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Method of obtaining polymer palladium carboxylates Method includes the dissolution of metallic palladium in concentrated nitric acid, evaporation of an obtained palladium nitrate solution. The palladium nitrate solution is evaporated at a temperature of (40-80)°C until palladium nitrate crystallisation starts, into the formed solution added is carboxylic acid in the form of a water-free or a water solution, in a liquid or crystalline state in an amount of (600-800)% of a molar amount of palladium in the initial palladium nitrate solution, or carboxylic acid anhydrite in an amount of (350-450)% of a molar amount of palladium in the initial palladium nitrate solution until crystallisation of polymer palladium carboxylate stops. |
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Method of producing palladium trifluoroacetate Method includes dissolving palladium metal in concentrated nitric acid and evaporating the obtained solution. The palladium nitrate solution is evaporated at (40-80)°C until palladium nitrate begins to crystallise. The formed solution at (30-80)°C is mixed with trifluoroacetic acid in amount of (600-800)% of the molar amount of palladium in the starting palladium nitrate solution or trifluoroacetic acid anhydride in amount of (350-450)% of the molar amount of palladium in the starting palladium nitrate solution until the end of crystallisation of polymeric palladium trifluoroacetate. The method also includes filtering the formed compound and conversion thereof into the end product by adding acetonitrile at (10-30)°C with weight ratio of the compound to acetonitrile of 1:(0.5-2). |
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Method of producing zinc acetate dihydrate Invention relates to a method of producing zinc acetate dihydrate. The method is realised by dissolving powdered zinc oxide or zinc hydroxide in aqueous acetic acid solution with ratio of reactants - zinc oxide (zinc hydroxide):water:acetic acid equal to 1:(1.6-2.0):(1.8-2.2) by weight; the obtained solution is then evaporated to oversaturation, gradually cooled to 0-5°C and held for 15-20 hours. The crystalline hydrate of zinc acetate precipitated from the solution is filtered and dried at 30-40°C. |
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Method of producing high-purity anhydrous zinc acetate Invention relates to the technology of producing salts of carboxylic acids, particularly acetic acid, and a method of producing high-purity anhydrous zinc acetate. High-purity zinc acetate is obtained by reacting a zinc-containing compound with acetic acid, where the zinc-containing compound used is diethylzinc which is pre-diluted with an inert solvent to concentration of not more than 20 wt %. The inert solvent used is preferably undecane. The invention enables to obtain high-purity anhydrous zinc acetate in which content of 18 limited metal impurities, according to chemical spectral analysis, is equal to 5·10-5 - 5·10-6 wt %. |
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Invention can be used in microelectronics, particularly for producing nonvolatile ferroelectric memory. The method of obtaining anhydrous lead (II) acetate for preparing anhydrous film-forming lead zirconate-titanate solutions involves reaction of lead oxide PbO, acetic acid and acetic anhydride and then drying the obtained lead (II) acetate in a vacuum. Anhydrous lead (II) acetate is obtained by solid-phase synthesis from lead oxide PbO via reaction thereof with a small amount of acetic acid (2-5 wt % of PbO) in the presence of acetic anhydride taken in excess of 5-10 wt % stoichiometric. Reactant residues - acetic acid and acetic anhydride - are removed by drying the obtained product in a vacuum to granular state. Subsequent dissolution of the anhydrous lead (II) acetate in a pure organic solvent and complexing reaction thereof with zirconium and titanium alkoxides is carried out at temperature 15-40°C. |
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Method of producing heteronuclear acetates of palladium with non-ferrous metals Invention relates to chemistry of platinum metals, particularly synthesis of palladium compounds, specifically synthesis of heteronuclear acetates of palladium with non-ferrous metals. The method of producing heteronuclear acetates of palladium with non-ferrous metals involves reaction of an acetate compound of palladium and a non-ferrous metal compound in a glacial acetic acid solution, where the reaction of compounds, taken in molar ratio palladium: non-ferrous metal of 1:(0.90-0.97), takes place in glacial acetic acid used in amount of (600-800)% of the molar amount of palladium, at temperature (70-90)°C with evaporation of the solvent to wet or dry residue, with repeated addition of glacial acetic acid in amount of (200-600)% of the molar amount of palladium, repeated evaporation of the solvent at temperature (80-120)°C, with treatment of the dry residue, pre-heated to (70-90)°C, with a solution of a mixture of benzene or toluene and acetic acid anhydride with volume ratio thereof equal to (4-8):1 respectively, the amount of the acetic acid anhydride being equal to (20-60)% of the molar amount of palladium, at temperature (70-100)°C for (2-30) minutes, cooling the obtained suspension to temperature (40-70)°C and filtering the desired compound. In another version, the method involves reaction of a palladium acetate and an acetate compound of a non-ferrous metal in glacial acetic acid solution with solvent evaporation, where the reaction of compounds, taken in molar ratio palladium: non-ferrous metal equal to 1:(0.90-0.97), takes place in glacial acetic acid used in amount of (400-600)% of the molar amount of palladium, at temperature (80-120)°C with solvent evaporation to a dry residue, with subsequent treatment thereof with a solution of a mixture of benzene or toluene and acetic acid anhydride, pre-heated to (70-90)°C, with volume ratio thereof equal to (4-8):1 respectively, the acetic acid anhydride being in amount of (20-60)% of the molar amount of palladium, at temperature (70-100)°C for (2-30) minutes, cooling the obtained suspension to temperature (40-70)°C and filtering the desired compound. |
