Method of producing malonate and manganese (ii) succinate
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
The invention relates to a technology for manganese salts of saturated dicarboxylic acids of the fatty series and can be used in various fields of chemical practice, and analytical control and research.
A method of obtaining manganese succinate (RF patent No. 2174508), according to which succinate d-elements receive the action of the sulphate of the corresponding d-metal reaction solution mixture of succinic acid and sodium hydroxide in a molar ratio of 1:2 at 80-85°C for 20-30 min, followed by cooling the reaction mixture to 10-15°C and separation of precipitated crystalline product by filtration, washing the precipitate with cold water (5-7°C) from sulfates and drying in a vacuum Cabinet at a temperature of 35-40°C and a pressure of 20 mm Hg
The disadvantages of this method are:
1. Although sodium succinate is not specifically singled out as a standalone product in terms of technology, the process is two-stage, namely getting succinate or sodium reaction solution and the cation exchange sodium salt of the reaction solution of the cation d-metal contact with sulphate of the metal.
2. Sodium hydroxide is easily watered with, and that required consideration in the preparation of the reaction solution; in the absence of the latter mixing acid and loci in a molar ratio of 1:2 predetermines some excess acid, you'll have to remove when cleaning the product.
3. In the process formed a byproduct sodium sulfate, which has to be disposed.
4. Used solutions may not be concentrated to avoid thickened paste product instead of easily filterable slurry. The temperature of 80-85°C involves heating primarily water as the solvent, which causes high power consumption of the process.
5. This process results in large amounts of wastewater that requires appropriate processing and other costs.
Closest to the claimed is a method of producing manganese acetate (II) (patent RF №2294921), according to which the specified salt is produced by direct interaction taken in a molar ratio of 2:1 metal and manganese dioxide with acetic acid in a solution of ethyl cellosolve, ethylene glycol, 1,4-dioxane, isoamyl or n-butyl alcohol in the presence of iodine supplements. The process is carried out in a bead mill, vertical type with high-speed paddle stirrer and glass beads as pereirago agent. The concentration of acetic acid in the liquid phase 3,4-5 mol/kg, the content of the metal and its oxide (of solid reactants) loading 11.8% of the liquid phase. The mass ratio of the liquid phase and the glass beads of 1:1.5. The iodine content in the liquid phase of 0.025-0,070 the ol/kg The process begins at room temperature and lead to the almost complete consumption of manganese dioxide. The salt suspension is separated from the main part of the unreacted metal and glass beads, and is directed to the filtering. The filtrate is returned to repeat the process, and the residue is purified from impurities of metal recrystallization.
The disadvantages of this method are:
1. Acetic acid is monobasic, while malonic and succinic acid is dibasic, and significantly more strong: PKandfor acetic acid, 4,75, malonic - 2,86 and 5,70, amber - 4,21 and 5,64. It is not certain that these acids in comparable terms will react the same type.
2. Marked dicarboxylic acid heavier in comparison with acetic acid and then in normal conditions are solid. Moreover, they have different solubility in different organic media. There is no reason to assume that they will be able to translate into the solution in the appropriate solvent in the amount of 3.4-5.0 g-EQ/kg, as this is easy to do in the case of acetic acid.
3. In the analyzed solution laid the excess metal from which you want to end the reaction mixture is separated, and the product is clear from its traces. In order not to carry out these operations in full, and even better to eliminate them completely, you need excess metal from the source to the load to be removed. And for this you need to know what the real excess metal is needed and how much it affects the characteristics of the redox process. Most likely, this parameter depends on the nature of the acid, but at this point in time is unknown.
4. Salt of acetic acid is preferentially stored in the solid phase, which gives the opportunity to separate it by filtration. There is no certainty that such a provision be retained in the case of malonic and succinic acids.
5. In the case of acetic acid by the criterion of the date of termination of the process is almost complete consumption of manganese dioxide. There is no reason to believe that this approach will continue during the transition to dicarboxylic acids.
6. The duration of the process with acetic acid in 100 minutes or more. At such speeds, the selection of the reaction heat is weakly violated isothermal or close to it mode process in the absence of forced cooling. It is not certain that this situation will continue during the transition to malonic and succinic acids, where the heat release rate can be considerably large.
The objective of the proposed solution is to match the molar ratio of manganese, dioxide and acid in the initial download, and such conditions for oxidation and restore the construction process, so he proceeded with acceptable speed and ended with the almost complete withdrawal of all loaded reagents in acceptable time.
