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IPC classes for russian patent Lead (ii) acetate synthesis method (RU 2398758):
          
 Method of obtaining palladium acetate / 2387633
Method of obtaining palladium acetate involves dissolving palladium metal in concentrated nitric acid, evaporation of the obtained solution and reaction with acetic acid, where the palladium nitrate solution after evaporation, before crystallisation of palladium (II) nitrate salt, is treated with nitrogen (II) oxide or a mixture of nitrogen (II) and (IV) oxides containing not more than 30% nitrogen (IV) oxide and acetic acid at temperature of the solution of 40-90°C with glacial acetic acid consumption of 1.5-2.5 l per kg of palladium in the solution and nitrogen (II) oxide or mixture of nitrogen (II) and (IV) oxides consumption of 1.0-2.0 m3 at normal conditions per 1 l of the initial palladium nitrate solution for 0.5-1.5 hours and the formed solution is heated in a nitrogen atmosphere at 110-140°C for not less than 2 hours with consumption of elementary nitrogen of approximately 30 m3 per 1 m3 of the formed solution.
 Method of palladium acetate production / 2344117
Invention refers to platinum metal salts synthesis, specifically palladium salts, namely palladium (II) acetate applied as catalyst or for production of initial salt for other palladium salts. Method of palladium acetate production includes as follows. Metal palladium is dissolved in concentrated nitric acid. Prepared solution is steamed prior to crystallisation of palladium nitrate salt, processed by ice acetic acid. Deposition is filtered and processed with ice acetic acid. Nitrate palladium solution is processed with ice acetic acid with sodium acetate additive in amount 1.5 - 2 kg per 1 kg of palladium in solution. Deposition is processed and dissolved in ice acetic acid in ratio 19-21 l per 1 kg of deposition with acetamide added in amount 0.1 - 0.2 kg per 1 kg of deposition. Solution is warmed at temperature 80 - 90 °C within at least 5 h and steams until salt is formed.
Method for obtaining palladium acetate / 2333196
Invention concerns platinum-group metal salt synthesis, particularly of palladium salts, namely palladium (II) acetate applied as catalyst or for obtaining basic salt to produce other palladium salts. The method for obtaining palladium acetate involves dissolution of metal palladium in concentrated nitric acid, evaporation of obtained solution and reaction with acetic acid, where, after evaporation but prior to palladium (II) nitrate crystallisation, the palladium nitrate solution is processed by a mix of acetic acid, acetic acid ethyl alcohol and acetic anhydride at (60-80)°C with (2.0-3.0) l of ice-cold acetic acid, (0.8-1.0) l of ethylacetate and (0.4-0.6) l of acetic anhydride per 1 kg of dissolved palladium for at least 1 hour, the resulting solution is heated at (90-110)°C for at least 3 hours and at (135-145)°C for at least 6 hours.
 Method for obtaining palladium acetate / 2333195
Invention concerns platinum-group metal salt synthesis, particularly of palladium salts, namely palladium (II) acetate applied as catalyst or for obtaining basic salt for production of other palladium salts. The method for obtaining palladium acetate involves dissolution of metal palladium in concentrated nitric acid, filtration and evaporation of palladium nitrate solution and reaction with acetic acid, where after evaporation but prior to palladium (II) nitrate crystallisation the palladium nitrate solution is processed by distilled water in the volume of (2-5) l per 1 kg of palladium in the initial nitrate solution, then by acetic acid diluted with water, with acid concentration of (30-70)% and volume of (1.5-2.5) l of acetic acid per 1 kg of palladium in the initial nitrate solution, the resulting solution being matured for at least 8 hours at (15-40)°C.
