Method of obtaining nanosized hydroxylapatite

FIELD: chemistry.

SUBSTANCE: invention relates to technology of obtaining inorganic materials, namely to methods of obtaining nanosized highly pure hydroxylapatite (HAP) in form of colloid solution or gel, which can be used for production of medico-preventive preparations for stomatology, for application on bone implants. Method of obtaining nanosized colloid hydroxylapatite includes synthesis of hydroxylapatite in saturated solution of calcium hydroxide, decanted after 24-hour settling from sedimented aggregates Ca(OH)2, by adding at rate 1.5-2.2 ml/min per litre of alkali solution 10-20% solution of orthophosphoric acid with constant mixing until pH value of reaction mixture is not lower than 10.5±0.5. Mixture is mixed during 20-30 minutes, settled during 1-2 hours and decanted until liquid phase stops forming on the surface. Obtain product represents colloid solution of highly pure hydroxylapatite with concentration 1.5-2%. Increase of hydroxylapatite concentration within the range from 2 to 30% is carried out by evaporation at temperature not higher than 60°C, and for obtaining nanosized hydroxylapatite with concentration 40±2% initial colloid solution is subjected to complete freezing with further unfreezing at temperature not more than 60°C and liquid phase decanting.

EFFECT: obtaining stable product with set in advance concentration, possessing higher penetrating ability and biochemical activity.

3 cl, 4 ex

 

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

In modern dentistry and orthopedics hydroxylapatite calcium displaces metals and other traditionally used materials (J. Amplantol, 1987, 13, No. 1, s-127; Med. Progr. Technol. 1982, No. 9, 129-136), as it provides sufficient strength and porosity of ceramics and thus has no antigenic properties and does not cause microcentro inflammatory response due to the identity of the mineral part of bone and enamel.

Known for a large number of methods for producing hydroxyapatite, for example, patent RF №2100274 (publ. 1997.12.27), No. 2038293 (publ. 1995.06.27).

A disadvantage of known methods is that they do not set a goal of obtaining nanosized particles of hydroxyapatite and is aimed at solving the problem of obtaining the finished product with a high purity of the phase composition in powder form, so at the final stage require high temperatures.

The closest selected for the prototype, is the method according to the patent of Russian Federation №2104924 (publ. 20.02.1998), which involves mixing calcium hydroxide and phosphoric acid, from taiwania, filtration and drying of the finished product. The advantage of this method is that it allows you to get hydroxylapatite when the molar ratio of the starting components of 1.33:2,50, in a fairly wide range without complex hardware design. The yield of hydroxyapatite is 100%.

The disadvantage of this method is that it does not seek to obtain nanosized particles of hydroxyapatite and, in addition, requires a sufficiently high temperature for drying (over 100° (C) and annealing (over 1000°). The use of hydroxyapatite in the form of powder provides before applying mandatory dilution liquid base that makes it difficult to obtain the necessary concentration and uniformity, particularly when it comes to achieve a colloidal state. Modern requirements to the quality of coatings on bone implants include the need to increase their adhesive characteristics and osteoconductive properties.

Object of the present invention is to provide a method of producing high-purity nano-hydroxyapatite with particle size not more than 200 nm in length and not more than 40 nm in width in the form of ready-to-use product with a predetermined concentration in a colloidal solution or gel.

The technical result is to increase the Prony the surrounding abilities and biochemical activity of hydroxyapatite, which provides:

- in relation to dentistry - extended re-mineralizing effect on tooth tissue, an increase in the adhesion characteristics to the organic and inorganic components of dentin,

- in relation to Orthopaedics, surgery and traumatology - the possibility of increasing the adhesion characteristics and osteoconductive properties of bioactive coatings on bone implants.

An additional effect is the possibility of getting the finished product with a predetermined concentration, which provides convenience when using it.

