CN104974467A - Nano-hydroxyapatite/polyether-ether-ketone composite material and bone repair body as well as preparation method and application thereof - Google Patents

Nano-hydroxyapatite/polyether-ether-ketone composite material and bone repair body as well as preparation method and application thereof Download PDF

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CN104974467A
CN104974467A CN201510437676.1A CN201510437676A CN104974467A CN 104974467 A CN104974467 A CN 104974467A CN 201510437676 A CN201510437676 A CN 201510437676A CN 104974467 A CN104974467 A CN 104974467A
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polyether
ether
bone
preparation
powder
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徐东
马旭辉
魏杰
蔡亮
张珏
宋文华
马瑞
汤晓峰
乔志龙
周兵
付俊祺
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Polymer Science Shenzhen New Materials Co Ltd
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Polymer Science Shenzhen New Materials Co Ltd
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Abstract

The invention discloses a nano-hydroxyapatite/polyether-ether-ketone composite material and a bone repair body as well as a preparation method and application thereof. The preparation method of the composite material comprises the following steps: uniformly mixing 30-35wt% of 200nm-1mu m hydroxyapatite powder and 65-70wt% of 5-15mu m polyether-ether-ketone powder to obtain mixed powder; and processing the mixed powder and moulding to obtain the composite material. The composite material has good biocompatibility and bioactivity as well as mechanical properties matching the bone tissue, effectively prevents the stress shielding effect, and can stimulate bone growth, accelerate bone healing, shorten the healing time of the injury after material implantation of bone and reduce the probability of second operation. The preparation technology of the composite material can be adjusted to prepare bone repair bodies different in shape, specification and mechanical properties to meet the clinical needs. Inflammatory reaction is avoided after the implantation of the bone repair bodies, the mechanical properties are matched with human bone, negative effects such as bone repair material loosening and bone resorption are prevented, and the clinical needs for bone repair can be met.

Description

Nanometer hydroxyapatite/polyether-ether-ketone composite material, bone prosthesis and its preparation method and application
Technical field
The present invention relates to polyetheretherketone field of compound material, particularly relate to a kind of nanometer hydroxyapatite/Peek Composite Material and Preparation Method and application thereof, especially also relating to a kind of bone prosthesis must apply and preparation method thereof.
Background technology
Along with the generally application of bone implant material, modern bone implant material is more and more higher for the requirement of its biological function, and Integrated implant concept has been widely deployed in the middle of the evaluation of bone implant.
And be widely used in clinical titanium base and ceramic base bone implant material at present, all there is the shortcoming that some self are difficult to overcome, such as, the mechanical strength of metal and ceramic bone implant material exceeds osseous tissue far away, easily stress shielding is there is after being implanted, and then cause bone resorption, osteanabrosis, and cause further implant loosen cause a series of complication.Polyether-ether-ketone (polyetheretherketone, PEEK) not only has excellent biocompatibility and biologically stable, and fatigue resistance is good, erosion resistance is strong; The Young's modulus of artificial bone manufactured with PEEK and osseous tissue match, and it has high strength, hard wear resistant and physical strength is not degenerated through sterilizing repeatedly.PEEK oneself obtain FDA (Food and Drug Administration, U.S. food Drug Administration) certification and be designated as " best long-term bone grafting material ", the U.S. has developed the long-term osteoarthrosis, elbow joint etc. implanted with PEEK.Therefore, than PEEK, there is clear superiority with metal and ceramic phase, be more suitable for carrying out long-term et al. Ke.But PEEK is lower because of its biological activity, not easily forms synostosis.
Hydroxyapatite (Ca 10(PO 4) 6(OH) 2, HA) and be the main inorganic composition of vertebrate skeletal, tooth, structure is also closely, in nano microcrystalline state, its surface has polarity, has stronger avidity with body tissue, forming firmly synostosis with osseous tissue, is generally acknowledged implantation of good performance.But its fragility is large, intensity is low and limit its use, and this patent in the compound of PEEK by it, is prepared a kind of matrix material with excellent mechanical performances and biocompatibility, had good potential applicability in clinical practice.
