Method of production of the formiate of manganese (ii)

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.

EFFECT: the invention ensures simplification of the method at usage of accessible reactants.

16 ex, 2 tbl

 

The invention relates to a technology for manganese salt of formic acid, which can be used as a reagent and catalysts of series of chemical reactions in the laboratory and in industrial practice, as well as in the analytical control.

A method of obtaining manganese formate by reacting a 50%aqueous solution of formic acid and manganese carbonate at 20°With subsequent crystallization of the product from solution (V.Sapletal, V.Ruzicka, Coll, Chesh. Thermal decomposition of some metalforlife. "Chenn. Conun", 22, No. 1, 1957, s).

The disadvantage of this method is the use as feedstock carbonate of manganese, which is previously obtained by precipitation from a solution of sulphate of manganese.

Closest to the claimed is a method of producing manganese formate by reacting contained in manganese ore manganese dioxide containing formic acid solution, which is used as water condensate production of synthetic fatty acids (A.S. USSR №1060612, application No. 3391216/23-04, publ. B 1983, No. 46).

The disadvantages of this method are:

1. As manganese compounds used manganese ore, containing in its composition in addition to the compounds of manganese (16.6%) of the masses.) compounds of other metals, namely iron (20.0% of the ACC.), copper (0,09% mass.) etc. that may engage in similar interactions with formic acid, forming a complex hardly separated mixture of formate.

2. Used as an acid reagent mixture of fatty acids, including, in addition to formic acid (10-12% of the mass.) as the main component, more acetic acid (5-7 wt. -%), propionic (3-5% wt.) and oil (1-3% wt.), capable of reacting with components of the ore and to supply simultaneously with formate other salts of manganese and carboxylic acids, which significantly complicates the separation of the reaction mixture and purification of formate. This method is not determined either by comparison of the competing ability of fatty acids in interaction with components of the ore, no information about the solubility or the specification of the operations branch of clay and sand components and other solids from the liquid phase or degree of decomposition of the iron ore components.

3. Manganese dioxide - known quite a strong oxidizer. If there is a formate, manganese (II), we need an appropriate reducing agent Mn4+→Mn2+in part the process is not defined. The reducing agent may be formic acid. But in this case it will not be put in the proper degree anion salt. Suppliers may be other acid.

4. The described method is not defined in Pratunam design, and in the process conditions between the solid and liquid reagents.

5. The process at 95°C for 5 hours very long. At this temperature, the volatility of formic, and acetic acid is high, and in order to avoid their losses requires the use of working effectively reverse condenser, as well as traps and other measures to ensure comfortable conditions for staff.

6. Noted a small range of variation of mass ratio of downloads of solid and liquid phases (1:(9÷10)). Carrying out the process at lower temperature and smaller proportion of solid and liquid phases does not provide a good yield of the target product. While it is not clear how this will affect the output of by-products and the necessary cleanup formate from them.

7. Target product isolated from the reaction mixture, most likely using a pre-concentration of the liquid phase, which is energy intensive and time consuming operation. Yes, and the process is very energy-intensive.

The objective of the proposed solutions is to get formate, manganese (II) manganese metal and its oxide in the interaction with formic acid in solutions of organic substances at room temperature.

This object is achieved in that the process between the solid is liquid phases are in a bead mill, vertical type, in the absence of the supply of external heat, the liquid phase is metered mass ratio of glass beads of 1:(1÷2) and solid reagents (4,9÷11):1, as it take a solution of formic acid in an organic solvent with a concentration of acid 3,5÷to 10.8 mol/kg and download the first or directly prepared from the components in the bead mill, and then it dissolved stimulating Supplement iodine in the amount of 0.025-0,100 mol/kg liquid phase, followed by the loading of the metal and its oxide in a molar ratio of 1.8-2,2):1, and the process begins and is carried out at room temperature until almost fully exhausted just downloaded oxide, after which the resulting suspension of 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. The manganese oxide is used MnO2, Mn2About3and Mn3O4. And as the organic solvent liquid phase - ethyl acetate, ethylene glycol, ethyl cellosolve, 1,4-dioxane, dimethylformamide, butyl alcohol.

Characteristics of the raw materials used.

Manganese reactive GOST 6008-90.

