Manganese (ii) fumarate synthesis method

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: method is easy to implement, the end product can be easily separated and there are no auxiliary materials which contaminate the obtained product.

2 cl, 11 ex

 

The invention relates to a technology for obtaining salts of manganese (II) and organic acids and can be used in various fields of chemical and other practices, analytical control and research.

The literature describes the possibility of a direct interaction of carboxylic acids, including fumaric, with manganese in the presence of mostly organic liquid phase and stimulating certain additives (Sedoideae, Amiano, Toumanova, Ivhave, Iautushenka. Some Macrokinetics characteristics of direct interaction of carboxylic acids with manganese in organic media in a bead mill. News of the Kursk state technical. Univ. 2008. No. 2(23). P.45-51). The process is carried out in a bead mill, vertical type with glass beads as pereirago agent mass ratio with loading the initial reaction mixture is not less than 1:1. However, even in such cases, the quantitative conversion of the reagent shortage of salt-product is often not achieved.

Another disadvantage of the identified variants is that in the absence of additional, and significant and diverse information, it cannot be formed in a method of obtaining a specific salt of manganese and carboxylic acids, including fumarata manganese.

Closest to the claimed what is the method of obtaining fumarata iron (II) (Patent BE 658067. Procédé de préparation du sel anhydre de fer left-hand drive vehicles l acide fumarique. Pub. 30.04.1965), according to which anhydrous fumarate, iron (II) produced by interaction of metallic iron with excess fumaric acid at elevated temperatures in aqueous medium in the absence of air.

The disadvantages of this method are:

1. In a series of voltages manganese is significantly to the left of iron, which determines the easier its interaction with the carboxylic acid in comparison with iron. Therefore, the related factor of the process conditions in the case of manganese must be significantly different in relation to the above in the known method for iron.

2. The salts of the dominant valence state of manganese is divalent. For iron, on the contrary, trivalent. Most likely, indicated in a known solution to a process without access of air when the implementation is similar to the process variant with manganese are not necessary.

3. There is no reason to assume that used in the known solution to the water environment will be acceptable, not to mention the best, upon receipt of manganese salt.

4. There is no reason to assume about the acceptability upon receipt of manganese salt of a temperature mode of obtaining fumarata iron (II).

5. Fumarate, manganese and fumarate, iron (II) significantly different from the AMI physical characteristics including the solubilities in different environments. This causes significant differences in the strength, fragility, adhesion characteristics, ability to soften and be liquefied, etc. blocking the metal surface sediments of these salts, as well as differences in the phase conditions of the reaction mixtures and the dominant phase accumulation of the target product is salt. Hence, significant differences in the methods and allocation of product and processing of reaction mixtures in General.

The objective of the proposed solution is to find such conditions for direct interaction of manganese with fumaric acid, which would provide a virtually quantitative conversion of the metal salt with a stoichiometric ratio of the reactants or with a small excess of carboxylic acid, as well as the buildup mostly in the form of a solid phase suspended particles, separated from the rest of the reaction mixture by filtration or settling.

The problem is solved in that the process is carried out in a bead mill, vertical type, the mass ratio of glass beads and loading the reaction mixture is 1:1, as the liquid phase loading take a solution of fumaric acid in an organic solvent containing acid 0,70-1,80 mol/kg, manganese metered in stoichiometric with Ki is lotay the amount or lack of up to 5%, the process begins with the loading solvent liquid phase and acid, as well as partial preparation of the acid solution in a running bead mill, and then load the metal and lead the process in the temperature range 25-35°C containment of the spontaneous growth temperature by the use of forced cooling and the control method of sampling and determination of the contents of manganese salt and the residual acid to achieve close to a settlement in the quantitative conversion of the reagent in the lack of values, after which the stirring and cooling stops, the suspension of the reaction mixture is separated from the glass beads, cooled to a temperature of 5.2 to 6.2°C and filtered, the filter cake washed with cooled to approximately the same temperature, the solvent of the liquid phase and is directed to purification by recrystallization, and the filtrate and the washing solvent in return repeated the process. As a solvent of the liquid phase using n-butyl, ISO-butyl, ISO-amyl alcohols and ethyl cellosolve.

Characteristics of the raw materials used

Manganese reactive GOST 6008-90.

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

n-Butyl alcohol according to GOST 6006-78.

ISO-Butyl alcohol according to GOST 9536-79.

ISO-Amyl alcohol according to GOST 5830-70.

The ethyl cellosolve according to GOST 8313-88.

