Method of producing iron (iii) benzoate |
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IPC classes for russian patent Method of producing iron (iii) benzoate (RU 2412153):
 Method of producing manganese (ii) m-nitrobenzoate / 2412152
Invention relates to a method of producing manganese (II) m-nitrobenzoate by reacting metal with acid in the presence of an oxidising agent, organic liquid phase and stimulating additive in a bead mill. The oxidising agent used is manganese peroxide taken in amount of 0.25-0.50 mol/(kg of the initial charge) and in molar ratio to metal equal to 1:1-1:3. The acid is taken in amount of (2.05÷2.15)
 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 iron benzoate (iii) / 2326861
Invention pertains to the perfection of the method of obtaining iron benzoate (III) from magnetite and crushed cast iron with their reaction with benzoic acid. The method is achieved through reaction of iron and its oxide with benzoic acid in an organic solvent in the presence of a stimulation additive in a small vertical mill. The liquid phase used is a 2.0-3.5 mol/kg solution of benzoic acid in a mixture of dimethyl formamide and an h-butyl spirit in a volume ratio of 2:3. The liquid phase is dosed with glass beads in a ratio of 1:1 and crushed pieces of cast iron with maximum linear diameter of up to 5 mm in a ratio of (3.3-4):1. The iron oxide Fe3O4 (magnetite) is loaded in a molar ratio to the acid of 1:(14-20). The stimulating additive used is molecular bromine or iodine in a quantity of 0.1 mol/kg. The process starts with preparation of the solution of the benzoic acid in a mixture solvent with heating, and addition and dissolving of the stimulating additive. At the end, the crushed cast iron and the iron oxide are added and heated to 70-90°C, with routine control using the method of selecting samples for accumulation of iron (II) and (III) salt in the reaction mixture until a practically quantitative disintegration of the acid. Stirring is then stopped. The reaction mixture is the separated from the glass beads and unreacted particles of cast iron, by passing through a filtering partition wall in the form of a group openings with diameter of 0.6-0.8 mm in the field of a magnet, are cooled down to 5-14°C with stirring and are taken for filtration. The sediment of the product is washed in a cooled solvent of a liquid phase, which is mixed with the primary filtrate and returned into the repeated process. The salt is accumulated and taken for cleaning through crystallisation.
Method of obtaining iron benzoate (iii) / 2326107
Invention pertains to the improved method of obtaining iron benzoate (III) through interaction of crushed iron with an acid with sparging air as an oxidising agent with use of stimulating additives in the reactor with a high speed blade mixer, in which the liquid phase is in the form of a 3.5-3.9 mol/kg solution of benzoic acid in a mixture of dimethyl formamide and n-butyl alcohol in mass ratios 1:1-1:1.5, containing 0.03-0.07 mol/kg iodine as a stimulating additive, which is brought into intensive contact with the crushed iron in mass ratio 4.44:1. The process itself starts with preparation of a solution of benzoic acid and iodine in a solvent mixture and is put into a vertical bead mill with mass ratios of the liquid phase to the glass bead of 1:1 with sparging air at a rate of 0.3-0.5 l/min for 1 kg of the liquid phase and temperature between 70°C and 80°C, maintained through a liquid heating bath, until full expenditure of the loaded acid. Mixing is then stopped. The reaction mixture is separated from the glass beads and unreacted particles of iron by passing through a metallic net, located in the field of a magnet. Filtering is then carried out. The residue obtained at the filter is dried or heated for recrystallisation from acetone, and the filtrate is analysed for content of iron salts and is returned to the repeated process.
 Preparing aromatic carboxylic acid ammonium salts / 2272805
Invention relates to the improved method for preparing aromatic carboxylic acid ammonium salts by reaction of aromatic carboxylic acid with ammonia in aprotonic solvent medium. Method involves carrying out the reaction in the closed vessel by continuous addition of aromatic carboxylic acid in aprotonic solvent medium and passing gaseous ammonia under condition providing maintenance of ammonia partial pressure in the range from 0.1 to 3 bars and elimination of ammonium salt suspension in aprotonic solvent. Method allows preparing ammonium salts as crystals of a definite size that exhibit narrow distribution by size.
