CN1323986C - Method for preparing CaO-P2O5-MgO glass reinforced porous beta-tricalcium phosphate bioceramics - Google Patents
Method for preparing CaO-P2O5-MgO glass reinforced porous beta-tricalcium phosphate bioceramics Download PDFInfo
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- CN1323986C CN1323986C CNB2006100133348A CN200610013334A CN1323986C CN 1323986 C CN1323986 C CN 1323986C CN B2006100133348 A CNB2006100133348 A CN B2006100133348A CN 200610013334 A CN200610013334 A CN 200610013334A CN 1323986 C CN1323986 C CN 1323986C
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Abstract
The present invention relates to a preparation method for CaO-P2O5-MgO glass reinforced porous beta-tricalcium phosphate bioceramic, which belongs to the technical field of the preparation for bioceramic. The present invention is characterized in that a raw material formula is weighed and taken according to the mass percent that P2 O5 to CaO to Na2 O to MgO equals to 62 to 41.4: 14.7 to 9.80: 18 to 12: 5.30 to 3.50, bioglass is obtained through fusion and devitrification heat treatment, and the components of the bioglass comprise sodium pyrophosphate and sodium phosphate calcium magnesium salt. The bioglass is added to beta-tricalcium phosphate powder, the mass ratio of the bioglass to the beta-tricalcium phosphate powder is 10 to 30%, and the porous bioceramic is prepared through a foam dipping method. The present invention has the advantages of high porosity of the porous ceramic which is prepared by the method, high intensity and good biological specificity, and can be used for bony tissue coloboma and repair and porous bioceramic of brackets of cell culture in vitro, drug release carriers, etc.
Description
Technical field
The present invention relates to a kind of CaO-P
2O
5-Na
2O-MgO glass strengthens porous bata-tricalcium phosphate biological ceramics preparation method, belongs to the biological ceramics preparing technical field.
Background technology
Porous biomaterial has irreplaceable function in organizational project, the series of calcium phosphate material has been widely used in Orthopeadic Surgery, plastic surgery and dental field because of its excellent biological compatibility and biological activity are considered to prepare the best bone renovating material of porous articles such as bionical bone, support and carrier.Bata-tricalcium phosphate is important binary compound in the calcium phosphorus system, generally believe it is a kind of absorbable biological active ceramic material, behind its implant into body, the energy degradation in vivo, the Ca that degrades, P enter the live body recycle system and form area of new bone, have excellent biological compatibility and bone inducibility.Merge speed in order to satisfy the needs that different tissues grows into and to increase bone, bone renovating material must be to have the porous material that high porosity, macropore connect mutually.Its ideal aperture size is 50～400 μ m, and porosity should be greater than 70%.But high porosity and low intensive contradiction restrict this Development of Materials and application always, and the ultimate compression strength of the series of calcium phosphate porous material of having reported at present is 0.3～3.3MPa, also is not enough to satisfy requirements for clinical application.Carried out the mechanical property that a large amount of correlative studys are intended to keep strongthener on the basis of high porosity in recent years, find that the interpolation of glassy phase not only can effectively improve the mechanical property of porous insert, also can regulate the degradation rate of bata-tricalcium phosphate simultaneously, make it to be complementary with new osteogenesis speed.