Manganese dioxide according to GOST 4470-79.

The oxide of manganese Mn2About3on THE other 6-09-3364-78.

The oxide m is Lanza Mn 3O4obtained by burning manganese dioxide in a muffle furnace at a temperature of 1100±15°With limited access of air.

Iodine crystal according to GOST 4159-79.

Formic acid 85% according to GOST 5848-73.

The ethyl acetate according to GOST 8313-88.

Ethylene glycol according to GOST 10164-75.

The ethyl cellosolve according to GOST 8313-88

n-butyl alcohol according to GOST 6006-78.

1,4-Dioxane according to GOST 10455-80.

Dimethylformamide under MRTU 6-09-2068-65.

The process of the inventive method the following. In ball mill vertical type with glass enclosure, a high-speed stirrer is made of Teflon or other inert and durable plastic material and equipped with a reflux-condenser, enter glass beads in a mass ratio of liquid phase (1÷2)-1, pre-cooked liquid phase or its components separately, as well as stimulating additive molecular iodine. Include mechanical mixing and dissolving stimulating additive in a solution of formic acid in an organic solvent. Then enter the metal and its oxide without interrupting mechanical mixing and the time taken for the beginning of the process. During the process without stopping stirring take samples of the reaction mixture, which determine the salt content and the residual amounts of formic acid and oxide of manganese. As soon as the main weight of the oxide of manganese is consumed, stirring is stopped, the reaction mixture is separated from the glass beads and the main mass of the heavy plates and particles of manganese, after which it sent for filtering. The filtrate, representing a saturated solution of manganese formate in a mixture of solvent and formic acid, and analyze together with unreacted metal and oxide residues returned to repeat the process. Sol sent for purification from admixtures during hot filtration and recrystallization.

Example No. 1.

In a ball mill with glass casing inner diameter of 55 mm and a height of 95 mm with Teflon paddle stirrer, spaced from the bottom of the reactor at 0.3 mm, and a reflux-condenser load of 50 g of glass beads with a diameter of 1.2÷1.8 mm and 50 g of formic acid in n-butyl alcohol with a concentration of 8.7 mol/kg. Then injected 0,635 g of iodine include mechanical stirring (1440 rpm) and for 10 min to prepare a solution of iodine in the liquid phase. Stopping stirring, enter 3,3 g of manganese metal, 2,61 g of manganese dioxide and the time taken for the beginning of the process. During the process, take samples of the reaction mixture and the results of the analysis determine the degree of conversion of the manganese dioxide and the amount of salts in the reaction mixture. After 120 minutes, it was over 99%and the salt content reached 1,11 the ol/kg The stop stirring and separating the reaction mass from the beads by passing it through a filter wall in a grid ˜0,2×0,2 mm This operation is performed so that the main mass of the heavy particles of manganese remained at the bottom bead mill and beads. The separated manganese return in the re process, and the suspension of salt FilterOutputStream return in the re process, and the resulting salt is recrystallized from an aqueous solution of formic acid, saturated with manganese formate.

Examples No. 2-8.

Source reagents, the solvent of the liquid phase, the amount of the liquid phase; loading and sequence of operations of the process, monitor its progress, upload the final reaction mixture, separation of the solid product and return the individual components in the re process similar to that described in example 1. Different concentrations of formic acid in the liquid phase, the method of preparation of the latter, the ratios of the masses of the liquid and solid phases and the liquid phase and beads, the molar ratio of the metal and its oxide in the download content stimulating supplements of iodine in the liquid phase. The results are shown in table. 1. Legend: ZB - in advance; NC - directly into the reactor under stirring estimated quantities of formic acid and solvent.

Table1

Characteristics of the processExample No.
2345678
The concentration of formic acid in the liquid phase, mol/kg3,54,85,26,97,49,310,8
The preparation method of the liquid phase3b3bNCNC3bNC3b
The mass ratio of the liquid and solid phases7:17,5:18:19:110,4:111:111:1
The mass ratio of the liquid phase and bead1:11:11:1,51:1,51:1,71:21:2
The molar ratio of manganese and manganese dioxidea 2.2:1a 2.2:12,05:1a 2.0:11,9:1a 1.8:1a 1.8:1
The iodine content in the liquid phase of the initial reaction mixture, mol/kg liquid phase0,1000,0750,070to 0.0600,040 0,0330,025
The duration of the dissolution of iodine in the liquid phase, min101010105113,5
The duration of the process until the termination, min170175167151138141133
The achieved degree of conversion of the manganese dioxide in the time of the termination process, %>98>98>98>98>98>98>98
The content of manganese formate in the final reaction mixture (suspension (results of analysis), mol/kg1,281,171,171,070,930,930,95

Examples No. 9-16.