 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.
Manganese (ii) fumarate synthesis method / 2376278
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.
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.
Method for preparing copper (ii) acetate monohydrate / 2246480
Invention relates to a method for preparing copper (II) acetate monohydrate that represents organic carboxylic acid salt. Copper (II) acetate monohydrate is prepared by crystallization from solution obtained by mixing acetic acid, alkaline metal acetates or ammonium with copper-containing spent solution used in etching printing boards. Method provides reducing cost of the proposed method for preparing copper (II) acetate monohydrate, retaining purity of product with simultaneous utilization of toxic waste in electronic engineering manufacture - the spent solution in etching printing boards. Also, invention provides reducing material consumptions in preparing copper (II) acetate monohydrate, expanding assortment of materials used for its preparing and utilization of toxic waste in electronic engineering manufacture. Product obtained by the proposed method can be used as pigment, fungicide and copper microfertilizer in agriculture, as catalyst in processes of polymerization, as a stabilizing agent of artificial fibers, for preparing galvanic solutions and preparing other copper compounds.
Method for preparing nickel oxalate / 2256647
Invention relates to the improved method for preparing nickel oxalate that can be used in preparing catalysts, ceramic materials and in manufacturing electric vacuum devices. Method involves preparing the reaction solution containing nickel (II) and oxalate, crystallization of product, separation of precipitate from solution and its drying. The reaction solution is prepared by mixing reagent as source of oxalate and spent solution from chemical nickel plating taken in the amount providing the mole ratio in the reaction solution nickel (II) : oxalate = 1.0:(0.8-2.8). Spent solution of chemical nickel plating contains as main components nickel (II), ligand for nickel (II), reducing agent and product of its oxidation. As spent solution of chemical nickel plating method involves using solution containing nickel (II), ligand for nickel (II), hypophosphite, phosphite as main components and pH value in the reaction solution is brought about from 2.5 to 7.5. As spent solution of chemical nickel plating method involves using solution containing nickel (II) and ligand for nickel (II) as main components. As a reducing agent method involves using substance taken among the group including hydrazine, borohydride, hydrazine borane, alkylaminoborane, dithionite, hydroxymethyl sulfinate, thiourea dioxide, product of reducing agent oxidation and pH value in the reaction solution is brought about 0.0 to 8.5. Invention provides reducing material consumptions for preparing nickel oxalate, expanded assortment of materials used for preparing nickel oxalate, utilization of manufacture waste, reduced cost of product and simultaneous utilization of the spent solution of chemical nickel plating representing toxic waste of manufacturing.
 Method for preparing copper (ii) salts with dicarboxylic acids / 2256648
Copper (II) salts with dicarboxylic acids are prepared by crystallization from reaction aqueous solution obtained by mixing reagent as source of dicarboxylic acid anion and waste from radio-electronic manufacturing - spent solution in etching printed boards. Solutions containing copper (II), ammonia or mineral acid, ammonium salts and other substances are used as the spent solution in etching printed boards. Dicarboxylic acid, dicarboxylic acid anhydride, dicarboxylic acid salt with sodium, potassium, ammonium or aqueous solutions of these substances are used as reagent representing the source of dicarboxylic acid anion. Prepared copper (II) salts can be used in manufacturing high-temperature superconductors, as fungicides and copper microfertilizers in agriculture, medicinal agents in veterinary science, for antibacterial treatment of water and in other fields. Invention provides reducing cost of products, retention of their purity, utilization of waste in radio-electronic manufacturing (spent solution in etching printed boards of different composite).
