Method of obtaining calcium phasphte nanoparticles, stabilised by salt matrix

FIELD: medicine.

SUBSTANCE: there is described method of obtaining of calcium phosphate nanoparticles, stabilised by salt matrix by interaction of components, first of which contains metal cation, and second contains anion. According to invention as the first component applied is water-soluble calcium salt, and as the second component, soluble orthophosphate, nanoparticles of water non-soluble calcium phosphate being formed, and salt matrix being formed from soluble by-product. Content of calcium phosphate nanoparticles in powder composite "oxide nanoparticles/salt matrix" constitutes 65-82 wt %.

EFFECT: method is aimed at creation of effective nanotechnologies, in order to prevent degradation, that is, aggregations of oxide nanoparticles of calcium phosphates.

5 tbl, 4 ex

 

The invention relates to the field of nanomaterials, including biomedical applications, and is aimed at creating an effective nanotechnology, with the aim of preventing degradation, i.e. aggregation of oxide nanoparticles of calcium phosphates composition xCaO·yP2Os·zH2O.

To stabilize the nanoparticles, i.e. to prevent aggregation, apply the synthesis of nanoparticles in mesoporous matrices such as silica-alumina (1) or glass matrices (2). However, removing the nanoparticles from such matrices requires the use of aggressive fluids (acids, alkalis).

Known methods of forming the powder of the composite nanoparticles/salt matrix" as a result of mechanochemical solid-phase synthesis of nanopowders SEO (3) as a result of exchange reactions of ZnO in the decomposition of Zn5(NO3)2(OH)8·2H2About (4), and compounds of Na0.5Bi0.5TiO3using topochemical method (5) in saline matrices. Salt matrix is formed in the solid phase is partly due to exchange reactions (3)and is payable when making the original mixture (3, 4, 5). However, such methods cannot be used for the formation of a powder composite nanoparticles/salt matrix of nanocrystalline calcium phosphates because of the need for the synthesis of maintaining a constant pH value.

Nai is more close to the present invention is a method of formation of the salt matrix for stabilization of oxide nanoparticles, including the synthesis of powder composite containing salt matrix (6), in which the nanoparticles and salt matrix are formed in the exchange reaction. The disadvantage of this method is the inability to adjust the pH level required for the synthesis of insoluble phosphates.

The aim of the present invention is to develop a method of producing nanoparticles of calcium phosphates, stable salt matrix. This goal was achieved by the present invention.

In the method for production of nanoparticles of calcium phosphates, stable salt matrix, the interaction of components, the first of which contains the cation of the metal, and the second contains the anion, according to the invention, as a first component, use a water-soluble salt of calcium, and as a second component, soluble orthophosphate, the formation of nanoparticles of water-insoluble phosphatate calcium, and salt matrix is formed from the soluble byproduct.

For the formation of the salt matrix includes nanoparticles of calcium phosphate composition xCaO·yP2O5·zH2O (or powder composite nanoparticles of calcium phosphate/salt matrix") to prepare the initial solution with a concentration of 0.25 to 1.00 M for [CA2+] and 0.15-0.60 M for [(RHO4)-3]. Powders of th the interaction of reagents, the precipitate and drying contain from 8 to 35% adsorbed byproduct of the reaction, which corresponds to the content of oxide nanoparticles in the composite 65-82 wt.%.

When using more dilute solutions (less than 0,25M for [CA2+] and 0.15 M for [RHO43-]) the number of adsorbed associated soluble reaction product is sufficient to prevent aggregation of the nanoparticles in powder composite. When using more concentrated solutions (>1.0 M for [CA2+] and 0.6 M for [(RHO4)3-]) the number of adsorbed product almost does not increase, because of the limited adsorption capacity of the surface of the nanoparticles of calcium phosphate.

Example 1

1 l of a 0.5 M solution of calcium chloride CaCl2poured to 1 l of 0.3 M solution of Na2HPO4containing as the regulator of pH NaOH, taken as 1.2-fold excess relative to the calculated reaction, at pH=8-10, T=60°C (1)

The synthesized powder after separation of the precipitate and drying is a powder composite nanoparticles of calcium phosphate/salt matrix in which nanoparticles of calcium phosphate is hydroxyapatite nanoparticles and salt matrix - sodium chloride. Powder composite contains 80% CA10(PO4)6(OH)2and 20 NaCl. Sodium chloride in this case represents a physical barrier to the flow of the aggregation of the nanoparticles of hydroxyapatite. Storage nanoparticles of hydroxyapatite in the salt matrix is a companion product for a long time under normal conditions, without heating to the melting temperature of the salt matrix. Removing nanopowder from the salt matrix is conducted by washing the resulting powder with water. Similarly extracted hydroxyapatite nanopowders synthesized by the reaction of (1) from solutions of other concentrations (table 1). The table shows that under these conditions, the extraction nanopowder from the salt matrix particle size of 20-40 nm. To obtain nanoceramics preferably colloidal forming of the suspension of nanoparticles of hydroxyapatite extracted from the salt matrix.

