CN103641466B - Stephanoporate calcium polyphosphate biomaterial preparation method - Google Patents
Stephanoporate calcium polyphosphate biomaterial preparation method Download PDFInfo
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- CN103641466B CN103641466B CN201310727005.XA CN201310727005A CN103641466B CN 103641466 B CN103641466 B CN 103641466B CN 201310727005 A CN201310727005 A CN 201310727005A CN 103641466 B CN103641466 B CN 103641466B
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- monocalcium phosphate
- calcining
- calcium polyphosphate
- biomaterial
- stephanoporate
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- 239000004132 Calcium polyphosphate Substances 0.000 title claims abstract description 25
- 235000019827 calcium polyphosphate Nutrition 0.000 title claims abstract description 25
- 239000012620 biological material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 claims abstract description 52
- 239000001506 calcium phosphate Substances 0.000 claims abstract description 52
- 229910000150 monocalcium phosphate Inorganic materials 0.000 claims abstract description 52
- 235000019691 monocalcium phosphate Nutrition 0.000 claims abstract description 52
- 238000001354 calcination Methods 0.000 claims abstract description 39
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 10
- 229910052573 porcelain Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 32
- 210000000988 bone and bone Anatomy 0.000 abstract description 17
- 230000007547 defect Effects 0.000 abstract description 12
- 238000006068 polycondensation reaction Methods 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 description 10
- 238000005245 sintering Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000004321 preservation Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 230000004071 biological effect Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000009837 dry grinding Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 2
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000002054 transplantation Methods 0.000 description 2
- 208000027205 Congenital disease Diseases 0.000 description 1
- 208000029767 Congenital, Hereditary, and Neonatal Diseases and Abnormalities Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 206010052428 Wound Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 239000004068 calcium phosphate ceramic Substances 0.000 description 1
- MWKXCSMICWVRGW-UHFFFAOYSA-N calcium;phosphane Chemical compound P.[Ca] MWKXCSMICWVRGW-UHFFFAOYSA-N 0.000 description 1
- 210000000845 cartilage Anatomy 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000000278 osteoconductive effect Effects 0.000 description 1
- 230000007170 pathology Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
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- Materials For Medical Uses (AREA)
Abstract
The present invention relates to stephanoporate calcium polyphosphate biomaterial preparation method, belong to biomedical materials field, comprise step (1) calcining monocalcium phosphate; (2) monocalcium phosphate after calcining is not calcined monocalcium phosphate mix with appropriate; (3) mixture that step 2 obtains at high temperature is sintered.The present invention utilizes the characteristic of monocalcium phosphate high-temperature polycondensation, makes himself polycondensation pore-forming define Bone Defect Repari stephanoporate calcium polyphosphate biomaterial, avoids the introducing of other impurity, can ensure the pure of material to greatest extent.
Description
Technical field
The present invention relates to stephanoporate calcium polyphosphate biomaterial preparation method, belong to biomedical materials field.
Background technology
The joint cartilage caused because of all multi-pathogenesis such as wound, tumour, infection, congenital disorders and Cranial defect very common clinically, its reparation is one of difficult problem of international Osteopathic Medicine always.For a long time, bone defect healing mainly takes autologous or allogenic bone transplantation, but autologous bone transplanting also exists serious defect in material source, increases extra wound and cost to patient, get bony site and pathology may occur, and available autologous bone source is very limited.Heteroplastic transplantation aspect, quite difficult, expensive in material screening, process, storage, also easily produce immunological rejection, and may cause the problems such as the introducing of pathogeny, operative failure rate is higher.
Calcium orthophosphate base biomaterial has similar composition to the mineral in bone, and possess good biological degradability, biological activity and osteoconductive, be prepared into and the high strength support of bone photo like functional structure by shaping, sintering process, implanting the calcium phosphorus product after degraded can be used for new bone remoulding as raw material by scleroblast.Therefore, the calcium phosphate ceramic material being representative with hydroxyapatite (HA), β tricalcium phosphate (β-TCP) becomes the study hotspot of bio-medical material, and is achieving market segment development in recent years.
