Method for obtaining palladium acetate

IPC classes for russian patent Method for obtaining palladium acetate (RU 2333196):

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

Another patents in same IPC classes:

Method for obtaining palladium acetate / 2333195

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.

Method obtaining pyrophosphate tetrammine platinum (ii) / 2331585

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Method of obtaining cis-diammino(1,1-cyclobutanedicarboxylate)platinum(ii) / 2330039

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Bis-benzizo selenium zolonyl derivatives with antitumor, antiinflammatory and antithrombotic activity and their application / 2324688

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Basic iron (iii) acetate producing method / 2314285

Method is realized by relation of metallic iron with acetic acid at presence of oxidizing agent; using molecular iodine, iron oxides such as Fe₂O_3, Fe₃O₄ and oxygen of air as oxidizing agent for converting impurity of iron (II) acetate to basic iron (III) acetate. Process is performed in beads mill at temperature 80°Cand at mass relation of liquid charge and glass beads 1 : 1. Iron is used in the form of shell abutted to lateral surface of reactor housing. Initial molar relation of iron oxide and iodine is 10 : 1. Molar relation of acetic acid, its anhydride and iron oxide is in range 100 : (2 - 5.99) : (2 - 2.5). In time moment of practically complete consumption of iron oxide, solid phase of reaction mixture is taken off by filtering. Simultaneously consumed reagents are replenished and filtrate is returned to reactor for repeating process. Number of processes to be repeated is no more than 5. At second stage residues of iron (II) salt are after-oxidized to basic iron (III) acetate due to drying up taken off solid phase of product in filter by means of blowing air at environmental temperature. Preferably, hematite, γ-oxide or minimum is used as Fe₂ O ₃ and magnetite and Fe₃O₄ x 4H₂Ois used asFe₃ O_4.

Catalyst for production of acrylic acid esters according to metathesis reaction of dialkyl malates (variants) and a catalytic composition based thereof / 2311231

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Method for production of cis-dichloroamminisopropylamine platinum(ii) / 2309158

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Methods for preparing ferric complexes with one salicylic acid anion / 2307118

Invention relates to technology of complexes of iron with salicylic acid suitable for use in a variety of technical areas and in medicine. Title complex is obtained via interaction of metal with acid using air oxygen as oxidant. Salicylic acid is used in butyl acetate or n-butyl alcohol solution with dissolved molecular iodine or potassium iodide. Iron is provided in the form of steel or cast iron shell, shaft, and blade of mechanical mixer as well as, agitated by the mixer, reduced iron powder fractions, broken cast iron or broken steel cuttings, cast iron or steel filings. Process is carried out at stirring with high-speed mechanical stirrer and air bubbling allowing self-heating of reaction mixture to 70-80°C until 1.72-1.85 mole/kg iron compounds is accumulated in reaction mixture in the form of suspension, whereupon mixing is stopped. Suspension is freed of unreacted fine iron and/or alloy(s) thereof and subjected to hot filtration, Filtrate is warmed to eliminate precipitated solid phase and then slowly cooled to ambient temperature. Precipitated solid phase is filtered off, dried, and recrystallized, while filtrate is recycled.

