Method for obtaining palladium acetate

IPC classes for russian patent Method for obtaining palladium acetate (RU 2333195):

C07F15 - Compounds containing elements of the 8th Group of the Periodic System

C07C51/41 - Preparation of salts of carboxylic acids by conversion of the acids or their salts into salts with the same carboxylic acid part (preparation of soap C11D)

C01G55 - Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum

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Basic iron (iii) acetate producing method / 2314285

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Method of production of iron (iii) complex with three anions of salicylic acid / 2304575

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Water-soluble iron-carbohydrate complexes, method for their preparing, medicinal agent, using / 2303039

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Method of zirconium carboxylate production / 2332398

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Basic iron (iii) acetate producing method / 2314285

Method for preparing manganese (ii) acetate / 2294921

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.

Method for preparing palladium acetate / 2288214

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.

Method of neutralization of the water combustible solutions of the acetic acid at the automated batching-packing machine / 2286307

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.

Method of production of lead tetraacetate / 2277530

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.

Ferrous acetate preparation method / 2269509

Method consists in that iron powder is oxidized in acetic acid/acetic anhydride (4%) medium with air oxygen bubbled through the medium, while maintaining iron-to-acetic acid molar ratio 5:1 and temperature 17-25°C. Reaction mixture is thoroughly stirred with blade stirrer at speed of rotation 720-1440 rpm until reaction mixture accumulates 0.75-0.96 mol/kg ferric salt. Thereafter, air is replaced by nitrogen and 4% acetic anhydride based on initially charged acetic acid is added, temperature is raised to 35-40°C, and iron is oxidized with ferric salt until full consumption of the latter. Resulting snow-white ferrous acetate suspension is separated from unreacted iron, filtered off, and dried. All above operations are carried out under a nitrogen atmosphere. Filtrate, which is saturated ferric acetate solution in acetic acid/acetic anhydride mixture, is recycled to reactor to be reprocessed or it is used according another destination.

Ferrous acetate preparation method / 2269508

Ferric acetate is prepared by interaction of metallic iron with acetic acid in presence of an oxidant. Process is carried out at ambient temperature in acetic acid/acetic anhydride medium (weight ratio 5:1) under nitrogen atmosphere. Molar ratio acetic acid/iron/basic ferric acetate is maintained the following: 10:8:1. Reaction mixture is thoroughly stirred with high-speed blade stirrer or shaken at shaking frequency 2 Hz. When consumption of basic ferric acetate is completed, suspension of ferrous acetate is separated by filtration from unreacted iron powder. Precipitate is dried and filtrate returned into the process.

Basic ferric acetate preparation method / 2268874

Implementation of the method comprises contacting iron in the form of iron powder or iron sidewall adjacent to a body with glacial acetic acid and air oxygen at 17-25°C and vigorous stirring effected by high-speed blade-type mechanical stirrer. Initial acetic acid-to-iron molar ratio is (224÷274):100. Acetic anhydride additive is preferably introduced in amount of 2% based on the initial concentration of acetic acid. When concentration of ferric salt in the mixture reaches 2.70-3.51 mole/kg, stirring is stopped and heavy unreacted iron particles are allowed to settle/ Major mass of product suspension is filtered off and thus obtained basic ferric acetate precipitate is dried. Filtrate, which is saturated acetic acid solution of basic ferric acetate, is returned into reactor to be reprocessed. Yield of desired product achieves 99.2-99.3%.

Zinc and aliphatic halogen-carboxylic acid salts for treatment of skin neoplasm and visible mucosa tissues / 2261243

Invention relates to zinc and aliphatic halogen-carboxylic acid salts that can be used in treatment of benign neoplasms of skin and visible mucosa tissues. Invention proposes the following formula of zinc and aliphatic halogen-carboxylic acid salts: (1): wherein R means -CHal₃, -CHHal₂, -CH₂Hal and (2): wherein R' means Alk, hydrogen atom (H); R'' means Hal; R' means Alk; R'' means H, Alk wherein in these formulae halogen atom can be represented by fluorine atom (F), chlorine atom (Cl), bromine atom (Br) or iodine atom (J). Invention provides the development of original preparation used in treatment of benign neoplasms of skin and visible mucosa tissues with low toxicity, rapid effect, expressed therapeutic effect and eliciting good tolerance, absence of complications in treatment, healing without formation of scar tissue. The development of the preparation provides expanding assortment of agents used in treatment of such diseases.

Method of zirconium carboxylate production / 2332398

FIELD: chemistry.

