Basic iron (iii) acetate producing method |
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IPC classes for russian patent Basic iron (iii) acetate producing method (RU 2314285):
    
 Methods for preparing ferric complexes with one salicylic acid anion / 2307118
Invention relates to technology of complexes of iron with salicylic acid suitable for use in a variety of technical areas and in medicine. Title complex is obtained via interaction of metal with acid using air oxygen as oxidant. Salicylic acid is used in butyl acetate or n-butyl alcohol solution with dissolved molecular iodine or potassium iodide. Iron is provided in the form of steel or cast iron shell, shaft, and blade of mechanical mixer as well as, agitated by the mixer, reduced iron powder fractions, broken cast iron or broken steel cuttings, cast iron or steel filings. Process is carried out at stirring with high-speed mechanical stirrer and air bubbling allowing self-heating of reaction mixture to 70-80°C until 1.72-1.85 mole/kg iron compounds is accumulated in reaction mixture in the form of suspension, whereupon mixing is stopped. Suspension is freed of unreacted fine iron and/or alloy(s) thereof and subjected to hot filtration, Filtrate is warmed to eliminate precipitated solid phase and then slowly cooled to ambient temperature. Precipitated solid phase is filtered off, dried, and recrystallized, while filtrate is recycled.
 Method of production of iron (iii) complex with three anions of salicylic acid / 2304575
Proposed iron (III) complex with three anions of salicylic acid is produced due to interaction of iron and its alloys with salicylic acid dissolved in dimethyl formamide in vertical bead-type mill provided with high-speed mechanical blade-type agitator at bubbling of air and spontaneous heating of reaction mixture to 80-90C. Iron is presented in form of steel or cast-iron ferrule over entire height of bead-type mill, steel shaft and blade of mechanical agitator, as well as in form of iron powder, fraction of broken cast iron, broken steel chips or cast-iron shot. Process is completed at accumulation of iron salts in reaction mixture of 1.12-1.30 mole/kg; 95% of these salts are in target compounds of iron (III). Hot suspension is filtered immediately and filtrate is cooled down for crystallization of main mass of iron (III) complex. Precipitated product is filtered and is directed for re-crystallization, if necessary. Filtrate is returned for repeated process.
Water-soluble iron-carbohydrate complexes, method for their preparing, medicinal agent, using / 2303039
Invention describes water-soluble iron-carbohydrate complexes containing 10-40 wt.-% of iron. Complexes can be prepared from ferric (III) salt aqueous solution and oxidation product aqueous solution of one or more maltodextrins with hypochlorite aqueous solution at alkaline pH value. In using one maltodextrin its dextrose equivalent is from 5 to 20, and in using mixture of maltodextrins the dextrose equivalent is from 5 to 20 and dextrose equivalent of each maltodextrin as component of mixture is from 2 to 40. Also, invention describes a method for preparing this complex and medicinal agents used in treatment and prophylaxis of states associated with iron deficiency.
 Method of preparing supported olefin polymerization catalysts / 2302292
Invention relates to an area of supported olefin polymerization organometallic catalysts containing organometallic complex LMX2, wherein L represents bic(imido)pyridine, M period IV transition metal (Ti, V, Cr. Fe. Co), X halogen, alkoxy or alkyl group, deposited on oxide support, namely large-pore silica gel with pore volume no greater than 1.3 cm3/g and specific surface not exciding 250 m2/g, which, prior to deposition of complex LMX2, is treated with trialkylaluminum AlR3 (R = Et or i-Bu) followed by heating SiO2/AlR3 product and dehydroxylation of support obtained.
