CN108046227A - A kind of method of the needle-shaped hydroxy calcium apatite of low temperature preparation micron order - Google Patents
A kind of method of the needle-shaped hydroxy calcium apatite of low temperature preparation micron order Download PDFInfo
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- CN108046227A CN108046227A CN201711389780.3A CN201711389780A CN108046227A CN 108046227 A CN108046227 A CN 108046227A CN 201711389780 A CN201711389780 A CN 201711389780A CN 108046227 A CN108046227 A CN 108046227A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/325—Preparation by double decomposition
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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Abstract
The invention discloses a kind of methods of the needle-shaped hydroxy calcium apatite of low temperature preparation micron order, include the following steps:(1) calcium salt is dissolved in the solution of polyhydroxy chain-like macromolecule compound, is configured to the solution that calcium ion concentration is 0.4~0.9mol/L, added the alkaline solution that hydroxide ion concentration is 0.5~1.5mol/L, obtain solution A;(2) phosphate is dissolved in the water, is configured to the solution B that phosphorus acid ion concentration is 2~4mol/L;It for 1.0: 1~2.0: 1 measurement solution A and solution B and is uniformly mixed by calcium-phosphorus ratio, obtains mixed solution C;(3) by the mixed solution C of step (2) be placed in 60~90 DEG C of water-baths reaction 48~72 it is small when;(4) by obtained product after centrifuging, wash, dry, the needle-shaped hydroxy calcium apatite of micron order is obtained.The present invention is with preparation process is simple, at low cost, preparation condition is easily controllable;Product major diameter processed is bigger, is applicable to the fields such as medical material, carrier material and adsorption and separation material, more can reach or meet clinical requirement.
Description
Technical field
The invention belongs to technical field of inorganic nano-material preparation, and in particular to a kind of needle-shaped hydroxyl of low temperature preparation micron order
The method of apatite calcium.
Background technology
Hydroxy calcium apatite (Hydroxyapatite, hereinafter referred to as CaHA) has excellent bioactivity and bio-compatible
Property, good ion exchange, absorption property and environmental-friendly characteristic, and have been to be concerned by more and more people and become research
Hot spot.
Native hydroxyl apatite calcium is in nature and is not present.At present, preparing the method for CaHA mainly has hydro-thermal method, molten
Sol-gel, molten-salt growth method, homogeneous precipitation method etc..Hydro-thermal method be prepare at present hydroxy calcium apatite whisker it is most common and most into
A kind of ripe method, Zhang Jizhong (publication number CN101297978A) have invented a kind of preparation method of hydroxyapatite nano pole,
The method is carried out under oleic acid-alcohol-water phase transfer system, the hydroxy apatite powder size uniform prepared, morphology controllable,
But required drug variety is various, and the optimal of the compactedness of reaction kettle and reaction system pressure during hydro-thermal reaction is not described in text
Parameter.Sun Kangning et al. (publication number CN102431986A) has invented a kind of preparation method of hydroxyapatite nanofiber, should
Method is to prepare hydroxyapatite fiber using homogeneous precipitation method, and diameter is about 20~30nm, length is about 200~
900nm, draw ratio is substantially controllable, and without other impurities phase, but product crystallinity and topography uniformity be not high, repeatability compared with
Difference, and major diameter is smaller.
The content of the invention
It is contemplated that above-mentioned technical problem is solved to a certain extent.
In order to solve the problems in the existing technology, the present invention provides a kind of needle-shaped hydroxyl calcium phosphorus of low temperature preparation micron order
The method of lime stone, this method preparation condition is simple, easily implements, and the preparation gained needle-shaped hydroxy calcium apatite draw ratio of micron order is big,
Yield is high.
