CN1267340C - Supersonic wave evoked bovine serum albumin mold plate method for preparing bar-shaped hydroxyapatite - Google Patents
Supersonic wave evoked bovine serum albumin mold plate method for preparing bar-shaped hydroxyapatite Download PDFInfo
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- CN1267340C CN1267340C CN 200510018105 CN200510018105A CN1267340C CN 1267340 C CN1267340 C CN 1267340C CN 200510018105 CN200510018105 CN 200510018105 CN 200510018105 A CN200510018105 A CN 200510018105A CN 1267340 C CN1267340 C CN 1267340C
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Abstract
The present invention relates to a supersonic wave induced bovine serum albumin template method for preparing bar-shaped hydroxyapatite. The hydroxyapatite power body is ahexagonal prism in the shape of a long bar or a bundle in the shape of a long bar, the diameter is from 0.5 mu m to 1 mu m, and the length is from 3 mu m to 6 mu m. The method of combining a supersonic wave inducing method with a bovine albumin template method is used for preparing a precursor, and a freeze-drying method is used for drying the precursor. The dried precursor is roasted for 1 hour at the temperature of 700 DEG C. to obtain the bar-shaped hydroxyapatite of the present invention. The bar-shaped hydroxyapatite crystal power body of the present invention can be used for preparing biological ceramics, material surface coatings and composite materials.
Description
Technical field
The present invention relates to the supersonic wave evoked bovine serum albumin mold plate method for preparing bar-shaped hydroxyapatite.
Background technology
Hydroxyapatite is an inorganic components main in the human body bone, has excellent biological compatibility, has been widely used in the damaged reparation of bone.At present, the type of hydroxyapatite application mainly contains block ceramic, particle, coating, matrix material.The preparation method mainly contains solid phase method, the precipitator method, hydrothermal method, mechanochemical reaction, sonochemistry method, sol-gel method.For the preparation of hydroxyapatite inorganic-organic composite material, the character of hydroxyapatite is an important parameters, such as size, and shape.In order to make hydroxyapatite reach toughness reinforcing purpose, need the preparation rhabdolith.The biological macromolecular template method is a kind of method that can prepare different shape of newly-developed, thereby can provide a kind of simple valid approach for preparation bar-shaped hydroxyapatite crystal.
Summary of the invention
The purpose of this invention is to provide a kind of bar-shaped hydroxyapatite crystal powder.
Another object of the present invention provides a kind of bar-shaped hydroxyapatite crystalline preparation method.
The hydroxy apatite powder of realizing goal of the invention is long bar-shaped six side's prisms or long bar-shaped brilliant bundle, and diameter is 0.5 μ m~1 μ m, and length is 3 μ m~6 μ m.
The preparation method of bar-shaped hydroxyapatite crystal powder of the present invention is, the method that adopts ultrasonic wave revulsion and bovine serum albumin mold plate method to combine prepares presoma, and adopting the dry presoma of freeze-drying, dried presoma made 700 ℃ of roastings in 1 hour.
The concrete grammar step is:
1st, biphosphate calcium solution and calcium hydroxide saturated solution are mixed (as with concentration being biphosphate calcium solution and the mixing in 1.2: 1 by volume of calcium hydroxide saturated solution of 8.97mmol/L) by the stoichiometric ratio that generates hydroxyapatite, under stirring fast, add bovine serum albumin, make wherein that bovine serum albumin concentration is 2-5g/L, mixing solutions;
2nd, the mixing solutions ultrasonic emulsification that step 1 is obtained was handled 2-8 minute, obtained the hydroxyapatite presoma;
3rd, the hydroxyapatite presoma that step 2 is obtained places cryogenic refrigerator freezing, treat into ice after, under vacuum condition, carry out lyophilize, obtain exsiccant hydroxyapatite precursor powder;
4th, the exsiccant hydroxyapatite precursor powder that step 3 is obtained places 700 ℃ of stove calcinings 1 hour, promptly obtains the bar-shaped hydroxyapatite crystal powder.
Bar-shaped hydroxyapatite crystal powder of the present invention can be applied to prepare biological ceramics, preparation material surface coating and preparation matrix material.
