SU947042A1 - Process for producing condensed mixed phosphates of alkali metals and metal selected from the series of cobalt, cadmium, manganese - Google Patents

Description

The goal is achieved by the method of obtaining condensed mixed phosphates, including the interaction of solutions of d-element chlorides and sodium trimetaphosphimate with first stirring for 0, an hour at the temperature of coynate, followed by heating the precipitates to a temperature of 500-700 ° C and keeping at this temperature for 1 -2 h

It is advisable in the preparation of cobalt polyphosphates NaCoCPO) and Na ColPO) to take the starting compounds in a molar ratio of cobalt chloride to sodium trimetaphosphimate, equal to 1: 0.9;

For the preparation of mixed trimeta. manganese phosphates or cadmium (P, 0), or NaCdCPjO) the starting compounds are taken in a molar ratio of metal chloride and sodium trimetaphosphimate, equal to 1: 3-5. The choice of the ratios of the starting compounds is optimal. Large ratios are impractical because of the high consumption of the starting compounds. At lower ratios, phases of variable composition are formed, when heated, which does not result in the formation of mixed condensed phosphates of strictly stoichiometric composition.

Thus, at a ratio m CPg, Naa, (), less than 1: 3, precipitates of variable composition are formed: Na; M {P 03N3H) 2iX (), where M Ип, Со, Cd.

In the case of the ratio:

The time of interaction in a mixture of CdCe Naj () –N2.0 is determined by the rate at which equilibrium is reached. is established within 0.5-1 h. An increase in the process duration over 1 h does not lead to a change in the reaction product. A mixing time of less than 0.5 hours leads to the formation of phases of variable composition.

The interaction time in mixtures is Na3 {P O N, H) - and MnCfj. .Na.

The choice of the temperature range is based on the fact that at a temperature below the heating product contains nitrogen, h, which leads to contamination of the condensed phosphates formed; heating the substance above results in the appearance of black inclusions in the product and partial decomposition of the substance obtained (see table).

The ratio N / P and P / Cd in the products of heating the precipitate obtained from solutions of CdCC and Ka- (Ro, 05M3N3), with a ratio of CdGHy., (),

Claims (2)