Method for preparing octa-4,5-carboxyphthalocyanine cobalt sodium salt / 2304582

Invention relates to an improved method for synthesis of octa-4,5-carboxyphthalocyanine cobalt sodium salt, or 2,3,9,10,16,17,23,24-octacarboxylic acid of phthalocyanine cobalt (terephthal) of the formula (I) . Terephthal is a synthetic preparation used in catalytic ("dark") therapy of cancer based on generation of oxygen reactive species in tumor directly by chemical manner and in combination with ascorbic acid being without using the physical effect. Method for preparing octa-4,5-carboxyphthalocyanine cobalt sodium salt involves melting pyromellitic acid dianhydride with cobalt salt in the presence of urea followed by alkaline hydrolysis of prepared octa-4,5-carboxyphthalcyanine cobalt tetraimide. Salt formed after hydrolysis is purified from impurities, in particularly, from oligomeric compounds by column chromatography method on aluminum oxide, following precipitation of octacarboxylic acid, its, its washing out, concentrating and purifying from residual inorganic salts by washing out with distilled water and by neutralization with sodium hydroxide aqueous solution also, treatment with apyrogenic activated carbon, filtration and drying the end substance. Purification of octa-4,5-carboxyphthalocyanine cobalt from residual inorganic salt is carried out preferably by electrodialysis method after its partial neutralization to pH 5.2-5.5 at current density 0.15-0.25 A/dm², temperature 20-35°C and the concentration 1.5-3.0% followed by complete neutralization to pH 8.7, treatment of obtained octacarboxy-PcCo salt solution with activated carbon, filtration and drying filtrate in a spray drier. Proposed method provides preparing octa-4,5-carbocyphthalocyanine cobalt salt of high purity degree and free of oligomeric compounds and residual chlorides.

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

Proposed iron (III) complex with three anions of salicylic acid is produced due to interaction of iron and its alloys with salicylic acid dissolved in dimethyl formamide in vertical bead-type mill provided with high-speed mechanical blade-type agitator at bubbling of air and spontaneous heating of reaction mixture to 80-90C. Iron is presented in form of steel or cast-iron ferrule over entire height of bead-type mill, steel shaft and blade of mechanical agitator, as well as in form of iron powder, fraction of broken cast iron, broken steel chips or cast-iron shot. Process is completed at accumulation of iron salts in reaction mixture of 1.12-1.30 mole/kg; 95% of these salts are in target compounds of iron (III). Hot suspension is filtered immediately and filtrate is cooled down for crystallization of main mass of iron (III) complex. Precipitated product is filtered and is directed for re-crystallization, if necessary. Filtrate is returned for repeated process.

Method for obtaining palladium acetate / 2333195

Method of zirconium carboxylate production / 2332398

Invention relates to chemistry of derivative transition metal and can be used in chemical industry while producing transition metal carboxylate and refers to improved method of zirconium carboxylate production through interreacting of zirconium chloride with carboxylate derivatives of general formula RCOOM, where R-linear and branched alkyl C_nH_2n+1 or non-saturated acid residue, where n=0-16, and M - proton or cation of alcali metal, in which alkali acid of aliphatic or non-saturated acids are used as RCOOM compounds, interacting of zirconium chloride with the compounds leads to solvent absence in solid with mechanical activation at mole ratio ZrCl₄: RCOOM within 1<m<4.5, where m is integral and broken number with the following extraction of derived zirconium carboxylate with an organic solvent.

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%.

Method for obtaining palladium acetate / 2333195

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 to produce other palladium salts. The method for obtaining palladium acetate involves dissolution of metal palladium in concentrated nitric acid, evaporation of obtained solution and reaction with acetic acid, where, after evaporation but prior to palladium (II) nitrate crystallisation, the palladium nitrate solution is processed by a mix of acetic acid, acetic acid ethyl alcohol and acetic anhydride at (60-80)°C with (2.0-3.0) l of ice-cold acetic acid, (0.8-1.0) l of ethylacetate and (0.4-0.6) l of acetic anhydride per 1 kg of dissolved palladium for at least 1 hour, the resulting solution is heated at (90-110)°C for at least 3 hours and at (135-145)°C for at least 6 hours.

EFFECT: obtaining high yield of monophase palladium (II) acetate without admixture of insoluble polymeric palladium (II) acetate and palladium (II) nitritoacetate.

3 cl, 1 tbl, 3 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 retrieve vinyl acetate or source of salt for other palladium salts, for example to obtain palladium acetylacetonate.

A known method of producing palladium(II) acetate [Pd₃(CH₃Soo)₆] 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. KR8904783, 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 a special way of separating or filtering.