 Method of preparing iron(iii) formate in presence of hydrogen peroxide / 2296745
Invention relates to preparation of salts of transition metals with organic acids, in particular to formic acid ferric salt. Method is accomplished via oxidation of ferrous formate with hydrogen peroxide in presence of formic acid and in absence of any dorm of iron as reducer in order to prevent reduction of ferric salt into original ferrous salt. As reducer, ferrous formate is used preliminarily recrystallized and dried or filtered off from reaction mixture suspension. Process is carried out in upright bead mill in two steps. In the first step, ferrous formate powder or precipitate is combined, stepwise or in one go, with 85% formic acid or mixture of filtrate with wash water formed during isolation of desired product to form pasty slurry ensuring stable functioning of bead mill. Second-step operation is effected in bead mill functioning mode involving forced cooling through side surfaces of reactor and continuous introduction of 12.5-25% hydrogen peroxide solution at a rate of 3.25-4.24 g H2O2 per 1 kg starting charge until degree of Fe(II) salt conversion achieves 85-90%. Supply velocity is then lowered until complete conversion is reached. Resulting product slurry is separated from beads and filtered. Filter cake is washed with 85% formic acid and recrystallized in saturated ferric formate solution containing 20-30% of formic acid. Wash liquid is combined with filtrate and used in the first step as described above.
 Method of preparing iron(ii) formate in presence of hydrogen peroxide as oxidant / 2296744
Invention relates to preparation of salts of transition metals with organic acids, in particular to formic acid ferric salt. Method is accomplished in bead mill provided with mechanical blade-type stirrer in aqueous formic acid solution (5-10 mole/kg). Iron is used in the form of steel sidewall across the height of reactor and also as particles of reduced iron stirred with stirrer together with glass beads, and/or as broken steel cuttings, and/or yet as split cast iron in any weight proportions. Method is accomplished by continuously introducing 10-20% hydrogen peroxide solution at a rate of 0.015-0,030 mole peroxide/min per 1 kg liquid phase (salt slurry) in presence of stimulating additive, in particular iodine, bromine, alkali metal or ferrous iodides or bromides in amounts (on conversion to halogens) 0.1-0.15 vole per 1 kg reaction mixture. When 1,2-1,5 mole/kg of ferrous salt is accumulated in reaction mixture, stirring and addition of hydrogen peroxide solution are stopped, product slurry is separated from unreacted iron and/or its alloys as well as from glass beads and filtered. Filtrate is recycled into process and precipitate is recrystallized from saturated iron formate solution of aqueous formic acid solution (1-2 mole/kg).
 Method of production of the ferric formiate (ii) / 2292331
The invention is pertaining to the field of chemical industry, in particular, to the method of production of the salts of iron and the organic acids, in particular, to production of the salt of the ferrous iron and the formic acid. The method is realized by the direct interaction of the acid with the iron, its alloys and the ferric oxides. The crumber with the beads and the backflow condenser is loaded with the organic solvent, the formic acid and the water in the mass ratio of 100:(85÷100): (15÷0). As the organic solvent they use ethylcellosolve, butyl acetate, butyl and amyl alcohols, ethylene glycol. The mass ratio of the beads and the liquid phase is 1:1. Ferric oxideFe2O3 orFe3O4 and the iodine are loaded in the amount of 0.40-0.56 or 0/21-0.42 and 0.03-0.1 mole/kg of the liquid phase accordingly. The iron is introduced in the form of the steel shell along the whole height of the reactor and additionally in form of the reduced iron, the fractions of the broken cast iron with dimensions of up to 5 mm and the steel chips in any ratio among themselves at total amount of 20 % from the mass of the liquid phase. The process is conducted at the temperature of 35-55°С practically till the complete consumption of the ferric oxide. The gained suspension is separated from the beads and the metal particles of the greater dimensions and subjected to centrifuging or sedimentation. The clarified liquid phase is returned to the repeated process, and the solid phase is dissolved at stirring action and warming up to 85-95°С in the water solution of the formic acid saturated by the ferric formiate (II) up to 1-2 mole/kg. The present solid impurities are removed at the hot filtration process and the filtrate is cooled and the salt crystals are separated. The technical result of the invention is simplification of the technology of the production process with utilization of the accessible raw.
