Method of obtaining nano-sized hydroxylapatite

FIELD: chemistry.

SUBSTANCE: nano-sized highly-pure hydroxylapatite (HAP) is obtained in form of alcohol colloid solution (gel), which can be used for production of medicinal preventive preparations in stomatology, for applying bioactive coating on bone implants. Method includes hydroxylapatite synthesis by adding solution of orthophosphoric acid to calcium hydroxide solution and exposure to ultrasound impact, and ethyl or isopropyl alcohol is added to colloid of highly-pure nano-sized hydroxylapatite with concentration from 5% to 40±2% in order to obtain concentration of hydrooxylapatite in alcohol from 0.2 to 20%. After that alcohol mixture is processed with ultrasound with frequency 10-50 kHz during 1-2 hours.

EFFECT: alcohol colloid of nano-sized hydroxylapatite with high stability.

2 cl, 3 ex

 

The invention relates to the technology of inorganic materials, namely the method of production of high-purity nano-hydroxyapatite (HAP) in the alcohol colloid (gel), which can be used for the production of medical materials, stimulating regeneration of bone defects, including dentistry.

A method of obtaining a suspension of hydroxyapatite by the RF patent №2122520, publ. 1998.11.27, which includes the interaction of calcium hydroxide with phosphoric acid in a closed circuit during serial passage of a suspension of calcium hydroxide through two zones with a continuous flow in the first zone of phosphoric acid in an amount necessary to achieve pH=10-11, the speed of flow of the suspension of 0.8-1.5 m/s, extract it from 1.0 to 1.5, dilution of the mixture in the second zone with a suspension of calcium hydroxide in 400-500 times, return the mixture in the first zone with multiplicity circulation 4-5 times during 10-20 min, followed by additional stirring of the mixture for 10-12 min after cessation acid and output the finished product. When this is received after additional stirring, the suspension is served in a phased treatment with sequential alternating stages of mixing and filtering.

The method allows to obtain homogeneous with Shiro is their range of concentration of a suspension of particles of hydroxyapatite, and paste hydroxyapatite, a uniform concentration composition.

The disadvantage of this method is its multi-stage, the complexity of hardware design, high intensity obtaining a slurry (paste) of hydroxyapatite.

The known method according to the patent of Russian Federation №2165389 (published 2001.04.20), including the synthesis of calcium phosphate, the processing of alcohol in a volume ratio solution of calcium phosphate:alcohol of 1:0.001 to 1, mixing it with an alcoholic alkali solution having the volumetric ratio of the aqueous alkali solution:alcohol of 1:0.001 to 1, to a pH of 10-12, separation, washing and drying the precipitate of the product at a temperature of not more than 60°C. In this way when used as a reaction mixture of water-alcohol solutions of calcium phosphate and alkali possible to obtain fine powders hydroxyapatite with particle size up to 0.3 to 1.0 μm. The introduction of alcohol in the reaction medium in this way is intended to prevent agglomeration of the particles, which allows to obtain fine hydroxylapatite with a particle size of 0.3 to 1 μm.

The disadvantage of this method lies in the fact that his task is to get the powder, not the spirit of a colloidal solution of nanosized hydroxyapatite.

The closest is a method of obtaining a suspension of hydroxyapatite by the RF patent №2149827, zakluchalsya, the production of fine hydroxyapatite is in the form of suspension is carried out by prilipanie 6-9%aqueous solution of phosphoric acid with at 70-120 ml/min to 20-55%suspension of calcium hydroxide pretreated with ultrasound with frequency 9-15 kHz within 1-2 hours. The formation of hydroxyapatite particles with a size of 1-5 μm occurs in the sump for 20-24 hours, the Concentration of hydroxyapatite in the finished suspension 320-350 g/L. the Disadvantage of this technical solution is that the size of hydroxyapatite particles in the suspension are 1-5 microns, i.e. they cannot be attributed to the nanoscale.

A common drawback of all these methods is that they do not provide the possibility of obtaining the finished alcohol colloid (gel) nanosized hydroxyapatite desired concentration with resistance to one year. And cooking alcohol colloidal solution (gel) of the suspension or powder of hydroxyapatite even with a particle size similar to that of the nano, on the job almost impossible.

The objective of the invention is to provide a method of obtaining alcohol colloid (gel) nanosized hydroxyapatite with a predetermined concentration for use in dentistry, and for applying a bioactive coating method, a Sol-gel.

Task ResetSystem way.