This object is achieved in that the manganese, dioxide and dicarboxylic acid in the initial download take in a molar ratio of (1+x):1:(2+x) to produce (2+x)m moles of salt, where x in the molar ratio of the loaded reagents take 0,4±0,1 for succinic acid and 1.0±0.1 malonic acid, a m - the number of moles of manganese dioxide in the download, iodine dosed in amounts of 0.05 mol/kg of the reaction mixture after loading of organic solvent and acid, but before loading dioxide manganese and metal, while the sum of the masses acid, metal and dioxide charge in the range of 15-25% by weight of the bootstrap, and the mass ratio of the beads and loading 1:1; the process begins at room temperature and are in conditions of forced cooling in the temperature range from room temperature up to 40°C, With the control method of sampling the reaction mixture until almost full expenditure of all loaded reagents in the target salt, after which it ceased, the suspension of the final reaction mixture is separated from the beads and filtered, the precipitated product is washed with a solvent liquid phase and is directed to the removal of traces of metal and its dioxide by recrystallization, and the filter is t, and the washing solvent in return repeated the process. As the organic solvent of the liquid phase take n-propyl, n-butyl and ISO-butyl alcohol, butyl acetate, xylene, white spirit and heptane
Characteristics of the raw materials used
Manganese reactive GOST 6008-90
Manganese dioxide according to GOST 4470-79
Iodine crystal according to GOST 4159-79
Malonic acid on THE 6-09-2608-77
Succinic acid according to GOST 6341-75
n-Propyl alcohol, GOST 9805-84
n-Butyl alcohol according to GOST 6006-78
ISO-Butyl alcohol according to GOST 9536-79
Butyl acetate according to GOST 8981-78
Heptane reference (TU 6-09-4520-77)
m-Xylene (TU 6-09-2438-77)
White spirit technical GOST 3134-78.
The process of the inventive method the following. In ball mill vertical type with glass enclosure and high-speed mechanical paddle stirrer of durable and indifferent to the process of plastic and glass beads as pereirago agent loads the calculated amount of beads and components initial load, in particular solvent liquid phase, dicarboxylic acids, stimulating supplements of iodine, metal and dioxide. Include mechanical mixing and the time taken for the beginning of the process. During the process, take samples of the reaction mixture comprising the components of the boot and products of their transformation, which determines the content of what she manganese and residual manganese dioxide and acid. As soon as the salt content of manganese sufficiently close to the calculated value, the process stops. The reaction mixture is separated from the glass beads and is sent to the filtering. Mixer, beads and casing mill washed with solvent liquid phase, which is then used to wash the precipitate obtained salt. The filtered solid salt is directed to the purification of the remaining traces of metal and its oxide by recrystallization, and the filtrate and the washing solvent in return repeated the process.
In a ball mill with glass casing inner diameter of 55 mm and a height of 104 mm, equipped with high-speed (1440 rpm) paddle stirrer made of durable fiberglass with a rectangular blade 52×40 mm, reflux-condenser and a liquid bath for forced cooling of the reaction mixture during the process, load consistently 100 g of glass beads with the diameter of the balls in the range from 1.5 to 2.8 mm, 80,73 g of n-butyl alcohol, 11,40 g of succinic acid, 1.27 g of iodine, 3.50 g of manganese dioxide and 3,10 g of manganese. Served water in a cooling bath, and a reflux - condenser and include mechanical stirring. The time taken for the beginning of the process. The temperature of the reaction mixture at this point was 18°C. In the course of the process control temperature is in the reaction zone and take samples of the reaction mixture, in which determine the salt content of manganese (II), as well as residual amounts of acid and manganese dioxide. 65 min-defined analysis of the salt content of manganese was equal 0,962 mol/kg, which is close to the calculated value (0,967 mol/kg), and the temperature in the reaction zone 29°C.
Repeated sampling and analysis confirmed the almost complete absence of unreacted manganese dioxide and acid in the reaction mixture.
Stop stirring the reaction mixture. The reaction mixture is separated from the glass beads passing through the wall in a grid with a cell size of ~0.3×0.3 mm, and then filtered. The reactor is assembled, the stirrer and the beads rinsed with running the mixer 30 g of n-butyl alcohol. Resulting mixture is sent to the flushing of sediment on the filter. The filtrate and the washing solvent in return repeated the process, and the precipitated product is directed to purification by recrystallization.
The product yield without taking into account losses during purification was 0,095 mol. The utilization of the acid on the formation of salts of 98.2%.