The reaction apparatus, the mass ratio of the loaded liquid phase and beads, the concentration of formic acid in the liquid phase, the mass of the liquid phase and metal, the molar ratio of downloads of metal and oxide, the preparation method of the liquid phase, the sequence of operations when loading, process and product selection, as well as stimulating additive similar to that described in example 1. Different nature of the oxide and solvent, liquid phase with the system, and the mass ratio of the liquid and solid phases in the boot. The results obtained are given in table. 2. Designations: EA - ethyl acetate, EG - ethylene glycol, EC - ethyl cellosolve, 1,4D - 1,4-dioxane

The positive effect of the proposed solution consists of:

1. The method is quite simple to perform, does not require external supply of heat and orientate on readily available raw materials.

2. Simplified the composition of the reaction mixture through the use of individual compounds. Approximately half of the accumulated salt raw material is manganese oxide, which is a natural connection.

3. Instrumentation process is simple and does not contain boiler-supervising equipment. This process can be successfully held in the low variant. It is not formed and does not accumulate any unwanted inhibitors that allows for the subsequent series in the apparatus filled with dead zones and not to lose the reaction mixture for this reason. There are no restrictions on the return of the spent liquid phase and unreacted metal and dioxide in the re process.

4. Pretty simple cleaning salt from solid impurities and recrystallization reduce losses at this stage to a minimum.

1. The method of producing formate, manganese (II) by direct interaction of the sid manganese with formic acid, characterized in that the process between the solid and liquid phases are in a bead mill, vertical type, in the absence of an external supply of heat, the liquid phase is metered mass ratio of glass beads of 1:(1÷2) and solid reagents (4,9÷11):1, as it take a solution of formic acid in an organic solvent with a concentration of acid 3,5÷to 10.8 mol/kg and download the first or directly prepared from the components in the bead mill, and then it dissolved stimulating Supplement iodine in the amount of 0.025-0,100 mol/kg liquid phase, followed by the loading of the metal and its oxide in a molar ratio of 1.8÷2,2):1, and the process begins and is carried out at room temperature until almost complete spending just downloaded oxide, after which the resulting suspension of 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.

2. The method according to claim 1, characterized in that as the oxide of manganese is used MnO2, Mn2O3and Mn3About4.

3. The method according to claim 1, characterized in that the organic solvent liquid phase using ethyl acetate, ethylene glycol, etincelle is ALW, 1,4-dioxane, dimethylformamide, butyl alcohol.



 

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3 ex, 1 tbl

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6 cl, 1 dwg, 1 tbl

FIELD: inorganic synthesis.

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1 tbl, 8 ex

FIELD: inorganic synthesis.

SUBSTANCE: invention relates to preparation of salts of transition metals with organic acids, in particular to formic acid ferric salt. Method is accomplished in bead mill provided with mechanical blade-type stirrer in aqueous formic acid solution (5-10 mole/kg). Iron is used in the form of steel sidewall across the height of reactor and also as particles of reduced iron stirred with stirrer together with glass beads, and/or as broken steel cuttings, and/or yet as split cast iron in any weight proportions. Method is accomplished by continuously introducing 10-20% hydrogen peroxide solution at a rate of 0.015-0,030 mole peroxide/min per 1 kg liquid phase (salt slurry) in presence of stimulating additive, in particular iodine, bromine, alkali metal or ferrous iodides or bromides in amounts (on conversion to halogens) 0.1-0.15 vole per 1 kg reaction mixture. When 1,2-1,5 mole/kg of ferrous salt is accumulated in reaction mixture, stirring and addition of hydrogen peroxide solution are stopped, product slurry is separated from unreacted iron and/or its alloys as well as from glass beads and filtered. Filtrate is recycled into process and precipitate is recrystallized from saturated iron formate solution of aqueous formic acid solution (1-2 mole/kg).