SUBSTANCE: invention concerns platinum-group metal salt synthesis, particularly of palladium salts, namely palladium (II) acetate applied as catalyst or for obtaining basic salt for production of other palladium salts. The method for obtaining palladium acetate involves dissolution of metal palladium in concentrated nitric acid, filtration and evaporation of palladium nitrate solution and reaction with acetic acid, where after evaporation but prior to palladium (II) nitrate crystallisation the palladium nitrate solution is processed by distilled water in the volume of (2-5) l per 1 kg of palladium in the initial nitrate solution, then by acetic acid diluted with water, with acid concentration of (30-70)% and volume of (1.5-2.5) l of acetic acid per 1 kg of palladium in the initial nitrate solution, the resulting solution being matured for at least 8 hours at (15-40)°C.

EFFECT: streamlined method for obtaining palladium (II) acetate and its synthesis in monophase condition without admixture of insoluble polymeric palladium (II) acetate and palladium (II) nitritoacetate.

2 cl, 1 tbl, 1 ex

The invention relates to the field of chemistry of the platinum metals, in particular the synthesis of compounds of palladium, namely the synthesis of palladium acetate, used as a catalyst, for example, to obtain a vinyl acetate or source of salt for other palladium salts, for example, to obtain palladium acetylacetonate.

A known method of producing palladium(II) acetate by dissolving palladium oxide in acetic acid. The palladium oxide is produced from palladium hydroxide deposited from chloride solution of palladium sodium hydroxide (Korea Patent No. KR 8904783, 1989). The disadvantage of this method is incomplete dissolution of palladium oxide in acetic acid, which requires additional filter operations. While palladium hydroxide obtained by precipitation with alkali, requires special allocation method.

A known method of producing palladium acetate by dissolving palladium mobiles in a mixture of glacial acetic acid and concentrated nitric acid in an inert atmosphere (Japan Patent No. JP 61047440, 1986). The disadvantage of this method is the need for the presence of an excess of palladium mobiles throughout the process, before crystallization of the product requires filtering solution from the mob. No excess palladium mobile leads to the formation of oxidative environment in solution (due to the Pris the effects of nitric acid or oxygen compounds of nitrogen), what contributes to the formation of insoluble in acetic acid and organic solvents polymeric palladium(II) acetate [Pd(CH₃Soo)₂]_n.

A known method of producing palladium(II) acetate by reacting one stripped off nitric acid solution of palladium with acetic acid at room temperature, filtration of the resulting precipitate and heating it in a mixture of acetic acid and ethyl ester of acetic acid and then heating in acetic acid (Patent of Russia №2288214). The disadvantage of this method is the staging process of obtaining palladium(II)acetate. Intermediate stage of the process is the selection of nitriloacetate palladium(II) [Pd₃(CH₃Soo)₅NO₂], selecting which inevitably presence of nitric acid that helps dissolve nitriloacetate palladium(II). The process of translation nitriloacetate palladium(II) palladium(II) acetate [Pd₃(CH₃Soo)₆] is characterized by the duration and requires a high temperature. In such conditions, the formation of nitrogen oxides, which possess oxidative capacity and catalyze the transfer of a soluble palladium(II) acetate [Pd₃(CH₃COO)₆] insoluble palladium(II) acetate [Pd(CH₃COO)₂]_n. To suppress the oxidative capacity of islow nitrogen in solution is injected ethyl ester acetic acid, lack of which is the interaction of water with the formation of ethyl alcohol, which is able to recover the palladium(II) acetate to palladium metal.

A known method of producing palladium(II) acetate by reacting a hydrated oxide of palladium(II) with acetic acid. Hydrated oxide of palladium(II) obtained by hydrolysis of a nitric acid solution of palladium nitrate aqueous solution of NaOH and repeated decantation formed by sediment (U.S. Patent No. 3318891, 1967). This method is adopted for the prototype.

The disadvantage of this method is incomplete dissolution of hydrated oxide of palladium(II) in acetic acid and the staging of the whole process, which complicates the implementation. Use a hydrated oxide of palladium(II) contaminated with alkali, which cannot be completely removed by repeated decantation. The presence of sodium acetate in acetic acid solution of palladium acetate leads to the formation of anionic complexes of the type [Pd(CH₃Soo)₄]^2-and [Pd₂(CH₃Soo)₆]^2-that in aqueous acetic acid solution capable when heated to recover to the metal.

The technical result, which directed the present invention is to simplify the process of obtaining palladium(II) acetate and getting it in monophase status is anyi [Pd ₃(CH₃Soo)₆] without additives polymeric palladium acetate(II) Catena-poly-[Pd(CH₃Soo)₂]_nand nitriloacetate palladium(II) [Pd₃(CH₃COO)₅NO₂].

The specified technical result is achieved by the fact that the nitric acid solution of palladium after evaporation, prior to the crystallization of salt nitrate, palladium(II), treated with distilled water and then diluted with water (30-70%) acetic acid at a temperature (15-40)°With consumption (2-5) l distilled water to 1 l prepared nitrate solution and (1.5 to 2.5 liters of acetic acid per 1 kg of palladium in solution.

