Method of making calcium-phosphate glass fibre materials

FIELD: process engineering.

SUBSTANCE: invention relates to medicine. Proposed method can be used in stomatology and orthopedics for production of medical materials stimulating recovery of bone tissue defects, for making dental stopping and dental pastes. It comprises preparation of mix containing compounds of calcium, phosphorus, silicon and sodium, impregnation of bioinertial incombustible porous matrix with made mix, matrix is composed of ceramics from aluminium or zirconium oxides followed by calcination. Note here that silicon compound represents tetraethoxysilane. Note also that phosphoric acid ether is used as phosphorus compound. Calcium and sodium compounds are represented by their carboxylates in polar organic solvent. This method includes making the thin layers on more strong bioinertial porous ceramics. Note also that said process involves no special complicated equipment and expensive reagents.

EFFECT: production of glass ceramics directly from solution omitting sol preparation stage, simplified and accelerated process.

7 cl, 5 ex

 

The invention relates to medical equipment, in particular the production of biocompatible implants based on calcium phosphates, and can be used in medicine, namely in dentistry and orthopedics.

Among materials for bone implants, special place is occupied bistecca, which currently are used in orthopaedic, dental and maxillofacial surgery. However, the possibility of direct implantation of the design, made from bioactive ceramic material for the reconstruction of the body with the damaged bone tissue is very limited. The reason is the low mechanical strength, including fatigue, and fracture toughness bioceramics, biotical and bioglass ceramics, which essentially, is 10-100 times lower than that of natural bone tissue.

In contrast to the calcium-phosphate ceramics are much more durable is porous ceramics made of aluminum oxide or zirconium. At the same time, this bioinert ceramics is that it is not possible to use it as implants.

Known methods of obtaining biostable in the form of porous ceramics based on calcium phosphates. Porous ceramics are mainly method burnable additives (which are used flour, gelatin, collagen, chitosan, and other), impregnation and subsequent calcination organically is (polyurethane) sponges, or foaming, for example, with the introduction of hydrogen peroxide.

When this porosity, for example, when using dodecyl-benzosulfimide sodium reaches up to 50-60%, and in the case of glycine or agar-agar is about 80%. Using burnable additives (for example, flour) with a particle size of 40-200 μm, enter in the amount of 37 wt.%, managed to get the calcium-phosphate ceramics with volumetric content then to 46%. As burnable additives used as the polymer is gelatin, collagen, chitosan, and others, with open porosity reaches 85%. Also use coral (the main substance of caso3), which during the hydrothermal treatment at 250°C for 24-48 h goes into hydroxyapatite, preserving the original microstructure and open porosity. Porous ceramics has a tensile strength in bending 2-11 MPa, which is two to three times less than the required values, with an increase of porosity, the strength of the material decreases dramatically [Barinov S.M., V.S. Komlev the Bioceramics based on calcium phosphates. - M.: Nauka, 2005. - 204 S. - ISBN 5-02-033724-2].

A method of obtaining porous bioactive glass-ceramic material including the production of semi-dry mass of the powder of calcium-phosphate glass composition (mol.%): P2O5- 39,10, Cao - 43,50, Al2O3- 4,35, In2About3- 4,35, TiO2- 4,35, ZrO2- 4,35 1% odnomestnoi polyvinyl alcohol, forming workpieces by pressing under a pressure of 2.5 MPa, firing blanks in isothermal conditions at a temperature of 950°C for 1 hour [Suchilin NV, Stroganov E.E. Sintered glass-ceramic materials based on calcium-phosphate glasses. // Glass and ceramics. - 2008. No. 8 - P.8-11].

The disadvantage of this method is unsatisfactory strength of the resulting porous ceramic.

The known method of forming a porous glass substrate, comprising the following stages: melting a mixture consisting mainly of 40-60% SiO2, 5-30% Na2O, 10-35% Cao and up to 12% R2About5at a temperature of 1350°C, cooling, grinding the obtained glass and forming a porous glass substrate by mixing the powder with a foaming agent, and hot pressing the powder and foaming agent in vacuum [U.S. Pat. U.S. No. 5676720, publ. 14.10.1997].

The disadvantages of this method include the high temperature glass melting, multi-stage and insufficient strength of the resulting porous ceramic.

