Method of producing highly pure tetrahydrate of manganese acetate |
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IPC classes for russian patent Method of producing highly pure tetrahydrate of manganese acetate (RU 2415835):
      
 Lead (ii) acetate synthesis method / 2398758
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
 Method of obtaining palladium acetate / 2387633
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.
 Method of palladium acetate production / 2344117
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.
Method for obtaining palladium acetate / 2333196
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.
 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 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 / 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 / 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 producing iron (iii) benzoate / 2412153
Invention relates to an improved method of producing iron (III) benzoate by reacting granulated cast iron with benzoic acid and atmospheric oxygen as an oxidising agent in the presence of sodium chloride as a stimulating additive. The latter is in amount of 0.015-0.200 mol/kg. Said reaction takes place in the presence of a liquid phase which is a solution of benzoic acid in n-butyl alcohol with concentration of 1.8-2.4 mol/kg, at temperature 30-70°C and bubbling air at a rate of 1.3 l/min per kg of the liquid phase in a vertical-type bead mill with a highly efficient and high rotational speed blade-type mixer with crossed four blades in the presence of glass beads, taken in weight ratio to the liquid phase equal to 1:1, and cast iron which is broken to pieces with maximum linear dimension of 5 mm, taken in amount of 30% of the weight of the glass beads and simultaneously acting as an impact agent and a milling agent. The housing and bottom of the bead mill are protected by well-matched steel cowling and false bottom with a bearing socket for the mechanical mixer and a filter partition combined with it for separating the reaction mixture from the glass beads and unreacted metal particles in the field of the magnet. The process is controlled through a sampling method and determining concentration of iron (II) and (III) salts, as well as unreacted benzoic acid. The process is stopped when the acid is virtually completely converted to the end product. The obtained reaction mixture is separated from the beads remaining in the reactor and particles of unreacted metal, then left to cool on its own to room temperature (solubility of iron (III) salts falls to 0.130-0.135 mol/kg) and then cooled to 8-12°C, and then filtered. The residue is washed with a small amount of cooled n-butyl alcohol and taken for recrystallisation. The filtrate and the washing solvent are returned to the repeated process. Part of the end product is also returned, which ensures 80-90% output of the solid product.
 Sodium diformate synthesis method / 2402523
Invention relates to a method of preparing a sodium formate-containing composition with formic acid content of not less than 35 % of the total weight of the said composition, in which a) a stream of formic acid with formic acid content of not less than 74 wt % is provided; b) a stream of formic acid from step a) together with sodium formate-containing streams from step f) and step h) are taken to the crystallisation step where an aqueous solution is obtained at high temperature, where the said solution has molar ratio HCOOH:Na[HCOO] greater than 1.5:1 and molar ratio HCOOH: H2O equal to at least 1.1:1; c) at the crystallisation step the aqueous solution from step b) is crystallised to obtain a stream which contains a solid phase and a mother solution; d) the stream obtained from step c) is taken to a separation step on which the solid phase is separated from the mother solution to obtain a stream which contains sodium diformate and a stream which contains a mother solution; e) the stream which contains the mother solution from step d) is divided into two parts; f) one part of the stream from step c) in form of a portion (A) is returned to step b); g) the other part of the stream from step e) in form of a portion (B) together with the stream, including a base, which contains sodium is taken to a neutralisation step to obtain a mixture which contains sodium formate, and where portions of the mother solution (A) and (B) complement each other to 100 wt %, and the weight ratio of portion (A) of the mother solution to portion (B) lies between 20:1 and 1:10; and b) the sodium formate-containing mixture from step g) and optionally from step h), if necessary after its withdrawal, is taken to the concentration step in form of a stream where a portion of water contained in that stream is released, where after separation of the portion of water a stream which contains sodium formate is obtained, which is directly returned to step b) or crystallised at the second crystallisation and separation step, and the obtained liquid phase is taken to the concentration step h) in form of a stream, and the solid phase is taken in form of a stream to step b). The obtained product can be used in industrial production, especially at relatively low temperatures.
