Ferrous acetate preparation method

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

 

The invention relates to a method for producing acetate ferrous iron, which finds application in various fields of industrial and laboratory chemical practices.

A method of obtaining acetates of divalent copper, Nickel and cobalt by the interaction of the metal with acetic acid in the presence of oxygen at 100-120°C, the oxygen pressure 0.4-0.6 MPa, and a molar ratio of metal and acetic acid 1:(5,2-5,3) (A.S. USSR №1097604).

The disadvantage of it is that at this temperature the solubility of oxygen in the liquid phase is very small. Moreover, in the presence of oxygen acetate iron (II) is easily oxidized in the salt of iron (III), which excludes the use of this oxidant in this embodiment, to obtain a salt of iron (II) metal and acetic acid.

Closest to the claimed is a method of producing acetate cobalt (A.S. USSR №1728222), according to which the process is carried out in a column type reactor filled with a metallic cobalt surface area 1-1000 cm2/g when applying acetic acid and oxidant in a molar ratio of 2:1 continuously in the upper part of the column with simultaneous selection of an aqueous solution of cobalt acetate from the bottom of the column, and as an oxidizer use hydrogen peroxide or peracetic acid.

The disadvantages of this with the person are:

1. The unsuitability of this oxidant due to slight oxidation of salts of iron (II) salt of iron (III), which is an effective catalyst for the decomposition of hydrogen peroxide, especially in homolytic option, accompanied by release of oxygen, which readily oxidizes acetate iron (II) salt of iron (III).

2. The selection of product by evaporation is too energy-intensive and slow stage, the efficiency of which is justified only for large scale production, which cannot be expected to salts of iron (II), the more precarious in relation to the impacts from the oxygen.

The objective of the proposed solution is to find such an oxidant for iron, which would not would transfer salt of iron (II) salt of iron (III), and replace the selection of product by evaporation on a more simple process - filtering.

This objective is achieved in that, as the oxidant, use the primary acetate iron (III), and the process is conducted in the medium of acetic acid and acetic anhydride in a weight ratio in the initial loading of 5:1 at room temperature in the absence of air or in a nitrogen atmosphere, and the molar ratio of acetic acid: iron: basic acetate of iron (III) 10:8:1 with vigorous stirring by shaking or high speed paddle mixer from procrasinate plastic until complete consumption of the basic acetate of iron (III), followed by the separation of the suspension of the acetate of iron (II) from unreacted iron powder, filtering and drying the precipitate in a nitrogen atmosphere, and returning the filtrate, representing a saturated solution of acetate of iron (II) in a mixture of acetic acid and acetic anhydride, to repeat the process with the new input of the next portion of the basic acetate of iron (III) and compensation components of the liquid phase during the filtration process.

Characteristics of the raw materials used

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

Acetic acid according to GOST 61-75

Acetic anhydride according to GOST 5815-77

Basic acetate of iron (III) was obtained by interaction of iron with iron oxides Fe2About3or Fe3O4in a bead mill in the acetic acid medium with the addition of acetic anhydride by filtration of the solid phase iron (III) salts and (II) and the additional oxidation of the residual components of the salt of iron (II) in basic acetate of iron (III) if the drying of the solid phase of the mixture of salts.

Carrying out the claimed process as follows. In placed on a mechanical shaker type reactor conical flask or in a device with a mixing paddle stirrer of inert plastic, equipped with nozzles in the lid for the implementation of flow of nitrogen through the gas space, load rated amount of glacial acetic acid, acetic anhydride, iron powder and basic acetate of iron (III). In the first case hermetic the closed reactor lid, include a mechanical shaker and observe the process. In the second embodiment include a paddle stirrer and serves duct nitrogen through the gas space of the reactor.

Initially, the reaction mixture is painted in brown-brown suspension of basic acetate of iron (III). Gradually the color brightens, there are white streaks, and then quickly turns into a white suspension of acetate of iron (II) over a heavy layer of unreacted iron powder at the bottom. The stop stirring, the suspension is separated from the iron and place the filter in a nitrogen atmosphere. The filtrate is returned to the reactor to repeat after you enter the next portion of the basic acetate of iron and compensation of losses during the filtration process. And the residue on the filter is dried in a flow of nitrogen and then in a nitrogen atmosphere in an oven, then use as directed.

