CN102432180A - Method for preparing bioactive glass ceramic material for bone defect restoration - Google Patents
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- CN102432180A CN102432180A CN2011102987353A CN201110298735A CN102432180A CN 102432180 A CN102432180 A CN 102432180A CN 2011102987353 A CN2011102987353 A CN 2011102987353A CN 201110298735 A CN201110298735 A CN 201110298735A CN 102432180 A CN102432180 A CN 102432180A
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Abstract
The invention discloses a method for preparing a bioactive glass ceramic material for bone defect restoration, which comprises the steps of: sieving the biological glass powder, adding the polyacrylamide solution, ball milling and mixing uniformly to obtain the biological glass slurry; pouring the slurry into a macromolecular reverse mould by centrifugal grouting, curing, drying and sintering at a temperature of between 900 DEG C and 1000 DEG C controlled by a program to remove the macromolecular reverse mould to prepare the bioactive glass ceramic material for bone defect restoration. The shape of the bioactive glass ceramic material for bone defect restoration prepared by the invention can be decided according to clinical demand, and the bioactive glass ceramic material for bone defect restoration has good mechanical strength, biocompatibility and degradability, high compression strength, good anti-dispersion performance and activity and adjustable and controllable degradation time. The preparation method provided by the invention has a simple process and low cost.
Description
Technical field
The invention belongs to the biological active materials field, relate to bone tissue restoration, filling and organizational project repair materials, be specifically related to be used for the preparation method of the biological activated glass ceramic material of bone defect repair.
Background technology
It is clinical common disease and frequently-occurring disease that the disease of bone is decreased.Through development bone reparation and bone alternate material, can help the osseous tissue of patient's repair deficiency or disappearance, recover the tissue function better.In bone tissue engineer, the ideal repair materials should meet following condition: excellent biological compatibility, biological degradability, plasticity-have the pore texture and the certain mechanical strength of three-dimensional porous and intercommunication.On bone defect repair research field, press for have with people's biomechanics of bone intensity be complementary, cell compatibility is good and promote the timbering material of freshman bone tissue's growth.
Biological active materials is to be used for organism is diagnosed, treats, repairs or replace its sick damage tissue, organ or promotes its materials with function.Typical case's representative of biological active materials has calcium phosphate bone cement, phosphatic rock and bio-vitric etc.These biological active materials are when the clinical application material of bone tissue restoration and bone tissue engineer; Owing to all be not quite similar on composition, structure and the intensity; Still has bigger difference with people's bone photo ratio; Cause its biocompatibility, degradable performance not ideal enough, thereby directly influence the repairing effect of osseous tissue.Solidification process can take place like the calcium phosphate bone cement material in injecting body the time, produce great amount of heat and destroy the tissue around it.Phosphatic rock is used as hard tissue repair and replacement with block, particle form quilt clinically widely, yet, since the fragility of block pottery, shortcomings such as the easy migration of particle, displacement, very difficult moulding, limited its application clinically.
Bio-vitric has good biological activity and biocompatibility, can be used as tissue reparation and twice-laid stuff, by Na
2O-CaO-SiO
2-P
2O
5The fusion bio-vitric of quaternary component also has with CaO-SiO
2-P
2O
5Sol-gel bio-vitric for component; All obtained good bone repairing effect clinically; Can be through changing each components contents to regulate its biological activity, degradation property and mechanical property; Satisfy the different clinical requirement, and, promote osteoblastic differentiation and propagation through activating more osteoblastic genes.But traditional bio-vitric support generally enbrittles greatly, the not high shortcoming of mechanical strength.
Summary of the invention
The objective of the invention is to deficiency, be provided for the preparation method of the biological activated glass ceramic material of bone defect repair to present bone impairment renovation material and technology of preparing aspect thereof.The shape and the pore dimension of the bone impairment renovation material of the present invention's preparation can be according to regulating according to clinical needs, and shape comprises porous cylindrical body, porous cubes and irregular block.
In order to achieve the above object, the present invention has adopted following technical scheme.
