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Invention relates to a process for starting up a separating process for purificative removal of acrylic acid crystals from a suspension S of crystals thereof in mother liquor with a hydraulic wash column, which has a crystal melt circuit including crystal melt space and also a process space and a distributor space which are separated by a floor with passages connecting the two spaces, where the crystal bed is formed for the first time by first filling the crystal melt circuit and, at least partly, the process space with an acrylic acid-comprising startup liquid, whose acrylic acid crystal formation temperature is less than or equal to the temperature of the suspension S increased by 15°C, and then continuing the filling of the wash column with the suspension S and optionally with control liquor until the difference between the pressure in the crystal melt space and the pressure in the distributor space falls suddenly, the arithmetic mean of the total waste liquor flow flowing through the filters of the filter tubes of the wash column up to this point in time, based on the area of all the filters, being not more than 80 m3/(m2·h). In the course of startup of the separating process for first development of the crystal bed in the process space the crystal melt circuit comprising the crystal melt space, and the process space of the previously unfilled wash column, are at first filled with an acrylic acid-comprising startup liquid AT such that the fill height of the startup liquid AT in the process space overtops at least the removal device, then the filling of the wash column is continued by using the pump P2 to conduct a stream ST* of the suspension S from the source QS through the delivery connections E1, E2 via the distributor space and through the passages U into the process space of the wash column and optionally using the pump P3 to conduct a substream of the waste liquor stream SM* conducted out of the wash column through the filter tubes as source QT*, as control liquor stream SL* through the delivery connections C1, C2 via the distributor space and the passages U and/or directly into the process space of the wash column, at least until the time tS, is attained at which the pressure difference PD=PK-PV, where PK - is the pressure existing at any desired point in the crystal melt space at a particular time in the supply of the stream ST*, and PV - is the pressure which exists at the same time at any desired point in the distributor space, no longer rises or remains constant as a function of the duration of the supply of the stream ST* but decreases suddenly, with the proviso that, until the time tS the mean superficial velocity on the filters F, calculated as the arithmetic mean of the total waste liquor flow ST* which flows at the particular time through the filters F of the filter tubes during the supply of the stream SM*, divided by the total area of all filters F, is not more than 80 m3/(m2·h), the acrylic acid-comprising startup liquid AT is one from which, in the course of cooling until crystallization sets in, the crystals which form in the course of crystallization are acrylic acid crystals, and between the crystal formation temperature TKB reported in degrees Celsius, of these acrylic acid crystals in the startup liquid AT, and the temperature TS reported in degrees Celsius, of the suspension S of the stream ST*, the following relationship is satisfied TKB≤TS+15°C. |
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Invention relates to method of obtaining stable in storage liquid superbasic salt of alkali or alkali earth metal. Method includes reaction of mixture of alkali or alkali earth base and aliphatic or aromatic carboxylic acid, in which equivalent ratio of metal base and carboxylic acid constitutes more than 1:1, in presence of liquid hydrocarbon, and carboxylation of reaction mixture in presence of 1,3-diketone. Also claimed are liquid superbasic salt of alkali or alkali earth metal, suitable for application in mixed metal stabilisers and halogen-containing polymer composition. |
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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 obtaining lead stearate Method of obtaining lead stearate includes the interaction of stearic acid with a water suspension of lead oxide with heating and intensive mixing with further filtration, drying, pre-packing and packing. Water, acetic acid as a catalyst and lead oxide are loaded with obtaining the water suspension of lead oxide. After that, it is heated to a temperature of 75-80°C and stearic acid is added, circulation is performed for 60-90 min at a temperature of thermal processing to 75-80°C. After that, the suspension of lead stearate is transferred into a condition of a stable emulsion, exposed at the said temperature for 100-120 min to pH of the solution being 4.0-6.0, acidic number to 0.5 mg and the content of the main substance 26-28%, with the following addition of water, mixing and filtration. The product drying is performed by hot air at a temperature of 60-80°C. |
