Method of obtaining manganese (ii) benzoate |
||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||
IPC classes for russian patent Method of obtaining manganese (ii) benzoate (RU 2391332):
          
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.
 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.
Iron (ii) oxalate synthesis method / 2376277
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.
 Method of producing iron (ii) fumarate / 2373217
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.
 Method of producing basic phthalate of iron (iii) / 2373186
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.
 Mechano-activated amorphous and amorphous-crystalline calcium salts of gluconic acid, compositions, methods of production, pharmaceutical preparations and method of treatment based on said preparations / 2373185
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.
Method of producing malonate and manganese (ii) succinate / 2373182
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.
 Method of producing manganese (ii) fumarate from manganese metal and manganese (iii) oxide / 2371430
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.
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.
 Method for preparing calcium stearate / 2259993
Invention relates to a method for preparing calcium stearate used for stabilization of plastic masses, in manufacture of paint and varnish materials, vitamin and medicinal preparations. Preparing calcium stearate is carried out by interaction of stearic acid and calcium oxide or hydroxide in the equimole ratio of reagents. The process is carried out in the solid phase under atmosphere pressure and intensive stirring without heating in the presence of zeolite of CaX type taken in the amount 6.7-16 wt.-%. Method provides simplifying technology due to a single stage process and improvement of economical indices.
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.
|
FIELD: chemistry. SUBSTANCE: 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+ EFFECT: design of an improved method of obtaining manganese benzoate. 9 ex
The invention relates to the technology of production of carboxylates of manganese (II) and can be used in various fields of chemical practice, research, and analytical control. A method of obtaining manganese formate (RF patent No. 2316536, publ. 10.02.2008, BI No. 4), whereby the target Sol receive a direct interaction of the metal and its oxide with a solution of formic acid in an organic solvent with a concentration of acid 3,5-10,8 mol/l and stimulating supplements of iodine in the amount of 0.025-0,100 mol/kg liquid phase, the dosed mass ratio of solid reagents (4,9÷11):1 and with glass beads of 1:(1÷2). As the oxide of manganese is used Mno2, MP2O3and MP3O4that take in a molar ratio with manganese 1:(1,8÷2,2). Downloads are in the sequence: the liquid phase as a whole or its components, then it is dissolved stimulating Supplement iodine, then enter the metal and its oxide. Next include mechanical stirring in a bead mill and lead the process in the absence of an external supply of heat to the almost complete consumption of the oxide. After this, the process stopped, the reaction mixture is separated from the glass beads and heavy particles of unreacted metal and then filtered. The precipitate of the target salt margins is sent to purification by recrystallization, and the filtrate is returned to repeat the process. As a solvent of the liquid phase using ethyl acetate, ethylene glycol, ethyl cellosolve, 1,4-dioxane, dimethylformamide and n-butyl alcohol. The disadvantages of this method are: 1. Acid is loaded into the remaining reagents in large stoichiometric excess. Formic acid is monobasic, liquid, with the lowest for carboxylic acids of molecular weight, which determines the opportunity to take her large excess. Besides it is well miscible with many organic solvents. Benzoic acid is more high molecular weight normally solid, but very limited and even poorly soluble in many organic solvents. Consequently, the excess for her homophase system is simply impossible. And the presence of large amount of solid phase in the initial reaction mixture is very unpredictable in relation to the impact on flowing redox process. 2. In this process the oxidation of manganese formally occurs due to the recovery of the compounds of Mn (III) and Mn (IV) (manganese-reducing agent, the oxides of manganese (III) and (IV) - oxidants). It is not certain that similar oxidant metal can act peroxide 3. Benzoic acid is somewhat weaker in comparison with ant (PKand4,2 against 3.8). It is far from clear how this will impact on the gross redox processes with their participation. Closest to the claimed, including in part the gross formula used oxidant (Mno2in both cases, is a method of producing manganese acetate (II) (patent RF №2294921, publ. 10.03.2007, BI No. 7) by direct interaction of oxidant with metal and acetic acid in the presence of stimulating supplements of iodine in a bead mill. In accordance with the metal and manganese dioxide taken in a molar ratio of 2:1 in the amount of 11.8% by weight of the liquid phase is an organic solvent (ethyl cellosolve, ethylene glycol, 1,4-dioxane, isoamyl or n-butyl alcohol and acetic acid in the amount of 3.4-5 mol/kg of the Liquid phase is metered in a molar ratio with glass beads of 1:1.5. It is dissolved and iodine in the amount of 0.025-0,070 mol/kg Loading is carried out in sequence: liquid phase or its components, iodine, metal and dioxide. The process begins at room temperature and the Vedas is t to the almost complete consumption of manganese dioxide. The reaction mixture is separated from the glass beads and heavy particles of unreacted metal, and then sent to the filter. The precipitated salt of the product was then purified by recrystallization, and the filtrate is returned to repeat the process. The disadvantages of this method are: 1, 2. As described in claims 1 and 2 in respect of the method of producing manganese formate. Molecular weight of acetic acid is not much different from formic acid and approximately