SU579266A1 - Method of preparing ethyl bromide - Google Patents

Description

The invention relates to a process for the production of ethyl bromide used in the production of ethyl liquid and also as an intermediate in the main organic synthesis industry. A known method of producing ethyl ethyl by treatment of ethyl alcohol with a solution of bromine and sulfur in the presence of sulfuric acid IJll. In this case, a solution of sulfur in bromine is added to a mixture of ethyl alcohol and sulfuric acid and the reaction is carried out at boiling. The process proceeds according to the schemes SgBP + SBrj + ISO ttgOft -l2 .jH5Br H-2H2 $ 04 - (- 4H20 As sulfuric acid and water accumulate in the reaction mass of sulfur in bromine decreases, and after about one third of the initial amount reacts alcohol, separation of the reaction mass occurs. The process becomes heterogeneous, and even with vigorous stirring the rate of synthesis decreases dramatically. The duration of one synthesis operation increases to 24-36 hours, removal of the product is 0.05-0.08 kg / liter. The disadvantages of this method are low production. Duration and impossibility of carrying out the process in a continuous way. To improve the process technology and carry it out in a continuous way, a solution of bromine and sulfur is proposed to be mixed with ethyl alcohol and the resulting mixture is added to sulfuric acid. Usually, the process is carried out at 85- .. in a continuous way is 0.61, 0 kg / l.h., i.e. 10-20 times more than when the process is conducted in a known manner. Example 1. In a mixer, continuously substitute a 30.93 g / h sulfur solution (1.94 g) in bromine (28.99 g) and 20.07 g / h ethyl alcohol. The resulting heated mixture is fed to a reactor containing 50 ml of diluted 45% sulfuric acid mixed with ethyl alcohol heated to 105 °. Ethyl bromide is continuously distilled from the reactor, which is purified and condensed. The waste reaction mixture of sulfuric acid condensate containing ethanol mixed with, -

Use 30.8 g / h {98% of stoichiometry based on the loadable grade) of ethyl bromide. With product m 1 kg /,

Example. 12.04 kg / h of a solution of sulfur (0.75 kg} in bromine (11.29 kg) and 7.75 kg / h1 of ETHYL alcohol) are continuously mixed into the gel-gelb. The resulting heated mixture is fed to the first stage of the reactor, containing heated to 89-95 with diluted 4j% sulfuric acid. In the first stage, the reaction mass flows into the second, where the temperature is maintained at 105-107 ° C. The bromide is not completed here. From the two stages of the reactor, the Irimalite is continuously distilled, which is purified and condensed,

In the second stage, the spent reaction mixture was continuously withdrawn with a dilute sulfuric acid with an admixture of ethyl alcohol.

Poluagat 14.95 kg / h (97% of stoichiometry n per loaded

bromine) ethyl bromide. Removal of the product 0.6 kg / l “hour.

Claims (2)

Invention Formula A method for the preparation of ethyl bromide and ethanol with solution and sulfur at a different temperature in the presence of sulfuric acid, which is different from the fact that, in order to improve the technological process of its process, its solution is continuously mixed: ethyl alcohol and the resulting mixture is added to sulfuric acid. 2. The method of pop, 1, otlichayusi and and with y & l that the process is conducted at 85-1. Sources of information taken during the examination li US patent 2359828, cl. 260 € 52; 10.10.44.