The reactor, the nature of the reagents and stimulating supplements, weight of downloads of each of the components and in General, the ratio of the mass of the load and the glass beads, the boot order of the components, the process and monitor the progress of its forms is Oia, the criterion of the date of termination of the process, the separation of the reaction mixture from the bead, separation of the product from the reaction mixture and its primary used washing solvent liquid phase is similar to that described in example 1. Differ by the nature of the used solvent. The obtained characteristics of the process and product yield are summarized in table 1.
|Load characteristics, process and output salts||Example No.|
|The solvent of the liquid phase||n-propyl alcohol||ISO-butyl alcohol||butyl acetate||m-xylene||white spirit||heptane|
|Operating temperature range, °C||18-28||18-27||18-31||18-24||18-23||18-2|
|The process duration, min||57||84||60||100||130||180|
|The yield of the product (excluding losses when cleaning), mol||0,096||0,095||0,096||0,095||0,095||0,095|
|The utilization of the acid to the target product, %||99,3||of 98.2||99,3||of 98.2||of 98.2||of 98.2|
The reactor, the nature of the reagents and solvent, the mass of the load, its relationship with the mass of glass beads, the iodine content in the boot, the boot order of the components and the process, the choice of the moment of termination of the process, the sequence of operations for separation of the reaction mixture from beads, selection of product, cleaning and return of the liquid phase in the reverse process similar to that described in example 1. Different value of x in a molar ratio of the reactants and the relative mass of the reactants in the initial download. Received financial p the tats are summarized in table 2.
|Load characteristics, process and output of product||Example No.|
|The value of x in a molar ratio of reagents||0,30||0,45||0,50||0,40||0,40||0,40|
|Download manganese dioxide mol||0,0349||0,0480||0,0538||0,0444||0,0495||0,0554|
|The relative mass of the reactants in the download, %||15,00||19,15||25,00||19,87||22,15||24,79|
|Operating temperature range, °C||22-33||22-39||22-38||23-40||22-40||25-40|
|The process duration, min||70||71||75||68||72||73|
|The yield of the product (excluding losses when cleaning), mol||0,079||0,100||0,132||0,105||0,116||0,131|
|The utilization of the acid to the target product, %||98,4||97,2||98,1||98,5||97,6||98,5|
The reactor, the nature of the metal, oxide and solvent, the mass of the load, its relationship with the mass of glass beads, the iodine content in the initial download, the boot order of the components of the reaction mixture and the process, the choice of the time of termination, the sequence of operations for separation of the reaction mixture from beads, selection of product, cleaning and returning the separated liquid phase in the re process similar to that described in PR the least 1. Differ in the use of malonic acid, the value of x in a molar ratio of the reactants and the relative mass of the reactants in the initial download. The results obtained are summarized in table 3.
|Load characteristics, process and output of product||Example No.|
|The value of x in a molar ratio of reagents||0,9||1,0||1,1||1,0||1,0||1,0|
|Download manganese dioxide mol||0,0303||0,0456||0,0476||0,0384||0,0411||0,0491|
|The relative mass of the reactants in the download, %||15,00||23,24||25,00||19,57||20,93||25,00|
|Operating temperature range, °C||22-36||22-35||22-32||24-40||24-39||24-34|
|The process duration, min||80||84||114||58||71||118|
|The yield of the product (excluding losses when cleaning), mol||0,086||0,134||0,145||0,112||0,121||0,144|
|The utilization of the acid to the target product, %||of 97.8||98,1||98,4||97,4||98,1||98,0|
The positive effect of the proposed solutions.
1. The proposed method uses the reagents, the main part of the mass which goes to the weight of the target product. Co-products are water and hydrogen, the formation of which takes only naznacite the other part of the initial mass of the reactants. Moreover, data related products do not require recycling and not polluting the target product.
2. In the proposed solution, there is no wastewater used the liquid phase returns to repeat the process and so can be repeated many times.
3. In the proposed process, there is no need to use heat. On the contrary, the reaction heat has to dissipate. In General, low-power process.
4. This process does not require any sophisticated equipment, especially boiler-supervising.
5. This process allows the use of a fairly wide range of solvents.
1. The method of producing malonate or succinate manganese (II) by direct interaction of the metal and its oxide with a carboxylic acid in the presence of an organic solvent and stimulating supplements of iodine in the bead mill, vertical type with a high speed stirrer and glass beads as pereirago means, characterized in that the manganese, dioxide and dicarboxylic acid in the initial download take in a molar ratio
(1+x):1:(2+x) to produce (2+x)m moles of salt, where x in the molar ratio of the loaded reagents take 0,4±0,1 for succinic acid and 1.0±0.1 malonic acid, a m - the number of moles of manganese dioxide in the download; iodine dosed in amounts of 0.05 mol/kg of the reaction mixtures and after loading of organic solvent and acid, but before downloading manganese dioxide and metal, while the sum of the masses acid, metal and dioxide charge in the range of 15-25% by weight of the bootstrap, and the mass ratio of the beads and loading 1:1, the process begins at room temperature and are in conditions of forced cooling in the temperature range from room temperature up to 40°C, With the control method of sampling to almost quantitative spending all loaded reagents in the target salt, after which it ceased, the suspension of the final reaction mixture is separated from the beads and filtered, the precipitated product is washed with a solvent liquid phase and sent for purification from traces of metal and its oxide 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 organic solvent liquid phase take n-propyl, n-butyl and ISO-butyl alcohol, butyl acetate, xylene, white spirit and heptane.
FIELD: organic synthesis.
