CN103896233A - Method for synthesizing hydroxyapatite nano material - Google Patents
Method for synthesizing hydroxyapatite nano material Download PDFInfo
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- CN103896233A CN103896233A CN201410128802.0A CN201410128802A CN103896233A CN 103896233 A CN103896233 A CN 103896233A CN 201410128802 A CN201410128802 A CN 201410128802A CN 103896233 A CN103896233 A CN 103896233A
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Abstract
The invention relates to a method for preparing a hydroxyapatite nano material. The method comprises the following steps: 1) adding glutamic acid into an aqueous solution of calcium chloride to obtain a mixed solution, wherein the molar ratio of glutamic acid to calcium chloride is (0-4): 1, and the concentration of the calcium chloride solution is 0.25 mol/L; 2) adding urea into an aqueous solution of sodium tripolyphosphate to obtain a mixed solution, wherein the molar ratio of sodium tripolyphosphate to calcium chloride is (1-10): 5, the molar ratio of urea to calcium chloride is (0-5): 1, and the concentration of the aqueous solution of sodium tripolyphosphate is 0.05-0.5 mol/L; 3) slowly dripping the mixed solution obtained in step 1) into the mixed solution obtained in step 2), stirring, transferring to a reaction kettle, then putting the reaction kettle into an oven, reacting for 10 hours at 180 DEG C, and centrifuging, washing and drying the obtained product to obtain the hydroxyapatite nano material. The method has the characteristics of simplicity, low cost and low pollution.
Description
Technical field
The invention belongs to field of nanometer material technology, relate in particular to a kind of synthetic method of hydroxyapatite nanoparticle.
Background technology
Hydroxyapatite is the main component of the mankind and other vertebrates bone, has good biocompatibility and osteoconductive nature, can produce Chemical bond with people's bone, and in body fluid, degraded provides growth required calcium and phosphorus ions for people's bone.Nano hydroxyapatite material has higher specific surface area, and it is had a wide range of applications in various fields such as biomaterials.
Simply, the hydroxyapatite nanoparticle of low cost, controlledly synthesis different-shape is significant for its performance study and application and development.Therefore, how can have very important significance for its practical application tool by the hydroxyapatite of the synthetic different-shape of simple method.
Summary of the invention
The object of the present invention is to provide the synthetic method of a kind of simple, low cost, the hydroxyapatite nanoparticle that pollution-free, pattern is controlled.
For achieving the above object, technical scheme of the present invention is:
A synthetic method for hydroxyapatite nanoparticle, is characterized in that, described hydroxyapatite nanoparticle consist of Ca
10(PO
4)
6(OH)
2, it is made by following steps:
1) L-glutamic acid is added in calcium chloride water and obtains mixing solutions, the mol ratio of its Glutamic Acid and calcium chloride is 0-4:1, and the concentration of calcium chloride solution is 0.25 mol/L;
2) urea is added in tripolyphosphate sodium water solution and obtains mixing solutions, wherein the mol ratio of tripoly phosphate sodium STPP and calcium chloride is 1-10:5, and urea and calcium chloride mol ratio are 0-5:1, and the concentration of tripolyphosphate sodium water solution is 0.05-0.5 mol/L;
3) step 1) gained mixing solutions is slowly added drop-wise to step 2) in gained mixing solutions, after stirring, proceed to reactor, then reactor is placed in to baking oven and at 180 DEG C, reacts 10 hours, by centrifugal products therefrom, wash, be drying to obtain described hydroxyapatite nanoparticle.
In such scheme, the baking oven in described step 3) is air dry oven, and reactor is teflon-lined high-temperature high-pressure reaction kettle.
In such scheme, the centrifuge washing step in described step 3) is to utilize water and ethanol to replace centrifuge washing, and drying temperature is 60 DEG C, and be 4 hours time of drying.
In such scheme, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 0:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 1:5; The mol ratio of urea and calcium chloride is 5:1; The concentration of tripolyphosphate sodium water solution is 0.05 mol/L.
In such scheme, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 0:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 10:5; The mol ratio of urea and calcium chloride is 5:1; The concentration of tripolyphosphate sodium water solution is 0.5 mol/L.
