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Preparation method of tert-butyl chloride

A technology of tert-butyl chloride and tert-butanol, which is applied in the field of preparation of tert-butyl chloride, can solve the problems of low reaction yield, high equipment investment, complex production process, etc., and achieves improved yield, less equipment investment, The effect of simple production process

Inactive Publication Date: 2016-03-16
JINAN CHENGHUI SHUANGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This prior art production process is more complicated, and equipment investment is high; The yield of reaction is lower

Method used

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  • Preparation method of tert-butyl chloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 200 grams of tert-butanol into a 1000ml reaction flask, stir, then add 400 grams of concentrated hydrochloric acid, 200 g of sodium chloride, control the temperature in a water bath at 50°C, stir and react for 5 hours, let stand for the first layering, and separate the water layer. After neutralizing the organic layer obtained by the first layering with 10 g of sodium hydroxide, let it stand for the second layering, separate the water layer, add 40 g of sodium sulfate to the organic layer obtained for the second layering, and dry it. After 1h, the desiccant was filtered off and distilled to obtain 240g of tert-butyl chloride. Yield 96%, GC99.7%.

Embodiment 2

[0026] Add 200 grams of tert-butanol into a 1000ml reaction flask, stir, then add 400 grams of concentrated sulfuric acid, 200 g of sodium chloride, control the temperature in a water bath at 60°C, stir and react for 7 hours, let stand for the first layering, and separate the water layer. After the organic layer obtained by the first layering was neutralized with 10 g of sodium carbonate, it was left to stand for the second layering, and the water layer was separated, and the organic layer obtained by the second layering was added with 50 g of sodium sulfate to dry. After drying for 1 h, the desiccant was filtered off and distilled to obtain 237 g of tert-butyl chloride. Yield 95%, GC99.8%.

Embodiment 3

[0028] Add 200 grams of tert-butanol into a 1000ml reaction flask, stir, then add 350 grams of glacial acetic acid, 200 g of calcium chloride, control the temperature in a water bath at 55°C, stir and react for 8 hours, let stand for the first layering, and separate the water layer. After the organic layer obtained by the first layering was neutralized with 10 g of sodium hydroxide, it was left to stand for the second layering, and the water layer was separated, and the organic layer obtained by the second layering was added with 40 g of calcium chloride to dry. After drying for 1 h, the desiccant was filtered off and distilled to obtain 240.3 g of tert-butyl chloride. Yield 96.2%, GC99.8%.

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Abstract

The invention discloses a preparation method of tert-butyl chloride. The tert-butyl chloride is synthesized through a chlorination reaction of tert-butyl alcohol under the catalysis of a metal chloride. The metal chloride is added as a catalyst in the preparation method, so the method has the advantages of simple production process, less device investment, realization of the reaction rate reaching 95% or above, and realization of the purity of a gas phase reaching 99.5% or above.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of tert-butyl chloride. Background technique [0002] Chlorinated alkanes are important organic chemical intermediates, which play a very important role in various industries such as medicine, pesticides and coatings. At present, the domestic production capacity of tert-butyl chloride is relatively small, and there are many manufacturers but small scale. The production process of this prior art is relatively complicated, and the equipment investment is high; the yield of the reaction is low. Contents of the invention [0003] Purpose of the present invention is exactly to provide a kind of preparation method of tert-butyl chloride for the defect of above-mentioned existence. The invention adopts tert-butanol to undergo chlorination reaction under the condition of metal chloride catalysis to synthesize tert-butyl chloride. The preparation metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/16C07C19/01
CPCC07C17/16
Inventor 刘玉凤胡俊峰李春杰刘凯唐铎
Owner JINAN CHENGHUI SHUANGDA CHEM
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