CN104307037A - Novel human bone substitute material and preparation method thereof - Google Patents
Novel human bone substitute material and preparation method thereof Download PDFInfo
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- CN104307037A CN104307037A CN201410616871.6A CN201410616871A CN104307037A CN 104307037 A CN104307037 A CN 104307037A CN 201410616871 A CN201410616871 A CN 201410616871A CN 104307037 A CN104307037 A CN 104307037A
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Abstract
The invention discloses a novel human bone substitute material, and aims to overcome the defect that the existing polyether ether ketone/ hydroxyapatite composite material is poor in bioactivity. The human bone substitute material contains polyether ether ketone and porous hydroxyapatite, wherein the porous hydroxyapatite has the porosity of 50-80% and the aperture of 100-250 microns. The polyether ether ketone and the porous hydroxyapatite are combined to form a composite material, and compared with the ordinary polyether ether ketone/ hydroxyapatite composite material, the composite material can promote cell proliferation better, so that the novel human bone substitute material with high bioactivity can be obtained.
Description
Technical field
One belongs to bioactive materials technical field, relates to a kind of people's bone alternate material and preparation method thereof.
Background technology
Hydroxyapatite is the important component part of skeleton, tooth, and its mass fraction about 70% in people's bone component, in the dental enamel of people, mass fraction is then more than 95%.Hydroxyapatite has good biocompatibility, biological activity and chemical stability, can combine closely with bone, is considered to the most promising ceramic artificial tooth and artificial bone replacing material.But pure hydroxyapatite mechanical performance compare is poor, poor as its dependability of artificial growth body.Which greatly limits it and carry the application in the bone replacement of position.
Polyether-ether-ketone is a kind of all aromatic hemicrystalline high polymer, the rigidity of this material is comparatively large, and dimensional stability is better, chemical stability, Heat stability is good, there is excellent chemical proofing, also there is outstanding tribological property, resistance to skimming wear and fretting wear; In addition, it also has good toughness, is the most outstanding in all plastics to the excellent fatigue durability of alternate stress.Therefore, polyether-ether-ketone is a kind of good reparation and the biomaterial replacing human body hard tissue.But polyetheretherketonematerials materials does not have biological activity, this also constrains its biologic applications.
Hydroxyapatite/polyether-ether-ketone Biocomposite material arouses great concern, and the two has extremely strong complementarity, both can improve the mechanical property of hydroxyapatite as composite, has again excellent biological activity concurrently.But the hydroxyapatite composition in current polyether-ether-ketone/hydroxyapatite composite material is solid construction.Because the hydroxyapatite composition in current polyether-ether-ketone/hydroxyapatite composite material is solid construction, after this material implants, freshman bone tissue only can form sclerotin on surface, although attachment closely, but the inside of hydroxyapatite of can not growing into, because contact area is little, hydroxyapatite can not physiological be combined fully with bone, and therefore the physiologically active of composite can not be fully played, and is difficult to the functional requirement meeting people's bone alternate material.
There are some researches show, the structure of hydroxyapatite directly affects tissue and grows into and be organized in the growth in implantation body, and loose structure is conducive to the growth promoting tissue, when connecting bore dia in material at 15-40 μm, namely allows fibrous tissue to grow into material internal; And aperture is when being 40-100 μm, the osteoid tissue of non-mineralising is allowed to grow into; , 150 μm time, can grow into for osseous tissue and provide ideal place in aperture.
Summary of the invention
For the defect of the biological activity difference that hydroxyapatite in prior art/polyether-ether-ketone Biocomposite material exists, the present invention is intended to provide a kind of novel people's bone alternate material and preparation method thereof for solving the problems of the technologies described above.
For achieving the above object, the technical solution adopted in the present invention is as follows:
A kind of people's bone alternate material, be polyether-ether-ketone/hydroxyapatite composite material, it is characterized in that, described people's bone alternate material comprises polyether-ether-ketone and porous hydroxyapatite, and the porosity of described porous hydroxyapatite is 50-80%, and aperture is 100-250 μm.
Preferably, the mass fraction of described people's bone alternate material component is: polyether-ether-ketone 70-90%, porous hydroxyapatite 10-30%.
