CN110538347A - High-porosity porous nano hydroxyapatite microspheres and preparation method thereof - Google Patents
High-porosity porous nano hydroxyapatite microspheres and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-porosity porous nano hydroxyapatite microsphere and a preparation method thereof. The hydroxyapatite composite microsphere prepared by the method has uniform size distribution, the particle size distribution range of 10-100 mu m and the central particle size of 20-60 mu m. The organic phase is added in the mixing process, so that the suspension stability of the suspension can be effectively enhanced, the prepared microspheres are uniform in size distribution, have larger particle size than the microspheres prepared by the traditional spray drying method, and can be used as an inner support material of an injection; the microspheres have good spherical shape and high porosity, and can enhance the injectability of the material.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a high-porosity porous nano hydroxyapatite microsphere and a preparation method thereof.
Background
Hydroxyapatite (HAP) has attracted extensive attention from biomaterials and medical professionals because its structure and composition are very close to human bone tissue. HAP is used as a bone filling material in orthopedics, stomatology and plastic surgery, is also used as a carrier for growth factors, drugs and the like, and shows good slow release performance. In order to meet different clinical requirements, researchers prepare HAPs in different shapes such as rods, dumbbells, spheres, tablets and the like. Spherical hydroxyapatite is currently receiving great attention due to its strong flowability, large specific surface area and high bulk density.
The method for preparing the hydroxyapatite microspheres is various, such as a hydrothermal method, an emulsion crosslinking method, a microwave method and a spray drying method. The emulsion crosslinking method is mainly used for preparing organic-inorganic composite hydroxyapatite microspheres, but the method has the problems that the microspheres are easy to agglomerate, the crosslinking agent is difficult to completely remove, and the like. The spray drying method has the advantages of simple operation, no need of adding toxic reagents, easy industrialization and the like, but also has the defects of irregular microspherical shape, wide particle size distribution and the like. The preparation method of the porous hydroxyapatite comprises a chemical foaming method, a pore-forming agent method, an organic foam impregnation method and an organic template method. When the porous hydroxyapatite is prepared by a chemical foaming method, the aperture and the porosity of the porous material are difficult to control, most of the pores of the porous material obtained by the method are closed, and the penetration rate of pores is poor. The porous hydroxyapatite prepared by the pore-forming agent method has low porosity and wide pore size distribution. In the process of drying and sintering, the organic foam impregnation method is easy to generate tiny cracks on the biological material, and the strength of the porous hydroxyapatite is reduced. The organic template method needs to select a proper surfactant, and the selected surfactant is possibly toxic and can be removed at high temperature under some conditions, so that the biological activity of the porous hydroxyapatite is reduced.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a preparation method of a high-porosity porous nano hydroxyapatite microsphere, which comprises the following steps:
The method comprises the following steps: adding the nano hydroxyapatite powder into water to prepare hydroxyapatite slurry with the content of 10-40% (w/v);
Step two: mixing the hydroxyapatite slurry, the pore-forming agent and the oleic acid in proportion, placing the mixture in a ball mill for ball milling for 6 to 24 hours, and obtaining uniform suspension after ball milling;
Step three: adding the suspension into an organic complexing agent, mixing in proportion, and then putting into a water bath kettle at 30-80 ℃ to be stirred and dissolved;
step four: carrying out spray drying granulation on the uniformly dissolved suspension to obtain solidified microspheres;
Step five: and (3) performing high-temperature dewaxing treatment on the prepared solidified microspheres, and calcining at high temperature to prepare the high-porosity porous nano hydroxyapatite microspheres.
Preferably, the weight ratio of the hydroxyapatite slurry to the pore-forming agent is 80-95: 20-5.
preferably, the organic complexing agent is any combination of one or more of gelatin, Arabic gum, chitosan, sodium alginate, polylactic acid and natural cellulose.
Preferably, the pore-forming agent is any one or any combination of carbon powder, graphite powder and acetylene black.
preferably, the stirring speed of the water bath kettle is 200-.
preferably, the dewaxing temperature is 800-1500 ℃, and the dewaxing treatment time is 30-120 min.
preferably, the high-temperature calcination temperature is 1000-1500 ℃, and the calcination time is 45-180 min.
