Method for preparing ferrous (ii) acetate

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

 

The invention relates to a technology for obtaining salts of acetic acid, in particular acetate anhydrous iron (II), which is used in various industries, analytical and applied chemistry.

A method of obtaining acetates of divalent copper, Nickel or cobalt dissolution of metals in acetic acid under oxygen pressure of 0.4-0.6 MPa at 100-120°and the molar ratio of metal:acetic acid 1:5,2÷5,3 (A.S. USSR №1097604).

The downside of it is quite high-temperature process in which the solubility of oxygen as oxidant in the liquid phase is very small, even when using high pressure.

Closest to the claimed is a method of producing acetate cobalt (A.S. USSR № 1728222), according to which as oxidant use hydrogen peroxide or peracetic acid, which is mixed with acetic acid in a molar ratio of 1:2 served continuously in the upper part of the column is filled with the metal cobalt with a specific surface area 1-1000 cm2/g with simultaneous selection of the bottom of the column an aqueous solution of cobalt acetate and evaporation of the latter with the aim of identifying the product by crystallization.

The disadvantages of this method are:

1. In anorganische environment determine udalenie the target product by evaporation, that is a separate process (or stage), very energy intensive and also long, and with the melt, the prospects for utilization of steam.

2. From water-organic media crystallizes only hydrated, in this case, for example, With(C2H3O2)2·4H2O, but not the anhydrous salt.

3. Used oxidant (hydrogen peroxide, in particular) in no way reflected in the weight of the resulting product, although it takes a direct part in the intermediate stages of this complex multi-stage redox process.

4. Cobalt with a specified specific surface need to get.

5. The model of this process is unlikely to be implemented for iron, because the acetate of iron (II) in solution is very sensitive to oxygen and is easily oxidized in basic acetate of iron (III). Hydrogen peroxide and percolate oxidize acetate iron (II) salt of iron (III) almost instantly. Therefore, even in an inert atmosphere, but with such oxidizing agents more realistic receive basic acetate of iron (III), but not acetate iron (II), not anhydrous and hydrated.

The objective of the proposed solutions is to receive acetate anhydrous iron (II), to avoid a stage evaporation in the allocation of the specified salt is the quality of the target product, and to use an oxidizer, which would bring a significant contribution to the mass produced product.

This object is achieved in that the oxidizer take iron oxide Fe2About3or Fe3O4and molecular iodine in the initial molar ratio of 100:6,3, and the process is conducted in a reactor of the type bead mill with glass beads in a mass ratio of the liquid phase of 1:1 with high-speed mechanical stirrer and reflux-condenser in a nitrogen atmosphere with the use of iron in the form of a coiled-type shells tape with equal working height of the side surface of the reactor height and initial loading of acetic acid, acetic anhydride and iron oxide in a molar ratio of 100:(6÷20):(2÷2,5) at 80°With periodic sampling of the solid phase of acetate of iron (II) by filtration in a nitrogen atmosphere, returning the filtrate together with the feed consumed by the formation of acetate of iron (II) acetic acid and iron oxide, as well as compensation of losses of acetic acid anhydride and iodine during the filtration process in the reactor to repeat the process. The Fe2About3take hematite, γoxide, iron oxide red, and as Fe3O4magnetite and Fe3O4·4H2Oh, and repeated the process carried out at least four times in a row.

Characteristics of ispolzuemogo raw materials

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

Iron carbonyl radio brand R-20 GOST 13610-79

The iron oxides:

