Method of preparing iron(ii) formate in presence of hydrogen peroxide as oxidant

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

 

The invention relates to the technology of production, isolation and purification of formate, iron (II) in aqueous media and can be used in various fields of laboratory and industrial chemistry, studies in other areas and held them in analytical control.

A known method of producing formate, iron (II) by the interaction of sulphate of iron (II) with sodium formate in aqueous solution in an inert environment (US patent No. 2688032, publ. 1952, serial No. 311733). The product is poorly soluble in water and resistant to oxidation in air.

The disadvantage of this method is that its implementation should have iron sulfate (II) and sodium formate, which are natural compounds are not, and in the chain of transformations during its getting to be located further than iron and formic acid, respectively.

Closest to the claimed is a method of obtaining basic formate or acetate India (A.S. USSR №454198), according to which the metal is subjected to interaction with acid in the presence of hydrogen peroxide at periodic heated to 80-100°followed by separation of the product by evaporation of a solution containing Sol-product, water and excess acid.

The disadvantages of this method are:

1. The periodic heating of the reaction mixture up to 80 to 100°With that depict is to place some difficulties in performance (periodic heat input is always more complex than continuous) and requires heightened security staff (metal - hydrogen peroxide at elevated temperatures does not refer to a known secure systems).

2. Salts of iron (III) are known to be highly efficient catalysts for the decomposition of hydrogen peroxide in several directions. In this respect, it is not clear whether such an oxidizing agent to use in a similar process with iron as a metal.

3. Target product have to allocate from the reaction mixture by evaporation, which is high-energy and long-term operation.

The objective of the proposed solutions is to get formate, iron (II) sharing of iodine or bromine (as oxidant iron) and hydrogen peroxide (oxidant iodide (bromide) iron (II), i.e. the stage, accompanied by replacement of the anion salt) in the absence of an external supply of heat at the natural folding due to gross ekzotermicheskie process temperature, as well as to simplify the extraction of the target product and significantly reduce its energy intensity and duration.

This object is achieved in that the oxidation of iron powder and(or) crushed(th) steel (cast iron) are in the absence of the supply of external heat in an aqueous solution of formic acid with a concentration of 5-10 mol/kg in the presence of in terms of halogen 0.1 to 0.15 mol/kg iodine (bromine) containing stimulating additives in intensive fur is practical stirring in a bead mill and a continuous injection of 10-20%aqueous hydrogen peroxide solution with a speed of 0.015-0,030 mole peroxide / kg liquid phase (slurry salt) in min) prior to the accumulation in suspension 1.2 to 1.5 mol/kg formate iron (II), after which the supply of hydrogen peroxide stop, stop mechanical stirring, a suspension of the reaction mixture is separated from the beads and unreacted metal (alloy), then filtered, the filtrate is returned to repeat the process, and the residue is recrystallized from 1-2 mol/kg of an aqueous solution of formic acid previously saturated formate, iron (II) at room temperature. At the same time as stimulating additives used iodine, bromide, iodides or bromides of alkali metals and iron (II).

Characteristics of the raw materials used

Iron recovered in THE 6-09-2227-81

Steel 3 on CMTU 1-84-67

Steel 45 GOST 1050-74

The grey cast iron grey 15-32 according to GOST 1412-70

Formic acid according to GOST 5848-73

Iodine crystal according to GOST 4159-79

Bromine according to GOST 4109-79

Iodide of sodium GOST 8422-66

Bromide of potassium according to GOST 4160-65

Hydrogen peroxide according to GOST 10929-76

Distilled water on THE 6709-72

Iodide (bromide) iron (II) received a direct interaction of iron with iodine (bromine) in a solution of iodide (bromide) iron (II) salt concentration of 0.68 or more mol/kg in terms of forced cooling with fractional input oxidant and reductant in moments of almost total expenditure entered in previous times oxidant to accumulation ˜2 mol/kg FeI2and ˜1,6 the ol/kg FeBr 2.