A known method of producing palladium(II) acetate by dissolving palladium mobiles in a mixture of glacial acetic acid and concentrated nitric acid in an inert atmosphere (Japan Patent No. JP61047440, 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 images is of oxidative environment in solution (due to the presence of nitric acid or oxygen compounds of nitrogen), what contributes to the formation of insoluble in acetic acid and organic solvents polymeric palladium acetate(II) Catena-poly-[Pd(CH₃Soo)₂]_n.

A known method of producing palladium(II) acetate by the interaction of palladium nitrate with acetic acid. The palladium nitrate is produced by evaporation to wet salts diluted nitric acid solution of palladium (inorganic synthesis Manual / edited Gbauer. M.: Mir, 1985. V.5, s). The disadvantage of this method is the presence of nitric acid and products of its decomposition in acetic acid, contributing to the dissolution of palladium(II) acetate and reduced product yield, as well as the formation of insoluble in acetic acid polymeric palladium(II)acetate.

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). This method is adopted for the prototype.

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(CH₃(COO)₅NO₂ ]during the formation of which is inevitably the 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 oxygen compounds of nitrogen with oxidative capacity and which catalysts translation soluble palladium(II) acetate [Pd₃(CH₃Soo)₆] insoluble palladium(II) acetate [Pd(CH₃Soo)₂]_n. To suppress the oxidative capacity of the nitrogen oxides in the solution is injected ethyl ester acetic acid, lack of which is interaction with water during prolonged heating in the presence of palladium compounds. The result is ethyl alcohol, which is able to recover the palladium(II) acetate to palladium metal.

The technical result, which is aimed by the invention, is to increase the output of palladium(II) acetate and getting it in monophase state [Pd₃(CH₃Soo)₆] without admixture of polymeric palladium acetate(II) Catena-poly-[Pd(CH₃Soo)₂]_nand nitriloacetate palladium(II) [Pd₃(CH₃COO)₅NO₂].

Set the initial technical result is achieved by what a nitric acid solution of palladium after evaporation, prior to the crystallization of salt nitrate, palladium(II), is treated with a mixture of glacial acetic acid, ethyl ester acetic acid (acetate) and acetic anhydride at a temperature (60-80)°With consumption (2,0-3,0) l acetic acid, (0,8-1,0) l ethyl acetate and (0,4-0,6) l acetic anhydride per 1 kg of palladium in solution, of not less than 1 h, and heating the resulting solution at a temperature (90-110)°With not less than 3 h and when (135-145)°With not less than 6 hours

The essence of the method is that the synthesis of palladium(II) acetate carry out the decomposition of nitrogroup and nitric acid by ethyl acetate. While nitric acid and comprehensively linked nitrogroup go into oxygen nitrogen compounds with lower oxidation state. Palladium forms a number of intermediate nitrite-nitroso-acetate compounds, which upon further heating become soluble treatery the palladium(II)acetate. In this process it is possible to avoid the formation of insoluble polymeric palladium(II)acetate. The negative effect of ethylacetate, due to interaction with water and the formation of ethanol, which regenerates the palladium(II) acetate to metal, does not manifest adding acetic anhydride, which reduces the activity of water. In this case the presence of acetic anhydride increases Rea the operating ability of ethyl acetate and this has a positive effect on the decomposition of nitric acid solution of palladium when translating it into acetate without isolation of intermediate nitrite-nitroso-acetate palladium compounds. While there is a decrease in the temperature of the transition nitriloacetate palladium(II) [Pd₃(CH₃COO)₅NO₂] palladium(II) acetate [Pd₃(CH₃COO)₆].

To reduce the duration of the process it is expedient to apply purging the reaction solution with an inert gas such as nitrogen. A faster removal of the decomposition products of nitric acid and nitrogroup - oxides of nitrogen, which reduces their nitrogenous capability.