 Method of production of zinc oxalate dihydrate / 2259347
Product obtained by this method may be used as pigment for production of catalysts of synthesis of inorganic and organic substances, manufacture of ceramic articles and production of oxide and other compounds of zinc. Proposed method includes preparation of reaction solution containing zinc (II) and oxalate, crystallization of target product, separation of sediment from solution and drying the sediment; reaction solution is prepared by mixing the solution of zinc plating process and oxalate-containing reagent; use is made of used solution of zinc plating process and reaction solution containing zinc (II) and oxalate at mole ratio of 1.0: (0.8-3.0) is prepared.
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FIELD: chemistry. SUBSTANCE: 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. EFFECT: improved method of producing iron benzoate. 1 tbl, 9 ex
The invention relates to the production of benzoate iron (III) and can be used in various fields of chemical and other types of practices, and analytical control and scientific research. A method of obtaining carboxylates of transition metals, lanthanides, and actinides (U.S. Pat. US No. 5220045), which is carried out by mixing the appropriate amounts of an inert organic solvent, metal nitrate, and organic carboxylic acids, including benzoic acid) and subsequent addition of ammonia and/or amine and/or tetraalkylammonium hydroxide with vigorous stirring at a temperature of from 20 to 40°C and a pressure of from 1 to 50 bar. After the exothermic reaction formed is separated aqueous phase, the carboxylates of metals are washed with water and dried at 80°C. in an inert solvent use aliphatic, cycloaliphatic or aromatic hydrocarbons containing from 4 to 20 carbon atoms. The disadvantages of this method: 1) it uses a large number of substances requiring its prior, in particular a metal nitrate, a salt of ammonium, amines, tetraalkylammonium hydroxide; 2) it formed the aqueous phase and additionally rinsing carboxylates water, contact with which can cause partial hydrolysis and lead to clicks the application of crystalline and complex compounds; 3) the method is not defined in part a reaction apparatus that implements a strong mixing of the reaction mass; 4) it does not fully characterized the products will be replaced by the anion of carboxylic acid, the nitrate anion. Closest to the claimed is a method of producing acetate iron (II) (U.S. Pat. Of the Russian Federation No. 2269509; BI, No. 4, 2006), whereby in the first stage as the oxidant used air mode sparging, and this step is carried out at intensive mechanical stirring with a high speed stirrer iron powder and acetic acid at a molar ratio of 5:1 with the addition of acetic anhydride in the amount of 4% by weight of loaded acid at a temperature of 17-25°C to accumulate in the system and salts of iron (III) in an amount of 0.75 to 0.96 mol/kg, which is next in the interaction with iron transformed into a salt of iron (II). The disadvantages of this method 1. Taken in the interaction and which is liquid acetic acid is a stoichiometric excess. Therefore, to fully react she can't and is present in considerable amounts in the reaction mixture at the time of the termination process. Separated from the liquid phase solid phase product will be contaminated captured excess acid and requires appropriate treatment. 2. As stimulating dobavlialsea acetic anhydride, that natural connection is not and requires advance of its receipt. 3. Benzoic acid is significantly different from the ant and the nature and molecular weight, and aggregate state at room temperature, and solubility in various solvents. As a consequence, the described concentration limits for acetic acid is not realizable in the case of benzoic acid. 4. There is no reason to assume that the solubility and other characteristics of acetate of iron (III) will be the same or at least similar to the corresponding characteristics of the benzoate iron (III). Therefore, there is no reason to expect that the method of separation of the product from the liquid phase of the reaction mixture by filtration can be implemented in both cases. The objective of the proposed solutions to resolve stoichiometric excess of benzoic acid in the download, as well as to find more affordable stimulating Supplement that provides rapid and almost quantitative expenditure acid target product, provided its preferential accumulation in the solid phase of the reaction mixture, which determines the ability of the Department by simple filtering. This object is achieved in that the solvent of the liquid phase take n-butyl alcohol, and