SU1414776A1 - Method of producing copper hydroxophosphate - Google Patents

Abstract

The invention relates to the technology of producing reactive salts of orthophosphoric acid, to a method for producing copper phosphates, which are used as chemical reagents, catalysts of a high degree of selectivity, micronutrients, heat-resistant coatings, and essential components in the dental prosthetic technique. The aim of the invention is to increase the yield of the product. Copper hydroxophosphate is prepared by introducing powdered copper hydroxocarbonate to boiling phosphoric acid at a concentration of 5.7–8.4%, taken in an amount of 105–107% of stoichiometry. The reaction is carried out for 4-5 hours, after which the precipitate of the product is separated from the mother liquor. The product of composition f; 55-2.05 a9o-f.feP04 is obtained with a yield of 99-100% CoO and 92-95%. 3 tab. (L

Description

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The invention relates to the technology of reactive salts of orthophosphoric acid, specifically to a method for the production of copper phosphates, which are used as chemical reagents, catalysts of a high degree of selectivity, micronutrients, heat-resistant coatings, and essential components in denture technology.

The purpose of the invention is to increase the yield of the product.

Example 1. In a reactor, 5.11 g of 88.15% Hz.P04 is poured, 50 ml of distilled HjO are added (acid concentration after dilution is 8.3%, dose is 105% of stoichiometry) and heated with stirring until boiling . 10 g of powdered copper hydroxocarbonate containing 69.57% CuO are introduced into boiling acid in small portions. The suspension is stirred for 4 hours while maintaining a constant temperature and volume of water in the reactor. The solid precipitate is separated from the solution, washed with 30-50 ml of cold distilled water and dried at 60-80 ° C for 3-4 hours.

The salt of the composition is obtained), oiP04 with a yield of 99.8% for Cu and 94.8% for. and 97.8% shee mass from theoretical. According to a known method, copper hydroxocarbonate is obtained by treating with a stoichiometric amount of phosphoric acid at 70 ° C powdered copper hydroxocarbonate. The reaction mixture is briefly heated to boiling point and the product is separated. The yield of 94%.

Based on the accuracy of the analysis methods stipulated by the technical conditions for copper phosphate basic, the composition of individual copper hydroxyphosphate may correspond to the average formula CU20HP04B for a certain range of individual ingredients. According to the calculations and experimental data of X-ray phase analysis, these oscillations are permissible within 4 + 0.10 Ci PiOsx 1 ± 0, or. .2.5 (OH),. ,, Pp4.

To obtain the salt of the indicated composition according to the proposed method, it is necessary to introduce powdered copper hydroxocarbonate into boiling HjPO, and not vice versa. In this case, a salt of a given composition is formed at a rate of 103-107% of stoichiometry. Lower norm does not provide completeness

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five

five

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initial carbonates, and an increase results in the formation of impurities of the crystalline hydrate of average copper phosphate ..

The effect of the order of mixing the reagents on the yield of the synthesis products is given in Table. one.

The effect of the concentration of the HzP04 solution at the exit of the synthesis products with a reaction time of 4 hours is given in Table 2.

The purity of the synthesized copper hydroxophosphate is provided by using a solution of phosphoric acid with a concentration of 5.7–8.4% (Table 2. In the reaction with a more dilute acid (4.9%), the decomposition of the initial copper carbonate is not reached, and Knows the final product of the synthesis. When the concentration of the acid is increased to 10%, a deterioration in the quality of the product is observed due to a change in the ratio between CuO in its composition (impurity of the average copper phosphate).

The effect of the reaction time on the yield of the synthesis products is given in Table. 3

As can be seen from the table. 3, the optimal synthesis time for a conforming product is 4-5 hours. If the process duration is reduced to 3 hours, the carbonate decomposition reaction may not be completed. An increase in the duration of the reaction is not advisable, since after 4 hours of synthesis the composition of the final products remains almost unchanged.

Using the proposed method for producing copper hydroxyphosphate, compared with limestone, a reduction in the complete cycle of salt production from 20–24 to 8 h, an increase in the yield of the final product by not less than 17%, an increase in the quality of the product, i.e. its greater compliance with the formula. and saving energy and labor costs due to the greater efficiency of the method.

Claims (1)

Formula inveni.ni  A method for producing copper hydroxyphosphate, which involves treating phosphoric acid with heating and stirring with powdered copper hydroxocarbonate, separating the product from 314U776 the mother liquor, followed by drying, about t-phosphoric acid concentration of 5.7 liters, and the fact that, with 8.4%, taken in the amount of 105-197% phosphoric acid concentration of 5.78, 4%, taken in the amount of 105-197% the goal of increasing product yield, hydro- from stoichiometry, and processing lead copper roxocarbonate is introduced into boiling A - 5 i. At 6-09-01- Suspension e 27% 346-76Cu (OH) CuCOj- nHjO offerable 1 Suspension 6.9% C (OH), CisOZ-pN., 0 2 Suspension NzP04 7,3% on Cu (OH), - CuCOj-nH 3Suspension, 3% Cu (OH) j-CuC03-riH20 4НзР04-5.7% on Cu (OH) 2-CdCOs (powdered) 5НЗРО -5.7% on Cu (OH) 2 CuCOj (powdered) 6НзР04-5.8% on Cu (OH 2-CSCB (powdered) . 7 NeR04 5.7% on Cu (OH) 2-CSCB (powdered) 8HzP04 5, .7% Cu (OH) i-CuCOj (powdered) 9HzP04-5.7% Cu (0ll) .j-CuSO (powdered) Famous Suspension Cu (OH) j-CuCO nI O HaPQj 85% A - 5 i. Table 1 20 120 90.5 4 120 Product contaminated with cairns 4 134 Product contaminated with carbonates. 8 134 The same 4 120 90.5 110 94.7 107 96.3 105 97.3 103.5 Product is contaminated with carbonates. 102 Also About 105 2-3 94.0 table 2 93.5 96,8 86.8 coins 95.2 98.6 Zonath 86.5 88.5 83,486-88 (pa Tabli.tsa 3 Also 97,796,8 97.3: 95.2 97.3 95.2 Product contaminated with carbonates   The method according to TU 6-09-01-346-76. The method is modeled according to TU 6-09-01-346-76.