Example 1

In the reactor with high-speed mechanical stirrer, a blade which is made of textolite, load 180 g of acetic acid, 36 g of acetic anhydride, RUR 134.4 g of recovered iron reactive purity and 57.3 g of basic acetate of iron (III). Include mechanical mixing and serves duct nitrogen through the gas space of the reactor. Temperature 17°C. In this mode are the process until such time as all of the loaded bases of the Oh acetate iron (III) does not react and the reaction mixture will look like a white suspension, above are located at the bottom of particles of unreacted iron. Analysis of the salt of iron (III) shows the almost complete absence of the latter. It took 1.8 hours.

Upon termination of the mixing particles of iron as the most severe very quickly are located in the area of the bottom of the reactor and can be easily separated from the rest of the suspension, which is directed to filtration under nitrogen atmosphere to obtain on the filter of a solid mass of iron acetate, drying of the latter on the filter and dried in an environment of heated nitrogen.

The filtrate, representing a saturated solution of acetate of iron (II) in a mixture of acetic acid and acetic anhydride, return to repeat the process with uploading spent on the target product of acetic acid and basic acetate of iron (III), as well as compensation of losses of the liquid phase during the filtration process.

The yield of solid product was 77,1 g or 98.5%. Restrictions on the number of retry processes is not set (6).

Example # 2

In a reactor of the type conical flask with a flat bottom impose 240 g of acetic acid, 48 g of acetic anhydride, 179,2 g restored iron reactive purity and 76.4 g of basic acetate of iron (III). The reactor is sealed and mounted on a work table of a mechanical shaker with a frequency of 2 Hz. Include in hivatal and observe the changes in the reactor. During the first 1.5 hours of the visible changes are not observed: the reaction mass is a brown suspension, fairly Autonomous moving over the iron particles moving in accordance with the operation of the mechanical shaker. Next, the reaction mixture is gradually brightens and by the end of the 4th hour turns into a white suspension above the unreacted particles of iron. The analysis shows the almost complete absence of iron (III) in it. From this point on, all further operations are performed in a flow of nitrogen. The suspension of the acetate of iron (II) is first separated from the heavy particles of unreacted iron, then filtered, the precipitate is dried in a nitrogen atmosphere, and the filtrate is returned to repeat the process, together with the uploading of acetic acid and loaded a new portion of the basic acetate of iron (III), as well as compensation of losses of the liquid phase during the filtration process.

The output of acetate of iron (II) was 103,36 g, or about 99%.

The positive effect of the proposed solution consists in the following:

1. Two-thirds of the final product is formed from an oxidizing agent, which is to get the proper purity easier than powdered reduced iron.

2. No energy-intensive and slow stage of evaporation.

3. The process is conducted at room temperatures and is quite simple instruments in the om design.

4. As the product turns acetate anhydrous iron (II), the solubility of which in the environment of acetic acid and acetic anhydride is about 0,037 mol/kg or less, which implies the presence of its predominantly in the solid phase.

5. In the process not accumulate substances that inhibit it. Therefore detachable when filtering the liquid phase may be used multiple times in the repeated processes.

The method of obtaining acetate iron (II) interaction of metallic iron with acetic acid in the presence of an oxidizer, wherein the oxidizer agents use basic acetate of iron (III), and the process is conducted in the medium of acetic acid and acetic anhydride in a weight ratio in the initial loading of 5:1 at room temperature in the absence of air or in a nitrogen atmosphere, and the molar ratio of acetic acid: iron: basic acetate of iron (III) 10:8:1, with intensive mixing by shaking with a frequency of 2 Hz or a high-speed paddle stirrer of inert and durable plastic to depletion of basic acetate of iron (III), followed by the separation of the suspension of the acetate of iron (II) from unreacted iron powder by filtering and drying the precipitate in a nitrogen atmosphere, and returning the filtrate to repeat the process.



 

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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.

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2 ex

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The invention relates to the production of salts of acetic acid
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FIELD: organic chemistry, chemical technology.

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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.

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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

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