Method of production of the ferric formiate (ii)

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

 

The invention relates to a technology for ferrous iron salt and formic acid and can be used in various fields of industrial and laboratory chemicals, to obtain the composite materials and analytical control.

It is known that the interaction of iron with formic acid in the presence of molecular iodine without limiting the contact of the reaction mixture with air leads to the accumulation of formate, iron (II) in quantities exceeding the stoichiometric in relation to the loaded iodine (Amiano, Sportwhat, Sviridonova. Some ways of spending of iron in solutions of iodine in low molecular weight fatty acids and evaluation of their competitive ability // proceedings of the Kursk state technical. Univ. Kursk 2003, №1 (10). P.59-63).

The disadvantages of this option are;

1. The use of a liquid medium only formic acid, which is quite volatile, which significantly restricts the upper limit of the temperature regime of the process and requires high performance reverse condenser and system for capturing acids in General.

2. The main raw material for cations product is iron, which is in contrast to iron oxide Fe2O3or Fe3O4the natural connection is not.

3. Too concentrated solutions m is RAVENOL acid secretion salt is very difficult.

Closest to the claimed is a method of producing acetate iron (II) patent of Russian Federation 2259994, publ. 10.09.2005, in accordance with which in interaction with acetic acid injected iron and iron oxide Fe2About3or Fe3O4in the presence of iodine as oxidant iron and acetic anhydride as nodosauridae funds and stimulating supplements at 80°in a nitrogen atmosphere, with periodic sampling of the solid phase of acetate of iron (II) to avoid excessive thickening of the suspension and converting the reaction mixture into a paste.

The disadvantages of this method are:

1. Quite a high temperature process (80°). Formic acid compared to acetic acid boils at a lower temperature, and hence more volatile. Therefore, with the flow of gas entrainment it much more, which requires improving the efficiency of the reverse condenser and additional technological solutions. Consequently, the use of formic acid as a basic component of the liquid phase of the reaction mixture at such temperature and other conditions is hardly possible.

2. The process in the environment (duct) nitrogen leads to increased entrainment of acid and poses significant difficulties not only in the process itself, but also in the allocation of the product, i.e. in the processing of actionnow mixture.

3. The model of this process is unlikely to be fully implemented for formic acid as the anhydride of formic acid does not exist, and therefore there is no fundamental ability to play used in the prototype formulation.

The objective of the proposed solutions is to obtain formate, iron (II) iron and iron oxides Fe2About3or Fe3O4in their interaction with dissolved organic media with formic acid in the absence of dehydrating means, inert gas environment and specific heat to provide the necessary temperature mode.

This object is achieved in that the load on the process consists of a liquid phase, iron oxide Fe2About3or Fe3O4, iodine, metallic iron and its alloys, while the liquid phase of the boot that includes an organic solvent, formic acid and water in a mass ratio of 100:(85÷100):(15÷0)take in relation to the mass of the bead 1:1, iron oxide Fe2About3or Fe3O4metered quantity 0,40-0,56 or of 0.21-0.42 mol/kg liquid phase, iodine load in the amount of 0.03-0.10 mol/kg liquid phase, iron impose a steel shell over the entire height of the side surface of the reactor and optionally in the form of powder recovered metal, pieces of broken Chu is una and (or) steel wool with a maximum linear size of 5 mm in any ratio between a total amount of 20% by weight of the liquid phase system, and the process starts when the ambient temperature and can be done without any obstacles in contact with air while limiting the spontaneously growing due to the exothermic stages temperature in the range of 35-55°to practically complete spending just loaded iron oxide, after which the stirring and cooling of the reactor ceased, the suspension of the reaction mixture is separated from the beads and large particles of metal from the discharge through the mesh in the drain pipe bead mill and subjected to centrifugation or sedimentation, after which the clarified liquid phase returns to repeat the process, and the residue dissolved in saturated iron formate 1-2 mol/kg water the formic acid when heated to 85-95°, solids finely dispersed iron residues of unreacted iron oxide, carbon from cast iron and steel are separated by hot filtration, the filtrate is left for natural cooling and crystallization of formate, iron (II). The organic solvent used ethyl cellosolve, butyl acetate, butyl alcohol, amyl alcohol, ethylene glycol. Specially in the initial loading is not mixed with water, and comes only with a dosed with formic acid.

Characteristics of the raw materials used.