It is the principle of utilizing ultrasonic cavitation that ultrasonic wave is induced, provide a high temperature in short period of time at the utmost point, highly compressed chemical reaction environment, make protein molecule generation crosslinking reaction, form a kind of tridimensional network, calcium phosphate precipitation is dissolved again, be deposited on again on the protein molecule, form a kind of mixture of protein-calcium phosphate.
Bovine serum albumin is for calcium phosphate precipitation provides template, and calcium phosphate precipitation is aligned.The formation of control bar-shaped hydroxyapatite in roasting process simultaneously.
Freeze-drying is in order to keep the structure of this protein-calcium phosphate complex, under vacuum condition, to make water sublimate, making its drying.
700 ℃ of roastings are to remove protein template, and make the calcium phosphate precipitation crystallization and form hydroxyapatite crystal.
Bar-shaped hydroxyapatite of the present invention, its manufacture method is simple and easy to control, safety non-pollution, starting material are easy to get.
Description of drawings
Fig. 1-the 4th, the microscopic appearance figure of the bar-shaped hydroxyapatite of embodiment 1-4 preparation,
As can be seen from Figure, the diameter of rhabdolith is the 0.3-1 micron, and length is the 3-8 micron.
Embodiment
Provide embodiment below and accompanying drawing is specifically narrated the present invention.
Compound concentration is the biphosphate calcium solution of 8.97mmol/L, is A solution; Preparation calcium hydroxide saturated solution is B solution.A and B solution were mixed in 1.2: 1 by volume, stir fast, add bovine serum albumin then, making its concentration is 2g/L.Carry out supersound process with ultrasonic emulsification instrument then, the time is 2-8 minute.Be placed on then in the cryogenic refrigerator freezing, treat into ice after, carry out lyophilize.At last the dry precursor powder is placed 700 ℃ silicon molybdenum stove to calcine 1 hour, promptly obtain bar-shaped hydroxyapatite.Detecting through X ray is hydroxyapatite.Crystal morphology and size are shown in Fig. 1 scanning electron microscope.
Embodiment 2
Compound concentration is the biphosphate calcium solution of 8.97mmol/L, square A solution; Preparation calcium hydroxide saturated solution is B solution.A and B solution were mixed in 1.2: 1 by volume, stir fast, add bovine serum albumin then, making its concentration is 3g/L.Carry out supersound process with ultrasonic emulsification instrument then, the time is 2-8 minute.Be placed on then in the cryogenic refrigerator freezing, treat into ice after, carry out lyophilize.At last the dry precursor powder is placed 700 ℃ silicon molybdenum stove to calcine 1 hour, promptly obtain bar-shaped hydroxyapatite.Detecting through X ray is hydroxyapatite.Crystal morphology and size are shown in Fig. 2 scanning electron microscope.
Embodiment 3
Compound concentration is the biphosphate calcium solution of 8.97mmol/L, is A solution; Preparation calcium hydroxide saturated solution is B solution.A and B solution were mixed in 1.2: 1 by volume, stir fast, add bovine serum albumin then, making its concentration is 4g/L.Carry out supersound process with ultrasonic emulsification instrument then, the time is 2-8 minute.Be placed on then in the cryogenic refrigerator freezing, treat into ice after, carry out lyophilize.At last the dry precursor powder is placed 700 ℃ silicon molybdenum stove to calcine 1 hour, promptly obtain bar-shaped hydroxyapatite.Detecting through X ray is hydroxyapatite.Crystal morphology and size are shown in Fig. 3 scanning electron microscope.
Embodiment 4
Compound concentration is the biphosphate calcium solution of 8.97mmol/L, is A solution; Preparation calcium hydroxide saturated solution is B solution.A and B solution were mixed in 1.2: 1 by volume, stir fast, add bovine serum albumin then, making its concentration is 5g/L.Carry out supersound process with ultrasonic emulsification instrument then, the time is 2-8 minute.Be placed on then in the cryogenic refrigerator freezing, treat into ice after, carry out lyophilize.At last the dry precursor powder is placed 700 ℃ silicon molybdenum stove to calcine 1 hour, promptly obtain bar-shaped hydroxyapatite.Detecting through X ray is hydroxyapatite.Crystal morphology and size are shown in Fig. 4 scanning electron microscope.
