The way to obtain methyl ethyl

 

(57) Abstract:

Usage: methyl ethyl is used in the manufacture of ethyl fluid as a product in the industry of organic synthesis. The inventive reagent 1: ethanol, reagent 2: bromine and sulfur. The synthesis conditions: high temperature, presence of water. Bromine and sulfur is injected in the form of a solution in methyl-ethyl. Output per ethanol reaches 90% 1 C.p. f-crystals.

The invention relates to methods of producing methyl ethyl used in the production of ethyl fluid, and also as an intermediate in industrial organic synthesis.

A method of obtaining methyl ethyl (prototype) by treatment with ethyl alcohol solution of bromine and sulfur at elevated temperature by adding to the reaction mass of water in quantity sufficient to maintain the mass relationship of water and the resulting sulfuric acid (0,8-2,0):1 (A. with. N 1092149, class C 07 C 19/02, 17/6). You get a high quality product with the content of the basic substance to a 99.0-99.5% and high yield according to the bromine: up to 98.5-98.7 per cent

The disadvantage of this method is the necessity of using 20% excess of ethyl alcohol to compensate for its p is TBE byproducts diethyl ether, ethylene, which when interacting with bromine gives dibromethane, products resinification.

The aim of the invention is to increase the output of products ethyl alcohol 90%

This goal is achieved by the fact that methyl ethyl receive bromirovanii ethanol bromine in the presence of sulfur reducing agent, while the bromine is fed to the synthesis in the form of its solution in ethyl bromide with a concentration of 400-1200 g/L.

The synthesis is carried out at a temperature rising from room temperature up to the boiling temperature of the reaction mass, and the distillation of methyl ethyl from the reaction zone, and in the synthesis reactor is metered aqueous solution of ethyl alcohol and a solution of bromine and sulfur in methyl-ethyl. The decrease in the concentration supplied to the synthesis of bromine and increasing the amount evaporated from the reaction mass of methyl ethyl stabilizes the temperature of the process, which reduces the formation of by-products and, accordingly, to increase the selectivity of the process the synthesized alcohol and the product quality.

The use solution with a concentration of bromine over 1200 g/l leads to a decrease in product yield up to 94-95% according to the bromine and the selectivity of the use of alcohol, reduction to the mA and 32 g of sulfur in 1000 ml (1450 g) methyl ethyl (concentration of bromine 480 g/l) and add it to a mixture of 300 g of ethanol and 72 g of water in a period of 2.0 hours The temperature of the reaction mass support in the state of boiling to complete the distillation of methyl ethyl. The total synthesis time is 3.0-3.5 h, the temperature of the reaction mass to the end of the exposure reaches 100-105aboutC. eye-Catching methyl ethyl divert through the reflux condenser, condenses and is collected under the layer of water for washing away impurities ethyl alcohol and NVG.

Get 2097,5 g of methyl ethyl. The basic substance content of 99.5% Yield according to the bromine 99,0% ethyl alcohol 90.7 percent

P R I m m e R 2. The synthesis is carried out as in example 1, but for dissolving bromine use 400 ml (580 g) methyl ethyl (concentration of bromine 1200 g/l). Get 1200 g of methyl ethyl basic substance content rate of 99.0% Yield according to the bromine 94,8% ethyl alcohol 87,2%

P R I m e R 3. The synthesis is carried out according to example 2, however, the synthesis obtain 310 g of ethyl alcohol.

Get 1220 g of methyl ethyl basic substance content of 99.1% Yield according to the bromine of 97.8% ethyl alcohol 87.1% of

P R I m e R 4. The synthesis is carried out according to example 2, however, the synthesis using 320 g of ethyl alcohol. Get 1225 g of methyl ethyl basic substance content of 99.1% Yield according to the bromine 98,6% in ethyl alcohol 85,1%

P R I m e R 5. Synthesis exercise is.

The total synthesis time increases to 4-4,5 hours. Get 2388 g of methyl ethyl. The basic substance content of 99.4% Yield according to the bromine of 99.1% ethyl alcohol and 91.2%

P R I m e R 6. The synthesis is carried out as in example 1, but for dissolving bromine use 440 ml (638 g) methyl ethyl (concentration of bromine 1090 g/l). Get 1284 g of methyl ethyl basic substance content of 99.1% Yield according to the bromine 98,8% ethyl alcohol to 89.9%

1. The WAY to OBTAIN METHYL ETHYL by processing ethanol bromine and sulfur in the presence of water at elevated temperature, characterized in that the bromine and sulfur is injected in the form of a solution in methyl-ethyl.

2. The method according to p. 1, characterized in that use a solution of bromine in methyl-ethyl with a concentration of 400 to 1200 g/l, and sulfur taken in stoichiometric amounts based on the bromine.

 

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