In the course of the research it was established that the process of obtaining acetate, palladium(II) recovering nitric acid solution of palladium acetate optimal conditions are:

- temperature interaction of a mixture of acetic acid, ethyl acetate and acetic anhydride with nitric acid solution of palladium (60-80)°C;

- consumption of glacial acetic acid (2.0 to 3.0) liters per 1 kg of palladium nitrate solution;

- consumption of ethyl acetate (0,8-1,0) liters per 1 kg of palladium nitrate solution;

- consumption of acetic anhydride (0.4 to 0.6) liters per 1 kg of palladium nitrate solution;

- the duration of the input mixture of ethyl acetate, acetic acid and acetic anhydride in the nitric acid solution of palladium is not less than 1 h;

- temperature heating of the solution after introduction of the mixture of acetic acid, ethyl acetate and acetic anhydride (90-110)°C;

- duration of heating of the solution at (90-110)°With not less than 3 hours;

- the temperature of the final heating (135-145)°C;

- duration of heating at (135-145)°With not less than 6 hours;

the consumption of nitrogen by injecting the reaction solution for faster removal of oxides of nitrogen (20-40) m³1 m³solution.

The temperature increase of the interaction of a mixture of acetic acid, ethyl acetate and acetic anhydride with nitric acid solution of palladium over 80°leads to strong evaporation of ethyl acetate, which further leads to its disadvantage and, as a consequence, obtaining a product with an admixture of polymeric palladium(II)acetate. Reducing the temperature below 60°leads to the appearance of an induction period of interaction, which increases the duration of the process.

Reducing the consumption of acetic acid of less than 2.0 liters per 1 kg of palladium nitrate solution leads to incomplete destruction of the intermediate nitrite-nitroso-acetate complexes of palladium(II)that ultimately leads to contamination of the product - palladium(II) acetate nitriloacetate complex of palladium(II). The increasing consumption of acetic acid is more than 3.0 liters per 1 kg of palladium nitrate solution leads to the increase of the quantity of solution and dissolving therein nitriloacetate palladium(II)that reduces the output of the product is A.

The reduction of the ethyl acetate less than 0.8 liters per 1 kg of palladium nitrate solution leads to incomplete removal of nitric acid, which further when the temperature leads to the formation of insoluble polymeric palladium(II)acetate. The increased consumption of added ethyl acetate over 1.0 l per 1 kg of palladium nitrate solution leads to the appearance of its surplus and dissolve in it a product that reduces the output of palladium(II)acetate.

The reduction of the acetic anhydride is less than 0.4 l per 1 kg of palladium nitrate solution leads to an increase in water activity, which upon further heating leads to the solution of ethanol and, as a consequence, contamination of the product metal palladium. The increase in the consumption of acetic anhydride over 0.6 liters per 1 kg of palladium nitrate solution leads to the manifestation of them restorative properties, which also leads to contamination of the product metal palladium.

Reducing the duration of adding a mixture of acetic acid, ethyl acetate and acetic anhydride in the nitric acid solution of palladium is less than 1 h leads to a more rapid flow of interaction and more intensive allocation of nitrogen oxide, which causes foaming. The increase in the duration of adding a mixture of ethyl acetate, acetic acid and acetic ang is drida in the nitric acid solution of palladium over 1 h increases the duration of the process.

The reduction of temperature of heating of the solution after introduction of the mixture of acetic acid, ethyl acetate and acetic anhydride is less than 90°leads to incomplete transfer intermediate nitrite-nitroso-acetate complexes of palladium(II) in nitriloacetate complex of palladium(II)that with further increase in temperature is the cause of intense decomposition nitrito-nitroso-acetate complexes of palladium(II) to insoluble polymeric palladium(II) acetate and pollution of the main product - soluble trehyadernogo of palladium(II)acetate. The temperature increase of the heating of the solution after introduction of the mixture of acetic acid, ethyl acetate and acetic anhydride over 110°leads to rapid decomposition nitrito-nitroso-acetate complexes of palladium(II) to insoluble polymeric palladium(II)acetate, which is the cause of the contamination is the main product.

Reduction of duration of heating of the solution after introduction of the mixture of acetic acid, ethyl acetate and acetic anhydride is less than 3 hours leads to incomplete transfer intermediate nitrite-nitroso-acetate complexes of palladium(II) in nitriloacetate complex of palladium(II), which further contaminates the main product insoluble polymeric palladium(II)acetate. The increased duration of the heating restorable 3 hours increases the duration of the whole process.

