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.
FIELD: organic synthesis catalysts.
SUBSTANCE: catalyst is prepared from allyl chloride production wastes comprising 30-50% 1,3-dichloropropenes, 30-60% 1,2-dichloropropane, and 3-5% 1,2,3-trichloropropane, which are treated at 5-10°C with 30-50% dimethylamine aqueous solution in such amount as to ensure stoichiometric ratio of dimethylamine with respect to 1,3-dichloropropenes. Resulting mixture is held at 20-25°C for 0.5-1.0 h and then 40-44 sodium hydroxide solution is added in stoichiometric amount regarding dimethylamine, after which clarified waste is added to dimethylamine at 60-70°C and stirring in amount ensuring stoichiometric ratio of dimethylamine to 1,3-dichloropropenes contained in clarified waste. Mixture is aged for 2-3 h, organic phase is separated, and remaining interaction phase is supplemented by C1-C4-alcohol or benzyl alcohol at alcohol-to-dimethylamine molar ratio 1:(1-3).
EFFECT: reduced expenses on starting materials.
2 cl, 3 ex
FIELD: chlororganic chemistry.
SUBSTANCE: invention relates to hydrochlorination catalyst containing aluminum η-oxide, doped with cesium chloride. Also method for methanol hydrochlorination in vapor phase using claimed catalyst is disclosed.
EFFECT: decreased selectivity to dimethyl ether and inhibited coke deposition on working catalyst.
16 cl, 6 tbl, 1 dwg, 20 ex
FIELD: industrial organic synthesis.
SUBSTANCE: process involves interaction of carbon tetrachloride with methanol in gas phase at elevated temperature in fixed-bed reactor accommodating two heterogeneous contact beds with different active ingredient concentrations, said active ingredient being zinc chloride deposited on solid carrier. Process can be carried out in presence of hydrogen chloride and/or water additives.
EFFECT: increased specific output of the process and lifetime of catalyst.
1 dwg, 3 tbl, 7 ex
SUBSTANCE: catalyst contains zinc chloride and carrier - porous granulated carbon-carbonic composition material based on pyrocarbon and nanodispersed carbon with specific surface by "БЭТ" 350-650 m2/g and total pore volume by water 0.55-0.85 cm3/g. Described is method of preparation of catalyst described above, which is prepared by impregnating carrier with water or hydrochloric acid solution of zinc chloride in two stages: zinc chloride sorption by carrier from water solution at temperature 15-25°C and evaporation of remaining part of solution at temperature 80-100°C. Also described is process on obtaining methylchloride by catalytic hydrochlorating of methanol, which is carried out in continuous reactor at temperature 140-200°C and contact time 0.6-1.11 s in presence of described above catalyst.
EFFECT: complete methanol conversion and complete selectivity to methylchloride.
7 cl, 6 ex, 4 dwg
SUBSTANCE: invention relates to a method of converting organochloride wastes containing tetrachloromethane to methyl chloride by reacting organochloride wastes with methanol at high temperature in a gas phase in a cascade consisting of at least two series-connected reactors, by periodically redistributing the stream of the initial mixture to the cascade reactors. All reactors have at least two heterogeneous contact layers with different concentration of the active ingredient which is zinc chloride deposited on a solid support. The process is preferably carried out in the presence of hydrogen chloride additive and/or water.
EFFECT: longer service life of catalyst.
2 cl, 2 dwg, 1 tbl, 5 ex
SUBSTANCE: methyl chloride synthesis method involves reacting methanol with hydrogen chloride in a synthesis reactor to obtain a vapour-gas mixture containing methyl chloride, and extraction of methyl chloride from vapour-gas mixture via partial condensation, followed by washing with initial methanol which is then fed into the synthesis reactor, and distillation purification where methyl chloride is extracted in form of a distillate. The initial methanol is fed into the system in three streams, wherein a stream A is fed for washing, stream B is fed for distillation purification and the remaining stream C is fed directly into the synthesis reactor. The ratio of stream A to the overall stream (A+B+C) of the initial methanol is between 0.1 and 0.5; the ratio of stream B is between 0.3 and 0.7; the ratio of stream C is between 0.05 and 0.5.
EFFECT: highly efficient process owing to avoiding recycling the desired product into the synthesis reactor.
5 cl, 1 dwg, 2 ex
SUBSTANCE: invention relates to a method of producing methyl chloride, which involves reacting methanol with hydrogen chloride in a synthesis reactor to obtain a vapour-gas mixture and partial condensation thereof, where methyl chloride is removed from the system in vapour form. The condensate is fed into a fractionation column using calcium chloride as an agent which decomposes the hydrochloric acid azeotrope. The still liquor from the column is fed for evaporation of water, which is removed from the process, and the evaporated still liquor is returned into the column at the feed level, wherein the vapour-gas stream collected from the top of the column is returned into the synthesis reactor, and the still liquor is partially removed from the system while simultaneously feeding fresh aqueous calcium chloride solution into the system. The method is characterised by that the still liquor is neutralised with an aqueous suspension of calcium hydroxide before evaporation to pH 6.5-8, and then clarified.
EFFECT: method which enables production with more complete recycling of hydrogen chloride and also enables to recycle chloride and salt wastes from other processes of an organosilicon complex, while preventing loss of hydrogen chloride and formation of waste water.
6 cl, 4 ex, 1 dwg
SUBSTANCE: invention relates to a method of producing perfluoroalkyl bromide from triphenylphosphine dibromide, obtained by reacting triphenylphosphine with bromine in acetonitrile at 0 °C, and 1,1,3-H-perfluoroheptanol at temperature of 170–180 °C for 90 minutes.
EFFECT: easy implementation, replacing original toxic raw material, while maintaining high output of end product.
1 cl, 1 tbl, 3 ex
SUBSTANCE: invention relates to organic chemistry, in particular, to a method of producing bromocyclohexane, widely used in chemical and pharmaceutical industry. Method comprises producing bromocyclohexane by reacting cyclohexanol with a bromating agent while heating. Brominating agent used is (45–48)% hydrobromic acid in presence of benzene with volume ratio of acid to benzene 1:0.75 and molar ratio acid to cyclohexanol 3.5:1, reaction mass is held for 4 hours with simultaneous distillation of benzene-water azeotrope at a temperature of 70–72 °C and returning benzene to reaction medium, and bromocyclohexane is separated from benzene fraction by distillation.
EFFECT: implementation of method ensures high output bromocyclohexane in bromation of cyclohexanol, reduces amount of wastes, as well as setting up recycling during synthesis of bromocyclohexane.
1 cl, 2 dwg, 1 ex