In such scheme, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 0:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 10:5; The mol ratio of urea and calcium chloride is 0:1; The concentration of tripolyphosphate sodium water solution is 0.5 mol/L.
In such scheme, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 1:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 1:5; The mol ratio of urea and calcium chloride is 5:1; The concentration of tripolyphosphate sodium water solution is 0.05 mol/L.
In such scheme, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 1:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 10:5; The mol ratio of urea and calcium chloride is 0:1; The concentration of tripolyphosphate sodium water solution is 0.5 mol/L.
In such scheme, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 4:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 10:5; The mol ratio of urea and calcium chloride is 5:1; The concentration of tripolyphosphate sodium water solution is 0.5 mol/L.
In such scheme, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 4:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 1:5; The mol ratio of urea and calcium chloride is 5:1; The concentration of tripolyphosphate sodium water solution is 0.05 mol/L.
Controlled nanoparticle, nanofiber, microballoon or the prism of referring to of pattern of the present invention.
The invention has the beneficial effects as follows: in simple reaction system, by changing the ratio of reactant, realized the controlledly synthesis of different-shape hydroxyapatite.The inventive method agents useful for same is conventional, low price; Synthesis step is simple; Product pattern is controlled, favorable dispersity.The different-shape hydroxyapatite nanoparticle of synthesized can be used for the every field such as artificial bone, medicine carrying material, medicine and functional toothpaste.
Brief description of the drawings
Fig. 1 is the stereoscan photograph that embodiment 1 obtains product.
Fig. 2 is the stereoscan photograph that embodiment 2 obtains product.
Fig. 3 is the stereoscan photograph that embodiment 3 obtains product.
Fig. 4 is the stereoscan photograph that embodiment 4 obtains product.
Fig. 5 is the stereoscan photograph that embodiment 4 obtains product.
Fig. 6 is the stereoscan photograph that embodiment 5 obtains product.
Fig. 7 is the stereoscan photograph that embodiment 6 obtains product.
Fig. 8 is the stereoscan photograph that embodiment 7 obtains product.
Fig. 9 is the XRD figure spectrum that embodiment 1 obtains product.
Figure 10 is the XRD figure spectrum that embodiment 2 obtains product.
Figure 11 is the XRD figure spectrum that embodiment 3 obtains product.
Figure 12 is the XRD figure spectrum that embodiment 4 obtains product.
Figure 13 is the XRD figure spectrum that embodiment 5 obtains product.
Figure 14 is the XRD figure spectrum that embodiment 6 obtains product.
Figure 15 is the XRD figure spectrum that embodiment 7 obtains product.
Embodiment
For a better understanding of the present invention, further illustrate content of the present invention below in conjunction with embodiment and accompanying drawing, but content of the present invention is not only confined to the following examples.
Embodiment 1
0.5549g calcium chloride adds in 20mL deionized water, under magnetic agitation, dissolves, and obtains calcium chloride solution; 0.3679g tripoly phosphate sodium STPP is joined in 20mL deionized water, under magnetic agitation, dissolve; 1.5012g urea is added in above-mentioned sodium tripolyphosphate solution, under magnetic agitation, dissolve, obtain mixed solution A; Calcium chloride solution is dropwise joined in mixed solution A, and magnetic agitation ten minutes, obtains mixing solutions B; Mixing solutions B proceeded in the reactor of 50mL, in 180 DEG C of reactions 10 hours.After reaction finishes, reactor naturally cools to room temperature, with deionized water and alternately centrifugal (9000 revs/min, 5 minutes) washing of ethanol; Product is dried 4 hours at 60 DEG C, obtains hydroxyapatite nanoparticle.Fig. 1 is the stereoscan photograph that obtains product, shows that the product of gained is homodisperse nano particle, and Fig. 9 is the XRD figure spectrum of product, with JCPDS card number: 74-0565(Ca
10(PO
4)
6(OH)
2) contrast, the product that gained is described is hydroxyapatite.
