Method for preparing manganese (ii) acetate

FIELD: chemical technology.

SUBSTANCE: invention relates to technology for synthesis of acetic acid inorganic salts. Method involves interaction of metallic manganese or its dioxide with acetic acid in the presence of oxidizing agent. Process is carried out in beaded mill of vertical type fitted with reflux cooling-condenser, high-speed blade mixer and glass beads as grinding agent loaded in the mass ratio to liquid phase = 1.5:1. Liquid phase represents glacial acid solution in ethylcellosolve, ethylene glycol, 1,4-dioxane, isoamyl alcohol and n-butyl alcohol as a solvent. The concentration of acid in liquid phase is 3.4-4 mole/kg. Then method involves loading iodine in the amount 0.025-0.070 mole/kg of liquid phase, metallic manganese and manganese dioxide in the mole ratio = 2:1 and taken in the amount 11.8% of liquid phase mass. The process starts at room temperature and carries out under self-heating condition to 30-38°C to practically complete consumption of manganese dioxide. Prepared salt suspension is separated from beads and unreacted manganese and filtered off. Filtrate is recovered to the repeated process and prepared precipitate is purified by recrystallization. Invention provides simplifying method using available raw and in low waste of the process.

EFFECT: improved method of synthesis.

3 cl, 9 ex

 

The invention relates to the technology of production of manganese salt and a carboxylic acid, in particular acetic acid, and can be used in various fields of industrial and laboratory chemicals and analytical control.

It is known that in the system iron-carboxylic acid-iodine oxide iron (III)-organic solvent flows through a series of chemical reactions, including circular, the primary end product of which is a salt of carboxylic acid. The main supplier of the specified cation salt is a metal oxide, while the share of metal depending on the nature of the oxide is only about 25-33% (Amiano, Sportwhat, Dosatore. A circular stage in the processes of production of iron salts of carboxylic acids. News of the Kursk state technical University, 2004, №1 (12). S-98).

The disadvantage of this approach is that the selected conditions, the main product of the transformation is a salt of iron (III), and to obtain a salt of divalent metal needs either a specially selected process conditions (which might not always), or additional offline restore process trivalent metal in the divalent.

Closest to the claimed is a method of producing acetate iron (II) (RU 2259994 C1, 10.09.2005 on application No. 2004104495/04 from 1.02.05), whereby the interaction of iron, oxide of Fe2About3or Fe3O4with iodine and acetic acid is carried out in a bead mill, vertical type with high-speed mechanical stirrer and a reflux-condenser, with glass beads in a mass ratio of liquid phase loading of 1:1 in a nitrogen atmosphere in the presence of acetic anhydride as a dehydrating and stimulating supplements at 80° with periodic sampling of the solid phase of the product by filtration in a nitrogen atmosphere, and returning the filtrate to repeat the process.

The disadvantages of this method are:

1. The process and selection of product in a nitrogen atmosphere, which significantly complicate and instrumentation of process and execution of the latter.

2. The use of hard and maintaining a virtually anhydrous medium, not only initially but throughout the process.

3. The process at 80°. At this temperature volatility and acetic acid, and acetic anhydride become apparent that requires working effectively reverse condenser, as well as traps and other measures to ensure comfortable conditions for staff.

4. No download more high-boiling organic solvent in the solution whose relative is eucast acetic acid significantly be decreased.

5. Suck is not necessary that the model method of producing iron acetate can be used when replacing iron and its oxide to manganese dioxide and this metal whose properties and dioxide, and salt-product is significantly different from the properties of iron and its oxide and acetate.

The objective of the proposed solutions is to obtain manganese acetate (II) of manganese metal and its oxide is similar in meaning to the above process with similar hardware design.

This object is achieved in that the process is carried out in a bead mill of the upright type, not requiring the supply of external heat, the loading of manganese metal and manganese dioxide is produced in a molar ratio of 2:1 in the amount of 11.8% by weight of the liquid phase, the liquid phase of the system consists of an organic solvent and acetic acid with a concentration of 3,4÷5 mol/kg and dosed in a mass ratio of glass beads of 1:1.5, in the liquid phase of the system dissolve the iodine in the amount of 0.025-0.07 mol/kg liquid phase, the loading is carried out in sequence: liquid phase or separate its components, iodine, metal and manganese dioxide; the process begins at room temperature and lead to the almost complete consumption of dioxide obtained a suspension of the salt is separated from the main part of the unreacted metal and Stekla the aqueous beads and sent for filtration, the precipitated salt is cleaned from impurities of the metal and its oxide by recrystallization, and the filtrate is directed to repeat the process.

The organic solvent used ethyl cellosolve, ethylene glycol, 1,4-dioxane, isoamyl and n-butyl alcohols.

And the presence in the liquid phase system of water up to 4 wt.% practically does not affect the characteristics of the process.

Characteristics of the raw materials used

Manganese reactive GOST 6008-90.

Manganese dioxide according to GOST 4470-79.

Iodine crystal according to GOST 4159-79.

Acetic acid according to GOST 61-75.

The ethyl cellosolve according to GOST 8313-88.

Ethylene glycol according to GOST 10164-75.

n-butyl alcohol according to GOST 6006-78.

Isoamyl alcohol according to GOST 5830-70.

1,4-Dioxaspiro 10455-80.

