CN106946486B - The synthetic method of calcium containing compound additive for calcium phosphate bone cement - Google Patents
The synthetic method of calcium containing compound additive for calcium phosphate bone cement Download PDFInfo
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- CN106946486B CN106946486B CN201710256324.5A CN201710256324A CN106946486B CN 106946486 B CN106946486 B CN 106946486B CN 201710256324 A CN201710256324 A CN 201710256324A CN 106946486 B CN106946486 B CN 106946486B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0042—Powdery mixtures
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/12—Phosphorus-containing materials, e.g. apatite
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Abstract
The invention discloses a kind of synthetic methods of calcium containing compound additive for calcium phosphate bone cement, comprising the following steps: (1) adds in calcium hydroxide suspension phosphoric acid solution, to be aged after reaction, obtain ageing liquid；(2) sodium carbonate liquor is added dropwise into the resulting ageing liquid of step (1), after reaction, adds dispersing agent, be centrifuged after mixing, then washing precipitate is dried；(3) powder after above-mentioned drying is placed in hot conditions and keeps the temperature a period of time, cooled down later to get the calcium containing compound additive.Compared with the existing technology, the synthetic method of inorganic-bone cement additive proposed by the present invention, products therefrom good crystallinity, particle size is sub-micrometer scale, the uniform mixing for realizing submicron order hydroxyapatite and calcium salt, the problems such as avoiding the uneven mixing being easy to produce during direct mechanical mixture, particle agglomeration.
Description
Technical field
The present invention relates to a kind of synthetic methods of calcium containing compound additive for calcium phosphate bone cement, belong to biological doctor
Use Material Field.
Background technique
Calcium phosphate bone cement is because having good biocompatibility and degradable in vivo to receive more and more attention.When
When total calcium, phosphorus substance amount ratio are lower than 1.67 in calcium phosphate bone cement, calcium-deficient apatite is formed after bone cement solidification.In bone
In the ingredient of cement, addition Nano-hydroxyapatite can be used as the nucleus that the stylish apatite of hydration and sclerosis is precipitated, be added calcium carbonate and
The calcium containing compounds such as calcium oxide can improve calcium amount total in cement, reduce the content of calcium deficiency apatite after solidifying.In addition, a large amount of
Studies have shown that or mixtures thereof calcium containing compounds such as hydroxyapatite, calcium carbonate and calcium oxide are added in the powder of bone cement,
There is positive effect to intensity, adjusting degradation rate, the adjusting curing time etc. of improving bone cement.Khairoun etc.
(Khairoun I,Boltong M G,Driessens F C,et al.Effect of calcium carbonate on
the compliance of an apatitic calcium phosphate bone cement.[J].Biomaterials,
1997,18 (18): 1535-1539.) hydroxyapatite and calcium carbonate are added into calcium phosphate bone cement, it is more high-strength obtaining
While spending, it is ensured that bone cement has curing time suitable for clinical application.
Under normal conditions, the calcium containing compounds mixture such as hydroxyapatite, calcium carbonate, calcium oxide be Jiang Gexiang proportionally
After weighing respectively, mechanical mixture is carried out using modes such as ball milling, grindings.Mechanical means be difficult to realize these compounds in micron or
The uniform mixing of nano-scale, and mixed process also easily leads to particle agglomeration, influences final using effect.It is therefore desirable for finding
A kind of method can disposably synthesize the hydroxyapatite of micron or nano-scale and the mixture of calcium oxide or calcium carbonate, and
And it can be realized regulation to each object phase relative amount.
Summary of the invention
Goal of the invention: in view of the above technical problems, it is an object of the present invention to provide a kind of calcics for calcium phosphate bone cement
The synthetic method of compound additive.