In the method, including synthesis of fine hydroxyapatite by prilipanie 6-9%aqueous solution of phosphoric acid with at 70-120 ml/min to 20-55%suspension of calcium hydroxide pretreated with ultrasound with frequency 9-15 kHz within 1-2 hours, with the following changes:

- synthesis of hydroxyapatite are not in suspension, and in a saturated solution of calcium hydroxide, which is prepared by mixing calcium oxide with water 10-20 g/l, sedimentation within days at a temperature of 20-25°and decanting from the precipitate of calcium hydroxide;

- received saturated solution of calcium hydroxide is poured 10-20%solution of orthophosphoric acid with a speed of 1.5-2.2 ml/min per one liter of the alkaline solution at a temperature of 20-25°until the pH of the reaction mixture to 10.5±0,5;

- produce stirring at room temperature (20-25° (C) for 20-30 minutes, then the resulting solution was defend and decanted by draining the clarified upper layer, repeating these procedures until such time as no longer to form a clarified upper layer. The result is a 1.5-2% colloidal solution of high-purity nano-sized hydroxyapatite particles which have a polycrystalline structure and consist of elongated crystallites with a size of 10-20 nm, oriented in a certain way and westray emyh in chains, including parallel and agglomerated whose dimensions do not exceed 200 nm in length and 40 nm in width;

- increasing the concentration of a colloidal solution of high-purity nano-sized hydroxyapatite is in the range from 1.5-2% up to 5-30% is carried out by evaporation at a temperature not above 60°C;

- increasing the concentration of high-purity nano-sized hydroxyapatite from 1.5-2 to 40±2% is administered by cryoablate: a colloidal solution with a concentration of hydroxyapatite 1,5-2% completely frozen in the freezer, then thawed at a temperature not above 60°and separating the liquid phase from the resulting precipitate in gel form large agglomerates;

- mix obtained 5-40%concentrate of high purity nano-sized hydroxyapatite with ethyl or isopropyl alcohol to obtain the concentration of hydroxyapatite in alcohol from 0.2% to 20%.

- processes the received alcohol colloid of high-purity nano-sized hydroxyapatite ultrasound frequency 10-50 kHz within 1-2 hours until complete homogenization.

Novelty and inventive step of the proposed technical solutions confirm the following characteristics:

- synthesis of hydroxyapatite are in a saturated solution of calcium hydroxide, which is prepared by mixing calcium oxide with water 10-20 g/l, sedimentation during the day ol the temperature 20-25° With and decanting from the precipitate of calcium hydroxide, poured 10-20%solution of orthophosphoric acid with a speed of 1.5-2.2 ml/min per one liter of the alkaline solution at a temperature of 20-25°until the pH of the reaction mixture to 10.5±0.5, and stirred at room temperature (20-25° (C) for 20-30 minutes, then the resulting solution was defend and decanted by draining the clarified upper layer, repeating these procedures until such time as no longer to form a clarified upper layer, and increase the concentration obtained 1,5-2% the colloidal solution of high-purity nano-sized hydroxyapatite up to 5-30% by evaporation, up to 40±2% by cryoablate;

- colloidal solution of high-purity nano-sized hydroxyapatite concentration from 5% to 40±2% mixed with ethyl or isopropyl alcohol, obtaining a concentration of hydroxyapatite in alcohol from 0.2 to 20%;

- obtained alcohol mixture containing 0.2-20% high-purity nano-sized hydroxyapatite, treated with ultrasound frequency 10-50 kHz within 1-2 hours until complete homogenization that allows you to split formed in the process of evaporation agglomerates and get a fully homogenized alcohol colloid (gel) nanosized hydroxyapatite.

As a result, the proposed method allows to obtain stable in BP is like alcohol colloid (gel) high-purity nano-sized hydroxyapatite dosing initial components in a fairly wide range without complex hardware design. Particles of hydroxyapatite synthesized by this method have a polycrystalline structure and consist of elongated crystallites with a size of 10-20 nm, oriented in a certain way and build in the chain, including parallel and agglomerated, which length does not exceed 100-200 nm, width of 30-40 nm.

The proposed method is as follows

Example 1.

Prepare a saturated solution of calcium hydroxide CA(Oh)2thoroughly mix and stand for 1 day at t(solution)=20-25°and pH(solution)=12.50±0,2.

The obtained alkaline solution decanted by draining the clarified upper layer. Saturated alkaline solution should be transparent and without aggregates of CA(Oh)2. The precipitate of CA(Oh)2you can fill with distilled water for reuse.

To the obtained after decanting the saturated alkaline solution of calcium hydroxide slowly with constant stirring and a temperature of 20-25°poured With 10-20%solution of orthophosphoric acid with a speed of 1.5-2.2 ml/min per 1 liter of the alkaline solution, controlling the pH using a pH meter, to achieve in the reaction mixture a pH above 10.5±0.5 in. The result is a colloidal solution of hydroxyapatite with particle sizes in the length of no more than 100-200 nm, width of 30-40 nm.

