Ferrous acetate preparation method

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

 

The invention relates to the technology of production of acetate of iron (II) and can be used in various fields of industrial and laboratory chemicals and analytical control.

A method of obtaining acetate mercury interaction of metallic mercury with peracetic acid formed from acetic acid and hydrogen peroxide directly into the reaction mixture in the presence of a catalyst (U.S. Pat. U.S. No. 2873289, CL 556-131, publ. 1960).

The disadvantage of it is that peracetic acid and hydrogen peroxide is too strong oxidants that in the presence of acetate of iron (II) is left as the target product and do not become a more stable salt of iron (III). Moreover, proposed in the patent the technology is quite complex and is based on the catalytic process, which always has high requirements to minimize the content of impurities in the system.

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

The disadvantages of this method are:

1. Relatively high process temperature at which the solubility of oxygen b the children is small even when used under high pressure.

2. Use instead of air, oxygen assumes certain conditions for safe conduct of the redox process.

3. Listed in the copyright certificate metals divalent state of the metal salts is the most stable and common, what can be said about the salts of divalent iron. For this reason it can be expected that a similar process mode for iron is hardly possible.

The purpose of this decision is to obtain the acetate of iron (II) in circumstances where the initial reagents are iron, acetic acid and oxygen in the air, while at lower temperatures and without using excessive pressure.

This object is achieved in that the process is conducted in two successive stages without changing the reaction apparatus, the break in time and dozagruzit reagents, and the first step as the oxidant used air mode sparging, and this step is carried out at intensive mechanical stirring with a high speed stirrer iron powder and acetic acid at a molar ratio of 5:1 with the addition of acetic anhydride in the amount of 4% by weight of loaded acid at a temperature of 17-25°to accumulate in the system and salts of iron (III) in an amount of 0.75 to 0.96 mol/kg, then the air supply replace for filing the zhota, add 4% by weight bootstrap acetic acid, acetic anhydride, increase the temperature to 35-40°and conducting the second stage of the process until complete consumption of the entire accumulated in the first phase of salt of iron (III) on the formation of salts of iron (II), which is in the form of a white suspension in the remaining liquid phase is separated from the heavy particles of unreacted iron, filtered and dried in a nitrogen atmosphere and formed during the filtration the filtrate is returned to the reactor to boot to re-process or used for any other purpose.

Characteristics of the raw materials used

Iron recovered in THE 6-09-2227-81

Acetic acid according to GOST 61-75

Acetic anhydride according to GOST 5815-77

The atmospheric air without any additional purification

The process of the inventive method the following. In a reactor equipped with a high speed stirrer vane type, reflux-condenser, a bubbler and a sampler, load rated amount of acetic acid, acetic anhydride and powdered iron. Include mechanical stirring, served on the air sparging and conduct the process at ambient temperature to accumulate in the reaction mixture a certain amount of salt of iron (III). The air is replaced with nitrogen, increase the temperature and continue the t stirring until when all accumulated in the first phase of the salt of iron (III) not to turn into a salt of iron (II). At this point, the stirring is stopped, allow heavy particles of unreacted iron to settle to the bottom, after which a white suspension of acetate of iron (II) is separated from the unreacted iron and is sent to the filtering. The precipitate is dried, and then dried to constant weight. When all this is done in a nitrogen atmosphere. Formed during the separation of the solid salt of acetate of iron (II), the filtrate is sent to the reactor at boot to re-process or used for any other purpose.

Example No. 1.