 Method of producing complex stabilisers for chlorine-containing polymers / 2400496
Carboxylic acids are reacted with oxides and/or hydroxides of Zn and Ca metals in the presence of glycerin, ionol, epoxidated soya oil, epoxy resin, diphenylol propane, phosphite NF while heating, in which the complex stabiliser is obtained through reaction of carboxylic acids with oxides and/or hydroxides of Ca, Zn, Mg, Al in the presence of glycerin and additives selected from ionol, epoxidated soya oil, epoxy resin, diphenylol propane, phosphite NF, diphenyl-n-butylphosphite, PES-5 polyethylsiloxane liquid, Penta-1006 or Penta-1005 plastic modifier, calcium stearate while heating, in which the carboxylic acids used are oleic acid, 2-ethylhexane acid, α,α'-branched C10-C26 monocarboxylic acids. The carboxylic acids are first reacted with oxides and/or hydroxides of Zn, Ca, Mg, Al and glycerin at 140-180ºC to obtain a mixture consisting of salts of carboxylic acids and glycerin monoether of carboxylic acid, and an additive is added to the reaction mass only when acid number not greater than 5 mg KOH/g is reached. The process is carried out in the following ratio of components, wt %: carboxylic acids 6.3-60.4; oxides and/or hydroxides of metals 1.2-8.3; glycerin 8.5-20.4; additives - the rest.
Lead (ii) acetate synthesis method / 2398758
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
 Purification of carboxylic acids through complexing with selective solvents / 2395486
Invention relates to an improved method of purifying carboxylic acid from a mixture which contains one or more carboxylic acids selected from a group consisting of terephthalic acid, isophthalic acid, orthophthalic acid and their mixtures, and also contains one or more substances selected from a group consisting of carboxybenzaldehyde, toluic acid and xylene. The method involves: bringing the mixture into contact with a selective solvent for crystallisation at temperature and in a period of time sufficient for formation of a suspension of a complex salt of carboxylic acid with the selective solvent for crystallisation without complete dissolution of the complex salt of carboxylic acid; extraction of the complex salt and decomposition of the complex salt in the selective solvent for crystallisation in order to obtain free carboxylic acid. The mixture containing unpurified carboxylic acid is brought into contact with the selective solvent for crystallisation in order to form a suspension of a complex salt of carboxylic acid with the selective solvent for crystallisation. The complex salt is extracted and, if desired, processed for extraction of free carboxylic acid.
 Method of producing heat stabilisers for chlorine-containing polymers / 2391360
Invention relates to an improved method of making heat stabilisers for chlorine-containing hydrocarbons, specifically to a method of obtaining stearates of bivalent metals used in polymer compositions based on chlorine-containing polymers such as polyvinyl chloride, vinylchloride copolymers, chlorinated polyvinylchloride etc. The method of producing heat stabilisers of chlorine-containing hydrocarbons involves reacting stearic acid and oxides or hydroxides of calcium, zinc, barium, magnesium or lead in form of separate of mixed salts of stearic acid in a solid phase with intense stirring. The process is carried out in the presence of sodium hydroxide or potassium hydroxide in amount of 0.05-0.15% of the mass of stearic acid and propylene carbonate or dimethylformamide, or hexamethapol or sulfolane or dimethylsulfoxide in amount of 0.005-0.05% of the mass of stearic acid at 40-95°C in a double-screw reactor. Catalysts of the process - sodium hydroxide or potassium hydroxide and propylene carbonate, or dimethylformamide, hexamethapol, sulfolane or dimethylsulfoxide facilitate considerable increase in activity of the surface of the substrate and, as a result, increase in the rate of the process and obtaining products in form of a homogeneous highly dispersed powder and prevention of secondary oligomerisation of the end product.