Conducting process savla the th following way. In ball mill vertical type with high-speed paddle stirrer and glass beads as pereirago agent mass ratio with loading the reaction mixture 1:1 load the calculated quantity of solvent liquid phase and fumaric acid. Include mechanical mixing and lead the preparation of a solution of fumaric acid for some time. 100%dissolution of the acid in this period is not required. Therefore, this operation is completed after a certain experimentally selected time. At this point, load the estimated number of metallic manganese, and the reactor vessel is placed in a cooling bath. All this is done without stopping stirring the reaction mixture. Adjusting the intensity of the removal of the reaction heat, establish and stabilize the temperature at a given level. During the process, take samples of the reaction mixture, which determine the number of accumulated salt of manganese (II) and the content of unreacted acid. To achieve the expected values of these characteristics, the process stops, remove the cooling bath, separating the reaction mixture from the glass beads, which are returned to the reactor where it is, the stirrer and the walls of the reactor is rinsed cooled to a temperature of ~6°C below the solvent of the liquid phase from ostad is in the reaction mixture.

The reaction mixture after cooling to 5.2 to 6.2°C and below is filtered, the residue on the filter is washed with a solvent from the reactor, and then removed from the filter and is directed to purification by recrystallization. And the filtrate and the washing solvent is returned back to 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 127 mm and high speed (2500 rpm) with a mechanical stirrer vane type with dimensions of the blade 51×56 mm Plexiglas thickness of 4.5 mm, with a reflux-condenser at the outlet of the gas space and a liquid cooling bath sequentially load of 100 g of glass beads, 81,2 g of n-butyl alcohol and of 12.76 g of fumaric acid. Include mechanical stirring for 10 min lead the preparation of the acid solution. Further down the liquid cooling bath so that at least 80% of the height of the reactor was immersed in a bath, serves duct cooling water and stopping stirring, enter 6,04 g of manganese metal. The time taken for the beginning of the process, which in this period was developed with maximum speed. The exothermic process that determines the growth temperature of the reaction mixture. Adjusting the intensity of the forced teplota is a, stabilize the temperature at 32±1°C, which support during the redox process.

In the course of the process using special sampler is inserted into the slot in the lid of the reactor, take samples of the reaction mixture, which determine the content fumarata manganese and the remaining acid. It turned out that 25, 50, 75 and more than 98%degree of conversion of manganese and acid (loaded in the stoichiometric ratio) achieved 5, 14, 21 and 53 minutes Upon receipt of the last time characteristics of the process stop, which stop mechanical stirring and removing the cooling bath.

The reactor is disconnected from the lid, remove from the frame of the frame, where it is always in the same position, and the contents transferred into a funnel with a mesh size of 0.3×0,3 mm mesh to separate the glass beads and return to the reactor, which again connects with a lid and put into place in frame frame. Next type 45 g chilled to 6.5°With n-butyl alcohol, include mechanical stirring for 5 min conducting washing the blades of the mixer, reactor vessels and beads from the remainder of the reaction mixture. Washed in this way the beads are separated from the leaching solvent and washed them the reaction mixture again and then sent to re-download the tortured.

The reaction mixture after the initial separation of the beads are cooled to 6°C and filtered. The filter cake was washed with chilled solvent after removal of the residue of the reaction mixture on the surfaces of the mixer, its shaft, the walls of the reactor and glass beads, after which it a few dried in air duct, remove the filter and sent to purification by recrystallization. And the filtrate is combined with proryvnym solvent and sent to re-download process.

The product yield without taking into account losses from the return of the salt product from the filtrate and proryvnym solvent in the re process and when cleaning amounted to 0.108 mol. The degree of conversion of the reactants on the separated solid product is 94%.

Examples No. 2-11

The reactor, reagents, loading weight, the order of operations when downloading, the process and the separation of the reaction mixture, the duration of the cooking acid solution, the control during the process, and the determination of the moment of its termination is similar to that described in example 1. Different initial acid content, stoichiometric deficiency of metal, nature of the solvent used, the temperature of the process, the temperature of the reaction mixture during the filtration process and the temperature of the leaching solvent. These differences and the results obtained are summarized in table. (C - the reaction mixture, n-BS, and the BS and the MSS and EC - n-butyl, ISO-butyl, ISO-amyl alcohols and ethyl cellosolve.)