0.5549g calcium chloride adds in 20mL deionized water, under magnetic agitation, dissolves, and obtains calcium chloride solution; 3.6786g tripoly phosphate sodium STPP is joined in 20mL deionized water, under magnetic agitation, dissolve; 1.5012g urea is added in above-mentioned sodium tripolyphosphate solution, under magnetic agitation, dissolve, obtain mixed solution A; Calcium chloride solution is dropwise joined in mixed solution A, and magnetic agitation ten minutes, obtains mixing solutions B; Mixing solutions B proceeded in the reactor of 50mL, in 180 DEG C of reactions 10 hours.After reaction finishes, reactor naturally cools to room temperature, with deionized water and alternately centrifugal (9000 revs/min, 5 minutes) washing of ethanol; Product is dried 4 hours at 60 DEG C, obtains hydroxyapatite nanoparticle.Fig. 2 is the stereoscan photograph that obtains product, shows that the product of gained is homodisperse nano particle, and Figure 10 is the XRD figure spectrum of product, with JCPDS card number: 74-0565(Ca
10(PO
4)
6(OH)
2) contrast, the product that gained is described is hydroxyapatite.
Embodiment 3
0.5549g calcium chloride adds in 20mL deionized water, under magnetic agitation, dissolves, and obtains calcium chloride solution; 3.6786g tripoly phosphate sodium STPP is joined in 20mL deionized water, under magnetic agitation, dissolve, obtain sodium tripolyphosphate solution; Calcium chloride solution is dropwise joined in sodium tripolyphosphate solution, and magnetic agitation ten minutes, obtains mixed solution A; Mixed solution A proceeded in the reactor that solvent is 50mL, in 180 DEG C of reactions 10 hours.After reaction finishes, reactor naturally cools to room temperature, with deionized water and alternately centrifugal (9000 revs/min, 5 minutes) washing of ethanol; Product is dried 4 hours at 60 DEG C, obtains hydroxyapatite nanofiber.Fig. 3 is the stereoscan photograph that obtains product, shows that the product of gained is nanofiber, and Figure 11 is the XRD figure spectrum of product, with JCPDS card number: 74-0565(Ca
10(PO
4)
6(OH)
2) contrast, the product that gained is described is hydroxyapatite.
Embodiment 4
0.5549g calcium chloride adds in 20mL deionized water, under magnetic agitation, dissolves; 0.7356g L-glutamic acid is added in above-mentioned calcium chloride solution, and heating for dissolving under magnetic agitation, obtains mixed solution A; 0.3679g tripoly phosphate sodium STPP is joined in 20mL deionized water, under magnetic agitation, dissolve; 1.5012g urea is added in above-mentioned sodium tripolyphosphate solution, under magnetic agitation, dissolve, obtain mixing solutions B; Mixed solution A is dropwise joined in mixing solutions B, and magnetic agitation ten minutes, obtains mixed solution C; Mixed solution C proceeded in the reactor of 50mL, in 180 DEG C of reactions 10 hours.After reaction finishes, reactor naturally cools to room temperature, with deionized water and alternately centrifugal (9000 revs/min, 5 minutes) washing of ethanol; Product is dried 4 hours at 60 DEG C, obtains hydroxyapatite nanoparticle.Fig. 4 and Fig. 5 are the stereoscan photographs that obtains product, show that the product of gained is nano particle and the microballoon that is assembled into by nano particle, and Figure 12 is the XRD figure spectrum of product, with JCPDS card number: 74-0565(Ca
10(PO
4)
6(OH)
2) contrast, the product that gained is described is hydroxyapatite.
Embodiment 5
0.5549g calcium chloride adds in 20mL deionized water, under magnetic agitation, dissolves; 0.7356g L-glutamic acid is added in above-mentioned calcium chloride solution, and heating for dissolving under magnetic agitation, obtains mixed solution A; 3.6786g tripoly phosphate sodium STPP is joined in 20mL deionized water, under magnetic agitation, dissolve, obtain sodium tripolyphosphate solution; Mixed solution A is dropwise joined in sodium tripolyphosphate solution, and magnetic agitation ten minutes, obtains mixing solutions B; Mixing solutions B proceeded in the reactor that solvent is 50mL, in 180 DEG C of reactions 10 hours.After reaction finishes, reactor naturally cools to room temperature, with deionized water and alternately centrifugal (9000 revs/min, 5 minutes) washing of ethanol; Product is dried 4 hours at 60 DEG C, obtains hydroxyapatite nanoparticle.Fig. 6 is the stereoscan photograph that obtains product, shows that the product of gained is homodisperse nanofiber, and Figure 13 is the XRD figure spectrum of product, with JCPDS card number: 74-0565(Ca
10(PO
4)
6(OH)
2) contrast, the product that gained is described is hydroxyapatite.
