Iron (ii) oxalate synthesis method

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing iron (II) oxalate by directly reacting metal with acid in the presence of atmospheric oxygen and a liquid phase while stirring. The process is carried out in a bead mill. The liquid phase solvent used is water with mass ratio of the liquid phase to glass beads equal to 1:1, content of oxalic acid in the initial load is between 0.5 and 2.0 mol/kg, and content of stimulating sodium chloride additive is between 0.02 and 0.10 mol/kg. Crushed grey cast iron which is stirred by a blade mixer is taken in amount of 30% of the mass of the rest of the load. The process is started and carried out at temperature in the interval from (50±2) to (93±2)°C while bubbling air under conditions for stabilising temperature using a heated liquid bath and controlling using a sample taking method and determination of content of iron (II) and (III) salts in the samples, and residual quantity of acid up to virtually complete conversion of the latter into salt. After that air bubbling, external heat supply for stabilising temperature and stirring are stopped. The suspension of the reaction mixture is separated from the glass beads and particles of unreacted metal alloy and filtered. The filtration residue is washed with distilled water and taken for further purification through recrystallisation, while the filtrate and the washing water are returned to the load for the repeated process. Iron (II) oxalate, which is separated from the reaction mixture by traditional filtering, is virtually the only product of conversion.

EFFECT: liquid phase used together with the sodium chloride additive can be repeatedly returned to the process.

10 ex, 1 tbl

 

The invention relates to the technology of production of oxalate of iron (II) and can be used in various fields of industrial production, scientific research and analytical control.

A known method of producing oxalate, iron (II), under which are the interaction of sulphate of iron (II) oxalate sodium (Pat. US 1899674). The resulting oxalate, iron (II) poorly soluble in water (220 ppm) and stands out from the reaction mixture by decanting or filtering.

The disadvantages of this method are:

1. The process is carried out by mixing two aqueous solutions in which water is the dominant mass component. After separation of the target salt it actually turns into waste, which need to be properly cleaned.

2. In the process of considering the interaction as a companion product formed sodium sulfate, which must be disposed of. Therefore, we need a suitable method such disposal.

3. And sodium oxalate, sulfate and iron (II) are products of a fairly deep processing of natural resources, which is quite acceptable for the laboratory, but is a very important factor in industrial production.

Closest to the claimed is a method for musk iron (III) with three anions salicia the Oh of the acid (U.S. Pat. Of the Russian Federation No. 2304575) by direct interaction of the metal with acid under stirring in the presence of oxygen as oxidant. As the liquid phase of the reaction mixture using a solution of salicylic acid or its mixture with the product in dimethylformamide to a concentration of acid 3,4-4.0 mol/kg of Iron taken in the form of a steel or cast-iron shell over the entire height of the reactor, the blades and shaft mechanical stirrer, and a floating stirrer powder recovered metal or of fractions of broken cast iron and broken steel shavings. The process begins and is carried out at a stirring and sparging air flow rate 3.9 to 5.4 l/min-kg load caused by heating the reaction mixture up to 80-90°C to accumulation of the product of the complex number 1,12-of 1.30 mol/kg. Upon reaching this point, the stirring and sparging of air is stopped, the slurry product is separated from the heavy particles of unreacted metal or alloy and filtered. The filtrate allow to cool down slowly to room temperature, after which it again filtered, the precipitated product is removed from the filters and sent to recrystallization, and the second filtrate is returned to repeat the process.

The disadvantages of this method are:

Salicylic acid is markedly weaker (PKand3,0 and 12.8) compared with oxalic (PKand1.3 and 4.3). Moreover, according to him the political nature are quite different acids. Therefore, there is no reason to believe that their interaction with iron is similar operations with similar performance characteristics of the latter.

2. Salicylic acid is prone to the formation of many complex compounds, which are dominated by the cation of iron (III). For oxalic acid is more typical of its metal salts. While there is no certainty that the target product is a salt of iron (III), but not the salt of iron (II).

3. Not necessarily that used in the cited method as solvent dimethylformamide would be not that best, but generally acceptable solvent for the interaction of oxalic acid with iron.

4. Do not cause any doubts significant differences in the physical characteristics of the products of the interaction of iron with salicylic acid and oxalic acid. This also applies to the solubility of the latter in different environments. Therefore, there may be different phases of accumulation of target products in the reaction mixtures, and further surgery for separation and purification of target products.

5. The process according to the known solution is carried out in conditions of self-heating of the reaction mixture up to 80 to 90°C. it is not necessary that the process of interaction of iron with oxalic acid will be the same exothermic and will maintain the operating temperature without the use of dive torches etc the and the external heat even in roll form.

The objective of the proposed solution is to find a solvent liquid phase and such conditions for direct interaction of oxalic acid with iron, in which almost the only product quantitative transformations loaded oxalic acid would be the oxalate of iron (II), predominantly accumulated in the form of a solid phase and separated from the rest of the reaction mixture by conventional filtering.