As the closest analogue is selected acquisition method biostable 45S5 containing calcium, phosphorus, sodium, and silicon [Junmin Qian, Yahong Kang, Zilin Wei, Wei Zhang. Fabrication and characterization of biomorphic 45S5 bioglass scaffold from sugarcane. Materials Science and Engineering: 2009. v.29. No. 4. pp.1361-1364]. The method is as follows: Tetra-ethoxysilane and triethyl phosphate is mixed with 1-Olamim solution of nitric acid and 60 minutes carry out the hydrolysis with stirring. Then gradually add to the mixture of the nitrates of calcium and sodium. After 6 hours stirring receive transparent liquid. For maturation Zola the mixture is kept for 5 days in a sealed container. The result is a Sol with a solids content of 35%. This Sol impregnated porous material from sugar cane (with a pore diameter of ~ 10 µm), which is further subjected to heat treatment at 1030°C. When this cane matrix fade and is formed of porous ceramic material.

The disadvantages of the method include a multi-stage, duration of the process and the lack of strength of the resulting ceramic.

The task of the invention is the simplification of the method of producing a porous calcium phosphate ceramics by reducing the time and number of stages, as well as increasing the strength of the obtained materials by creating bioactive layers of the same shape, then, more durable porous bioinert implants.

The problem is solved in that in the method of obtaining calcium-phosphate ceramic material, comprising preparing a mixture containing compounds of calcium, phosphorus, silicon and sodium, the impregnation mixture biologically inert porous matrix with subsequent annealing, the silicon compound used tetraethoxysilane is, as the phosphorus compounds used ether phosphoric acid, in contrast to the known method, as compounds of calcium and sodium are carboxylates in a polar organic solvent, as a biologically inert matrix used avigorous porous matrix, and the calcination after impregnation is carried out at a temperature of 1000-1200°C.

While the preparation of the solution for impregnation of bioinert ceramics lead when heated until dissolved compounds of calcium, phosphorus, silicon and sodium, as carboxylates of calcium and sodium use their oleates, as the polar organic solvent used, for example, turpentine or benzene, in ether phosphoric acid is used, for example, triethyl phosphate or tributyl phosphate, as navigaciya porous matrix durable ceramics made of aluminum oxide or zirconium, before annealing impregnated with a solution of the porous matrix is heated to 200-250°C to remove excess solvent.

In the General case, the method is as follows.

The components of the glass in the form of calcium oleate and sodium oleate in a predetermined ratio are dissolved in a polar organic solvent. In the resulting solution is added in a predetermined ratio, the triethyl phosphate or tributyl phosphate, tetraethoxysilane and heated to 160-180°C to complete the RA is the creation of all components. For the production of bioactive implants obtained solution impregnated porous bioinert implants followed by heating at 200-250°C to remove excess solvent and calcined at a temperature of 1000-1200°C. When it is formed on the porous bioinert implants thin bioactive calcium phosphate glass-ceramic layers, the shape of the pores.

Conducting high-temperature processing of the intermediate product in the specified temperature range due to the fact that in these conditions ensures complete combustion of organic matter and the formation of a ceramic phase of the target product, and therefore the temperature rise above 1200°C is not economically feasible. It was established experimentally that the time of heat treatment of the residue obtained after removal of the solvent, at a temperature of 1000-1200°C is not more than 1 hour.

Through the use of more durable (compared to known porous matrix) navigaciya ceramic porous biologically inert matrix made of aluminum oxide or zirconium impregnated with the obtained solution containing the components of the glass: tetraethoxysilane, triethyl phosphate or tributyl phosphate and carboxylates of calcium and sodium in a polar organic solvent, onto the porous matrix directly from the solution (and not from Zola) is formed is described thin calcium phosphate layers, the shape of the pores. The result is Biosafety calcium-phosphate materials.

The technical result of the invention is to achieve the possibility of obtaining bioactive glassceramics not from Zola, but directly out of solution easily penetrates into the pores of the matrix, bypassing the stage of education Zola, allowing you to build on a solid porous bioinert implants, bioactive calcium phosphate layers, the shape of the pores, which significantly simplifies the method and reduces the process time. If this process does not require complicated special equipment and expensive reagents.

Enablement of the claimed invention, the following examples.

Example 1. In 20 ml of turpentine when heated dissolve 1.1 g of calcium oleate, 1.0 g of sodium oleate, add 0.1 ml of tributyl phosphate and 0.7 ml of tetraethoxysilane. The heating is conducted at a temperature of 180°C until complete dissolution of all components. This solution impregnated porous bioinert ceramics aluminum oxide. The impregnated product is first heated to 200-250°C to remove excess turpentine, and then calcined at 1100°C for 1 hour. The result of bioactive ceramics with thin bioactive coating that meets the composition of the calcium-phosphate ceramics, soda is official in %: P2O5- 6, Cao - 24,5, Na2O - 24,5, SiO2- 45,0.