The process of the inventive method the following. In ball mill vertical type with glass enclosure, a high-speed stirrer is made of Teflon or other inert and durable plastic and with a reflux-condenser injected glass beads, pre-cooked liquid phase or its components separately, iodine, manganese and manganese dioxide. Include mechanical stirring, and the time taken for the beginning of the process. During the process without stopping stirring take samples of the reaction mixture, which determine the salt content of the East and the exact amounts of acetic acid and manganese dioxide. As soon as the bulk of the manganese dioxide is consumed, stop stirring, the reaction mixture is separated from the glass beads and the main mass of the heavy plates and particles of manganese, after which it sent for filtering. The filtrate, representing a saturated solution of manganese acetate in a mixture of solvent and acetic acid, analyze, and return in the re process. And solid phase are sent to clean salt from impurities in the hot filtration and recrystallization.

Example No. 1.

In a ball mill with glass casing inner diameter of 63.7 mm and height 159 mm with Teflon paddle stirrer, spaced from the bottom of the reactor at 0.3 mm, and a reflux-condenser load 250 g of glass beads with a diameter of 0.9-1.8 mm and 167 g of a solution of acetic acid in ethyl cellosolve. The concentration of acid 3.4 mol/kg Then enter 11 g of manganese metal, 8.7 g of manganese dioxide and 1.27 g of iodine. Include mechanical stirring (1440 rpm) and the time taken for the beginning of the process. The temperature in the reaction zone at this point 21°C. during the process, take samples of the reaction mixture and the results of the analysis determine the degree of conversion of the manganese dioxide. After 113 minutes, it was over 99%. The temperature of the reaction mixture at this point was reached 33°C. Stirring is stopped and separate the reaction mass from the beads, passing it through a kind of filter with grid with cells of 0.4·0.5 mm instead of filtering partition. This operation is performed so that the main mass of the heavy particles of manganese remained at the bottom bead mill and beads. The last without any rinse immediately return to the ball mill, and the suspension is very slow settling of salt in the number of 179 g filter. The filtrate is returned to repeat the process, and the solid mass is recrystallized from aqueous acetic acid and acetate of manganese. Finally, 43,3 g Mn(ASON3)2·4H2O.

Examples No. 2-9.

The reaction apparatus, the loading of the beads and the liquid phase, the dosage of manganese and manganese dioxide, the sequence of operations when downloading, the process and the product selection is similar to that described in example 1. Different concentration of acetic acid in the liquid phase, the nature of the solvent and iodine. The results obtained are summarized in the table. Legend: solvents EC - ethyl cellosolve, EG - ethylene glycol, 1,4D - 1,4-dioxane, IAS - isoamyl alcohol, NBS is n-butyl alcohol, RV - water reaction.

td align="center"> 3 74
Table
Characteristics of the processExample No.
2456789
The nature of the solvent liquid phaseEH1,4 DIASNBSECECECEC
The concentration of acetic acid in the liquid phase, mol/kg3,43,43,43,44,14,54,55,0
Dosage of iodine, mol/kg liquid phase0,0500,0520,0530,0510,0700,0420,0610,025
The water content in the reaction mixture, wt.%PB (˜2)PB (˜2)PB (˜2)PB (˜2)PB+0,5PB+1,0PB+1,5PB+2,0
Temperature, °With: start process1719151721201918
end3330362538293226
The process duration, min981251725410385157
Unloaded the suspension of the reaction mixture, g184175177168183177178175
The obtained salt after recrystallization (*4H2Oh)44,244,742,1to 38.3to 45.444,242,841,7

The positive effect of the proposed solutions.

1. The method is quite simple to perform, does not require external supply of heat and focused on readily available raw materials. Approximately half of the accumulated salt raw material is manganese dioxide, which is the natural connection.

2. Instrumentation process is simple and does not contain boiler-supervising equipment. This process can be successfully held in the low variant. It is not formed and does not accumulate any unwanted inhibitors that allows for the subsequent series in the apparatus filled with dead zones and not to lose the reaction mixture for this reason. There are no restrictions on the return of the spent liquid phase and unreacted metal and dioxide in the re process.

3. Pretty simple cleaning with whom or from solids and recrystallization reduce losses at this stage to a minimum.

1. A method of producing manganese acetate (II) by direct interaction of the metal and manganese dioxide with acetic acid in the presence of additives iodine as oxidant in a bead mill, vertical type with a reflux-condenser, a high-speed paddle stirrer and glass beads as pereirago agent, characterized in that the loading of manganese metal and manganese dioxide is produced in a molar ratio of 2:1 in the amount of 11.8% by weight of the liquid phase, the liquid phase of the system consists of an organic solvent and acetic acid with a concentration of 3,4÷5 mol/kg and dosed in a mass ratio with glass beads 1:1.5, in the liquid phase of the system dissolve the iodine in the amount of 0.025-0,070 mol/kg liquid phase, the loading is carried out in sequence: liquid phase or its components separately, iodine, metal and manganese dioxide; the process begins at room temperature and lead to the almost complete consumption of dioxide obtained a suspension of the salt is separated from the main part of the unreacted metal and glass beads, and sent to the filtration, the precipitated salt is cleaned from impurities of the metal and its oxide by recrystallization, and the filtrate is directed to repeat the process.

2. The method according to claim 1, characterized in that the organic solvent used, etincelle is ALW, ethylene glycol, 1,4-dioxane, isoamyl and n-butyl alcohols.

3. The method according to claim 1, characterized in that the presence in the liquid phase system of water up to 4 wt.% practically does not affect the characteristics of the process.



 

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14 cl, 5 ex

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