Be used for the preparation method of the biological activated glass ceramic material of bone defect repair, comprise the steps:
(1) the bio-vitric powder is crossed 200 mesh sieves, add the ROHM amine aqueous solution, milling mixing obtains the bio-vitric slurry;
(2) the bio-vitric slurry that step (1) is obtained dropwise adds in the polymer reverse, and the polymer reverse is carried out centrifugal grouting in whizzer, in 70 ~ 75 ℃ of water-baths, solidify 1 ~ 2h after, 50 ~ 70 ℃ of drying 48 ~ 72h obtain solid material;
(3) solid material that step (2) is obtained is removed the polymer reverse in 900 ~ 1000 ℃ of calcinings under temperature programmed control, make the biological activated glass ceramic material that is used for the bone defect repair.
Bio-vitric powder according to the invention is Na
2O-CaO-SiO
2-P
2O
5Bio-vitric powder and/or CaO-SiO
2-P
2O
5The bio-vitric powder.
Na according to the invention
2O-CaO-SiO
2-P
2O
5The material of bio-vitric powder is formed mass percent: quicklime 20 ~ 25%, Vanadium Pentoxide in FLAKES 5 ~ 7%, sodium oxide 20 ~ 25%, silicon-dioxide 43 ~ 49%; Said CaO-SiO
2-P
2The material of O bio-vitric powder is formed mass percent: quicklime 14 ~ 33%, Vanadium Pentoxide in FLAKES 0 ~ 9%, silicon-dioxide 58 ~ 80%.
The volume(tric)fraction of bio-vitric powder is 50 ~ 60% in the bio-vitric slurry according to the invention.
The pore dimension of polymer reverse according to the invention is 500 ~ 1000 microns, and geometrical shape is cubes, rectangular parallelepiped or right cylinder.
The process of temperature programmed control according to the invention comprises following three phases:
(1) temperature rise period: the temperature of solid material is risen to 900 ~ 1000 ℃ with the speed of 2 ~ 3 ℃/min;
(2) holding stage: the temperature of solid material is kept 1 ~ 2h at 900 ~ 1000 ℃;
(3) temperature-fall period: be cooled to 10 ~ 30 ℃ naturally.
The volume(tric)fraction of poly amic acid is 4 ~ 8% in the ROHM amine aqueous solution according to the invention.
The rotating speed of centrifugal grouting according to the invention is 800 ~ 1200r/min.
Polymer reverse according to the invention is photosensitive resin reverse or polymkeric substance reverse; Said photosensitive resin reverse adopts the photocuring forming technique, is feedstock production with the photosensitive resin; Said polymkeric substance reverse adopts the 3 D-printing technology, is feedstock production with the polymkeric substance.
Photosensitive resin according to the invention is a unsaturated polyester resin, comprises gathering meso lactic acid or polycaprolactone; Said polymkeric substance is that polylactic acid-glycolic guanidine-acetic acid multipolymer or acrylonitrile-butadiene-styrene copolymer (are called for short: ABS resin).
Na according to the invention
2O-CaO-SiO
2-P
2O
5The preparation process of bio-vitric powder is with reference to [Lefebvre L. such as Lefebvre L; Chevalier J.; Gremillard L. Structural transformations of bioactive glass 45S5 with thermal treatments. Acta Materiala; 2007,55 (10), 3305 ~ 3313] document; Specifically may further comprise the steps: with analytically pure yellow soda ash, lime carbonate, tricalcium phosphate and silicon-dioxide in proportion weighing and thorough mixing evenly after, put into platinum crucible in 1400 ℃ of fusion 120min; Pour melten glass liquid in deionized water shrend then, obtain the amorphous phase bioactivity glass; With after the water filtering in 60 ℃ of dry 24h, with the speed ball milling 3h of 480rpm, cross 200 mesh sieves, promptly get Na
2O-CaO-SiO
2-P
2O
5The bio-vitric powder.