Example 2. In 20 ml of benzene by heating dissolve 1.1 g of calcium oleate, 0.96 g of sodium oleate, add 0.1 ml of tributyl phosphate and 0.7 ml of tetraethoxysilane. The heating is conducted at a temperature of 170°C until complete dissolution of all components. This solution impregnated porous bioinert ceramics aluminum oxide. The impregnated product is first heated at 200-250°C to remove excess benzene, and then calcined at 1200°C for 0.5 hour. The result of bioactive ceramics with thin bioactive coating that meets the composition of calcium phosphate glass ceramics containing in %: P2O5- 6, Cao - 25,5, Na2O - 23,5, SiO2- 45,0.

Example 3. In 20 ml of turpentine when heated dissolve 1.1 g of calcium oleate, 0,92 g of sodium oleate, add 0.1 ml of tributyl phosphate and 0.7 ml of tetraethoxysilane. The heating is conducted at a temperature of 180°C until complete dissolution of all components. This solution impregnated porous bioinert ceramics zirconium oxide. The impregnated product is first heated at 200-250°C to remove excess turpentine, and then calcined at 1000°C for 1 hour. The result of bioactive ceramics with thin bioactive coating that meets the composition of calcium phosphate glass ceramics containing in %: P 2O5- 6, Cao Is 26.5, Na2O - 22,5, SiO2- 45,0.

Example 4. In 20 ml of turpentine when heated dissolve 1.1 g of calcium oleate, 0,92 g of sodium oleate, add 0.1 ml of triethyl phosphate and 0.7 ml of tetraethoxysilane. The heating is conducted at a temperature of 180°C until complete dissolution of all components. This solution impregnated porous bioinert ceramics zirconium oxide. The impregnated product is first heated at 200-250°C to remove excess turpentine and then calcined at a temperature of 1150°C for 55 minutes as a result of bioactive ceramics with thin bioactive coating that meets the composition of calcium phosphate glass ceramics containing in %: P2O5- 7, Cao Is 26.5, Na2O - 22,5, SiO2- 44,0.

Example 5. In 20 ml of turpentine when heated dissolve 1.1 g of calcium oleate, 0,92 g of sodium oleate, add 0.1 ml of triethyl phosphate and 0.7 ml of tetraethoxysilane. The heating is conducted at a temperature of 160°C until complete dissolution of all components. This solution impregnated porous bioinert ceramics zirconium oxide. The impregnated product is first heated at 200-250°C to remove excess turpentine, and then calcined at 1100°C for 1 hour. The result of bioactive ceramics with thin bioactive coating that meets the composition of calcium phosphate glass ceramics containing in %: P2Osub> 5- 7, Cao Is 26.5, Na2O - 22,5, SiO2- 44,0.

1. The method of obtaining calcium-phosphate ceramic material, comprising preparing a mixture containing compounds of calcium, phosphorus, silicon and sodium, the impregnation mixture biologically inert porous matrix with subsequent annealing, the silicon compound using tetraethoxysilane as the phosphorus compounds used ether phosphoric acid, characterized in that compounds of calcium and sodium are carboxylates in a polar organic solvent, as a biologically inert matrix used avigorous porous matrix, and the calcination after impregnation is carried out at a temperature of 1000-1200°C.

2. The method according to claim 1, characterized in that the preparation of a mixture of lead when heated in the temperature range of 160-180°C until dissolved compounds of calcium, phosphorus, silicon and sodium.

3. The method according to claim 1, characterized in that as carboxylates of calcium and sodium use the oleates of these compounds.

4. The method according to claim 1, characterized in that as the polar organic solvent used, for example, turpentine or benzene.

5. The method according to claim 1, characterized in that the ester of phosphoric acid is used, for example, triethyl phosphate or tributyl phosphate.

6. The method according to claim 1, characterized in that the as navigaciya porous matrix ceramics made of aluminum oxide or zirconium.

7. The method according to claim 1, characterized in that before annealing impregnated with a solution of the porous matrix is heated to 200-250°C to remove excess solvent.



 

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19 cl, 1 dwg, 4 tbl

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