Technical solution: the invention discloses a kind of synthesis sides of calcium containing compound additive for calcium phosphate bone cement
Method, comprising the following steps:
(1) phosphoric acid solution is added in calcium hydroxide suspension, to be aged after reaction, obtains ageing liquid；
(2) sodium carbonate liquor is added dropwise into the resulting ageing liquid of step (1), after reaction, adds dispersing agent, mix
After uniformly then centrifugation, washing precipitate are dried；
(3) powder after above-mentioned drying is placed in hot conditions and keeps the temperature a period of time, cooled down later to get the calcic
Compound additive.
It it is preferred that the calcium containing compound additive is the mixture of hydroxyapatite and calcium oxide, or is hydroxy-apatite
The mixture of stone and calcium oxide, calcium carbonate.
It is preferred that dispersing agent described in step (2) is one of PEG-20000, PVP or starch.
It is preferred that the synthetic method of the calcium containing compound additive for calcium phosphate bone cement, includes the following steps:
(1) under the conditions of strong stirring, phosphoric acid solution is added in calcium hydroxide suspension, it is small to be aged 12 after reaction
When；
(2) it is added dropwise sodium carbonate liquor into (1) resulting ageing liquid, the reaction was continued 1 hour under the conditions of strong stirring, by closing
Dispersing agent is added at the amount that 2g is added in the every 1000ml of overall solution volume, liquid centrifugation will be aged after mixing to dispersing agent dissolution,
And washed with dehydrated alcohol, gained sediment is dried at 80 DEG C；
(3) powder after drying is placed in 750 DEG C of high-temperature calcination stoves and keeps the temperature 1~4 hour, furnace cooling later obtains hydroxyl
The mixture of base apatite, calcium oxide and calcium carbonate.
It is preferred that the molar ratio of calcium hydroxide described in step (1) and phosphoric acid is 2.0-5.0, reaction medium is deionized water.
It is preferred that the amount of the sodium carbonate of addition described in step (2) and the molar ratio of calcium hydroxide are 0.167-0.667.
It is preferred that strong stirring condition in the step (1) and (2) are as follows: mechanical stirring, speed 600r/min.
Technical effect: compared with the existing technology, the synthetic method of inorganic-bone cement additive proposed by the present invention, using acid
Property raw material and basic materials directly react, do not needed in reaction process addition template, do not need adjust solution ph, technique repeat
Property is good, passes through the relative amount of each object phase in the calcium phosphorus ration in feed change, that is, controllable product.Reaction system calcium hydroxide
It is excessive, it is easier to obtain hydroxyapatite in the alkaline environment that calcium hydroxide slightly soluble is formed, and the later period is molten by the way that sodium carbonate is added dropwise
Liquid directly converts calcium carbonate for the calcium hydroxide not reacted completely, completely or partially decomposes and generates during subsequent calcination
Calcium oxide, products therefrom are the mixture of hydroxyapatite and calcium oxide or hydroxyapatite and calcium oxide, calcium carbonate.Synthesis
Product good crystallinity, product are sub-micrometer scale, realize hydroxyapatite and calcium containing compound in the uniform of nanometer sub-micron
Mixing and association growth, are more advantageous to the formation containing Carbonated hydroxyapatite during hydration and sclerosis.
Detailed description of the invention:
Fig. 1 is the XRD spectrum of 1 products therefrom of the embodiment of the present invention；
Fig. 2 is the XRD spectrum of 3 products therefrom of the embodiment of the present invention；
Fig. 3 is the XRD spectrum of 5 products therefrom of the embodiment of the present invention；
Fig. 4 is the TEM map of 5 products therefrom of the embodiment of the present invention.
Specific embodiment
According to following embodiments, the present invention may be better understood.And as it will be easily appreciated by one skilled in the art that embodiment
Described specific test result is merely to illustrate the present invention, without that should will not limit sheet described in claims
Invention.
Embodiment 1
(1) phosphoric acid solution of 0.15mol/L and the calcium hydroxide suspension of 0.3mol/L are prepared, control calcium-phosphorus ratio is 2.0,
A certain amount of phosphoric acid solution is added in calcium hydroxide suspension under the conditions of strong stirring, it is small to be aged 12 after reaction
When.