The process of the inventive method the following. In a ball mill with steel case and steel shell over the entire height, as well as with high-speed paddle stirrer made of steel, the lower profile which follows the profile of the bottom of the reactor, and selected experimentally optimal number of beads load calculated quantity of an aqueous solution of formic acid, powder recovered iron and(or) broken into pieces with a maximum linear dimension of 5 mm steel shavings and(or) broken cast iron, as well as stimulating supplements. The reactor is placed on designed for it in the mounted on the frame installation with automatic feeding of hydrogen peroxide with an adjustable flow rate. Include mechanical mixing and the flow of hydrogen peroxide and the time taken for the beginning of the process. The temperature at the initial time is the environment. In the process she begins to grow, which is a consequence of the presence of exothermic stages in this gross-out process. At the quite early stages appears solid formate, iron (II), which turns the reaction mixture in a suspension of the product.

By weight of the total quantity of the injected hydrogen peroxide is a significant part of the mass of initial liquid reaction mixtures is I. This factor has to be considered when selecting the source download: the volume of the reactor should ensure the addition of the specified amount of oxidant and at the end of the process not to be overloaded.

During the process, take samples of the reaction mixture, which analyze the content of divalent or trivalent iron. As soon as the content of the formate, iron (II) is 1.2-1.5 mol/kg, stop the supply of hydrogen peroxide and off mechanical stirrer. Give a little time to settle to the bottom of the heavy particles of unreacted iron or its alloy. Then the suspension of the salt product is drained through the drain pipe with a metal grid with cells of 0.5×0.5 mm and subjected to filtration. Solid product with impurities of carbon from the alloy remains on the filter, and the filtrate, containing unreacted formic acid, dissolved salts of iron (II) and iron (III) and the main part of the stimulating supplements are sent to re-download process. The precipitated product is subjected to recrystallization from 1-2 mol/kg of an aqueous solution of formic acid previously saturated formate, iron (II) at room temperature.

Example 1

In ball mill vertical type with stainless steel inner diameter of 79 mm and a height of 145 mm with steel shell over the entire height, equipped with vysokooborotnye the th (1440 rpm) paddle stirrer with thick blades not less than 5 mm, external reflux-condenser, a loading opening, a system for continuous dosing of hydrogen peroxide with adjustable mass velocity, a sampler and a drain pipe at the bottom with grid with cells of 0.5×0.5 mm, allowing to separate the glass beads and large particles of unreacted metal and / or alloy from a fairly easy fluid suspension of the product as well as glass beads in the amount of 250 g of unreacted metal and / or alloy and a portion of the reaction mixture prior experience in the dead zone of the reaction apparatus, introduced 200 g of aqueous formic acid at a concentration of 5 mol/kg, 25 g of recovered iron, 5,11 g of crystalline iodine, and broken into pieces of steel shavings steel (45) number to the total number of floating stirrer metal (unreacted from past experience and added load was 90, the Reactor is put into place in mounted on a single frame setup, make the necessary connections include mechanical mixing and serving 20%solution of hydrogen peroxide with an initial mass rate of 1 g/min the time taken for the beginning of the experiment. The temperature at the beginning was 19°C. during the process, take samples of the reaction mixture, which define separate salt glands is (II) and iron (III). At the same time adjusting the feed rate of the hydrogen peroxide solution so that the mass rate of the oxidant in the reaction zone is not depended on the degree of dilution of the reaction mixture introduced him water, i.e. would have been about equal.

Through 94 minutes of the process in this mode the content of iron salts in the suspension reached 1.5 mol/kg, and the temperature rose to 47°C. Off mechanical stirring and stop the flow of hydrogen peroxide solution into the reaction zone. Give 3 minutes for sedimentation of heavy particles of iron and its alloys in the area below the drain pipe with mesh to separate the beads and through the last merge 343 g of a suspension of formate, iron (II) directly on the filter, vacuum filter node. After filtering the precipitate from the filter are sent to recrystallization from a solution with a content of formic acid is 1.8 mol/kg and formate, iron (II) in the saturation point at room temperature. And the separated filtrate is directed to the re-download process. Taking into account losses during recrystallization and partial conversion of salt in the crystalline output formate, iron (II) ˜75,

Examples 2-11

Laboratory setup the reactor, the sequence of loading operations, the process, the isolation and purification of the product are similar to those described in note the re 1. Different concentrations of formic acid in the original solution, the mass ratio of the metal and its alloys in the download, nature and number of stimulating additives, the concentration of the injected hydrogen peroxide solution and the mass throughput of the oxidizer, as well as the content of the formate, iron (II) in the final reaction mixture. The results obtained are summarized in table.