The patent of relevant bioactivity glass synthetic method is more, and as CN 03149539.7, US 5,675,720, and US 5,125971, US6,413,538 etc.Chinese patent 03149539.7 has been introduced at CaO-SiO
2Pass through to add Na in the system
2O, CaF
2Or B
2O
3The synthetic P that do not contain
2O
5Glass, and use this bioactivity glass to prepare the method for calcium phosphate glass sintered compact as sintering agent.Another kind of common bio-vitric system is at SiO
2-P
2O
5Add basic metal or alkaline earth metal oxide in the matrix.As United States Patent (USP) 5,675,720 disclose and have consisted of CaO-Na
2O-SiO
2-P
2O
5The preparation method of multiporous biological glass material; Equally, patent US6,413,538 have introduced method and the biological nature thereof with this type of glass preparation biological hard tissue material.Bio-vitric improves the sintering character of matrix body and Mechanical Properties is existing reports by adding in calcium phosphate ceramic.The bio-vitric composition is mainly and contains SiO
2The glass system, the vitreum that adopts as U.S. Pat 5,125971 is: CaO-MgO-Na
2O-SiO
2Clinically confirmed that these contain SiO
2Glass has good biocompatibility, and when weighting material of repairing as sclerous tissues or equivalent material, vitreum forms silicon-rich layer by dissolving-being deposited on the interface in body fluid, helps Ca in the body fluid
2+, PO
3-Ion migration is to the host interface, forms the amorphous calcium phosphate film on silicon-rich layer, again with body fluid in OH
-And CO
3 2-In conjunction with generation class phosphatic rock, thereby with the host take place glutinous the company and fusion.But SiO
2Not the moiety of human body hard tissue, can not degradation in vivo, so this class glass can only be considered as the material of biologically active, and finally can not become the part of tissue.
Carry out in recent years with CaO-P
2O
5Be discovering of glass host material: CaO-P
2O
5The vitreum cording has more excellent biological activity, mechanical property and workability.Toshihiro Kasuga (Bioactivecalcium pyrophosphate glasses and glass-ceramics, Acta Biomaterials, 1 (2005) 55-64) has reported 60CaO-30P
2O
5-3TiO
2-7Na
2The preparation method of O glass and glass-pottery and correlated performance are CaO-P
2O
5The exploitation of system bio-vitric and ceramics-glass provides foundation.
Summary of the invention
The object of the present invention is to provide a kind of CaO-P
2O
5-Na
2O-MgO glass strengthens porous bata-tricalcium phosphate biological ceramics preparation method, porous ceramics hole with this method preparation connects, have higher intensity and good biological nature, the porous bio-ceramic of can be used for that osseous tissue is damaged, reparation and cell in vitro being cultivated support and drug release carrier etc.
The present invention is realized by the following technical programs, a kind of CaO-P
2O
5-Na
2O-MgO glass strengthens porous bata-tricalcium phosphate biological ceramics preparation method; It is characterized in that comprising following process:
1. with P
2O
5, CaO, Na
2O and MgO, by its mass ratio is (62～41.4): (14.7～9.80): (18～12): the raw material ground and mixed of (5.30～3.50) is even, slowly add deionized water, stir, do not emerge to there being bubble, dry back made the block bio-vitric of oyster white in 900～980 ℃ of fusion 1-2 hours, grind sieve, standby;
2. above-mentioned bio-vitric is carried out following thermal treatment: 700～720 ℃ are incubated half an hour, are cooled to room temperature; 740～750 ℃ are incubated 1 hour, and in 800 ℃ of insulations 2 hours, furnace cooling, gained composition were the bio-vitric of trisodium phosphate and sodium phosphate calcium magnesium salts again;
3. trisodium phosphate is very easily water-soluble, and solution is strong basicity, adds deionized water before the preparation slip in the bio-vitric powder, constantly stirs, and removes container clear liquid at the middle and upper levels, is 7～8.5 until pH value of solution for several times repeatedly;
4. be 1.5 accurately to take by weighing CaCO by the Ca/P mol ratio
3And CaHPO
42H
2O makes the bata-tricalcium phosphate that median size is 380nm (β-TCP) by the mechanical-chemical hybrid system; Add by step 1 and 2 prepared bio-vitrics in β-TCP powder, its mass percent is 10～30%, and adding volumetric molar concentration in mixed powder is the ammonium polyacrylate (PAANH of 0.02mol/ml
4) dispersion agent, the consumption of ammonium polyacrylate is to add 0.08～0.1ml in every gram mixed powder, adds deionized water again, and ball milling made good fluidity in 30～50 minutes, and solid load is 60～70% slurry; Urethane or polyethers porous foam with moulding immerses in this slurry then, and the dipping body is dried to base substrate under wet environment, and base substrate again in 1000～1100 ℃ of sintering 2～4 hours, obtains porous bata-tricalcium phosphate biological ceramics 1 after the cooling after 550～600 ℃ of pre-burnings
Prepare above-mentioned bio-vitric and adopt P
2O
5Compound be NH
4H
2PO
4Or (NH
4)
2HPO
4Or both mixtures;
The compound for preparing above-mentioned bio-vitric employing CaO is CaCO
3Or Ca (OH)
2
Prepare above-mentioned bio-vitric and adopt Na
2The compound of O is Na
2CO
3
The compound for preparing above-mentioned bio-vitric employing MgO is MgCO
3, Mg (OH)
2Or (MgCO
3)
4Mg (OH)
25H
2O;
The porosity that the glass of present method preparation strengthens the bata-tricalcium phosphate porous bio-ceramic is 45～93%, and pore diameter range is 50～600 μ m, and pore distribution is even, and the ultimate compression strength of material is at 1.5～17MPa.Scleroblast and porous ceramics support are united cultivation, and the result shows: support sticks respond wellly to osteoblastic, is suitable for cell adhesion, creeps.