hematite according to GOST 4173-77

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

γoxide according to GOST 3 540-82

magnetite according to GOST 26475-85

Iodine crystal according to GOST 4159-79

Acetic acid according to GOST 61-75

Acetic anhydride according to GOST 5815-77

Steel 3 on CMTU 1-84-67

The process of the inventive method the following. In ball mill vertical type with glass (for reactive product purity) or steel (for technical product) housing and the agitator vane type of dense and inert plastic or steel, and with a reflux-condenser is placed with a small gap to the chassis bent-type shell of iron or steel tape with a height that meets the working height of the reactor. Connect the mill shell with cover with stuffing box mixers, accessories for temperature control, sampling and providing gas flow and loading nozzle. Through the latter enter the estimated amount of the mixture of acetic acid and acetic anhydride, and oxide of iron, iodine and glass beads as pereirago agent. Include stirring and heating. Then organize duct nitrogen through the gas space of the bead mill. The exit temperature is URS the specified mode remains of the oxygen in the air is almost completely spent on chemical transformations and, from this point, the main raw material for producing acetate become iron oxide and iron. The solubility of acetate of iron (II) in the selected environment and conditions, it is quite small and after a short time all resulting in further salt goes into the solid phase. From this point, the reaction mixture turns into a corresponding complex suspension with solid phases of iron oxide and salt. Upon reaching almost total consumption of iron oxide suspension acetate iron (II) through a grid at the bottom of the pipe mill to separate from the glass beads is directed to filtration, then the filtrate is recycled back to the reactor, hold enter another portion of iron oxide, as well as recharge spent on the formation of acetate of iron (II) acetic acid and compensation of loss of components of the liquid phase during the filtration, then repeated the process of obtaining the target salt. Recharge acetic anhydride and iodine for such compensation shall be allowed to not every time. The process stops if necessary, recharge the tape or after obtaining the required amount of salt.

Drying the filtered salts is carried out in a nitrogen atmosphere.

Example 1

In the glass case vertical bead mill type internal diameter of 63.7 mm and a height of 109 mm insert a shell of the floor is si iron of a thickness of ˜ 0.8 mm with an external diameter of ˜62 mm, height 65 mm and weight 77,85, After this case is connected to the fixed stationary on the frame cover with a mechanical stirrer vane type of Teflon and reflux-condenser. Through the loading hatch in the lid consistently give 110,85 g of glass beads with a diameter of 0.9÷1.6 mm, 100 g of glacial acetic acid, 10.2 g of acetic anhydride, to 6.67 g of hematite and 0,667 g of molecular iodine. Close the loading door, down a liquid heating bath from below so that the working part of the bead mill was immersed in a preheated to 65°With fluid again include heating in the bath include mechanical stirring agitator bead mill with the speed of 1260 rpm and serves duct nitrogen through the gas space of the reactor with a flow rate of 0.28 l/min After 20 min the temperature in the reaction zone reaches 80°C. Stabilize the temperature at this level and carry out the process within 140 min, holding control over the expenditure of the oxide by the method of sampling and analysis of samples. During this time, almost all the input hematite have time to fully react in salt, the bulk of which is in the solid phase.

The resulting suspension with a uniformly distributed through the volume of the solid phase direct in nitrogen atmosphere for filtration, then the filtrate to the number of 91.6 g return in a bead mill to repeat the process. With him is injected into the reactor 19 g of glacial acetic acid and 6.7 g of hematite as compensation unreacted reagents and loss of the liquid phase during the filtration process. Stabilize the temperature at 80°and conduct proceedings for 110 min, which all entered the second time hematite time to change into acetate of iron (II). Spend again the separation of the reaction mixture from beads, filtration of the solid phase of acetate of iron (II), the return of the filtrate in number to 91.1 g of bead mill, enter a new portion of hematite aid of acetic acid and other components of the liquid phase. Next, perform a stabilization of the temperature, the following process for 135 min, then the cycle departments, aid, following repeated the process, etc.

In particular, in the second, third and fourth re-processes the input hematite amounted to 6.7 g each time, the input of acetic acid was 20, 20, and 22 g of acetic anhydride, 1.5 g of molecular iodine on 0,114 g before the third and fourth re-processes. The duration of the second, third and fourth re-processes 114, 97, and 105 minutes For five consecutive processes the received 104,7 g dried in nitrogen atmosphere acetate iron (II). The content of acetate of iron in suspension before filtration fluctuated in the range of 1.00-1.15 mol/kg Further accumulation of the product in suspension was necelesobrazno the output due to a sharp reduction in the flow speed of the chemical interactions in such conditions.

Examples 2-7.

The reactor, the boot order of the reagents, the sequence of operations of the process, separating the suspension from the beads and solid acetate of iron in the slurry, the temperature mode, the number of retry processes similar to those described in example 1. Different nature of the iron oxide and the molar ratio of acetic acid: acetic anhydride: iron oxide, dozagruzki to repeat the process. The results obtained are summarized in table 1

Example No. 8.

