Method of producing iron (ii) fumarate

FIELD: chemistry.

SUBSTANCE: iron (II) fumarate can be used in different fields of chemical practice, in analytical control and in scientific research, through direct reaction of iron with fumaric acid in the presence of a catalyst, where the catalyst used is molecular iodine in amount of 0.025 to 0.1 mol/kg of the initial load, iron is taken in large excess in form of shells on the entire height of the reactor, false bottom and blade mixer, as well as in form of crushed cast iron and(or) reduced iron powder, the liquid phase solvent used is butylacetate, in which iodine and fumaric acid are at least partially dissolved, where fumaric acid is taken in amount of 0.8 to 1.2 mol/kg of the initial load, loading is done in the sequence: glass beads, liquid phase solvent, fumaric acid, iodine, and then crushed cast iron and(or) reduced iron powder; the process is started at room temperature and is carried out in a vertical type bead mill with ratio of mass of beads to mass of crushed cast iron and(or) reduced iron powder equal to 4:1, at temperature ranging from 18 to 45°C while bubbling air with flow rate of 0.95 l/min-kg of the liquid phase and using forced cooling and controlling using a sampling method until complete exhaustion of the loaded acid for formation of salt, after which stirring and cooling are stopped, the reaction mixture is separated from glass beads and unreacted crushed cast iron and(or) reduced iron powder and filtered, the residue is washed with butylacetate and taken for recrystallisation, and the filtrate and washing butylacetate are returned to the repeated process. Amount of acid used in extracting the product (without loss during purification) ranges from 89 to 96.5%, which depends on conditions for carrying out the process.

EFFECT: improved method of producing said product.

8 ex

 

The invention relates to a technology for obtaining salts of iron (II) and fumaric acid and can be used in various fields of chemical practice, analytical control and scientific research.

A method of obtaining fumarata iron (II) (patent GB 1048867, publ. 23.11.1966), according to which this salt is obtained by mixing a hot solution of fumaric acid (60-100°C) with metallic iron in the absence of air. The resulting perfumers separated by filtration, washed with hot water and dried under vacuum.

The disadvantages of this method are:

to use a hot solution of fumaric acid, the receipt of which is an independent stage, requiring some time and the supply of external heat;

- carrying out the process in the absence of air;

- drying the obtained salt under vacuum.

A method of obtaining anhydrous fumarata iron (II) (patent BE 658067, publ. 30.04.1965) interaction of metallic iron with excess fumaric acid at elevated temperatures in aqueous medium in the absence of air.

The disadvantages of this method are:

- in the above patent GB, and

- use of excess fumaric acid, which have to be separated from the reaction mixture and somewhere to use, and received the second salt is additionally clear from this reagent.

Closest to the claimed is a method for fumarata iron (II) (patent HU 40678, publ. 28.01.1987), according to which the interaction of fumaric acid and metallic iron lead in an inert reaction medium in the presence of a catalyst, which can be (in)organic acids or salts of iron at a temperature of 80-100°C.

The disadvantages of this method are:

1. Quite a high temperature process for the achievement of which requires external supply of heat and which cannot be maintained without such a connection.

2. Acid catalysts can react with iron to the formation of the corresponding salts, from which, as from residual acids have clear target product.

3. The need to create an inert reaction medium and to maintain it during the ongoing process.

The objective of the proposed solutions is to conduct a direct interaction of iron and its alloy with fumaric acid in a milder temperature conditions without the supply of external heat to achieve and maintain the desired temperature, without limitation, contact the reaction mixture with air or even when the bubbling of the last with a small flow, without the use of an inert reaction medium and excess fumaric acid, and mineral and carboxylic acids in which the quality of the catalysts.

This object is achieved in that the catalyst using molecular iodine in the amount of 0.025-0.1 mol/kg initial load, iron take in a large excess in the form of a shell over the entire height of the reactor, the false bottom and blade mixer, and also in the form of crushed iron and (or) powder recovered iron, as a solvent of the liquid phase using butyl acetate, in which dissolve, at least partially, iodine and fumaric acid, dosed at 0.8-1.2 mol/kg initial loading, the loading of lead in the sequence of glass beads with a liquid solvent phase, fumaric acid, iodine, and then crushed iron and (or) powder recovered iron; the process begins at room temperature and are in a bead mill, vertical type, the mass ratio of beads and crushed iron and (or) powder recovered iron 4:1 in the temperature range 18-45°C while bubbling air with a flow rate of 0.95 l/min·kg liquid phase and the use of forced cooling and the control method of sampling to practically complete consumption uploaded acid on the formation of the salt, after which the stirring and cooling to stop the reaction mixture is separated from the glass beads and unreacted crushed iron and (or) powder recovered iron and filtered, OS the dock washed with butyl acetate and sent for recrystallization, and the filtrate and wash butyl acetate return repeated the process.

Characteristics of raw materials.