Description of drawings
The X-ray diffracting spectrum of the bio-vitric that Fig. 1 makes for the embodiment of the invention 1;
The glass that Fig. 2 makes for the embodiment of the invention 3 strengthens the Photomicrograph of bata-tricalcium phosphate porous bio-ceramic;
Fig. 3 is the Photomicrograph of MC3T3-E1 cell on the carrier that the embodiment of the invention 3 makes after cultivating a week in the DMEM nutrient solution (Gibco, the U.S.);
Fig. 4 is the Photomicrograph of the porous material of MC3T3-E1 cell on the carrier that the embodiment of the invention 3 makes after cultivating a week in the DMEM nutrient solution (Gibco, the U.S.).
Embodiment
Embodiment 1:CaO-P
2O
5-Na
2The O-MgO bio-vitric
With NH
4H
2PO
4, Ca (OH)
2, Na
2CO
3, (MgCO
3)
4Mg (OH)
25H
2O is a raw material, presses the P in the raw material
2O
5: CaO: Na
2O: the MgO mass percent is 62: 14.7: 18: 5.30, and total mass is 100 grams, accurately takes by weighing 47.12 gram NH
4H
2PO
4, 19.45 gram Ca (OH)
2, 30.19 gram Na
2CO
3With 63.69 gram (MgCO
3)
4Mg (OH)
25H
2O.Alleged former abrasive lapping is even, pour in the beaker, slowly add deionized water, and constantly stir, emerge until no bubble.With compound in baking oven in 80 ℃ of freeze-day with constant temperature, carry out igneous fusion then, its system is: at 300～400 ℃ and 700～800 ℃ of temperature sections, temperature rise rate is 1.5 ℃/minute, at 400 ℃～700 ℃ and 700 ℃～910 ℃ temperature sections, temperature rise rate is 3.5 ℃/minute, is warming up to 910 ℃ of insulations 1 hour.Glass after the fusion with the furnace temperature naturally cooling, grind, sieve.With the glass powder after grinding 700 ℃ of thermal treatment half an hour, be cooled to room temperature, be warming up to 740 ℃ of insulations 1 hour again, then in 800 ℃ of thermal treatments 2 hours, with the furnace temperature naturally cooling, after heat treatment the composition of gained bio-vitric is the composite granule of trisodium phosphate and sodium phosphate calcium magnesium salts.
Embodiment 2:CaO-P
2O
5-Na
2The O-MgO bio-vitric
With (NH
4)
2HPO
4, CaCO
3, Na
2CO
3, MgCO
3Be raw material, press the P in the raw material
2O
5: CaO: Na
2O: the MgO mass percent is 41.4: 9.80: 12: 3.50, and total mass is 50 grams, accurately takes by weighing 26.98 gram (NH
4)
2HPO
4, 13.06 gram CaCO
3, 15.40 gram Na
2CO
3With 5.46 gram MgCO
3Alleged former abrasive lapping is even, pour in the beaker, slowly add deionized water, and constantly stir, emerge until no bubble.With compound in baking oven in 80 ℃ of freeze-day with constant temperature, carry out igneous fusion then, its system is: at 300～400 ℃ and 700～800 ℃ of temperature sections, temperature rise rate is 1.5 ℃/minute, at 400 ℃～700 ℃ and 700 ℃～980 ℃ temperature sections, temperature rise rate is 3.5 ℃/minute, is warming up to 980 ℃ of insulations 2 hours.Glass after the fusion grinds, sieves with the stove naturally cooling.Glass fine powder after grinding 720 ℃ of thermal treatment half an hour, is cooled to room temperature, is warming up to 750 ℃ of insulations 1 hour again, then in 800 ℃ of thermal treatments 2 hours, with the stove naturally cooling.After heat treatment the composition of gained bio-vitric is the composite granule of trisodium phosphate and sodium phosphate calcium magnesium salts.