To achieve these goals, in a first aspect, the present invention uses polyhydroxy chain-like macromolecule compound as template,
Because there is great amount of hydroxy group on its surface, Ca2+ is attached to its surface, and OH- and PO43-, which is further added dropwise, increases ion concentration, when reaching hydroxyl
Precipitation is initially formed during the solubility product of base apatite calcium, and hydroxy calcium apatite is nucleated, grown on the template until reaching molten
Solution and sedimentation equilibrium, in addition, the adhesive force between product and template can be effectively improved by reacting liquid pH value regulation and control.
To achieve these goals, in second aspect, the present invention introduces expanding gas in preparation process, make reactant it
Between contact surface increase, reaction it is more abundant.In addition, there are gradient, further induction productions for pH value when expanding gas are near liquid level
Object settles.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of method of the needle-shaped hydroxy calcium apatite of low temperature preparation micron order, comprises the following steps:
(1) calcium salt is dissolved in the solution of polyhydroxy chain-like macromolecule compound, be configured to calcium ion concentration for 0.4~
The solution of 0.9mol/L adds the alkaline solution that hydroxide ion concentration is 0.5~1.5mol/L, obtains mixed solution A;(2)
Phosphate is dissolved in the water, is configured to the solution B that phosphorus acid ion concentration is 2~4mol/L;Molar ratio by calcium and phosphorus is
1.0~2.0: 1, it measures solution A and solution B is mixed, obtain solution C;
(3) by the solution C of step (2) be placed in 60~90 DEG C of water-baths reaction 48~72 it is small when, obtain product;
(4) product for obtaining step (3) obtains the needle-shaped hydroxy calcium apatite of micron order after centrifuging, wash, dry.
Further, the calcium salt described in step (1) is calcium carbonate, calcium nitrate, calcium chloride, calcium oxide, calcium bicarbonate, phosphorus
One kind in sour hydrogen calcium.
Further, polyhydroxy chain-like macromolecule compound described in step (1) is using polyvinyl alcohol (PVA), poly- second two
One kind in alcohol (PEG), sodium carboxymethylcellulose (CMC), chitosan, hyaluronic acid.
Further, the alkaline solution described in step (1) is potassium hydroxide, sodium hydroxide, magnesium hydroxide, hydroxide
One kind in barium, ammonia spirit.
Further, the phosphate described in step (2) be monoammonium phosphate, ammonium dihydrogen phosphate, disodium-hydrogen, phosphoric acid
One kind in sodium dihydrogen, potassium dihydrogen phosphate.
Further, the solution C described in step (2) is milky suspension.
Further, centrifuge, wash described in step (4) and be:With water, absolute ethyl alcohol centrifuge washing.
Further, centrifuge, wash described in step (4) and be:Water centrifuge washing is used successively 2 times, absolute ethyl alcohol centrifugation is washed
It washs 3 times.
Further, drying is described in step (4):In 50~80 DEG C of thermostatic drying chamber, when drying 24~48 is small.
Further, the length of the needle-shaped hydroxy calcium apatite of micron order described in step (4) is more than 150 microns, and diameter exists
Between 0.5~3 micron.
Compared with prior art, beneficial effects of the present invention are as follows:Preparation process is simple, at low cost, preparation condition is easy to
Control, environmentally protective, yield is high;The needle-shaped hydroxy calcium apatite length of micron order of preparation is more than 150 microns, and diameter is 0.5~3
Micron between, major diameter is bigger, is applicable to the fields such as medical material, carrier material and adsorption and separation material, can more reach or
Meet clinical requirement.
Description of the drawings
Fig. 1 is the SEM figures of the needle-shaped hydroxy calcium apatite of micron order prepared by the embodiment of the present invention 1;
Fig. 2 is the XRD spectrum of the needle-shaped hydroxy calcium apatite of micron order prepared by the embodiment of the present invention 1;
Fig. 3 is the FT-IR figures of the needle-shaped hydroxy calcium apatite of micron order prepared by the embodiment of the present invention 1.
Specific embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is further explained, below by ginseng
The embodiment for examining attached drawing description is exemplary, it is intended to for explaining the present invention, and is not considered as limiting the invention.