Method of production of the ferric formiate (ii) in the water medium / 2292330
The invention is pertaining to the field of chemical industry, in particular, to the method of production of the salts of the metals of the organic acids, in particular, to production of the salt of the ferrous iron and the formic acid. The method is realized by the direct interaction of the formic acid water solution with the iron and/or its alloys and the ferric oxidesFe2O3 and Fe3O4 in the bead crumber of the vertical type along the whole its height with the steel shell, with the heat supply and equipped with the mechanical stirrer and the backflow condenser-refrigerator. The apparatus is loaded with 23-46 % water solution of the formic acid as the liquid phase in the mass ratio with the glass beads as 1:1.25 and then introduce the oxide - Fe3O4 orFe2O3 in amount of 0.27-0.49 or 0.48-0.64 mole/kg of the liquid phase accordingly, and besides in amount of 18 % from the mass of the liquid phase they add the powder of the reduced iron and-or the crushed cast iron, and-or the crushed steel chips in any mass ratios. Switch on the mechanical stirring and heating and keep the temperature in the reaction zone within the limits of 55-75°С. The process is terminated, when practically the whole loaded oxide is completely consumed. The suspension of the salt is separated from the non-reacted iron, its alloy and the beads and dilute with the water up to the contents of the formic acid within the limits of 1-2 mole/kg. The gained mass at stirring action is slowly heated up to temperature of 85-95°С, controlling transformation of the solid phase into the solution. The gained solution is subjected to the hot filtration, evaporation, cooling and separation of the salt crystals. The filtrate and the earlier the gained distillate are sent back to the repeated process. The technical result of the invention is simplification of the technology of the production process with utilization of the accessible raw.
Method of production of iron formate (ii) / 2291856
Proposed method consists in loading preliminarily prepared aqueous solution of formic acid at concentration of 4.5-10 mole/kg into reactor provided with bladed mixer, back-flow condenser-cooler and air bubbler. Then, powder of reduced iron and/or broken iron and/or steel chips at any mass ratio in total amount of 20.0-30.6% of mass of liquid phase and stimulating iodine additive in the amount of 0.016-0.164 mole/kg of liquid phase are introduced. Reactor may be provided with steel or cast iron ferrule over entire height. At mechanical mixing, consumption of air for bubbling is maintained between 1.2 and 2.0 l/(min·kg of liquid phase). Working temperature range is 45-65°C which is maintained by external cooling. Process is discontinued when content of iron salts (II) in reaction mixture reaches 1.8-2.0 mole/kg. Suspension of salt in liquid phase is separated from unreacted iron particles and is filtered afterwards. Filtrate is directed for repeated process and salt sediment is re-crystallized from aqueous solution saturated with iron formate by formic acid at concentration of 1-2 mole/kg at heating to temperature of 95°C followed by natural cooling.
Method of production of the ferric formiate (iii) / 2291855
The invention is pertaining to the field of chemical industry, in particular, to the method of production of the ferric formiate (III). The invention is dealt with the organic salts of the transition metals, in particular to production of the salt of the ferric iron and the formic acid. The method is realized by the direct interaction of the regenerated iron powder with the formic acid at presence of the molecular iodine and oxygen of the air as the oxidizing agents. The process is running in the medium of dimethylformamide as the dissolvent for preparation of the necessary liquid phase with the concentrations of the formic acid and iodine of 4.5-10 and 0.03-0.11 mole/kg accordingly. The mass ratio of the liquid phase and the powder of the regenerated iron is 3:1. The process starts at the room temperature and is conducted in the conditions of the forced cooling at the temperature of 50-80°С at the rate of the air consumption for the bubbling of 0.6-1.2 l\minute per 1 kg of the liquid phase. The process is terminated at accumulation of the ferric formiate (III) in the suspension up to 1-1.2 mole/kg. The suspension is separated from the particles of the non-reacted iron and then filtered. The filtrate is recycled to the repeated process, and the ferric formiate (III) (salt) is dried and either is used as required, or additionally is purified by the recrystallization. The technical result of the invention is simplification of the method with improvement of the economic indicators and the increased purity of the final product.
