Method of producing manganese (ii) fumarate from manganese metal and manganese (iii) oxide

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: design of a low-waste method, which allows for obtaining target product from available manganese oxide with an easy to implement process.

9 ex

 

The invention relates to the technology of salts of manganese and can be used in various fields of chemical and other practices, analytical control and scientific research.

A method of obtaining manganese acetate (U.S. Pat. Of the Russian Federation No. 2294921, publ. 10.03.2007, bull. No. 7) by direct interaction of the metal and manganese dioxide with acetic acid in the presence of additives iodine as oxidant in a bead mill, vertical type, in accordance with which the loading of the metal and its oxide is produced in a molar ratio of 2:1 in the amount of 11.8% by weight of a liquid phase comprising an organic solvent and acetic acid with a concentration of 3.4-5 mol/kg and dosed in a mass ratio of glass beads of 1:1.5; in the liquid phase dissolved iodine in the amount of 0.025-0,070 mol/kg liquid phase, loading produce in sequence: liquid phase or its components separately, iodine, metal and dioxide; the process begins at room temperature and lead to the almost complete consumption of dioxide; obtained a suspension of the salt is separated from the main part of the unreacted metal and glass beads, and sent for filtration, the filtrate is returned to repeat the process, and the precipitate of product was then purified by recrystallization. The organic solvent used ethyl-cellosolve, trangleball, 1,4-dioxane, ISO-amyl and n-butyl alcohols. And the content in the liquid phase of water up to 4 wt.% practically does not affect the characteristics of the process.

The disadvantages of this method are:

1. As the oxidant used manganese dioxide Mno2. It is far from clear that it can be replaced by manganese oxide (III) PM2About3and get an equivalent described or closer result.

2. Acetic acid is monobasic, pretty low molecular weight normally liquid, able to mix with many solvents in a fairly wide ranges of ratios. Fumaric acid is dibasic, unsaturated, more high molecular weight normally solid, solubility in different solvents will be very different. There is no reason to expect that the conditions of the processes of obtaining salts of acetate and fumarata manganese (II) will be identical throughout the complex or its defining part.

3. To create noticeable and even a significant excess of acetic acid in the initial download is very simple, because this acid may be not only a reactant, but also part of a combined solvent of the liquid phase. Fumaric acid in the past as impossible, and to create a large surplus in the download is much more complicated.

Closest to sawla what the PTO is a method of producing formate, manganese (II) (U.S. Pat. Of the Russian Federation No. 2316536, publ. 10.02.2008, bull. No. 4), whereby the target salt is produced by direct interaction of manganese oxide with a solution of formic acid in an organic solvent with a concentration of acid 3,5÷10,8 mol/kg, as manganese oxide used MnO2, MP2O3,

MP2O4the process is carried out in the presence of manganese metal in a molar ratio of oxide (1,8÷2,2):1 in the presence of a liquid phase, the dosed mass ratio of solid reagents (4,9÷11):1 and with glass beads of 1:(1÷2), as well as stimulating supplements of iodine in the amount of 0.025÷0,100 mol/kg liquid phase; loading lead to sequence the liquid phase as a whole or its components, then it is dissolved stimulating Supplement iodine, followed by loading of the metal and its oxide, further include mechanical stirring bead mills and lead the process in the absence of an external supply of heat to the almost complete consumption of the oxide, after which the reaction mixture is separated from the glass beads and heavy particles of unreacted metal and filtered, the precipitate of manganese formate sent for recrystallization, and unreacted manganese and the filtrate is returned to repeat the process. As a solvent of the liquid phase using ethyl acetate, ethylene glycol, ethyl cellosolve, 14-dioxane, dimethylformamide and n-butyl alcohol.

The disadvantages of this method are:

1. As described in claim 2 and 3 in respect of the method of producing manganese acetate. Formic acid is more low molecular weight in respect of acetic acid. Therefore, it allows the creation of a more stoichiometric excess of this reagent in the download.

2. In the known solution the metal is loaded in relation oxide with a substantial stoichiometric excess, which entails the separation of the unreacted part from the rest of the reaction mixture, and return to the re-download process. Preferably an excess of metal loading to exclude and eliminate the associated operations for separation and recycling.

3. The ability of the product mainly accumulate in the solid phase under other equal conditions predetermined by the solubility and other physical properties of the target salt, and hence the nature of the acid. There is no reason to believe that formate and fumarate, manganese will have similar physical characteristics, allowing the separation of the product from the rest of the reaction mixture to conduct identical ways.