Summary of the invention
Technical problem to be solved by this invention: overcome existing bone renovating material mechanical compatibility and do not mate with bone, and cause stress shielding and cause material to loosen and bone resorption, cause knitting speed excessively slow, or shortage biological activity, cannot with formation synosteotic defect, a kind of nanometer hydroxyapatite/Peek Composite Material and Preparation Method and application are provided, and a kind of bone prosthesis obtained by this nanometer hydroxyapatite/polyether-ether-ketone composite material and preparation method thereof.This nanometer hydroxyapatite/polyether-ether-ketone composite material has good biocompatibility and biological activity, has with osseous tissue the mechanical compatibility comparatively mated, can stimulation of bone growth, and accelerated bone heals, and reduces the healing time of wound after bone implant material.This nanometer hydroxyapatite/polyether-ether-ketone composite material simple for process, the preparation technology of this nanometer hydroxyapatite/polyether-ether-ketone composite material of adjustable prepares the bone prosthesis of different shapes, specification and mechanical property to adapt to clinical user demand.This bone prosthesis has good, biocompatibility, biomechanics of bone consistency, can shorten bone healing time, its intensity is high, corrosion resistance good, long service life.Can not be caused inflammation after the implantation of this bone prosthesis reaction, and the mechanical properties such as its Young's modulus, toughness and breaking tenacity are mated with people's bone photo, the bone renovating material that stress shielding can not be caused to cause loosens and the negative effect such as bone resorption, can meet the clinical needs for Bone Defect Repari.
The present invention is achieved through the following technical solutions above-mentioned technique effect.
The nanometer hydroxyapatite used in the present invention is prepared from by sol-gel method.With four water-calcium nitrate and trimethyl phosphite 99 for raw material, water and dehydrated alcohol are solvent, are under the condition of 7.5 after mix and blend 48h at pH, and after 190 DEG C of dry 2h, 600 DEG C of calcining 1h are prepared from.
The invention provides a kind of preparation method of nanometer hydroxyapatite/polyether-ether-ketone composite material, it comprises the steps: raw material: polyether-ether-ketone powder and hydroxyapatite powder mix powdered; By it machine-shaping, to obtain final product; Wherein, the consumption of nanometer hydroxyapatite accounts for 30% ~ 35% of raw material gross weight, and the consumption of polyether-ether-ketone accounts for 65% ~ 70% of raw material gross weight; The particle diameter of nanometer hydroxyapatite powder is 200nm ~ 1 μm, and the particle diameter of polyether-ether-ketone powder is 5 μm ~ 15 μm.
Wherein, the particle diameter of described nanometer hydroxyapatite is preferably 200nm ~ 1 μm.
Wherein, the particle diameter of described polyether-ether-ketone powder is preferably 5 μm ~ 15 μm.
Wherein, the method for described mixing and condition are method and the condition of this area routine, are as the criterion to mix.Described mixing comparatively should be carried out in mixing machine.
Wherein, the method for described machine-shaping and condition can be method and the condition of this area routine.Described machine-shaping is comparatively preferably injection moulding or molding sintering is shaping.
The method of described injection moulding and condition can be method and the condition of this area routine.Described injection moulding is preferably carried out in injection moulding machine.The temperature of described injection moulding is preferably 350 DEG C ~ 370 DEG C.The pressure of described injection moulding is preferably 40MPa ~ 80MPa.
The method that described molding sintering is shaping and condition can be method and the condition of this area routine.Described molding sintering is shaping preferably to be undertaken by following working method: by described mixed powder compression moulding, and heat up sintering; The speed of described intensification is 3 DEG C/min; The temperature of described sintering is 355 DEG C ~ 375 DEG C; The soaking time of described sintering is 90 ~ 180 minutes, is preferably 120 minutes.
In the present invention, the shape of the nanometer hydroxyapatite/polyether-ether-ketone composite material obtained after not limiting described machine-shaping.As described in machine-shaping mould used be the mould of bone prosthesis product, then described hydroxyapatite/polyether-ether-ketone composite material directly can be used as bone prosthesis.If mould used in described machine-shaping is not the mould of bone prosthesis product, then by the operation of follow-up processing treatment, the operations such as such as grinding, mechanical workout, to prepare the bone prosthesis of desired shape.
Present invention also offers a kind of nanometer hydroxyapatite/polyether-ether-ketone composite material obtained by above-mentioned preparation method.
In the present invention, described nanometer hydroxyapatite/polyether-ether-ketone composite material is a kind of matrix material of nanometer hydroxyapatite reinforced polyether ether ketone.