EFFECT: simplified finished product isolation stage, reduced total process time, and reduced power consumption.

1 tbl, 11 ex

FIELD: chemical industry; methods of production of the salts of iron and the organic acids.

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the method of production of the salts of iron and the organic acids, in particular, to production of the salt of the ferrous iron and the formic acid. The method is realized by the direct interaction of the acid with the iron, its alloys and the ferric oxides. The crumber with the beads and the backflow condenser is loaded with the organic solvent, the formic acid and the water in the mass ratio of 100:(85÷100): (15÷0). As the organic solvent they use ethylcellosolve, butyl acetate, butyl and amyl alcohols, ethylene glycol. The mass ratio of the beads and the liquid phase is 1:1. Ferric oxideFe2O3 orFe3O4 and the iodine are loaded in the amount of 0.40-0.56 or 0/21-0.42 and 0.03-0.1 mole/kg of the liquid phase accordingly. The iron is introduced in the form of the steel shell along the whole height of the reactor and additionally in form of the reduced iron, the fractions of the broken cast iron with dimensions of up to 5 mm and the steel chips in any ratio among themselves at total amount of 20 % from the mass of the liquid phase. The process is conducted at the temperature of 35-55°С practically till the complete consumption of the ferric oxide. The gained suspension is separated from the beads and the metal particles of the greater dimensions and subjected to centrifuging or sedimentation. The clarified liquid phase is returned to the repeated process, and the solid phase is dissolved at stirring action and warming up to 85-95°С in the water solution of the formic acid saturated by the ferric formiate (II) up to 1-2 mole/kg. The present solid impurities are removed at the hot filtration process and the filtrate is cooled and the salt crystals are separated. The technical result of the invention is simplification of the technology of the production process with utilization of the accessible raw.

EFFECT: the invention ensures simplification of the technology of the production process with utilization of the accessible raw.

3 cl, 17 ex

FIELD: chemical industry; methods of production of the salts of iron and the organic acids.

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the method of production of the salts of the metals of the organic acids, in particular, to production of the salt of the ferrous iron and the formic acid. The method is realized by the direct interaction of the formic acid water solution with the iron and/or its alloys and the ferric oxidesFe2O3 and Fe3O4 in the bead crumber of the vertical type along the whole its height with the steel shell, with the heat supply and equipped with the mechanical stirrer and the backflow condenser-refrigerator. The apparatus is loaded with 23-46 % water solution of the formic acid as the liquid phase in the mass ratio with the glass beads as 1:1.25 and then introduce the oxide - Fe3O4 orFe2O3 in amount of 0.27-0.49 or 0.48-0.64 mole/kg of the liquid phase accordingly, and besides in amount of 18 % from the mass of the liquid phase they add the powder of the reduced iron and-or the crushed cast iron, and-or the crushed steel chips in any mass ratios. Switch on the mechanical stirring and heating and keep the temperature in the reaction zone within the limits of 55-75°С. The process is terminated, when practically the whole loaded oxide is completely consumed. The suspension of the salt is separated from the non-reacted iron, its alloy and the beads and dilute with the water up to the contents of the formic acid within the limits of 1-2 mole/kg. The gained mass at stirring action is slowly heated up to temperature of 85-95°С, controlling transformation of the solid phase into the solution. The gained solution is subjected to the hot filtration, evaporation, cooling and separation of the salt crystals. The filtrate and the earlier the gained distillate are sent back to the repeated process. The technical result of the invention is simplification of the technology of the production process with utilization of the accessible raw.

EFFECT: the invention ensures simplification of the technology of the production process with utilization of the accessible raw.

10 ex

FIELD: production of salts of organic acids, salt of ferrous iron and formic acid in particular.