Load characteristics, process and product yieldExample No.
234567891011
the content in the initial PC, mol/kg
- fumaric acid0,700,951,251,501,801,801,051,051,401,05
- manganese0,700,951,251,501,761,711,051,051,331,05
the solvent of the liquid phasen-BSn-BSn-BSn-BSn-BSn-BSand-BSand-asand-asEC
zastabilizirovalsia temperature holding process (±1°C)25272933353532303428
time (min) achieve the degree of conversion of the manganese salt is a product
0,2514555668141215
0,5030181310121229453930
0,7548302421302976716270
0,9884667988105102118 111115121
the washing solvent, % by weight PC40424345505043414542
the temperature of the reaction mixture at the time of filtration, °Cof 5.4the 5.75,55,26,06,1of 5.46,26,15,5
the temperature of the refrigerated leaching solvent, °C6,36,45,96,06,26,35,85,66,35,8
the product yield without taking into account losses from the return of the filtrate and the washing solvent while cleaning % of theory. 0,690,931,231,481,731,681,031,031,311,03
the degree of conversion of the reactant in the Vice on the separated solid product, % of theory.89929595969695969795

The positive effect of the proposed solution is:

1. The proposed solution is the highest of all possible options for the transition of the mass of the initial reactants to the mass of the target product. The byproduct is hydrogen, the molecular weight is small, which does not require its disposal, is not a pollutant neither the environment nor the target product.

2. Used solvents for the liquid phase are available and repeatedly return to repeat the process.

3. Product accumulates predominantly in the solid phase and can be easily removed by simple filtration.

4. In this solution there is no spare is gateline substances, which would not have contributed a lot to the weight of the target product and to some extent polluted the target product.

5. Instrumentation process easy and not a boiler-supervising.

1. The method of obtaining fumarata manganese (II) by direct interaction of the metal with an acid, wherein the process is carried out in a bead mill, vertical type, the mass ratio of beads and loading the reaction mixture is 1:1, as the liquid phase loading take a solution of fumaric acid in an organic solvent containing acid 0,70-1,80 mol/kg, manganese metered in stoichiometric acid number or the lack of up to 5%, the process begins with the loading solvent liquid phase and acid and preparation of the acid solution in a running bead mill, and then load the metal and lead the process in the temperature range of 25-35°C containment of the spontaneous growth temperature by the use of forced cooling and the control method of sampling and determination of the contents of manganese salt and the residual acid to achieve close to a settlement in the quantitative conversion of the reagent in the lack of values, after which the stirring and cooling stops, the suspension of the reaction mixture is separated from the glass beads, cooled to a temperature of 5.2 to 6.2°C and Phil is trout, the filter cake was washed with cooled to approximately the same temperature, the solvent of the liquid phase and is directed to purification by recrystallization, and the filtrate and the washing solvent in return repeated the process.

2. The method according to claim 1, characterized in that the solvent of the liquid phase take n-butyl, ISO-butyl, ISO-amyl alcohols and ethyl cellosolve.



 

Same patents:

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

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SUBSTANCE: invention is related to improved method for preparation of manganese oxalate (II) by means of direct interaction of metal with acid in bead mill in presence of liquid phase, in which manganese and oxalic acid are loaded into bead mill in stoichiometric ratio in amount of 0.75-2.4 mole/kg of load at mass ratio of load and glass beads of 1:1.2, liquid phase dissolvent used is water or organic substance, or mixture of organic substances; loading is carried out in the following sequence: liquid phase dissolvent, acid, then metal; process is started at room temperature and is carried out under conditions of forced cooling in the temperature range of 18-39°C with control over procedure by sampling method to practically complete spend of loaded reagents for product making, afterwards mixing and cooling are terminated, suspension of reaction mixture is separated from glass beads and filtered, salt deposit is sent for product cleaning from traces of non-reacted metal, and filtrate is returned into repeated process.

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2 cl, 13 ex, 2 tbl

FIELD: chemical industry; methods of production of the manganese salts with the organic acids.

SUBSTANCE: the invention is pertaining to production of the manganese salts with the organic acids in particular, to the salt of the divalent manganese and formic acid. The method is exercised by interaction of manganese, its oxides in the state of the highest valence with the formic acid solution in the organic solvent in the presence of iodine as the stimulating additive. The production process is conducted in the bead grinder of the vertical type having the revertive cooler-condenser, the high-speed paddle stirrer and the glass beads of in the capacity of the grinding agent loaded in the mass ratio to the loading of the liquid phase as (1÷2): 1. The liquid phase consists of the formic acid solution in the organic solvent. The concentration of the acid is taken within the range of 3.5÷10.8 mole/kg. In the loaded liquid phase they dissolve the stimulating additive of iodine in the amount of 0.025-0.100 mole/kg of the liquid phase. The ratio of the masses of the liquid phase and the total of the metallic manganese and the manganese oxide are as(4.9÷11):1. The molar ratio of the metal and the oxide in the loading is as (1.8÷2.,2):1. The metal and the oxide are loaded the last. It is preferable in the capacity of the dissolvent to use the butyl alcohol, ethyl acetate, ethylene glycol, 1.4-dioxane, dimethyl formamide. The production process is started and conducted at the indoor temperature up to practically complete(consumption of the whole loaded manganese oxide. Then the stirring is stopped, the suspension of the salt is separated from the beads and the nonreacted manganese and after that conduct filtration. The filtrate and the nonreacted manganese are returned into the repeated production process, and the filtered out settling of the manganese salt is exposed to purification by recrystallization. The technical result of the invention is - simplification of the method at usage of accessible reactants.