nanoparticles
Table 1
The synthesis conditionsThe composition of the powder compositeThe average size of particles in suspension, after removal of the stabilizing salt matrix
[Ca2+][PO43-]matrix
CA10(PO4)6(OH)2NaCl, %
10.25 M0.15 M92820-40 nm
20,50 M0.30 M802020-40 nm
31,00 M0.60 M653520-40 nm

Example 2

1 l of 0.3 M solution (NH4)2HPO4poured to 1 l of 0.5 M solution of calcium nitrate CA(NO3)2containing as the regulator of pH NH4OH, taken as 1.2-fold excess relative to calculated according to reaction (2), at pH=9, T=60°C.

The synthesized powder after separation of the precipitate and drying is a powder composite nanoparticles of calcium phosphate/salt matrix in which the nanoparticles of calcium phosphate this hydroxyapatite nanoparticles and salt matrix - ammonium nitrate. Powder composite nanoparticles of calcium phosphate/salt matrix" contains 80% CA10(PO4)6(OH)2and 20% of NH4NO3. The ammonium nitrate in this case represents a physical barrier to the flow of the aggregation of the nanoparticles of hydroxyapatite. Storage nanoparticles of hydroxyapatite in the salt matrix is a companion product for a long time under normal conditions, without heating to the melting point or thermal decomposition of the salt matrix. Removing nanopowder from the salt matrix is conducted by washing the resulting powder with water.

Similarly extracted hydroxyapatite nanopowders synthesized according to reaction (2) from solutions of other concentrations (table 2). The table shows that under these conditions, the extraction nanopowder from the salt matrix particle size of 20-40 nm. To obtain nanoceramics preferably colloidal forming of the suspension of nanoparticles of hydroxyapatite extracted from the salt matrix.

Table 2
The synthesis conditionsThe composition of the powders is th composite The average size of particles in suspension, after removal of the stabilizing salt matrix
[Ca2+][PO43-]nanoparticlesmatrix
CA10(RHO4)6(OH)2, %NH4NO3, %
10.25 M0.15 M92830-60 nm
20,50 M0.30 M802030-60 nm
31,00 M0.60 M653530-60 nm

To retrieve the hydroxyapatite nanopowder from the salt matrix ammonium nitrate is also possible another method of extraction, which is associated with a relatively low temperature of razlozhyeniya ammonium, which lies in the range of 150-250°C. For this method of extraction nanopowder of hydroxyapatite in the salt matrix ammonium nitrate is carried out in the range 300-400°C for 3-6 hours. When processing at temperatures below 300°C and less than 3 hours unable to completely release the powder from the salt matrix. When processing at temperatures above

400°C and more than 6 hours may flow initial stage of sintering, leading to reduction in specific surface area and increase the size of the particles.

Similarly extracted hydroxyapatite nanopowders synthesized according to reaction (2) from solutions of other concentrations (table 3). The table shows that under these conditions, the extraction nanopowder from the salt matrix specific surface area of the powder is 40-60 m2/year Recovered hydroxyapatite powder can be used to obtain nanoceramics using a cold hydrostatic pressing.

Table 3
The composition of the powder compositeT treatment, °CDuration, hoursSpecific surface area, m2/g
nanoparticlesmatrix
CA10(RHO4)6(OH)2,%NH4NO3, %
1928300240-60
28020350440-60
36535400640-60

Example 3

1 l of a 0.5 M solution of calcium acetate CA(CH3Soo)2poured to 1 l of 0.3 M solution of K2HPO4containing as the regulator of pH CON, taken as 1.2-fold excess relative to the calculated reaction, pH=8-11, T=60°C (3)

The synthesized powder after separation of the precipitate and drying is a powder composite nanoparticles of calcium phosphate/salt matrix in which nanoparticles of calcium phosphate is hydroxyapatite nanoparticles, salt matrix - acetate to the lia. Powder composite nanoparticles of calcium phosphate/salt matrix" contains 80% CA10(PO4)6(OH)2and 20% KCH3COO. Potassium acetate in this case represents a physical barrier to the flow of the aggregation of the nanoparticles of hydroxyapatite. Storage nanoparticles of hydroxyapatite in the salt matrix is a companion product for a long time under normal conditions, without heating to a temperature of thermal decomposition of the salt matrix. Removing hydroxyapatite nanopowder from the salt matrix is conducted by washing the resulting powder with water.