Preferably, the spraying temperature is 250 ℃ to 500 ℃, the feeding speed is 10 to 30ml/min, and the spraying pressure is 0.05 to 0.1 MPa.
The invention also provides a high-porosity porous nano hydroxyapatite microsphere which is prepared by adopting the preparation method, the particle size distribution range of the high-porosity porous nano hydroxyapatite microsphere is 10-100 mu m, the central particle size is 20-60 mu m, and the porosity is 60-90%.
Compared with the prior art, the invention has the beneficial effects that: the hydroxyapatite composite microsphere prepared by the method has uniform size distribution, the particle size distribution range of 10-100 mu m and the central particle size of 20-60 mu m. The organic phase is added in the mixing process, so that the suspension stability of the suspension can be effectively enhanced, the prepared microspheres are uniform in size distribution, have larger particle size than the microspheres prepared by the traditional spray drying method, and can be used as an inner support material of an injection; the microspheres have good spherical shape and high porosity, and can enhance the injectability of the material.
Detailed Description
The method for preparing the high-porosity porous nano-hydroxyapatite microspheres according to the present invention will be described in more detail below, in which preferred embodiments of the present invention are shown, it being understood that a person skilled in the art may modify the invention described herein while still achieving the advantageous effects of the present invention. Accordingly, the following description should be construed as broadly as possible to those skilled in the art and not as limiting the invention.
Example 1
the preparation method of the porous nano hydroxyapatite microspheres with high porosity comprises the following steps:
The method comprises the following steps: adding the nano hydroxyapatite powder into water to prepare hydroxyapatite slurry with the content of 10-40% (w/v);
Step two: mixing hydroxyapatite slurry, a pore-forming agent and oleic acid in proportion, wherein the weight ratio of the hydroxyapatite slurry to the pore-forming agent is 80: 20. Ball-milling in a ball mill for 6-24 hours to obtain uniform suspension; the pore former is carbon powder.
step three: adding the suspension into an organic complexing agent, mixing in proportion, and then putting into a water bath kettle at 80 ℃ to be stirred and dissolved; the organic complexing agent is the combination of gelatin, Arabic gum, chitosan and sodium alginate. The stirring speed of the water bath kettle is 600r/min, and the dissolving time is 5 h.
Step four: carrying out spray drying granulation on the uniformly dissolved suspension, wherein the spraying temperature is 250 ℃, the feeding speed is 10ml/min, and the spraying pressure is 0.05MPa, so as to obtain solidified microspheres;
step five: carrying out high-temperature dewaxing treatment on the prepared solidified microspheres, wherein the dewaxing temperature is 800 ℃, and the dewaxing treatment time is 120 min; and then calcining the mixture at a high temperature of 1000 ℃ for 120min to prepare the high-porosity porous nano hydroxyapatite microspheres. In this embodiment 1, the particle size distribution range of the porous hydroxyapatite nanoparticles with high porosity is 20-75 μm, the central particle size is 20-60 μm, and the porosity is 78%.
Example 2
The preparation method of the porous nano hydroxyapatite microspheres with high porosity comprises the following steps:
the method comprises the following steps: adding the nano hydroxyapatite powder into water to prepare hydroxyapatite slurry with the content of 10-40% (w/v);
Step two: mixing hydroxyapatite slurry, a pore-forming agent and oleic acid in proportion, wherein the weight ratio of the hydroxyapatite slurry to the pore-forming agent is 85: 15. Ball-milling in a ball mill for 6-24 hours to obtain uniform suspension; the pore former is carbon powder.
Step three: adding the suspension into an organic complexing agent, mixing in proportion, and then putting into a water bath kettle at 50 ℃ to be stirred and dissolved; the organic complexing agent is the combination of gelatin, Arabic gum, chitosan and sodium alginate. The stirring speed of the water bath kettle is 250r/min, and the dissolving time is 5 h.