This object is achieved in that the process is carried out in a bead mill, as a solvent of the liquid phase using water when the mass ratio of the liquid phase and the glass beads of 1:1, the content of oxalic acid in the initial download from 0.5 to 2.0 mol/kg, and stimulating additives sodium chloride 0.02 to 0.1 mol/kg, a floating paddle stirrer trimmed grey cast iron take in the amount of 30% by weight of the rest of the boot process starts and is carried out in the temperature range(50±2)-(93±2)°when the bubbling of air temperature stabilization with by using a heated liquid bath and the control method of sampling and determination of contents of salts of iron (II) and (III), as well as residual amounts of acid up to almost complete conversion of the latter into salt, then sparging air supply external heat to stabilize the the temperature and the stirring stopped, the suspension of the reaction mixture is separated from the glass beads and particles of unreacted metal alloy and filtered, the residue on the filter is washed with distilled water and sent for further purification by recrystallization, and the filtrate and wash water is returned back to re-download process.

Characteristics of the raw materials used

Steel 45 GOST 1050-74.

Cast iron grey brand midrange GOST 1412-70.

Oxalic acid according to GOST 5873-68.

Sodium chloride according to GOST 4233-66.

Distilled water according to GOST 6709-72.

The process of the inventive method the following. In a ball mill with steel, stainless steel, protected along the entire height of the well adjacent the shell and a false bottom with a thrust bearing for the shaft end of the agitator of steel 45, a mechanical stirrer vane-type cover on the flange joint with access to a reflux-condenser, stuffing box and jacks for measuring the temperature of the bubbler and the sampler, load rated amount of the glass beads, distilled water, oxalic acid, sodium chloride, and crushed gray cast iron. Casing bead mill is placed in a massive liquid stabilizing bath, preheated to a temperature of 6-8°C below the working temperature of the process. Include mechanical the second stirring and serving air sparging. The time taken for the beginning of the process. Stabilize the air flow rate and temperature of the process at a given level and in this mode, hold the salt accumulation product in the form of suspended solid phase to the almost complete consumption of the loaded oxalic acid. The controls are a method of sampling the reaction mixture and the determination of the content of salts of iron (II) and (III) and the residual acid.

Upon completion of the air sparging and stirring is stopped, the reactor endure beyond the stabilizing bath, the reaction mixture is separated from the glass beads and particles of unreacted iron and then filtered. The precipitate is washed with a small amount of distilled water, removed from the filter and is directed to additional purification by recrystallization. And the filtrate and wash water containing trace amounts of unreacted acid, and dissolved salts of iron (II) and (III) and stimulating additive NaCl, return to the re-download process.

Example 1

In a ball mill, vertical type, the casing and the bottom of which is protected by a shell with an inner diameter of 79 mm and a wall thickness of 2.5 mm and a false bottom with a thrust bearing for high-speed (1560 rpm) paddle agitators are arranged crosswise at an angle of 90° four blades with SATRO is with shell 1.3 mm and a height of 44 mm, with flange connection with a cover of stainless steel with a thickness of 15 mm, which is the way at a reflux-condenser, stuffing box shaft mixer, socket for external bubbler, sampler and measure the temperature directly at the wall of the shell, load 200 g of glass beads, 174,2 g of distilled water, of 0.59 g of sodium chloride and 25,21 g containing 2 molecules of water of crystallization with oxalic acid. The reactor is put into place in the frame frame, combined with a lid, bring the preheated stabilization bath so that ~90% of the height of the reactor was heated fluid, include periodically stirring and after 13 min heat the contents to a temperature of 60°C. Insert submerged bubbler, serves a current of air through dasarathy hatch introduced 60 g of crushed gray cast iron, include mechanical mixing and the time taken for the beginning of the process. Stabilize the air flow and the temperature of the reaction mixture at 65±2°C and in this mode are getting salt to practically complete consumption uploaded acid. The controls are a method of sampling the reaction mixture and the determination of the content of salts of iron (II) and (III), as well as unreacted acid. In this case, 25, 50, 75, and committed to a 100% degree of conversion of CIS is the notes achieved respectively through 9, 32, 71 and 127 min from the beginning of the process.

At the last moment the stirring and sparging of air is stopped, the reactor is cut off from the cover and associated reverse condenser, removed from the socket frame frame and simultaneously stabilizing the temperature of the liquid bath, and the contents poured into the vessel at the entrance to which is placed in the field of a permanent magnet grid with hole sizes of 0.3×0,3 mm On this lattice is delayed glass beads and unreacted particles of iron, which are washed with 50 g of distilled water. Subsequently the washed beads and particles of iron with the specified lattice are removed and returned to the re-download process.

The separated suspension of the reaction mixture with the product serves to vacuum filtration. The filter cake is washed with wash water from the beads and particles of the alloy and sent for further purification by recrystallization. And the filtrate and wash water containing the main part is used as a stimulating additives of sodium chloride, and small amounts of salts of iron (II) and (III) and oxalic acid in return repeated the process.

The number of the selected product in this example 0,194 mol (excluding losses recrystallization). It is spending to obtain 97%downloaded acid.