equal to 1: 3. 59 Thus, heating mixed manganese, cobalt, and cadmium trimetaphosphimates to 500–700 ° C and holding at this temperature for 1-2 hours results in condensed phosphates of strictly stoichiometric composition. Example 1. 25 ml of a manganese chloride solution containing 1 g is mixed with 25 ml of sodium trimetaphosphimate solution containing 5.68 g of Na3 (). H2.0 (ratio MnCCj.- Na (P 0,) x 1: 3). The resulting homogeneous solution is kept at room temperature for 6 hours. The precipitated crystals are filtered on Shott filter No. 1, washed once with acetone, then with ether. Get 3.6 g MadMP () 2 .. Yield 85%. The precipitate obtained is heated at a rate of 15 ° C / min to 600 ° C and maintained at this temperature for 1 hour. The formation of manganese trimetaphosphate of Na.Mn (P Od) is confirmed by chemical analysis and paper chromatography. 2.7 g is obtained. Yield 851. Found;%: 20.08; MPO 11.38 Q 68.54). Calculated,%: 19,9b; MpO 11.43; R.05- 68.51. Example 2. 25 ml of a solution of cobalt chloride containing 1 g of CoC is mixed with 25 ml of a solution of sodium trimetaphosphimate containing 1.58 g,) (ratio of Na (РЗ 0 Nj Н,) HjO 1: 1). The resulting homogeneous solution is kept at room temperature for 5 hours. The precipitated crystals from the filter on the filter Shott No. 1, washed once with acetone, then with ether. 1.6 g of NaCo are obtained (P., X7HiO. Yield 86%. The precipitate obtained is heated at a rate of 20 (/ min to 700 ° C and maintained at this temperature for 2 hours. The formation of polyphosphate is confirmed by chemical analysis and paper chromatography) cobalt composition of NaCo (PO). Obtain 1.1 g. Yield 86%. 9.74; CoO 23.51; Found,%: P2 05-66.75 MaCo (P05) C 9.72; CoO 23.9; Calculated,%: PRI me R 3. 25 ml of a solution of cobalt chloride containing 1 g of CoCEj-1 cm are dissolved with 25 ml of sodium trimetaphosphimate solution containing 6.32 g of Na3 (P306N H) - kV (CoCf-j6H2 0 ratio) p 4 1: +). The resulting homogeneous solution is removed. live at room temperature for k hours.The precipitated crystals are filtered on Shott filter No. 1, washed once with acetone, then with ether.Get 3 g (P ,,), 2. Exit The resulting precipitate is heated at a rate of 20 C / min to and maintained at this temperature for 1.5 hours. Data of chemical analysis and chromatography on paper confirmed the formation of cobalt polyphosphate of composition Na4Co (PO). 2.25 g are obtained. Yield 86%. Found,%: Ma „0 13.80; CoO 12.05; 68.15 (RO) b, Calculated,%: 19, CoO 11.99; , - 68.17 Example 4. 25 ml of cadmium chloride solution containing 1 g of CdCP / j.- 2 ,, is mixed with 25 ml of sodium trimetaphosphimate solution containing 8.20 g ,, 0 (, Nj, H) 4H, ( the ratio of CdCC.2 .- 2, 5H2.0: Na (, f) "4H, O 1: 5). The mixture is stirred at room temperature for 1 hour. The precipitate is filtered on Shott filter No. 4, washed three times with water, once with acetone, then with ether. Obtain 1, 9 g of NaCd (PO, N-H.,). Exit 98%. . The precipitate obtained is heated at a speed of min to 500 s and maintained at this temperature for 2 hours. Data on chemical analysis and chromatography on paper confirm the formation of cadmium trimetaphosphate with the composition NaCd (). Get 1.6 g. Yield 98%. 8.30; CdO 34.55; Found% P O ,, 57,25 NaCd (P.50p) t; a, 0 8,32; CdO 34.48; Calculated R-go; 57.20. The manganese, cobalt and cadmium phosphate phosphates are based on the use of non-toxic, non-aggressive substances. The elimination of multiple abrasion and heating operations simplifies the process. In addition, the heating time is reduced to 1-2 hours compared with the known method, in which the starting components are heated at 700-8 ° C for an hour. The duration of the process according to the proposed method is at most 8 hours, i.e. the time required to obtain mixed condensed manganese phosphates, cobalt and cadmium is shortened by a factor of 3 in comparison with the prototype. The proposed method does not require repeated thorough grinding of reagents, and rax e-ifa-spororo observance of the stoichiometric ratio of the initial components and allows obtaining high-quality condensed phosphates with a sufficiently high yield (85-98). The compounds obtained by the proposed method can be used as catalysts, as well as matrices for activation by ions of rare-earth elements. Claim 1. Method for producing condensed mixed phosphates of alkali metals and a metal selected from the series of the interaction of the compound of these metals and the phosphorus compound, characterized in that, to simplify the process, reduce the duration of the process, chloride or cobalt are used as starting compounds. , or cadmium, or manganese and sodium trimetaphosphimate and the process is carried out at room temperature for 0.5-6.0 hours, followed by heating the mixture to a temperature of 500-700 ° C and keeping it for 1-2 hours. 2, the method according to claim 1, wherein in order to obtain mixed trimetaphosphates or manganese or cadmium, the starting compounds are taken in a molar ratio of metal chloride and sodium trimetaphosphimate equal to 1: W-B3. The method according to claim 1-, This means that, in order to obtain mixed cobalt polyphosphates, the starting compounds are taken in a molar ratio of metal chloride and sodium trimetaphosphimate, equal to 1: 0.9. Sources of information taken into account in the examination 1.Tordjman J., Qui О.T. Laugt M. Bull. Soc. fr. Mineral Cristallogr 1970, 93, 160-165. 2.Mehrotra R.C., Yyas P.C., Oza C.K. - Indian J. Chem, 1972, 10, No. 7, 726-730.