SUBSTANCE: invention concerns an improved method for synthesis of manganese(II) succinate tetrahydrate wherein manganese(II) carbonate is portionwise added to succinic acid aqueous solution at molar ratio 1:1:4.5, respectively, under continuous stirring and, while maintaining constant temperature 60-65°C, each subsequent portion being added after complete dissolution of preceding manganese carbonate portion, after which desired product is isolated via recrystallization. Method can be used under industrial-scale conditions.
EFFECT: improved purity of product and minimum reactants used.
3 dwg, 2 tbl, 5 ex
FIELD: organic chemistry, chemical technology.
SUBSTANCE: invention relates to improved method (variants) for conversion of maleic acid to 1,4-butanediol, gamma-butyrolactone and/or tetrahydrofuran. Method for synthesis for at least one of product chosen from a group comprising gamma-butyrolactone, 1,4-butanediol and tetrahydrofuran involves the following steps: creature of the first hydrogenation zone and the second hydrogenation zone that are bound successively; feeding to the first zone of a raw flow that comprises maleic acid; caring out reaction in the first hydrogenation zone of the parent maleic acid and hydrogen in contact with a catalyst to yield the reaction product comprising succinic acid; feeding to the second zone the hydrogenation product from the first hydrogenation zone; carrying out the hydrogenation reaction of the reaction product obtained in the first hydrogenation zone in the second hydrogenation zone in contact with a catalyst for preparing a product that comprises at least one product from a group comprising gamma-butyrolactone, 1,4-butanediol and tetrahydrofuran. Method involves control over temperature in first hydrogenation zone by manner that maleic acid temperature in the raw flow and temperature in the first hydrogenation zone doesn't exceed 120°C, and the reaction heat liberated in the first hydrogenation zone is used in enhancing the reaction product reaction above 130°C before feeding the reaction product from the first hydrogenation zone to the second hydrogenation zone resulting to minimal corrosion effect of maleic acid and enhancing time for working life of reactor and improving the complete effectiveness of the process.
EFFECT: improved method of synthesis.
13 cl, 1 ex
FIELD: production of calcium succinate useful in pharmacology, veterinary, medicine as drug or bioactive additive.
SUBSTANCE: calcium succinate in obtained by reaction of calcium chloride solution with reactive mixture of succinic acid and sodium hydroxide in molar ratio of 1:2, respectively at 20-30°C. Calcium chloride solution is added for 2 hours followed by mixture conditioning for 3 hours for crystallization finishing. Precipitate is separated, washed on filter and dried at 100°C for 12 hours. Target product is obtained in form of monohydrate.
EFFECT: accelerated method with reduced energy consumption.
FIELD: new 2,4,6-trimethyl-3-oxypyridine nitrosuccinate and method for production thereof.
SUBSTANCE: claimed compound is useful in medicine as future antiishemic agent with vasodilatation effect and has potent protective action in barotraumatic damages and ballistic wounds due to inhibition of secondary necrosis creation and progress. Compound of present invention is obtained by nitration of malic acid with mixture of sulfuric and nitric acids, separation of nitrohydroxymalic acid and treatment thereof with 2,4,6-trimethyl-3-oxypyridine in alcohol media with subsequent isolation of target product.
EFFECT: new antiishemic agent.
2 cl, 1 ex
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.
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
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
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.
EFFECT: method makes it possible to produce target product in absence of manganese dioxide and stimulating additive at temperatures close to room temperature.
2 cl, 13 ex, 2 tbl
SUBSTANCE: invention relates to improved method of salicylates of alkaline earth metals for application as detergents for lubricating materials. Method of obtaining alkylated salicytates of alkaline earth metals includes following stages: A) alkylating salicylic acid with linear α-olefin, containing, at last, 14 carbon atoms, in presence of water-free methane sulfonic acid with formation of oil-soluble alkylated salicylic acid; B) neutralisation of oil-soluble alkylated salicylic acid; C) excessive alkalisation of oil-soluble alkylated salicylic acid by carboxylating lime by means of CO2 in presence of oxygen-containing organic solvent and surface-active substance; D) filtration of stage (C) product; and E) removal of solvent by distillation. Alternatively, alkylsalicylic acid can be subjected to interaction with preliminary processed with alkali highly-alkaline sulfonate of earth alkaline metal, for instance, with calcium sulfonate, in order to obtain salicylate salts of earth alkaline metals with different per cent content of dispersed salts of alkaline earth metals carbonates. In claimed method it is not necessary to filter end product which is preferable doe industry.
EFFECT: obtaining salicylates of alkaline earth metals for application as detergents for lubricating materials.
8 cl, 4 ex
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
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
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
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
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: organic chemistry, chemical technology, agriculture.
SUBSTANCE: 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.
EFFECT: improved preparing method.
6 cl, 1 tbl, 6 ex