CN101297978A - Preparation method of hydroxyapatite nano pole - Google Patents
Preparation method of hydroxyapatite nano pole Download PDFInfo
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- CN101297978A CN101297978A CNA2008101241917A CN200810124191A CN101297978A CN 101297978 A CN101297978 A CN 101297978A CN A2008101241917 A CNA2008101241917 A CN A2008101241917A CN 200810124191 A CN200810124191 A CN 200810124191A CN 101297978 A CN101297978 A CN 101297978A
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Abstract
The invention discloses a preparation method of a hydroxyapatite nano-rod, which adopts an oleic acid-ethanol-water phase transfer system with low cost to prepare the hydroxyapatite nano-rod with uniform size, controllable appearance and nano-scale. The hydroxyapatite nano-rod is prepared by the steps as follows: a. firstly, the oleic acid, ethanol and an additive are mixed; b. secondly, a calcium salt aqueous solution is dispersed into the oleic acid-ethanol mixed medium; the volume content of the calcium salt aqueous solution in a final mixed solution is 5 percent to 15 percent; the mass volume concentration of the calcium salt is 0.1 percent to 10 percent; c. then,a phosphate aqueous solution is added and mixed at room temperature; the mass volume concentration of the phosphate is 0.1 percent to 10 percent; d. the mixture generated from step c reacts in a reactor between 80 DEG C and 200 DEG C; e. centrifugation is carried out to remove a supernatant fluid and the obtained object is washed by a cleaning solvent and then dried so as to obtain the hydroxyapatite nano-rod. The preparation method is characterized by low production cost and comparatively high product quality, thus being hopeful to be applied in the medical field.
Description
Technical field
The present invention relates to a kind of preparation method of hydroxyapatite nano pole, particularly by adopting synthetic even, the controlled high-performance hydroxyapatite nano pole of size of cheap oleic acid-alcohol-water phase transfer system.Belong to the technical field that medical hydroxyapatite is made.
Background technology
Hydroxyapatite (hydroxyapatite, HA), molecular formula Ca
10(PO
4)
6(OH)
2, it is a kind of acicular crystal.Main inorganic composition at occurring in nature animal skeleton and tooth is exactly a hydroxyapatite.In sclerotin, hydroxyapatite accounts for 60% greatly.Hydroxyapatite has good biocompatibility, has a wide range of applications in fields such as the surface modification that comprises bone tissue engineering scaffold, implantation instrument, artificial tooth, medicament slow releases at present and has obtained good society and economic benefit.
The source of hydroxyapatite comprises extraction and two kinds of approach of synthetic of natural bone.The step of obtaining hydroxyapatite from natural bone comprises cleaning, high-temperature calcination and the mechanical activation comminution of skeleton.This method can obtain the hydroapatite particles that size is about hundreds of nanometers.Its composition of the hydroxyapatite that this method is obtained is similar to skeleton, and biocompatibility is better, and preparation cost is comparatively cheap.But the high-temperature calcination step that this method adopted is because the time is longer, and energy consumption is higher, and the multistage pulverizing in the mechanical activation comminution, complex steps, and will obtain the granule that size is about hundreds of nanometers and needed ball milling tens of hours, production efficiency is still waiting to improve.Therefore, this method does not also really enter application at present.
The artificial-synthetic hydroxyapatite is the present comparatively general preparation method of obtaining hydroxyapatite.People have developed multiple preparation methoies such as mechanochemical reaction, microwave solid phase synthesis, the sedimentation method, hydrothermal synthesis method, sol-gal process, reverse microemulsion process.Wherein all there are problems such as size inequality, granule are big, pattern is irregular in the prepared hydroxyapatite of most methods at aspects such as size, patterns.And these problems have produced problems such as comprising performance quality control difficulty, homodisperse difficulty for the application of hydroxyapatite.