The present invention also provides the preparation method of described people's bone alternate material, comprise the following steps: by dried porous hydroxyapatite and polyether-ether-ketone powder body, according to the mass percentage of hydroxyapatite be 10% ~ 30% mixing, after putting into ball mill ball milling, put into baking oven inner drying again, obtained described people's bone alternate material.
The preparation method of described porous hydroxyapatite is: after hydroxyapatite powder mixes with methylcellulose powder, slurry is mixed into again with deionized water, degassed through ultrasonic vibration, 50 DEG C-90 DEG C oven dry, are then warming up to 250 DEG C with the speed of 0.5 DEG C/min in an oven, insulation, 1250 DEG C are warmed up to again with the speed of 3 DEG C/min, insulation, furnace cooling, to room temperature, can obtain porous hydroxyapatite.
Described hydroxyapatite and the mass ratio of methylcellulose are 1:0.5-1:1; Obtained porous hydroxyapatite porosity is 50-80%, and aperture is 100-250 μm.
The invention has the beneficial effects as follows: people's bone alternate material of the present invention is polyether-ether-ketone/porous hydroxyapatite composite, by on the basis of current material, adopt porous hydroxyapatite to substitute common hydroxyapatite, effectively can improve the biological activity of people's bone alternate material.Experimental data shows, compared with common polyether-ether-ketone/hydroxyapatite composite material, polyether-ether-ketone/porous hydroxyapatite composite more can promote cell proliferation.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not limited with detailed description of the invention, but is limited by claim.
Accompanying drawing explanation
Fig. 1 PEEK/10%p-HA and PEEK/10%HA composite change the impact of on cell proliferation rate in time.
The PEEK/p-HA composite of the different constituent of Fig. 2 changes the impact of on cell proliferation rate in time.
Detailed description of the invention
Below by specific embodiment, technical solutions according to the invention are further described in detail, but are necessary to point out that following examples are only for the description to summary of the invention, do not form limiting the scope of the invention.In following examples, hydroxyapatite is abbreviated as HA, and porous hydroxyapatite is abbreviated as p-HA, and polyether-ether-ketone is abbreviated as PEEK.
Embodiment 1
A kind of novel people's bone alternate material and preparation method thereof, step is as follows:
1) preparation of porous hydroxyapatite:
Take 10gHA powder, 5g methylcellulose powder, after the two being mixed, then be mixed into slurry with 500mL deionized water, after mixture being carried out Ultrasonic Pulverization, degassed 45min, in the baking oven of 90 DEG C, dry more than 24h.After being cooled to room temperature, be heated to 250 DEG C with the programming rate of 0.5 DEG C/min, insulation 20min, then be warming up to 1250 DEG C with the speed of 3 DEG C/min, after insulation 5h, be cooled to room temperature with the speed of 3 DEG C/min, p-HA powder can be obtained.
2) preparation of PEEK/p-HA composite:
By dried p-HA and PEEK powder body mixing, put into ball mill ball milling 30min fast, then put into baking oven inner drying 2h, PEEK/p-HA composite can be obtained.
In the present embodiment, the mass fraction of p-HA in PEEK/p-HA composite is 10%.
Embodiment 2
1) preparation of porous hydroxyapatite:
Take 10gHA powder, 8g methylcellulose powder, after the two being mixed, then be mixed into slurry with 500mL deionized water, after mixture being carried out Ultrasonic Pulverization, degassed 45min, in the baking oven of 90 DEG C, dry more than 24h.After being cooled to room temperature, be heated to 250 DEG C with the programming rate of 0.5 DEG C/min, insulation 30min, then be warming up to 1250 DEG C with the speed of 3 DEG C/min, after insulation 6h, be cooled to room temperature with the speed of 3 DEG C/min, p-HA powder can be obtained.
2) preparation of PEEK/p-HA composite:
Identical with embodiment 1, difference is in the present embodiment, and the mass fraction of p-HA in PEEK/p-HA composite is 20%.
Embodiment 3
1) preparation of porous hydroxyapatite:
Take 10gHA powder, 10 g methylcellulose powder, after the two being mixed, then be mixed into slurry with 500mL deionized water, after mixture being carried out Ultrasonic Pulverization, degassed 45min, in the baking oven of 90 DEG C, dry more than 24h.After being cooled to room temperature, be heated to 250 DEG C with the programming rate of 0.5 DEG C/min, insulation 20min, then be warming up to 1250 DEG C with the speed of 3 DEG C/min, after insulation 5h, be cooled to room temperature with the speed of 3 DEG C/min, p-HA powder can be obtained.