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

Steel 45 GOST 1050-74

Cast iron grey brand midrange GOST 1412-70

Fumaric acid under MRTU 6-09-4881-67

Iodine crystal according to GOST 4159-79

Butyl acetate under MRTU 6-09-5743-68.

The process of the inventive method the following. Into a steel casing bead mill with the shell over the entire height, a false bottom and the high-speed paddle stirrer made of steel 45, load calculated quantity of glass beads, butyl acetate, fumaric acid, iodine, and crushed iron and (or) powder recovered iron. Include mechanical mixing and serving air sparging, stabilize the air flow injected forced cooling of the reactor through a liquid bath and water is supplied to the reverse cooling condenser. The moment when mechanical mixing mistaken for the beginning of the experiment. During the process, take samples of the reaction mixture, which determine the salt content of iron (II) and (III) and residual amounts of acid. The process is accompanied by a temperature rise in the reaction zone, which keep using forced cooling at the level of ≤45°C.

As soon as the results of the analysis of svidetel who are on almost the full expenditure of all loaded acid, cooling, air sparging and stirring is ceased, the reaction mixture (suspension) is separated from the glass beads and unreacted crushed metal and its alloy, and then filtered. The precipitate is washed with a solvent liquid phase and sent for recrystallization. And the filtrate and the washing solvent is returned in the reverse process.

Example 1

In having a fixed location on the frame frame bead mill, vertical type, the casing and the bottom of which is protected by a shell with an outer diameter of ~80 mm and a wall thickness of 3.5 mm and a false bottom with a thrust bearing for high-speed (1440 rpm) blade mixer with the width of the plate 71 mm and a height of 42 mm and a flange with a cover, in which there is a branch to a reflux-condenser, a stuffing box for mixer chamber for submerged bubbler, a pocket for thermocouple and a slot to insert the sampler, load 200 g of glass beads with a diameter of 1.8-2.7 mm, 173 g of butyl acetate, 23,21 g of fumaric acid, 3,81 g of iodine, and then 50 g of crushed gray cast iron with a maximum linear dimension of the particles less than 5 mm Include mechanical stirring, serves air sparging with a flow rate of 0.95 l/min·kg liquid phase, and the time taken for the beginning of the process. It starts immediately and is accompanied by an increase of temperature in the area reacts is I. Keep it with a large volume of water cooling bath. Initial temperature of water in it and specifies the upper limit of the temperature range in the reaction zone. In this example, it was 25°C. if the initial temperature of the water in the bath 18°C.

During the process, take samples of the reaction mixture, which analyze the content of salts of iron (II) and iron (III), separately iodide iron (II) and molecular iodine, and the remaining unreacted acid.

After 120 minutes from the beginning of the experiment, the analysis showed the salt content of iron (II) 0.98 mol/kg, and salts of iron (III) 0.015 mol/kg, a residual content of acid <0.01 mol/kg, which indicated almost complete termination of the process. Mixing and sparging of air is stopped, the reactor is disconnected from the lid and removed from the cooling bath and its contents poured into the container lattice with dimensions of 0.3×0.4 mm, which is within the field of a permanent magnet. On this lattice remains whole beads and virtually the entire captured the reaction mixture unreacted iron. Further they are removed from the grid and return to repeat the process.

The collected suspension of the reaction mixture is fed to vacuum filtration. The precipitate was washed with 50 g of butyl acetate to remove mainly iodide iron (II) and traces of molecular iodine, then e.g. the keys on further purification by recrystallization. As the filtrate, representing a solution of salts (including iodide) iron (II) and iron (III), as well as the washing solvent in return repeated the process.

The number of the selected product in this example (without taking into account losses during recrystallization) is rate of 0.193 mol. It is in the spending of 96.5% loaded acid to obtain.

Examples 2-8

The reactor, the solvent, the flow rate of air sparging, the weight of the initial reaction mixture and the crushed iron-bearing material in it, the boot order of the components, the sequence of operations during the inspection, the determination of the moment of termination of the process, the separation of a suspension of the product from the beads and unreacted metal alloy, separation of the product from the suspension and directions of the separated components of the reaction mixture similar to that described in example 1. Are fragmented nature of iron-containing material containing iodine and fumaric acid in the initial download. These differences and the results obtained are summarized in table (MF - trimmed grey cast iron; residence permit powder recovered iron).

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

1. As the iron-containing material is trimmed grey cast iron, which may be a waste of processing p is the itsindustry.

2. Used as a catalyst iodine less contaminates the product in comparison with mineral and carboxylic acids, as well as educated them or entered as a catalyst salts of iron. This is predetermined by the fact that resulting from the interaction of iodine with iron iodide, iron (II) up to 80-90% of its maximum (theoretically possible) number is located on the surface of iron or its alloy, i.e. where it is formed and where it is oxidized by oxygen in salt fumaric acid and molecular iodine, which immediately turns into FeI2. Falling in the reaction mixture of the iodide of iron (II) and (I2(traces) are in solution and basically go back in again with the filtrate and proryvnym solvent.