Domestic Li Yadong research group proposed employing linoleic acid-ethanol-water system and utilizes liquid-solid-liquid phase metastasis successfully to prepare hydroxyapatite nano pole in 2004.Before the uniformity of its pattern, the Modulatory character of size have all surpassed various methodologies.But the linoleic acid cost is higher, and this has hindered the popularization of its application to a certain extent.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of preparation method that adopts the hydroxyapatite nano pole of oleic acid-alcohol-water phase transfer system, this method can make things convenient for and obtains the high-quality hydroxyapatite nano pole that size is even on nanoscale, pattern is controlled at an easy rate, therefore is expected to be widely used in medical domain.
Technical scheme: the present invention proposes to adopt the oleic acid of relative low price to substitute linoleic acid, promptly prepares hydroxyapatite nano pole by oleic acid-ethanol-water system.Not only size is even, pattern is controlled for hydroxyapatite nano pole by the preparation of this method, and price is comparatively cheap, for the medical hydroxyapatite material of high-quality obtain and promote provide new may.
The preparation method of hydroxyapatite nano pole of the present invention is characterized in that being prepared as follows:
A. at first oleic acid, ethanol and additive are mixed, wherein the volume content of oleic acid in final mixed solution is 5%-15%, and the volume content of ethanol in final mixed solution is 30%-60%;
B. secondly calcium saline solution is distributed in above-mentioned oleic acid-ethanol blending agent, the volume content of calcium saline solution in final mixed solution is 5%-15%, and the quality volumetric concentration of calcium salt is 0.1%-10%;
C. add the aqueous phosphatic mixed at room temperature then, the volume content of aqueous phosphatic in final mixed solution is 5%-15%, and phosphatic quality volumetric concentration is 0.1%-10%;
D. the mixture that step c is produced reacted 2-24 hour between 80-200 degree centigrade in reactor;
E. centrifugal removal supernatant also cleans after drying with cleaning solvent, obtains hydroxyapatite nano pole.
Additive among the step a is enuatrol or 18 ammonia.
Cleaning solvent is water, ethanol, ethyl acetate in the step e.
Beneficial effect: hydroxyapatite nano pole is subjected to showing great attention to of people owing to being worth in the medical domain extensive application.Yet obtain at present hydroxyapatite nano pole method or size, pattern is wayward or price comparison is expensive, thereby has influenced its application performance and range of application.
For this reason, the present invention proposes to adopt the high-quality hydroxyapatite nano pole that cheap oleic acid-preparation of alcohol-water phase transfer system is even in the nanoscale inside dimension, pattern is controlled, for the medical hydroxyapatite material of high-quality obtain and promote provide new may.
The specific embodiment
A. at first oleic acid, ethanol and additive are mixed, wherein the volume content of oleic acid in final mixed solution is 5%-15%, and the volume content of ethanol in final mixed solution is 30%-60%;
B. secondly calcium saline solution is distributed in above-mentioned oleic acid-ethanol blending agent, the volume content of calcium saline solution in final mixed solution is 5%-15%, and the quality volumetric concentration of calcium salt is 0.1%-10%;
C. add the aqueous phosphatic mixed at room temperature then, the volume content of aqueous phosphatic in final mixed solution is 5%-15%, and phosphatic quality volumetric concentration is 0.1%-10%;
D. the mixture that step c is produced reacted 2-24 hour between 80-200 degree centigrade in reactor;
E. centrifugal removal supernatant also cleans after drying with cleaning solvent, obtains hydroxyapatite nano pole.
Additive among the step a is enuatrol or 18 ammonia.
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1:
1 measures 16ml oleic acid respectively, and the 64ml dehydrated alcohol slowly adds the 6.4g enuatrol while stirring, makes its mix homogeneously;
2 take by weighing the 2g lime nitrate, are dissolved in the 30ml distilled water;
3 slowly pour calcium nitrate solution into enuatrol, and ethanol in the oleic mixed solution, and makes its mix homogeneously by magnetic stirring apparatus;
4 with above-mentioned solution stirring 30 minutes, made it finish ion exchange;
5 take by weighing the 2g sodium phosphate, are dissolved in the 30ml distilled water;
6 sodium radio-phosphate,P-32 solutions add to be finished in the solution of ion exchange, and stirs 5 minutes;
7 above-mentioned mixed liquors are poured reactor into, and reactor is placed Constant Temp. Oven, and it was reacted 8 hours under 90 ℃ condition;
8 take out product, and water, ethanol, ethyl acetate ultrasonic cleaning are centrifugal 3 times successively, and dry back products therefrom is the about 10nm of diameter, is about the 200nm hydroxyapatite nano pole.