(2) molar ratio for controlling sodium carbonate and calcium hydroxide is to be added dropwise 50ml 0.5mol/L's in 0.167, Xiang Chenhua liquid
Sodium carbonate liquor, the reaction was continued under stirring 1 hour, is added later by the amount that 2g is added in the every 1000ml of synthetic solvent total volume
Ageing liquid is centrifuged, gained sediment is washed with dehydrated alcohol, dried at 80 DEG C by PVP as dispersing agent after dispersing agent dissolution
It is dry.
(3) powder after drying is placed in 750 DEG C of high-temperature calcination stoves and keeps the temperature 1 hour, furnace cooling later obtains hydroxyl phosphorus
The mixture of lime stone, calcium oxide and calcium carbonate.
Embodiment 2
(1) phosphoric acid solution of 0.12mol/L and the calcium hydroxide suspension of 0.3mol/L are prepared, control calcium-phosphorus ratio is 2.5,
A certain amount of phosphoric acid solution is added in calcium hydroxide suspension under the conditions of strong stirring, it is small to be aged 12 after reaction
When.
(2) molar ratio for controlling sodium carbonate and calcium hydroxide is to be added dropwise 100ml 0.5mol/L's in 0.333, Xiang Chenhua liquid
Sodium carbonate liquor, the reaction was continued under stirring 1 hour, is added later by the amount that 2g is added in the every 1000ml of synthetic solvent total volume
Ageing liquid is centrifuged, gained sediment is washed with dehydrated alcohol, 80 by PEG-20000 as dispersing agent after dispersing agent dissolution
It is dried at DEG C.
(3) powder after drying is placed in 750 DEG C of high-temperature calcination stoves and keeps the temperature 2 hours, furnace cooling later obtains hydroxyl phosphorus
The mixture of lime stone, calcium oxide and calcium carbonate.
Embodiment 3
(1) phosphoric acid solution of 0.1mol/L and the calcium hydroxide suspension of 0.3mol/L are prepared, control calcium-phosphorus ratio is 3.5,
A certain amount of phosphoric acid solution is added in calcium hydroxide suspension under the conditions of strong stirring, it is small to be aged 12 after reaction
When.
(2) molar ratio for controlling sodium carbonate and calcium hydroxide is that 1157ml 0.5mol/L is added dropwise in 0.524, Xiang Chenhua liquid
Sodium carbonate liquor, the reaction was continued under stirring 1 hour, and 2g starch is added by the every 1000ml of synthetic solvent total volume later and makees
For dispersing agent, ageing liquid is centrifuged after dispersing agent dissolution, gained sediment is washed with dehydrated alcohol, dried at 80 DEG C.
(3) powder after drying is placed in 750 DEG C of high-temperature calcination stoves and keeps the temperature 3 hours, furnace cooling later obtains hydroxyl phosphorus
The mixture of lime stone, calcium oxide and calcium carbonate.
Embodiment 4
(1) phosphoric acid solution of 0.075mol/L and the calcium hydroxide suspension of 0.3mol/L are prepared, control calcium-phosphorus ratio is
4.5, a certain amount of phosphoric acid solution is added in calcium hydroxide suspension under the conditions of strong stirring, to be aged 12 after reaction
Hour.
(2) molar ratio for controlling sodium carbonate and calcium hydroxide is to be added dropwise 189ml 0.5mol/L's in 0.630, Xiang Chenhua liquid
Sodium carbonate liquor, the reaction was continued under stirring 1 hour, and the conduct of 2g starch is added by the every 1000ml of synthetic solvent total volume later
Ageing liquid is centrifuged by dispersing agent after dispersing agent dissolution, and gained sediment is washed with dehydrated alcohol, dried at 80 DEG C.
(3) powder after drying is placed in 750 DEG C of high-temperature calcination stoves and keeps the temperature 4 hours, furnace cooling later obtains hydroxyl phosphorus
The mixture of lime stone, calcium oxide and calcium carbonate.