CaO-SiO according to the invention
2-P
2O
5The preparation process of bio-vitric powder is with reference to [Zhong J. such as Zhong J.; Greenspan D.C. Processing and properties of sol-gel bioactive glasses. J Biomed Mater Res., 2000,53 (6): 694 ~ 701] and [Chen X. such as Chen X.; Meng Y.; Li Y., et al. Investigation on bio-mineralization of melt and sol-gel derived bioactive glasses. Applied Surface Science, 2008; .255 (2): 562 ~ 564] bibliographical information; Specifically may further comprise the steps: in beaker, add hydrochloric acid catalyst and the tetraethoxysilance of deionized water, 2mol/L, stir hydrolysis 30min at ambient temperature after, add tricresyl phosphate second fat and continue to stir 30min; Add four water-calcium nitrate again, stir the colloidal sol that the back obtains transparent stable homogeneous; The at room temperature static ageing certain hour of colloidal sol fully carries out hydrolysis-condensation reaction, forms wet gel; Wet gel placed 140 ℃ of dryings 2 days, obtained xerogel after making solvent evaporation; Xerogel is obtained particulate state bioactive sol-gel glass in 650 ℃ of heat treatment for solidification technologies; With the speed ball milling 3h of 480rpm, cross 200 mesh sieves, promptly get CaO-SiO
2-P
2O
5The bio-vitric powder.
The biological activated glass ceramic material shape of the present invention's preparation can be according to clinical needs decision, and its internal void is 500 ~ 1000 μ m, and porosity is 45 ~ 65%.
The present invention compared with prior art has following advantage and unusual effect:
(1) the biological glass ceramic bone renovating material of the present invention's preparation has multiple shape selection, can adapt to the damaged filling of bone of different sites and shape; The materials chemistry adjustable components, thus the physicochemical property of material and use characteristics can be adjusted in certain limit; Preparation is simple, and processing parameter is easy to control and advantage such as output is big;
(2) profile of the biological glass ceramic bone renovating material of the present invention's preparation and internal void structure help growing into and the damaged reparation of bone of freshman bone tissue.
(3) the biological glass ceramic bone impairment renovation material of the present invention's preparation has good mechanical intensity, biocompatibility and certain biodegradability.
Description of drawings
Fig. 1 is the micro-CT photo of the biological activated glass ceramic material of the embodiment of the invention 1 preparation.
Fig. 2 is that the ESEM on the biological activated glass ceramic material surface of the embodiment of the invention 1 preparation (is called for short: SEM) photo.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed description, but the scope that the present invention requires to protect is not limited to this.
Embodiment 1
Adopt Na
2O-CaO-SiO
2-P
2O
5The bio-vitric powder.
(1) with 58.63g yellow soda ash 52.33g lime carbonate, 18.36g tricalcium phosphate and 63.00g silicon-dioxide thorough mixing evenly after; Put into platinum crucible in 1400 ℃ of fusion 120min, pour melten glass liquid in deionized water shrend then, obtain the amorphous phase bioactivity glass; With after the water filtering in electric drying oven with forced convection in 60 ℃ of dry 24h; With speed ball milling 3h in planetary ball mill of 480rpm, cross 200 mesh sieves, promptly get Na
2O-CaO-SiO
2-P
2O
5The bio-vitric powder, each material consists of: 24.5% quicklime, 6g Vanadium Pentoxide in FLAKES, 24.5% sodium oxide, 45% silicon-dioxide;
(2) with 100g Na
2O-CaO-SiO
2-P
2O
5It is in 6% the ROHM amine aqueous solution that the bio-vitric powder adds the 100mL volume(tric)fraction, and 3 hours mixings of ball milling obtain volume(tric)fraction and be 50% bio-vitric slurry;
(3) the bio-vitric slurry that step (1) is obtained dropwise adds in the unsaturated polyester resin reverse; The polymer reverse is carried out centrifugal grouting with 800r/min in the appearance L550 type whizzer of Hunan; Place 70 ℃ of water-baths to solidify 2h; Be positioned in the loft drier in 50 ℃ of dry 72h, obtain solid material;
(4) solid material is put into the zirconium white saggar, keep 2h after with the speed of 2 ℃/min the temperature of solid material being risen to 900 ℃; Naturally be cooled to 10 ℃, make the biological activated glass ceramic material that is used for the bone defect repair.
Embodiment 2
Adopt Na
2O-CaO-SiO
2-P
2O
5Bio-vitric powder and CaO-SiO
2-P
2O
5The mixture of bio-vitric powder, wherein Na
2O-CaO-P
2O
5-SiO
2The massfraction of bio-vitric powder is 99%, CaO-P
2O
5-SiO
2The massfraction of bio-vitric powder is 1%.
