The method of obtaining tetrathionate of tetraethylammonium

IPC classes for russian patent The method of obtaining tetrathionate of tetraethylammonium (RU 2057135):

C07F13 - Compounds containing elements of the 7th Group of the Periodic System

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(57) Abstract:

Usage: in inorganic chemistry and to obtain tocomplex elements of the seventh group, in particular to obtain tetrathionate of tetraethylammonium, which can find application in organic synthesis. The inventive method, including the dissolution of the original substances and their interaction in an alcohol solution, ammonium perrhenate dissolved in ammonia-ethanol solution, and then injected aqueous solutions of hydroxide tetraethylammonium and ammonium polysulfide and through the reaction mixture miss the sulphide precipitate is filtered off and the mother liquor is returned to the beginning of the process. Yield 96%. 1 C. p. F.-ly.

The invention relates to inorganic chemistry, namely to receive tocomplex elements of the seventh group, in particular to a method for tetrathionate of tetraethylammonium.

Tetrathionate can be used as starting compounds for various polynuclear Homo - and heterometallic serosoderjaschei complexes of rhenium and catalysts based on them.

A method of obtaining tetrathionate tetrabutylammonium [(n-Bu₄N)ReS₄] consisting in shadowstrike potassium (KOH) and boil. The resulting mixture is filtered into a solution of tetrabutylammonium bromide deposited precipitate is filtered off. The yield of the target product 20% [1]
The disadvantages of the method are: low yield of the target product, a high consumption of reagents (up to 2 l of ammonia to 2 g Re₂O₇), the use of Re₂O₇expensive and unsustainable in the air due to the high hygroscopic substances.

Closest to the present invention is a method of obtaining tetrathionate of tetraethylammonium. Tetraethylammonium bromide dissolved in the metal solution of ammonium polysulfide and enter Re₂O₇. The mixture is heated, then the precipitate is filtered off and the filtrate is left in a closed vessel under argon. After 1-2 days the precipitated crystals filtered off. The yield of the target product is 71% [2]
The disadvantages of the method are: the complexity of the method due to the use of unstable air Re₂O₇the need for process in an inert atmosphere, labor-intensive process, requiring a lot of time to prepare a methanol solution of ammonium polysulfide, so as to obtain the necessary carefully dried methanol and dry ammonia and hydrogen sulfide. In addition to the what is the difficulty in recycling, obtained by carrying out this method.

The objective of the invention is to provide a simple, technologically advanced way to obtain a product with a practically quantitative yield, and to use available reagents that do not require pre-cleaning and resistant to air, to carry out the process with fewer reagents and reusing the mother liquor, which is very important for the environment and recycling.

The task is solved in that tetratogenic of tetraethylammonium get interaction derived tetraethylammonium with ammonium polysulfide and registertask reagent in the environment of the solvent, followed by separation of the target product, as derived tetraethylammonium hydroxide use of tetraethylammonium, as registertimer reagent use ammonium perrhenate and the process is conducted in an aqueous-ammonia-alcohol medium by sequential processing of ammonium perrhenate in the ammonia-ethanol solution aqueous solutions of hydroxide tetraethylammonium and ammonium polysulfide, and the subsequent transmission of hydrogen sulfide in the reaction mass resulting from the reaction of the target product is filtered off, and match isawanya instead of Re₂O₇simple reagent of ammonium perrhenate, dissolution of ammonium perrhenate in aqueous ammonia-ethanol solution, the introduction of aqueous solutions of hydroxide tetraethylammonium and ammonium polysulfide, passing through the reaction mixture of hydrogen sulfide, reusing the mother liquor, i.e., returning the mother liquor to the process.

This allows to simplify the method and to increase the yield of the target product to 95-96% which is especially important considering the high cost of rhenium.

As a source of reagent is used, the ammonium perrhenate NH₄ReO₄since this salt is soluble in ammonia-ethanol mixture and readily available. Dissolving salt in ammonia-ethanol solution, on the one hand, allows one to quickly and completely without heating to dissolve the original salt, and ethanol environment allows to avoid the formation of oxocomplexes that would defile the obtained product.

The use of ammonia solution contributes to the dissolution of ammonium perrhenate and serves the formation of ammonium sulfide by passing hydrogen sulfide (H₂S.