 Method of zirconium carboxylate production / 2332398
Invention relates to chemistry of derivative transition metal and can be used in chemical industry while producing transition metal carboxylate and refers to improved method of zirconium carboxylate production through interreacting of zirconium chloride with carboxylate derivatives of general formula RCOOM, where R-linear and branched alkyl CnH2n+1 or non-saturated acid residue, where n=0-16, and M - proton or cation of alcali metal, in which alkali acid of aliphatic or non-saturated acids are used as RCOOM compounds, interacting of zirconium chloride with the compounds leads to solvent absence in solid with mechanical activation at mole ratio ZrCl4: RCOOM within 1<m<4.5, where m is integral and broken number with the following extraction of derived zirconium carboxylate with an organic solvent.
 Basic iron (iii) acetate producing method / 2314285
Method is realized by relation of metallic iron with acetic acid at presence of oxidizing agent; using molecular iodine, iron oxides such as Fe2O3, Fe3O4 and oxygen of air as oxidizing agent for converting impurity of iron (II) acetate to basic iron (III) acetate. Process is performed in beads mill at temperature 80°Cand at mass relation of liquid charge and glass beads 1 : 1. Iron is used in the form of shell abutted to lateral surface of reactor housing. Initial molar relation of iron oxide and iodine is 10 : 1. Molar relation of acetic acid, its anhydride and iron oxide is in range 100 : (2 - 5.99) : (2 - 2.5). In time moment of practically complete consumption of iron oxide, solid phase of reaction mixture is taken off by filtering. Simultaneously consumed reagents are replenished and filtrate is returned to reactor for repeating process. Number of processes to be repeated is no more than 5. At second stage residues of iron (II) salt are after-oxidized to basic iron (III) acetate due to drying up taken off solid phase of product in filter by means of blowing air at environmental temperature. Preferably, hematite, γ-oxide or minimum is used as Fe2 O 3 and magnetite and Fe3O4 x 4H2Ois used asFe3 O4.
Method for preparing manganese (ii) acetate / 2294921
Invention relates to technology for synthesis of acetic acid inorganic salts. Method involves interaction of metallic manganese or its dioxide with acetic acid in the presence of oxidizing agent. Process is carried out in beaded mill of vertical type fitted with reflux cooling-condenser, high-speed blade mixer and glass beads as grinding agent loaded in the mass ratio to liquid phase = 1.5:1. Liquid phase represents glacial acid solution in ethylcellosolve, ethylene glycol, 1,4-dioxane, isoamyl alcohol and n-butyl alcohol as a solvent. The concentration of acid in liquid phase is 3.4-4 mole/kg. Then method involves loading iodine in the amount 0.025-0.070 mole/kg of liquid phase, metallic manganese and manganese dioxide in the mole ratio = 2:1 and taken in the amount 11.8% of liquid phase mass. The process starts at room temperature and carries out under self-heating condition to 30-38°C to practically complete consumption of manganese dioxide. Prepared salt suspension is separated from beads and unreacted manganese and filtered off. Filtrate is recovered to the repeated process and prepared precipitate is purified by recrystallization. Invention provides simplifying method using available raw and in low waste of the process.
 Method for preparing palladium acetate / 2288214
Invention relates to a method for synthesis of platinum metal salts, in particular, palladium salts, namely, palladium (II) acetate. Method for synthesis of palladium (II) acetate involves dissolving metallic palladium in concentrated nitric acid, filtering and evaporation of palladium nitrate solution, its treatment with glacial acetic acid, filtration of formed sediment and its treatment with acetic acid ethyl ester and glacial acetic acid for its conversion to palladium (II) acetate followed by heating the prepared suspension for 6 h. Method provides preparing palladium (II) acetate with high yield in monophase state and without impurities of insoluble polymeric palladium (II) acetate.
