Method of production of lead tetraacetate

FIELD: chemical industry; methods of production of acetates.

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the method of production of lead tetraacetate. The method provides for realization of interaction of the red-lead with anhydrous acetic acid at the temperatures of 30-40°C with the subsequent separation of the target product not later than 3-5 hours after the termination of reaction. In the capacity of the dehydrating reagent is used the by-product of the interaction - lead diacetate, which forms the hydrated complex with water. The invention ensures production of lead tetraacetate equal to 70-75 % from the theoretical value. The technical result of the invention is simplification of the production process, improvement of the economic features.

EFFECT: the invention ensures simplification of the production process, improvement of the economic features.

1 ex

 

The present invention relates to the field of production of salts of acetic acid, in particular of the leads to compounds, which lead.

The leads to compounds, which lead is used as a mild and selective oxidizing agent in the synthesis of complex organic compounds, in particular drugs.

A known method of obtaining leads to compounds, which lead the interaction of red lead (Pb3O4with anhydrous acetic acid [Ber., 56, 1375 (1923)]. The interaction is usually described by the equation:

The process is carried out by powder minium small portions over 5-10 g to heated to 55-65°With acetic acid with constant stirring of the reaction mixture. Each new portion of minium add after the dissolution and disappearance of color from the previous one. After the interaction, the reaction mixture was cooled to room temperature, and the resulting product is filtered off from the reaction solution, washed with a small amount of acetic acid and recrystallized from heated to 50°With solution. According to the known method 600 g red lead get 300-350 g leads to compounds, which lead, which corresponds to the estimated yield of the target product 77-90% of theoretical. However, trying to reproduce the known method shows that under these conditions the greater part of the formed leads to compounds, which lead already in the course of the synthesis is hydrolyzed by reaction with water:

The result is a viscous black sludge consisting mainly of fine lead dioxide, and the real yield of the target product does not exceed 25% of theoretical.

Known more modern way of obtaining leads to compounds, which lead the interaction of red lead with acetic acid in the presence of acetic anhydride [Lyser, Mfisher, Reagents for organic synthesis, M., Peace., 1970, Vol.3, s; Organikum, M., Mir, 1979, Vol.2, s; inorganic synthesis Manual, Ed. by G. Brauer, M., Mir, 1985, Vol.3, s]. Acetic anhydride in this way fulfills the function of a dehydrating reagent, irreversibly binding reaction water:

Acetic anhydride is added in sufficient quantity to complete the dehydration reaction medium. This prevents the hydrolysis of the target product and enhance its real output to 70-75%. Technologically well-known method is carried out as described earlier similar - by red lead powder in small portions to heated to 55-65°With a mixture of acetic acid and acetic anhydride.

This known method of obtaining leads to compounds, which lead closest to the proposed invention for the purpose and technical nature and is selected as a prototype.

The lack of PR is the totype is used as the dehydrating reagent is expensive and scarce substances - acetic anhydride.

The problem solved by the invention, is an exception from the reaction mixture of acetic anhydride, resulting in the simplification and cheapening of the production process leads to compounds, which lead.

The problem is solved in that in the known method of obtaining leads to compounds, which lead, including the interaction of red lead with anhydrous acetic acid in the presence of a dehydrating reagent by heating and separation of sludge leads to compounds, which lead from the reaction solution, as the dehydrating reagent is used which is formed during the interaction of the diacetate of lead, the interaction process is carried out at a temperature of 30-40°and the Department of sludge leads to compounds, which lead from the reaction solution and the washing is carried out not later than 3-5 hours after the end of the interaction.

When carrying out the synthesis leads to compounds, which lead us found that the actual interaction between lead and acetic acid differs from the conventional reactions (1) and is accompanied by the formation of hydrated complex reaction between water and the diacetate of lead:

This set captures the reaction water, turning it into an inactive state and preventing the target product from hydrolysis. Thus the diacetate of lead performs in reacherous the th mixture function dehydrating reagent. However, the diacetate of lead retains this function only up to a temperature of 30-40°because they formed by hydrated complex is thermally unstable above this temperature appreciably decomposes, releasing water of crystallization. Complete decomposition of the complex occurs at a temperature of 70-75°C. Therefore, in accordance with the invention the process of interaction perform it at a temperature of 30-40°C.