Method for preparing manganese (ii) acetate / 2294921
Invention relates to technology for synthesis of acetic acid inorganic salts. Method involves interaction of metallic manganese or its dioxide with acetic acid in the presence of oxidizing agent. Process is carried out in beaded mill of vertical type fitted with reflux cooling-condenser, high-speed blade mixer and glass beads as grinding agent loaded in the mass ratio to liquid phase = 1.5:1. Liquid phase represents glacial acid solution in ethylcellosolve, ethylene glycol, 1,4-dioxane, isoamyl alcohol and n-butyl alcohol as a solvent. The concentration of acid in liquid phase is 3.4-4 mole/kg. Then method involves loading iodine in the amount 0.025-0.070 mole/kg of liquid phase, metallic manganese and manganese dioxide in the mole ratio = 2:1 and taken in the amount 11.8% of liquid phase mass. The process starts at room temperature and carries out under self-heating condition to 30-38°C to practically complete consumption of manganese dioxide. Prepared salt suspension is separated from beads and unreacted manganese and filtered off. Filtrate is recovered to the repeated process and prepared precipitate is purified by recrystallization. Invention provides simplifying method using available raw and in low waste of the process.
 Method for preparing palladium acetate / 2288214
Invention relates to a method for synthesis of platinum metal salts, in particular, palladium salts, namely, palladium (II) acetate. Method for synthesis of palladium (II) acetate involves dissolving metallic palladium in concentrated nitric acid, filtering and evaporation of palladium nitrate solution, its treatment with glacial acetic acid, filtration of formed sediment and its treatment with acetic acid ethyl ester and glacial acetic acid for its conversion to palladium (II) acetate followed by heating the prepared suspension for 6 h. Method provides preparing palladium (II) acetate with high yield in monophase state and without impurities of insoluble polymeric palladium (II) acetate.
 Method of neutralization of the water combustible solutions of the acetic acid at the automated batching-packing machine / 2286307
The invention is pertaining to the field of chemical industry, in particular, to the method neutralization of the acetic acid and its solutions at leakages and accidents. The method of neutralization of the water combustible solutions of the acetic acids at the computerized batching-packing production line provides for the treatment of the surface, on which there is a leakage of the acetic acid, with the powdery anhydrous sodium carbonate. The treatment of the spilled acetic acid is exercised till formation of the paste and the paste is left on the surface for a while. At the second and the subsequent leakage of the acetic acid on the tray and at formation of the liquid phase the place of the spill is treated with a sodium carbonate till formation of the paste with the purpose for binding the liquid phase. In the case the acetic acid spills on the surfaces located outside of the tray, the neutralization of the acetic acid is exercised by water till gaining the 25-30 % solution. The surface treatment with the powder of the sodium carbonate at the first spill is exercised at the following components ratio (in mass %): Na2CO3:CH3C00H = 1.6÷4.0:1. The invention ensures reduction of the wastes of the production process, allows to reduce emissionof CO2 and allows to diminish toxicity of the production process.
 Method of production of lead tetraacetate / 2277530
The invention is pertaining to the field of chemical industry, in particular, to the method of production of lead tetraacetate. The method provides for realization of interaction of the red-lead with anhydrous acetic acid at the temperatures of 30-40°C with the subsequent separation of the target product not later than 3-5 hours after the termination of reaction. In the capacity of the dehydrating reagent is used the by-product of the interaction - lead diacetate, which forms the hydrated complex with water. The invention ensures production of lead tetraacetate equal to 70-75 % from the theoretical value. The technical result of the invention is simplification of the production process, improvement of the economic features.
Ferrous acetate preparation method / 2269509
Method consists in that iron powder is oxidized in acetic acid/acetic anhydride (4%) medium with air oxygen bubbled through the medium, while maintaining iron-to-acetic acid molar ratio 5:1 and temperature 17-25°C. Reaction mixture is thoroughly stirred with blade stirrer at speed of rotation 720-1440 rpm until reaction mixture accumulates 0.75-0.96 mol/kg ferric salt. Thereafter, air is replaced by nitrogen and 4% acetic anhydride based on initially charged acetic acid is added, temperature is raised to 35-40°C, and iron is oxidized with ferric salt until full consumption of the latter. Resulting snow-white ferrous acetate suspension is separated from unreacted iron, filtered off, and dried. All above operations are carried out under a nitrogen atmosphere. Filtrate, which is saturated ferric acetate solution in acetic acid/acetic anhydride mixture, is recycled to reactor to be reprocessed or it is used according another destination.