 Method of neutralization of the water combustible solutions of the acetic acid at the automated batching-packing machine / 2286307
The invention is pertaining to the field of chemical industry, in particular, to the method neutralization of the acetic acid and its solutions at leakages and accidents. The method of neutralization of the water combustible solutions of the acetic acids at the computerized batching-packing production line provides for the treatment of the surface, on which there is a leakage of the acetic acid, with the powdery anhydrous sodium carbonate. The treatment of the spilled acetic acid is exercised till formation of the paste and the paste is left on the surface for a while. At the second and the subsequent leakage of the acetic acid on the tray and at formation of the liquid phase the place of the spill is treated with a sodium carbonate till formation of the paste with the purpose for binding the liquid phase. In the case the acetic acid spills on the surfaces located outside of the tray, the neutralization of the acetic acid is exercised by water till gaining the 25-30 % solution. The surface treatment with the powder of the sodium carbonate at the first spill is exercised at the following components ratio (in mass %): Na2CO3:CH3C00H = 1.6÷4.0:1. The invention ensures reduction of the wastes of the production process, allows to reduce emissionof CO2 and allows to diminish toxicity of the production process.
 Method of 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.
 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.
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.
Preparation comprising water-soluble triterpenic acid salts and method for its preparing / 2244426
Invention relates to a method for preparing the preparation comprising triterpenic acid water-soluble salts and additionally added protein-containing product and vegetable raw, the source of triterpenic acids taken in the following ratio of components, wt.-%: protein-containing product, 10-17; triterpenic acid sodium salts, 4-5, and vegetable raw, the balance. Method involves mixing triterpenic acid-containing vegetable raw with the protein-containing product taken in the ratio = (9-11):(1-2), mechanical-chemical treatment of this mixture in activator device, mixing of prepared semi-finished product with sodium carbonate or sodium hydrocarbonate taken in the ratio = (92-97):(3.5-8.3) and repeated treatment in the activator device. Method involves applying flow-type ball vibration-centrifugal or ellipse-centrifugal mills as the activator device that provide the acceleration of milling bodies up to 170-250 m/c2 and time for treatment for 1.5-3 min. Invention provides simplifying the process and the complex processing waste in lumber industry.
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FIELD: chemistry. SUBSTANCE: invention relates to 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 EFFECT: design of an improved method of obtaining lead acetate. 2 cl, 15 ex
The invention relates to the technology of production of carboxylates of lead (II) and can be used in various fields of chemical practice, analytical control and in carrying out various scientific studies. A method of obtaining lead acetate (A.S. USSR № 1664785 CL C07C 53/10, publ. 23.07.91, bull. No. 27), according to which the lead oxide is treated with a solution of ammonium acetate in dimethylformamide at their molar ratio of 1:(2,0-2,2):(13-325) when heated to boiling and kept in the boiling mode for a certain period of time. The solid phase of the reaction mixture is filtered, the filtrate evaporated in vacuum and get the product with output from 73% to almost quantitative and the basic substance content above 90%. The disadvantages of this method are: 1. Dimethylformamide as the solvent boils at a temperature of 150°, the boiling point of a solution of ammonium acetate in it a bit higher. Even higher, we should expect the boiling point of the reaction mixture, representing a solution of acetate of ammonium and lead in DMF. Therefore, the high temperature process requiring the supply of external heat and the corresponding reactor with a good reflux-condenser and heat insulation. 2. Quite a difficult selection of the target reaction product: separation of the liquid phase of the reaction is ionic mixture from the residual solid phase, evaporation of the filtrate in vacuo with the formation of a solid salt, washing of the residue after evaporation of isopropyl alcohol, drying the separated solid phase of the target product. Some stages require special equipment operating under vacuum, for example. 3. In the chemical transformation of volatile products are formed, in particular ammonia and water, which requires the creation of a safe work environment for staff. 