stimulating additives - sodium chloride is the number of 0,015-0,200 mol/kg liquid phase, the initial concentration of the acid in the liquid phase 1.8 to 2.4 mol/kg, the loading of lead in sequence: glass beads in a mass ratio of the liquid phase of 1:1, broken iron in the amount of 30% by weight of glass beads, solvent, benzoic acid and catalytic additive, the process starts with the dissolution of benzoic acid, o the reaction mixture at the operating temperature and supply air with a flow rate of 1.3 l/min per kg of the liquid phase and are in working effectively bead mill, vertical type at a temperature of 30-70°C to practically complete consumption uploaded acid on the formation of iron salts (III), then stop stirring, external heat and air flow, the reaction mixture is separated from the beads and unreacted metal particles passing through a grid with a cell size of 0.5×0.5 mm, which is in the field of action of the magnet, and then leave on spontaneous cooling to room temperature, followed by forced cooling to a temperature of 8-12°C, then filtered, the precipitate washed with a small amount of cooled n-butyl alcohol and sent to purification by recrystallization, and the filtrate is mixed with proryvnym solvent and together with unreacted metal in return repeated the process. Characteristics of the raw materials used Be sauna acid according to GOST 10521-78 Cast iron grey brand midrange 15-32 according to GOST 1412-70 Steel 45 GOST 1050-74 n-Butyl alcohol according to GOST 6006-51 The sodium chloride on THE 113-13-14-82 The process of the inventive method include into an efficient ball mill vertical type load rated amount of the glass beads, broken iron, solvent, liquid phase, benzoic acid and sodium chloride as stimulating supplements. Sum of external heat, include mechanical stirring bead mill, deduce the temperature at the working value and serves the air sparging with a specified flow rate. The time taken for the beginning of the process. On his turn take samples of the reaction mixture, which determine the salt content of iron (II) and iron (III)and acid. As soon as the content of unreacted acid close to zero, mixing, heating, and air flow ceased, the reaction mixture is separated from the glass beads and particles of unreacted metal and leave for spontaneous cooling to room temperature to move the main mass of the formed salt of iron (III) in the solid phase (runs a bit slow). To increase the transition of the product in the solid phase is carried out forced cooling of the reaction mixture up to 8-12°C, after which it is subjected to vacuum filtration. In C the entry of the last residue washed with a small amount of pre-chilled solvent and sent to purification by recrystallization. The filtrate and the washing solvent is mixed together with unreacted metal in return repeated the process. This operation can be carried out repeatedly. It allows to increase the output of the solid of the desired product due to the circulation of any amount in the form of a solution in the solvent of the filtrate and washing n-butyl alcohol). Example 1 In ball mill vertical type with a diameter of 86 mm and a height of 135 mm, barrel and cap made of stainless steel, with cruciform blade stirrer height of the blade 37 mm and a thickness of 5.1 mm, equipped with a reflux-condenser, a supply of external heat and air sparging, and a protective cowling of steel 45 over the entire height of the hull and a false bottom with a thrust bearing for the agitator and neverendum in it with holes 0.5 mm in diameter, forming a filter wall type mesh for separating the reaction mixture at discharge from remaining in the case of glass beads with a diameter of 2,0-3,1 mm 200 g and unreacted metal particles, injected 151,2 g of n-butyl alcohol, and 48.8 g of benzoic acid, 1.2 g of sodium chloride and 60 g of broken iron as iron. Before the powder particles recovered iron and broken steel shavings accidents cast iron has the advantage that in the process of work execution shock function is s and functions additional pereirago agent of relatively large particles (with linear sizes up to 5 mm) cast iron can easily break up into many small particles, accompanied by restoration of additional work surface and reduction of the negative consequences of its locking surface sediments of the product. Served cold water in a reflux-condenser, introducing heated reactor using liquid heating baths include mechanical mixing and deduce the temperature at 60±1°C. it spent to 24.5 minutes Stabilize the temperature at a given level and serves the air sparging with a flow rate of 1.3 l/min per 1 kg of the liquid phase. The time taken for the beginning