Step four: carrying out spray drying granulation on the uniformly dissolved suspension, wherein the spraying temperature is 250 ℃, the feeding speed is 10ml/min, and the spraying pressure is 0.05MPa, so as to obtain solidified microspheres;
Step five: carrying out high-temperature dewaxing treatment on the prepared solidified microspheres, wherein the dewaxing temperature is 1500 ℃, and the dewaxing treatment time is 60 min; and then calcining the mixture at a high temperature of 1000 ℃ for 180min to prepare the high-porosity porous nano hydroxyapatite microspheres. In this embodiment 2, the particle size distribution range of the porous hydroxyapatite nanoparticles with high porosity is 60-85 μm, the central particle size is 20-60 μm, and the porosity is 78%.
Example 3
The preparation method of the porous nano hydroxyapatite microspheres with high porosity comprises the following steps:
the method comprises the following steps: adding the nano hydroxyapatite powder into water to prepare hydroxyapatite slurry with the content of 10-40% (w/v);
step two: mixing hydroxyapatite slurry, a pore-forming agent and oleic acid in proportion, wherein the weight ratio of the hydroxyapatite slurry to the pore-forming agent is 95: 5. Ball-milling in a ball mill for 6-24 hours to obtain uniform suspension; the pore former is carbon powder.
step three: adding the suspension into an organic complexing agent, mixing in proportion, and then putting into a water bath kettle at 50 ℃ to be stirred and dissolved; the organic complexing agent is the combination of gelatin, Arabic gum, chitosan and sodium alginate. The stirring speed of the water bath kettle is 250r/min, and the dissolving time is 5 h.
step four: carrying out spray drying granulation on the uniformly dissolved suspension, wherein the spraying temperature is 250 ℃, the feeding speed is 10ml/min, and the spraying pressure is 0.1MPa, so as to obtain solidified microspheres;
step five: carrying out high-temperature dewaxing treatment on the prepared solidified microspheres, wherein the dewaxing temperature is 1500 ℃, and the dewaxing treatment time is 60 min; and then calcining the mixture at a high temperature of 1000 ℃ for 180min to prepare the high-porosity porous nano hydroxyapatite microspheres. In this embodiment 3, the particle size distribution range of the porous hydroxyapatite nanoparticles with high porosity is 50-85 μm, the central particle size is 20-60 μm, and the porosity is 89%. The high-porosity porous nano hydroxyapatite microspheres prepared by the embodiment have high porosity, almost complete penetration and moderate mechanical strength.
The above description is only a preferred embodiment of the present invention, and does not limit the present invention in any way. It will be understood by those skilled in the art that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A preparation method of porous nano hydroxyapatite microspheres with high porosity is characterized by comprising the following steps:
The method comprises the following steps: adding the nano hydroxyapatite powder into water to prepare hydroxyapatite slurry with the content of 10-40% (w/v);
Step two: mixing the hydroxyapatite slurry, the pore-forming agent and the oleic acid in proportion, placing the mixture in a ball mill for ball milling for 6 to 24 hours, and obtaining uniform suspension after ball milling;
step three: adding the suspension into an organic complexing agent, mixing in proportion, and then putting into a water bath kettle at 30-80 ℃ to be stirred and dissolved;
Step four: carrying out spray drying granulation on the uniformly dissolved suspension to obtain solidified microspheres;
step five: and (3) performing high-temperature dewaxing treatment on the prepared solidified microspheres, and calcining at high temperature to prepare the high-porosity porous nano hydroxyapatite microspheres.
2. The preparation method of the high-porosity porous nano hydroxyapatite microspheres according to claim 1, wherein the weight ratio of the hydroxyapatite slurry to the pore forming agent is 80-95: 20-5.
3. the preparation method of the high-porosity porous nano hydroxyapatite microspheres according to claim 1, wherein the organic complexing agent is one or more of gelatin, acacia, chitosan, sodium alginate, polylactic acid and natural cellulose.
4. The preparation method of the high-porosity porous nano hydroxyapatite microspheres according to claim 1, wherein the pore forming agent is any one or any combination of carbon powder, graphite powder and acetylene black.
5. The method for preparing porous nano hydroxyapatite microspheres with high porosity according to claim 1, wherein the stirring speed of the water bath is 200-600r/min, and the dissolving time is 2-5 h.