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Method of producing potassium acetate Invention relates to a method of producing potassium acetate by reacting potassium hydroxide with aqueous acetic acid solution and subsequent steps for treating the obtained potassium acetate. The method involves filtration treatment of the obtained potassium acetate solution, evaporation of the filtrate at 105-115°C, cooling to 55-65°C and vacuum crystallisation. The method is characterised by that the starting products used are crystalline potassium hydroxide and 40-60% acetic acid, which is added to potassium hydroxide in 30-35% stoichiometric excess and while keeping temperature of the reaction mass at 80-90°C, and that the potassium acetate crystals formed after the vacuum crystallisation step are further centrifuged at 500-2000 rpm and then vacuum dried at 145-155°C. |
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Deicing composition contains the following (wt %): bischofite 51.2-57.6, alkali metal hydrophosphate 0.3-0.7, alkali and/or alkali-earth metal acetate 0.5-3.0, alkali metal carbonate 0.3-0.5 and talc 0.01-0.05, water - the balance. The solution has pH 6.5-8.5 and density 1240-1260 kg/m3. |
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Method of producng basic copper (ii) acetate Method involves reaction of a metal oxide with an acid in a bead mill in the presence of a stimulant. The process takes place in the presence of a liquid phase, the solvent of which is distilled water. Copper oxide is added in amount of 1.8-3.3 mol/kg in molar ratio to acetic acid equal to (1:1.7)-(1:2.1). The stimulant is added in amount of 0.05 mol/kg. Addition is performed in the following sequence: glass beads, liquid phase solvent, acetic acid, stimulant and copper (II) oxide, in molar ratio of the glass beads to the rest of the material equal to (1:1)-(1.5:1). Further, the material undergoes mechanical mixing and the process is carried out while constantly cooling in temperature range of 20-45°C until almost complete conversion of the loaded copper (II) oxide into a salt. Mixing and cooling are then stopped. The suspension of the reaction mixture is then separated from the glass beads. This suspension is mixed with washing water with reaction mixture residue, left for 1-2.5 hours and filtered. The product residue is thoroughly squeezed and taken for purification via recrystallisation, and the filtrate is returned to repeated process. |
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Method of producing highly pure tetrahydrate of manganese acetate Invention relates to a method of producing tetrahydrate of manganese acetate, relating to chemical engineering of manganese compounds and can be used in producing pure manganese salts used in electronic industry as raw material for making solid-electrolyte capacitors. The method of producing tetrahydrate of manganese acetate involves leaching manganese carbonate with dilute chemically pure nitric acid, followed by filtration, dissolution of manganese carbonate in glacial acetic acid solution, alkalisation of the obtained product manganese acetate solution with aqueous ammonia solution, filtration of manganese acetate solution clarified by settling with separation of a precipitate of impurities from the solution, and evaporation of the solution to concentration 32-32.5 wt %, and addition acetic acid and crystallisation of manganese acetate from the solution by cooling at temperature 50-15°C, and adding into the solution nucleating agents from crystals of the tetrahydrate of manganese acetate in amount of 0.05 wt %, holding the suspension the crystalline manganese acetate precipitate obtained after crystallisation at final crystallisation temperature while stirring constantly, separating the crystalline manganese acetate precipitate followed by washing the crystalline precipitate with a saturated solution of pure manganese acetate and/or acetone at temperature equal to final crystallisation temperature. |
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Lead (ii) acetate synthesis method Invention relates to an improved method for synthesis of lead (II) acetate through direct reaction of a metal, its dioxide with a carboxylic acid in the presence of an organic liquid phase and a stimulating iodine additive in a vertical bead mill, where the oxidising agent and the reagent in deficit are lead dioxide taken in amount of 0.4-0.6 mol/kg, metal and acetic acid are taken in amount of 0.6-1.5 mol/kg and respectively so as to obtain mol/kg of a salt product, where nPbO2 is amount of lead dioxide in mol/kg. The stimulating additive used is iodine taken in amount of 0.01-0.05 mol/kg liquid phase, the base of which is initially composed of an organic solvent and acetic acid and iodine dissolved in the said solvent. Components of the reaction mixture are loaded in the following sequence: liquid phase solvent, acetic acid, metal, its dioxide, molecular iodine. Mass ratio of the components and glass beads is at least 1:1.5; the process starts at room temperature and is carried out at maximum temperature of 30-50°C under forced cooling conditions and while controlling using a sampling method and determining content of accumulated salt and unreacted lead dioxide and acetic acid in the said samples until the oxidising agent is virtually exhausted, after which the process is stopped. The suspension of the reaction mixture is separated from the glass beads and thin films of unreacted metal by passing through netting with cell size of 0.3×0.3 mm as a filter partition. The beads and unreacted metal are returned to the reactor where together with the housing, mixer and other components of the reactor are washed with the liquid phase solvent from reaction mixture remaining after discharge thereby obtaining a washing solvent; the suspension of the reaction mixture is filtered, the residue on the filter is treated with the washing solvent, pressed well and taken for cleaning through recrystallisation, and the obtained filtrate in a mixture with the washing solvent is returned to the repeated process. Output the filtered off product is 93-98% of the theoretical output. |