of the process. During its course take samples of the reaction mixture, which analyze the content of salts of iron (II) and iron (III), as well as unreacted benzoic acid. After 75 min the content of the latter was close to zero, and the content of salts of iron (III) about 3 times less than the initial concentration of benzoic acid (0.67 mol/kg). The salt content of iron (II) at this point is estimated trace quantities. All this gives grounds to terminate the process. Remove the heating of the reactor, cooling the reverse condenser, stop the bubbling of air and mechanical agitation, raise the mixer above the heel, providing access to neverendum holes in it, fail to properly magnet and start deleting the reaction mixture through the discharge shall acrobat, leaving the reactor beads and unreacted metal particles. Upon completion of this activity, the reaction mixture is allowed to slowly cool to room temperature, and then cooled to a temperature of 10°C. as a result of this operation, 85% of the resulting benzoate iron (III) is in the solid phase, which is filtered off, washed with 20 g pre-cooled n-butyl alcohol, again filtered and sent for purification by recrystallization. The filtrate, containing 15% of the product, mixed with proryvnym solvent and sent to re-process. The output of the solid benzoate iron (III) can be increased, if the filtrate (filtrate and the washing solvent) to be subjected to concentration by distillation of part of the solvent followed by cooling, filtration of precipitated in the solid phase salt and return the remaining filtrate in the re process. Objective obstacles to this process is complete, no. Examples 2-9 The reactor plant component, reagents, solvent and catalytic additive, the load operation and its value, the sequence of operations of the process, processing of the reaction mixture and extraction of product similar to that described in example 1. Different initial content of benzoic acid and catalytic additives in loading and temperature to perform the surveillance process and cooling of the reaction mixture before filtering the precipitated solid product. Characteristics of such processes are given in the table.
The positive effect of the proposed solution is as follows: 1. Used stimulatory Supplement (NaCl) is available, is a natural connection, moreover, its effectiveness is not inferior to the more scarce and costly addition of acetic anhydride. 2. The single-stage process, not requiring for their high flow temperatures, simple in hardware design, easily controlled and managed. 3. The target product is separated from the reaction mixture by simple filtration and can be cleaned easily accessible by recrystallization. 4. Facilitate process flow cast iron is not only affordable, but also can be just a waste of other industries. 5. In the process there is no inhibitors that prevent repeated and repeated use of the liquid phase and the dissolved components that are substantially the point of view of simplification of the environmental performance of the process. The method of obtaining benzoate iron (III) single-stage interaction between the metal and acid in the presence of an organic solvent, oxygen as oxidant and catalytic additives, characterized in that the solvent of the liquid phase take n-butyl alcohol, and stimulating additives - sodium chloride in an amount of 0.015-0,200 mol/kg liquid phase, the initial concentration of the acid in the liquid phase 1.8 to 2.4 mol/kg, the loading of lead in sequence: glass beads in a mass ratio of the liquid phase of 1:1, broken iron in the amount of 30% by weight of glass beads, solvent, benzoic acid and catalytic additive, the process starts with the dissolution of benzoic acid, o the reaction mixture at the operating temperature and supply air with a flow rate of 1.3 l/min·kg liquid phase and are in working effectively bead mill, vertical type at a temperature in the range of 30-70°C to practically complete consumption uploaded acid on the formation of salts of iron (III), then stop stirring, external heat and air flow, the reaction mixture is separated from the beads and unreacted metal particles passing through a grid with a cell size of 0.5×0.5 mm, which is in the field of action of the magnet, then leave on spontaneous cooling to room temperature, followed prinou is sustained fashion cooled to a temperature of 8-12°C, then filtered, the precipitate washed with a small amount of cooled n-butyl alcohol and sent to purification by recrystallization, and the filtrate is mixed with proryvnym solvent and together with unreacted metal in return repeated the process.
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