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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 stearate Method of producing zinc stearate involves reacting stearic acid and zinc hydroxide with heating and intense stirring, followed by heat treatment, filtration, drying and packaging. When reacting stearic acid and zinc hydroxide, hydrochloric acid is further added to the mixture as a catalyst. The reaction is carried out in an aqueous medium which is heated to 96-98°C. Circulation is carried out for 2.0 hours. The zinc stearate suspension is then turned into a stable emulsion state and held at that temperature for 30-45 minutes. Further, heat treatment is carried out to aggregate particles, which are then held for 20-25 minutes to solution pH 4.5-5.0, acid number of 5.0 mg and basic substance content of 10-11%. Water is added, followed by stirring and filtering. The precipitate is dried with hot air at temperature of 80-90°C. |
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Method of obtaining calcium stearate Invention relates to improved method of obtaining calcium stearate by interaction of stearic acid and calcium hydroxide with heating and intensive mixing, further filtration and drying of sediment. Interaction of stearic acid and calcium hydroxide is performed in water medium, with emulsion being heated to 58-65°C, being brought into state of stable emulsion, kept at said temperature for 20-40 minutes until solution pH is 8.0-9.0, with further thermal processing for aggregation of particles with constant stirring and increase of temperature to 70-85°C, and exposure for 10-15 minutes to solution pH 7.5-9.0; after which water is poured in and mixing and filtration are carried out. |
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Method of obtaining dibasic lead stearate, polyvinyl chloride stabiliser Invention relates to petrochemical synthesis, in particular to method of obtaining dibasic lead stearate polyvinyl stabiliser, and can be applied as thermostabiliser in production of polyvinylchloride resins and made of them products, for instance, in casting under pressure, non-transparent and semi-transparent insulation for cables, which additionally possesses strong lubricating property in extrusion, etc. Essence of method of obtaining dibasic lead stearate polyvinyl stabiliser consists in the following. Preliminary preparation of raw material is carried out, after which interaction of sodium hydroxide, lead oxide and stearic acid takes place in reactor in heated state with intensive mixing, the process being carried out in solid phase, with further precipitation and synthesis of dibasic lead stearate, thermal processing of thereof suspension, suspension circulation, filtration, drying, pre-packing and packing of end-product, sodium hydroxide is charged, water suspension of litharge is prepared and solid stearic acid is charged, reaction mass is heated to temperature 45°C, kept at said temperature for 15-20 minutes, then temperature is raised to 60-65°C within 25-35 minutes and kept until homogeneous mass is obtained, with suspension circulation being carried out during entire cycle of synthesis, and when synthesis of dibasic lead stearate finishes, suspension is subjected to thermal processing in order to aggregate particles by heating to temperature 90-98°C, keeping for 10-15 minutes with continuous mixing until acid number of product reaches not more than 1 mg KOH/g. |
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Method of obtaining ammonium salts of fumaric or succinic acid Invention relates to improved method of obtaining ammonium salts of fumaric or succinic acid, which are used for production of biologically active additives or medications, as well as in veterinary and food industry. Method lies in neutralisation of respective acid with neutralising compound in water medium, where as neutralising compound ammonium carbonate or bicarbonate is used, with molar stoichiometric or exceeding stoichiometry by 4-5% ratio of acid and ammonium carbonate or bicarbonate, neutralisation is carried out in saturated water solution of synthesised salt, at temperature not higher than 40°C, with further product separation and its drying at temperature not higher than 70°C. Method can be realised in conditions of industrial production. It is possible to obtain ecologically pure salts with content of main substance not lower than 99.0 wt %, and output not lower than 98%. |
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Method of producing salt solution of dibasic acids and diamines Invention relates to an improved method of producing a salt solution of dibasic acids and at least one diamine for producing a polyamide. The method of producing an aqueous solution (A) of salts of dibasic acids and at least one diamine is realised by mixing at least two dibasic acids and at least one diamine, with mass concentration of the salt in the range of 40-70%, wherein the method includes the following steps of: obtaining, in a reactor, an aqueous solution (A') of at least one diamine and at least dibasic acid, wherein molar ratio dibasic acid/diamine is less than 1 and preferably less than or equal to 0.9; feeding into said reactor, in which there is a liquid containing water and diamine at temperature ranging from 55 to 95°C (inclusively) and preferably ranging from 60 to 90°C (inclusively), a stream (B') which contains a dibasic acid, optionally a stream which contains diamine and optionally a stream which contains water; wherein the flow rate of one or more of the fed streams is controlled in order constantly keep temperature of the solution in the reactor below boiling point at the given operating pressure therein; wherein the amount of water and diamine in the liquid component, as well as the flow rate of the fed streams is controlled