Embodiment 1:
A kind of method of the needle-shaped hydroxy calcium apatite of low temperature preparation micron order, comprises the following steps:
(1) by dissolution of calcium carbonate in polyethylene glycol (PEG) solution, it is the molten of 0.4mol/L to be configured to calcium ion concentration
Liquid adds the sodium hydroxide solution that hydroxide ion concentration is 0.5mol/L, obtains solution A;
(2) ammonium dihydrogen phosphate is dissolved in the water, is configured to the solution B that phosphorus acid ion concentration is 2mol/L;By calcium phosphorus
Than measuring solution As and solution B for 2: 1 and being uniformly mixed, mixed solution C is obtained;
(3) by the mixed solution C of step (2) be placed in 60 DEG C of water-baths reaction 72 it is small when;
(4) obtained product is used to water centrifuge washing successively 2 times, absolute ethyl alcohol washs 3 times, is subsequently placed in 50 DEG C of constant temperature and does
When drying 48 is small in dry case, the needle-shaped hydroxy calcium apatite of micron order is obtained.
Attached drawing 1 is the scanning electron microscopic picture according to the product prepared by above-mentioned rate of charge, it can be seen from the figure that product is in
Needle-shaped pattern, length are more than 200um, and diameter is between 0.5~2um.
The XRD spectrum for the product that attached drawing 2 is prepared for embodiment 1, in Fig. 2 each diffraction maximum with JCPDS standard cards (09-
0432) match, show product as hydroxy calcium apatite, while there is no other diffraction miscellaneous peaks in XRD spectrum, illustrate that the present invention carries
The method gone out can prepare the hydroxy calcium apatite of single object phase.
Attached drawing 3 is the FT-IR figures of the product prepared.There are apparent OH- (3399cm-1,2941cm-1,1650cm- in figure
1) and the characteristic peak of P043- (1038cm-1,603cm-1,567cm-1), further proof products therefrom are hydroxyapatite.
Embodiment 2:
(1) calcium chloride is dissolved in sodium carboxymethylcellulose (CMC) solution, is configured to calcium ion concentration as 0.6mol/L
Solution, add hydroxide ion concentration be 1.0mol/L barium hydroxide solution, obtain solution A;
(2) monoammonium phosphate is dissolved in the water, is configured to the solution B that phosphorus acid ion concentration is 2mol/L;By calcium phosphorus
Than measuring solution As and solution B for 1.67: 1 and being uniformly mixed, mixed solution C is obtained;
(3) by the mixed solution C of step (2) be placed in 70 DEG C of water-baths reaction 64 it is small when;
(4) obtained product is used to water centrifuge washing successively 1 time, absolute ethyl alcohol washs 3 times, is subsequently placed in 80 DEG C of constant temperature and does
When drying 24 is small in dry case, the needle-shaped hydroxy calcium apatite of micron order is obtained.
Embodiment 3:
(1) calcium nitrate is dissolved in poly-vinyl alcohol solution, is configured to the solution that calcium ion concentration is 0.5mol/L, then adds
Enter the potassium hydroxide solution that hydroxide ion concentration is 0.8mol/L, obtain solution A;
(2) monoammonium phosphate is dissolved in the water, is configured to the solution B that phosphorus acid ion concentration is 2mol/L;By calcium phosphorus
Than measuring solution As and solution B for 1.5: 1 and being uniformly mixed, mixed solution C is obtained;
(3) by the mixed solution C of step (2) be placed in 60 DEG C of water-baths reaction 72 it is small when;
(4) obtained product is used to water centrifuge washing successively 2 times, absolute ethyl alcohol washs 3 times, is subsequently placed in 60 DEG C of constant temperature and does
When drying 40 is small in dry case, the needle-shaped hydroxy calcium apatite of micron order, draw ratio 70 are obtained.