Present invention also offers the application of described nanometer hydroxyapatite/polyether-ether-ketone composite material in bone prosthesis.
Wherein, described bone prosthesis is spinal bone dummy or tooth implant.Described spinal bone dummy, also referred to as Invasive lumbar fusion device, comprises strength Invasive lumbar fusion device and chest/waist Invasive lumbar fusion device.
Present invention also offers a kind of preparation method of bone prosthesis, it comprises the steps: raw material: polyether-ether-ketone powder and hydroxyapatite powder mix powdered; By it machine-shaping, to obtain final product; Wherein, the consumption of nanometer hydroxyapatite accounts for 30% ~ 35% of raw material gross weight, and the consumption of polyether-ether-ketone accounts for 65% ~ 70% of raw material gross weight; The particle diameter of nanometer hydroxyapatite powder is 200nm ~ 1 μm, and the particle diameter of polyether-ether-ketone powder is 5 μm ~ 15 μm.
Wherein, the particle diameter of described bioactivity glass powder is preferably 200nm ~ 1 μm.
Wherein, the particle diameter of described polyether-ether-ketone powder is preferably 5 μm ~ 15 μm.
Wherein, the method for described mixing and condition can be method and the condition of this area routine, are as the criterion to mix.Described mixing is preferably carried out in mixing machine.
Wherein, the mould of described bone prosthesis product is the conventional mould used when preparing bone prosthesis product, is preferably the mould of spinal bone dummy or the mould of tooth implant.Described spinal bone dummy, also referred to as Invasive lumbar fusion device, comprises strength Invasive lumbar fusion device and chest/waist Invasive lumbar fusion device.
Wherein, the method for described machine-shaping and condition can be method and the condition of this area routine.Described machine-shaping is preferably that injection moulding or molding sintering are shaping.
The method of described injection moulding and condition can be method and the condition of this area routine.Described injection moulding is preferably carried out in injection moulding machine.The temperature of described injection moulding is preferably 350 DEG C ~ 370 DEG C.The pressure of described injection moulding is preferably 40MPa ~ 80MPa.
The method that described molding sintering is shaping and condition can be method and the condition of this area routine.Described molding sintering is shaping preferably to be undertaken by following working method: by described mixed powder compression moulding, then heat up, sinter molding; The speed of described intensification is 3 DEG C/min; The temperature of described sintering is 355 DEG C ~ 375 DEG C; The soaking time of described sintering is 90 ~ 180 minutes, is preferably 120 minutes.
In the present invention, in the preparation method of described bone prosthesis, after described machine-shaping, also carry out surface coarsening process.Described surface coarsening process is preferably carried out in the steps below: use surface coarsening machine, carry out surface coarsening with hydroapatite particles to the block that described machine-shaping obtains, and forms to described block surface the porous surface that aperture is 100 μm ~ 300 μm.The particle diameter of described hydroapatite particles is preferably 50 μm ~ 200 μm.
Present invention also offers a kind of bone prosthesis obtained by above-mentioned preparation method.
Wherein, described bone prosthesis is spinal bone dummy or tooth implant.Described spinal bone dummy, also referred to as Invasive lumbar fusion device, comprises strength Invasive lumbar fusion device and chest/waist Invasive lumbar fusion device.
In the present invention, the shape of described bone prosthesis can according to actual needs by selecting different moulds to change with specification.
In the present invention, the mechanical performance index of described bone renovating material is roughly as follows:
Young's modulus is 3.2GPa ~ 7.5GPa, and ultimate compression strength is 125MPa ~ 163GPa, and tensile strength is 82MPa ~ 112MPa, and bending strength is 85MPa ~ 114MPa.
On the basis meeting this area general knowledge, above-mentioned each optimum condition, can arbitrary combination, obtains the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material are all commercially.
Positive progressive effect of the present invention is:
(1) nanometer hydroxyapatite/polyether-ether-ketone composite material of the present invention is simple for process, and the preparation technology of this nanometer hydroxyapatite/polyether-ether-ketone composite material of adjustable prepares the bone prosthesis of different shapes, specification and mechanical property to meet clinical demand.
(2) surface texture technology is adopted to process composite material molded body surface, coarse structure is formed at composite material surface, have larger specific surface area, osteocyte/osseous tissue and blood vessel are easily grown in porous hole, make osseous tissue and implant more easily form synostosis.