in order to constantly keep molar ratio of the dibasic acids/diamines less than 1; wherein the dibasic acid in stream (B') is an aliphatic or cycloaliphatic dibasic acid in which the number of carbon atoms is greater than 10, or an aromatic dibasic acid; and the aqueous solution (A'), coming from the fist step, is mixed with stream (B"), which contains at least one dibasic acid, wherein the dibasic acid is an aliphatic or cycloaliphatic dibasic acid in which the number of carbon atoms is less than or equal to 10, and optionally an additional amount of water and/or diamine to obtain an aqueous solution (formed by a mixture of (A') and (B")), in which the molar ratio dibasic acids/diamines ranges from 0.9 to 1.1 and preferably from 0.98 to 1.02 (inclusively); wherein said solution is heated to temperature not higher than the boiling point of the solution at operating pressure at least through release of heat of reaction between at least one diamine and dibasic acids; wherein said operations are carried out to obtain a solution (A) of dibasic acids and at least one diamine with the required concentration and composition. |
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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 for preparing diisopropylammonium dichloroacetate Invention refers to organic chemistry and medicine, and concerns a method for preparing diisopropylammonium dichloroacetate used in medicine by a reaction of diisopropylamine with dichloracetic acid at temperature 25-55°C in a medium of prepared aqueous solution of diisopropylammonium dichloroacetate prepared by a reaction of an aqueous solution of diisopropylamine with dichloracetic acid at temperature max. 10°C to be crystallised with cooling, filtration and drying. |
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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 transferring heat to liquid mixture containing at least one (meth)acrylic monomer Invention relates to a method of transferring heat to a liquid mixture containing at least one (meth)acrylic monomer selected from a group comprising acrylic acid, methacrylic acid, hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, glycidyl acrylate, glycidyl methacrylate, methyl acrylate, methyl methacrylate, n-butyl acrylate, isobutyl acrylate, isobutyl methacrylate, n-butyl methacrylate, tert-butyl acrylate, tert-butyl methacrylate, ethyl acrylate, ethyl methacrylate, 2-ethylhexyl acrylate and 2-ethylhexyl methacrylate, through an indirect heat exchanger on whose primary side a fluid heat carrier flows and on whose secondary side simultaneously flows said liquid mixture containing at least one (meth)acrylic monomer, wherein the liquid mixture containing at least one (meth)acrylic monomer, in order to reduce contamination, additionally contains at least one active compound other than (meth)acrylic monomers which is selected from a group consisting of tertiary amines, salts formed from a tertiary amine and a Bransted acid, and quaternary ammonium compounds, under the condition that none of the tertiary and quaternary nitrogen atoms in the at least one active compound bears a phenyl group but at least some of said tertiary and quaternary nitrogen atoms bear at least one alkyl group. |
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Metallo-β-lactamase inhibitors Maleic acid derivatives having general formula |
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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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Production of acidic propionates Invention relates to a solid composition having antifungal action and containing at least one compound which contains propionic acid, selected from a group comprising compounds of formula (I): (Mn+)(H+)x(CH3CH2C(O)O-)(n+x) (I), in which Mn+ denotes sodium, wherein n denotes 1, and x denotes a number from 1.8 to 2.2, [NaH2(CH3CH2C(O)O)3] and [NaH1.3(CH3CH2C(O)O)2.3], wherein content of said at least one compound containing propionic acid is at least 96 wt % per total weight of the composition; and a method of preparing a solid composition containing at least one compound of formula (I) containing propionic acid, in which Mn+ denotes sodium, wherein n denotes 1 and x denotes a number from 0.25 to 5, according to which, from neutral sodium propionate and propionic acid in molar ratio from 1:0.25 to 1:5, while heating, a homogeneous mixture is obtained or at least partial solidification of this mixture is caused, wherein moisture content of the homogeneous mixture is less than 1 wt % per total weight of the mixture or crystallisation of said mixture is caused, wherein moisture content of the homogeneous mixture varies from 1 to 15 wt % per total weight of the mixture. |