Embodiment 5
(1) phosphoric acid solution of 0.06mol/L and the calcium hydroxide suspension of 0.3mol/L are prepared, control calcium-phosphorus ratio is 5.0,
A certain amount of phosphoric acid solution is added in calcium hydroxide suspension under the conditions of strong stirring, it is small to be aged 12 after reaction
When.
(2) molar ratio for controlling sodium carbonate and calcium hydroxide is to be added dropwise 200ml 0.5mol/L's in 0.667, Xiang Chenhua liquid
Sodium carbonate liquor, the reaction was continued under stirring 1 hour, and 2gPEG- is added by the every 1000ml of synthetic solvent total volume later
20000 are used as dispersing agent, are centrifuged ageing liquid after dispersing agent dissolution, gained sediment is washed with dehydrated alcohol, at 80 DEG C
Drying.
(3) powder after drying is placed in 750 DEG C of high-temperature calcination stoves and keeps the temperature 2 hours, furnace cooling later obtains hydroxyl phosphorus
The mixture of lime stone, calcium oxide and calcium carbonate.
It can be obtained by Fig. 1 result, the diffraction maximum of hydroxyapatite and calcium oxide is kissed with standard diagram completely in XRD spectrum
Close, diffraction maximum 2 θ=37.43 °, 32.21 °, 53.93 ° at for calcium oxide three strongest peak, 2 θ=31.89 °, 32.99 °,
Diffraction maximum at 25.84 ° is the three strongest peak of hydroxyapatite, and product is the mixture of hydroxyapatite and calcium oxide.In raw material
Calcium hydroxide part and phosphatase reaction generate hydroxyapatite, remaining part then with the later period be added sodium carbonate react generation carbon
Sour calcium all decomposes in calcination process since calcium carbonate content is less, generates calcium oxide, so final product is hydroxyl phosphorus
The mixture of lime stone and calcium oxide.
Can be obtained by Fig. 2 result, hydroxyapatite and calcium oxide in XRD spectrum, calcium carbonate diffraction maximum and standard diagram
Fit like a glove, the diffraction maximum at 2 θ=37.43 °, 32.21 °, 53.93 ° be calcium oxide three strongest peak, 2 θ=31.89 °,
Diffraction maximum at 32.99 °, 25.84 ° is the three strongest peak of hydroxyapatite, and the diffraction maximum at 2 θ=29.38 °, 2297 ° is carbon
The two powers peak of sour calcium.Product is the mixture of hydroxyapatite and calcium oxide, calcium carbonate.Calcium hydroxide part and phosphorus in raw material
Acid reaction generate hydroxyapatite, remaining part then with the later period be added sodium carbonate react generation calcium carbonate, calcium carbonate content compared with
Height, the decomposed in calcination process generate calcium oxide, so final product is hydroxyapatite and calcium oxide, calcium carbonate
Mixture.
Can be obtained by Fig. 3 result, hydroxyapatite and calcium oxide in XRD spectrum, calcium carbonate diffraction maximum and standard diagram
Fit like a glove, the diffraction maximum at 2 θ=37.43 °, 32.21 °, 53.93 ° be calcium oxide three strongest peak, 2 θ=31.89 °,
Diffraction maximum at 32.99 °, 25.84 ° is the three strongest peak of hydroxyapatite, and the diffraction maximum at 2 θ=29.38 °, 2297 ° is carbon
The two powers peak of sour calcium.Product is the mixture of hydroxyapatite and calcium oxide, calcium carbonate.Calcium hydroxide part and phosphorus in raw material
Acid reaction generate hydroxyapatite, remaining part then with the later period be added sodium carbonate react generation calcium carbonate, calcium carbonate content compared with
Height, the decomposed in calcination process generate calcium oxide, so final product is hydroxyapatite and calcium oxide, calcium carbonate
Mixture.It is high in intensity ratio Fig. 2 of calcium oxide in the diffraction maximum, show that calcium oxide content increases.