4. There is no reason to assume that the transition from use as a reagent low molecular weight monobasic acid to the more high-molecular unsaturated dibasic Ki the lot will not lead to noticeable changes in the sequence of the individual operations and their modal characteristics.

The objective of the proposed solution is to find such ratios downloads metal and its oxide MP2About3and conditions of their interaction with fumaric acid, which would provide almost quantitative conversion of both metal and oxide in the Sol with a relatively small excess carboxylic acid and salt in the final reaction mixture predominantly in the solid phase, and separating the latter by simple filtering.

This object is achieved in that the loading of the metal and its oxide charge in a molar ratio of (2±0,1):1 total number 7,87÷of 10.93% by weight of the boot, the acid is injected with 15-25%excess of the rated value equal to the number of moles of metal and twice the number of moles of metal oxide in the download, as the basis of the liquid phase take ISO-amyl alcohol in which is dissolved a stimulating Supplement iodine in the amount of 0.02 to 0.05 mol/kg, loading start with glass beads introduced into the mass ratio of the reaction mixture of 1.35:1, then enter the solvent liquid phase, acid and stimulating additive and after a short stirring without stopping the metal oxide and the metal, taking this moment for the beginning of the process, immediately impose forced cooling, stabilize the operating temperature in the range 33-45°C in this mode, bring the process to an almost quantitative conversion of the loaded metal and its oxide in the target salt, after stirring and external cooling to stop the reaction mixture is separated from the glass beads, cooled to a temperature of 5-6°C and maintained at this temperature for 1-2 hours, the solid phase target salt is filtered and washed on the filter is cooled to approximately the same temperature ISO-amyl alcohol, and then sent for purification by recrystallization, and the filtrate and the washing solvent containing excess acid, the bulk of the stimulating additive and a small amount of dissolved target salt, return to the re-download process.

Characteristics of the raw materials used

Manganese reactive GOST 6008-90.

Manganese oxide MP2O3on THE other 6-09-3364-78.

Iodine crystal according to GOST 4159-79.

Fumaric acid on THE 6-09-4008-75.

ISO-Amyl alcohol according to GOST 5830-70.

The process of the inventive method the following. In a ball mill, vertical type, equipped with a high-speed stirrer vane type, reversible refrigerator-condenser and cooling bath with cold running water as a cooling agent, enter the estimated number of glass beads, solvent, liquid phase, fumaric acid and stimulating supplements of iodine. Include mechanical mixing and after 5-10 minutes, stopping stirring, the lead calculated quantity of metal and its oxide MP 2About3. The time taken for the beginning of the process. Immediately casing bead mill is immersed in a cooling bath and observe the temperature change in the reaction zone. The process is exothermic, at what expense, and also work bead mill, its contents are starting to heat up. Adjusting the degree of immersion of the hull bead mill in bath, cooling water temperature and the speed of its flow, stabilize the temperature within the operating range and in this mode, bring the process to an almost quantitative conversion of the metal and its oxide in the target Sol. This point is determined by the method of sampling and determination of the contents of the accumulated salt of manganese (II), and spent oxide of manganese, manganese and acid.

At the end of the process, the mixing and cooling is stopped, the reactor is removed from the slot of a frame of a frame and its contents poured into a container with a mesh size of 0.3×0.3 mm, where the separation of glass beads from a solution-suspension of the reaction mixture. To reduce the solubility of the target salt in the liquid phase of the reaction mixture is slowly cooled down to the last 5-6°C and maintained at this temperature for 1.5-2 hours, and then filtered.

The separated beads return to the ball mill, which is placed in the corresponding socket of the skeleton frame and lead in working sostoyaniyam impose a certain amount of solvent liquid phase, include mechanical mixing process, the washed beads and the surface of the stirrer and the body from remaining on them the reaction mixture. Then the washing solvent is separated from the beads, cooled to 5-6°C and used for washing the precipitate target salt on the filter. The washed precipitate is drained, a few dried in a stream of air is removed from the filter and sent for further purification by recrystallization. And the filtrate and the washing solvent after analyses on the content of the acid, iodine, iodide, manganese and fumarata manganese and determine the mass return to the re-download process.

Example 1.