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Perfluorocarboxylic acid salt and synthesis method thereof Invention relates to an improved method of producing a perfluorocarboxylic acid salt, having iron content of at most 10 ppm by weight, and having formula (1), where RF denotes a C1-10-univalent perfluorinated organic group, each of X1 and X2 independently denotes a fluorine atom or a trifluoromethyl group, k is an integer not less than 1, and M+ denotes an ammonium ion or an alkyl-substituted ammonium ion, which involves a step for hydrolysis of a compound (2) of formula (2) with water using reaction apparatus equipped with a reactor in which at least its inner surface is made from a fluoropolymer, where the amount of the water used ranges from 0.9 to 1.2 mole per mole of compound (2), wherein content of HF in the reaction product is at most 0.1 wt %, and the obtained reaction product is distilled for purification purposes, thereby obtaining a compound (3) of formula (3), and a step for formation of a salt of compound (3) in order to obtain a salt of perflurocarboxylic acid, where RF, X1, X2 and k are the same as in formula (1). The method enables to obtain a perfluorocarboxylic acid salt with excellent capacity to reduce surface tension, which can be used to produce fluorinated polymers without colouration of polymers under the effect of high temperature. Rp(OCF(X1)CF2)k-1OCF(X2)COO-M+ (1) Rp(OCF(X1)CF2)k-1OCF(X2)COF (2) RF (OCF(X1)CF2)k-1OCF(X2)COOH (3). |
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Method of recycling monochloroacetic acid production wastes (versions) Invention relates to chemical engineering and specifically to methods of recycling monochloroacetic acid production wastes, used in production of carboxymethyl cellulose, pharmaceutical preparations, pesticides and ethylene diamine tetraacetic acid. Methods of recycling monochloroacetic acid production wastes involve treating the mother solution obtained from purifying monochloroacetic acid, wherein treatment is carried out by neutralising the mother solution with 30-44% aqueous sodium hydroxide solution at temperature 40-45°C until achieving pH 7-7.5, followed by reaction of the reaction mixture with 25% aqueous ammonia solution in molar ratio of monochloroacetic acid to ammonia equal to 1:1.39-1.46 until achieving pH 8.5-9, with step-wise increase in temperature, first to 50-70°C for 2-3 hours, maintaining pH of the mixture by adding 30% aqueous sodium hydroxide solution, and then to 80-105°C for 1-2 hours, followed by cooling and, if necessary, followed by neutralisation of the reaction mixture with hydrochloric acid at temperature 15-60°C for 0.5-2 hours until pH of the mixture equals 1. |
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Method of preparing diacid/diamine salt solutions Invention relates to an improved method of preparing diamine and diacid salt solutions, obtained by mixing diacid and diamine, with weight concentration of the salt ranging from 50% to 80%. The method involves obtaining in a first reactor an aqueous solution of diamine and diacid with molar ratio of diacid to diamine ranging from 1.5 to 5 and with concentration of dissolved particles in water ranging from 40 to 75 wt %, by feeding into the said reactor either an aqueous solution with at least 50 vol. % diamine and diacid with molar ratio ranging from 1.5 to 5, or water making up at least 10% of the total amount of water fed into said reactor, a stream containing diacid, a stream containing diamine and, possibly, a stream of water at temperature T1, where the flow of the fed streams containing acid and the stream containing diamine are is regulated such that temperature of the solution in the reactor constantly remains below the boiling point at operating pressure of the reactor, and molar ratio of diacid to diamine is greater than 1.1, wherein the amount of the fed acid is at least 90% of the total weight of the acid needed to obtain the desired amount of aqueous salt solution; the amount of the fed water is at least 75% of the total weight of the water needed to obtain the desired amount of aqueous salt solution. The aqueous solution obtained in the first reactor is then moved to a second reactor fitted with a condenser and a stream containing diamine is fed into the second reactor to obtain molar ratio of diacid to diamine between 0.9 and 1.1, wherein the temperature of the solution is raised to a value at most equal to boiling point of the solution at operating pressure at least by removing heat released during the reaction between the diamine and diacid and, possibly, the amount of water and/or additional diacid need to obtain a salt solution with the desired concentration and molar ratio of diacid to diamine is used. |
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Method of producing solid sodium diformate composition Invention relates to a method of producing a solid sodium diformate composition, having forming acid content of at least 35% of the total weight of the sodium diformate composition, in which aqueous solution (E) is prepared at high temperature, said solution containing sodium formate and formic acid in molar ratio HCOOH:HCOONa higher than 1.5:1, and having molar ratio HCOOH:H2O of at least 1.1:1, said aqueous solution (E) is crystallised to obtain a solid phase and a mother solution, and the solid phase is separated from the mother solution, where (i) the mother solution is completely or partially fed into a distillation apparatus; (ii) the mother solution in the distillation apparatus is mixed with a sodium-containing base to obtain a mixture (B) which contains sodium formate and formic acid; (iii) the mixture (B) obtained at step (ii) is mixed with formic acid to obtain aqueous solution (E); or the mixture (B) obtained at step (ii) is removed from the distillation apparatus and taken for crystallisation, or, at the crystallisation step, mixed with formic acid to obtain an aqueous solution; and (iv) excess water is primarily removed by tapping from the distillation apparatus; the invention also relates to use of the solid sodium formate composition obtained using the disclosed method as an animal feed additive, particularly feed for non-ruminants, especially pigs and/or birds. |