Embodiment 3: glass strengthens tricalcium phosphate porous ceramic
Raw material: with medical grade lime carbonate (CaCO
3) and dicalcium phosphate dihydrate (CaHPO
42H
2O) be raw material, by the Ca/P mol ratio be 1.5 accurately take by weighing 171.1 the gram CaHPO
42H
2O and 50.0 gram CaCO
3, institute's weighing is poured in the ball grinder, add deionized water and zirconium oxide balls.By material: abrading-ball: water is to carry out proportioning at 1: 3: 2.2 by mass ratio, with compound high speed ball milling 16 hours in baking oven in 85 ℃ of freeze-day with constant temperature, dry back is 830 ℃ of calcinings, obtaining median size is the beta-calcium phosphate powder of 380nm.
Technology: the bio-vitric that bata-tricalcium phosphate and embodiment 1 are made is to take by weighing the mixed powders that gross weight is 50 grams at 80: 20 by mass percentage, measure 33 ml deionized water, adding volumetric molar concentration in deionized water is the 4 ml polypropylenes acid ammonium of 0.02mol/ml, mix grinding is 30 minutes on the particle sphere grinding machine, abrading-ball is an agate ball, makes the solid load mass ratio and be 60% slurry; Slip after grinding is poured in the charge groove, polyurethane sponge is immersed in the slip, the sponge that will be soaked with slip is then taken out, and by muller the unnecessary slip in the sponge is ground; The sponge formed body that is wrapped up by slip humidity greater than 90% environment in after dry 12 hours, dry in baking oven again; Drying temperature is 80 ℃, the pre-burning in sintering oven of dry sample, and heating schedule is: room temperature to 180 ℃ is 2 ℃/minute, and 180～400 ℃ is 0.8 ℃/minute, and 400～600 ℃ is 1.2 ℃/minute; The pre-burning sample directly is warming up to 1000 ℃, and heat-up rate is 2.5 ℃/minute, is incubated 4 hours, can obtain porosity and be 79% porous ceramics, and pore size is between 100～650 μ m, and mean compressive strength is 3.8MPa.
Embodiment 4: glass strengthens tricalcium phosphate porous ceramic
With embodiment 3 prepared bata-tricalcium phosphates and bio-vitric is to take by weighing the mixed powders that gross weight is 100 grams at 90: 10 by mass percentage, measure 43 ml deionized water, in deionized water, add 10 ml polypropylenes acid ammonium, mix grinding is 40 minutes on the particle sphere grinding machine, abrading-ball is an agate ball, makes the solid load mass ratio and be 70% slurry; Slip after grinding is poured in the charge groove, polyurethane sponge is immersed in the slip, the sponge that will be soaked with slip is then taken out, and by muller the unnecessary slip in the sponge is ground; The sponge formed body that is wrapped up by slip humidity greater than 90% environment in after dry 12 hours, dry in baking oven again; The pre-burning in sintering oven of dry sample, heating schedule is: room temperature to 180 ℃ is 2 ℃/minute, and 180～400 ℃ is 0.8 ℃/minute, and 400～600 ℃ is 1.2 ℃/minute; The pre-burning sample directly is warming up to 1000 ℃, and heat-up rate is 2.5 ℃/minute, is incubated 4 hours, can obtain porosity and be 84% porous ceramics, and pore size is between 50～500 μ m, and mean compressive strength is 2.1MPa.