(3) nanometer hydroxyapatite/polyether-ether-ketone composite material of the present invention has good biological activity and biocompatibility, good mechanical compatibility is had with osseous tissue, can stimulation of bone growth, accelerated bone heals, and reduces the healing time after bone implant material.
(4) bone prosthesis of the present invention has good biocompatibility, biological activity, biomechanics of bone consistency and germ resistance, can shorten bone healing time.Can not be caused inflammation after using this bone prosthesis to implant reaction, and the mechanical properties such as its Young's modulus, toughness and breaking tenacity are mated with people's bone photo, the bone renovating material that stress shielding can not be caused to cause loosens and the negative effect such as bone resorption, can meet the clinical needs for Bone Defect Repari.
Accompanying drawing explanation
In order to be illustrated more clearly in technical scheme of the present invention, be briefly described to the accompanying drawing used required in embodiment below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the TEM picture of nanometer hydroxyapatite used in patent of the present invention.
Fig. 2 is the shape picture of the nanometer hydroxyapatite/polyether-ether-ketone composite material sample (Ф 10 × 2mm) used in the cytotoxicity test experiments of effect example 2.
Fig. 3 is the hydroxyapatite/polyether-ether-ketone composite material optical density(OD) figure carrying out cytotoxicity experiment in effect example 2.
Fig. 4 is the sample photo of bone prosthesis in effect example 3 (embodiment 7 sample).
Fig. 5 is at the macro morphology photo of dog femoral implantable bone dummy after 3 months in effect example 3.
Fig. 6 and Fig. 7 is that the bone prosthesis in effect example 3 implants the tissue slice of dog femoral defect place after 3 months.
Embodiment
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or selects according to catalogue.
Embodiment 1
The preparation method of hydroxyapatite/polyether-ether-ketone composite material, it comprises the steps:
By raw material: 3kg (30wt%) nanometer hydroxyapatite powder (particle diameter is 500nm) and 7kg (70wt%) polyether-ether-ketone powder (particle diameter is 10 μm) Homogeneous phase mixing in mixing machine, obtain mixed powder; Then with injection moulding machine by mixed powder injection moulding (using the mould of non-bone prosthesis product), to obtain final product; Wherein, the temperature of injection moulding is 365 DEG C; The pressure of injection moulding is 40MPa.The mechanical property of this nanometer hydroxyapatite/polyether-ether-ketone composite material is in table 1.
Embodiment 2
The preparation method of nanometer hydroxyapatite/polyether-ether-ketone composite material, it comprises the steps:
By raw material: 3kg (30wt%) nanometer hydroxyapatite powder (particle diameter is 500nm) and 7kg (70wt%) polyether-ether-ketone powder (particle diameter is 10 μm) carry out raw material Homogeneous phase mixing in mixing machine, obtain mixed powder; Then with injection moulding machine by mixed powder injection moulding (using the mould of non-bone prosthesis product), to obtain final product; Wherein, the temperature of injection moulding is 370 DEG C; The pressure of injection moulding is 75MPa.The mechanical property of this hydroxyapatite/polyether-ether-ketone composite material is in table 1.
Embodiment 3
The preparation method of bone prosthesis, it comprises the steps:
By raw material: 3.5kg (35wt%) nanometer hydroxyapatite powder (particle diameter is 500nm) and 6.5kg (65wt%) polyether-ether-ketone powder (particle diameter is 15 μm) carry out raw material Homogeneous phase mixing in mixing machine, obtain mixed powder; Then with injection moulding machine by mixed powder injection moulding in the mould of dog alveolar repair body, to obtain final product; Wherein, the temperature of injection moulding is 360 DEG C; The pressure of injection moulding is 60MPa.The mechanical property of this bone prosthesis is in table 1.
Embodiment 4
The preparation method of hydroxyapatite/polyether-ether-ketone composite material, it comprises the steps:
By raw material: 3kg (30wt%) nanometer hydroxyapatite powder (particle diameter is 500nm) and 7kg (70wt%) polyether-ether-ketone powder (particle diameter is 12 μm) carry out raw material Homogeneous phase mixing in mixing machine, obtain mixed powder; Then with mould by mixed powder compression moulding (using the mould of non-bone prosthesis product), then heat up in sintering oven, sinter molding, to obtain final product; Wherein, sintering temperature is 355 DEG C; The heat-up rate of sintering oven is 2 DEG C/min; Soaking time is 90 minutes.The mechanical property of this nanometer hydroxyapatite/polyether-ether-ketone composite material is in table 1.