Embodiment 6
0.5549g calcium chloride adds in 20mL deionized water, under magnetic agitation, dissolves; 2.9426g L-glutamic acid is added in above-mentioned calcium chloride solution, and heating for dissolving under magnetic agitation, obtains mixed solution A; 3.6786g tripoly phosphate sodium STPP is joined in 20mL deionized water, under magnetic agitation, dissolve; 1.5012g urea is added in above-mentioned sodium tripolyphosphate solution, under magnetic agitation, dissolve, obtain mixing solutions B; Mixed solution A is dropwise joined in mixing solutions B, and magnetic agitation ten minutes, obtains mixed solution C; Mixed solution C proceeded in the reactor of 50mL, in 180 DEG C of reactions 10 hours.After reaction finishes, reactor naturally cools to room temperature, with deionized water and alternately centrifugal (9000 revs/min, 5 minutes) washing of ethanol; Product is dried 4 hours at 60 DEG C, obtains hydroxyapatite particles.Fig. 7 is the stereoscan photograph that obtains product, and the product that shows gained is the hydroxyapatite prism of assembling bunchy, and Figure 14 is the XRD figure spectrum of product, with JCPDS card number: 74-0565(Ca
10(PO
4)
6(OH)
2) contrast, the product that gained is described is hydroxyapatite.
Embodiment 7
0.5549g calcium chloride adds in 20mL deionized water, under magnetic agitation, dissolves; 2.9426g L-glutamic acid is added in above-mentioned calcium chloride solution, and heating for dissolving under magnetic agitation, obtains mixed solution A; 0.3679g tripoly phosphate sodium STPP is joined in 20mL deionized water, under magnetic agitation, dissolve; 1.5012g urea is added in above-mentioned sodium tripolyphosphate solution, under magnetic agitation, dissolve, obtain mixing solutions B; Mixed solution A is dropwise joined in mixing solutions B, and magnetic agitation ten minutes, obtains mixed solution C; Mixed solution C proceeded in the reactor of 50mL, in 180 DEG C of reactions 10 hours.After reaction finishes, reactor naturally cools to room temperature, with deionized water and alternately centrifugal (9000 revs/min, 5 minutes) washing of ethanol; Product is dried 4 hours at 60 DEG C, obtains hydroxyapatite micro-sphere and prism.Fig. 8 is the stereoscan photograph that obtains product, shows that the product of gained is hydroxyapatite micro-sphere and prism, and Figure 15 is the XRD figure spectrum of product, with JCPDS card number: 74-0565(Ca
10(PO
4)
6(OH)
2) contrast, the product that gained is described is hydroxyapatite.
Claims (10)
1. a synthetic method for hydroxyapatite nanoparticle, is characterized in that, described hydroxyapatite nanoparticle consist of Ca
10(PO
4)
6(OH)
2, it is made by following steps:
1) L-glutamic acid is added in calcium chloride water and obtains mixing solutions, the mol ratio of its Glutamic Acid and calcium chloride is 0-4:1, and the concentration of calcium chloride solution is 0.25 mol/L;
2) urea is added in tripolyphosphate sodium water solution and obtains mixing solutions, wherein the mol ratio of tripoly phosphate sodium STPP and calcium chloride is 1-10:5, and urea and calcium chloride mol ratio are 0-5:1, and the concentration of tripolyphosphate sodium water solution is 0.05-0.5 mol/L;
3) step 1) gained mixing solutions is slowly added drop-wise to step 2) in gained mixing solutions, after stirring, proceed to reactor, then reactor is placed in to baking oven and at 180 DEG C, reacts 10 hours, by centrifugal products therefrom, wash, be drying to obtain described hydroxyapatite nanoparticle.
2. synthetic method as claimed in claim 1, is characterized in that, the baking oven in described step 3) is air dry oven, and reactor is teflon-lined high-temperature high-pressure reaction kettle.