 Method of obtaining manganese (ii) benzoate / 2391332
Invention relates to a method of obtaining manganese (II) benzoate through direct reaction of metal with carboxylic acid in the presence of an oxidising agent, a stimulating iodine additive and a liquid phase organic solvent in a bead mill, in which the oxidising agent used is manganese peroxide taken in amount of 0.15-0.50 mol/kg, and molar ratio of metal:peroxide equal to (1.5.2.2):1; benzoic acid is taken in amount of (2,05÷2,1)·(nMn+
Method of obtaining palladium acetate / 2387633
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.
Method of producing carboxylates of rare-earth elements / 2382760
Method involves reacting oxides of rare-earth elements (REE) with α, α'-branched monobasic carboxylic acids with 8-20 carbon atoms while stirring at high temperature, as well as their mixtures in the presence of water with molar ratio of water to the rare-earth element equal to 1-3:1, with subsequent cooling, addition of solvent and azeotropic drying of the obtained solutions of carboxylates of rare-earth elements through distillation of the azeotropic solvent-water mixture, where the process is carried out while heating to 100°C and further at a rate of 10°C per hour to 150°C, with removal of the bulk of water during synthesis with a stream of inert gas fed to the bottom of the reactor and bubbled through the reaction mixture, without the stage of elutriation from unreacted oxides of rare-earth elements. The proposed method combines high output and purity of the product with simplification of the technique with minimal loss of reagents and minimal consumption of solvent.
 1-13c-caprylic acid synthesis method / 2382025
Invention relates to a method for synthesis of 1-13C-caprylic acid which is used as a diagnostic preparation when diagnosing motor-evacuation functions of the stomach. The method involves hydrocarboxylation reaction of 1-heptene with carbon monoxide 13CO and water at temperature 100-170°C and pressure not above 5 MPa, in the presence of a solvent and a catalyst system which contains a complex compound of palladium and triphenylphosphine in ratio ranging from 1:2 to 1:100, where the solvent used is dioxane and/or aromatic hydrodrocarbon.
Preparation comprising water-soluble triterpenic acid salts and method for its preparing / 2244426
Invention relates to a method for preparing the preparation comprising triterpenic acid water-soluble salts and additionally added protein-containing product and vegetable raw, the source of triterpenic acids taken in the following ratio of components, wt.-%: protein-containing product, 10-17; triterpenic acid sodium salts, 4-5, and vegetable raw, the balance. Method involves mixing triterpenic acid-containing vegetable raw with the protein-containing product taken in the ratio = (9-11):(1-2), mechanical-chemical treatment of this mixture in activator device, mixing of prepared semi-finished product with sodium carbonate or sodium hydrocarbonate taken in the ratio = (92-97):(3.5-8.3) and repeated treatment in the activator device. Method involves applying flow-type ball vibration-centrifugal or ellipse-centrifugal mills as the activator device that provide the acceleration of milling bodies up to 170-250 m/c2 and time for treatment for 1.5-3 min. Invention provides simplifying the process and the complex processing waste in lumber industry.