In a ball mill made of stainless steel which has the dimensions: diameter 80 mm, height 200 mm, wall thickness 11 mm, with a smaller gap insert a shell of steel 3 height 110,9 mm and weight 384,5, the Housing shell is connected to the lid with a paddle stirrer, reflux-condenser and a loading opening. The agitator shaft with a flexible coupling connected to an electric motor rigidly mounted on the upper platform of the skeleton frame. Through the charging port injected 350 g of glass beads with a diameter of 0.9÷2.1 mm and 350 g of a mixture containing 298,4 g of glacial acetic acid and 50 g of acetic anhydride. Next enter 1,60 g of solid iodine and 23,15 g of magnetite. The molar ratio of acetic acid: oxsny anhydride: iron oxide 100:9,86:2 and the molar ratio of iron oxide: iodine 100:6,3. Close C the loaders hatch, serves duct nitrogen with a flow rate of 0.36 l/min through the gas space of the bead mill, the last case is placed in moving along the longitudinal axis of the reactor, heating the liquid bath, include heating the latter and mechanical stirring in a bead mill, paddle mixer with a speed of 1440 rpm Deduce the temperature at 80°, which took 37 minutes Stabilize the temperature at this level and in such conditions continue stirring for 75 minutes the Results of the control method of sampling show that by this time, almost the entire magnetite reacted and content of molecular iodine in the reaction mixture is close to zero.

Stop stirring bead mill, the heating bath is lowered down so that the drain pipe of the mill building, containing in the upper part of a screen to separate the beads from the suspension of the reaction mixture, was available for connection to the node filtering, perform this connection, using it as a cooler for cooling the suspension, open the shutoff valve on inlet and conduct filtering acetate iron (II). When this duct nitrogen through the gas space of the bead mill is redirected to the node filtering.

The filtrate is returned to repeat the process, increasing its mass by the addition of 52 g of uksosn the th acid and 3 g of acetic anhydride in order to compensate for the expenditure of the first to the formation of salt as well as inevitable during the filtration loss (wetted sediment, the walls of the filter, the receiving tank and so on). Metered and 23.2 g of magnetite, and then perform all operations on output and temperature stabilization, process control, an end to the separation of the solid product, the actual separation by filtration and repetition just described for the second repeated the process. Just spent four repeated process, although restrictions on the possible number of them are not identified. The question is, how fully and successfully conducted the compensation of acetic acid, acetic anhydride and iodine before each repeated the process. Made options are summarized in table 2

Table 2

Compensated and the input componentDosage in g
the secondthe thirdfourth
Acetic acid52,345,8to 49.9
Acetic anhydride4,17,2the 3.8
iodine0,210,210,23
magnetite23,2723,19of 23.11

For these five processes received 331,7 g of dry solid acetate iron (II), n is that spent 534 min (re-processes: the first 23+84, the second 27+77, the third 19+80 and fourth 21+91) of them at the conclusion of temperature on the mode 127 minutes also remained 308 g of the solution of acetate of iron (II) in a mixture of acetic acid and acetic anhydride with the addition of iodine (mostly in the form of FeJ2), which can be used to continue the process in the subsequent repeated the process.

The positive effect of the proposed solution is as follows:

1. This process does not require high temperatures and is quite simple in hardware design. It uses the available raw materials, and not necessarily reactive purity.

2. The selection of product is not an independent phase, and occurs during the process. Thus instead of energy-intensive and prolonged evaporation is used much more easy filtering.

3. Received the product in anhydrous environment does not contain water of crystallization. Therefore, do not need special stage to remove it.

4. Major contamination of the product is accounted for iodide iron (II) and to a lesser extent on the molecular iodine. These impurities can be removed by recrystallization of the product from a mixture of acetic acid and acetic anhydride. Moreover, obtained after separation of the recrystallized product, the filtrate is returned to the main process either as the original liquid medium, either as podpitat what's liquid phases.