Embodiment 5
The preparation method of nanometer hydroxyapatite/polyether-ether-ketone composite material, it comprises the steps:
By raw material: 3kg (30wt%) nanometer hydroxyapatite powder (particle diameter is 500nm) and 7kg (70wt%) polyether-ether-ketone powder (particle diameter is 12 μm) carry out raw material Homogeneous phase mixing in mixing machine, obtain mixed powder; Then with mould by mixed powder compression moulding (using the mould of non-bone prosthesis product), then heat up in sintering oven, sinter molding, to obtain final product; Wherein, sintering temperature is 360 DEG C; The heat-up rate of sintering oven is 3 DEG C/min; Soaking time is 120 minutes.The mechanical property of this hydroxyapatite/polyether-ether-ketone composite material is in table 1.
Embodiment 6
The preparation method of bone prosthesis, it comprises the steps:
Operate according to the composition of raw materials of embodiment 1 and preparation method, in the mould of dog femoral dummy after injection moulding, carry out the operation of surface coarsening process, specific as follows: to use surface coarsening machine, with hydroapatite particles, surface coarsening process is carried out to the block after shaping, form to described block surface the porous surface that aperture is 100 μm ~ 300 μm, obtain bone prosthesis; Wherein, the particle diameter of hydroapatite particles is 50 μm ~ 200 μm.After carrying out surface coarsening process, Fig. 4 is shown in by scanning electron microscope (SEM) photo of this bone prosthesis.
Comparative example 1
Raw material: 1kg nanometer hydroxyapatite powder (particle diameter is 500nm) and 9kg polyether-ether-ketone powder (particle diameter is 10 μm), carries out the preparation of matrix material according to the preparation method of embodiment 1.The mechanical property of this matrix material is in table 1.
Comparative example 2
Raw material: 2kg nanometer hydroxyapatite powder (particle diameter is 500nm) and 8kg polyether-ether-ketone powder (particle diameter is 10 μm), carries out the preparation of matrix material according to the preparation method of embodiment 1.The mechanical property of this matrix material is in table 1.
Comparative example 3
Raw material: 5kg nanometer hydroxyapatite powder (particle diameter is 500nm) and 5kg polyether-ether-ketone powder (particle diameter is 10 μm), carries out the preparation of matrix material according to the preparation method of embodiment 1.The mechanical property of this matrix material is in table 1.
Effect example 1
Mechanical property test:
Carried out Mechanics Performance Testing to the bone prosthesis of embodiment 1 ~ 5 and comparative example 1 ~ 3, test result is in table 1.
The mechanical property of the bone prosthesis of table 1 embodiment 1 ~ 5
From table 1, compared to the matrix material obtained by comparative example, the Young's modulus of nanometer hydroxyapatite/polyether-ether-ketone composite material of the present invention and people's bone closer to, and parameters index in mechanical property is more excellent, is very suitable for the equivalent material (bone and tooth) as human body hard tissue.
Effect example 2
The cytotoxicity experiment of nanometer hydroxyapatite/polyether-ether-ketone composite material:
Nanometer hydroxyapatite/the polyether-ether-ketone composite material obtained to embodiment 1 and 4 carries out cytotoxicity experiment, and wherein sample diameter is 10mm, and thickness is 2mm, specifically sees Fig. 1.The concrete grammar of cytotoxicity experiment is as follows:
According to the biological safety of ISO:10993-5 cytotoxicity standard testing matrix material.At 37 DEG C, two kinds of samples (200mg/mL) in serum-free cell culture medium soak 24 hours, filter to obtain vat liquor.With the concentration in 3 × 102/ holes, inoblast is inoculated into 96 hole tissue culturing plates, after continuing to hatch 1 day, discard substratum, PBS cleans 3 times; Add the vat liquor containing 10%FBS, continue cultivation 1 day; Do not add material vat liquor containing 10%FBS as experiment blank group.When test duration point, every hole adds 30 pi of MTT solution, continues to hatch cultivation after 4 hours, discards nutrient solution, PBS cleans 3 times, and every hole adds 100 microlitre DMSO, and room temperature left standstill after 10 minutes, by microplate reader at 490nm wavelength place, survey the absorbance of solution, see Fig. 3.As seen from Figure 3, compared with blank (tissue culturing plate TCP), the absorbance of experimental group (sample of embodiment 1 and 4) does not have significant difference, shows that these two kinds of matrix materials do not have negative impact to fibroblastic growth.Known as calculated, the ratio of the cell survival rate of the cell in material vat liquor and blank group, all more than 95%, proves that these two samples all do not have toxicity to inoblast.