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FIELD: chemistry. SUBSTANCE: 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. EFFECT: obtaining highly pure powdered tetrahydrate of manganese acetate. 8 cl, 2 tbl, 2 ex
The invention relates to the field of chemical technology compounds manganese and can be used to obtain pure salts of manganese, used in the electronics industry as raw material for the manufacture of oxide-semiconductor capacitors. Salts of manganese, namely the tetrahydrate of manganese acetate and uranyl nitrate manganese, used to create the cathode plates oxide-semiconductor capacitor, which serves as the solid electrolyte of manganese dioxide obtained by pyrolysis of a mixed solution of these salts. A method of obtaining acetate tetrahydrate manganese, described in patent RU 2294921, CL SS 53/10, C07F 13/00, publ. 10.03.2007, which includes the interaction of manganese metal or its oxide with acetic acid in the presence of an oxidant. The process is carried out in a bead mill, vertical type with a reflux-condenser, a high-speed paddle stirrer and glass beads as pereirago agent loaded in a mass ratio to the liquid phase of 1.5:1. The liquid phase is a solution of glacial acetic acid in a solvent, which is used as the ethyl cellosolve, ethylene glycol, 1,4-dioxane, isoamyl and n-butyl alcohols. The concentration of acid in the liquid phase is 3.4-5 mol/kg Later in the LM the positive phase load: iodine in the amount of 0.025-0,070 mol/kg liquid phase, metallic manganese and manganese dioxide at a molar ratio of 2:1 in the amount of 11.8 wt.% the liquid phase. The process begins at room temperature and lead with self heating up to 30-38°C - almost to the total consumption of manganese dioxide. The resulting suspension of the salt is separated from the beads and unreacted manganese and filtered. The filtrate is returned to repeat the process, and the residue is purified by recrystallization. The disadvantage of this method is the contamination of the product with organic impurities present in the solvent. The closest (prototype) to the proposed method of obtaining acetate tetrahydrate manganese is a method described in the application CN A, CL SS 53/10, SS 51/41, publ. 15.06.2005, including the reaction between glacial acetic acid and electrolytic manganese, filtration, clarification, concentrated under vacuum solution of manganese acetate, crystallization upon cooling from a solution of manganese acetate and the tendency of the crystals of the acetate tetrahydrate of manganese. Gives a pure product with a basic substance content of 98.5-99%. The disadvantage of this method is to obtain manganese acetate with a lower content of the basic substance is not high enough purity that can significantly improve the electrical characteristics of capacitors with solid electrolyte of d is the oxide of manganese. The objective of the invention is to obtain tetrahydrate of manganese acetate with high purity, which enables the manufacture of capacitors with solid electrolyte of manganese dioxide with the best electrical properties. This problem is solved by developing a method of producing acetate tetrahydrate of manganese with such technical results, such as high purity product, acetate tetrahydrate of manganese, and a high content of basic substance at low losses of manganese. We propose a method of obtaining acetate tetrahydrate manganese high purity, including the dissolution of carbonate of manganese in the solution of chemically pure glacial acetic acid; filtering the received production of a solution of acetate of manganese, pre-clarified by settling, separating from the solution the precipitate impurities; evaporation was acidified with acetic acid solution of manganese acetate to a concentration of 32-32,5 wt.%; crystallization of the concentrated solution of acetate of manganese by cooling, followed by curing the resulting suspension crystalline precipitate tetrahydrate of manganese acetate under stirring; the separation of a crystalline precipitate acetate tetrahydrate of manganese from the waste solution, followed by washing the crystalline precipitate rich R is a target of pure acetate of manganese and/or acetone. Thus, before dissolving produce the leaching of manganese carbonate followed by filtration, and the leaching is carried out at a dilution of chemically pure nitric acid, deionized water to a concentration of 2-5 wt.%, the ratio of the liquid and solid phases is approximately 5:1 by volume, the temperature of 20-50°C. and constant stirring for 5-30 minutes; obtained by dissolving production acetate solution of manganese are alkalinization of 20%aqueous ammonia solution with constant stirring until the solution pH 7-7,5; carry out the production process of evaporation of a solution to a concentration of 32-32,5 wt.% acidification 46%acetic acid, taken in the ratio of at least 1.7:1000 by volume; obtained after crystallization suspension of a crystalline precipitate tetrahydrate of manganese acetate is maintained at a constant stirring for 15-45 minutes, and the crystalline precipitate tetrahydrate of manganese acetate was washed with a saturated solution of pure acetate of manganese and/or acetone at a ratio of liquid and solid phases is not less than 3:1 by volume with multiplicity washing 1-3. All of these modes are optimized. Leaching of the raw material, manganese carbonate, is a pre-process stage, which has already achieved a good effect on cleaning from impurities, as in the leaching of trudnoudaljaemye impurity well derived from the waste solution, and when using the above optimized modes maximum useful effect is minimized contamination by impurity chlorides, calcium, copper and iron production of a solution of acetate of manganese at low losses of manganese. The use of chemically pure nitric acid with a concentration of less than 2 wt.