RU1805129C - Method of synthesis of di-2-ethylhexylphosphate metals - Google Patents

Abstract

SUMMARY OF THE INVENTION: the product is di-2-ethClChexylphosphates of metals with grade m (C8Hi70), where n is 2, if M is Co (II), MD, Ca, Ba, Nl, Zn, Cd, Cu (II) and n is 3, if M Fe (II) and Zn (II), the yield is 90 - 98 percent. Reagent 1: aqueous solution of potassium di-2-ethylhexyl phosphate. Reagent 2: an aqueous solution of sulfate MD, Cu, Co, Ba, Ni, Zn, Cd or chloride Fe (II) or Zn (II). Reaction conditions: at a temperature of 70 - 90 ° C, a molar ratio of M +: (CaHNTbO P00 1.5: 2 and pH 8 - 9 when using sulfates Md, Ca, Ba, Ni in the case of using salt Co, Cu, Zn, Cd; or at room temperature and molar ratio M + (CbH 170) 2 1: 3 in the presence of hydrochloric acid using iron or zinc chloride.

Description

The invention relates to methods for producing di-2-ethylhexylphosphates of metals of the composition M ((CeHi70) 2 P00) p, where p 2; M Ma2 +, Ca2V, Ba2 Co2 +, NI2YCu2 +, Zn2 +, + Csg. n 3, Fe3 +, 1p3 + etc., which are used as oil-soluble surface-active substances, and also as extraction reagents.

The aim of the invention is to simplify the synthesis procedure, reduce the consumption of organic solvents and increase the yield of target products.

This goal is achieved by the fact that metal di-2-ethylhexylphosphates precipitate from aqueous solutions of potassium di-2-ethylhexylphosphate, acting in excess of water-soluble metal salts against stoichiometry when adjusting the pH and temperature of solutions depending on the tendency of the metal cation to hydrolyze . Compact wax-like precipitates are separated by decantation, washed with water and dried in air. Additional purification of the preparations is achieved by dissolving them in a suitable organic solvent (CCI4, P-C7H16, toluene), filtering the solution and precipitating salts from it with excess acetone (except NiX2).

Example 1. To 100 ml of a 0.2 mol / L aqueous solution of CH, heated to 70 - 90 ° C and having a pH of 8 - 9, 25 ml of a hot solution of 0.6 mol / L of magnesium sulfate was added. The precipitate formed is washed with hot water and dried to constant weight. 13 g of a white wax-like substance are obtained. In a similar manner, CaX3, BaX2 and NiXa are obtained. (See table).

Example 2. To 500 ml of a 0.2 mol / L aqueous solution of KX with a pH of 5–6, heated to 70–90 ° С, 300 ml of a hot 0.25 mol / L solution of copper sulfate are poured. The precipitate was separated by decantation, washed with hot water and dried in air. Obtain 31 g of blue crystalline substance C

00

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wa. If necessary, the preparation is further purified by dissolving 0.5 mol / L CuXa in carbon tetrachloride with the addition of 10 vol.% Acetone to lower the viscosity of the solution, then filtering through a paper or glass filter and precipitating with a triple excess of acetone. In a similar way receive other MHg, (see table).

Example 5 To 300 ml of a 0.1 mol / L aqueous solution of 10 KX, 100 ml of a 0.15 mol / L aqueous solution of ferric chloride containing 0.1 mol / L HCI was added. Precipitation was carried out at room temperature, the white wax-like mass was separated by decantation, washed with water and dried in air. 9.2 g of substance are obtained. Further purification is carried out in the same manner as in Example 2. Salts of other three-charged cations are likewise obtained (see table). twenty

The proposed method is notable for simplicity, since there is no need to filter precipitates due to their compact wax-like structure and significant yields of target products.

comrade Organic solvents are required.

only if necessary

salt cleaning.

Claims (1)

SUMMARY OF THE INVENTION Method for the preparation of di-2-ethylhexylphosphates of metals of general formula M (SvN 170) 2, where n 2, if M Co (II), Md, Ca, Ba, Ni, Zn, Cd, Cu (I); n 3, if M Fe (III), In (III), the interaction of potassium di-2-ethylhexylphosphate with an aqueous solution of sulphate Md, Cu, Co, Ca, Ba, Ni, Zn, Cd or with Fe (lit) or In (111) chloride, vol. that, in order to simplify the process, potassium di-2-ethylhexylphosphate is used in the form of an aqueous solution; the ith process is carried out at a temperature of 70 - 90 ° C, molar ratio M +: (CaHnPb P00 1.5: 2 and pH 8-9 in the case of using sulfate Md, Ca, Ba, Ni and pH 5-7 in the case of using the salts of Co, Cu, Zn, Cd or at room temperature at a molar ratio (CsHnOJa 1: 3 in the presence of hydrochloric acid using iron chloride Is indie. The results of the analysis obtained by the described method of di-2-ethylhexylphosphates