And product cost is low, work efficiency is high.
The present invention also provides a kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composites as described above
Preparation method, comprising the following steps:
(1) it polishes carbon fiber reinforced polyether-ether-ketone forming composite surface, then cleaning, drying；
(2) by the step (1), treated that carbon fiber reinforced polyether-ether-ketone forming composite is placed in sulfuric acid solution
It takes out after being soaked for a period of time and is rinsed with deionized water, immerse in deionized water save later；
(3) it takes out the step (2) treated carbon fiber reinforced polyether-ether-ketone forming composite and dry, then set
10~15min is impregnated in graphene oxide solution, then takes out to be placed in 60~120 DEG C of drying boxes and dry, and is repeated in oxygen
It is impregnated in graphite alkene solution and drying operation 2~5 times, last surface-functionalized carbon fiber reinforced polyether-ether-ketone tooth obtained by drying
Section's composite material.
Preferably, it is polished in the step (1) using sand paper, specific grinding turn are as follows: the polishing of 120 mesh sand paper, 600
The polishing of mesh sand paper, the polishing of 2000 mesh sand paper, the polishing of 3000 mesh sand paper, the standard polished every time is smooth round and smooth to be polishing to, must not
There is scratch, recess etc..
Preferably, the cleaning in the step (1) be successively using acetone, dehydrated alcohol, deionized water cleaning, and it is each clear
Wash 15~30min.
The beneficial effect of above-mentioned optimal technical scheme is: successively being cleaned using the solvent of different function and is completely removed carbon fiber
Tie up reinforced polyether ether ketone forming composite surface contaminant and remaining organic solution.
Preferably, the mass fraction of the sulfuric acid solution in the step (2) be 50%~98%, and soaking time be 2~
30min。
The beneficial effect of above-mentioned optimal technical scheme is: the sulfuric acid concentration within the scope of this can effectively change carbon fiber increasing
The surface geometry of strong polyether-ether-ketone composite material, increases its surface pore, assigns its completely new surface topography, crosses low concentration
Surface topography improvement is undesirable.
Preferably, the concentration of the graphene oxide solution is 0.1wt%~5.0wt%.
The beneficial effect of above-mentioned optimal technical scheme is: using the concentration range graphene solution, graphene energy and matrix
It combines closely, not easily to fall off, the surface functional group for effectively changing carbon fiber reinforced polyetheretherketonecomposite composite material is constituted, and it is complete to assign it
New surface characteristic promotes its biocompatibility and osteogenic.
Preferably, the graphene oxide is one of single layer, multilayer graphene oxide or mixture.
It can be seen via above technical scheme that compared with prior art, the present invention provides a kind of surface-functionalized carbon fibers
Reinforced polyether ether ketone dental composite is tieed up, by sulfonation and the functionalization of graphene oxide to fibre reinforced polyethers ether
Ketone composite material is surface-treated to obtain the surface-functionalized fibre reinforced polyethers of cladding graphene oxide functional layer
Ether ketone composite material, functional layer is strong with basal body binding force, not easily to fall off, and it is compound effectively to change carbon fiber reinforced polyether-ether-ketone
The surface geometry and surface functional group of material are constituted, and assign carbon fiber reinforced polyetheretherketonecomposite composite material completely new surface shape
Looks and surface characteristic promote its biocompatibility and osteogenic, and then promote its application in terms of medical material, it is important that
Operating method of the invention is simple and easy, is surface-treated mild condition, is suitable for large-scale promotion and application, medicine with higher
Value.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 attached drawing is the carbon fiber reinforced polyether-ether-ketone forming composite surface texture figure of comparative example 1 of the present invention；
Fig. 2 attached drawing is the surface texture figure of carbon fiber reinforced polyether-ether-ketone forming composite after sulfonation of the present invention processing；
Fig. 3 attached drawing is that carbon fiber reinforced polyether-ether-ketone dentistry of the present invention after surface of graphene oxide functionalization is multiple
The surface texture figure of condensation material；
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
The preparation method of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite specifically includes the following steps:
(1) at 360 DEG C injection molding carbon fiber-containing 20wt% carbon fiber reinforced polyether-ether-ketone forming composite, it
It successively then successively uses acetone using 120 mesh, 600 mesh, 2000 mesh, 3000 mesh sand paper polishing surface afterwards, dehydrated alcohol, go
Ionized water cleaning, and each cleaning 15min cleaning, be placed in 60 DEG C of drying boxes and dry；
(2) by step (1), treated that carbon fiber reinforced polyether-ether-ketone forming composite is placed in mass fraction 80%
It takes out after impregnating 10min in sulfuric acid solution and is rinsed with deionized water, immerse in deionized water impregnate 10min later；
(3) the carbon fiber reinforced polyether-ether-ketone forming composite that takes out that step (2) treated and in 60 DEG C of oven dryings
12h is subsequently placed in the graphene oxide solution of 1wt% and impregnates 10min, then takes out to be placed in 100 DEG C of drying boxes and dry,
It repeats to impregnate in graphene oxide solution and drying operation 4 times, last surface-functionalized fibre reinforced polyethers obtained by drying
Ether ketone dental composite.