Embodiment 4:
(1) by Calcium oxide dissolution in polyglycol solution, the solution that calcium ion concentration is 0.6mol/L is configured to, then is added
Enter the barium hydroxide solution that hydroxide ion concentration is 1.0mol/L, obtain solution A;
(2) ammonium dihydrogen phosphate is dissolved in the water, is configured to the solution B that phosphorus acid ion concentration is 2.5mol/L;By calcium
Phosphorus ratio is 1.8: 1 measurement solution As and solution B and is uniformly mixed, and obtains mixed solution C;
(3) by the mixed solution C of step (2) be placed in 90 DEG C of water-baths reaction 42 it is small when;
(4) obtained product is used to water centrifuge washing successively 2 times, absolute ethyl alcohol washs 3 times, is subsequently placed in 80 DEG C of constant temperature and does
When drying 24 is small in dry case, the needle-shaped hydroxy calcium apatite of micron order, draw ratio 150 are obtained.
Embodiment 5:
(1) calcium bicarbonate is dissolved in carboxymethylcellulose sodium solution, it is 0.7mol/L's to be configured to calcium ion concentration
Solution adds the magnesium hydroxide solution that hydroxide ion concentration is 1.2mol/L, obtains solution A;
(2) disodium-hydrogen is dissolved in the water, is configured to the solution B that phosphorus acid ion concentration is 3mol/L;By calcium phosphorus
Than measuring solution As and solution B for 1.7: 1 and being uniformly mixed, mixed solution C is obtained;
(3) by the mixed solution C of step (2) be placed in 70 DEG C of water-baths reaction 48 it is small when;
(4) obtained product is used to water centrifuge washing successively 1 time, absolute ethyl alcohol washs 3 times, is subsequently placed in 70 DEG C of constant temperature and does
When drying 36 is small in dry case, the needle-shaped hydroxy calcium apatite of micron order, draw ratio 270 are obtained.
Embodiment 6:
(1) calcium monohydrogen phosphate is dissolved in chitosan solution, it is the molten of 0.8mol/L to be configured to calcium ion concentration
Liquid adds the sodium hydroxide solution that hydroxide ion concentration is 1.4mol/L, obtains solution A;
(2) sodium dihydrogen phosphate is dissolved in the water, is configured to the solution B that phosphorus acid ion concentration is 3.5mol/L;By calcium
Phosphorus ratio is 1.4: 1 measurement solution As and solution B and is uniformly mixed, and obtains mixed solution C;
(3) by the mixed solution C of step (2) be placed in 65 DEG C of water-baths reaction 68 it is small when;
(4) obtained product is used to water centrifuge washing successively 1 time, absolute ethyl alcohol washs 3 times, is subsequently placed in 65 DEG C of constant temperature and does
When drying 45 is small in dry case, the needle-shaped hydroxy calcium apatite of micron order, draw ratio 200 are obtained.
Embodiment 7:
(1) calcium chloride is dissolved in hyaluronic acid solution, is configured to the solution that calcium ion concentration is 0.9mol/L, then adds
Enter the ammonia spirit that hydroxide ion concentration is 1.5mol/L, obtain solution A;
(2) potassium dihydrogen phosphate is dissolved in the water, is configured to the solution B that phosphorus acid ion concentration is 4mol/L;By calcium phosphorus
Than measuring solution As and solution B for 1.7: 1 and being uniformly mixed, mixed solution C is obtained;
(3) by the mixed solution C of step (2) be placed in 60 DEG C of water-baths reaction 72 it is small when;
(4) obtained product is used to water centrifuge washing successively 1 time, absolute ethyl alcohol washs 3 times, is subsequently placed in 75 DEG C of constant temperature and does
When drying 30 is small in dry case, the needle-shaped hydroxy calcium apatite of micron order, draw ratio 100 are obtained.
Embodiment 3-7 rate of charges see the table below shown in 1.
Material ratio used in 1 each embodiment of table
Although the embodiment of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, those of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification.