Ferrous acetate preparation method / 2269508
Ferric acetate is prepared by interaction of metallic iron with acetic acid in presence of an oxidant. Process is carried out at ambient temperature in acetic acid/acetic anhydride medium (weight ratio 5:1) under nitrogen atmosphere. Molar ratio acetic acid/iron/basic ferric acetate is maintained the following: 10:8:1. Reaction mixture is thoroughly stirred with high-speed blade stirrer or shaken at shaking frequency 2 Hz. When consumption of basic ferric acetate is completed, suspension of ferrous acetate is separated by filtration from unreacted iron powder. Precipitate is dried and filtrate returned into the process.
Basic ferric acetate preparation method / 2268874
Implementation of the method comprises contacting iron in the form of iron powder or iron sidewall adjacent to a body with glacial acetic acid and air oxygen at 17-25°C and vigorous stirring effected by high-speed blade-type mechanical stirrer. Initial acetic acid-to-iron molar ratio is (224÷274):100. Acetic anhydride additive is preferably introduced in amount of 2% based on the initial concentration of acetic acid. When concentration of ferric salt in the mixture reaches 2.70-3.51 mole/kg, stirring is stopped and heavy unreacted iron particles are allowed to settle/ Major mass of product suspension is filtered off and thus obtained basic ferric acetate precipitate is dried. Filtrate, which is saturated acetic acid solution of basic ferric acetate, is returned into reactor to be reprocessed. Yield of desired product achieves 99.2-99.3%.
 Zinc and aliphatic halogen-carboxylic acid salts for treatment of skin neoplasm and visible mucosa tissues / 2261243
Invention relates to zinc and aliphatic halogen-carboxylic acid salts that can be used in treatment of benign neoplasms of skin and visible mucosa tissues. Invention proposes the following formula of zinc and aliphatic halogen-carboxylic acid salts: (1):
 Method for preparing ferrous (ii) acetate / 2259994
Invention relates to a method for preparing acetic acid salts, in particular, anhydrous ferrous (II) acetate. Method for preparing anhydrous ferrous (II) acetate involves interaction of metallic iron with acetic acid in the presence of oxidizing agents of ferric oxide Fe2O3 or Fe3O4 and molecular iodine in the mole ratio acetic acid : acetic anhydride : iron oxide = 100:(6-20):(2-2.5), respectively, and in the mole ratio iron oxide : iodine = 100:6.3. The process is carried out at temperature 80°C in the beaded mill of vertical type with high-rotation blade mixer and reflux condenser in the mass ratio of glass beads and liquid phase in the charge = 1:1. The process is carried out with periodic taking off samples of the end product solid phase by filtering and the following recover filtrate and feeding with acetic acid and iron oxide. For compensation of components loss of liquid phase in filtering there are recovered into reactor to the repeated process that is carried out for four times at a time. All procedures of the basic process and filtration are carried out in nitrogen medium. Preferably, method involves using hematite, γ-oxide, iron minium, magnetite or Fe3O4 x 4 H2O as the iron oxide source. Invention provides possibility for preparing anhydrous ferrous (II) acetate and simplifying method due to excluding the evaporation stage in isolation of salt.
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 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.