2) preparation of PEEK/p-HA composite:
Identical with embodiment 1, difference is in the present embodiment, and the mass fraction of p-HA in PEEK/p-HA composite is 30%.
Comparative example
Directly adopt HA powder, according to embodiment 1 step 2) identical method prepares PEEK/10%HA composite.
Embodiment 4
The performance of the PEEK/p-HA material prepared by embodiment 1-3 is tested, is described in detail as follows.
The porosity using Archimedes method to measure p-HA material is 50-80%.
The aperture using mercury injection method to measure p-HA material is 100-250 μm.
After the sterilizing of PEEK/10%HA, PEEK/10%p-HA, PEEK/20%p-HA, PEEK/30%p-HA composite high-pressure, often kind of material DMEM culture medium is made into suspension by the concentration of 20mg/mL.
When carrying out toxotest, employing be WST-1 reagent method.WST-1 is a kind of compound being similar to MTT, deposits in case at electronics coupled reagent, can be generated orange-yellow crystallization first a ceremonial jade-ladle, used in libation by more Intramitochondrial dehydrogenase reduction.The MG-63 cells of exponential phase is adherent with the trypsinization of 0.25%, and with containing 10%(V/V) the DMEM in high glucose culture fluid of hyclone makes cell suspension, and in the 96 every holes of orifice plate, add 90 μ L, control cell density and be about 10
4/ hole, edge hole sterile phosphate buffer solution (PBS) is filled.The Tissue Culture Plate inoculated is put into incubator and cultivates 24h, add the culture fluid (5 multiple holes established by each sample) containing above-mentioned various material configured, put into incubator Dual culture 48h.Respectively the 12nd, 24,36,48h time, Aspirate supernatant, rinses 2 times gently with aseptic PBS, and every hole adds 100 μ L culture medium and 10 μ LWST-1 solution, continues to cultivate 4h, at the light absorption value in each hole of measurement, enzyme mark detector OD450nm place.Blank well and control wells are set simultaneously.
Measurement result as shown in Figure 1 and Figure 2.Wherein, cell survival rate %=(test group OD meansigma methods-blank group OD meansigma methods)/(matched group OD meansigma methods-blank group OD meansigma methods) × 100%.
Elaborate below in conjunction with the biological property of test result to PEEK/p-HA material.
Fig. 1 display be the impact of PEEK/10%p-HA and PEEK/10%HA on cell proliferation rate.Can find out, compared with common HA, the HA of porous more can promote the propagation of cell, and along with the prolongation of action time, this effect is more obvious.
Fig. 2 display be the impact of the PEEK/p-HA composite on cell proliferation rate of different constituent.Can see, in the time range of test, in material, the content of p-HA is higher, and material is stronger for the facilitation of cell proliferation,
The foregoing is only preferred embodiments of the present invention, not in order to limit the present invention, all within aim of the present invention and principle, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. people's bone alternate material, for polyether-ether-ketone/hydroxyapatite composite material, it is characterized in that: described people's bone alternate material comprises polyether-ether-ketone and porous hydroxyapatite, the porosity of described porous hydroxyapatite is 50-80%, and aperture is 100-250 μm.
2. people's bone alternate material according to claim 1, is characterized in that, the mass fraction of described people's bone alternate material component is: polyether-ether-ketone 70-90%, porous hydroxyapatite 10-30%.
3. people's bone alternate material according to claim 1, is characterized in that, described people's bone alternate material adopts following methods preparation:
1) after hydroxyapatite powder mixes with methylcellulose powder, slurry is mixed into again with deionized water, degassed through ultrasonic vibration, 50 DEG C-90 DEG C oven dry, are then warming up to 250 DEG C with the speed of 0.5 DEG C/min in an oven, insulation, be warmed up to 1250 DEG C with the speed of 3 DEG C/min again, insulation, furnace cooling is to room temperature, obtained porosity is 50-80%, and aperture is the porous hydroxyapatite of 100-250 μm;
2) by dried porous hydroxyapatite and polyether-ether-ketone powder body, be 10% ~ 30% mixing according to the mass percentage of hydroxyapatite, after putting into ball mill ball milling, then put into baking oven inner drying, obtained described people's bone alternate material.