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Method of producing palladium propionate Invention relates to synthesis of platinum metal salts, particularly palladium salts and specifically palladium propionate. The method of producing palladium propionate involves dissolving palladium metal in concentrated nitric acid, evaporation of the obtained solution, wherein after evaporation and before crystallisation of the palladium (II) nitrate salt at solution temperature (15-80)°C, the palladium nitrate is treated with NO taken in amount of (0.3-0.7) m3 (standard conditions) per 1 kg of the initial palladium metal and propionic acid is added in amount of (2.0-3.0) l per 1 kg of the initial palladium metal or propionic acid anhydride in amount of (2.0-2.5) l per 1 kg of palladium. The formed solution or suspension heated in an inert gas atmosphere in amount of approximately 20 m3 (standard conditions) per 1 m3, at temperature (90-120)°C for (30-60) minutes if propionic acid is added, or at temperature (80-110)°C for not less than 30 minutes if propionic acid anhydride is added, and the obtained solution or suspension is cooled to temperature not higher than 20°C, with crystallisation of the product for not less than 6 hours. |
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Invention relates to a chrysophanol conjugate or its derivative, characterised by general formula (I), in which R1-R8 is a group selected from -H, -OH, -OCH3, -CH3, provided that not less than two groups from R1-R8 denote -H or provided that one or two of groups R2, R3, R6 and R7 are a -COOH group, M is a nitrogen organic base selected from a group comprising chitosamin, glucosamin, or a basic amino acid selected from a group comprising arginine, lysine, carnitine, and group M is bonded to the chrysophanol part in the conjugate. |
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Metal salts of fatty acids and synthesis method thereof Method for synthesis of metal salts of fatty acids as a process additive for rubber mixtures involves saponification of fatty wastes with 8-12% aqueous sodium hydroxide solution at temperature 80-90°C and then adding water to the formed hydrolysate, where the water is added in an amount which is equal to or 1.5-2.0 times greater than the volume of the hydrolysate, and then with a water-soluble zinc or calcium salt or mixtures thereof. The fatty wastes used is a fatty portion of soap stock of vegetable oil obtained from the complex effect of an electrolyte or deemulsifying agent on the wastes, except a preliminary distillation step. The metal salts have melting point of 65-85°C, density 1100-2200 kg/m3 and weight ratio of fatty acids 77-82%. |
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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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Method of producing iron (iii) benzoate 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. |
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Sodium diformate synthesis method 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. |
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Method of producing complex stabilisers for chlorine-containing polymers 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. |
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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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Purification of carboxylic acids through complexing with selective solvents 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. |
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Method of producing heat stabilisers for chlorine-containing polymers 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. |
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Method of obtaining manganese (ii) benzoate 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+), where nMn and - number of moles of metal and its peroxide in the load, the liquid phase solvent used is butylacetate and the stimulating additive of molecular iodine is taken in amount of 0.02-0.05 mol/kg; the process is started and carried out while stirring intensely and under forced cooling at temperature ranging from room temperature to 45-60°C until achieving virtually quantitative consumption of metal and its peroxide into a product, after which stirring and forced cooling of the reaction mixture are stopped, the reaction mixture is separated from the glass beads and filtered, the glass beads and reactor components are washed with a liquid phase solvent which is then taken for washing the residue on the filter, the obtained filtrate is cooled to 7-10°C and kept at that temperature for 2-2.5 hours for completion of crystallisation of the product, the suspension formed is filtered, the obtained residues of the product are separately taken for cleaning through recrystallisation, and the filtrate is returned for the repeated process. Output the extracted solid product is 87-97% of the theoretical output. A portion of the product is returned for the repeated process together the filtrate. |
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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 producing carboxylates of rare-earth elements 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. |
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1-13c-caprylic acid synthesis method 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. |