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FIELD: salts of iron and organic acid producing processes, namely production of salt of iron (III) and acetic acid. SUBSTANCE: method is realized by relation of metallic iron with acetic acid at presence of oxidizing agent; using molecular iodine, iron oxides such as Fe2O3, Fe3O4 and oxygen of air as oxidizing agent for converting impurity of iron (II) acetate to basic iron (III) acetate. Process is performed in beads mill at temperature 80°Cand at mass relation of liquid charge and glass beads 1 : 1. Iron is used in the form of shell abutted to lateral surface of reactor housing. Initial molar relation of iron oxide and iodine is 10 : 1. Molar relation of acetic acid, its anhydride and iron oxide is in range 100 : (2 - 5.99) : (2 - 2.5). In time moment of practically complete consumption of iron oxide, solid phase of reaction mixture is taken off by filtering. Simultaneously consumed reagents are replenished and filtrate is returned to reactor for repeating process. Number of processes to be repeated is no more than 5. At second stage residues of iron (II) salt are after-oxidized to basic iron (III) acetate due to drying up taken off solid phase of product in filter by means of blowing air at environmental temperature. Preferably, hematite, γ-oxide or minimum is used as Fe2 O 3 and magnetite and Fe3O4 x 4H2Ois used asFe3 O4. EFFECT: simplified process, usage of available reagents. 3 cl, 9 notes, 2 tbl
The invention relates to a technology for obtaining salts of acetic acid, in particular of the basic acetate of iron (III), and can be used in various industries, as well as in the laboratory in analytical and applied chemistry. It is known that in the acetic acid medium molecular iodine oxidizes the iron with the formation of salts of iron (II) and iron (III) (Ivanov, A.M., S. p. Altukhov, Filimonova SV Some ways of spending of iron in solutions of iodine in low molecular weight fatty acids and evaluation of their competitive ability // proceedings of the Kursk state technical. Univ. Kursk, 2003, №1 (10). P.59-63). On the other hand, the oxides of iron (III) oxidizes iodide iron (II) emitting able to react with the iron of molecular iodine (A.M. Ivanov, S. p. Altukhov, Filimonova SV Certain patterns of iron oxidation by molecular iodine, and iodine iron (II, III) and potassium oxides of iron (III) in organic media under vigorous stirring // Sat. materials of the V international scientific-technical. conference "Medical-ecological information technology - 2002". Kursk: the Publishing house of the Kursk state technical. University, 2002. S). These two processes occur at significantly different temperatures and therefore mechanically nor the place, nor in time not to be merged. Closest to the claimed is a method of obtaining basic formate or acetate India (A.S. WITH THE CF No. 454198), whereby acetic acid is subjected to interaction with the metal in the presence of hydrogen peroxide at periodic heated to 80-100°and subsequent isolation of the product by evaporation of a solution containing a fairly large amount of water and acetic acid. The disadvantages of this method are: 1. Use as an oxidizer aqueous solution of hydrogen peroxide, which determines the selection of the target product by evaporation, which is quite energy intensive and prolonged virtually independent of the process (stage). 2. The model of this process cannot be extended to iron, because iron salts (III) are very effective catalysts homolytic decomposition of hydrogen peroxide, which implies large unproductive losses of this oxidant. 3. Iron easily corrodes formation of oxides on its surface. Water and oxygen are used to facilitate this process. Therefore, the target product will be contaminated with oxides, which will require additional cleaning. 4. The main source of the cation of the target salt is a metal, which will first obtain and properly cleaned of impurities. It would be highly desirable to obtain a salt of acetic acid, at least partially, to use b is more available metal joints, and even better natural origin, for example the oxides. The objective of the proposed solutions is to get the basic acetate of iron (III) with the simultaneous use as a source of cation not only iron, but also its oxides Fe2About3and Fe2O4and to eliminate energy-intensive and prolonged stage of evaporation in the allocation of the target product. This object is achieved in that the process of obtaining the product of the interaction of iron and acetic acid are two phases that differ by the nature of the used oxidant. At the first stage as an oxidizer take iron oxide Fe2About3or Fe2O4and molecular iodine in a molar ratio of 10:1, and the process is carried out at 80°in a bead mill, vertical type with glass beads as pereirago oxide agent mass