%, leads to reduced efficiency of the leaching of impurities from manganese carbonate, and with a concentration above 5 wt.% to accelerate the dissolution of manganese and growth loss of manganese from the waste solution. The temperature of the leaching below 20°C leads to a decrease in the efficiency of purification of manganese carbonate, and above 50°C to accelerate the dissolution of carbonate of manganese and growth loss of manganese. The duration of the leaching beyond the optimal time, or reduces the extent of excretion of manganese carbonate impurities, when the process is less than 5 minutes, or contributes to the increase of losses of manganese, when the process goes more than 30 minutes. Alkalinization of production of a solution of acetate of manganese to the optimum pH of 7-7,5 aqueous solution of ammonia under stirring promotes the release of production of a solution of the residual impurities of iron and heavy metals, and pH less than 7 leads to an increase in the content of the project of heavy metals in the final solution, and more than 7.5 - immaterial to reduce the residual content of impurities of heavy metals in the final solution and increased consumption of ammonia solution. The production process of evaporation of a solution to a concentration of 32-32,5 wt.% acidification 46%acetic acid, taken in the optimal case, mentioned above, the ratio, helps eliminate hydrolysis of the acetate of manganese. With the introduction of acetic acid in fewer losses increase manganese due to hydrolysis. Keeping under stirring in optimal time period specified above, the suspension of a crystalline precipitate acetate tetrahydrate of manganese after crystallization and washing the crystalline precipitate a saturated solution of pure acetate of manganese and/or acetone in the above optimal values of the ratio of liquid and solid phases and the frequency of washing, and give a good cleaning efficiency crystalline precipitate acetate tetrahydrate of manganese impurities and help reduce the content of impurities in the product, but the parameters beyond the optimal value, or reduce the cleaning efficiency crystalline precipitate of impurities, when the parameters are underestimated or not increase the degree of purification, when the parameters are overestimated. In the present invention the problem is solved and obtained is shown above technical results due to the following factors. High purity product, acetate tetrahydrate of manganese, is achieved by purification from impurities at several stages of the process: first, at the preliminary stage leaching of the raw material, carbonate of manganese, - thanks to the introduction of major impurities, such as chlorides, iron, calcium, copper, lead, waste mortar, and then at the stage of alkalizing production of a solution of acetate of manganese - thanks to the removal of residual impurities, mainly iron and heavy metals, from the waste solution, then at operation keeping under stirring suspension of a crystalline precipitate acetate tetrahydrate of manganese after crystallization is due to the optimal mixing time, and on flushing crystalline precipitate tetrahydrate of manganese acetate saturated solution of pure acetate of manganese and/or acetone - through the optimal values of the ratio of liquid and solid phases and the frequency of washing (the optimal value and the modes specified above). High content of the basic substance at low losses of manganese contribute to how the above factors that increase the cleaning efficiency of the finished product from impurities, and factors that reduce the loss of manganese from the waste solution: at the stage of evaporation of productive solution due to the use of the program acidifying with acetic acid in optimal quantities, at the stage of leaching of carbonate of manganese - through the use of diluted chemically pure nitric acid with an optimal concentration and the optimal modes for the temperature and the duration of the process (the optimal value and the modes specified above). The present invention is implemented at OJSC "Elecond", garapon a production section for salts of manganese, uranyl nitrate tetrahydrate manganese and manganese acetate, high purity, which are used as raw material in the production of tantalum and niobium oxide-semiconductor capacitors to obtain the cathode sheath in the form of a solid electrolyte of manganese dioxide by pyrolysis of a mixed solution of these salts, in which the acetate tetrahydrate manganese is a necessary additional component. Technology of production of acetate tetrahydrate manganese high purity includes the following steps: 1. Leaching of the raw material, manganese carbonate, for which the original powder of manganese carbonate is poured 2-5%solution of chemically pure nitric acid at a ratio of liquid and solid phases is approximately 5:1 by volume and constant stirring for 5-30 minutes at a temperature of 