In ball mill vertical type with glass enclosure in the form of a Cup with an inner diameter of 53.7 mm and a height of 133 mm, equipped with a reflux-condenser, high speed (2500 rpm) with a mechanical stirrer vane type with a rectangular blade of the PCB dimensions 51×56 mm and a thickness of 4.2 mm, load 135 g of glass beads with a diameter of 1.8-2.6 mm, 65,57 g of ISO-amyl alcohol, 23,21 g of fumaric acid and 0.51 g of crystalline iodine. The reactor is put into place in the frame frame, cover with stuffing box for mixer loading opening, the outlet at a reflux-condenser and jacks for measuring temperature, and sampler and include mechanical is stirring. After 10 min the solution acid and iodine in ISO-amyl alcohol through the loading hatch without mechanical mixing, enter 4,39 g manganese and 6,32 g of oxide MP2O3. The time taken for the beginning of the redox process. Immediately below summarize the cooling bath with a flowing cooling water and observe the temperature change in time. By varying the depth of immersion of the body in a bath and a feed rate of cooling water, set the working temperature at 42±1°C, which is maintained until the process is complete.

In the course of the process take samples of the reaction mixture, which determine the content fumarata manganese, acid and metal oxide. It turned out that 25, 50, 75 and more than 98%of estimated target salt the degree of conversion achieved respectively for 4, 12, 28 and 56 minutes after 60 min stirring and cooling stop, casing bead mill disconnect from the lid with agitator and down, allowing the remaining stirrer reaction mixture to partially drain that spend 5 minutes After that, the reactor is poured into the receiving tank filter grid with a cell size of 0.3×0.3 mm as a filter partition. The reaction mixture is in the form of a solution-suspension of the salt falls down, Ana the grid is glass beads. It is removed from the grid and return to the reactor. The last place in the workplace in a frame a frame is connected to the lid with agitator and collect in working condition. Added 43 g of ISO-amyl alcohol, include mechanical mixing and washed the surface of the housing, agitator, its shaft and beads from the remainder of the reaction mixture within 5 minutes After the wash solvent is separated from the beads as described above and is directed to cooling to 5.3°C.

In parallel with the cleaning of the reactor, beads and agitators from the remainder of the reaction mixture collected after separation of the solution-suspension of the target salt cooled over 1 hour to a temperature of 5.6°C and maintained at this temperature 115 minutes Then cooled reaction mixture is subjected to vacuum filtration. The filter cake was washed with chilled spent solvent, and then sent for purification by recrystallization. And the filtrate and the washing solvent containing unreacted acid, iodine-containing stimulatory Supplement (partly in the form MnI2) and a small amount of dissolved fumarata manganese, return to the re-download process.

The output is separated by filtration product is 94% of the calculated values in almost quantitative consumption of the metal and its oxide MP2About3on education is the W target salt.

Examples 2-9

The reactor, the initial reactants, the solvent of the liquid phase, stimulating additive, the weight of the load and its relationship to the mass of glass beads, the order of operations when downloading, the process termination and separation of the product from the reaction mixture similar to that described in example 1. Different molar ratio of the content of the metal oxide loading, absolute metal content, excess fumaric acid, the total amount of solid reagent loading, the initial dosage of iodine and an operating temperature of the process. These differences and the results obtained are given in table. (PC - reaction mixture)

Load characteristics, process and product yieldExample
23456789
the initial content of a metal oxide, mol/kg0,300,300,300,330,370,40 0,400,40
the molar ratio of metal oxide to load1,9:1a 2.0:12,1:1a 2.0:1a 2.0:11,9:1a 2.0:12,1:1
the content of fumaric acid, mol/kg1,461,451,541,561,791,90to 1.861,89
the estimated excess fumaric acid, %2521251821221615
mass loaded ISO-amyl alcohol, g73,9174,1073,0272,2668,7066,5267,0766,62
share TV is rdih reactants (metal and oxide) download weight%7,878,038,208,84to 9.9110,4910,71of 10.93
the iodine content in the original PC, mol/kg0,0500,041being 0.0360,0310,0240,0370,0470,020
the operating temperature of the process, °C3337403836454543
time (min) achieve a certain percentage (in %) yield of the desired salt from the calculated value
0,2564 347345
0,50118891671114
0,752116152229162636
0,983531293641405567
the total duration
process min
4035364247486174
the washing solvent, % by weight PC 3739414340464547
the temperature of the reaction mixture at the time of filtration, °C5,0the 5.76,06,05,8of 5.45,25,1
the temperature of the refrigerated leaching solvent, °C5,35,25,0of 5.4the 5.75,86,06,0
excerpt chilled PC before filtering, min1201151119287607382
the output is separated by filtration of the target product, % of theory.9494 959596949697

The positive effect of the proposed solution is:

1. Up to 50% of the target salt is obtained from oxide of manganese MP2About3that compared with a metallic manganese more accessible, being a natural connection (Brunet, manganite).