ratio of liquid phase loading 1:1, with high-speed mechanical stirrer and reflux-condenser in the absence of air flow through the gas space of the reactor, but without particular limitations regarding the exclusion of this space from the atmosphere, with the use of iron in the form of the shell adjacent to the side surface of the reactor vessel and with the original download of acetic acid, acetic anhydride and nitric oxide iron mass ratio of 100:(2÷5,99):(2÷ 2,5), with the selection of the solid phase of the reaction mixture by filtration, carried out at the moment almost complete consumption of iron oxide, with the return of the filtrate simultaneously with the feed consumed by the formation of acetic acid and iron oxide and compensation components of the liquid phase during the filtration process in the reactor to repeat the process. The second step consists in the additional oxidation separated in the sediment during the filtration of the salts of iron (II) in basic acetate of iron (III) oxygen in the selected drying of the solid phase on the filter due to the flow of air at ambient temperature. At the same time as the oxide of Fe2About3use hematite, γoxide or red iron oxide as Fe2O4magnetite or Fe3O4·4H2O, and repeated the process carried out at least 5 times in a row or with some interruptions. Characteristics of the raw materials used the reactive iron in THE 6-09-2227-81 iron carbonyl radio brand R-20 GOST 13610-79 The iron oxides: hematite according to GOST 4173-77 minium on THE 113-00-38-160-96 γoxide according to GOST 3540-82 magnetite according to GOST 26475-85 iodine crystal according to GOST 4159-79 acetic acid according to GOST 61-75 acetic anhydride according to GOST 5815-77 The process of the inventive method the following. In equipped with reflux-con is satrom and heated using movable along the longitudinal axis of the liquid bath ball mill is placed adjacent with as small as possible clearance to the body shell of iron, glass beads, loading of the liquid phase (a mixture of glacial acetic acid and acetic anhydride), as well as iodine and iron oxide Fe2O3or Fe2O4. Include mechanical mixing and heating with pre-heated liquid bath and bring the temperature to the preset mode. Continue mixing in the stable regime the temperature controlling method of sampling the accumulation of iron salts in the reaction mixture. Upon reaching almost complete spending just loaded iron oxide obtained reaction mixture in the cooling mode is directed to filtration, after separating it from the beads passing through a filter with mesh of appropriate sizes. The filtrate immediately return to repeat the process, adding to its uploading spent on the formation of acetic acid and iron oxide, as well as compensation of losses of the components of the liquid phase during the filtration (statistics option on the principle of returning the weight to the value of the initial load). Then a second process in accordance with the above sequence of operations. Separated on the filter is a solid phase, a mixture of iron (III) salts and iron (II), dried in air duct. When the operation is finally oxidized salt as is ESA (II) in basic acetate of iron (III), who is the target product of this process. Repeated the process according to the described scheme are performed several times (at least not less than 5) or directly one after the other, or with some interruptions. During the last bead mill must be completed loading and interrupted her free exit to the atmosphere through a reflux condenser. Example No. 1. In ball mill vertical type of the glass casing inner diameter of 63.7 mm and a height of 109 mm and inserted metal shell height of 70 mm and weight 84,13 g, which are attached tightly to the fixed iron frame cover with stuffing box and seals for mechanical stirrer vane type with the shaft and blades of the PCB, and with a reflux-condenser, outcrop in the atmosphere, and a loading opening impose 115,4 g of glass beads and the loading of the reaction mixture, consisting of 110,44 g glacial acetic acid, 3,76 g of acetic anhydride, 1,17 g of molecular iodine and 7,35 g γ-oxide Fe2About3jet clean. Include mechanical mixing, bottom down preheated to 85°liquid bath so that the entire height of the working zone of the reactor was immersed in the heating liquid, cooling water serves to reverse this b the IR capacitor and deduce the temperature at 80° C for 15 minutes Stabilize the temperature in this mode, carry out the process. On his turn without stopping stirring take samples of the reaction mixture, which determine the salt content of iron (II) and iron (III), a residual amount of iron oxide. As soon as the latter reaches the zero value (in this case, after 108 minutes), stirring is stopped and the reaction mixture is connected through a grid to separate the beads