1. The method of obtaining acetate iron (II), the interaction of metallic iron with acetic acid in the presence of an oxidizer, wherein the oxidizer agents take iron oxide Fe2O3or Fe3O4and molecular iodine in the initial molar ratio of 100:6,3, and the process is conducted in a reactor of the type bead mill with glass beads in a mass ratio of liquid phase loading 1:1, with high-speed mechanical stirrer and reflux-condenser in a nitrogen atmosphere with the use of iron in the form of a coiled-type shells tape a height equal to the working height of the side surface of the reactor, and the initial loading of acetic acid, acetic anhydride and iron oxide in a molar ratio of 100:(6÷20):(2÷2,5) at 80°C, with periodic sampling of the solid phase of acetate of iron (II) by filtration in a nitrogen atmosphere, returning the filtrate together with the feed consumed by the formation of acetate of iron (II) acetic acid and iron oxide, as well as compensation of losses of acetic acid anhydride and iodine during the filtration process in the reactor to repeat the process.

2. The method according to claim 1, characterized in that the iron oxide used hematite, γoxide, red iron oxide, magnetite and Fe3O4·4H2O.

3. The method according to claim 1, characterized in that the re process PR is lead not less than four times in a row.



 

Same patents:

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

The invention relates to petrochemistry, specifically to the production dialkyldithiocarbamate accelerators of vulcanization of rubbers

The invention relates to a method for the polymerization of 1-olefins which can be used in catalytic systems and which include nitrogen-containing compounds of transition metals, including structural unit represented by the formula (V), where M represents Fe (II), Fe (III), Ru (II), Ru (III) or Ru (IV), X represents an atom of Cl or Br, T denotes the oxidation state of the transition metal M and b is the valency of the group X, the values of each of R1, R2, R3, R4and R6independently from each other selected from hydrogen, methyl, ethyl, n-propyl, n-butyl, n-hexyl, n-octyle, and values of each of R5and R7independently from each other selected from phenyl, 1-naphthyl, 2-naphthyl, 2-methylphenyl, 2-ethylphenyl, 2,6-diisopropylphenyl, 2,3-diisopropylphenyl, 2,4-diisopropylphenyl, 2,6-di-n-butylphenyl, 2,6-dimetilfenil, 2,3-dimetilfenil, 2,4-dimetilfenil, 2-tert-butylphenyl, 2,6-diphenylphenol, 2,4,6-trimetilfenil, 2,6-triptoreline, 4-bromo-2,6-dimetilfenil, 3,5-dichloro-2,6-diethylphenyl and 2,6-bis(2,6-dimetilfenil)phenyl, the cyclohexyl and pyridinyl

The invention relates to the field of ORGANOMETALLIC compounds, namely bis-cyclopentadienyl (ferrocene)

The invention relates to a new stable complex compound containing macrocyclic tetradentate ligand having the structure of formula I, where R1and R2have the same or different values are related or unrelated, and each is selected from the group consisting of hydrogen, halogen, methyl, CF3and, if they are connected, cyclopropyl, cyclobutyl, cyclopentyl or cyclohexyl, are spatial and confirmation difficult, so that the oxidative degradation of complex metal compound is limited, when the complex is in the presence of an oxidizing environment, Z represents a stable to oxidation atom, which metallocomplexes selected from nitrogen and oxygen, X represents an oxidation resistant functional group selected from O or NRswhere Rsrepresents a methyl, phenyl, hydroxyl, auxillou group, CF3or CH2CF3, R3, R4, R5represent fragments of connecting adjacent Z atoms containing structure described in the claims
The invention relates to methods for dilaceration chelates of iron and can be used, for example, in agriculture as a protective means and in veterinary medicine

The invention relates to the synthesis of bridge mu-oxo-perchloroethene (III) of tetraalkylammonium General formula [R4N]3[Fe2Cl7O], where R is lower alkyl, and to a method for bridging mu-oxo-perchloroethene (III) of tetraalkylammonium possessing properties improper ferroelectric

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing copper (II) acetate monohydrate that represents organic carboxylic acid salt. Copper (II) acetate monohydrate is prepared by crystallization from solution obtained by mixing acetic acid, alkaline metal acetates or ammonium with copper-containing spent solution used in etching printing boards. Method provides reducing cost of the proposed method for preparing copper (II) acetate monohydrate, retaining purity of product with simultaneous utilization of toxic waste in electronic engineering manufacture - the spent solution in etching printing boards. Also, invention provides reducing material consumptions in preparing copper (II) acetate monohydrate, expanding assortment of materials used for its preparing and utilization of toxic waste in electronic engineering manufacture. Product obtained by the proposed method can be used as pigment, fungicide and copper microfertilizer in agriculture, as catalyst in processes of polymerization, as a stabilizing agent of artificial fibers, for preparing galvanic solutions and preparing other copper compounds.