4. The main part of the reaction mixture presents high-boiling solvent (DMF). On its heating, maintaining for a certain period of time the boiling point, and further by evaporation under vacuum to spend a lot of heat input, which makes the energy-intensive process. 5. Leaves much to be desired purity and yield of the obtained product. 6. In General, the process is complicated and a large number of operations that require a variety of equipment in a fairly large number of Closest to the claimed is a method of producing manganese acetate (II) (patent RF № 2294921, publ. 10.03.2007, bull. No. 7). In accordance with a direct interaction between the metal and its oxide in a molar ratio of 2:1 with acetic acid is carried out in the presence of the bulk liquid phase is an organic solvent (ethyl cellosolve, ethylene glycol, 1,4-dioxane, isoamyl or n-butyl with the RTIs), which is dissolved acetic acid (3,4-5 mol/kg) and molecular iodine (0,025-0.07 mol/kg) as stimulating supplements. The sum of the masses of metal and its oxide is 11.8% by weight of the liquid phase. The mass ratio of the liquid phase and the glass beads of 1:1.5. The boot sequence is as follows: glass beads, liquid phase or its components (solvent, acid and iodine), then the metal and its oxide. The end of the boot and sustainable stirring bead mill mistaken for the beginning of the process. The process begins at room temperature and lead to the almost complete consumption of manganese dioxide. While the bulk of the product accumulates in suspended in the reaction mixture, the solid phase. The suspension of the final reaction mixture is separated from the glass beads and heavy particles of unreacted metal and filtered. 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. There is no reason to assume that the transition from a system Mn-MnO2acetic acid to the system Pb-PbO2acetic acid will automatically ensure the efficiency of the process and close the conditions of its occurrence with technologically acceptable speeds and with almost quantitative conversion of the reagent shortage. In-p is pout, MnO2and PbO2quite differently strong oxidizing agents. This applies in comparison of manganese and lead as reductants. Secondly, the physical characteristics of the metal are very different. The lead is considerably heavier in comparison with manganese metal and this metal is soft and malleable, while manganese fragile and easily partitioning used in the bead mill. 2. If with lead and its dioxide process would be possible, then there is no reason to assume that will be acceptable to be used in the prototype, the molar ratio of metal: its dioxide, and the mass ratio of the sum of the metal and its oxide with the liquid phase of the system. 3. There is no reason to believe that favorable solvents liquid phases upon receipt of manganese acetate (II) will remain the same when carrying out a similar process in the system lead - dioxide. This fully applies to the nature and amount of the stimulating additive process. 4. There is no doubt that the solubility in different media, as well as other physical properties of the acetates of manganese and lead are significantly different from each other. This implies the absence of any guarantee that, when the flow is similar to the structure of the process for receiving lead acetate product will mainly accumulate in the form of suspender the bath of the solid phase, easily separated by simple filtration or centrifugation and purified in a similar way. In this case the obtained supernatant-the filtrate will be not only possible, but advisable to return to repeat the process. The objective of the proposed solution is to find such molar ratio of the reactants and the mass of their correlation with the solvent liquid phase, the whole boot process and boot and glass beads, as well as the nature of the solvent liquid phase and stimulating supplements, a number of recent and other conditions for the redox process, the implementation of which would provide almost quantitative conversion of lead dioxide in salt, predominantly accumulated in the form of suspended solid phase, easily detachable from the rest of the reaction mixture by simple filtration. This object is achieved in that the oxidizer reagent in the lack of take the lead dioxide in the amount of 0.4-0.6 mol/kg, metal and acetic acid is dosed in amounts of from 0.6 to 1.5 mol/kg, respectively Characteristics of raw materials used: Lead metal in THE 6-09-3523-74. Lead dioxide, according to GOST 4216-78. Acetic acid according to GOST 61-75. Iodine crystal according to GOST 4159-79. ISO-Propyl alcohol according to GOST 9805-84. ISO-Butyl alcohol according to GOST 9536-79. The ethyl cellosolve according to GOST 8313-88. Dimethylformamide