Embodiment 2
The preparation method of surface-functionalized polyether-ether-ketone dental composite specifically includes the following steps:
(1) the injection molding polyether-ether-ketone forming composite at 350 DEG C successively uses 120 mesh, 600 mesh, 2000 later
Mesh, 3000 mesh sand paper polishing surface, then successively using acetone, dehydrated alcohol, deionized water cleaning, and each cleaning 20min is clear
Wash, be placed in 60 DEG C of drying boxes and dry；
(2) by step (1), treated that polyether-ether-ketone forming composite is placed in the sulfuric acid solution of mass fraction 50%
It takes out after impregnating 30min and is rinsed with deionized water, immerse in deionized water impregnate 10min later；
(3) the polyether-ether-ketone forming composite that takes out that step (2) treated and in 60 DEG C of oven drying 12h, then sets
10min is impregnated in the graphene oxide solution of 5wt%, then takes out to be placed in 80 DEG C of drying boxes and dry, repetition is aoxidizing
It is impregnated in graphene solution and drying operation 5 times, last surface-functionalized polyether-ether-ketone dental composite obtained by drying.
Embodiment 3
The preparation method of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite specifically includes the following steps:
(1) at 390 DEG C injection molding carbon fiber-containing 60wt% carbon fiber reinforced polyether-ether-ketone forming composite, it
It successively then successively uses acetone using 120 mesh, 600 mesh, 2000 mesh, 3000 mesh sand paper polishing surface afterwards, dehydrated alcohol, go
Ionized water cleaning, and each cleaning 20min cleaning, be placed in 60 DEG C of drying boxes and dry；
(2) by step (1), treated that carbon fiber reinforced polyether-ether-ketone forming composite is placed in mass fraction 98%
It takes out after impregnating 2min in sulfuric acid solution and is rinsed with deionized water, immerse in deionized water impregnate 10min later；
(3) the carbon fiber reinforced polyether-ether-ketone forming composite that takes out that step (2) treated and in 60 DEG C of oven dryings
12h is subsequently placed in the graphene oxide solution of 0.1wt% and impregnates 10min, then takes out to be placed in 100 DEG C of drying boxes and dry
It is dry, it repeats to impregnate in graphene oxide solution and drying operation 3 times, last surface-functionalized fibre reinforced obtained by drying is poly-
Ether ether ketone dental composite.
Comparative example 1
The carbon fiber reinforced polyether-ether-ketone forming composite of injection molding carbon fiber-containing 60wt% at 390 DEG C, later
Successively using 120 mesh, 600 mesh, 2000 mesh, 3000 mesh sand paper polish surface, then successively using acetone, dehydrated alcohol, go from
The cleaning of sub- water, and each cleaning 20min cleaning, be placed in 60 DEG C of drying boxes and dry, obtain carbon fiber reinforced polyether-ether-ketone at
Type composite material.
Test example
The material of above-described embodiment 1-3 and comparative example 1 are tested for the property, test process and result are as follows:
1) Surface Characterization is carried out to embodiment 1 and comparative example 1 respectively as a result as illustrated in the accompanying drawings from 1 to 3 to be shown by attached drawing 1-3
Compared to the material of comparative example 1, in technical solution of the present invention, it can make material surface that there is porous performance after sulfonation processing,
Convenient for the attachment of material, after graphene oxide solution immersion treatment, graphene oxide uniformly and is firmly attached to substrate table
Face, it was demonstrated that required product has been made according to the technical solution of the present invention.