Reducing the temperature of the secondary heating of the solution is less than 135°leads to incomplete transition nitriloacetate complex of palladium(II) acetate, and, as a consequence, contamination of the product - soluble trehyadernogo of palladium(II)acetate. The increase in temperature of the secondary heating solution over 145°leads to boiling of the reaction solution, which causes foaming.

Reducing the length of the secondary heating of the solution is less than 6 hours leads to incomplete transition nitriloacetate complex of palladium(II) acetate, which is a cause of contamination of the product. The increased duration of the warm solution over 6 hours increases the duration of the whole process.

Reducing the amount of nitrogen by injecting the reaction solution is less than 20 m³1 m³solution leads to a large residual content of oxides of nitrogen, which is the loss of the feasibility of transmission of a current of inert gas to remove oxides of nitrogen. The increase in the current of nitrogen over 40 m³1 m³solution causes foaming of the solution.

Examples of the method

As the initial product for experiments No. 1-33 (see table) to obtain a palladium(II) acetate was prepared solution of palladium nitrate by dissolving palladium metal in nitric acid is the same and its 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 brought to the required temperature, was added in portions calculated volume mixture of acetic acid, ethyl acetate and acetic anhydride and stirred. After adding the total volume of the mixture of acetic acid, ethyl acetate and acetic anhydride increased warming of the solution to a predetermined temperature, and the solution was kept under stirring for a certain period of time. Then again increased heating of the solution to the required temperature and the solution again was kept under stirring for a certain period of time. The resulting solution or suspension of palladium(II) acetate was cooled to room temperature (20° (C) and the precipitate of palladium(II) acetate was separated by filtration, were unloaded on a baking sheet and dried at 120°C for three hours. The residue was 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. 1-30).

Example 2

The process was carried out according to example 1, but the reactor was introduced nitrogen through the solution and the entire process was performed by passing nitrogen through the reaction solution. This reduced the duration by the CA (see The table experience No. 31).

Example 3

The process was carried out according to example 1, but without the precipitate from the mother liquor. After keeping the reaction solution at a temperature of preheating 135-140°within 6 hours of the reaction, the suspension is passed to a complete evaporation of acetic acid and obtain a dry salt. This has increased the product yield, but increased the duration of the process (see Table, experiments No. 32-33).

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 polymeric palladium acetate.

Obtaining palladium(II)acetate
A) no experience	1	2	3	4	5	6	7	8	9	10	11	12	13	14	15	16
B) the Absence or presence of nitrogen through the reaction solution, - or+, respectively	-	-	-	-	-	-	-	-	-	-	-	-	-	-		-
C) the temperature of the interaction of a mixture of acetic acid, ethyl acetate and acetic anhydride with nitric acid solution of palladium °	50¹	60	70	80	90	70	70	70	70	70	70	70	70	70	70	70
D) Consumption of acetic acid per 1 kg of palladium in solution, l	2	2	2	2	2	1	3	4	2	2	2	2	2	2	2	2
D) Consumption of ethyl acetate per 1 kg of palladium in solution, l	1	1	1	1	1	1	1	1	0,6	0,8	1,2	1	1	1	1	1
E) Consumption of acetic anhydride per 1 kg of palladium in solution, l	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0	0,2	0,4	0,6	0,8
G) Duration of introduction of the mixture of acetic acid, ethyl acetate and acetic anhydride, h	2	1	1	1	1	1	1	1	1	1	1	1	1	1	1	1
C) the temperature of the heating solution after introduction of the mixture of acetic acid, ethyl acetate and acetic anhydride, °	100	100	100	100	100	100	100	100	100	100	100	100	100	100	100	100
And Duration of warming of the solution after introduction of the mixture of acetic acid, ethyl acetate and acetic anhydride, h	3	3	3	3	3	3	3	3	3	3	3	3	3	3	3	3
K) the temperature of the secondary heating solution, °	140	140	140	140	140	140	140	140	140	140	140	140	140	140	140	140
L) the duration of the secondary heating solution h	6	6	6	6	6	6	6	6	6	6	6	6	6	6	6	6
M) Output %	93	92	92	92	94	94	90	88	94	95	93	95	94	94	94	92
¹The beginning of the interaction is characterized by a long induction period, which requires an increase in the duration of introduction of the mixture of acetic acid, ethyl acetate and acetic anhydride in the original nitric acid solution of palladium.