under MRTU 6-09-2068-65. Butyl acetate according to GOST 8981-78. The process of the inventive method the following. In a ball mill, vertical type, equipped with a reflux-condenser, high-speed mechanical stirrer vane type and a cooling water bath with cold running water, enter the estimated number of glass beads, solvent, liquid phase, acetic acid, lead him dioxide and molecular iodine. Include mechanical mixing and the time taken for the beginning of the process. Immediately serves cooling water in a reflux-condenser and cooling down the water bath so that the reactor vessel was immersed in a bath of not less than 2/3 of its height. The degree of immersion of the reactor in bath and duct cold water through it adjust so that the maximum during the process is and the temperature in the reaction zone does not exceed 30-50°C. During the process, take samples of the reaction mixture, which define the contents of the accumulated salts of lead, as well as unreacted lead dioxide and acetic acid. The results of this control determines the moment of quantitative consumption of lead dioxide, i.e. the time of the termination process. At the end of the mixing process in the bead mill, the supply of water in a reflux-condenser, stop, lower the cooling bath down, disconnect the casing bead mill from its cover (threaded connection), the contents of the reactor are transferred into the funnel of the node separation of the reaction mixture from the beads and plates of unreacted lead thickness of 0.2-0.3 mm (initial granules, pieces under the action of the beads during the process, then rolled into plates of this thickness)containing as a filter partition the grid with a cell size of 0.3×0,3 mm Glass beads and unreacted metal is carefully removed from the grid of the specified node and returns in case the reactor. Last put in intended for him Jack skeleton frame and connected to the lid of the reactor with a mechanical stirrer and reflux-condenser. The assembled ball mill load calculation quantity of solvent liquid phase include mechanical mixing and washed building is with, mechanical stirrer, other elements of the reactor and glass beads from remaining on them when unloading and separation of the residue of the reaction mixture. Next, separate the beads and unreacted metal from leaching solvent and sent to re-download process. Separated from the beads, the reaction mixture is filtered, the filter cake obtained is washed proryvnym solvent is removed from the filter and is directed to purification by recrystallization, and the filtrate together with proryvnym solvent in return repeated the process. Example No. 1. In a ball mill with glass thick-walled housing with a flat bottom with an inner diameter of 53.2 mm and a height of 143 mm, connected through the corresponding outlet in the lid with a reflux-condenser and equipped with high-speed mechanical paddle agitator with shaft and rectangular blade 50×46 mm from the PCB, consistently load of 160 g of glass beads, to 52.1 g of ISO-butyl alcohol as solvent, 13,71 g of acetic acid, 20,72 g lead, chopped into pieces with a maximum linear size up to 5 mm, 13,16 g of lead dioxide and 0.31 g of molecular iodine. The reactor vessel with the download link threaded connection with the cap containing the stuffing box above the row at a reflux-condenser, and slot pocket thermocouple and the sampler. Collected the mill is placed in the corresponding socket of the skeleton frame, fasten securely into the slot in the standard, always repeating from experience to experience the situation. Bring liquid cooling bath bottom so that approximately 100 mm of the reactor vessel was in the cooling water serves flowing cooling water in a reflux-condenser and cooling bath, include mechanical mixing and the time taken for the beginning of the process. During the redox process without stopping the stirring at certain points in time take samples of the reaction mixture, which define the content of the accumulated salts of lead (II), as well as unreacted lead dioxide and acetic acid. Based on the results of such monitoring to build kinetic curves of accumulation of these components, which determine the time to reach 25, 50, 75 and 98 and over the degree of conversion of the reactant in the lack (in this case, lead dioxide). It was equal to 3, 7, 31, 124 min, respectively. The maximum temperature in the reaction zone is fixed at 14 min from the beginning of the process and is equal to 43°C. After 130 min stop the flow of water in a reflux-condenser and cooling bath and stirring the reaction mixture in the reactor. Bath opus is up down freeing the body of the mill, followed by disconnecting it from the lid of the reactor. Disconnected the reactor vessel is not immediately removed, allowing 3 