From based materials by after biomedical boundary investigation and application, calcium polyphosphate (CPP) is also studied is gradually a kind of new type bone tissue engineering material having biological activity, controllable biodegradable and higher force performance with confirming, cause extensive concern both domestic and external in recent years, become the engineering material of bone tissue of a new generation.The domestic and international preparation to porous C PP at present mainly adopt melting → wire drawing → shrend → oven dry → ethanol wet-milling → interpolation pore-forming material shaping → sintering preparation technology, the deficiency of this mode is: easily pollute material, causes purity not reach medical rank; Sintering schedule also because of uncontrollable polyreaction, influencing each other between crystal conversion temperature and material vesicular structure, and causes failing obtaining desirable material property, limits CPP material carrying out in clinical study and application aspect.
Summary of the invention
According to above the deficiencies in the prior art, the object of the invention is to: a kind of stephanoporate calcium polyphosphate biomaterial preparation method is provided, simple, fully meet the medical requirement that material is pure, stable.
Stephanoporate calcium polyphosphate biomaterial preparation method of the present invention, comprises the steps:
(1) monocalcium phosphate is calcined;
(2) monocalcium phosphate after calcining is not calcined monocalcium phosphate mix with appropriate;
(3) mixture that step 2 obtains at high temperature is sintered.
In step 1, monocalcium phosphate calcining temperature is 300 ~ 500 DEG C.
In step 1, monocalcium phosphate calcining temperature is 650 ~ 750 DEG C.
Monocalcium phosphate in step 2 after calcining with not calcine monocalcium phosphate mass ratio be 1:(0 ~ 3).
Monocalcium phosphate in step 2 after calcining with not calcine monocalcium phosphate mass ratio be 1:(0.5 ~ 4).
Soaking time is 1 ~ 2 hour.
Mixture step 2 obtained grinds, and the powder after grinding sieves, and gets the powder that particle diameter is 100 ~ 500 μm, puts into crucible compacting, is incubated 1 ~ 2 hour under being then heated to 950 ~ 970 DEG C of conditions.
Monocalcium phosphate molecular formula is Ca (H
2pO
4)
2, its chemical equation at high temperature calcined is as follows:
Experimental data shows, monocalcium phosphate is after 300 ~ 500 DEG C or 650 ~ 750 DEG C of calcinings, and have obvious weightlessness, this is mainly due to monocalcium phosphate generation polycondensation, and the crystal water in it runs off rapidly and causes.After the crystal water in early stage runs off, because whole reaction system is still solid-state, the water in it can not volatilize completely, makes calcium polyphosphate DeR occur simultaneously, and its reaction process is the inverse process of above-mentioned reaction:
When after monocalcium phosphate calcining certain hour, reaction reaches balance, no longer has obvious weightlessness.Appropriate monocalcium phosphate of not calcining is mixed with the monocalcium phosphate after calcining, grind, sieves, 1 ~ 2 hour is incubated under mixture being heated to 950 ~ 970 DEG C of conditions, monocalcium phosphate after calcining and do not calcine monocalcium phosphate and polycondensation occurs simultaneously be converted into calcium polyphosphate, because weightless degree is different, both mix and generate stephanoporate calcium polyphosphate after reacting, and the porosity of calcium polyphosphate can be controlled by the particle diameter grinding rear powder.
The present invention utilizes the characteristic of monocalcium phosphate high-temperature polycondensation, makes himself polycondensation pore-forming define Bone Defect Repari stephanoporate calcium polyphosphate biomaterial.Doing so avoids the introducing of other impurity, the pure of material can be ensured to greatest extent.Thus make this material only containing the skeletonization such as calcium, phosphorus element, as calcium source stable in New born formation and phosphorus source, can fully meet medically pure, stable requirement.And the aperture, inside of final calcium polyphosphate biomaterial can be controlled by the particle diameter controlling grinding powder, various cell can be better met, the growth of blood vessel, thus repair various Cranial defect better.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
Calcining monocalcium phosphate:
Weigh in the balance and get Powdered monocalcium phosphate 300g, put into quartz crucible, after adding a cover protection, put into electric furnace, be warming up to 350 DEG C with the speed of 4 DEG C/m, be incubated naturally cooling after 1 ~ 2 hour, thus obtain the calcining material of loose bulk.After this calcining material mortar or ball mill crushing, put into loft drier for subsequent use.