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Manganese (ii) fumarate synthesis method Method of synthesis of manganese (II) fumarate through direct reaction of metal with acid is presented. The process is carried out in a vertical type bead mill with mass ratio of beads to the reaction mixture equal to 1:1, and the liquid phase is a solution of fumaric acid in an organic solvent with content of acid of 0.70-1.80 mol/kg. Manganese is taken in stoichiometric amount with acid or in deficiency of up to 5%. The process is started by loading the liquid phase solvent and acid and preparation of the acid solution in a bead mill, after which metal is loaded and the process is carried out at temperature ranging from 25 to 35°C while preventing spontaneous increase of temperature through forced cooling and controlling through sample taking and determination of manganese salt in the samples and residual amount of acid until attaining values close to calculated values during quantitative conversion of the reagent in deficiency. After that stirring and cooling are stopped. The suspension of the reaction mixture is separated from the glass beads, cooled to temperature between 5.2 and 6.2°C and filtered. The filtering residue is washed with the liquid phase solvent, cooled to approximately the same temperature, and taken for purification by recrystallisation. The filtrate and the washing solvent are returned to the repeated process. |
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Iron (ii) oxalate synthesis method Invention relates to a method of producing iron (II) oxalate by directly reacting metal with acid in the presence of atmospheric oxygen and a liquid phase while stirring. The process is carried out in a bead mill. The liquid phase solvent used is water with mass ratio of the liquid phase to glass beads equal to 1:1, content of oxalic acid in the initial load is between 0.5 and 2.0 mol/kg, and content of stimulating sodium chloride additive is between 0.02 and 0.10 mol/kg. Crushed grey cast iron which is stirred by a blade mixer is taken in amount of 30% of the mass of the rest of the load. The process is started and carried out at temperature in the interval from (50±2) to (93±2)°C while bubbling air under conditions for stabilising temperature using a heated liquid bath and controlling using a sample taking method and determination of content of iron (II) and (III) salts in the samples, and residual quantity of acid up to virtually complete conversion of the latter into salt. After that air bubbling, external heat supply for stabilising temperature and stirring are stopped. The suspension of the reaction mixture is separated from the glass beads and particles of unreacted metal alloy and filtered. The filtration residue is washed with distilled water and taken for further purification through recrystallisation, while the filtrate and the washing water are returned to the load for the repeated process. Iron (II) oxalate, which is separated from the reaction mixture by traditional filtering, is virtually the only product of conversion. |
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Method of producing iron (ii) fumarate Iron (II) fumarate can be used in different fields of chemical practice, in analytical control and in scientific research, through direct reaction of iron with fumaric acid in the presence of a catalyst, where the catalyst used is molecular iodine in amount of 0.025 to 0.1 mol/kg of the initial load, iron is taken in large excess in form of shells on the entire height of the reactor, false bottom and blade mixer, as well as in form of crushed cast iron and(or) reduced iron powder, the liquid phase solvent used is butylacetate, in which iodine and fumaric acid are at least partially dissolved, where fumaric acid is taken in amount of 0.8 to 1.2 mol/kg of the initial load, loading is done in the sequence: glass beads, liquid phase solvent, fumaric acid, iodine, and then crushed cast iron and(or) reduced iron powder; the process is started at room temperature and is carried out in a vertical type bead mill with ratio of mass of beads to mass of crushed cast iron and(or) reduced iron powder equal to 4:1, at temperature ranging from 18 to 45°C while bubbling air with flow rate of 0.95 l/min-kg of the liquid phase and using forced cooling and controlling using a sampling method until complete exhaustion of the loaded acid for formation of salt, after which stirring and cooling are stopped, the reaction mixture is separated from glass beads and unreacted crushed cast iron and(or) reduced iron powder and filtered, the residue is washed with butylacetate and taken for recrystallisation, and the filtrate and washing butylacetate are returned to the repeated process. Amount of acid used in extracting the product (without loss during purification) ranges from 89 to 96.5%, which depends on conditions for carrying out the process. |