Introduction hydroxide tetraethylammonium [(C₂H₅)₄NOH] the resulting product, affordable and stable during storage, which allows to carry out the reaction under normal conditions and gives the opportunity not to contaminate the reaction mixture extraneous ions, as in the substitution of NH₄⁺on (C₂H₅)₄N⁺there is only the additional number of NH₄OH.

The use of the mother liquor may due to the fact that during the reaction consumes NH₄ReO₄(solid), H₂S (gas) and (C₂H₅)₄NOH (aqueous solution). All other reagents serve as a medium for education (C₂H₅)₄NReS₄. Thus, in the mother solution is added an aqueous solution (C₂H₅)₄NOH, however, the quantity (5 ml) practically does not change the volume of the mother liquor. The amount of ammonium perrhenate is determined by its solubility, and the introduction of a hydroxide of tetraethylammonium is abundant for a complete passage of the reaction.

Pass hydrogen sulfide through the mother solution due to the formation of sulfide in the ammonia-ethanol solution and substitution of oxygen in ReO₄^-the sulfur in the formation of the target product.

Thus, the use of the mother liquor allows the 95-96%
Industrial applicability is illustrated by examples.

The method is as follows.

To a solution of ammonium perrhenate in a mixture of ammonia-ethanol add the hydroxide of tetraethylammonium, ammonium polysulfide and within 5 min after the reaction mixture miss sulfide. After the reaction, the mixture is left for a day, the precipitation tetrathionate of tetraethylammonium separated by filtration, washed and dried. The resulting crystalline product precipitates dark purple color. The yield of the target product 95-96%
P R I m e R 1. 2 g of ammonium perrhenate dissolved in 30 ml of aqueous ammonia solution and 10 ml of 30% aqueous solution of hydroxide of tetraethylammonium. To the solution was added ethanol, a few milliliters of ammonium polysulfide and a saturated solution of hydrogen sulfide for 5 minutes at 24 h, the precipitation was filtered, washed with ethanol, ether and dried in vacuum. Received 3,15 g (C₂H₅)₄NReS₄. The output is 95.2%
Found, From 22.0; N 4,6; N 3,14; S 29,1; Re 41,0.

For C₈H₂₀NReS₄calculated From 21.6; H 4.5; N 3,15; S 28,9; Re 41,9.

The IR spectrum_Re-S482 cm-1.

Data of x-ray phase analysis are in good agreement with literature data, Polak and 10 ml of 30% aqueous solution of hydroxide of tetraethylammonium. To the solution was added ethanol, a few milliliters of ammonium polysulfide and a saturated solution of hydrogen sulfide for 5 minutes at 24 h, the precipitation was filtered, washed with ethanol, ether and dried in vacuum. Received 2.85 g (C₂H₅)₄NReS₄. Output 95.6% of
To the stock solution was added 1 g of ammonium perrhenate. The resulting solution was saturated with hydrogen sulfide for 5 minutes at 24 h, the precipitation was filtered. Obtained 1.6 g of product. The output 96%
P R I m e R 3. To the stock solution obtained according to example 2, was added 2.2 g of ammonium perrhenate and 5 ml of hydroxide tetraethylammonium. The resulting solution was saturated with hydrogen sulfide 5 minutes After 24 hours the precipitate was filtered. Obtained 3.5 g of product. Output 95.9% of
The method allows to obtain tetratogenic of tetraethylammonium, which can be used to produce polynuclear tocomplex rhenium and catalysts based on them.

1. The METHOD of OBTAINING TETRATHIONATE of TETRAETHYLAMMONIUM interaction derived tetraethylammonium with ammonium polysulfide and registertask reagent in the environment of the solvent, followed by separation of the target product, characterized in that as a derivative of tetraethylammonium use Hydra the water-ammonia-alcohol medium by sequential processing of perinata of ammonia in the ammonia-ethanol solution aqueous solutions of hydroxide tetraethylammonium and ammonium polysulfide and subsequent transmission of hydrogen sulfide in the reaction mass.

2. The method according to p. 1, characterized in that the resulting solid reaction, the target product is filtered off and the mother liquor is returned to the beginning of the process.