are sent to the filtering. The separated filtrate number 94,71 g return in a bead mill to repeat the process. To it add 19,31 g of acetic acid, 1,25 g of acetic anhydride, to 0.23 g of iodine and 7.47 g γ-Fe2About3include mechanical stirring, heating serves over 11 min deduce the temperature specified on 80°and a second process as described above within 106 minutes In parallel with the re process are finally oxidized salts of iron (II) in basic acetate of iron (III) on the filter, providing duct air through the layer of filter cake at room temperature. It took 60 minutes Simultaneously with the additional oxidation of the salt of iron (II) during this operation is the drying of sludge from captured during the filtration of the liquid components of the reaction mixture (mainly acetic acid and less acetic of any the reed). Upon completion of the first re-process the reaction mixture is separated from the beads, then filtered, the filtrate is directed to the second repeated the process, and the filter cake is treated with a flow of air for 55 min to additional oxidation of the salt of iron (II) in basic acetate of iron (III). Just re-processes carried out 5. The additional loading of raw materials and their characteristics are shown in table 1. Table 1
In the original and in the five subsequent re-processes the received 151,2 g of dried basic acetate (III). This remained the filtrate in the number of 89.2 g, which may be returned to the process after proper feeding of acetic acid, acetic anhydride and iodine and enter the next portion γ-oxide. Examples 2-9. The reaction apparatus, the sequence of operations for loading, the output temperature of the specified mode and its stabilization, the process of separating the reaction mixture from the beads and the solid phase from it, additional oxidation of salts of iron (II) in the separated solid precipitate on the filter, returning the filtrate to re-process the uploading of components of the liquid phase, taking into account the compensation of losses in the filter, enter a new portion of the iron oxide and the first and subsequent repeated processes, the number of retry processes similar to those described in example 1. Different nature of the iron oxide, the initial molar ratio of acetic acid, acetic anhydride and iron oxide, the presence of a break in the conduct of subsequent re-process and other temporal characteristics. The results obtained are summarized in table 2.
The positive effect of the proposed solution consists in the following: 1. The method is implemented at relatively low temperatures, in the absence of pressure, simple in hardware design, has many simple solutions to maintain the set temperature mode. 2. There is no energy-intensive stages of type evaporation of the solution. The filtrate can be reused for its intended purpose or to compensate for the liquid phase during the filtration process. 3. From 2/3 to 3/4 of the formed salt is obtained from iron oxide, which can be used available natural minerals. 1. The method of obtaining basic acetate of iron (III) interaction of metallic iron with acetic acid in the presence of an oxidant, wherein in the first stage as an oxidizer take iron oxide Fe2O3or Fe3O4and molecular iodine in the initial molar ratio of 10:1, and the process is carried out at 80°in a bead mill, vertical type with glass beads as pereirago oxide agent mass ratio of liquid phase loading 1:1, with high-speed mechanical stirrer and reflux-condenser in the absence of a duct of the air is through the gas space of the reactor, but without particular limitations regarding the exclusion of this space of the reactor from the atmosphere, with the use of iron in the form of the shell adjacent to the side surface of the reactor vessel, and with the original download of acetic acid, acetic anhydride and iron oxide in a molar ratio of 100:(2-5,99):(2-2,5), with the selection of the solid phase of the reaction mixture by filtration, carried out at the moment almost complete consumption of iron oxide, with the return of the filtrate simultaneously with the feed consumed by the formation of acetic acid and iron oxide and compensation components of the liquid phase during the filtration process in the reactor repeat the process and finally oxidized in the second stage, any salt of iron (II) in basic acetate of iron (III) if the selected drying of the solid phase of the product on the filter due to the flow of air at ambient temperature. 2. The method according to claim 1, characterized in that the iron oxide Fe2About3take hematite, γoxide or red lead, and as Fe3O4magnetite and Fe3O4·4H2O. 3. The method according to claim 1, characterized in that the re process is carried out at least 5 times in a row or with some interruptions.
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