Obtaining palladium(II) acetate (continued)
And	17	18	19	20	21	22	23	24	25	26	27	28	29	30	31	32	33
B	-	-	-	-	-	-	-	-	-/td>	-	-	-	-	-	+	+	-
In	70	70	70	70	70	70	70	70	70	70	70	70	70	70	70	70	70
G	2	2	2	2	2	2	2	2	2	2	2	2	2	2	2	2	2
D	1	1	1	1	1	1	1	1	1	1	1	1	1	1	1	1	1
E	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5	0,5
W	0,5²	1,5	1	1	1	1	1	1	1	1	1	1	1	1	1	1
3	100	100	70	90	110	120	100	100	100	100	100	100	100	100	100	100	100
And	3	3	3	3	3	3	2	4	3	3	3	3	3	3	At least 1.5	1,5	3
To	140	140	140	140	140	140	140	140	120	130	140	150³	140	140	140	140	140
L	6	6	6	6	6	6	6	6	6	6	6	6	5	7	No man is e 3	3+2⁴	6+4⁴
M	92	92	93	92	92	93	92	92	92	92	92	93	92	92	92	100⁵	100^s
²There is intense emission of nitrogen oxides, which leads to foaming of the solution.
³Is the boiling of the reaction solution, which leads to its foaming.
⁴Heating of the suspension, after heating the solution at 140°With, lead to the receipt of dry salts. Three hours with the air supply and six hours without air are warming up, then spent two hours with the air supply and four hours without air evaporated the solution.
⁵Quantitative output is achieved by using highly pure reagents and palladium.
According to x-ray phase analysis of the products of experiments No. 5, 9, 19, 22 observed the presence of two crystalline phases: mainstream - treatery the palladium(II) acetate [Pd₃(CH₃Soo)₆] and impurity phase polymer palladium acetate(II) Catena-poly-[Pd(CH_{3 Soo)₂]_n;}
in the products of experiments№№6, 13, 23, 25, 29 main phase crystal treatery the palladium(II) acetate [Pd₃(CH₃Soo)₆] and impurity phase - crystalline nitriloacetate palladium(II) [Pd₃(CH₃COO)₅NO₂];
in the products of experiments No. 12, 16, 30 main phase crystal treatery the palladium(II) acetate [Pd₃(CH₃COO)₆] and impurity phase - metallic palladium; in all other experiments observed a pure phase trehyadernogo of palladium(II) acetate [Pd₃(CH₃Soo)₆].

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) is treated with a mixture of acetic acid, ethyl ester acetic acid and acetic anhydride at a temperature (60-80)°With consumption (2,0-3,0) l glacial acetic acid, (0,8-1,0) l ethyl acetate and (0,4-0,6) l acetic anhydride per 1 kg of palladium in the solution is not less than 1 hour, heat the resulting solution at a temperature (90-110)°With not less than 3 h and (135-145)°With not less than 6 hours

2. The method according to claim 1, from which causesa fact, before adding a mixture of acetic acid, ethyl ester acetic acid and acetic anhydride via the nitric acid solution of palladium pass a stream of nitrogen with a flow rate (20-40) m³1 m³solution with the duration of heating of a solution of palladium after introduction of the mixture of acetic acid, ethyl ester acetic acid and acetic anhydride at a temperature (90-110)°With at least 1.5 h and at a temperature (135-145)°With not less than 3 hours

3. The method according to claim 1, characterized in that the heating of the suspension of palladium acetate after heating the solution at (135-140)°With lead to get dry salts.