Embodiment 5: Bioexperiment
Embodiment 3 prepared porous ceramicss are carried out cell adhesion, growth and propagation test; Concrete grammar is: the porous support to embodiment 3 carries out high temperature, autoclave sterilization, prefabricated being of a size of: 0.5cm * 0.5cm * 1.5cm, totally 12 (sterile packed), prefabricated 12 of unidimensional allograph bone (sterile packed).To make 1 * 10 behind about about 90% MC3T3-E1 cell dissociation, washing, the centrifugal counting at the bottom of covering with bottle
6The cell suspension of/ml, negative pressure is inoculated on cytoskeleton and the allograph bone respectively, puts 37 ℃, 5%CO
2Take out after cultivating 4h in the saturated humidity cell culture incubator.Again compound rest is placed 35mm * 10mm culture dish respectively, add the nutrient solution that contains 10% foetal calf serum, put cell culture incubator in 37 ℃, 5%CO
2And cultivate under the saturated humidity condition.Cultivate 4 of porous osteocyte ceramics brackets respectively at cultivating respectively to get in the 1st day, 3 days, 5 days to unite, PBS liquid washes repeatedly, add 5% tryptic digestive juice digestion 10 minutes, draw Digestive system flushing timbering material, the MC3T3-E1 cell is come off fully, collect washing fluid and end digestion, be settled to 4ml after every porous ceramics support and allograph bone washing fluid are centrifugal, carry out cell counting and observation of cell form under opticmicroscope.Fig. 3 and Fig. 4 are the Photomicrograph the MC3T3-E1 cell is cultivated a week in the DMEM nutrient solution after, and can be observed porous osteocyte ceramics bracket and scleroblast has the good ability that conforms in external environment.Table 1 is to cultivate the propagation quantity of scleroblast on differing materials after 1 day, 3 days and 5 days, statistical result is presented at otherness index P＜0.05 of cultivating the 1st, 3,5 day two groups of data, there were significant differences, show prolongation with incubation time, osteoblastic quantity has had tangible increase in the cytoskeleton, the proof scleroblast has carried out normal propagation in support, can normal growth, and performance is better than the allograph bone support.
The propagation quantity of table 1 scleroblast on differing materials
Claims (5)
1. CaO-P
2O
5-Na
2O-MgO glass strengthens porous bata-tricalcium phosphate biological ceramics preparation method, it is characterized in that comprising following process:
(1). with P
2O
5, CaO, Na
2O and MgO, by its mass ratio is (62～41.4): (14.7～9.80): (18～12): the raw material ground and mixed of (5.30～3.50) is even, slowly add deionized water, stir, do not emerge to there being bubble, dry back made the block bio-vitric of oyster white in 900～980 ℃ of fusion 1-2 hours, grind sieve, standby;
(2). above-mentioned bio-vitric is carried out following thermal treatment: 700～720 ℃ are incubated half an hour, are cooled to room temperature; 740～750 ℃ are incubated 1 hour, and in 800 ℃ of insulations 2 hours, furnace cooling, gained composition were the bio-vitric of trisodium phosphate and sodium phosphate calcium magnesium salts again;
(3). trisodium phosphate is very easily water-soluble, and solution is strong basicity, adds deionized water before the preparation slip in the bio-vitric powder, constantly stirs, and removes container clear liquid at the middle and upper levels, is 7～8.5 until pH value of solution for several times repeatedly;
(4). by the Ca/P mol ratio is 1.5 accurately to take by weighing CaCO
3And CaHPO
42H
2O makes the bata-tricalcium phosphate that median size is 380nm by the mechanical-chemical hybrid system; In β-TCP powder, add by step (1) and (2) prepared bio-vitric, its mass percent is 10～30%, adding volumetric molar concentration in mixed powder is the ammonium polyacrylate dispersion agent of 0.02mol/ml, the consumption of ammonium polyacrylate is to add 0.08～0.1ml in every gram mixed powder, add deionized water again, ball milling made good fluidity in 30～50 minutes, and the solid phase mass content is 60～70% slurry; Urethane or polyethers porous foam with moulding immerses in this slurry then, the dipping body is dried to base substrate under wet environment, base substrate again in 1000～1100 ℃ of sintering 2～4 hours, obtains porous bata-tricalcium phosphate biological ceramics after the cooling after 550～600 ℃ of pre-burnings.
