CN106744765A - The method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate - Google Patents
The method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate Download PDFInfo
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- CN106744765A CN106744765A CN201611068024.6A CN201611068024A CN106744765A CN 106744765 A CN106744765 A CN 106744765A CN 201611068024 A CN201611068024 A CN 201611068024A CN 106744765 A CN106744765 A CN 106744765A
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- China
- Prior art keywords
- sphere
- calcium carbonate
- hydroxyapatite micro
- template
- hollow hydroxyapatite
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Medicinal Preparation (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to technical field of function materials, and in particular to a kind of method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate.The method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate, comprises the following steps：（1）The preparation of calcium carbonate microspheres；（2）The preparation of hollow hydroxyapatite micro-sphere.The hollow hydroxyapatite micro-sphere form for preparing of the invention is uniform, size is consistent；Using less reagent, there is potential application prospect in medical domain in ball preferably.
Description
Technical field
The present invention relates to technical field of function materials, and in particular to one kind prepares hollow hydroxy-apatite by template of calcium carbonate
The method of stone microballoon.
Background technology
Hydroxyapatite has the structure and composition similar to the inorganic constituents of organism bone, determines that it has well
Biocompatibility, bioactivity and osteoconductive energy, therefore, hydroxyapatite is widely used in biomedical sector, such as
The aspect such as drug delivery and tissue repair.
And the pattern and property of hydroxyapatite determine the application of hydroxyapatite, hollow hydroxyapatite micro-sphere has
Larger specific surface area, has broader practice prospect in drug delivery and tissue repair.Prepare hydroxyapatite micro-sphere
Method it is more, but preparation method is more complicated or higher to equipment requirement mostly, and such as spray drying needs more complicated experiment
Journey and higher device requirement, the hydroxyapatite micro-sphere of rule is prepared using gamma transition method, but preparation temperature is 1200 DEG C,
And consume substantial amounts of raw material.Other prepare the method for hydroxyapatite micro-sphere mostly using organic reagent, and this has a strong impact on
Application of the hydroxyapatite micro-sphere in organism.
The content of the invention
The present invention is directed to propose a kind of method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate.
Technical program of the present invention lies in：
The method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate, comprises the following steps：
（1）The preparation of calcium carbonate microspheres
The Citric Acid Mono for weighing 0.1 ~ 0.3 mol adds 100 ~ 120 mL CaCl2During concentration is for the solution of 0.5mol/L,
Stirring is uniformly dissolved it, and the pH values that solution is adjusted with NaOH solution are 5.8, pour into 100 mL 0.5mol/L's under stirring
Na2CO3Solution, 22 ~ 24h of standing sedimentation after being well mixed；Filtering, water washing and is dried with distillation；
（2）The preparation of hollow hydroxyapatite micro-sphere
By (NH4) of 0.0024 ~ 0.0036 mol2HPO4Fully dissolved in 40mL distilled water, add 0.004mol's
CaCO3, the pH values that solution is adjusted with NaOH solution are 12, are transferred to hydro-thermal in the polytetrafluoroethylene (PTFE) autoclave pressure of 40mL；Naturally it is cold
But to room temperature, with distilling water washing and drying, hollow hydroxyapatite micro-sphere is obtained.
Described CaCO3Calcium phosphorus mol ratio is 5: 3.
The concentration of described NaOH solution is 1.0 ~ 1.3 mol/L.
The temperature of described hydro-thermal is 120 ~ 140 DEG C, and the hydro-thermal time is 40 ~ 42h.
Described dry temperature is 50 ~ 55 DEG C, and the hydro-thermal time is 23 ~ 24h.
Described drying temperature is 50 ~ 60 DEG C.
The technical effects of the invention are that：
The hollow hydroxyapatite micro-sphere form for preparing of the invention is uniform, size is consistent；Using less reagent, in ball compared with
It is good, there is potential application prospect in medical domain.
Specific embodiment
The method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate, comprises the following steps：
Embodiment 1
（1）The preparation of calcium carbonate microspheres
The Citric Acid Mono for weighing 0.1 ~ 0.3 mol adds 100 ~ 120 mL CaCl2During concentration is for the solution of 0.5mol/L,
Stirring is uniformly dissolved it, and the pH values that solution is adjusted with NaOH solution are 5.8, pour into 100 mL 0.5mol/L's under stirring
Na2CO3Solution, 22 ~ 24h of standing sedimentation after being well mixed；Filtering, water washing and is dried with distillation；
（2）The preparation of hollow hydroxyapatite micro-sphere
By (NH4) of 0.0024 ~ 0.0036 mol2HPO4Fully dissolved in 40mL distilled water, add 0.004mol's
CaCO3, the pH values that solution is adjusted with NaOH solution are 12, are transferred to hydro-thermal in the polytetrafluoroethylene (PTFE) autoclave pressure of 40mL；Naturally it is cold
But to room temperature, with distilling water washing and drying, hollow hydroxyapatite micro-sphere is obtained.
Embodiment 2
（1）The preparation of calcium carbonate microspheres
The Citric Acid Mono for weighing 0.1 mol adds 100 mL CaCl2Concentration is in the solution of 0.5mol/L, stirring makes it
It is uniformly dissolved, the pH values that solution is adjusted with NaOH solution are 5.8, and the Na of 100 mL 0.5mol/L is poured under stirring2CO3It is molten
Liquid, standing sedimentation 22h after being well mixed；Filtering, water washing and is dried with distillation；
（2）The preparation of hollow hydroxyapatite micro-sphere
By (NH4) of 0.0024mol2HPO4Fully dissolved in 40mL distilled water, add the CaCO of 0.004mol3, use NaOH
The pH values of solution regulation solution are 12, are transferred to hydro-thermal in the polytetrafluoroethylene (PTFE) autoclave pressure of 40mL；Room temperature is naturally cooled to, with steaming
Distilled water is washed and dried, and obtains hollow hydroxyapatite micro-sphere.