The problem is solved due to the fact that for the synthesis of hydroxyapatite, comprising mixing calcium hydroxide and phosphoric acid at room temperature, sedimentation, filtration and drying of the finished product, unlike the prototype used a saturated solution of calcium hydroxide obtained by decanting the aqueous solution from the precipitated aggregates of CA(Oh)2after the daily advocate, which is poured with stirring at a rate of 1.5-2.2 ml/min per liter of the alkaline solution of 10-20%solution of orthophosphoric acid, continue stirring for 20-30 minutes, then assert within 1-2 hours and decanted, repeated settling and decantation until, while on the surface will not cease to form the liquid phase. In poluchaut,5-2% colloidal solution of high purity hydroxyapatite with particle size not more than 200 nm in length and not more than 40 nm in width. To increase the concentration of a colloidal solution of nanosized hydroxyapatite in the range from 1.5-2% to 30% are dried by evaporation at a temperature not above 60°C. And to obtain nanosized hydroxyapatite with a concentration of 40±2%, the resulting colloidal solution of high-purity nano-sized hydroxyapatite concentration of 1.5-2% is subjected to a complete freezing with subsequent thawing at a temperature of not more than 60°separating precipitated precipitated gel-like agglomerates of high-purity nano-sized hydroxyapatite from the liquid phase by decantation.

Distinctive signs, confirming the novelty and inventive step of the claimed method:

- synthesis of hydroxyapatite is carried out in a saturated solution of calcium hydroxide, obtained by decanting from the settled aggregates of calcium hydroxide day, after settling at room temperature. This technical solution allows for the synthesis of hydroxyapatite in ion-molecular solution of calcium hydroxide, which does not contain certain components that results in the receipt of hydroxyapatite particles not larger than 200 nm in length and not more than 40 nm in width;

- with constant stirring poured 10-20%solution of phosphoric acid at a rate of 1.5-2.2 ml/min per liter of alkaline rest the RA to achieve pH=10,5± 0.5 and continue stirring for 20-30 minutes. It must comply with the condition: the higher the concentration of the acid, the lower the speed prilipanie and Vice versa. The fulfillment of these conditions (the dependence of the rate of prilipanie from acid concentration and volume of a saturated solution of calcium hydroxide) allows to synthesize nano-sized particles of hydroxyapatite evenly in full of the reaction mixture and gently bring the pH to 10.5±0,5, but not below, in order to avoid the formation of other CA-P compounds;

after one two-hour settling decanted clarified upper layer by repeating the procedure of settling and decanting, until the termination of the appearance on the surface of the liquid phase, which allows to obtain a colloidal solution of nanosized hydroxyapatite with a concentration of 1.5-2%;

- an increase in the concentration of a colloidal solution of hydroxyapatite in the range of 2 to 30% is carried out by evaporation at a temperature not more than 60°C. This solution allows you to stop the drying process at the time the required concentration of the finished product in the form of a colloidal solution or gel. An additional advantage is energy saving, as it does not require the use of high temperatures at the time of receipt of hydroxyapatite in the form of powder, as well as the usability of the finished item is of oducti with known concentration. Increasing the concentration above 30% by evaporation is undesirable - this leads to the formation on the surface of the gel hydroxyapatite solid agglomerates. The temperature of evaporation below 40°extend the process of evaporation, and above it there is the threat of crystallization of hydroxyapatite;

- to obtain nanosized hydroxyapatite with a concentration of 40±2% of the formed colloidal solution of hydroxyapatite concentration of 1.5-2% is subjected to a complete freezing with subsequent thawing at a temperature of not more than 60°With, in the hydroxylapatite receive in the form of precipitated in the sediment of large gel-like agglomerates, which are separated from the liquid phase by decantation. The obtained gel-like agglomerates having the property of plasticity, consist of nano-sized particles of high purity hydroxyapatite.

The particles of the dispersed phase in a colloidal system at a concentration of 1.5-2% of hydroxyapatite evenly fill the entire volume of the dispersion medium, and the system is sedimentation-resistant. In the evaporation process when reaching 8-30% concentration or freeze with obtaining a concentration of 40±2% structuring of colloidal solution, and it transforms into a gel. The use of the proposed method are nanoscale hydroxylapatite with the size of the piece is the length of 100-200 nm, width of 30-40 nm in the form of a colloidal solution or gel with a predetermined concentration of preserving without changing its properties for at least 3 months. The use of the finished product with a predetermined concentration increases ease of use.

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 Ca(OH)2you can fill with distilled water for reuse.