Effect example 3
Animal implants experiment:
The bone prosthesis (concrete shape is shown in Fig. 4) of the dog femoral obtained by embodiment 7 is implanted dog femoral defect place.Fig. 5 implants gained is roughly observed at dog femoral defect place photo after 3 months, and arrow points place is the bone prosthesis implanted.Fig. 6 is that this bone prosthesis implants the tissue slice of dog femoral defect place after 3 months.In Fig. 6 and Fig. 7, long arrow represents the bonding interface of bone and embedded material, and M represents bone prosthesis, the new osseous tissue formed of B representative.From Fig. 6 and Fig. 7, this bone prosthesis and osseous tissue closely combine grow together (Integrated implant), illustrate that this bone prosthesis has good biological activity and biocompatibility thus, as body implanting material, can repair and replacement bone tissue.Result shows, this bone prosthesis can promote the formation of osseous tissue and grow around bone prosthesis, and bone prosthesis is formed with osseous tissue and is firmly combined.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.

Claims (10)

1. a preparation method for nanometer hydroxyapatite/polyether-ether-ketone composite material, is characterized in that, it comprises the steps: raw material: polyether-ether-ketone powder and hydroxyapatite powder mix powdered; By it machine-shaping, to obtain final product; Wherein, the consumption of nanometer hydroxyapatite accounts for 30% ~ 35% of raw material gross weight, and the consumption of polyether-ether-ketone accounts for 65% ~ 70% of raw material gross weight; The particle diameter of nanometer hydroxyapatite powder is 200nm ~ 1 μm, and the particle diameter of polyether-ether-ketone powder is 5 μm ~ 15 μm.
2. preparation method as claimed in claim 1, it is characterized in that, the particle diameter of described nanometer hydroxyapatite powder is 200nm ~ 1 μm; And/or the particle diameter of described polyether-ether-ketone powder is 5 μm ~ 15 μm; And/or, described in be blended in mixing machine and carry out; And/or described machine-shaping is that injection moulding or molding sintering are shaping.
3. preparation method as claimed in claim 2, it is characterized in that, described injection moulding is carried out in injection moulding machine; The temperature of described injection moulding is 350 DEG C ~ 370 DEG C; The pressure of described injection moulding is 40MPa ~ 80MPa; And/or described molding sintering is shaping to carry out according to such as following working method: by as described in Homogeneous phase mixing powder pressing forming, then to heat up, sinter molding; The speed of described intensification is 3 DEG C/min; The temperature of described sintering is 355 DEG C-375 DEG C; The soaking time of described sintering is 90 minutes ~ 180 minutes.
4. nanometer hydroxyapatite/the polyether-ether-ketone composite material obtained by preparation method described in any one of claims 1 to 3.
5. the application of nanometer hydroxyapatite/polyether-ether-ketone composite material in bone prosthesis as claimed in claim 4.
6. a preparation method for bone prosthesis, is characterized in that, it comprises the steps: raw material: polyether-ether-ketone powder and hydroxyapatite powder mix powdered; By it machine-shaping, to obtain final product; Wherein, the consumption of nanometer hydroxyapatite accounts for 30% ~ 35% of raw material gross weight, and the consumption of polyether-ether-ketone accounts for 65% ~ 70% of raw material gross weight; The particle diameter of nanometer hydroxyapatite powder is 200nm ~ 1 μm, and the particle diameter of polyether-ether-ketone powder is 5 μm ~ 15 μm.
7. preparation method as claimed in claim 6, it is characterized in that, the particle diameter of described nano-hydroxy-apatite is 200nm ~ 1 μm; And/or the particle diameter of described polyether-ether-ketone powder is 5 μm ~ 15 μm; And/or, described in be blended in mixing machine and carry out; And/or described machine-shaping is that injection moulding or molding sintering are shaping; And/or the mould of described bone prosthesis product is the mould of spinal bone dummy or the mould of tooth implant.