The positive effect is the following:

1. The process does not require heat and can proceed at room temperature or slightly increase due to the reaction heat, which indicates low intensity.

2. In the reaction zone during the process there is no significant concentrations of hydrogen peroxide and permorming acid, which provides additional security for such a process.

3. The bulk product is accumulated in the solid phase, which is easily separated by simple filtration.

4. The product can be quite good and easily cleaned by available and well-tested recrystallization. In this case, for the latter does not require any substances that are not used in the main process.

5. Obtained by recrystallization saturated formate solutions formic acid with some stimulating content iodine - or bromine is aderrasi additives can be used in the main process.

6. Stimulating Supplement is actually used repeatedly in several ongoing processes including and without intermediate fertilization.

7. In the process not accumulate any chemical inhibitors and undesirable for reasons other substances. Therefore, the reactor washed before each experience is not necessary that favors the reduction of losses due to dead zones and other articles.

1. The method of producing formate, iron (II) in the presence of hydrogen peroxide as oxidant by direct interaction of the metal with the acid in an aqueous medium, characterized in that the oxidation of iron powder and (or) crushed(th) steel (cast iron) are in the absence of the supply of external heat in an aqueous solution of formic acid with a concentration of 5-10 mol/kg in the presence of in terms of halogen 0.1 to 0.15 mol/kg iodine(bromine)containing stimulating additives under intensive mechanical stirring in a bead mill and a continuous injection of 10-20%aqueous hydrogen peroxide solution with a speed of 0.015-0,030 mole peroxide/kg liquid phase (slurry salt) in min) prior to the accumulation in suspension of 1.2 to 1.5 mol/kg formate, iron (II), after which the supply of hydrogen peroxide stop, stop mechanical stirring, a suspension of the reaction mixture is separated from the beads and unreacted metal (alloy), the ATEM filter, the filtrate is returned to repeat the process, and the residue is recrystallized from 1-2 mol/kg of an aqueous solution of formic acid previously saturated formate, iron (II) at room temperature.

2. The method according to claim 1, characterized in that as stimulating additives used iodine, bromide, iodides or bromides of alkali metals and iron (II).



 

Same patents:

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: inorganic chemistry, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing metal complex compounds, in particular, to iron complex (chelate) as its concentrated solution. Method is carried out by interaction of iron salt in an aqueous medium with a chelate-forming agent wherein N,N,N',N'-ethylenediaminetetraacetic acid is used as a chelating agent and citric acid that are added simultaneously or successively. The process is carried out at temperature 70-90°C and in the process of mixing iron salt or after mixing with chelate-forming agent an aqueous solution of ammonia or ammonium citrate is added for providing pH value of the end product 2.0-2.3. The complex-forming agent can comprise succinic acid additionally. Method provides preparing iron chelate as a concentrated solution with the content of iron 60-100 g/l. Invention can be used in agriculture for root and leaf feeding of plants.

EFFECT: improved preparing method.

4 cl, 6 ex

FIELD: inorganic syntheses.

SUBSTANCE: method consists in that iron powder is oxidized in acetic acid/acetic anhydride (4%) medium with air oxygen bubbled through the medium, while maintaining iron-to-acetic acid molar ratio 5:1 and temperature 17-25°C. Reaction mixture is thoroughly stirred with blade stirrer at speed of rotation 720-1440 rpm until reaction mixture accumulates 0.75-0.96 mol/kg ferric salt. Thereafter, air is replaced by nitrogen and 4% acetic anhydride based on initially charged acetic acid is added, temperature is raised to 35-40°C, and iron is oxidized with ferric salt until full consumption of the latter. Resulting snow-white ferrous acetate suspension is separated from unreacted iron, filtered off, and dried. All above operations are carried out under a nitrogen atmosphere. Filtrate, which is saturated ferric acetate solution in acetic acid/acetic anhydride mixture, is recycled to reactor to be reprocessed or it is used according another destination.