equal to half the molecular weight of benzoic acid. As formic acid, it is liquid. Therefore, the excess acid reagent may be large. As oxidant, their gross formulas are the same (Mno2). But completely different in structure dioxide 3. There is no reason to assume that the transition from acetic acid to benzoic will not require replacement of the solvent liquid phase, as well as changes in the magnitude limit of the salt concentration in the final reaction mixture, at which time the process should be stopped to avoid pastes and other difficult to process systems. Therefore, the initial loading of reagents to what must be done this way, to exceeding the permissible content of the product in the final reaction mixture would be automatically excluded. It is clear that in the well-known and inventive solutions they may not be the same. 4. In the known solution the accumulation of the mass of the product took place in the solid phase, leading to the possibility of its separation by simple filtration. It is well that this situation would persist and upon receipt of manganese benzoate. But this does not mean that it will occur automatically, as it is not clear that this option is possible at all. All that is necessary to prove and to find the conditions for obtaining a favorable option. 5. At this point in time reference and periodical literature there is not enough information to compare the solubilities of acetate and benzoate manganese in most organic environments. Consequently, it is impossible to predict and changes in heterogenety processes in the transition from acetic acid to benzoic acid. It is not possible to estimate the duration of the process in the absence of their experimental determination. Especially when replacing Mno2-dioxide on Mno2-peroxide. The task of the invention is to find a solvent, the ratio of downloads metal, peroxide and acid, boot, as well as conditions for obtaining benzoate Marga is CA (II), that would provide almost quantitative conversion of all reagents in the target salt, as well as the accumulation of the main mass of the salt in the solid phase of the reaction mixture, easily separated by simple filtration. This object is achieved in that, as the oxidant by direct interaction of manganese with benzoic acid take peroxide of manganese Characteristics of the raw materials used Manganese reactive GOST 6008-90 Peroxide of manganese GOST 4470-48 Iodine crystal according to GOST 4159-79 Benzoic acid according to GOST 6413-77 Butyl acetate according to GOST 8981-78 The process of the inventive method the following. In a ball mill, vertical type, equipped with a high-speed stirrer vane type, cooling water jacket with cold running water as a cooling agent and a reflux-condenser, enter the estimated number of glass beads, solvent, liquid phase, stimulating supplements of iodine, benzoic acid. Include mechanical mixing and lead for a while dissolving acid and additives. Then enter manganese and its peroxide and the time taken for the beginning of the process. Immediately serves the cooling of the reactor by adjusting the feed rate of the cold water so that the temperature in the reaction zone does not exceed 45-60°C. during the process, take samples of the reaction mixture, which define the content of the accumulated salts of manganese, as well as residual amounts of metal, its peroxide and benzoic acid. This enables timely the military to determine the time of termination of the redox process (residual metal content and peroxide tend to zero). At the end of the mixing process in a bead mill and the cooling is stopped, the reactor vessel with the reaction mixture and glass beads detach from the lid with agitator and removed from the special Jack skeleton frame. The reactor is poured into the receiving container node filtering mesh with a cell size of 0.3×0.3 mm as a filter partition. Here occurs the separation of the reaction mixture from the glass beads. Next, the glass beads are removed from the filter septum and return to the reactor. Last put in intended for it's nest in the framework installation and connect with a lid. Pour the calculated amount of solvent liquid phase include mixing and washed beads and elements of the reactor from the remainder of the reaction mixture. Stirring is stopped, again remove the reactor from his workplace, and its content is separated from the glass beads, as noted above. Released from the beads, the reaction mixture is directed to the filtering. Separate suspended in the liquid solid phase, which was washed with a solvent after washing the beads, and digester residues from the reaction mixture. The beads are sent for training to the re process, and the filtrate and the washing solvent on cooling to 7-10°C and holding at this temperature for determi is Lenogo time sufficient to complete the crystallization of the product in such conditions. Precipitated solids filtered off, removed from the filter and sent to purification by recrystallization. Mix it with the original filtered the solid phase usually does not make sense, because the first contaminated products mechanical wear plastic blade mechanical stirrer. Therefore, cleaning of the separated solid precipitation product has the sense to separate. Obtained by the second filtering, the filtrate is returned to the re-download process. Example 1 In ball mill vertical type with housing in the form of a Cup with a flat bottom of a thick-walled glass with an inner diameter of 52.8 mm and height 141 mm, with cooling jacket for almost the entire height of the hull and under the bottom of the beaker equipped with a high speed stirrer with a rectangular blade Plexiglas with dimensions 50×46 mm and a thickness of 3.8 mm, and a reflux-condenser with running water as a cooling agent, load consistently 145 g of glass beads, 59,03 g of butyl acetate as a solvent of the liquid phase, 30,74 g of benzoic acid and 1.27 g of iodine as a catalyst additives. Include mechanical stirring for 5 min to prepare a solution of suspension of benzoic acid and stimulating supplements of iodine. P is after this, stopping stirring, enter and 4.40 g of manganese