8. preparation method as claimed in claim 7, it is characterized in that, described injection moulding is carried out in injection moulding machine; The temperature of described injection moulding is 350 DEG C ~ 370 DEG C; The pressure of described injection moulding is 40MPa ~ 80MPa; And/or described molding sintering is shaping to carry out according to following working method: by described mixed powder compression moulding, then heat up, sinter molding; The speed of described intensification is 3 DEG C/min; The temperature of described sintering is 355 DEG C-375 DEG C; The soaking time of described sintering is 90 ~ 180 minutes.
9. the preparation method as described in any one of claim 6 ~ 8, is characterized in that, after described machine-shaping, carries out coarse surface process; Described surface coarsening process is carried out in accordance with the following steps: use surface coarsening machine, be that 50 μm ~ 200 μm hydroapatite particles carry out surface coarsening to the block that described machine-shaping obtains with particle diameter, form to described block surface the porous surface that aperture is 100 μm ~ 300 μm.
10. the bone prosthesis obtained as any one of claim 6 ~ 8 preparation method.
CN201510437676.1A 2015-07-23 2015-07-23 Nano-hydroxyapatite/polyether-ether-ketone composite material and bone repair body as well as preparation method and application thereof Pending CN104974467A (en)

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CN106421922A (en) * 2016-10-09 2017-02-22 太原理工大学 Modified hydroxyapatite/carbon nanotube/polyetheretherketon composite material and preparation method thereof
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CN108084638A (en) * 2017-12-29 2018-05-29 吉林省中研高性能工程塑料股份有限公司 A kind of medical grade modified polyetheretherketonefiber and preparation method
CN108159498A (en) * 2017-12-05 2018-06-15 宜宾天原集团股份有限公司 A kind of preparation method of polyether-ether-ketone Biocomposite material
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CN110885533A (en) * 2019-12-03 2020-03-17 常州华森医疗器械有限公司 High-bioactivity PEEK composite material artificial joint prosthesis and preparation method thereof
CN110885532A (en) * 2019-12-03 2020-03-17 常州华森医疗器械有限公司 High-bioactivity polyether-ether-ketone composite material artificial prosthesis and preparation method thereof
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CN115737933A (en) * 2022-11-29 2023-03-07 华南理工大学 Radial gradient hydroxyapatite/polyether-ether-ketone composite material bracket with large-surface-through-hole structure and preparation method and application thereof

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CN106308959A (en) * 2016-08-26 2017-01-11 南宁越洋科技有限公司 Bioactive glass ceramic fiber-PEEK resin composite artificial tooth and preparation method
CN106421922A (en) * 2016-10-09 2017-02-22 太原理工大学 Modified hydroxyapatite/carbon nanotube/polyetheretherketon composite material and preparation method thereof
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CN109568669A (en) * 2018-11-30 2019-04-05 重庆医科大学附属永川医院 A kind of implantation material and preparation method thereof fixed for backbone reparation
CN109568669B (en) * 2018-11-30 2021-05-11 重庆医科大学附属永川医院 Implant material for spinal column repair and fixation and preparation method thereof
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CN110152068B (en) * 2019-05-31 2022-03-01 武汉理工大学 Polyether-ether-ketone/nano-hydroxyapatite composite material and preparation method and application thereof
CN110559488A (en) * 2019-10-25 2019-12-13 中国科学院长春应用化学研究所 calcium sulfate-containing polyetheretherketone particulate bone filling material and preparation method thereof
CN110885533A (en) * 2019-12-03 2020-03-17 常州华森医疗器械有限公司 High-bioactivity PEEK composite material artificial joint prosthesis and preparation method thereof
CN110885532A (en) * 2019-12-03 2020-03-17 常州华森医疗器械有限公司 High-bioactivity polyether-ether-ketone composite material artificial prosthesis and preparation method thereof
CN111888530A (en) * 2020-04-20 2020-11-06 上海交通大学医学院附属仁济医院 Zinc oxide-polyether-ether-ketone composite material, preparation method and application thereof, and artificial joint formed by zinc oxide-polyether-ether-ketone composite material
CN113877003A (en) * 2021-10-19 2022-01-04 吉林省中研高分子材料股份有限公司 Medical-grade composite material and preparation method thereof
CN115737933A (en) * 2022-11-29 2023-03-07 华南理工大学 Radial gradient hydroxyapatite/polyether-ether-ketone composite material bracket with large-surface-through-hole structure and preparation method and application thereof

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