The reaction mixture obtained in a known manner with acetic anhydride, does not contain water and can persist for a long time. In the reaction mixture obtained by the proposed method, water is present in the bound state in the form of a hydrated complex. During prolonged storage leads to compounds, which lead takes the water of crystallization of the complex and slowly hydrolyzed. Therefore, in the proposed method, the precipitate obtained product as soon as possible (no later than 3-5 hours) after the interaction is separated from the reaction solution containing hydrated complex. The selected residue is washed with anhydrous acetic acid and crystallized. For a valid period of time (3-5 hours) leads to compounds, which lead does not have time to either hydrolyzed in an appreciable degree, and the final yield of the desired product as in the known method is 70-75% of theoretical is O.

The proposed method is carried out by continuous powder red lead to anhydrous acetic acid. The process of interaction between them ectothermic, which leads to spontaneous heating of the reaction mixture, which depends on the speed of powder. So minium sprinkled with speed, providing heating the reaction mixture up to 30-40°during the whole process of their interaction. After the end of the process precipitate tetraacetate lead no later than 3-5 hours is separated from the reaction solution, washed his portion of anhydrous acetic acid and crystallized.

The interaction between lead and anhydrous acetic acid at a temperature of 30-40°and separating the resulting precipitate leads to compounds, which lead from the reaction solution no later than 3-5 hours after the interaction are essential features of the present invention. Conducting the process at a temperature of 30-40°allows you to use as a dehydrating reagent a by-product of the interaction - diacetate of lead and eliminated from the reaction mixture of acetic anhydride. Separating the formed precipitate leads to compounds, which lead from the reaction solution no later than 3-5 hours after the end of the interaction allows you to save the resulting product. Together, these significant prospect who signs provide leads to compounds, which lead to the same output as by a known method (70-75%), but without the use of acetic anhydride.

These characteristics are not known from available sources of scientific and technical information and are new, providing simplification and cheapening of the production process leads to compounds, which lead.

The following is a specific example of the invention.

Example.

In a three-neck glass flask of 3 l equipped with a mechanical stirrer, thermometer and a funnel for loading minium, fill in 2.2 l of anhydrous acetic acid. Then the flask is gradually sprinkled 900 g of red lead. The process begins at room temperature (20-25°C), while during the powder, it has improved and is kept in the range of 30-40°C. Under these conditions, the interaction process is completed within 1-1 .5 hours of education in the reaction mixture a pale pink precipitate of the desired product. This precipitate was separated from the reaction solution on a Buechner funnel with a paper filter and washed with a portion of anhydrous acetic acid (200-300 ml). Washed from hydrated complex precipitate back into the flask, poured to him, 0.6 l of anhydrous acetic acid and briefly heated to complete dissolution (80-90°). After the flask with a hot solution of warm and insert for slow cooling. The solution grow large, needle glassy crystals of Tetra is Zetta lead. These crystals are separated from mother liquor by filtration over a Buchner funnel and dried under vacuum to constant weight. Get 420 g leads to compounds, which lead. The yield of the target product is 72% of theoretical.

Thus, the invention provides for obtaining leads to compounds, which lead to the release of 70-75% without the use of expensive and scarce acetic anhydride.

The method for obtaining leads to compounds, which lead, including the interaction of red lead with anhydrous acetic acid in the presence of a dehydrating reagent at elevated temperature and separating the resulting precipitate leads to compounds, which lead from the reaction solution, characterized in that as the dehydrating reagent is used which is formed during the interaction of the diacetate of lead, the interaction process is carried out at a temperature of 30-40°and the formed precipitate leads to compounds, which lead is separated from the reaction solution no later than 3-5 h after the end of the interaction.



 

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2 ex

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13 ex

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The invention relates to the production of salts of acetic acid
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FIELD: organic chemistry, chemical technology.