SUBSTANCE: proposed method consists in loading preliminarily prepared aqueous solution of formic acid at concentration of 4.5-10 mole/kg into reactor provided with bladed mixer, back-flow condenser-cooler and air bubbler. Then, powder of reduced iron and/or broken iron and/or steel chips at any mass ratio in total amount of 20.0-30.6% of mass of liquid phase and stimulating iodine additive in the amount of 0.016-0.164 mole/kg of liquid phase are introduced. Reactor may be provided with steel or cast iron ferrule over entire height. At mechanical mixing, consumption of air for bubbling is maintained between 1.2 and 2.0 l/(min·kg of liquid phase). Working temperature range is 45-65°C which is maintained by external cooling. Process is discontinued when content of iron salts (II) in reaction mixture reaches 1.8-2.0 mole/kg. Suspension of salt in liquid phase is separated from unreacted iron particles and is filtered afterwards. Filtrate is directed for repeated process and salt sediment is re-crystallized from aqueous solution saturated with iron formate by formic acid at concentration of 1-2 mole/kg at heating to temperature of 95°C followed by natural cooling.

EFFECT: enhanced efficiency.

1 tbl, 9 ex

FIELD: chemical industry; methods of production of the ferric formiate (III).

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the method of production of the ferric formiate (III). The invention is dealt with the organic salts of the transition metals, in particular to production of the salt of the ferric iron and the formic acid. The method is realized by the direct interaction of the regenerated iron powder with the formic acid at presence of the molecular iodine and oxygen of the air as the oxidizing agents. The process is running in the medium of dimethylformamide as the dissolvent for preparation of the necessary liquid phase with the concentrations of the formic acid and iodine of 4.5-10 and 0.03-0.11 mole/kg accordingly. The mass ratio of the liquid phase and the powder of the regenerated iron is 3:1. The process starts at the room temperature and is conducted in the conditions of the forced cooling at the temperature of 50-80°С at the rate of the air consumption for the bubbling of 0.6-1.2 l\minute per 1 kg of the liquid phase. The process is terminated at accumulation of the ferric formiate (III) in the suspension up to 1-1.2 mole/kg. The suspension is separated from the particles of the non-reacted iron and then filtered. The filtrate is recycled to the repeated process, and the ferric formiate (III) (salt) is dried and either is used as required, or additionally is purified by the recrystallization. The technical result of the invention is simplification of the method with improvement of the economic indicators and the increased purity of the final product.

EFFECT: the invention ensures simplification of the method with improvement of the economic indicators and the increased purity of the final product.

8 ex

FIELD: anti-conglomeration agents.

SUBSTANCE: invention relates to loose product based on potassium formate, which contains 0.1 to 1% water and 0.5-5% water-soluble conglomeration-preventing agent, such as potassium carbonate or potassium hydroxide, which possesses affinity for water and corresponds to equilibrium humidity below equilibrium 15% relative humidity (22°C) for potassium formate.

EFFECT: provided modifying and conglomeration preventing agents for potassium formate to allow it to achieve looseness under practical storage and processing conditions.

3 cl, 4 tbl, 4 ex

The invention relates to an improved method of separation of polyols, such as neopentyl glycol or atrial, and sodium formate or calcium, comprising adding to the mixture of the partial organic solvent, in which the polyhydric alcohol is dissolved, the crystallization of sodium formate or calcium, Department of formate sodium or calcium from the solution of a polyhydric alcohol in an organic solvent, for example, by filtration, recycling of organic solvent, cooling the solution and crystallization of a polyhydric alcohol, and as the organic solvent used solvent aromatic series such as toluene, after adding to the mixture of the partial substances organic solvent, the resulting mixture is heated to boiling point and produce at this temperature simultaneously: dehydration of the mixture by distillation with water recirculation separated from water, organic solvent, crystallization dissolved in an organic solvent, sodium formate or calcium and dissolution in an organic solvent, a polyhydric alcohol

The invention relates to a method for the simultaneous receipt of pentaerythritol and sodium formate used in the chemical, leather and paint and other industries

FIELD: anti-conglomeration agents.

SUBSTANCE: invention relates to loose product based on potassium formate, which contains 0.1 to 1% water and 0.5-5% water-soluble conglomeration-preventing agent, such as potassium carbonate or potassium hydroxide, which possesses affinity for water and corresponds to equilibrium humidity below equilibrium 15% relative humidity (22°C) for potassium formate.

EFFECT: provided modifying and conglomeration preventing agents for potassium formate to allow it to achieve looseness under practical storage and processing conditions.

3 cl, 4 tbl, 4 ex

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