minutes for draining remaining on the blade and the shaft of the stirrer of the reaction mixture. After that, the contents of the reactor gently transferred into a funnel of node separation of the reaction mixture from the glass beads and the unreacted metal is present in the form of thin leaves of plates with thickness of 0.1-0.3 mm) on a grid with a cell size of 0.3×0.3 mm as a filter partition. The detainee on the mesh beads and unreacted metal is carefully removed from the grid and return to the reactor. The last set into place on the frame frame, collect the whole installation, enter 40 g of ISO-butyl alcohol, include mechanical mixing and hold it flush to the remaining reaction mixture from the surface of the reactor, its shaft, the other elements of the reactor, as well as from the surfaces of returned glass beads and unreacted lead within 5 minutes After that, a second compartment glass beads and plates of unreacted lead from the flushing solvent through the previously described sequence of operations. In parallel with the washing of hard surfaces from the remainder of the reaction mixture is carried out by filtering the previously separated suspension reaction, see the C and subsequent washing of the filtercake proryvnym solvent, centrifuge sludge, eat it with a filter and send to additional purification by recrystallization. The mixture of the filtrate and the washing solvent containing unreacted acid, the products of transformation of stimulating additives (mainly iodide of lead) and 0,021 mol/kg of lead acetate return on the re-download process. The output of the separated solid product was to 0.108 mol or 97% of the calculated value. Examples No. 2-9. The reactor and its elements, the sequence of loading operations, the process, the determination of the time of termination, separation of glass beads and unreacted metal from the rest of the reaction mixture, processing of the reaction mixture, separation of the target product and recycling of the solvent and components stimulating supplements, as well as the nature of the solvent and the mass ratio of the load and the glass beads is similar to that described in example 1. Different initial dosage of lead dioxide, the molar ratio of lead dioxide and metal loading, the dosage of acetic acid, iodine, washing solvent, and the maximum temperature of the reaction mixture in the reactor during the process. These differences and other characteristics of the process are given in table 1. (PC - reaction mixture)
Examples No. 10-15. The reactor and its elements, download lead him dioxide and acetic acid, the sequence of operations of loading, carrying out the process is and, determine the moment of its termination, separation of glass beads and unreacted metal from the reaction mixture, processing suspensions PC, separation of the target product and recycling of the solvent and components of stimulating additives similar to those described in example 1. Differ by the nature of the used solvent, the content of stimulating supplements of iodine, and the mass ratio of the load and glass beads. These differences and other characteristics of the process are given in table 2. (Notation: IPs-ISO-propyl alcohol; IBS-ISO-butyl alcohol; EC - ethyl cellosolve; BA - butyl acetate, DMF - dimethylformamide)
The positive effect of the proposed solution consists of: 1. In mild temperature conditions, and supported by the reaction heat at a moderate intensity and easily organized forced cooling. 2. The bulk product is accumulated in the form of suspended solid phase and can be easily removed by simple filtration. 3. The reaction mixture after removal of the solid product and the washing solvent is returned in the re process and do not require any special disposal. 4. Returned in re-process the excess metal is easily separated from the rest of the reaction mixture, together with glass is m beads 5. In the proposed solution, there is no volatile environmental pollution and sewage. 6. Instrumentation process does not contain boiler-supervising equipment. 7. Monitoring the progress of the process simple and easy to organize. 1. The method of obtaining acetate lead (II) by direct interaction of the metal, its oxide with a carboxylic acid in the presence of an organic liquid phase and stimulating supplements of iodine in the bead mill, vertical type, characterized in that the oxidizer reagent in the lack of take the lead dioxide in the amount of 0.4-0.6 mol/kg, metal and acetic acid is dosed in amounts of from 0.6 to 1.5 mol/kg, respectively 2. The method according to claim 1, characterized in that the solvent of the liquid phase used isopropyl, isobutyl alcohol, ethyl cellosolve, dimethylformamide and butyl acetate.
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