Claims (5)
1, a kind of hydroxy apatite powder is characterized in that this powder is long bar-shaped six side's prisms or long bar-shaped brilliant bundle, and diameter is 0.5 μ m~1 μ m, and length is 3 μ m~6 μ m.
2, a kind of method for preparing the described hydroxy apatite powder of claim 1 is characterized in that method steps is:
1st, biphosphate calcium solution and calcium hydroxide saturated solution are mixed by the stoichiometric ratio that generates hydroxyapatite, under stirring fast, add bovine serum albumin, make wherein that bovine serum albumin concentration is 2-5g/L, mixing solutions;
The 2.th mixing solutions ultrasonic emulsification that step 1 is obtained was handled 2-8 minute, obtained the hydroxyapatite presoma;
3rd, the hydroxyapatite presoma that step 2 is obtained places cryogenic refrigerator freezing, treat into ice after, under vacuum condition, carry out lyophilize, obtain exsiccant hydroxyapatite precursor powder;
4th, the exsiccant hydroxyapatite precursor powder that step 3 is obtained places 700 ℃ of stove calcinings 1 hour, promptly obtains the bar-shaped hydroxyapatite crystal powder.
3, the application of the described hydroxy apatite powder of claim 1 in the preparation biological ceramics.
4, the application of the described hydroxy apatite powder of claim 1 in preparation material surface coating.
5, the application of the described hydroxy apatite powder of claim 1 in the preparation matrix material.
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Cited By (2)
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US11634257B2 (en) | 2017-10-09 | 2023-04-25 | Terumo Bct Biotechnologies, Llc | Lyophilization container and method of using same |
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CN100341776C (en) * | 2006-02-22 | 2007-10-10 | 福建师范大学 | Method for prenaring spherical hydroxy-apatite nano crystal |
CN103601166B (en) * | 2013-11-11 | 2015-07-29 | 陕西科技大学 | Growth nano bar-shape hydroxyapatite on a glass substrate and preparation method thereof |
CN103588186A (en) * | 2013-11-14 | 2014-02-19 | 安徽淮化股份有限公司 | Preparation method of nano-hydroxyapatite |
CN104211037B (en) * | 2014-08-07 | 2016-06-01 | 华中农业大学 | Phosvitin and polypeptide thereof is utilized to catalyze and synthesize the method for biomimetic material hydroxyapatite |
CN107265426B (en) * | 2016-04-07 | 2019-12-10 | 武汉亚洲生物材料有限公司 | template-mediated synthesis of silicon-containing hydroxyapatite material and preparation method thereof |
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Cited By (8)
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US11634257B2 (en) | 2017-10-09 | 2023-04-25 | Terumo Bct Biotechnologies, Llc | Lyophilization container and method of using same |
US11604026B2 (en) | 2019-03-14 | 2023-03-14 | Terumo Bct Biotechnologies, Llc | Lyophilization loading tray assembly and system |
US11609043B2 (en) | 2019-03-14 | 2023-03-21 | Terumo Bct Biotechnologies, Llc | Lyophilization container fill fixture, system and method of use |
US11609042B2 (en) | 2019-03-14 | 2023-03-21 | Terumo Bct Biotechnologies, Llc | Multi-part lyophilization container and method of use |
US11740019B2 (en) | 2019-03-14 | 2023-08-29 | Terumo Bct Biotechnologies, Llc | Lyophilization loading tray assembly and system |
US11747082B2 (en) | 2019-03-14 | 2023-09-05 | Terumo Bct Biotechnologies, Llc | Multi-part lyophilization container and method of use |
US11815311B2 (en) | 2019-03-14 | 2023-11-14 | Terumo Bct Biotechnologies, Llc | Lyophilization container fill fixture, system and method of use |
US11994343B2 (en) | 2019-03-14 | 2024-05-28 | Terumo Bct Biotechnologies, Llc | Multi-part lyophilization container and method of use |
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