RU2553471C2 - Method for producing copper (ii) glycinate (ii) in presence of acetophenoneoxime - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: invention refers to chemistry, more specifically to a method for producing copper glycinate that can find application as biologically active and feed additives. A method involves heating fine glycine powder and powdered copper in water (or dimethylformamide) at constant stirring of a reaction mixture. The precipitate is decanted, dissolved; the solution is filtered, boiled off partially; after cooling down with ethanol, copper (II) glycinate is deposited; the mixture is filtered; the complex is washed in petroleum ester and dried. Before heating, the reaction mixture is added with an oxidiser, which is presented by acetophenoneoxime in the following ratio, wt %: glycine - 3.35-6.00; copper - 1.52-2.60; water (or dimethylformamide) - 89.32-80.53; acetophenoneoxime - 5.81-10.87.

EFFECT: method is implemented in the presence of acetophenoneoxime and enables increasing the copper (II) glycinate yield.

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Description

The invention relates to the field of chemistry, in particular to the direct synthesis of complex compounds from a metal in a compact state and a chelating agent in the presence of a solvent and used to obtain metal complex compounds, the selective separation and disposal of non-ferrous, including precious metals from spent catalysts, sludges and other wastes production, protection of metals from corrosion.

A known method of producing copper (II) glycinate by the interaction of methanol solutions of glycine and copper (II) hydroxocarbonate (see book. MS Novakovsky. Laboratory work on the chemistry of complex compounds. - Kharkov: From the Kharkov University. - 1972, p. 80). However, methanol negatively affects human health, and before using copper (II) glycinate as a biologically active substance, the use of an aqueous solution is required, which complicates the isolation and purification of the complex compound.

The closest in technical essence is a method for the direct synthesis of copper (II) glycinate, including the interaction of metallic copper powder with glycine in water or dimethylformamide at the boiling point of the reaction mixture for 1 hour or while maintaining the specified reaction mixtures at room temperature for 20-30 days (see Art. Ogorodnikova N.P., Starkova N.N., Ryabukhin Yu.I. A direct method for the synthesis of complexes of copper (II) with amino acids in non-aqueous solvents. University proceedings. Chemistry and chemical technology, 2009. - V. 52 . - Issue 12. - S.45-47). However, the yields of the complex are 80%, 7-14% of copper goes into the oxidized state, i.e. the proposed method is not effective enough.

The technical problem is to improve the method by adding an additional component, an oxidizing agent, to the reaction system in order to increase the efficiency of the transition of copper to the oxidized state and, therefore, the output of copper (II) glycinate.

EFFECT: increased yield of copper (II) glycinate. It is achieved by the fact that in a method comprising heating finely ground glycine powder and powdered copper in water (or dimethylformamide) with constant stirring of the reaction mixture, decanting the precipitate, dissolving it, filtering the solution, partially evaporating it, and precipitating copper glycinate (II) after cooling with ethyl alcohol (II ), filtering the mixture, washing the complex with petroleum ether, drying, add an oxidizing agent to the reaction mixture before heating, using acetophenone oxime, followed by em component ratio, wt.%:

glycine 3.35-6.00 copper 1.52-2.60 water (or dimethylformamide) 89.32-80.53 acetophenone oxime 5.81-10.87

The method is as follows. Finely ground glycine powder and powdered copper are placed in a round-bottom flask with a reflux condenser or water, water (or dimethylformamide) is added as a solvent. The suspension is heated to 80-90 ° C for 1.5 hours with constant stirring of the reaction mixture. The method is characterized in that acetophenonoxime is additionally introduced into the system. After boiling, the aqueous solution is filtered, the solution is partially evaporated at a temperature of 50 ° C, and after cooling, copper (II) glycinate is precipitated from the solution with ethyl alcohol. The blue-violet precipitate formed by boiling the mixture in dimethylformamide is separated from the hot solution by decantation. Then the precipitate is dissolved in a minimum amount of water and the mixture is filtered. The aqueous solution was partially evaporated and, after cooling, adding ethyl alcohol, precipitated reaction products, which were filtered off. The resulting copper (II) glycinate is purified either by recrystallization in a minimum amount of water, partially evaporating the solutions when heated to 50 ° C, or by reprecipitation from a minimum amount of water with ethyl alcohol. Then the complex is filtered off, washed 3 times with petroleum ether, kept in an oven at a temperature of 105 ° C for an hour and in a desiccator with anhydrous Na ₂ SO ₄ for a day. The method is carried out in the following ratio of components, wt.%:

glycine 3.35-6.00 copper 1.52-2.60 water (or dimethylformamide) 89.32-80.53 acetophenone oxime 5.81-10.87

The yield of the complex is 90%, 40-50% of copper goes into the oxidized state. Thus, acetophenone oxime promotes the transfer of copper to the oxidized state, but does not exhibit chelating ability and, without forming a complex compound with copper, does not have a competing effect on glycine. In this case, an increase in the yield of copper (II) glycinate occurs.

Thus, the addition of acetophenone oxime leads to a more effective interaction of copper with glycine, the process proceeds in a single step and allows one to obtain copper (II) glycinate with a higher yield.

Example 1 of the method. In a round bottom flask with a reflux condenser, finely ground glycine powder and powdered copper are placed, water and a twofold excess of acetophenone oxime are added, in the following ratio, wt.%:

glycine 5.52-6.47 copper 2,50-2,93 water (or dimethylformamide) 73.58-86.28 acetophenone oxime 18.40-4.32

The suspension with constant stirring is heated to 90 ° C for 2 hours. Then the solution is filtered off, partially evaporated at a temperature of 50 ° C and, after cooling, copper (II) glycinate is precipitated from the solution with ethyl alcohol, which is purified by reprecipitation of a minimum amount of water with ethyl alcohol. Then the complex is washed 3 times with petroleum ether, kept in an oven at a temperature of 105 ° C for an hour and in a desiccator with anhydrous Na ₂ SO ₄ for a day. In this case, 46% of copper goes into the oxidized state, the yield of copper (II) glycinate is 90-91%, that is, an increase in the amount of the oxidizing agent - acetophenone oxime and the reaction time of the components of the mixture does not significantly increase the yield of the complex.

Adding an oxidizing agent, acetophenone oxime, to the reaction mixture promotes a more efficient transition of copper into the complex and, as a result, increases the yield of copper (II) glycinate.

Thus, the method allows one-step with a fairly high yield to obtain copper (II) glycinate from copper powder and glycine without the use of aggressive media and strong oxidizing agents. The invention can be applied to obtain biologically active and feed additives. In this case, the problems of the assimilation of trace elements by organisms are eliminated, since copper is introduced in a pharmacologically active form, which reduces the toxicity of this metal.

Information sources

1. Novakovsky M.S. Laboratory work on the chemistry of complex compounds. - Kharkov: Because of Kharkov University. - 1972, p. 80.

2. Ogorodnikova NP, Starkova NN, Ryabukhin Yu.I. A direct method for the synthesis of complexes of copper (II) with amino acids in non-aqueous solvents. University News. Chemistry and chemical technology, 2009. - V. 52. - Issue 12. - S. 45-47.

Claims (1)

A method of producing copper (II) glycinate in the presence of acetophenone oxime, comprising heating finely ground glycine powder and powdered copper in water (or dimethylformamide) with constant stirring of the reaction mixture, decanting the precipitate, dissolving it, filtering the solution, partially evaporating it, and precipitating glycinate with ethanol after cooling copper (II), filtering the mixture, washing the complex with petroleum ether, drying, characterized in that an oxidizing agent is added to the reaction mixture before heating, The substance of which is used acetophenone oxime, in the following ratio of components, wt.%:
glycine 3.35-6.00 copper 1.52-2.60 water (or dimethylformamide) 89.32-80.53 acetophenone oxime 5.81-10.87