Similarly extracted hydroxyapatite nanopowders synthesized according to reaction (3) from solutions of other concentrations (table 4). The table shows that under these conditions the extraction of hydroxyapatite nanopowder from the salt matrix particle size of 30-50 nm. To obtain nanoceramics preferably colloidal forming of the suspension of nanoparticles of hydroxyapatite extracted from the salt matrix.

Table 4
The synthesis conditionsThe composition of the powder compositeThe average size of the p particles in suspension, after removal of the stabilizing salt matrix
[CA2+][PO43-]
CA10(PO4)6(OH)2, %KCH3COO, %
10.25 M0.15 M92830-50 nm
20,50 M0.30 M802030-50 nm
31,00 M0.60 M653530-50 nm

Example 4

1 l of a 0.5 M solution of calcium chloride CaCl2poured to 1 l of a 0.5 M solution of Na2HPO4by reaction pH=4, T=40°C (4)

The synthesized powder after separation of the precipitate and drying is a powder composite nanoparticles of calcium phosphate/salt matrix", inwhich nanoparticles of calcium phosphate this nanoparticles brushite CaHPO4·2H2O, salt matrix - sodium chloride NaCl. Powder composite nanoparticles of calcium phosphate/salt matrix" contains 80% CaHPO4·2H2O and 20% NaCl. Sodium chloride in this case represents a physical barrier to the flow of the aggregation of the nanoparticles monetite. Storage nanoparticles of brushite in the salt matrix is a companion product for a long time under normal conditions, without heating to the melting temperature of the salt matrix. Removing nanopowder from the salt matrix is conducted by washing the resulting powder with water.

Similarly extracted nanopowders of brushite, synthesized according to reaction (4) from solutions of other concentrations (table 5). The table shows that under these conditions, the extraction nanopowder from the salt matrix particle size is 40-60 nm. To obtain nanoceramics preferably colloidal forming of the particle suspension of brushite extracted from the salt matrix.

Table 5
The synthesis conditionsThe composition of the powder compositeThe average size of particles in suspension, the Le removal of the stabilizing salt matrix
[Ca2+][PO43-]CaHPO4·2H2O %NaCl, %
10,25M0,25M92840-60 nm
20,50M0,50M802040-60 nm
31,00M1,00M653540-60 nm

Literature

1. Tretyakov UD, A.V. Lukashin, A.A. Eliseev Synthesis of functional nanocomposites based on solid-phase nanoreactors. // USP. 2004, T, No. 9, S-998.

2. Matthew J. Dejneka, Christy Powell, Nick Borrelli, Dimitre Ouzounov, Alex Gaeta Transparent Magnetic Glass-Ceramics II J. Am. Ceram. Soc. 2005, Vol.88. No. 9. P.2435-2441.

3. T.Tsuzuki and P.G. McCormick, Synthesis of ultrafine ceria powder by mechanochemical processing// J. Am. Ceram. Soc. 2001, Vol.84, No. 7 P.1453-1458.

4. Chong Phui Fah, Junmin Xue, John Wang nanosized Zinc oxide particle derived from mechanical activation of Zn5(NO3)8*2H2O in sodium cloride // J. Am. Ceram. Soc. 2002, Vol.85. No. 1. P.273-275.

5. J.T.Zeng, K.W.Kwok, W.K.Tam, H.Y.Tian, X.P.Jiang, and H.L.W.Chan, Plate-like Na0.5Bi0.5TiO3 template synthesized unit b topochemical method // J. Am. Ceram. Soc. 2006. Vol.89, No. 12, P.3850-3853.

6. T.Tsuzuki, W.T.A.Harrison, P.G.McCormick. Synthesis of ultrafine gadolinium oxide powder by mechanochemical processing // J. Alloys and compounds, 1998, Vol.281, P.146-151.

A method for producing powder of composite nanoparticles of calcium phosphate/salt matrix interaction components, the first of which contains the cation of the metal, and the second contains the anion, characterized in that the first component using water-soluble salt of calcium concentration of 0.25 to 1.00 M for [CA2+]and as a second component soluble orthophosphate concentration of 0.15 to 1.00 M [(PO4)3-], the formation of nanoparticles of water-insoluble phosphatate calcium, and salt matrix is formed from the soluble byproduct, the content of nanoparticles of calcium phosphates in powder composite is 65-82 wt.%.



 

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