EFFECT: simplified technology and improved economical characteristics of process due to use of inexpensive oxidant.

2 ex

FIELD: inorganic syntheses.

SUBSTANCE: ferric acetate is prepared by interaction of metallic iron with acetic acid in presence of an oxidant. Process is carried out at ambient temperature in acetic acid/acetic anhydride medium (weight ratio 5:1) under nitrogen atmosphere. Molar ratio acetic acid/iron/basic ferric acetate is maintained the following: 10:8:1. Reaction mixture is thoroughly stirred with high-speed blade stirrer or shaken at shaking frequency 2 Hz. When consumption of basic ferric acetate is completed, suspension of ferrous acetate is separated by filtration from unreacted iron powder. Precipitate is dried and filtrate returned into the process.

EFFECT: simplified process due to selection of optimal oxidant.

2 ex

FIELD: industrial inorganic synthesis.

SUBSTANCE: implementation of the method comprises contacting iron in the form of iron powder or iron sidewall adjacent to a body with glacial acetic acid and air oxygen at 17-25°C and vigorous stirring effected by high-speed blade-type mechanical stirrer. Initial acetic acid-to-iron molar ratio is (224÷274):100. Acetic anhydride additive is preferably introduced in amount of 2% based on the initial concentration of acetic acid. When concentration of ferric salt in the mixture reaches 2.70-3.51 mole/kg, stirring is stopped and heavy unreacted iron particles are allowed to settle/ Major mass of product suspension is filtered off and thus obtained basic ferric acetate precipitate is dried. Filtrate, which is saturated acetic acid solution of basic ferric acetate, is returned into reactor to be reprocessed. Yield of desired product achieves 99.2-99.3%.

EFFECT: simplified process and improved economical efficiency due to utilization of inexpensive raw material and accessible oxidant.

2 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for preparing acetic acid salts, in particular, anhydrous ferrous (II) acetate. Method for preparing anhydrous ferrous (II) acetate involves interaction of metallic iron with acetic acid in the presence of oxidizing agents of ferric oxide Fe2O3 or Fe3O4 and molecular iodine in the mole ratio acetic acid : acetic anhydride : iron oxide = 100:(6-20):(2-2.5), respectively, and in the mole ratio iron oxide : iodine = 100:6.3. The process is carried out at temperature 80°C in the beaded mill of vertical type with high-rotation blade mixer and reflux condenser in the mass ratio of glass beads and liquid phase in the charge = 1:1. The process is carried out with periodic taking off samples of the end product solid phase by filtering and the following recover filtrate and feeding with acetic acid and iron oxide. For compensation of components loss of liquid phase in filtering there are recovered into reactor to the repeated process that is carried out for four times at a time. All procedures of the basic process and filtration are carried out in nitrogen medium. Preferably, method involves using hematite, γ-oxide, iron minium, magnetite or Fe3O4 x 4 H2O as the iron oxide source. Invention provides possibility for preparing anhydrous ferrous (II) acetate and simplifying method due to excluding the evaporation stage in isolation of salt.

EFFECT: improved preparing method.

3 cl, 2 tbl, 8 ex

FIELD: inorganic synthesis.

SUBSTANCE: invention provides heterometallic neodymium (III) and iron (III) malate having formula I:

appropriate for synthesis of mixed oxides with perovskite structure, which are used as catalysts in oxidative catalysis of unsaturated acyclic hydrocarbons and as materials used in microwave frequency technology and in computer memory materials. Preparation consists in electrolysis of concentrated aqueous solution of neodymium (III) chloride and malic acid at 1:3 ratio in presence of pyridine with pressed reduced iron anode and inert cathode at anode current density 1 A/cm2, followed by separating precipitate and washing it with organic solvent before drying.

EFFECT: enlarged assortment of oxidation catalysts.

2 cl, 1 dwg, 2 tbl

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

The invention relates to a technology for technical formate sodium from aqueous solution technical Chlorella, which is a waste product of chloroform
The invention relates to the production of sodium formiate and obtaining thus purified chloroform

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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