Method of obtaining palladium acetate

FIELD: chemistry.

SUBSTANCE: method of obtaining palladium acetate involves dissolving palladium metal in concentrated nitric acid, evaporation of the obtained solution and reaction with acetic acid, where the palladium nitrate solution after evaporation, before crystallisation of palladium (II) nitrate salt, is treated with nitrogen (II) oxide or a mixture of nitrogen (II) and (IV) oxides containing not more than 30% nitrogen (IV) oxide and acetic acid at temperature of the solution of 40-90°C with glacial acetic acid consumption of 1.5-2.5 l per kg of palladium in the solution and nitrogen (II) oxide or mixture of nitrogen (II) and (IV) oxides consumption of 1.0-2.0 m3 at normal conditions per 1 l of the initial palladium nitrate solution for 0.5-1.5 hours and the formed solution is heated in a nitrogen atmosphere at 110-140°C for not less than 2 hours with consumption of elementary nitrogen of approximately 30 m3 per 1 m3 of the formed solution.

EFFECT: obtaining palladium acetate in monophase state and avoding formation of impurities of insoluble palladium catena-poly-acetate.

3 cl, 35 ex, 1 tbl

 

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 an integral part of the catalyst or source of salt for other palladium salts and catalysts containing palladium.

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). 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 its 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 stabilization of anionic complexes of the type

[PD(CH3Soo)4]2-and [PD2(CH3Soo)6]2-that in aqueous solution of acetic acid is able to recover to the metal.

A known method of producing palladium(II) acetate by the interaction of palladium nitrate with acetic kislatalar palladium is produced by evaporation to wet salts diluted nitric acid solution of palladium (inorganic synthesis Manual. Ed. Gbauer. M.: Mir, 1985, volume 5, s). The disadvantage of this method is the duration of obtaining a solid palladium nitrate and the presence in its composition of oxide of palladium, are not completely soluble in acetic acid, which, ultimately, leads to contamination of the product with palladium oxide.

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. 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 presence of nitric acid or oxygen compounds of nitrogen), which promotes the formation of insoluble in acetic acid and organic solvents Catena-Poliform of palladium(II) acetate [PD(CH3Soo)2]n. This is shown in the patent process parameters (temperature of the reaction medium to 70-80°C, the molar amount of nitric acid 0.8-1.5 on the number of palladium, the amount of acetic acid in the range of 5-100% (wt.), preferably 20-50% (wt.), from the base amount of palladium), the formation of nitrite is of palladium acetate [PD 3(CH3Soo)5NO2].

A known method of producing palladium(II) acetate by reacting a dilute water solution of palladium nitrate with acetic acid (Patent of Russia №2333195, 10.09.2008). The disadvantage of this method is the presence of nitric acid and products of its decomposition, contributing to the dissolution of palladium acetate and nitrotyrosine that may lead to the selection nitrite acetate palladium compounds [Pd3(CH3COO)5NO2].

A known method of producing palladium acetate by precipitation with acetic acid from a solution of palladium nitrate nitrite acetate palladium compounds [Pd3(CH3COO)5NO2] and then its translation in palladium acetate [PD3(CH3Soo)6] by heating in acetic acid with the addition of ethyl acetate (Patent of Russia №2288214, 27.11.2006). The disadvantage of this method is the staging process and prolonged heating in acetic acid with the addition of ethyl acetate. This may result in partial recovery of palladium from appearance in the reaction solution of the product of decomposition of the ether - ethanol. Without additives ethyl acetate decomposition nitrite acetate palladium compounds is accompanied by partial formation of oxidative reagent is nitric acid, resulting in the reaction product Catena-Poliform is Zetta palladium [PD(CH 3Soo)2]n.

A known method of producing palladium acetate by reacting solution of palladium nitrate with acetic acid and ethyl ester, acetic acid (Patent of Russia №2333196,10.09.2008). This method is adopted for the prototype.

The disadvantage of this method is the intensive oxidation of acetate that is causing it dosed introduction. This causes increase in the duration of the process. However, due to the low boiling point of ethyl acetate and its ability to decomposition of acetic acid and ethanol is necessary to maintain the temperature of decomposition of the nitrates in the range of 70-90°C, which can lead to the selection of the intermediate nitrite-nitroso-acetate palladium compounds. Long-term warming of the solution with ethyl acetate may lead to partial recovery of palladium.

The technical result, which is aimed by the invention, is getting it in monophase state [PD3(CH3Soo)6] and reducing the duration of the process.

The specified technical result is achieved in that in a solution of palladium nitrate after evaporation prior to the crystallization of salt nitrate, palladium(II) when the temperature of the solution (40-90°C begin to skip nitric oxide(II) or a mixture of oxides of nitrogen(II) and (IV)the content of oxides of nitrogen(IV) not more than 30% and add glacial acetic acid with a flow rate of NO (1.0-2.0) m 3when N.U. 1 l of a solution of palladium nitrate containing palladium is not less than 500 g/l and free nitric acid not more than 200 g/l glacial acetic acid (1.5 to 2.5 liters per 1 kg of palladium in solution within (0.5-1.5) h and heating the resulting solution in an atmosphere of elemental nitrogen at a temperature of (110-140)°C for at least 2 hours with a nitrogen flow of about 30 m31 m3the resulting solution.