Embodiment 2:
Reactor reaction temperature among the embodiment 1 is risen to 120 degrees centigrade, and the identical about 20nm of diameter that obtains of all the other conditions is about the hydroxyapatite nano pole of 100nm.
Claims (2)
1, a kind of preparation method of hydroxyapatite nano pole is characterized in that being prepared as follows:
A. at first oleic acid, ethanol and additive are mixed, wherein the volume content of oleic acid in final mixed solution is 5%-15%, and the volume content of ethanol in final mixed solution is 30%-60%;
B. secondly calcium saline solution is distributed in above-mentioned oleic acid-ethanol blending agent, the volume content of calcium saline solution in final mixed solution is 5%-15%, and the quality volumetric concentration of calcium salt is 0.1%-10%;
C. add the aqueous phosphatic mixed at room temperature then, the volume content of aqueous phosphatic in final mixed solution is 5%-15%, and phosphatic quality volumetric concentration is 0.1%-10%;
D. the mixture that step c is produced reacted 2-24 hour between 80-200 degree centigrade in reactor;
E. centrifugal removal supernatant also cleans after drying with cleaning solvent, obtains hydroxyapatite nano pole.
2, the preparation method of hydroxyapatite nano pole according to claim 1 is characterized in that the additive among the step a is enuatrol or 18 ammonia.
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| CNA2008101241917A CN101297978A (en) | 2008-06-17 | 2008-06-17 | Preparation method of hydroxyapatite nano pole |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491300A (en) * | 2011-11-16 | 2012-06-13 | 陕西巨子生物技术有限公司 | Preparation method of amphiphilic monodisperse hydroxyapatite monocrystal nanorod |
| RU2457174C1 (en) * | 2011-03-21 | 2012-07-27 | Учреждение Российской академии наук Институт химии Дальневосточного отделения РАН (ИХ ДВО РАН) | Method of producing nanosized hydroxyapatite powder |
| CN103626144A (en) * | 2013-12-13 | 2014-03-12 | 中国科学院上海硅酸盐研究所 | High temperature resistant non-combustible hydroxyapatite paper with high flexibility and preparation method thereof |
| CN103803489A (en) * | 2014-03-05 | 2014-05-21 | 中国科学院上海硅酸盐研究所 | Preparation method of large-size hydroxyl apatite microtube ordered array |
| CN105129756A (en) * | 2015-09-22 | 2015-12-09 | 西北大学 | Method for preparing sub-nanometer hydroxyapatite ultrafine-needles through low-temperature mineralization |
| CN105217593A (en) * | 2015-09-22 | 2016-01-06 | 西北大学 | The preparation method of the sub-nano wire of the ultra-fine hydroxyapatite of a kind of flexibility |
| CN106063947A (en) * | 2016-05-25 | 2016-11-02 | 西北大学 | The preparation method that a kind of selenium is nano hydroxylapatite doped |
| CN109573973A (en) * | 2018-12-21 | 2019-04-05 | 湖北工业大学 | A kind of method that two-step method prepares Oil soluble hydroxy apatite nanometer rods |
| CN109908405A (en) * | 2019-03-10 | 2019-06-21 | 西北大学 | A kind of porous bone renovating bracket material and preparation method thereof |
| CN110787323A (en) * | 2019-11-15 | 2020-02-14 | 山东大学 | HAp-CSA-SF composite gel material and preparation method and application thereof |
| CN111115600A (en) * | 2018-10-30 | 2020-05-08 | 天津工业大学 | Method for synthesizing hydroxyapatite concave-convex nano rod with assistance of ethyl acetate |