3. synthetic method as claimed in claim 1, is characterized in that, the centrifuge washing step in described step 3) is to utilize water and ethanol to replace centrifuge washing, and drying temperature is 60 DEG C, and be 4 hours time of drying.
4. synthetic method as claimed in claim 1, is characterized in that, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 0:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 1:5; The mol ratio of urea and calcium chloride is 5:1; The concentration of tripolyphosphate sodium water solution is 0.05 mol/L.
5. synthetic method as claimed in claim 1, is characterized in that, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 0:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 10:5; The mol ratio of urea and calcium chloride is 5:1; The concentration of tripolyphosphate sodium water solution is 0.5 mol/L.
6. synthetic method as claimed in claim 1, is characterized in that, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 0:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 10:5; The mol ratio of urea and calcium chloride is 0:1; The concentration of tripolyphosphate sodium water solution is 0.5 mol/L.
7. synthetic method as claimed in claim 1, is characterized in that, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 1:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 1:5; The mol ratio of urea and calcium chloride is 5:1; The concentration of tripolyphosphate sodium water solution is 0.05 mol/L.
8. synthetic method as claimed in claim 1, is characterized in that, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 1:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 10:5; The mol ratio of urea and calcium chloride is 0:1; The concentration of tripolyphosphate sodium water solution is 0.5 mol/L.
9. synthetic method as claimed in claim 1, is characterized in that, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 4:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 10:5; The mol ratio of urea and calcium chloride is 5:1; The concentration of tripolyphosphate sodium water solution is 0.5 mol/L.
10. synthetic method as claimed in claim 1, is characterized in that, the mol ratio of described step 1) Glutamic Acid and calcium chloride is 4:1; Described step 2) in the mol ratio of tripoly phosphate sodium STPP and calcium chloride be 1:5; The mol ratio of urea and calcium chloride is 5:1; The concentration of tripolyphosphate sodium water solution is 0.05 mol/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104555966A (en) * | 2014-12-10 | 2015-04-29 | 华南理工大学 | Organic biomolecular composite calcium phosphate nanoparticles and preparation method thereof |
| CN113943192A (en) * | 2021-12-06 | 2022-01-18 | 厦门紫金矿冶技术有限公司 | Nano hybrid N, P slow release fertilizer and preparation method thereof |
| CN115246636A (en) * | 2022-03-30 | 2022-10-28 | 南京大学 | Preparation method of calcium polyphosphate with high biological activity |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583288A (en) * | 2012-02-01 | 2012-07-18 | 福州大学 | Hydroxyapatite nanorod as well as preparation method and alignment controlling method thereof |
| CN103420364A (en) * | 2013-07-13 | 2013-12-04 | 西南交通大学 | Preparation method of grapheme/hydroxyapatite composite material |
-
2014
- 2014-04-01 CN CN201410128802.0A patent/CN103896233B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583288A (en) * | 2012-02-01 | 2012-07-18 | 福州大学 | Hydroxyapatite nanorod as well as preparation method and alignment controlling method thereof |
| CN103420364A (en) * | 2013-07-13 | 2013-12-04 | 西南交通大学 | Preparation method of grapheme/hydroxyapatite composite material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104555966A (en) * | 2014-12-10 | 2015-04-29 | 华南理工大学 | Organic biomolecular composite calcium phosphate nanoparticles and preparation method thereof |
| CN113943192A (en) * | 2021-12-06 | 2022-01-18 | 厦门紫金矿冶技术有限公司 | Nano hybrid N, P slow release fertilizer and preparation method thereof |
| CN115246636A (en) * | 2022-03-30 | 2022-10-28 | 南京大学 | Preparation method of calcium polyphosphate with high biological activity |
| CN115246636B (en) * | 2022-03-30 | 2023-10-24 | 南京大学 | Preparation method of bioactive high calcium polyphosphate |
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Effective date of registration: 20181009 Address after: 430070 122 Luo Shi Road, Wuchang, Wuhan, Hubei. Patentee after: Wuhan Huawei Biological Material Engineering Co Ltd Address before: 430070 Hubei Province, Wuhan city Hongshan District Luoshi Road No. 122 Patentee before: Wuhan University of Technology |