3. The bulk of the catalyst is returned to repeat the process without any special methods and techniques for concentration, separation and purification.

4. The proposed low-temperature process and can support operating temperature range due to its own heat and heat generated by the work of the bead mill.

5. Instrumentation process is simple and the equipment is not boiler-supervising.

6. The process of selective; formed as an impurity salt of iron (III) returns to repeat the process with the filtrate and proryvnym solvent is m, where has the ability to react with iron and turn into the target salt of iron (II).

7. Used solvent accessible and for the most part is returned to the process without requiring the use of special methods of cleaning, recycling, etc. In this case, a refund may be repeated.

The method of obtaining fumarata iron (II) by direct interaction of iron with fumaric acid in the presence of a catalyst, wherein the catalyst using molecular iodine in the amount of 0.025-0.1 mol/kg initial load, iron take in a large excess in the form of a shell over the entire height of the reactor, the false bottom and blade mixer, and also in the form of crushed iron and(or) powder recovered iron, as a solvent of the liquid phase using butyl acetate, in which is dissolved at least partially iodine and fumaric acid, dosed at 0.8-1.2 mol/kg source download, download lead in the sequence of glass beads with a liquid solvent phase, fumaric acid, iodine, and then crushed iron and(or) powder recovered iron; the process begins at room temperature and are in a bead mill, vertical type, the mass ratio of beads and crushed iron and(or) powder recovered iron 4:1 in the temperature range 18-45°C at barbeau is even air flow rate of 0.95 l/min·kg liquid phase and the use of forced cooling and the control method of sampling to practically complete consumption of the loaded acids for salt formation, after stirring and cooling to stop the reaction mixture is separated from the glass beads and unreacted crushed iron and(or) powder recovered iron and filtered, the precipitate washed with butyl acetate and sent for recrystallization, and the filtrate and wash butyl acetate return in the re process.



 

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9 ex

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6 cl, 3 dwg, 1 tbl, 68 ex

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EFFECT: obtaining target product of high degree of purity, which does not contain admixture anions and cations, which eliminates necessity of long washing of obtained sediment.

6 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention is related to improved method for preparation of manganese oxalate (II) by means of direct interaction of metal with acid in bead mill in presence of liquid phase, in which manganese and oxalic acid are loaded into bead mill in stoichiometric ratio in amount of 0.75-2.4 mole/kg of load at mass ratio of load and glass beads of 1:1.2, liquid phase dissolvent used is water or organic substance, or mixture of organic substances; loading is carried out in the following sequence: liquid phase dissolvent, acid, then metal; process is started at room temperature and is carried out under conditions of forced cooling in the temperature range of 18-39°C with control over procedure by sampling method to practically complete spend of loaded reagents for product making, afterwards mixing and cooling are terminated, suspension of reaction mixture is separated from glass beads and filtered, salt deposit is sent for product cleaning from traces of non-reacted metal, and filtrate is returned into repeated process.

EFFECT: method makes it possible to produce target product in absence of manganese dioxide and stimulating additive at temperatures close to room temperature.

2 cl, 13 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to improved method of salicylates of alkaline earth metals for application as detergents for lubricating materials. Method of obtaining alkylated salicytates of alkaline earth metals includes following stages: A) alkylating salicylic acid with linear α-olefin, containing, at last, 14 carbon atoms, in presence of water-free methane sulfonic acid with formation of oil-soluble alkylated salicylic acid; B) neutralisation of oil-soluble alkylated salicylic acid; C) excessive alkalisation of oil-soluble alkylated salicylic acid by carboxylating lime by means of CO2 in presence of oxygen-containing organic solvent and surface-active substance; D) filtration of stage (C) product; and E) removal of solvent by distillation. Alternatively, alkylsalicylic acid can be subjected to interaction with preliminary processed with alkali highly-alkaline sulfonate of earth alkaline metal, for instance, with calcium sulfonate, in order to obtain salicylate salts of earth alkaline metals with different per cent content of dispersed salts of alkaline earth metals carbonates. In claimed method it is not necessary to filter end product which is preferable doe industry.

EFFECT: obtaining salicylates of alkaline earth metals for application as detergents for lubricating materials.

8 cl, 4 ex

FIELD: chemistry.

SUBSTANCE: invention refers to organic chemistry, to chlororganic technology, specifically to advanced method of chloroacetic sodium salt production allowing for high quality with minimum power inputs. Method of chloroacetic sodium salt production (Na-CA) is characterised by that dry initial components that are soda ash (Na2CO3) and chloroacetic acid (CA) are continuously dispensed in stoichiometric ratio to desintegrator or dismembrator with linear speed of disk pins 30-150 m/s, where exposed to mechanochemical influence. Thereafter produced Na-CA is continuously supplied to drying. Produced in offered method Na-CA completely meets quality requirements of standard documents.

EFFECT: high quality products with minimum power inputs.

7 cl, 2 dwg, 3 ex, 1 tbl

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