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Method of obtaining palladium acetate 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. |
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Method of palladium acetate production Invention refers to platinum metal salts synthesis, specifically palladium salts, namely palladium (II) acetate applied as catalyst or for production of initial salt for other palladium salts. Method of palladium acetate production includes as follows. Metal palladium is dissolved in concentrated nitric acid. Prepared solution is steamed prior to crystallisation of palladium nitrate salt, processed by ice acetic acid. Deposition is filtered and processed with ice acetic acid. Nitrate palladium solution is processed with ice acetic acid with sodium acetate additive in amount 1.5 - 2 kg per 1 kg of palladium in solution. Deposition is processed and dissolved in ice acetic acid in ratio 19-21 l per 1 kg of deposition with acetamide added in amount 0.1 - 0.2 kg per 1 kg of deposition. Solution is warmed at temperature 80 - 90 °C within at least 5 h and steams until salt is formed. |
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Method for obtaining palladium acetate 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. |
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Method for obtaining palladium acetate 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. |
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Method of zirconium carboxylate production 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. |
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Basic iron (iii) acetate producing method 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. |
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Method for preparing manganese (ii) acetate 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. |
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Method for preparing palladium acetate 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. |
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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. |
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Method of production of lead tetraacetate 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. |
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Ferrous acetate preparation method 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. |
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Ferrous acetate preparation method 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. |
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Basic ferric acetate preparation method 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%. |
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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. |
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Method for preparing ferrous (ii) acetate Invention relates to a method for preparing acetic acid salts, in particular, anhydrous ferrous (II) acetate. Method for preparing anhydrous ferrous (II) acetate involves interaction of metallic iron with acetic acid in the presence of oxidizing agents of ferric oxide Fe2O3 or Fe3O4 and molecular iodine in the mole ratio acetic acid : acetic anhydride : iron oxide = 100:(6-20):(2-2.5), respectively, and in the mole ratio iron oxide : iodine = 100:6.3. The process is carried out at temperature 80°C in the beaded mill of vertical type with high-rotation blade mixer and reflux condenser in the mass ratio of glass beads and liquid phase in the charge = 1:1. The process is carried out with periodic taking off samples of the end product solid phase by filtering and the following recover filtrate and feeding with acetic acid and iron oxide. For compensation of components loss of liquid phase in filtering there are recovered into reactor to the repeated process that is carried out for four times at a time. All procedures of the basic process and filtration are carried out in nitrogen medium. Preferably, method involves using hematite, γ-oxide, iron minium, magnetite or Fe3O4 x 4 H2O as the iron oxide source. Invention provides possibility for preparing anhydrous ferrous (II) acetate and simplifying method due to excluding the evaporation stage in isolation of salt. |
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Method for preparing copper (ii) acetate monohydrate Invention relates to a method for preparing copper (II) acetate monohydrate that represents organic carboxylic acid salt. Copper (II) acetate monohydrate is prepared by crystallization from solution obtained by mixing acetic acid, alkaline metal acetates or ammonium with copper-containing spent solution used in etching printing boards. Method provides reducing cost of the proposed method for preparing copper (II) acetate monohydrate, retaining purity of product with simultaneous utilization of toxic waste in electronic engineering manufacture - the spent solution in etching printing boards. Also, invention provides reducing material consumptions in preparing copper (II) acetate monohydrate, expanding assortment of materials used for its preparing and utilization of toxic waste in electronic engineering manufacture. Product obtained by the proposed method can be used as pigment, fungicide and copper microfertilizer in agriculture, as catalyst in processes of polymerization, as a stabilizing agent of artificial fibers, for preparing galvanic solutions and preparing other copper compounds. |
Another patent 2551322.