2) hydrophilicity test is carried out to embodiment 1-3 and comparative example material 1:
Contact angle test: hydrophily detection is carried out to sample using contact angle measurement, Static Water is measured using sessile drop method
Contact angle, measures the surface hydrophilicity of sample, and every group of sample repeats detection 3 times and be averaged.The experimental results showed that embodiment 1-
3 contact angle is far smaller than 90 °, has hydrophily, shows that it can be soaked by tissue liquid, is in close contact with bone tissue,
And the carbon fiber reinforced polyetheretherketonecomposite composite material of comparative example 1 be it is hydrophobic, that is, show in through the invention using graphene oxide
To the functionalization of material surface, the hydrophilicity of material is effectively improved.
3) experiment of induced osteogenesis performance is carried out to embodiment 1-3 and comparative example material 1, embodiment 1-3 osteoinductive can be good
It is good, and combine closely with bone tissue, comparative example is unable to compact growth with bone tissue and exists without obvious self-bone grafting ability
Together.Illustrate in the present invention using graphene oxide to the ideal synosteosis of imparting material after the functionalization of material surface
Effect；
4) bio-toxicity analysis is carried out to embodiment 1-3 and comparative example material 1, cell and tissue do not occur not as the result is shown
Good reaction, growth and development is good, illustrates cell-free and tissue toxicity of the invention, and surface-modified rear material has good biology
Compatibility；
5) mechanical performance and Mechanics Performance Testing are carried out to embodiment 1-3 and comparative example material 1, there is excellent mechanicalness
Can and mechanical property, and difference is little, illustrates the present invention using graphene oxide to still may be used after the functionalization of material surface
Reach ideal mechanical performance and mechanical property, meets planting body intensity needs.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (8)
1. a kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite, which is characterized in that including fibre reinforced
Polyether-ether-ketone forming composite and graphene oxide layer, it is poly- that the graphene oxide layer is uniformly wrapped on the fibre reinforced
Ether ether ketone forming composite surface.
2. a kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite according to claim 1, feature
It is, carbon fiber content is 0wt%~60wt% in the carbon fiber reinforced polyether-ether-ketone forming composite.
3. a kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite according to claim 2, feature
Be, the carbon fiber reinforced polyether-ether-ketone forming composite be injection molding, 350 ± 40 DEG C of forming temperature.
4. a kind of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite as claimed in any one of claims 1 to 3
Preparation method, which comprises the following steps:
(1) it polishes carbon fiber reinforced polyether-ether-ketone forming composite surface, then cleaning, drying；
(2) by the step (1), treated that carbon fiber reinforced polyether-ether-ketone forming composite is placed in sulfuric acid solution impregnates
It takes out after a period of time and is rinsed with deionized water, immerse in deionized water save later；
(3) it takes out the step (2) treated carbon fiber reinforced polyether-ether-ketone forming composite and dry, be subsequently placed in oxygen
10~15min is impregnated in graphite alkene solution, then takes out to be placed in 60~120 DEG C of drying boxes and dry, and is repeated in oxidation stone
It is impregnated in black alkene solution and drying operation 2~5 times, last surface-functionalized carbon fiber reinforced polyether-ether-ketone dentistry obtained by drying is multiple
Condensation material.
5. a kind of preparation side of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite according to claim 4
Method, which is characterized in that cleaning in the step (1) be successively using acetone, dehydrated alcohol, deionized water cleaning, and it is each clear
Wash 15~30min.
6. a kind of preparation side of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite according to claim 4
Method, which is characterized in that sulfuric acid solution mass fraction in the step (2) is 50%~98%, and soaking time be 2~
30min。
7. a kind of preparation side of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite according to claim 4
Method, which is characterized in that the concentration of the graphene oxide solution is 0.1wt%~5.0wt%.
8. a kind of preparation side of surface-functionalized carbon fiber reinforced polyether-ether-ketone dental composite according to claim 4
Method, which is characterized in that the graphene oxide is one of single layer, multilayer graphene oxide or mixture.
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