Monocalcium phosphate after calcining is not calcined monocalcium phosphate mix with appropriate:
Take calcining material 80g, Powdered monocalcium phosphate 20g respectively, after mixing, use ball mill dry ball milling 1 minute, obtained powder is crossed 40 orders and 80 mesh sieves, get the triage on 80 mesh sieves, gained powder particle size is about 200 ~ 400 μm.
Mixture at high temperature sinters:
The powder prepared is put into crucible and compacting, then crucible is put into electric furnace and sinter.Temperature rise rate is: room temperature to 200 DEG C is 2 DEG C/m, and 200 DEG C ~ 960 DEG C is 4 DEG C/m, and heat preservation sintering 2 hours, makes it fully sinter porcelain into.After naturally cooling, obtained aperture is about the Bone Defect Repari stephanoporate calcium polyphosphate biomaterial of 100 ~ 400 μm.
Embodiment 2
Calcining monocalcium phosphate:
Weigh in the balance and get Powdered monocalcium phosphate 300g, put into quartz crucible, after adding a cover protection, put into electric furnace, be warming up to 500 DEG C with the speed of 4 DEG C/m, be incubated naturally cooling after 1 ~ 2 hour, thus obtain the calcining material of loose bulk.After this calcining material mortar or ball mill crushing, put into loft drier for subsequent use.
Monocalcium phosphate after calcining is not calcined monocalcium phosphate mix with appropriate:
Take calcining material 80g, Powdered monocalcium phosphate 240g respectively, after mixing, use ball mill dry ball milling 1 minute, obtained powder is crossed 40 orders and 120 mesh sieves, get the triage on 120 mesh sieves, gained powder particle size is about 100 ~ 400 μm.
Mixture at high temperature sinters:
The powder prepared is put into crucible and compacting, then crucible is put into electric furnace and sinter.Temperature rise rate is: room temperature to 200 DEG C is 2 DEG C/m, and 200 DEG C ~ 950 DEG C is 4 DEG C/m, and heat preservation sintering 2 hours, makes it fully sinter porcelain into.After naturally cooling, obtained aperture is about the Bone Defect Repari stephanoporate calcium polyphosphate biomaterial of 100 ~ 400 μm.
Embodiment 3
Calcining monocalcium phosphate:
Weigh in the balance and get Powdered monocalcium phosphate 300g, put into quartz crucible, after adding a cover protection, put into electric furnace, be warming up to 300 DEG C with the speed of 4 DEG C/m, be incubated naturally cooling after 1 ~ 2 hour, thus obtain the calcining material of loose bulk.After this calcining material mortar or ball mill crushing, put into loft drier for subsequent use.
Take calcining material 80g, use ball mill dry ball milling 1 minute, obtained powder is crossed 120 mesh sieves, and gained powder particle size is about 100 μm.
Mixture at high temperature sinters:
The powder prepared is put into crucible and compacting, then crucible is put into electric furnace and sinter.Temperature rise rate is: room temperature to 200 DEG C is 2 DEG C/m, and 200 DEG C ~ 970 DEG C is 4 DEG C/m, and heat preservation sintering 2 hours, makes it fully sinter porcelain into.After naturally cooling, obtained aperture is about the Bone Defect Repari stephanoporate calcium polyphosphate biomaterial of 50 ~ 300 μm.
After monocalcium phosphate preroasting, crystal water in it runs off, and its reaction reaches certain equilibrium state, and abrasive dust sinters again, monocalcium phosphate is forming stephanoporate calcium polyphosphate under polycondensation, and the powder particle size that its aperture can be screened by the abrasive dust stage controls.
Embodiment 4
Calcining monocalcium phosphate:
Weigh in the balance and get Powdered monocalcium phosphate 200g, put into quartz crucible, after adding a cover protection, put into electric furnace, be warming up to 650 DEG C with the speed of 4 DEG C/m, be incubated naturally cooling after 1 hour, thus obtain block calcining material.After the preliminary fragmentation of this calcining material, put into loft drier for subsequent use.
Monocalcium phosphate after calcining is not calcined monocalcium phosphate mix with appropriate:
Take calcining material 50g, Powdered monocalcium phosphate 25g respectively, after mixing, use ball mill dry grinding 2 minutes, obtained powder is crossed 60 mesh sieves, and the powder particle size obtained is less than 250 μm.