To the obtained after decanting the saturated alkaline solution of calcium hydroxide in the amount of 1 liter slowly with constant stirring and a temperature of 20-25°poured With 10%solution of orthophosphoric acid with a speed of 2.2 ml/min, continuously monitoring the pH using a pH meter, to achieve in the reaction mixture a pH above 10.5±0.5 in. The result is often a colloidal solution of hydroxyapatite with particle sizes along the length of 100-200 nm, width of 30-40 nm.

The solution is stirred for 20-30 minutes and allow to settle for 1-2 hours a colloidal solution of hydroxyapatite deposited and is about 1/3 of the volume, the mixture is decanted by draining the clarified upper layer. The procedure of settling and decantation, 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 with particle sizes along the length of 100-200 nm, width of 30-40 nm.

Example 2.

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 in the amount of 1 liter slowly with constant stirring and a temperature of 20-25°poured With a 20%solution of orthophosphoric acid with a speed of 1.5 ml/min, continuously monitoring the pH using a pH meter, to achieve in the reaction mixture a pH above 10.5±0.5 in. The result is often a colloidal solution of hydroxyapatite with particle sizes along the length of 100-200 nm, width of 30-40 nm.

The solution is stirred for 20-30 minute 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. The procedure of settling and decantation, 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 with particle sizes along the length of 100-200 nm, width of 30-40 nm.

Example 3.

A colloidal solution of high purity hydroxyapatite obtained in example 1 or example 2 is subjected to drying by evaporation at a temperature not more than 60°to increase the concentration of the hydroxyapatite is in the range from 1.5-2% to 30%. Maintaining control over the changes in the concentration and stop the evaporation process in the moment of reaching the required concentration of hydroxyapatite. The result is high-purity nano-hydroxylapatite in the form of a colloidal solution or gel with a predetermined concentration in the range from 1.5-2% to 30%.

Example 4.

A colloidal solution of high purity hydroxyapatite obtained in example 1 or example 2 is subjected to a complete freeze in the freezer. Defrost at a temperature not above 60°C. In the hydroxylapatite precipitate large gel agglomerates of particles retained the nano (the length of 100-200 nm, width of 30-40 nm), hold the decantation of the liquid phase. Cryoablate allows you to increase the concentration of the finished product up to 40±2%.

Thus, the authors propose a simple and reliable method of obtaining high-purity nano-hydroxyapatite with particle size of hydroxyapatite on the length of 100-200 nm, width of 30-40 nm in the form of ready-to-use colloidal or gel-like product with a predetermined concentration.

1. Method of producing nanoscale hydroxyapatite, comprising the synthesis of hydroxyapatite in a saturated solution of calcium hydroxide, dekotirovaniem day, after settling from the settled units of 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; continue stirring for 20-30 minutes, then assert within 1-2 h and decanted, repeated settling and decantation until, while on the surface will not cease to form the liquid phase.

2. Method of producing nanoscale hydroxyapatite, comprising the synthesis of hydroxyapatite in a saturated solution of calcium hydroxide, dekotirovaniem day, after settling from the settled units of CA(Oh)2by prilipanie with a speed of 1.5-2.2 ml/min on the ITR alkaline solution of 10-20% solution of orthophosphoric acid with constant stirring, before reaching the pH value of the reaction mixture above 10.5±0,5; continue stirring for 20-30 minutes, then assert within 1-2 h and decanted, repeated settling and decantation until, while on the surface will not cease to form a liquid phase, conduct drying the formed colloidal solution of hydroxyapatite concentration of 1.5-2% by evaporation at a temperature not above 60°C.

3. Method of producing nanoscale hydroxyapatite, comprising the synthesis of hydroxyapatite in a saturated solution of calcium hydroxide, dekotirovaniem day, after settling from the settled units of 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; continue stirring for 20-30 minutes, then assert within 1-2 h and decanted, repeated settling and decantation until, while on the surface will not cease to form a liquid phase, the obtained colloidal solution of hydroxyapatite concentration of 1.5-2% is subjected to cryoablate, including full freezing with subsequent thawing at a temperature of not more than 60°, hold the decantation of the liquid phase.



 

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