EFFECT: improved preparing method.

14 cl, 5 ex

The invention relates to the production of salts of acetic acid
The invention relates to waste disposal and the simultaneous achievement of commercial products and can be used in other industries where liquid wastes with a content of acetic acid

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing copper (II) acetate monohydrate that represents organic carboxylic acid salt. Copper (II) acetate monohydrate is prepared by crystallization from solution obtained by mixing acetic acid, alkaline metal acetates or ammonium with copper-containing spent solution used in etching printing boards. Method provides reducing cost of the proposed method for preparing copper (II) acetate monohydrate, retaining purity of product with simultaneous utilization of toxic waste in electronic engineering manufacture - the spent solution in etching printing boards. Also, invention provides reducing material consumptions in preparing copper (II) acetate monohydrate, expanding assortment of materials used for its preparing and utilization of toxic waste in electronic engineering manufacture. Product obtained by the proposed method can be used as pigment, fungicide and copper microfertilizer in agriculture, as catalyst in processes of polymerization, as a stabilizing agent of artificial fibers, for preparing galvanic solutions and preparing other copper compounds.

EFFECT: improved preparing method.

14 cl, 5 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: organic chemistry, medicine, dermatology.

SUBSTANCE: invention relates to zinc and aliphatic halogen-carboxylic acid salts that can be used in treatment of benign neoplasms of skin and visible mucosa tissues. Invention proposes the following formula of zinc and aliphatic halogen-carboxylic acid salts: (1): wherein R means -CHal3, -CHHal2, -CH2Hal and (2): wherein R' means Alk, hydrogen atom (H); R'' means Hal; R' means Alk; R'' means H, Alk wherein in these formulae halogen atom can be represented by fluorine atom (F), chlorine atom (Cl), bromine atom (Br) or iodine atom (J). Invention provides the development of original preparation used in treatment of benign neoplasms of skin and visible mucosa tissues with low toxicity, rapid effect, expressed therapeutic effect and eliciting good tolerance, absence of complications in treatment, healing without formation of scar tissue. The development of the preparation provides expanding assortment of agents used in treatment of such diseases.

EFFECT: enhanced and valuable properties of agents.

13 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: 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: 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: chemical industry; methods of production of acetates.

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the method of production of lead tetraacetate. The method provides for realization of interaction of the red-lead with anhydrous acetic acid at the temperatures of 30-40°C with the subsequent separation of the target product not later than 3-5 hours after the termination of reaction. In the capacity of the dehydrating reagent is used the by-product of the interaction - lead diacetate, which forms the hydrated complex with water. The invention ensures production of lead tetraacetate equal to 70-75 % from the theoretical value. The technical result of the invention is simplification of the production process, improvement of the economic features.

EFFECT: the invention ensures simplification of the production process, improvement of the economic features.

1 ex

FIELD: chemical industry; methods of neutralization of the water combustible solutions of the acetic acids at the computerized batching-packing machine.

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the method neutralization of the acetic acid and its solutions at leakages and accidents. The method of neutralization of the water combustible solutions of the acetic acids at the computerized batching-packing production line provides for the treatment of the surface, on which there is a leakage of the acetic acid, with the powdery anhydrous sodium carbonate. The treatment of the spilled acetic acid is exercised till formation of the paste and the paste is left on the surface for a while. At the second and the subsequent leakage of the acetic acid on the tray and at formation of the liquid phase the place of the spill is treated with a sodium carbonate till formation of the paste with the purpose for binding the liquid phase. In the case the acetic acid spills on the surfaces located outside of the tray, the neutralization of the acetic acid is exercised by water till gaining the 25-30 % solution. The surface treatment with the powder of the sodium carbonate at the first spill is exercised at the following components ratio (in mass %): Na2CO3:CH3C00H = 1.6÷4.0:1. The invention ensures reduction of the wastes of the production process, allows to reduce emissionof CO2 and allows to diminish toxicity of the production process.

EFFECT: the invention ensures reduction of the wastes of the production process, reduction of emissionof CO2 and reduction toxicity of the production process.

Up!