RussianPatents.com

Method for obtaining palladium acetate

Method for obtaining palladium acetate
IPC classes for russian patent Method for obtaining palladium acetate (RU 2333195):
Another patents in same IPC classes:
Method obtaining pyrophosphate tetrammine platinum (ii) / 2331585
Invention pertains to the method of obtaining platinum (II) compounds, and specifically to pyrophosphate tetrammine di-platinum (II), which can be used as an intermediate compound during synthesis of cis-dichlorodiammineplatinum (II). The method involves adding sodium pyrophosphate to a solution of potassium tetrachloroplatinate (II) in a medium of ammonium acetate and heating the mixture for 1 hour on a water bath at pH=5, with subsequent addition of a second portion of sodium pyrophosphate and heating the solution for 4 hours. The released salt of pyrophosphate tetrammine diplatinum (II) is washed in water and spirit and dried at room temperature.
Method of obtaining cis-diammino(1,1-cyclobutanedicarboxylate)platinum(ii) / 2330039
Described is the improved method of obtaining cis-diammino(1,1-cyclobytanedicarboxylate)platinum(II) which relates to the compound of metals of the platinum group(MPG), in particular to the synthesis of the compounds of platinum, namely, to the synthesis of the compound cis-diammino(1,1-cyclobytanedicarboxylate)platinum(II), which is the biologically active coordination compound of platinum and can be used as the active substance of antitumorigenic medicine. The method is achieved by processing the cis-isomer of the ammine complex of platinum(II) Pt(NH3)2X2 (where X - Cl, Br, I) by the oxide or hydroxide of silver and cyclobutane-1,1-dicarboxylic acid, separation of the sediment of the insoluble salt of silver from the solution and by crystallisation of cis-diammino(1,1-cyclobytanedicarboxylate)platinum(II).
Bis-benzizo selenium zolonyl derivatives with antitumor, antiinflammatory and antithrombotic activity and their application Bis-benzizo selenium zolonyl derivatives with antitumor, antiinflammatory and antithrombotic activity and their application / 2324688
Invention relates to the benzo-iso-selenium zolonyl derivatives with the general formula (I) or (II) , where R - C1-C6-alkylen, phenyliden, biphenyliden, R' - polysaccharide residue or residue , where M - Pt or Pd.
Basic iron (iii) acetate producing method 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 Fe2O3, 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 O4.
Catalyst for production of acrylic acid esters according to metathesis reaction of dialkyl malates (variants) and a catalytic composition based thereof Catalyst for production of acrylic acid esters according to metathesis reaction of dialkyl malates (variants) and a catalytic composition based thereof / 2311231
Invention is dealing with preparation of homogenous catalyst for production of acrylic acid esters according to metathesis reaction of malates with ethylene. Two variants of preparing catalyst are developed. In particular, catalyst of general formula , wherein A1, A2 represent chlorine, L dihydroimidazole ligand, R1, R2, R3, the same or different, are substituents selected from hydrogen, alkyl, trialkylsylyl, and alkoxy; and catalyst of formula are proposed. Use of these catalysts allows number of cycles of metathesis reaction of dialkyl malates with ethylene to be increased both under moderate temperature (about 50°C) conditions when reaction is carried out without distillation of product and at temperatures about 120°C when acrylate produced is distilled out of reaction mixture. Catalytic composition is further developed allowing not only number of reaction cycles but also catalyst lifetime to be increased. Such composition contains indicated catalyst and 2-isopropoxystyrene or its derivative at molar ratio 1:(5-500), respectively.
Method for production of cis-dichloroamminisopropylamine platinum(ii) / 2309158
Potassium trichloroammineplatinate(II) salt is dissolved in aqueous solution of isopropylamine chloride at room temperature; isopropylamine is added to solution and over 40 min process id finished. Obtained cis-dichloroamminisopropylamine platinum(II) salt is filtered, washed with alcohol and dried. Yield of cis-[PtNH3(i-C3H7NH2)Cl] is 84 % from theoretical one. Complex of cis-[PtNH3(i-C3H7NH2)Cl] compound is characterized by elemental analysis, X-ray crystal analysis, IR- and UV-spectroscopy. Impurities such as [Pt(i-C3H7NH2)4].[Pt(NH3)Cl3]2 and KCl is not found, hence purification of said salt is not required. Claimed compound is useful in medicine as antitumor drug.
Methods for preparing ferric complexes with one salicylic acid anion 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 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 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.
Water-soluble iron-carbohydrate complexes, method for their preparing, medicinal agent, using / 2303039
Invention describes water-soluble iron-carbohydrate complexes containing 10-40 wt.-% of iron. Complexes can be prepared from ferric (III) salt aqueous solution and oxidation product aqueous solution of one or more maltodextrins with hypochlorite aqueous solution at alkaline pH value. In using one maltodextrin its dextrose equivalent is from 5 to 20, and in using mixture of maltodextrins the dextrose equivalent is from 5 to 20 and dextrose equivalent of each maltodextrin as component of mixture is from 2 to 40. Also, invention describes a method for preparing this complex and medicinal agents used in treatment and prophylaxis of states associated with iron deficiency.
Method of zirconium carboxylate production 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 CnH2n+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 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 Fe2O3, 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 O4.
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 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 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 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 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 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 CnH2n+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.

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

 

© 2013-2015 Russian business network RussianPatents.com - Special Russian commercial information project for world wide. Foreign filing in English.