R is the target stirred for 20-30 minutes and allow to settle, 1-2 hours a colloidal solution of hydroxyapatite deposited and is 1/3 of the total volume of the mixture is decanted by draining the clarified upper layer. Procedures for settling and decanting, repeat until, while on the surface will not cease to form the liquid phase.

The resulting product is a 1.5 to 2% colloidal solution of high purity hydroxyapatite in the form of elongated crystallites with a size of 10-20 nm, oriented in a certain way and build in the chain, including parallel and agglomerated whose dimensions do not exceed 200 nm in length and 40 nm in width. Then a colloidal solution of hydroxyapatite is evaporated at a temperature not more than 60°to increase the concentration of hydroxyapatite at least 5%but not more than 30%. Poured ethyl or isopropyl alcohol to obtain the concentration of hydroxyapatite in an alcohol solution from 0.2 to 1% and treated with ultrasound frequency 10-50 kHz within 1-2 hours until complete homogenization alcohol solution of hydroxyapatite. Get sedimentation-resistant 0,2-1% alcohol colloid of hydroxyapatite, which can be used for applying a bioactive coating method, a Sol-gel. The stability of such a colloid is maintained for at least six months.

Example 2.

Spend the synthesis of hydroxyapatite in example 1 and Then to increase the concentration of a colloidal solution of nanosized hydroxyapatite in the range from 1.5-2 to 10-30% spend evaporation at a temperature not above 60° C.

The obtained nano-hydroxylapatite with a concentration of from 10 to 30% diluted with ethyl or isopropyl alcohol to obtain 5-20% concentration of hydroxyapatite in an alcohol solution and treated with ultrasound frequency 10-50 kHz within 1-2 hours until complete homogenization alcohol solution of hydroxyapatite.

Example 3.

Spend the synthesis of hydroxyapatite in example 1. Then spend cribrarula colloidal solution of nanosized hydroxyapatite to increase the concentration up to 40±2%. A colloidal solution of hydroxyapatite completely frozen in the freezer. Defrost at a temperature not above 60°C, decanted liquid phase from hydroxyapatite is deposited in the sediment in the gel form large agglomerates;

Then agglomerates of hydroxyapatite diluted with ethyl or isopropyl alcohol to 5-20% concentration of hydroxyapatite in alcohol and treated with ultrasound frequency 10-50 kHz to complete homogenization of the mixture at least 2 hours.

Obtained according to example 2 and 3 alcoholic gel hydroxyapatite is resistant for at least one year and can be used as the basis for the treatment and prevention of paints and pastes in dentistry.

Thus, the authors propose a simple and reliable method of obtaining nanosized hydroxyapatite in the form of alcohol stake is oida (gel), which allows to obtain the target product with a predetermined concentration (in a rather wide interval) without complex hardware design. Synthesis of hydroxyapatite this method allows to obtain hydroxylapatite in the form of elongated crystallites with a size of 10-20 nm, oriented in a certain way and build in the chain, including parallel and agglomerated whose dimensions do not exceed 200 nm in length and 40 nm in width, this form of crystals contributes to the formation of stable coagulation structures.

1. The method of obtaining alcohol colloid (gel) nanosized hydroxyapatite, comprising the synthesis of hydroxyapatite by prilipanie to a solution of calcium hydroxide solution of orthophosphoric acid, the effect of ultrasound within 1-2 h, characterized in that the colloid nano-sized hydroxyapatite concentration of 5-40±2% add ethyl or isopropyl alcohol to a concentration of hydroxyapatite in an alcohol solution from 0.2 to 20%, and the exposure to produce ultrasound with a frequency of 10-50 kHz after the addition of alcohol.

2. The method of obtaining alcohol colloid (gel) nanosized hydroxyapatite according to claim 1, characterized in that the synthesis of hydroxyapatite are in a saturated solution of calcium hydroxide, dekotirovaniem day, after settling from the settled unit is in Ca(OH) 2by prilipanie with a speed of 1.5-2.2 ml/min per liter of the alkaline solution of 10-20%solution of orthophosphoric acid with constant stirring until the pH of the reaction mixture above 10.5±0,5; stirred for 20-30 min, defend within 1-2 h and decanted clarified upper layer; the concentration of the formed colloidal solution of hydroxyapatite increase from 1.5 to 2 to 5 to 30% by evaporation at a temperature not above 60°or from 1.5-2 to 40±2% by TrioBrake, including full freezing with subsequent thawing at a temperature of not more than 60°and decanting the liquid phase.



 

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