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Method of producing basic phthalate of iron (iii) Invention relates to an improved method of producing basic phthalate of iron (III), which is used in chemical practice, analytical control and scientific research, through direct reaction of iron with atmospheric oxygen and phthalic acid in the presence of organic solvent, where the stimulating additive used is hydrochloric acid and inorganic chlorides in amount ranging from 0.013 to 0.062 mol/kg of the load. The liquid phase solvent is n-butyl alcohol iron which is crushed and moved in the reaction zone in form of steel balls with diametre ranging from 2.2 to 3.7 mm, alone or in combination with crushed cast iron in any mass ratio. Initial content of phthalic acid is varied from 1.0 to 1.5 mol/kg of the load. The reactor used is a vertical type bead mill with the grinding agent in form of steel balls and crushed alloy of iron together with glass beads in mass ratio of iron-containing reagent, beads and the rest of the load equal to 1:1:0.6 with a spill pipe as a bubbler during the process. Loading is done in the following sequence: grinding agent and moved metal, liquid phase solvent, phthalic acid, chlorine-containing stimulating agent, and the process itself starts with heating contents of the reactor to 35°, is carried out with self-heating in the range 35 to 50°C while stirring continuously, bubbling air at a rate of 2.3 to 3.1 l/(min kg of load), while maintaining temperature using a cooling liquid bath and controlling the process using a sampling method until exhaustion of all loaded acid, after which bubbling is stopped. Suspension of the reaction mixture is let to flow under gravity through a net lying in the field of a permanent magnet into the receiving tank of a vacuum filter, after which it is filtered. The residue is washed with the liquid phase solvent and taken for purification, and the primary filtrate and washing solvent are returned to the repeated process. |
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Crystalline calcium salt of gluconic acid or its compound with excipients is processed in grinding activator devices, or to a value of supplied specific energy of not more than 10.4 kJ/g and achieving amorphous-crystalline state, or to a value of specific energy of not less than 10.5 kJ/g and achieving amorphous state. The obtained substances are analysed using X-ray diffraction, infrared, NMR, EPR spectroscopy, mass- and chromatography-mass spectrometry and differential thermal analysis. |
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Method of producing malonate and manganese (ii) succinate Invention relates to a method of producing malonate or manganese (II) succinate, which can be used in different areas of chemical practice, in analytical control and scientific research, through direct reaction of a metal and its dioxide with carboxylic acid in the presence of an organic solvent and stimulating iodine additive in a vertical type bead mill with a high-speed mixer and glass beads as grinding medium, where manganese, its dioxide and carboxylic acid in the initial load are taken in molar ratio 1+x):1:(2+x) so as to obtain (2+x)m moles of salt, where x in the given molar ratio of reagents equals 0.4±0.1 for amber acid and 1.0±0.1 for malonic acid, and m is the number of moles of manganese dioxide in the load; iodine is taken in amount of 0.05 mol/kg of the reaction mixture after loading organic solvent and acid, but before loading manganese dioxide and metal. Total mass of acid, metal and its dioxide lies between 15 and 25% of the mass of the initial load, and ratio of mass of beads to mass of the load is 1:1. The process is started at room temperature and carried out under forced cooling conditions at temperature ranging from room temperature to 40°C while controlling by taking samples until exhaustion of all loaded reagents into the target salt, after which the process is stopped. The suspension of the final reaction mixture is separated from the beads and filtered. The product residue is washed with a liquid phase solvent and taken for purification from trace metal and its dioxide through recrystallisation, and the filtrate and washing solvent are returned to the repeated process. |
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Method of producing manganese (ii) fumarate from manganese metal and manganese (iii) oxide Invention relates to an improved method of producing manganese (II) fumarate from manganese metal and its oxide (III) through direct reaction of the metal and its oxide Mn2O3 with an acid in the presence of a liquid phase and a stimulating iodine additive in a vertical type bead mill with glass beads as grinding agent. The metal and its oxide are loaded in molar ratio (2±0.1):1 in total amount of 7.87 to 10.93% of the mass of the load. Acid is added with 15 to 25% excess of the calculated value, equal to the number of moles of metal and twice the number of moles of metal oxide in the load. The base of the liquid phase is isoamyl alcohol, in which the iodine stimulating additive is dissolved in amount of 0.02 to 0.05 mol/kg. Glass beads are loaded first, in mass ratio to the reaction mixture of 1.35:1, and then later the liquid phase solvent, acid and stimulating additive, and after brief stirring, metal oxide and metal, stirring all the while. Taking this moment as the beginning of the process, forced cooling is introduced right away. Operating temperature is stabilised in the range 33 to 45°C and in this mode, the process is carried out until virtually quantitative conversion of metal and its oxide to the target salt, after which stirring and forced cooling are stopped. The reaction mixture is separated from the glass beads, cooled to temperature 5 to 6°C and kept at that temperature for 1 to 2 hours. The solid phase of the target salt is filtered off and washed with isoamyl on a filter cooled to approximately the same temperature, after which it is taken for purification by recrystallisation. The filtrate and the cleaning solvent, containing excess acid, the bulk of the stimulating additive and a certain amount of dissolved target salt, are returned for loading in the repeated process. The process is carried out in light temperature conditions. The target substance can be easily separated. |