The essence of the method is that the synthesis of palladium(II) acetate carry out the recovery of palladium nitrate nitrogen oxide(II) to soluble in acetic acid nitrite compounds of palladium(II)that translate into palladium(II) acetate by heating in acetic acid. Nitric oxide(II) allows you to restore oxygen nitrogen compounds(V) and to eliminate the manifestations of their oxidative properties. The absence of an oxidant, prevents further heating of the solution education is not soluble in acetic acid and some organic solvents Catena-Poliform of palladium(II)acetate. When recovering the nitric oxide(II) nitric acid is reduced to nitrogen oxide(IV-II), which are removed from the reaction zone, while the nitric oxide(II) is oxidized to nitrogen oxide(IV), which is also removed from the reaction zone. Inert (nitrogen) atmosphere, which is the warming of the solution and removal of nitrogen oxides, it is necessary the ima to avoid oxidation of the oxygen compounds of nitrogen(II-IV) oxygen to oxygen nitrogen compounds(IV-V) and manifestations of their oxidative properties. The transmission of elementary nitrogen through the reaction solution also contributes to a more rapid removal of nitrogen oxides from a solution that makes the whole process more efficient.

In the course of the research it was established that the process of obtaining palladium(II) acetate recovery of palladium nitrate nitrogen oxide(II) in the presence of acetic acid and heating in an atmosphere of elemental nitrogen optimum conditions are:

- temperature interaction of nitric oxide(II) and acetic acid with a solution of palladium nitrate (40-90°C;

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

- consumption of nitric oxide(And) (1.0-2.0) m3when N.U. 1 l of a solution of palladium nitrate containing palladium is not less than 500 g/l and free nitric acid not more than 200 g/l;

- the content of oxides of nitrogen(IV) in a mixture of oxides of nitrogen (II) and (IV)passing through nitric-acetic acid solution of palladium, not more than 30%;

- the duration of the transmission through a solution of oxide of nitrogen(II) or a mixture of oxides of nitrogen(II) and (IV) in a solution of palladium nitrate (0.5-1.5) h;

- temperature heating of the solution after introduction of the mixture of nitric oxide(II) and inert gas (110-140)°C;

- duration of heating of the solution in an atmosphere of elemental nitrogen with (110-140)°C for at least 2 hours.

Increase the tempo of the atmospheric temperature interaction of nitric oxide(II) and acetic acid with a solution of palladium nitrate more than 90°C leads to an increase nitrosurea ability of oxides of nitrogen(II-IV) in solution, that eventually leads to the formation of low-soluble and resistant to the action of acetic acid nitrosamino acetate connection palladium [Pd2(NO)2(CH3COO)2]4that contaminates the target product. Reducing the temperature less than 40°C leads to a decrease of the reactivity of acetic acid and education polimorfnogo sediment nitrite palladium compounds of unknown composition, complete dissolution which in acetic acid it requires large quantities.

Consumption of added acetic acid less than 1.5 liters per 1 kg of palladium in the solution leads to the lack of acetic acid, which, ultimately, contributes to the formation of nitrite acetate palladium compounds [PD3(CH3Soo)5NO2] and the contamination of the main product. The increase in consumption of added acetic acid more than 2.5 liters per 1 kg of palladium in the solution leads to a reduction of yield of palladium(II) acetate due to its dissolution in excess of acetic acid

Consumption of nitric oxide(II) less than 1.0 m3(N.U.) 1 l of a solution of palladium nitrate leads to incomplete recovery of the oxygen compounds of nitrogen(V), the manifestation of oxidative properties, which upon further increase of temperature leads to the formation of insoluble in acetic acid Catena-polyacetate of palladium, which, in the end, zag is jasneet product. The increase in the consumption of nitric oxide(II) more than 2.0 m31 l of a solution of palladium nitrate leads to the emergence of surpluses in the future may lead to the formation of [PD3(CH3Soo)5NO2], which also contaminates the product, or requires a longer duration of heating of the solution.

The increase in the content of nitrogen oxides(IV) in the gas mixture of nitrogen oxides (II) and (IV) more than 30% leads to the manifestation of oxidative properties of the solution, which further leads to the formation of insoluble in acetic acid Catena-Poliform of palladium acetate and contamination of the product. The use of pure nitrogen oxide(II) leads to a more expensive process due to the higher value of the net or NO additional costs for cleaning.

Reducing the duration of transmission of nitric oxide(II) through the reaction solution is less than 0.5 hours can lead to incomplete recovery of the oxygen compounds of nitrogen(V), the manifestation of oxidative properties, which upon further increase of temperature leads to the formation of insoluble in acetic acid Catena-polyacetate palladium, which eventually contaminates the product. The increase in the length of the input of nitrogen oxide(II) in the reaction solution over 1.5 hours leads to an increase in the duration of the whole process, which reduces its effectiveness.