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FIELD: chemical technology.

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3 cl, 2 tbl, 8 ex

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13 ex

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2 ex

FIELD: inorganic syntheses.

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2 ex

FIELD: inorganic syntheses.

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EFFECT: simplified technology and improved economical characteristics of process due to use of inexpensive oxidant.

2 ex

FIELD: chemical industry; methods of production of acetates.

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the method of production of lead tetraacetate. The method provides for realization of interaction of the red-lead with anhydrous acetic acid at the temperatures of 30-40°C with the subsequent separation of the target product not later than 3-5 hours after the termination of reaction. In the capacity of the dehydrating reagent is used the by-product of the interaction - lead diacetate, which forms the hydrated complex with water. The invention ensures production of lead tetraacetate equal to 70-75 % from the theoretical value. The technical result of the invention is simplification of the production process, improvement of the economic features.

EFFECT: the invention ensures simplification of the production process, improvement of the economic features.

1 ex

FIELD: chemical industry; methods of neutralization of the water combustible solutions of the acetic acids at the computerized batching-packing machine.

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the method neutralization of the acetic acid and its solutions at leakages and accidents. The method of neutralization of the water combustible solutions of the acetic acids at the computerized batching-packing production line provides for the treatment of the surface, on which there is a leakage of the acetic acid, with the powdery anhydrous sodium carbonate. The treatment of the spilled acetic acid is exercised till formation of the paste and the paste is left on the surface for a while. At the second and the subsequent leakage of the acetic acid on the tray and at formation of the liquid phase the place of the spill is treated with a sodium carbonate till formation of the paste with the purpose for binding the liquid phase. In the case the acetic acid spills on the surfaces located outside of the tray, the neutralization of the acetic acid is exercised by water till gaining the 25-30 % solution. The surface treatment with the powder of the sodium carbonate at the first spill is exercised at the following components ratio (in mass %): Na2CO3:CH3C00H = 1.6÷4.0:1. The invention ensures reduction of the wastes of the production process, allows to reduce emissionof CO2 and allows to diminish toxicity of the production process.

EFFECT: the invention ensures reduction of the wastes of the production process, reduction of emissionof CO2 and reduction toxicity of the production process.

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for synthesis of platinum metal salts, in particular, palladium salts, namely, palladium (II) acetate. Method for synthesis of palladium (II) acetate involves dissolving metallic palladium in concentrated nitric acid, filtering and evaporation of palladium nitrate solution, its treatment with glacial acetic acid, filtration of formed sediment and its treatment with acetic acid ethyl ester and glacial acetic acid for its conversion to palladium (II) acetate followed by heating the prepared suspension for 6 h. Method provides preparing palladium (II) acetate with high yield in monophase state and without impurities of insoluble polymeric palladium (II) acetate.

EFFECT: improved method of synthesis.

3 cl, 2 tbl, 21 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to technology for synthesis of acetic acid inorganic salts. Method involves interaction of metallic manganese or its dioxide with acetic acid in the presence of oxidizing agent. Process is carried out in beaded mill of vertical type fitted with reflux cooling-condenser, high-speed blade mixer and glass beads as grinding agent loaded in the mass ratio to liquid phase = 1.5:1. Liquid phase represents glacial acid solution in ethylcellosolve, ethylene glycol, 1,4-dioxane, isoamyl alcohol and n-butyl alcohol as a solvent. The concentration of acid in liquid phase is 3.4-4 mole/kg. Then method involves loading iodine in the amount 0.025-0.070 mole/kg of liquid phase, metallic manganese and manganese dioxide in the mole ratio = 2:1 and taken in the amount 11.8% of liquid phase mass. The process starts at room temperature and carries out under self-heating condition to 30-38°C to practically complete consumption of manganese dioxide. Prepared salt suspension is separated from beads and unreacted manganese and filtered off. Filtrate is recovered to the repeated process and prepared precipitate is purified by recrystallization. Invention provides simplifying method using available raw and in low waste of the process.

EFFECT: improved method of synthesis.

3 cl, 9 ex

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