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16 ex, 2 tbl

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3 ex, 1 tbl

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EFFECT: improved method of synthesis.

3 cl, 9 ex

FIELD: catalyst preparation methods.

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EFFECT: improved economical and environmental characteristics of process.

FIELD: organic chemistry, medicine, physiology.

SUBSTANCE: invention relates to agents for regulation (maintaining or suppression) of physical working ability and/or adaptation to different variants represented by solvated complex compounds of the general formula (I): Katm+[L1qEL2]Ann- x p.Solv (I) wherein L1 means aminothiols of the formula: R1NHCH(R2)(CH2)1-2SR3 wherein R1 means hydrogen atom (H), (C1-C20)-alkyl or RCO; R means (C1-C19)-alkyl; R2 means H or carboxyl; R3 means H, (C1-C20)-alkyl, (C2-C20)-alkenyl or benzyl; q = 1, 2 or 3; L2 means halogen atom, water and/or organic ligand. For example, bis-(N-acetyl-L-cysteinato)aquozinc (II) diheptahydrate suppresses physical working ability and in the dose 50 mg/kg increases reviving time of mice by 6 times and cats - by 2.8fold under conditions of acute hypoxia with hypercapnia, and increases reviving time of mice by 4 times under conditions of acute hypobaric hypoxia. Under the same conditions the known antihypoxic agents amtizol, acizol or mexidol are inactive or less active significantly by their activity. Bis-(N-acetyl-L-cysteinato)-ferrous (II) pentahydrate is more active as compared with the known antihypoxic agents and protects experimental animals in 4 variants of hypoxia. Bis-(N-acetyl-L-cysteinato)zinc (II) sulfate octahydrate is similar to enumerated compounds by its antihypoxic activity.

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4 cl, 1 dwg, 11 tbl, 33 ex

The invention relates to the objects of the invention characterized in the claims, i.e

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: improved method of producing said product.

8 ex

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 organic synthesis

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: liquid phase used together with the sodium chloride additive can be repeatedly returned to the process.

10 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: improved method of producing said product.

8 ex

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: non-waste method at low temperature; wastes from other industries can be used as reagents; desired products can be separated by simple filtration.

2 cl, 8 ex

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: mechano-activated amorphous and amorphous-crystalline compounds and compositions are used as active compounds for making pharmaceutical preparations.

13 cl, 10 dwg, 12 ex

FIELD: chemistry.

SUBSTANCE: 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.

EFFECT: process takes place at acceptable rates and ends with virtually complete consumption of all loaded reagents.

2 cl, 19 ex

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

FIELD: medicine.

SUBSTANCE: invention refers to a new product in the form of solution for treatment of benign, virus, premalignant and malignant nonmetastasing skin affections, dysontogenetic lesions of visible mucous membranes, skin mycoses, wrinkle correction and senile pigment spots. The product represents a compound of general formula H2SeO3·x·[R-CXY-(CH2)m-COOH], where x=2-6 prepared from reaction of selenium dioxide and haloid carboxylic acids of general formula R-CXY-(CH2)m-COOH, where R = phenyl, alkyl of general formula CnH2n+1; n=1-5, X=H or Y, Y=F, CI, Br or J, m = 0-10. Besides, the invention concerns a product in the form of solution for treatment benign, virus, premalignant and malignant nonmetastasing skin affections, dysontogenetic lesions of visible mucous membranes, skin mycoses, wrinkle correction and senile pigment spots, containing 0.1-50 wt % of said product, 1-99 wt % of haloid carboxylic acids and the rest - water. Also the invention concerns method of treatment of various skin diseases, including topic applications of the product.

EFFECT: improved clinical effectiveness of the product and method of treatment.

6 cl, 3 dwg, 1 tbl, 68 ex

FIELD: chemistry.

SUBSTANCE: invention relates to improved method of obtaining nickel (II) oxalate NiC2O4·2H2O, which includes preparing of reaction water solution, which contains nickel (II), precipitation of nickel oxalate, separating of sediment from solution and its drying, in which as nickel source used are solutions of nickel chloride, nitrate, sulphate, and as reagent-precipator used is anionite AB-17-8 in oxalate form. Obtained product can be applied in industry for producing catalysts, metal films, polymetal alloys, ceramic-metal and ferromagnetic substances, as well as in production of electrovacuum devices.

EFFECT: obtaining target product of high degree of purity, which does not contain admixture anions and cations, which eliminates necessity of long washing of obtained sediment.

6 tbl, 3 ex

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