20-50°C, followed by operations: filtering, for example, a Buechner funnel and washing the crystals of carbonate of manganese on the ionized water, for example, on the filter when the ratio of the liquid and solid phases 3:1 by volume. Thus there is a refining of the raw material due to the discharge from the waste solution of major impurities: chloride, iron, calcium, copper, lead; 2. Dissolution of carbonate of manganese in solution of pure acetic acid by chemical reaction MnCO3+2CH3COOH+3H2About→Mn(CH3Soo)2·4H2O+CO2↑-, what loads are cleared according to claim 1 manganese carbonate in 20%solution of chemically pure glacial acetic acid at the ratio of liquid and solid phases of 1.5:1 by weight in small portions during 30 minutes with constant stirring using a stirrer and spend dissolution at elevated temperature and constant stirring until the termination of allocation of gas bubbles and achievements of pH 5-6. The resulting product solution of acetate of manganese. The duration of the dissolution process is not standardized, because it depends on the performance of the installation; 3. Alkalinization of production of a solution of acetate of manganese, which in the final solution at a temperature of 45-55°C and stirring gradually add 20%aqueous ammonia solution to obtain a pH of 7-7,5, and then stirred production solution for 30 minutes. When this occurs the precipitation of residual Neretva imih impurities, mainly, hydroxides of heavy metals; 4. Filtering for approximately 20 minutes using a vacuum filter pre-clarified by sedimentation production of a solution of manganese acetate. When this occurs the separation of a solution of acetate of manganese precipitate impurities. The duration of the clarification process is not standardized, because it depends on the performance of the installation; 5. Evaporation of a solution of acetate of manganese, which is introduced into a solution of manganese acetate 46%acetic acid in a ratio of at least 1.7:1000 by volume to suppress unwanted hydrolysis of the acetate of manganese and reduce losses of manganese and evaporated the solution to the concentration 32-32,5 wt.%; 6. Crystallization from a solution of acetate of manganese, which, with constant stirring using a stirrer, is carried out by forced cooling in the temperature range from 50 to 15°C obtained according to claim 5 concentrated solution of manganese acetate as entered in the amount of 0.05 wt.% the seed crystal tetrahydrate of manganese acetate, followed by curing the resulting suspension crystalline precipitate acetate tetrahydrate of manganese in the final crystallization temperature, 15°C and continuous stirring for 15-45 minutes. 7. Department crystalline precipitate acetate tetrahydrate manganese tododaho solution by filtering the resulting suspension according to claim 6 using, for example, a vacuum filter, followed by washing the crystalline precipitate a saturated solution of pure acetate of manganese at a temperature equal to the final crystallization temperature, 15°C, and/or acetone at a ratio of liquid and solid phases is not less than 3:1 by volume with multiplicity washing 1-3. This gives the finished product is a crystalline powder acetate tetrahydrate of manganese. Below are examples of the implementation of technology for acetate tetrahydrate of manganese: the proposed method of (example 1) and the prototype method (example 2). Example 1 As a raw material for production of acetate tetrahydrate manganese high purity used the powder of manganese carbonate in the form of manganese (II) carbonate basic water mark "h" (MnCO3·mMn(OH)2·nH2O) GOST 7205-77 and acetic acid brand "H. including ice GOST 61-75. The original powder of carbonate of manganese contained impurities, wt.%: the chloride ions 0,0173, sulfate ions is 0, the calcium - 0,09614, iron - 0,00577, lead - 0,005, copper - 0,002. Getting tetrahydrate of manganese acetate with high purity was produced according to the above-described technology of the proposed method. When the leaching was used nitric acid brand "H. H." GOST 4461-77, the dissolution was carried out at a temperature of 45-55°C, and it took about 5 hours and clarification by sedimentation production p is the target acetate manganese took about 12 hours; evaporation was made up to concentrations 32-32 .5 wt.%; at the stage of crystallization has introduced a seed crystal acetate tetrahydrate of manganese in the amount of 0.05 wt.% and carried out forced cooling at a rate of 1°C. per minute and kept in suspension with constant stirring for 30 minutes; the crystalline precipitate acetate tetrahydrate manganese once washed with saturated, to 24.66%, solution of pure manganese acetate and acetone. Example 2 To obtain the tetrahydrate of manganese acetate was used electrolytic metal manganese GOST 6008-90 and the rest of the raw material as in example 1. The process of obtaining carried out in accordance with the process steps described in method prototype. The results are obtained in examples 1 and 2 product, acetate tetrahydrate of manganese, the content of the basic substance and impurities are presented in table 1. Were also made of niobium oxide-semiconductor capacitors C-52, par 16B×68 µf, with cathode plates obtained with the use of acetate tetrahydrate of manganese by the present method and the method prototype. Electrical characteristics of the capacitors are presented in table 2.