Mixture at high temperature sinters:
The powder prepared is put into crucible and compacting, then crucible is put into electric furnace and sinter.Temperature rise rate is: room temperature to 200 DEG C is 2 DEG C/m, and 200 DEG C ~ 960 DEG C is 4 DEG C/m, and heat preservation sintering 2 hours, makes it fully sinter porcelain into.After naturally cooling, obtained aperture is about the Bone Defect Repari stephanoporate calcium polyphosphate biomaterial of 100 ~ 400 μm.
Embodiment 5
Calcining monocalcium phosphate:
Weigh in the balance and get Powdered monocalcium phosphate 200g, put into quartz crucible, after adding a cover protection, put into electric furnace, be warming up to 750 DEG C with the speed of 4 DEG C/m, be incubated naturally cooling after 1 hour, thus obtain block calcining material.After the preliminary fragmentation of this calcining material, put into loft drier for subsequent use.
Monocalcium phosphate after calcining is not calcined monocalcium phosphate mix with appropriate:
Take calcining material 50g, Powdered monocalcium phosphate 200g respectively, after mixing, use ball mill dry grinding 1 minute, obtained powder is crossed 40 mesh sieves, and the powder particle size obtained is less than 400 μm.
Mixture at high temperature sinters:
The powder prepared is put into crucible and compacting, then crucible is put into electric furnace and sinter.Temperature rise rate is: room temperature to 200 DEG C is 2 DEG C/m, and 200 DEG C ~ 960 DEG C is 4 DEG C/m, and heat preservation sintering 2 hours, makes it fully sinter porcelain into.After naturally cooling, obtained aperture is about the Bone Defect Repari stephanoporate calcium polyphosphate biomaterial of 100 ~ 500 μm.
The stephanoporate calcium polyphosphate biomaterial obtained by embodiment 1 ~ 5, pore diameter range is 50 ~ 500 μm, utilize the characteristic of monocalcium phosphate high-temperature polycondensation, himself polycondensation pore-forming is made to define Bone Defect Repari stephanoporate calcium polyphosphate biomaterial, avoid the introducing of other impurity, the pure of material can be ensured to greatest extent.
Claims (1)
1. a stephanoporate calcium polyphosphate biomaterial preparation method, is characterized in that comprising the steps:
(1) calcine monocalcium phosphate, calcining temperature is 650 ~ 750 DEG C, and soaking time is 1 ~ 2 hour;
(2) by the monocalcium phosphate after calcining with in right amount do not calcine monocalcium phosphate and mix, the monocalcium phosphate after calcining and not calcine monocalcium phosphate mass ratio be 1:(0.5 ~ 4);
(3) ground by the mixture that step 2 obtains, the powder after grinding sieves, and gets the powder that particle diameter is 100 ~ 500 μm, puts into crucible compacting, is incubated 1 ~ 2 hour, makes it fully sinter porcelain under being then heated to 950 ~ 970 DEG C of conditions.
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| CN108607119B (en) * | 2018-03-20 | 2020-06-23 | 山东大学 | Calcium polyphosphate surface polydopamine modified composite biological ceramic and preparation method thereof |
| CN116283017B (en) * | 2023-03-16 | 2024-10-18 | 广西产研院新型功能材料研究所有限公司 | Modified calcium tripolyphosphate, preparation method and application thereof in producing corrosion-resistant ceramic-based-semi-metal friction linings |
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| CN102276291A (en) * | 2011-06-09 | 2011-12-14 | 重庆大学 | Method for preparing porous calcium phosphate biological ceramic material |
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| CN101352583B (en) * | 2007-07-29 | 2012-03-14 | 山东硅苑新材料科技股份有限公司 | Stephanoporate calcium polyphosphate biological ceramic and preparation method thereof |
| CN101407414A (en) * | 2008-11-06 | 2009-04-15 | 上海交通大学 | Method for preparing calcium polyphosphate / tricalcium phosphate two-phase biological ceramic |
| AU2010327923B2 (en) * | 2009-12-11 | 2015-05-07 | Latitude 18, Inc. | Inorganic phosphate compositions and methods |
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