Examples No. 2-10

The reactor, the nature of the reagents, solvent, liquid phase and stimulating supplements, weight of the initial reaction mixture and the crushed iron-bearing material in the boot, the boot order of the components, the sequence of operations for the control and determination of the moment of the termination process, the separation of the suspension of the reaction mixture from the beads and unreacted iron, the selection of its product and directions of the components of the separated reaction mixture similar to that described in example 1. Different concentrations of oxalic acid and sodium chloride in the initial download, and temperature of the process. These differences and the results obtained are presented in table.

Load characteristics, process and product yieldExample No.
2345678910
1234578910
The initial content of acid loading, mol/kg1,01,01,01,00,51,251,501,752,0
The initial NaCl content, mol/kg0,020,0350,0800,10,10,0670,020,050,10
The temperature of the process, °C75±175±175±150±275±158±193±290±280±2
The time to reach the degree of conversion (%) oxalic acid, min
251295467788
50392921243041354475
757863475850627189150
99 or more14398619575105115181203
The number of allocated product, mol
0,1900,1920,1940,1920,0930,2420,2920,3410,393
The degree of spending loaded acid in the isolated product, %
959697969397979898

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

1. The main m the SSA initial reagents goes to the weight of the target product. Related products (water and partly molecular hydrogen) have a small molecular weight, does not contaminate the target product, does not require the allocation and utilization, are not environmental pollutants.

2. Used to process the liquid phase can be repeatedly returned to repeat the process and the substance is not converted into waste water.

3. Together with the liquid phase in the re process is returned and the bulk is used as a stimulating additives of sodium chloride. And washing of the beads, particles of unreacted alloy of iron and then precipitate on the filter with distilled water help to reduce losses of such additives.

4. In technological terms, the proposed single-stage process. It uses the available raw material (an alloy of iron, oxygen), including waste from other industries (combat grey cast iron, sawdust etc). As stimulating additive is sodium chloride are also of natural origin.

5. The process is simple in relation to the hardware design does not contain boiler-supervising equipment, can be implemented in the chemicals industry standard equipment.

6. The process is moderately exothermic, is able to maintain the temperature at the working level due to its own heat. Intensive external heating need the look at first, i.e. before you start the main process.

The method of producing oxalate, iron (II) by direct interaction of the metal with acid in the presence of oxygen and a liquid phase under stirring, wherein the process is carried out in a bead mill, as a solvent of the liquid phase using water when the mass ratio of the liquid phase and the glass beads of 1:1, the content of oxalic acid in the initial download from 0.5 to 2.0 mol/kg, and stimulating additives sodium chloride 0.02 to 0.10 mol/kg, a floating paddle stirrer trimmed grey cast iron take in the amount of 30% by weight of the rest of the boot process starts and is carried out at a temperature in the interval(50±2)-(93±2)°when the bubbling of air temperature stabilization using the heated liquid baths and control method for sampling and determination of contents of salts of iron (II) and (III), as well as residual amounts of acid up to almost complete conversion of the latter into salt, then sparging air supply external heat to stabilize the temperature and the stirring stops, the suspension of the reaction mixture is separated from the glass beads and particles of unreacted metal alloy and filtered, the residue on the filter is washed with distilled water and sent for additional purification by recrystallization, and the filtrate and wash water return is amaut to load in the re process.



 

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12 cl, 7 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to the improved method for preparing nickel oxalate that can be used in preparing catalysts, ceramic materials and in manufacturing electric vacuum devices. Method involves preparing the reaction solution containing nickel (II) and oxalate, crystallization of product, separation of precipitate from solution and its drying. The reaction solution is prepared by mixing reagent as source of oxalate and spent solution from chemical nickel plating taken in the amount providing the mole ratio in the reaction solution nickel (II) : oxalate = 1.0:(0.8-2.8). Spent solution of chemical nickel plating contains as main components nickel (II), ligand for nickel (II), reducing agent and product of its oxidation. As spent solution of chemical nickel plating method involves using solution containing nickel (II), ligand for nickel (II), hypophosphite, phosphite as main components and pH value in the reaction solution is brought about from 2.5 to 7.5. As spent solution of chemical nickel plating method involves using solution containing nickel (II) and ligand for nickel (II) as main components. As a reducing agent method involves using substance taken among the group including hydrazine, borohydride, hydrazine borane, alkylaminoborane, dithionite, hydroxymethyl sulfinate, thiourea dioxide, product of reducing agent oxidation and pH value in the reaction solution is brought about 0.0 to 8.5. Invention provides reducing material consumptions for preparing nickel oxalate, expanded assortment of materials used for preparing nickel oxalate, utilization of manufacture waste, reduced cost of product and simultaneous utilization of the spent solution of chemical nickel plating representing toxic waste of manufacturing.

EFFECT: improved method for preparing.

16 cl, 19 ex

The invention relates to the field of chemical engineering of complex compounds, in particular, to a method for dihydrate dioxalate(II) ammonium composition (NH4)2Cu(C2O4)2·2H2O, which can be used for antibacterial treatment of water in the production of high-temperature superconductors, for preparation of electrolyte copper plating, as a fungicide and copper micronutrients in agriculture, to obtain copper catalysts
The invention relates to an improved process for the preparation of oxalate, copper (II), which can be used as a blue pigment in the production of high-temperature superconductors, to obtain copper catalysts

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

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