(1) with 59.82g yellow soda ash, 53.40 g lime carbonate, 15.30g tricalcium phosphate and 63.00 g silicon-dioxide thorough mixing evenly after; Put into platinum crucible in 1400 ℃ of fusion 120min, pour melten glass liquid in deionized water shrend then, obtain the amorphous phase bioactivity glass; With after the water filtering in electric drying oven with forced convection in 60 ℃ of dry 24h; With speed ball milling 3h in planetary ball mill of 480rpm, cross 200 mesh sieves, promptly get Na
2O-CaO-SiO
2-P
2O
5The bio-vitric powder, each material consists of: 25% quicklime, 5g Vanadium Pentoxide in FLAKES, 25% sodium oxide, 45% silicon-dioxide;
(2) hydrochloric acid catalyst and the 25.56mL tetraethoxysilance of adding 18.72mL deionized water, 3.12mL 2mol/L in beaker; After stirring hydrolysis 30min at ambient temperature; Add 2.61mL tricresyl phosphate second fat and continue to stir 30min; Add the 16.24g four water-calcium nitrate again, stir the colloidal sol that the back obtains transparent stable homogeneous; The at room temperature still aging 48h of colloidal sol fully carries out hydrolysis-condensation reaction, forms wet gel; Wet gel placed 140 ℃ of dryings 2 days, obtained xerogel after making solvent evaporation; Xerogel is obtained particulate state bioactive sol-gel glass in 650 ℃ of heat treatment for solidification technologies; With the speed ball milling 3h of 480rpm, cross 200 mesh sieves, promptly get CaO-SiO
2-P
2O
5The bio-vitric powder, each material consists of: 33% quicklime, 9% Vanadium Pentoxide in FLAKES and 58% silicon-dioxide;
(3) with 99g Na
2O-CaO-SiO
2-P
2O
5Bio-vitric powder and 1g CaO-SiO
2-P
2O
5The bio-vitric powder mixes, and adds the 100mL volume(tric)fraction and is in 6% the ROHM amine aqueous solution, and 3 hours mixings of ball milling obtain volume(tric)fraction and be 50% bio-vitric slurry;
(4) the bio-vitric slurry that step (1) is obtained dropwise adds in the ABS resin reverse; Reverse is carried out centrifugal grouting with 1000r/min in the appearance L550 type whizzer of Hunan; After placing 75 ℃ of water-baths to solidify 1h, be positioned in the loft drier, obtain solid material in 70 ℃ of dry 48h;
(5) solid material is put into the zirconium white saggar, keep 1h after with the speed of 3 ℃/min the temperature of solid material being risen to 1000 ℃; Naturally be cooled to 30 ℃, make the biological activated glass ceramic material that is used for the bone defect repair.
Embodiment 3
Adopt Na
2O-CaO-SiO
2-P
2O
5Bio-vitric powder and CaO-SiO
2-P
2O
5The mixture of bio-vitric powder, wherein Na
2O-CaO-P
2O
5-SiO
2The massfraction of bio-vitric powder is 50%, CaO-P
2O
5-SiO
2The massfraction of bio-vitric powder is 50%.