Decrease the temperature begins heating the solution after input of nitrogen oxide(II) less than 110°C leads to incomplete decomposition nitrite acetate compounds of palladium, which leads to crystallization [PD3(CH3Soo)5NO2] and the contamination of the main product. The temperature increase of the heating of the solution after input of nitrogen oxide(II) more than 140°C leads to the boiling solution and may be accompanied by the release of solution from the reactor.

Reduction of duration of heating of the solution after input of nitrogen oxide(II) less than 2 hours leads to incomplete decomposition nitrite acetate compounds of palladium, which leads to crystallization [PD3(CH3Soo)5NO2] and the contamination of the main product. The increased duration of the heating of the solution after input of nitrogen oxide(II) more than 2 hours leads to an increase in the total duration of the process, which reduces its effectiveness.

Examples of the method

As the initial product for experiments No. 1-35 (table) 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 the solution of 650 g/l, free of nitric acid and 170 g/l

Example 1

In a closed reactor with heating, mixing system, feeding system, ozonation gases through the reaction solution and cooling system and vapor recovery have introduced a certain amount of the prepared solution of nitric the number of palladium. The solution was heated to the required temperature and through the solution with stirring missed a mixture of oxides of nitrogen (II) and (IV) the content of oxides of nitrogen(IV) not more than 30% with the required flow rate of nitrogen oxide(II). After turning the system ozonation of oxides of nitrogen was introduced glacial acetic acid. Heating the resulting solution, and the transmission of oxides of nitrogen were within the required time. Then raised the temperature of the solution, turn off the supply of nitrogen oxide(II) and the solution was kept under stirring necessary duration. Next, turn off the heating and the solution was cooled to room temperature. Then turn off the flow of nitrogen, the resulting palladium acetate was removed by filtration, were unloaded on a baking sheet and dried in air at 120°C for four hours. The precipitate of palladium acetate were weighed, and analyzed for the content of palladium and determine the phase composition. The mother liquor is sent to regeneration. These experiments are shown in table (experiments No. 1-34).

Example 2

The process was carried out according to example 1, but the precipitate of palladium acetate was not separated from the mother liquor. While maintaining suspension of the product at 120°C under vacuum and without passing nitrogen for a further three hours, the solution was evaporated until complete evaporation of the solution and obtain the dry salt. This has increased the product yield, novelities the duration of the process (table, experience No. 35),

As seen from the above examples, the use of the proposed method allows to obtain a palladium(II) acetate with high yield in monophase state and to exclude the appearance of impurities insoluble Catena-Poliform of palladium(II)acetate.

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 solution of nitric acid, palladium after evaporation, prior to the crystallization of salt nitrate, palladium (II), is treated with nitric oxide (II) or a mixture of oxides of nitrogen (II) and (IV) the content of oxides of nitrogen (IV) not more than 30% and acetic acid at a solution temperature of 40-90°C with a flow rate of 1.5 to 2.5 liters of glacial acetic acid per 1 kg of palladium in solution and flow nitric oxide (II) or a mixture of oxides of nitrogen (II) and (IV) 1,0-2,0 m3when N.U. 1 l of the starting solution of nitric acid, palladium within 0.5-1.5 h and heating the resulting solution in a nitrogen atmosphere at a temperature of 110-140°C for at least 2 h with a flow rate of elemental nitrogen is about 30 m per 1 m of the resulting solution.

2. The method according to claim 1, characterized in that the evaporation of a solution of nitric acid, palladium carried out until the content of palladium is not less than 500 g/l and free nitric acid is not b is over 200 g/L.

3. The method according to claim 1, characterized in that the heating of the suspension of palladium acetate in solution at 110-140°C lead to the receipt of dry salts.



 

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3 cl, 2 tbl, 21 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 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: inorganic syntheses.

SUBSTANCE: 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.

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

2 ex

FIELD: chemistry.

SUBSTANCE: method involves reacting oxides of rare-earth elements (REE) with α, α'-branched monobasic carboxylic acids with 8-20 carbon atoms while stirring at high temperature, as well as their mixtures in the presence of water with molar ratio of water to the rare-earth element equal to 1-3:1, with subsequent cooling, addition of solvent and azeotropic drying of the obtained solutions of carboxylates of rare-earth elements through distillation of the azeotropic solvent-water mixture, where the process is carried out while heating to 100°C and further at a rate of 10°C per hour to 150°C, with removal of the bulk of water during synthesis with a stream of inert gas fed to the bottom of the reactor and bubbled through the reaction mixture, without the stage of elutriation from unreacted oxides of rare-earth elements. The proposed method combines high output and purity of the product with simplification of the technique with minimal loss of reagents and minimal consumption of solvent.

EFFECT: obtaining carboxylates of rare-earth elements which are not prone to oligomerisation during azeotropic drying of their solutions and storage, and catalysts based on said compounds can be prepared with or without cooling and have high activity.

8 ex

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