The method of obtaining complex compounds of zirconium or hafnium with d-fructose

 

(57) Abstract:

The invention relates to a method for production of the complex compounds of zirconium or hafnium with D-fructose General formula Me4(OH)8-n(C6H9O5)nH2O16-2n]Cl8,

where Me is zirconium or hafnium, n = 1 to 4, an integer, by interacting oxychloride, zirconium or hafnium with D-fructose. The target product is isolated in the form of an aqueous solution or as a dry powder by known techniques. The proposed complex compounds suitable for the modification of polymers by creating composite materials.

The invention relates to the production of new complex compounds of zirconium or hafnium with organic ligands.

A method of obtaining complex compounds of zirconium or hafnium with various organic ligands (see encyclopedia of Chemical in 5 volumes. M : Soviet encyclopedia. T. 1, 1988, S. 506; M: Great Russian encyclopedia. So 5, 1998, S. 386).

Also known is a method of obtaining complex compounds of zirconium or hafnium with amino acid, for example with-alanine General formula 1

IU(OH)2AND2X23H2O (1)

where Me is zirconium or hafnium;

sigalovada or oxynitride zirconium or hafnium with-alanine in aqueous medium, followed by separation of the target product by known methods (see copyright certificate 484220 "Method of production of the complex compounds of zirconium or hafnium with-alanine". Bull. 34, 1975).

The aim of the invention is the expansion of the range of complex compounds of zirconium or hafnium.

The proposed compound of zirconium or hafnium with ketoaldehydes D-fructose satisfies the General formula 2

[Me4(OH)8-n(C6H9O5)n(H2O)16-2n]Cl8, (2)

where Me is zirconium or hafnium,

n = 1-4, an integer.

The proposed connection is produced by the interaction oxychloride, zirconium or hafnium, corresponding to the General formula 3

MeOCl28H2O (3)

where Me is zirconium or hafnium, with D-fructose in aqueous medium, followed by separation of complex compounds of zirconium or hafnium in the form of an aqueous solution or powder known techniques.

Example 1. A portion 99,83 g ZrOCl28H2Oh are dissolved in 105 ml of water at 40oC. To the resulting solution was added a solution of 55,80 g D-fructose in 70 ml of water. The solution was stirred at 60oC for 15 min before the appearance of yellow color, filtered through filter paper and continue to stir at this temperature for a further 120 min, the settlement of the UNC connection zirconium [Zr4(OH)4(C6H9O5)4(H2O)8] Cl8where n= 4, is placed in an airtight container for storage, use as a target product.

The complex compound of zirconium in the form of a brown powder is obtained by evaporating the above-described aqueous solution on a rotary evaporator at 85oWith under a water-jet vacuum pump. The yield of dry matter is 108,94 g or 75% in terms of dry ingredients. According to elemental analysis of dry matter was found (experimental/theoretical): Zr 23,9/24,2%; From 19.3/19,1%, N 3,6/3,7%; Cl 18,6/18,9%.

Example 2. Synthesis of complex compounds of hafnium with D-fructose carried out analogously to example 1. To a solution of 70,3 g HfOCl28H2About 100 ml of water was added a solution of 6.85 g of D-fructose in 15 ml of water. The yield of dry matter [Hf4(OH)4(C6H9ABOUT5)4(H2O)8] Cl8is 46,29 g or 60% in terms of dry ingredients. According to elemental analysis of dry matter was found (experimental/theoretical): Hf 39,1/39.5 per cent; From 15.4/15.6 per cent; N 3,1/3,0%; Cl is 15.1/15.3 per cent.

Example 3. Synthesis of complex compounds of zirconium, D-fructose, in which n= 1, carried out analogously to example 1. To 99,83 g ZrOCl2N(OH)7(C6H9O5)(H2O)14] Cl8is 91,4 g or 80.3% in terms of dry ingredients. According to elemental analysis of dry matter was found (experimental/theoretical): Zr 30,6/30,9%; From 5.9/6.1 per cent; N Of 3.8/3.7%; And Cl 24,3/24,0%.

The obtained substances soluble in water and dimethylformamide.

IR and UV spectroscopy, and elemental analysis showed that during the reaction of D-fructose turns to ,-unsaturated carbonyl compound, which forms with cations of zirconium or hafnium chelate compound.

The proposed complex compounds are very stable in solution and is suitable for modification of polymers by creating composite materials.

The method of obtaining complex compounds of zirconium or hafnium with D-fructose General formula

IU4(OH)8-n(C6H9O5)n(H2O)16-2n] Cl8< / BR>
where Me is zirconium or hafnium;

n - 1 - 4 integer, characterized in that oxychloride, zirconium or hafnium is subjected to interaction with D-fructose, followed by separation of the target product in the form of an aqueous solution or as a dry powder known reception

 

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