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Invention refers to a new product in the form of solution for treatment of benign, virus, premalignant and malignant nonmetastasing skin affections, dysontogenetic lesions of visible mucous membranes, skin mycoses, wrinkle correction and senile pigment spots. The product represents a compound of general formula H2SeO3·x·[R-CXY-(CH2)m-COOH], where x=2-6 prepared from reaction of selenium dioxide and haloid carboxylic acids of general formula R-CXY-(CH2)m-COOH, where R = phenyl, alkyl of general formula CnH2n+1; n=1-5, X=H or Y, Y=F, CI, Br or J, m = 0-10. Besides, the invention concerns a product in the form of solution for treatment benign, virus, premalignant and malignant nonmetastasing skin affections, dysontogenetic lesions of visible mucous membranes, skin mycoses, wrinkle correction and senile pigment spots, containing 0.1-50 wt % of said product, 1-99 wt % of haloid carboxylic acids and the rest - water. Also the invention concerns method of treatment of various skin diseases, including topic applications of the product. |
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Method of obtaining nickel (ii) oxalate dihydrate Invention relates to improved method of obtaining nickel (II) oxalate NiC2O4·2H2O, which includes preparing of reaction water solution, which contains nickel (II), precipitation of nickel oxalate, separating of sediment from solution and its drying, in which as nickel source used are solutions of nickel chloride, nitrate, sulphate, and as reagent-precipator used is anionite AB-17-8 in oxalate form. Obtained product can be applied in industry for producing catalysts, metal films, polymetal alloys, ceramic-metal and ferromagnetic substances, as well as in production of electrovacuum devices. |
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Method for preparation of manganese oxalate (ii) Invention is related to improved method for preparation of manganese oxalate (II) by means of direct interaction of metal with acid in bead mill in presence of liquid phase, in which manganese and oxalic acid are loaded into bead mill in stoichiometric ratio in amount of 0.75-2.4 mole/kg of load at mass ratio of load and glass beads of 1:1.2, liquid phase dissolvent used is water or organic substance, or mixture of organic substances; loading is carried out in the following sequence: liquid phase dissolvent, acid, then metal; process is started at room temperature and is carried out under conditions of forced cooling in the temperature range of 18-39°C with control over procedure by sampling method to practically complete spend of loaded reagents for product making, afterwards mixing and cooling are terminated, suspension of reaction mixture is separated from glass beads and filtered, salt deposit is sent for product cleaning from traces of non-reacted metal, and filtrate is returned into repeated process. |
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Method of obtaining detergents for lubricants Invention relates to improved method of salicylates of alkaline earth metals for application as detergents for lubricating materials. Method of obtaining alkylated salicytates of alkaline earth metals includes following stages: A) alkylating salicylic acid with linear α-olefin, containing, at last, 14 carbon atoms, in presence of water-free methane sulfonic acid with formation of oil-soluble alkylated salicylic acid; B) neutralisation of oil-soluble alkylated salicylic acid; C) excessive alkalisation of oil-soluble alkylated salicylic acid by carboxylating lime by means of CO2 in presence of oxygen-containing organic solvent and surface-active substance; D) filtration of stage (C) product; and E) removal of solvent by distillation. Alternatively, alkylsalicylic acid can be subjected to interaction with preliminary processed with alkali highly-alkaline sulfonate of earth alkaline metal, for instance, with calcium sulfonate, in order to obtain salicylate salts of earth alkaline metals with different per cent content of dispersed salts of alkaline earth metals carbonates. In claimed method it is not necessary to filter end product which is preferable doe industry. |
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Method of chloroacetic sodium salt production Invention refers to organic chemistry, to chlororganic technology, specifically to advanced method of chloroacetic sodium salt production allowing for high quality with minimum power inputs. Method of chloroacetic sodium salt production (Na-CA) is characterised by that dry initial components that are soda ash (Na2CO3) and chloroacetic acid (CA) are continuously dispensed in stoichiometric ratio to desintegrator or dismembrator with linear speed of disk pins 30-150 m/s, where exposed to mechanochemical influence. Thereafter produced Na-CA is continuously supplied to drying. Produced in offered method Na-CA completely meets quality requirements of standard documents. |
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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. |
Another patent 2551220.