4. the preparation method of people's bone alternate material, comprise the following steps: by dried porous hydroxyapatite and polyether-ether-ketone powder body, according to the mass percentage of porous hydroxyapatite be 10% ~ 30% mixing, after putting into ball mill ball milling, put into baking oven inner drying again, obtained described people's bone alternate material.
5. the preparation method of people's bone alternate material according to claim 4, it is characterized in that, the preparation method of described porous hydroxyapatite is: after hydroxyapatite powder mixes with methylcellulose powder, then is mixed into slurry with deionized water, degassed through ultrasonic vibration, 50 DEG C-90 DEG C oven dry, are then warming up to 250 DEG C with the speed of 0.5 DEG C/min in an oven, insulation, 1250 DEG C are warmed up to again with the speed of 3 DEG C/min, insulation, furnace cooling, to room temperature, namely obtains porous hydroxyapatite.
6. the preparation method of people's bone alternate material according to claim 5, is characterized in that, described hydroxyapatite and the mass ratio of methylcellulose are 1:0.5-1:1.
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| CN104906635A (en) * | 2015-06-19 | 2015-09-16 | 四川大学 | Poly(ether-ether-ketone)/nano hydroxyapatite dental implant and manufacturing method thereof |
| CN105000569A (en) * | 2015-07-23 | 2015-10-28 | 深圳市科聚新材料有限公司 | Mesoporous magnesium silicate/ hydroxyapatite/ polyether-ether-ketone composite material, bone restoration and preparation method and application thereof |
| WO2017035893A1 (en) * | 2015-09-02 | 2017-03-09 | 广东银禧科技股份有限公司 | Polyetheretherketone/nano-hydroxyapatite composite material for sls technology and preparation method thereof |
| CN106674547A (en) * | 2016-11-28 | 2017-05-17 | 安徽省春谷3D打印智能装备产业技术研究院有限公司 | Spheroidization method of polyether-ether-ketone-hydroxyapatite (Peek-HA) 3D printing powder |
| CN110152068A (en) * | 2019-05-31 | 2019-08-23 | 武汉理工大学 | A kind of polyether-ether-ketone/nano hydroxyapatite composite material and its preparation method and application |
| 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 |
| CN114601975A (en) * | 2022-04-02 | 2022-06-10 | 奥精医疗科技股份有限公司 | Polyether-ether-ketone composite mineralized collagen material and preparation method and application 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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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104906635A (en) * | 2015-06-19 | 2015-09-16 | 四川大学 | Poly(ether-ether-ketone)/nano hydroxyapatite dental implant and manufacturing method thereof |
| CN104906635B (en) * | 2015-06-19 | 2017-05-31 | 四川大学 | A kind of polyether-ether-ketone/nanometer hydroxyapatite tooth implant and preparation method thereof |
| CN105000569A (en) * | 2015-07-23 | 2015-10-28 | 深圳市科聚新材料有限公司 | Mesoporous magnesium silicate/ hydroxyapatite/ polyether-ether-ketone composite material, bone restoration and preparation method and application thereof |
| WO2017035893A1 (en) * | 2015-09-02 | 2017-03-09 | 广东银禧科技股份有限公司 | Polyetheretherketone/nano-hydroxyapatite composite material for sls technology and preparation method thereof |
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| CN106674547A (en) * | 2016-11-28 | 2017-05-17 | 安徽省春谷3D打印智能装备产业技术研究院有限公司 | Spheroidization method of polyether-ether-ketone-hydroxyapatite (Peek-HA) 3D printing powder |
| CN110152068A (en) * | 2019-05-31 | 2019-08-23 | 武汉理工大学 | A kind of polyether-ether-ketone/nano hydroxyapatite composite material and its preparation method and application |
| 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 |
| 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 |
| CN114601975A (en) * | 2022-04-02 | 2022-06-10 | 奥精医疗科技股份有限公司 | Polyether-ether-ketone composite mineralized collagen material and preparation method and application thereof |
| CN114601975B (en) * | 2022-04-02 | 2022-12-06 | 奥精医疗科技股份有限公司 | Polyether-ether-ketone composite mineralized collagen material as well as preparation method and application 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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