The reactive iron in THE 6-09-2227-81

Steel 3 what about CMTU 1-84-67

Steel 45 GOST 1050-74

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

The iron oxides:

hematite according to GOST 4173-77

minium on THE 113-00-38-160-96

γoxide according to GOST 3540-82

magnetite according to GOST 26475-85

Formic acid according to GOST 5848-73

Iodine crystal according to GOST 4159-79

The ethyl cellosolve according to GOST 8313-88

Butyl acetate on P-12-68

Butyl alcohol according to GOST 6006-78

Amyl alcohol according to GOST 5830-77

Ethylene glycol according to GOST 10164-75

The process of the inventive method the following. In a ball mill, vertical type, equipped with high-speed paddle stirrer, reflux-condenser, a drain pipe with a grid with a cell size of 0.5×0.5 mm, steel shell over the entire height of the casing and forced cooling, enter the glass beads and the liquid phase of the boot, and also iron oxide, crystalline iodine powder recovered iron and / or broken cast iron and (or) broken into pieces of steel shavings in appropriate quantities. Ball mill is placed on the workstation, connect the necessary communications and the forced cooling system include mechanical mixing and the time taken for the beginning of the process. Observe the change of the temperature of the reaction mixture. First, she almost does not change, then starts autoscoring to grow. Include in WriteLine cooling and stabilize temperature in the range of 35-55° C.

Upon reaching almost total consumption of iron oxide mixing ceased, the reaction mixture is separated from the beads and large pieces of unreacted iron and shaving at the sink through the bottom pipe with mesh and directed by centrifugation or sedimentation. The clarified liquid phase returns to repeat the process, and the residue is dissolved under heating in saturated formate, iron (II) 1-2 mol/kg aqueous solution of formic acid under stirring. Upon completion of the dissolution process the resulting mass was filtered, the solids removed and the filtrate is left for slow cooling and crystallization of formate, iron (II). Upon completion of crystallization of the solid product is separated and dried, and the filtrate is directed to the preparation of saturated formate, iron (II) 1-2 mol/kg solution of formic acid.

Example 1

In ball mill vertical type stainless steel (inner diameter of 80 mm and a height of 200 mm with a spherical bottom and a drain pipe located at a height of 10 mm from the bottom point), equipped with a paddle agitator with bottom profile of the blade, repeating spherical bottom and separated from it by 0.3-0.6 mm, and cover with stuffing box for stirrer, reflux-condenser, a loading opening, a pocket for thermocouple and socket for OTB the RA samples during the process, and filled with dead zones of the apparatus, the reaction mixture of the previous give 450 g of beads and 450 g of a liquid phase, representing a solution of formic acid and iodine in ethyl cellosolve concentrations 9,24 mol/kg and 0.1 mol/kg, respectively. For preparation of this solution was used in 85%formic acid is taken in a ratio by weight with the solvent 1:1. Thus, the initial mass ratio of solvent : acid: water is 100:85:15 then load 90 g of recovered iron and 43.8 g of iron oxide Fe3O4. include mechanical stirring (1440 rpm, power 0.5 kW). The initial temperature of 20°C. Observe the temperature change along the way. After 15 min she was 30°C. Serve cooled with liquid baths and keep the temperature at 36±1°C. in Parallel without interrupting the mixing take samples of the reaction mixture, which determine the total content of salts of iron (II), and the residual quantity of iron oxide at the moment. As soon as the latter becomes close to zero, and this happened after 80 min after the start, mechanical stirring is stopped, give a few minutes for sedimentation of heavy particles of iron and through the mesh drain pipe with a cell size of 0.5×0.5 mm separating the reaction mixture from the beads. the thus, the uploaded 505 g of the reaction mixture, which are quite viscous, but still moving the suspension is slightly pink. The salt content of iron in her analysis of 1.5 mol/kg

The resulting slurry is directed to the centrifugation, the clarified layer selected, weighed, determine the salt content of iron (II) it and return to repeat the process. The remaining compacted sludge is transferred into a heat resistant container with blade mechanical stirrer, into which is injected 750 g saturated formate, iron (II) solution of formic acid with a concentration of 1.12 mol/kg Include mechanical mixing and heating. Lead dissolution of deposited sediment within 83 minutes On achieving almost complete dissolution of all sludge heating ceased. The temperature at this point was 91°C. the Solution is mixed with the solid phase quickly transferred to heated to approximately the temperature of the filter and maintain the separation of undissolved impurities. The mass of the latter was 0.38, this is mainly of fine particles of unreacted oxide.

The filtrate is left for natural cooling and crystallization of formate, iron (II). After 12 hours, filtering the precipitated precipitate formate, iron (II) and dried. Received 116,5 g dry salt. The filtrate after determining the salt content of iron and formic acid used in the t for solution preparation for subsequent recrystallization.