Wherein, described CaCO3Calcium phosphorus mol ratio is 5: 3.The concentration of described NaOH solution is 1.0mol/L.Institute
The temperature of the hydro-thermal stated is 120 DEG C, and the hydro-thermal time is 40h.Described dry temperature is 50 DEG C, and the hydro-thermal time is 23h.It is described
Drying temperature be 50 DEG C.
Embodiment 3
（1）The preparation of calcium carbonate microspheres
The Citric Acid Mono for weighing 0.3 mol adds 120 mL CaCl2Concentration is in the solution of 0.5mol/L, stirring makes it
It is uniformly dissolved, the pH values that solution is adjusted with NaOH solution are 5.8, and the Na of 100 mL 0.5mol/L is poured under stirring2CO3It is molten
Liquid, standing sedimentation 24h after being well mixed；Filtering, water washing and is dried with distillation；
（2）The preparation of hollow hydroxyapatite micro-sphere
By (NH4) of 0.0036 mol2HPO4Fully dissolved in 40mL distilled water, add the CaCO of 0.004mol3, use NaOH
The pH values of solution regulation solution are 12, are transferred to hydro-thermal in the polytetrafluoroethylene (PTFE) autoclave pressure of 40mL；Room temperature is naturally cooled to, with steaming
Distilled water is washed and dried, and obtains hollow hydroxyapatite micro-sphere.
Wherein, described CaCO3Calcium phosphorus mol ratio is 5: 3.The concentration of described NaOH solution is 1.3 mol/L.Institute
The temperature of the hydro-thermal stated is 140 DEG C, and the hydro-thermal time is 42h.Described dry temperature is 55 DEG C, and the hydro-thermal time is 24h.It is described
Drying temperature be 60 DEG C.
Claims (6)
1. the method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate, it is characterised in that：Comprise the following steps：
（1）The preparation of calcium carbonate microspheres
The Citric Acid Mono for weighing 0.1 ~ 0.3 mol adds 100 ~ 120 mL CaCl2During concentration is for the solution of 0.5mol/L, stir
Mixing is uniformly dissolved it, and the pH values that solution is adjusted with NaOH solution are 5.8, pour into 100 mL 0.5mol/L's under stirring
Na2CO3Solution, 22 ~ 24h of standing sedimentation after being well mixed；Filtering, water washing and is dried with distillation；
（2）The preparation of hollow hydroxyapatite micro-sphere
By (NH4) of 0.0024 ~ 0.0036 mol2HPO4Fully dissolved in 40mL distilled water, add 0.004mol's
CaCO3, the pH values that solution is adjusted with NaOH solution are 12, are transferred to hydro-thermal in the polytetrafluoroethylene (PTFE) autoclave pressure of 40mL；Naturally it is cold
But to room temperature, with distilling water washing and drying, hollow hydroxyapatite micro-sphere is obtained.
2. the method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate according to claim 1, its feature exists
In：Described CaCO3Calcium phosphorus mol ratio is 5: 3.
3. the method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate according to claim 1, its feature exists
In：The concentration of described NaOH solution is 1.0 ~ 1.3 mol/L.
4. the method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate according to claim 1, its feature exists
In：The temperature of described hydro-thermal is 120 ~ 140 DEG C, and the hydro-thermal time is 40 ~ 42h.
5. the method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate according to claim 1, its feature exists
In：Described dry temperature is 50 ~ 55 DEG C, and the hydro-thermal time is 23 ~ 24h.
6. the method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate according to claim 1, its feature exists
In：Described drying temperature is 50 ~ 60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611068024.6A CN106744765A (en) | 2016-11-29 | 2016-11-29 | The method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate |
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| CN201611068024.6A CN106744765A (en) | 2016-11-29 | 2016-11-29 | The method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate |
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| CN106744765A true CN106744765A (en) | 2017-05-31 |
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| CN201611068024.6A Pending CN106744765A (en) | 2016-11-29 | 2016-11-29 | The method for preparing hollow hydroxyapatite micro-sphere as template with calcium carbonate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125290A (en) * | 2020-09-15 | 2020-12-25 | 上海摩漾生物科技有限公司 | Calcium-phosphorus microsphere material containing defect sites and preparation and application thereof |
| CN112500097A (en) * | 2020-12-28 | 2021-03-16 | 湖北工业大学 | Self-repairing steel slag-slag concrete and preparation method thereof |
-
2016
- 2016-11-29 CN CN201611068024.6A patent/CN106744765A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125290A (en) * | 2020-09-15 | 2020-12-25 | 上海摩漾生物科技有限公司 | Calcium-phosphorus microsphere material containing defect sites and preparation and application thereof |
| CN112500097A (en) * | 2020-12-28 | 2021-03-16 | 湖北工业大学 | Self-repairing steel slag-slag concrete and preparation method thereof |
| CN112500097B (en) * | 2020-12-28 | 2022-06-14 | 湖北工业大学 | Self-repairing steel slag-slag concrete and preparation method thereof |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170531 |
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| WD01 | Invention patent application deemed withdrawn after publication |