(1)) with 39.32g yellow soda ash, 35.09g lime carbonate, 13.11g tricalcium phosphate and 48.00g silicon-dioxide thorough mixing evenly after; Put into platinum crucible in 1400 ℃ of fusion 120min, pour melten glass liquid in deionized water shrend then, obtain the amorphous phase bioactivity glass; With after the water filtering in electric drying oven with forced convection in 60 ℃ of dry 24h; With speed ball milling 3h in planetary ball mill of 480rpm, cross 200 mesh sieves, promptly get Na
2O-CaO-SiO
2-P
2O
5The bio-vitric powder, each material consists of: 23% quicklime, 6% Vanadium Pentoxide in FLAKES, 23% sodium oxide and 48% silicon-dioxide;
(2) hydrochloric acid catalyst and the 127.80mL tetraethoxysilance of adding 93.6mL deionized water, 15.57mL 2mol/L in beaker; After stirring hydrolysis 30min at ambient temperature; Add 13.03mL tricresyl phosphate second fat and continue to stir 30min; Add the 81.21g four water-calcium nitrate again, stir the colloidal sol that the back obtains transparent stable homogeneous; The at room temperature still aging 48h of colloidal sol fully carries out hydrolysis-condensation reaction, forms wet gel; Wet gel placed 140 ℃ of dryings 2 days, obtained xerogel after making solvent evaporation; Xerogel is obtained particulate state bioactive sol-gel glass in 650 ℃ of heat treatment for solidification technologies; With the speed ball milling 3h of 480rpm, cross 200 mesh sieves, promptly get CaO-SiO
2-P
2O
5The bio-vitric powder, each material consists of: 14% quicklime, 9% Vanadium Pentoxide in FLAKES and 77% silicon-dioxide;
(3) with 50gNa
2O-CaO-SiO
2-P
2O
5Bio-vitric powder and 50gCaO-SiO
2-P
2O
5The bio-vitric powder mixes, and adds the 82mL volume(tric)fraction and is in 6% the ROHM amine aqueous solution, and 3 hours mixings of ball milling obtain volume(tric)fraction and be 55% bio-vitric slurry;
(4) the bio-vitric slurry that step (1) is obtained dropwise adds in the polylactic acid-glycolic guanidine-acetic acid multipolymer reverse; Reverse is carried out centrifugal grouting with 1200r/min in the appearance L550 type whizzer of Hunan; After placing 72 ℃ of water-baths to solidify 1.5h; Be positioned in the loft drier in 60 ℃ of dry 60h, obtain solid material;
(5) solid material is put into the zirconium white saggar, keep 1.5h after with the speed of 2 ℃/min the temperature of solid material being risen to 950 ℃; Naturally be cooled to 20 ℃, make the biological activated glass ceramic material that is used for the bone defect repair.
Embodiment 4
Adopt Na
2O-CaO-SiO
2-P
2O
5Bio-vitric powder and CaO-SiO
2The mixture of bio-vitric powder, wherein Na
2O-CaO-P
2O
5-SiO
2The massfraction of bio-vitric powder is 1%, CaO-SiO
2The massfraction of bio-vitric powder is 99%.
(1) with 37.61g yellow soda ash, 33.57g lime carbonate, 15.30g tricalcium phosphate and 49.00 g silicon-dioxide thorough mixing evenly after; Put into platinum crucible in 1400 ℃ of fusion 120min, pour melten glass liquid in deionized water shrend then, obtain the amorphous phase bioactivity glass; With after the water filtering in electric drying oven with forced convection in 60 ℃ of dry 24h; With speed ball milling 3h in planetary ball mill of 480rpm, cross 200 mesh sieves, promptly get Na
2O-CaO-SiO
2-P
2O
5The bio-vitric powder, each material consists of: 22% quicklime, 7% Vanadium Pentoxide in FLAKES, 22% sodium oxide and 49% silicon-dioxide;
(2) hydrochloric acid catalyst and the 400.00mL tetraethoxysilance of adding 249.6mL deionized water, 38.40mL 2mol/L in beaker; After stirring hydrolysis 30min at ambient temperature; Add the 103.76g four water-calcium nitrate again, stir the colloidal sol that the back obtains transparent stable homogeneous; The at room temperature still aging 48h of colloidal sol fully carries out hydrolysis-condensation reaction, forms wet gel; Wet gel placed 140 ℃ of dryings 2 days, obtained xerogel after making solvent evaporation; Xerogel is obtained particulate state bioactive sol-gel glass in 650 ℃ of heat treatment for solidification technologies; With the speed ball milling 3h of 480rpm, cross 200 mesh sieves, promptly get CaO-SiO
2The bio-vitric powder, each material consists of: 20% quicklime and 80% silicon-dioxide;
(3) with 1gNa
2O-CaO-SiO
2-P
2O
5Bio-vitric powder and 99gCaO-SiO
2The bio-vitric powder mixes, and adds the 67mL volume(tric)fraction and is in 6% the ROHM amine aqueous solution, and 3 hours mixings of ball milling obtain volume(tric)fraction and be 60% bio-vitric slurry;
(4) the bio-vitric slurry that step (1) is obtained dropwise adds in the unsaturated polyester resin polymer reverse; Reverse is carried out centrifugal grouting with 1000r/min in the appearance L550 type whizzer of Hunan; After placing 72 ℃ of water-baths to solidify 1.5h; Be positioned in the loft drier in 60 ℃ of dry 60h, obtain solid material;
(5) solid material is put into the zirconium white saggar, keep 1.5h after with the speed of 2 ℃/min the temperature of solid material being risen to 950 ℃; Naturally be cooled to 20 ℃, make the biological activated glass ceramic material that is used for the bone defect repair.