Examples 2-10

Used bead mill, the number of beads in it, thinner, iron oxide, loading of the liquid phase and the sequence of operations of the process and selection of a product similar to that described in example 1. Different concentrations of formic acid and iodine in the initial liquid phase, the use of broken cast iron, broken steel wool and mixtures thereof with each other and with reduced iron and the amount of Fe3O4in the download. The results obtained are summarized in the table. (Designation: PC - reaction mixture, of state - liquid phase boot; CP - centrifugation, sedimentation)

Example 11-17

Used bead mill, a number of loaded beads and liquid phases, the sequence of operations of the process of acquisition and allocation of formate, iron (II) is similar to that described in example 1. Differ in the nature and quantity of the iron oxide, as well as the nature of the solvent. The results obtained are summarized in the table. (Designation: EC - ethyl cellosolve, EG - ethylene glycol, BA - butyl acetate, BS - butyl alcohol, AC - amyl alcohol).

The positive effect of the proposed solution consists of:

1. This process does not require external supply of heat, simple in hardware design, easily problemy and safely performed while downloading where heating of the reaction mixture when the cooling system is not leading to boiling and too rapid boil.

2. In this process the bulk salt is formed from a metal oxide, the almost complete expenditure of which uniquely determines the end of the process.

3. This process uses the available raw materials, and optional reactive purity, and the resulting product is easily detected from the reaction mixture and can be sufficiently purified by recrystallization.

1. The method of producing formate, iron (II) by direct interaction of the acid with iron, alloys and oxides of Fe2About3and Fe3About4in the presence of stimulating supplements of iodine in a bead mill with a reflux-condenser, a high-speed paddle stirrer and glass beads as pereirago agent, characterized in that the loading process consists of a liquid phase, iron oxide Fe2About3or Fe3About4, iodine, metallic iron and its alloys, while the liquid phase of the boot that includes an organic solvent, formic acid and water in a mass ratio of 100:(85-100):(15-0), take in relation to the mass of the bead 1:1, iron oxide Fe2About3or Fe3About4metered quantity 0,40-0,56 or of 0.21-0.42 mol/kg liquid phase iodine load in the amount of 0.03-0.10 mol/kg liquid phase, iron is administered in the form of a steel shell over the entire height of the side surface of the reactor and optionally in the form of powder recovered iron, pieces of broken cast iron and(or) steel wool with a maximum linear size of 5 mm in any ratio between a total amount of 20% by weight of the liquid phase system, and the process starting at ambient temperature and can be done without any obstacles in contact with air while containing spontaneously growing due to the exothermic stages temperature forced cooling in the range of 35-55°to practically complete spending just loaded iron oxide, after which the stirring and stop cooling, the suspension of the reaction mixture is separated from the beads and large particles of metal by passing through the mesh in the drain pipe bead mill and subjected to centrifugation or sedimentation, after which the clarified liquid phase returns to repeat the process, and the residue dissolved in saturated formate, iron (II) 1-2 mol/kg aqueous solution of formic acid when heated to 85-95°, solids finely dispersed iron residues of unreacted iron oxide and carbon from cast iron and steel are separated by hot filtration, the filtrate is left for natural cooling and crystallization of form a is the iron (II).

2. The method according to claim 1, characterized in that the organic solvent used ethyl cellosolve, butyl acetate, butyl alcohol, amyl alcohol, ethylene glycol.

3. The method according to claim 1, characterized in that especially in the initial loading is not mixed with water, and comes only with a dosed with formic acid.



 

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 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, in particular two-component heterogeneous immobilized catalyst for ethylene polymerization.

SUBSTANCE: claimed catalyst includes alumina, mixture of transition metal complexes with nitrogen skeleton ligands (e.g., iron chloride bis-(imino)pyridil complex and nickel bromide bis-(imino)acetonaphthyl complex). According the first embodiment catalyst is prepared by application of homogeneous mixture of transition metal complexes onto substrate. iron chloride bis-(imino)pyridil complex and nickel bromide bis-(imino)acetonaphthyl complex (or vise versa) are alternately applied onto substrate. According the third embodiment catalyst is obtained by mixing of complexes individually applied onto substrate. Method for polyethylene producing by using catalyst of present invention also is disclosed.

EFFECT: catalyst for producing polyethylene with various molecular weights, including short chain branches, from single ethylene as starting material.

7 cl, 5 tbl, 27 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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