-
2008
- 2008-06-17 CN CNA2008101241917A patent/CN101297978A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2457174C1 (en) * | 2011-03-21 | 2012-07-27 | Учреждение Российской академии наук Институт химии Дальневосточного отделения РАН (ИХ ДВО РАН) | Method of producing nanosized hydroxyapatite powder |
| CN102491300A (en) * | 2011-11-16 | 2012-06-13 | 陕西巨子生物技术有限公司 | Preparation method of amphiphilic monodisperse hydroxyapatite monocrystal nanorod |
| CN102491300B (en) * | 2011-11-16 | 2014-09-03 | 陕西巨子生物技术有限公司 | Preparation method of amphiphilic monodisperse hydroxyapatite monocrystal nanorod |
| CN103626144A (en) * | 2013-12-13 | 2014-03-12 | 中国科学院上海硅酸盐研究所 | High temperature resistant non-combustible hydroxyapatite paper with high flexibility and preparation method thereof |
| WO2015085814A1 (en) * | 2013-12-13 | 2015-06-18 | Shanghai Institute Of Ceramics, Chinese Academy Of Sciences | Ultralong hydroxyapatite nanowire/microwire, method of preparing same, hydroxyapatite paper comprising same and preparation method thereof |
| CN103626144B (en) * | 2013-12-13 | 2015-07-15 | 中国科学院上海硅酸盐研究所 | High temperature resistant non-combustible hydroxyapatite paper with high flexibility and preparation method thereof |
| US9822488B2 (en) | 2013-12-13 | 2017-11-21 | Shanghai Institute Of Ceramics, Chinese Academy Of Sciences | Ultralong hydroxyapatite nanowire/microwire, method of preparing same, hydroxyapatite paper comprising same and preparation method thereof |
| CN103803489A (en) * | 2014-03-05 | 2014-05-21 | 中国科学院上海硅酸盐研究所 | Preparation method of large-size hydroxyl apatite microtube ordered array |
| CN105217593A (en) * | 2015-09-22 | 2016-01-06 | 西北大学 | The preparation method of the sub-nano wire of the ultra-fine hydroxyapatite of a kind of flexibility |
| CN105217593B (en) * | 2015-09-22 | 2017-07-28 | 西北大学 | A kind of preparation method of the sub- nano wire of flexible ultra-fine hydroxyapatite |
| CN105129756A (en) * | 2015-09-22 | 2015-12-09 | 西北大学 | Method for preparing sub-nanometer hydroxyapatite ultrafine-needles through low-temperature mineralization |
| CN106063947A (en) * | 2016-05-25 | 2016-11-02 | 西北大学 | The preparation method that a kind of selenium is nano hydroxylapatite doped |
| CN111115600A (en) * | 2018-10-30 | 2020-05-08 | 天津工业大学 | Method for synthesizing hydroxyapatite concave-convex nano rod with assistance of ethyl acetate |
| CN111115600B (en) * | 2018-10-30 | 2022-12-13 | 天津工业大学 | Method for synthesizing hydroxyapatite Dan Aotu nano-rod with assistance of ethyl acetate |
| CN109573973A (en) * | 2018-12-21 | 2019-04-05 | 湖北工业大学 | A kind of method that two-step method prepares Oil soluble hydroxy apatite nanometer rods |
| CN109908405A (en) * | 2019-03-10 | 2019-06-21 | 西北大学 | A kind of porous bone renovating bracket material and preparation method thereof |
| CN109908405B (en) * | 2019-03-10 | 2020-07-03 | 西北大学 | Porous bone repair scaffold material and preparation method thereof |
| CN110787323A (en) * | 2019-11-15 | 2020-02-14 | 山东大学 | HAp-CSA-SF composite gel material and preparation method and application thereof |
| CN110787323B (en) * | 2019-11-15 | 2020-11-24 | 山东大学 | HAp-CSA-SF composite gel material and preparation method and application thereof |
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Open date: 20081105 |