The essence of the method is that the synthesis of palladium(II) acetate carry replacement nitrogroup in the complex of palladium nitrate to acetate. Since the reaction produces nitric acid, to inhibit nitration in the water solution is introduced. When this water is also needed to inhibit nitrosation. Because the original nitric acid solution of palladium was obtained by dissolving palladium metal in nitric acid, then the solution contains dissolved nitrogen oxides that contribute to nitrotyrosine. The process without the presence of water is characterized by the formation nitrosated palladium acetate - nitriloacetate palladium [Pd₃(CH₃Soo)₅NO₂].

the course of the research it is established, for carrying out the process of obtaining acetate, palladium(II) from dilute nitric acid solution of palladium substitution kompleksirovanii nitrogroup on acetate the introduction of acetic acid, the optimum conditions are:

- the temperature of the dilute nitric acid solution of palladium distilled water of not more than 40°C;

- consumption of distilled water to 1 l the original prepared nitric acid solution (2-5) l;

- dilution water acetic acid to its mass content (30-70%);

- temperature interaction of dilute acetic acid with nitric acid solution of palladium (15-40)°C;

- consumption of glacial acetic acid per 1 kg of palladium nitrate solution (1.5 to 2.5) l;

- the duration of the crystallization process of palladium(II) acetate with stirring the reaction solution is not less than 8 hours

The temperature of the dilution one stripped off nitric acid solution, more than 40°leads to partial hydrolysis of a complex of palladium nitrate, which, ultimately, leads to the admixture of palladium hydroxide.

Consumption of added water is less than 2 l per 1 l of original prepared nitric acid solution of palladium leads to the manifestation in solution reactions, nitration and nitrosation, which, ultimately, leads to the appearance of impurity polymer acetate pall is palladium(II) or nitriloacetate palladium(II). The increase in consumption of added distilled water for more than 5 l per 1 l of original prepared nitric acid solution of palladium increases the number of reaction solution, which requires a larger volume of the reactor, as well as to increase the solubility of the product.

Increasing dilution water glacial acetic acid to its mass content of less than 30% leads to decrease its reactivity, which, ultimately, leads to a decrease in product yield. The decrease in the dilution water glacial acetic acid to its mass content of more than 70% can lead to processes of nitrosation, which, ultimately, leads to the selection nitriloacetate complex of palladium or contamination of the main product.

The temperature increase of the input of dilute acetic acid in the nitric acid solution of palladium over 40°leads to processes of nitrosation or nitration than due to the appearance of impurity nitriloacetate or acetate polymer complex of palladium.

Consumption of added acetic acid less than 1.5 liters per 1 kg of palladium nitrate solution leads to its disadvantage and incomplete replacement of the entire palladium nitrate. The increase in consumption of added acetic acid more than 2.5 liters per 1 kg of palladium nitrate solution leads to an increase in the number of solution and dissolving therein the product.

Reducing the duration of the process of substitution of less than 8 h leads to incomplete crystallization of the product.

The temperature increase of the interaction of water and acetic acid, with nitric acid solution of palladium over 40°leads to the manifestation in solution reactions, nitration and nitrosation, which, ultimately, leads to the appearance of the polymer admixture of palladium(II) acetate or nitriloacetate palladium(II). Reducing the temperature less than 15°slows down the exchange interaction, which increases the duration of the process.

Examples of the method

As the initial product for experiments No. 1-28 (table 1) to obtain a palladium(II) acetate was prepared solution of palladium nitrate by dissolving palladium metal in nitric acid and evaporation. The content of palladium in a solution of 500 g/l, free of nitric acid 200 g/l

Example 1

In a certain amount of cooked nitric acid solution of palladium was added the calculated amount of distilled water and then the solution is diluted with water acetic acid and stirred. The precipitate of palladium(II) acetate was removed by filtration, washed with distilled water, were unloaded on a baking sheet and dried at 40°C for 24 hours. The residue was weighed, and analyzed for palladium content was determined phase SOS is AB. The mother liquor is sent to regeneration. These experiments are shown in table 1.

As seen from the above examples, the use of the proposed method allows to obtain a palladium(II) acetate in monophase state and to exclude the appearance of impurities insoluble polymeric palladium(II) acetate and nitriloacetate compounds of palladium(II).

1. The method of producing palladium acetate, including the dissolution of metallic palladium in concentrated nitric acid, evaporation of the resulting solution and carrying out the reaction with acetic acid, characterized in that the nitric acid solution of palladium after evaporation, prior to the crystallization of salt nitrate, palladium(II), treated with distilled water in volume (2-5) liters per 1 kg of palladium in the original nitrate solution, then diluted with water, acetic acid (30-70%) with flow rate of 1.5 to 2.5 liters of acetic acid per 1 kg of palladium in the original nitrate solution and the resulting solution stand at least 8 hours at a temperature of (15-40)°C.

2. The method according to claim 1, characterized in that the process of evaporation of nitric acid solution of palladium carried out until the content of palladium 500 g/l and free nitric acid 200 g/l