It can be obtained by Fig. 4 result, upper left square object is mutually hydroxyapatite, and bottom right square object is mutually the mixing of calcium carbonate and calcium oxide
Object, final product are hydroxyapatite and calcium carbonate, oxidation calcium compound, and particle size is sub-micrometer scale.
Claims (5)
1. the synthetic method of the calcium containing compound additive for calcium phosphate bone cement, which comprises the following steps:
(1) phosphoric acid solution is added in calcium hydroxide suspension, to be aged after reaction, obtains ageing liquid；The hydroxide
The molar ratio of calcium and phosphoric acid is 2.0-5.0, and reaction medium is deionized water；
(2) sodium carbonate liquor is added dropwise into the resulting ageing liquid of step (1), after reaction, adds dispersing agent, be uniformly mixed
After be centrifuged, then washing precipitate is dried；The amount of the sodium carbonate of the addition and the molar ratio of calcium hydroxide are 0.167-
0.667；
(3) powder after above-mentioned drying is placed in 750 DEG C of high-temperature calcination stoves and keeps the temperature 1~4 hour, cooled down later to get described
Calcium containing compound additive.
2. the synthetic method of the calcium containing compound additive according to claim 1 for calcium phosphate bone cement, feature
It is, the calcium containing compound additive is the mixture of hydroxyapatite and calcium oxide, or is hydroxyapatite and oxidation
The mixture of calcium, calcium carbonate.
3. the synthetic method of the calcium containing compound additive according to claim 1 for calcium phosphate bone cement, feature
It is, dispersing agent described in step (2) is one of PEG-20000, PVP or starch.
4. the synthetic method of the calcium containing compound additive according to claim 1 for calcium phosphate bone cement, feature
It is, includes the following steps:
(1) under the conditions of strong stirring, phosphoric acid solution is added in calcium hydroxide suspension, is aged 12 hours after reaction；
(2) it is added dropwise sodium carbonate liquor into (1) resulting ageing liquid, the reaction was continued 1 hour under the conditions of strong stirring, molten by synthesizing
Dispersing agent is added in the amount that 2g is added in the every 1000ml of liquid total volume, will be aged liquid centrifugation after mixing to dispersing agent dissolution, and be used in combination
Dehydrated alcohol washing, gained sediment are dried at 80 DEG C；
(3) powder after drying is placed in 750 DEG C of high-temperature calcination stoves and keeps the temperature 1~4 hour, furnace cooling later obtains hydroxyl phosphorus
The mixture of lime stone, calcium oxide and calcium carbonate.
5. the synthetic method of the calcium containing compound additive according to claim 1 for calcium phosphate bone cement, feature
It is, strong stirring condition in the step (1) and (2) are as follows: mechanical stirring, speed 600r/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1390607A (en) * | 2001-06-12 | 2003-01-15 | 中国人民解放军总医院 | Modified hydroxyphosphorite as substitute of bone and its preparing process and application |
| CN101254910A (en) * | 2008-04-14 | 2008-09-03 | 北京化工大学 | Method for preparing calcium phosphate composite powder |
| CN103961741A (en) * | 2014-05-14 | 2014-08-06 | 常州大学 | Calcium phosphate bone repair material and preparation method thereof |
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| US9078955B2 (en) * | 2010-10-26 | 2015-07-14 | Cap Biomaterials, Llc | Composites of hydroxyapatite and calcium carbonate and related methods of preparation and use |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1390607A (en) * | 2001-06-12 | 2003-01-15 | 中国人民解放军总医院 | Modified hydroxyphosphorite as substitute of bone and its preparing process and application |
| CN101254910A (en) * | 2008-04-14 | 2008-09-03 | 北京化工大学 | Method for preparing calcium phosphate composite powder |
| CN103961741A (en) * | 2014-05-14 | 2014-08-06 | 常州大学 | Calcium phosphate bone repair material and preparation method thereof |
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