and 4,56 g of peroxide of manganese MnO2·1,5H2O. the Last moment mistaken for the beginning of the process. Immediately serves the flowing cooling water in the jacket of the reactor and a reflux condenser. During the process, take samples of the reaction mixture, which define the content of the accumulated salt of manganese (II), and the residual metal content, peroxide and benzoic acid. From these data, determine the time to reach 25, 50, 75 and more than 97%of the output of manganese benzoate from the calculated value. In this example, it was respectively 5, 12, 20 and 40 minutes, the Temperature of the reaction mixture in these moments was 49, 54, 58, and 60°C. After 45 min from the beginning of the process it stops. To stop this mechanical mixing and cease to supply water in the cooling jacket and a reflux condenser. The reactor is cut off from the cover associated with reflux-condenser and containing stuffing box mechanical stirrer, as well as the charging port and slot sampler and measure the temperature, then removed from the slot of a frame of the frame so that with stirrer, its shaft, the reaction mixture is able to flow into the reactor, which takes approximately 3 minutes After the reactor is poured into the receiving voranc the node filtering mesh with a cell size of 0.3×0.3 mm as a filter partition. The reaction mixture (suspension of the salt in solution) at a temperature of 57°C gravity falls in a team capacity, while the grid remains the glass beads with the remnants of the reaction mixture. His carefully removed from the grid and return to the reactor, which put into place in the frame plate and connected with the cover. In such assembled reactor load of 40 g of butyl acetate and include stirring for 5 minutes In parallel, the suspension of the team's capacity is filtered at a temperature of 50°C, and the capacity to return to its original location. Agitation of the leaching solvent is stopped, the reactor was removed, and its contents poured into the receiving funnel with mesh as a filter partition. The washed beads with mesh back to the reactor for re process. As the washing solvent used for washing the precipitate on the filter. Upon completion of this operation, the washed precipitate of the salt is removed from the filter and sent to purification by recrystallization. Such treatment is removed and the solid products of mechanical destruction of the plastic blade mechanical stirrer. The collected filtrate and the washing solvent is cooled to a temperature of 8.5±0.1°C and incubated for 2 hours. Vegascasinoonline benzoate manganese (II) is filtered off and then dried. And the resulting filtrate containing excess acid, the products of transformation of stimulating the existing additives and dissolved manganese benzoate sent to re-download process. The output is separated by filtration product was 93% of the calculated values in almost quantitative consumption of the metal and its peroxide in the target product. The difference accounts for the loss by separation of the reaction mixture and return to seep in again. Examples No. 2-9 The reactor, the initial reactants, the solvent of the liquid phase, stimulating Supplement iodine, loading weight and the ratio by weight of glass beads, boot order, reagents, process, monitor the progress of the course, the time of the termination process, the order of separation of the reaction mixture from the glass beads, remove residual reaction mixture with beads and elements of the reactor, separation and purification of the product, and returning the filtrate and the washing solvent in the re process similar to that described in example 1. Different initial peroxide content of manganese in the initial download, the ratio of metal: peroxide; an excess of benzoic acid, the content of stimulating supplements of iodine, the upper bound of the temperature range in which the redox process, as well as the temperature of the cooling of the filtrate and the washing solvent and the duration of crystallization of manganese benzoate. These differences and the resulting characteristics of the process are given in table. (PC - reaction mixture is).
The positive effect of the present invention 1. The process is carried out in mild temperature conditions, supported by the reaction heat. The organization of forced cooling of the big difficulties is. A cooling agent is running water, which could be used in a closed loop. 2. The bulk product is accumulated in the solid phase in suspension and subsequently separated by simple filtration. 3. Used solid reagents (manganese and its peroxide) is almost completely transformed into a salt is a product that eliminates the necessity of their separation from the final reaction mixture, and subsequent purification of the product from them. A slight excess of acid with races is voditelem liquid phase and the dissolved product - salt is returned to repeat the process multiple times without any preconcentration and separation of such a solution. As a consequence, the output of the separated product increases with the initial loading of metal and peroxide, and loads in General. 4. During the process no volatile environmental pollution and sewage. 5. Instrumentation process easy. There is no boiler-supervising equipment. Simple and monitoring the progress of the process. The termination process can be determined simply and reliably. The method of obtaining benzoate manganese (II) direct interaction of the metal with a carboxylic acid in the presence of an oxidant, stimulating supplements of iodine and an organic solvent of the liquid phase in a bead mill, characterized in that as an oxidizer take peroxide of manganese in the amount of 0.15 to 0.50 mol/kg, and the molar ratio of the metal-peroxide (1,5÷2,2):1; benzoic acid taken in the quantity (2,05÷2,1)·(nMn+
|
|||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||
in the interaction that is about the valence state of the manganese will not change. There is currently no reliable data to map the oxide and peroxide of manganese as a potential oxidant metal and make a definite conclusion in this regard.