Fig. 1 is the micro-CT photo of the biological active glass ceramic bone renovating material of the embodiment of the invention 1 preparation; Can find out; Bone renovating material of the present invention has the stack type pore passage structure, such microstructure helps organizing grow into transmission and metabolism with nutritive substance.
Fig. 2 is the SEM photo on the biological active glass ceramic bone renovating material surface of the embodiment of the invention 1 preparation, can see that partial crystallization appears in material, and this makes material have better mechanical property.
Claims (10)
1. be used for the preparation method of the biological activated glass ceramic material of bone defect repair, it is characterized in that, comprise the steps:
(1) the bio-vitric powder is sieved, add the ROHM amine aqueous solution, milling mixing obtains the bio-vitric slurry;
(2) the bio-vitric slurry that step (1) is obtained dropwise adds in the polymer reverse, and the polymer reverse is carried out centrifugal grouting in whizzer, in 70 ~ 75 ℃ of water-baths, solidify 1 ~ 2h after, 50 ~ 70 ℃ of drying 48 ~ 72h obtain solid material;
(3) solid material that step (2) is obtained is removed the polymer reverse in 900 ~ 1000 ℃ of calcinings under temperature programmed control, make the biological activated glass ceramic material that is used for the bone defect repair.
2. preparation method according to claim 1 is characterized in that, said bio-vitric powder is Na
2O-CaO-SiO
2-P
2O
5Bio-vitric powder and/or CaO-SiO
2-P
2O
5The bio-vitric powder.
3. preparation method according to claim 2 is characterized in that, said Na
2O-CaO-SiO
2-P
2O
5The material of bio-vitric powder is formed mass percent: quicklime 20 ~ 25%, Vanadium Pentoxide in FLAKES 5 ~ 7%, sodium oxide 20 ~ 25%, silicon-dioxide 43 ~ 49%; Said CaO-SiO
2-P
2The material of O bio-vitric powder is formed mass percent: quicklime 14 ~ 33%, Vanadium Pentoxide in FLAKES 0 ~ 9%, silicon-dioxide 58 ~ 80%.
4. preparation method according to claim 3 is characterized in that, the volume(tric)fraction of bio-vitric powder is 50 ~ 60% in the said bio-vitric slurry.
5. preparation method according to claim 4 is characterized in that, the pore dimension of said polymer reverse is 500 ~ 1000 microns, and geometrical shape is cubes, rectangular parallelepiped or right cylinder.
6. according to the described preparation method of one of claim 1 ~ 5, it is characterized in that the process of said temperature programmed control comprises following three phases:
(1) temperature rise period: the temperature of solid material is risen to 900 ~ 1000 ℃ with the speed of 2 ~ 3 ℃/min;
(2) holding stage: the temperature of solid material is kept 1 ~ 2h at 900 ~ 1000 ℃;
(3) temperature-fall period: be cooled to 10 ~ 30 ℃ naturally.
7. preparation method according to claim 6 is characterized in that, the volume(tric)fraction of poly amic acid is 4 ~ 8% in the said ROHM amine aqueous solution.
8. preparation method according to claim 7 is characterized in that, the rotating speed of said centrifugal grouting is 800 ~ 1200r/min.
9. preparation method according to claim 8 is characterized in that, said polymer reverse is photosensitive resin reverse or polymkeric substance reverse.
10. preparation method according to claim 9 is characterized in that said photosensitive resin is a unsaturated polyester resin, comprises gathering meso lactic acid or polycaprolactone; Said polymkeric substance is polylactic acid-glycolic guanidine-acetic acid multipolymer or acrylonitrile-butadiene-styrene copolymer.
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