6. The preparation method of the high-porosity porous nano hydroxyapatite microspheres according to claim 1, wherein the dewaxing temperature is 800 to 1500 ℃, and the dewaxing treatment time is 30 to 120 min.
7. the preparation method of the high-porosity porous nano hydroxyapatite microspheres according to claim 1, wherein the high-temperature calcination temperature is 1000-1500 ℃, and the calcination time is 45-180 min.
8. The method for preparing porous nano hydroxyapatite microspheres with high porosity according to claim 1, wherein the spraying temperature is 250 ℃ and 500 ℃, the feeding speed is 10-30ml/min, and the spraying pressure is 0.05-0.1 MPa.
9. The preparation method of the high-porosity porous nano hydroxyapatite microspheres according to any one of claims 1 to 8, wherein the high-porosity porous nano hydroxyapatite microspheres have a particle size distribution range of 10 to 100 μm, a central particle size of 20 to 60 μm, and a porosity of 60 to 90%.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| BE20195546A BE1027375B1 (en) | 2018-12-10 | 2019-08-20 | High porosity porous nanohydroxyapatite microsphere and its preparation process |
| NL2023794A NL2023794B1 (en) | 2018-12-12 | 2019-09-09 | Porous Nano-hydroxyapatite Microsphere with High Porosity and a Preparation Method Thereof |
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| CN2018115149125 | 2018-12-12 | ||
| CN201811514912.5A CN109529111A (en) | 2018-12-12 | 2018-12-12 | High porosity porous nano hydroxyapatite micro-sphere and preparation method thereof |
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| CN201910324114.4A Pending CN110538347A (en) | 2018-12-10 | 2019-04-22 | High-porosity porous nano hydroxyapatite microspheres and preparation method thereof |
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| BE1027375B1 (en) * | 2018-12-10 | 2021-01-26 | Shanghai Moyang Biotechnology Co Ltd | High porosity porous nanohydroxyapatite microsphere and its preparation process |
| CN110681323B (en) * | 2019-08-26 | 2021-12-21 | 上海摩漾生物科技有限公司 | Golf ball type degradable microsphere with micro-topological structure and preparation method thereof |
| CN115572177A (en) * | 2021-07-05 | 2023-01-06 | 陈月端 | Bone filler prepared from natural calcium-containing waste and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343054A (en) * | 2008-08-19 | 2009-01-14 | 华南理工大学 | Preparation method of hydroxyapatite microsphere |
| CN106458585A (en) * | 2014-03-03 | 2017-02-22 | 百维科技有限责任公司 | Spherical porous hydroxyapatite sorbent and methods thereof |
| CN108178656A (en) * | 2018-01-11 | 2018-06-19 | 江西理工大学 | A kind of high porosity porous ceramics microballoon and preparation method thereof |
| CN109529110A (en) * | 2018-12-10 | 2019-03-29 | 上海摩漾生物科技有限公司 | Porous nano hydroxyapatite sustained-release gel preparation method |
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- 2018-12-12 CN CN201811514912.5A patent/CN109529111A/en active Pending
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- 2019-04-22 CN CN201910324114.4A patent/CN110538347A/en active Pending
- 2019-09-09 NL NL2023794A patent/NL2023794B1/en active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343054A (en) * | 2008-08-19 | 2009-01-14 | 华南理工大学 | Preparation method of hydroxyapatite microsphere |
| CN106458585A (en) * | 2014-03-03 | 2017-02-22 | 百维科技有限责任公司 | Spherical porous hydroxyapatite sorbent and methods thereof |
| CN108178656A (en) * | 2018-01-11 | 2018-06-19 | 江西理工大学 | A kind of high porosity porous ceramics microballoon and preparation method thereof |
| CN109529110A (en) * | 2018-12-10 | 2019-03-29 | 上海摩漾生物科技有限公司 | Porous nano hydroxyapatite sustained-release gel preparation method |
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| NL2023794B1 (en) | 2020-11-18 |
| NL2023794A (en) | 2020-10-27 |
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