In the reactor volume 483 ml, equipped with a Teflon stirrer blade type (720 rpm), reflux-condenser, providing a free exit of the gas space of the reactor to the atmosphere, a bubbler and a sampler that allows sampling without stopping stirring, download 205,9 g glacial acetic acid, and 8.2 g of acetic anhydride and 38,44 g of powder recovered iron with a maximum linear particle size of not more than 0.6 mm, the Molar ratio of acid and reducing agent in the initial download 5:1. The initial temperature of 17°C. Include mechanical stirring and sparging with air flow rate of 0.23 l/min In this mode leads to accumulation of salt in the reaction mixture W is found in (III) in an amount of 0.96 mol/kg This happened through 139 minutes

Stopping stirring, replace the air with nitrogen, increase the temperature of the reaction mixture to 35°add to 8.2 g of acetic anhydride and periodically monitor the salt content of iron (II) and iron (III) in the reaction mixture. Through 87 min flow of the second stage of the analysis showed almost complete absence of salts of iron (III) in the reaction mixture.

Mixing stop, give 5 min for sedimentation and localization in the area of the spherical bottom of the reactor unreacted particles of iron, block the exit to the atmosphere of the feedback condenser and through which is near the bottom of the reactor side socket white suspension acetate iron (II) is sent to the node filtering. Automatically in this node is sent and the flow of nitrogen, which provides some drying of the precipitate on the filter. In the future, the residue is finally dried in an oven under nitrogen atmosphere. As the filtrate, representing a saturated solution of acetate of iron (II) in a mixture of acetic acid and acetic anhydride, is sent to the reactor at boot to re-process or to use a different purpose.

The dry weight of acetate of iron (II) to 56.1 g, a content of acetate of iron (II) in the filtrate and in the reactor 1,2, Thus, the product yield of 99.3%.

Example No. 2.

The reactor and it is equipment similar to that described in example 1. Volume 519 ml, the mixer rotation speed 1440 rpm Stirrer made of stainless steel.

Initial acetic acid 231,81 g of acetic anhydride 9,27 g, restored iron 43,26, the Initial temperature of 25°C. the air Flow rate of 0.27 l/min Through 103 min to conduct the process under stirring under these conditions, the salt content of iron in the reaction mixture was 0.75 mol/kg

Without stopping stirring replace the air with nitrogen, add 9,27 g of acetic anhydride, raise the temperature of the reaction mixture to 40°and after 79 minutes of the second phase in the reaction mixture were present only salt of iron (II).

The selection of a product similar to that described in example 1. The dry weight of acetate of iron (II) was 45.6 g and ˜2 g remained in the reactor and returned with the filtrate, i.e. the yield of 99.4%.

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

1. The process conditions are very mild, instrumentation is simple and does not require any special solutions.

2. Use available natural oxidant.

3. To download no foreign contaminants. Therefore, the purity of the product is fully determined by the purity of the used iron.

4. The selection of the product is simple filtration of the suspension.

The method of obtaining acetate is Eliza (II) interaction of the metal with acetic acid in the presence of an oxidant, characterized in that the process is conducted in two successive stages without changing the reaction apparatus, the break in time and dozagruzit reagents, and the first step as the oxidant used air mode sparging, and this step is carried out at intensive mechanical stirring with a high speed stirrer iron powder and acetic acid at a molar ratio of 5:1 with the addition of acetic anhydride in the amount of 4% by weight of loaded acid at a temperature of 17-25°to accumulate in the system and salts of iron (III) in an amount of 0.75 to 0.96 mol/kg, then the air supply is replaced by a flow of nitrogen, add 4% by weight bootstrap acetic acid, acetic anhydride, increase the temperature to 35-40°and conducting the second stage to the full expenditure of all accumulated in the first phase of salt of iron (III) on the formation of salts of iron (II), which is in the form of a white suspension in the remaining liquid phase is separated from the heavy particles of unreacted iron, filtered and dried in a nitrogen atmosphere and formed during the filtration the filtrate is returned to the reactor to boot to re-process or used for any other purpose.



 

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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.

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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.

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FIELD: chemical technology.

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FIELD: inorganic synthesis.

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

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7 cl, 5 tbl, 27 ex

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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.

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FIELD: chemical technology.

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3 cl, 2 tbl, 8 ex

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EFFECT: improved preparing method.

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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

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