2. The process is carried out in mild conditions of temperature, largely supported by the reaction heat and a small forced cooling.

3. The selected liquid phase allows for the use of additional cooling PC to ensure transition of the main mass of the accumulated target salt in the solid phase, easily distinguishable by simple filtering.

4. During the process, do not accumulate any inhibitors interaction that allows detachable liquid phase to repeatedly return to repeat the process. This return must be disposed of unreacted carboxylic acid and catalytic additive (I2and iodide, manganese). All this allows to characterize this process as low.

5. When carrying out this process, there is no volatile wastes pollution to the environment.

6. Instrumentation process is very simple. There is no boiler-supervising about what orogovenia. Pretty simple and current control methods, as well as determining the date of termination of the redox process.

The method of obtaining fumarata manganese (II) metal and its oxide (III) by direct interaction of the metal and its oxide Mn2About3with acid in the presence of a liquid phase and stimulating supplements of iodine in the bead mill, vertical type with glass beads as pereirago agent, characterized in that the loading of the metal and its oxide charge in a molar ratio of (2±0,1):1 total number 7,87-of 10.93% by weight of the boot, the acid is injected with 15-25%excess of the rated value equal to the number of moles of metal and twice the number of moles of metal oxide in the download, as the basis of the liquid phase take isoamyl alcohol in which is dissolved a stimulating Supplement iodine in the amount of 0.02-0.05 mol/kg, loading start with glass beads introduced into the mass ratio of the reaction mixture of 1.35:1, then enter the solvent liquid phase, acid and stimulating additive and after a short stirring without stopping the metal oxide and the metal, taking this moment for the beginning of the process, immediately impose forced cooling, stabilize the operating temperature in the range 33-45°C in this mode, bring the process to an almost quantitative accepts the stop of the loaded metal and its oxide in the target salt, after stirring and external cooling to stop the reaction mixture is separated from the glass beads, cool the temperature of 5-6°C and maintained at this temperature for 1-2 h, the solid phase target salt is filtered and washed on the filter is cooled to approximately the same temperature isoamyl alcohol, and then sent for purification by recrystallization, and the filtrate and the washing solvent containing excess acid, the bulk of the stimulating additive and a small amount of dissolved target salt, return to the re-download process.



 

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8 cl, 4 ex

FIELD: chemistry.

SUBSTANCE: invention refers to organic chemistry, to chlororganic technology, specifically to advanced method of chloroacetic sodium salt production allowing for high quality with minimum power inputs. Method of chloroacetic sodium salt production (Na-CA) is characterised by that dry initial components that are soda ash (Na2CO3) and chloroacetic acid (CA) are continuously dispensed in stoichiometric ratio to desintegrator or dismembrator with linear speed of disk pins 30-150 m/s, where exposed to mechanochemical influence. Thereafter produced Na-CA is continuously supplied to drying. Produced in offered method Na-CA completely meets quality requirements of standard documents.

EFFECT: high quality products with minimum power inputs.

7 cl, 2 dwg, 3 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: simplification of monophase palladium (II) acetate production with decreased adverse environmental effects of process products.

2 cl, 2 tbl, 4 ex

FIELD: chemistry.

SUBSTANCE: preparation of liquid flow I, containing formic acid, and liquid flow II, containing alkali metal formate, is carried out; liquid flows I and II are supplied to rectification column in such way that for liquid flow II place for feeding into rectifying column is chosen higher than place of feeding liquid flow I, or the same place as for liquid flow I, liquid flows I and II are mixed in rectification column, removing water from upper part of rectification column, and lower flow, containing formic acid formate is removed from rectification column, lower flow being separated in form of melt, which contains less than 0.5 wt % of water.

EFFECT: improved method of production of formic acid formates.

10 cl, 4 ex

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: obtaining high yield of monophase palladium (II) acetate without admixture of insoluble polymeric palladium (II) acetate and palladium (II) nitritoacetate.

3 cl, 1 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: streamlined method for obtaining palladium (II) acetate and its synthesis in monophase condition without admixture of insoluble polymeric palladium (II) acetate and palladium (II) nitritoacetate.

2 cl, 1 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: duration decrease and efficiency increase of zirconium carboxylate production; elimination of chemically pollutant effluents formation.

5 cl, 1 tbl, 14 ex

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