2. by the described CaO-P of claim 1
2O
5-Na
2O-MgO glass strengthens porous bata-tricalcium phosphate biological ceramics preparation method, it is characterized in that, the preparation bio-vitric adopts P
2O
5Compound be NH
4H
2PO
4Or (NH
4)
2HPO
4Or both mixtures.
3. by the described CaO-P of claim 1
2O
5-Na
2O-MgO glass strengthens porous bata-tricalcium phosphate biological ceramics preparation method, it is characterized in that, it is CaCO that the preparation bio-vitric adopts the compound of CaO
3Or Ca (OH)
2
4. by the described CaO-P of claim 1
2O
5-Na
2O-MgO glass strengthens porous bata-tricalcium phosphate biological ceramics preparation method, it is characterized in that, the preparation bio-vitric adopts Na
2The compound of O is Na
2CO
3
5. by the described CaO-P of claim 1
2O
5-Na
2O-MgO glass strengthens porous bata-tricalcium phosphate biological ceramics preparation method, it is characterized in that, it is MgCO that the preparation bio-vitric adopts the compound of MgO
3, Mg (OH)
2Or (MgCO
3)
4Mg (OH)
25H
2O.
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| CN101050062B (en) * | 2007-05-15 | 2010-05-19 | 中国人民解放军第二军医大学 | Method for preparing slow releasing carrier of medication of microcrystalline glass in series of calcium phosphate |
| CN101695586B (en) * | 2009-10-30 | 2012-11-07 | 河北工业大学 | High-intensity porous bone repair material and method for preparing same |
| CN101857372B (en) * | 2010-06-17 | 2011-11-30 | 天津大学 | Nanometer metallic in-situ grown and enhanced porous calcium-phosphorus glass ceramic and preparation method thereof |
| CN102743794B (en) * | 2011-04-20 | 2014-09-24 | 国家纳米科学中心 | Medicinal slow release support and preparation method thereof |
| CN102517636A (en) * | 2011-12-23 | 2012-06-27 | 许国华 | In-situ grown nano-grade hydroxyapatite whisker powder, porous ceramic, preparation methods thereof, and applications thereof |
| CN102886072A (en) * | 2012-10-09 | 2013-01-23 | 天津大学 | Degraded glass ceramic thin film for medical magnesium alloy surface and preparation method of degraded glass ceramic thin film |
| CN104045365B (en) * | 2013-03-12 | 2016-08-17 | 珠海霍普金斯医药研究院股份有限公司 | A kind of method preparing calcium pyrophosphate crystal whisker toughened organizational project cancellous bony material |
| CN104030718B (en) * | 2014-05-20 | 2015-08-19 | 广州医科大学 | Porous calcium carbonate ceramic of a kind of trace elements that adulterates and its preparation method and application |
| CN104721880B (en) * | 2015-02-11 | 2017-06-20 | 华东理工大学 | β tricalcium phosphates/mesoporous bioglass compound rest and preparation method and application |
| CN106007699B (en) * | 2016-05-23 | 2019-01-11 | 广州医科大学 | Bata-tricalcium phosphate/calcium carbonate biphase ceramics material and preparation method thereof |
| CN107056274A (en) * | 2017-03-31 | 2017-08-18 | 合肥图腾龙医疗用品开发有限公司 | A kind of bioceramic material and preparation method thereof |
| CN107892561A (en) * | 2017-11-03 | 2018-04-10 | 常州通和建筑工程有限公司 | A kind of preparation method of high-strength degradable multiporous bioceramic |
| CN108395236A (en) * | 2018-01-25 | 2018-08-14 | 合肥中科富华新材料有限公司 | A kind of preparation method and applications of bioceramic |
| TWI764332B (en) * | 2020-10-22 | 2022-05-11 | 擎睿生醫有限公司 | Bone graft composition |
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