Claims (10)
- A kind of 1. method of the needle-shaped hydroxy calcium apatite of low temperature preparation micron order, which is characterized in that it is prepared by homogeneous precipitation method, Comprise the following steps:(1) calcium salt is dissolved in the solution of polyhydroxy chain-like macromolecule compound, be configured to calcium ion concentration for 0.4~ The solution of 0.9mol/L adds the alkaline solution that hydroxide ion concentration is 0.5~1.5mol/L, obtains solution A;(2) phosphate is dissolved in the water, is configured to the solution B that phosphorus acid ion concentration is 2~4mol/L;By rubbing for calcium and phosphorus You measure solution A and solution B are mixed, obtain solution C than being 1.0: 1~2.0: 1;(3) by the solution C of step (2) be placed in 60~90 DEG C of water-baths reaction 48~72 it is small when, obtain product;(4) product for obtaining step (3) obtains the needle-shaped hydroxy calcium apatite of micron order after centrifuging, wash, dry.
- 2. a kind of method of needle-shaped hydroxy calcium apatite of low temperature preparation micron order according to claim 1, which is characterized in that Calcium salt described in step (1) is using calcium carbonate, calcium nitrate, calcium chloride, calcium oxide, calcium bicarbonate, calcium monohydrogen phosphate, calcirm-fluoride, three One kind in fluorine methanesulfonic acid calcium.
- 3. a kind of method of needle-shaped hydroxy calcium apatite of low temperature preparation micron order according to claim 1, which is characterized in that Polyhydroxy chain-like macromolecule compound described in step (1) is polyvinyl alcohol, polyethylene glycol, sodium carboxymethylcellulose, deacetylated One kind in chitin, hyaluronic acid.
- 4. a kind of method of needle-shaped hydroxy calcium apatite of low temperature preparation micron order according to claim 1, which is characterized in that Alkaline solution described in step (1) is potassium hydroxide, one kind in sodium hydroxide, magnesium hydroxide, barium hydroxide, ammonia spirit.
- 5. a kind of method of needle-shaped hydroxy calcium apatite of low temperature preparation micron order according to claim 1, which is characterized in that Phosphate described in step (2) is using monoammonium phosphate, ammonium dihydrogen phosphate, disodium-hydrogen, sodium dihydrogen phosphate, potassium dihydrogen phosphate In one kind.
- 6. a kind of method of needle-shaped hydroxy calcium apatite of low temperature preparation micron order according to claim 1, which is characterized in that Mixed solution C described in step (2) is milky suspension.
- 7. a kind of method of needle-shaped hydroxy calcium apatite of low temperature preparation micron order according to claim 1, which is characterized in that It centrifuges, wash described in step (4) and be:With water, absolute ethyl alcohol centrifuge washing.
- 8. a kind of method of needle-shaped hydroxy calcium apatite of low temperature preparation micron order according to claim 7, it is characterised in that: It centrifuges, wash described in step (4) and be:Water centrifuge washing is used successively 2 times, absolute ethyl alcohol centrifuge washing 3 times.
- 9. a kind of method of needle-shaped hydroxy calcium apatite of low temperature preparation micron order according to claim 1, which is characterized in that Drying described in step (4) is:In 50~80 DEG C of thermostatic drying chamber, when drying 24~48 is small.
- 10. a kind of method of needle-shaped hydroxy calcium apatite of low temperature preparation micron order according to claim 1, feature exist In the length of the needle-shaped hydroxy calcium apatite of micron order described in step (4) is more than 150 microns, and diameter is between 0.5~3 micron.
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Cited By (1)
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CN110885071A (en) * | 2019-12-17 | 2020-03-17 | 衢州学院 | Micron-sized ultra-long calcium-based wormlike micelle template and hydroxy calcium apatite whisker |
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CN110885071B (en) * | 2019-12-17 | 2021-07-09 | 衢州学院 | Micron-sized ultra-long calcium-based wormlike micelle template and hydroxy calcium apatite whisker |
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Application publication date: 20180518 |