From the presented data in table 1 it follows that the process of obtaining acetate tetrahydrate manganese according to the claimed method allows to obtain a higher quality product compared with the method of the prototype with a higher content of basic substance, and with less impurities.
Presented in table 2 data shows that the tetrahydrate of manganese acetate obtained by the present method allows to manufacture a capacitor with better electrical characteristics, with lower values of leakage current tangent of loss, equivalent series resistance and impedance in comparison with the tetrahydrate of manganese acetate, obtained by the method prototype. Thus, the inventive method provides receiving tetrahydrate of manganese acetate with high purity and allows us to produce oxide-semiconductor capacitors with improved electrical characteristics. 1. The method of obtaining acetate tetrahydrate manganese, characterized in that it includes the leaching of manganese carbonate diluted chemically pure nitric acid followed by filtration, dissolution of manganese carbonate in a solution of glacial acetic acid, alkalization received production of a solution of manganese acetate aqueous solution, AMIA is a, filtering clarified by sedimentation solution of acetate of manganese separation from solution precipitate impurities, evaporation of the solution to the concentration 32-32,5 wt.% with the addition of acetic acid and crystallization from a concentrated solution of acetate of manganese by cooling, which is carried out in the temperature range from 50 to 15°C, with the introduction into the solution of the seed crystal acetate tetrahydrate of manganese in the amount of 0.05 wt.%, keeping obtained after crystallization suspension of a crystalline precipitate of manganese acetate at finite temperature crystallization under stirring, separating the crystalline precipitate of manganese acetate, followed by washing the crystalline precipitate a saturated solution of pure acetate of manganese and/or acetone at a temperature equal to the final crystallization temperature. 2. The method according to claim 1, characterized in that the leaching of carbonate of manganese use of chemically pure nitric acid, diluted to a concentration of 2-5%, with a ratio of liquid and solid phases is approximately 5:1 by volume). 3. The method according to claim 1, characterized in that the leaching of manganese carbonate is carried out at a temperature of 20-50°C. 4. The method according to claim 1, characterized in that the duration of the leaching of manganese carbonate is 5-30 minutes 5. The method according to claim 1, characterized in, Thu the alkalization of manganese acetate is carried out at a temperature of 45-55°C to obtain a pH of 7-7,5, gradually adding a 20%ammonia solution with constant stirring. 6. The method according to claim 1, characterized in that the one stripped off acidification of the solution are 46%acetic acid is introduced in a ratio of at least 1.7:1000 by volume. 7. The method according to claim 1, characterized in that after crystallization, the suspension is obtained a crystalline precipitate is maintained at a constant stirring for 15-45 minutes 8. The method according to claim 1, characterized in that the washing of the crystalline precipitate of manganese acetate saturated solution of pure acetate of manganese and/or acetone is carried out at a ratio of liquid and solid phases is not less than 3:1 with multiplicity washing 1-3.
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