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Tower type continuous dehydration technique for trichloroacetaldehyde monohydrate

A technology for hydrating trichloroacetaldehyde and trichloroacetaldehyde, which is applied in directions such as separation/purification of carbonyl compounds, can solve the problems of long residence time of trichloroacetaldehyde, high degree of oxidation, low product yield, etc. High temperature oxidation and decomposition and other side reactions, good quality and high product yield

Inactive Publication Date: 2008-07-09
荆州沙隆达控股有限公司
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is that chloral stays in the kettle for a long time, is highly oxidized by concentrated sulfuric acid, and the product yield is low, and the material needs to go through two vaporization and condensation processes, and the production energy consumption is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Get chloral hydrate 300g (content 70%), control vaporization temperature 100 ℃, feed from the tower kettle of packed tower, tower body insulation 120 ℃, evenly add concentrated H 2 SO 4 180g, reaction time 15min, 210g fraction collected at the top of the tower, content 98%, yield 98%.

Embodiment 2

[0012] Get chloral hydrate 300g (content 70%), control vaporization temperature 150 ℃, feed from the tower kettle of plate tower, tower body insulation 100 ℃, add concentrated H evenly from the top of the tower 2 SO 4 180g, reaction time 10min, 214g fraction collected at the top of the tower, content 98%, yield 98.2%.

Embodiment 3

[0014] Get chloral hydrate 300g (content 70%), control vaporization temperature 130 ℃, feed from the tower kettle of packed tower, tower body insulation 110 ℃, evenly add concentrated H 2 SO 4 180g, reaction time 20min, 214g fraction collected at the top of the tower, content 98%, yield 98.2%.

[0015] The comparative test of the present invention and traditional tank type semi-continuous dehydration process is as follows:

[0016] Reaction time Reaction temperature Yield

[0017] Kettle semi-continuous dehydration process 1 120min 110℃ 94%

[0018] 2 90min 120℃ 94.5%

[0019] 3 60min 140℃ 94%

[0020] Continuous dehydration technology method 1 10min 120℃ 98%

[0021] 2 15min 110℃ 98.2%

[0022] 3 20min 120℃ 98.2%

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Abstract

Disclosed is a tower type continuous dewatering technology of chloral hydrate, technical characteristic of which is that dilute sulphuric acid is discharged out from the bottom of the tower, the chloral hydrate enters from a certain portion at the bottom of the tower, concentrated sulfuric acid enters from the top of the tower, and refined chloral is discharged out from the top of the tower. The whole process is the continuous dewatering operation and the technique is simple, fast and fluently, which realizes continuous dewatering of chloral hydrate with relatively less equipments and relatively low energy consumption. The technique can be controlled easily and operated relatively stably. Compared with other existing dewatering techniques, the invention not only can reduce investment of equipments, but also is small in area and low in energy consumption. Further, the invention can decrease dewatering cost of chloral hydrate obviously and improve product quality.

Description

Technical field: [0001] The invention relates to a dehydration method of chloral, in particular to a continuous dehydration method of hydrated chloral. Background technique: [0002] Chloral is an important raw material for the synthesis of dichlorvos and trichlorfon. Chloral is obtained by dehydrating chloral hydrate through concentrated sulfuric acid. At present, most of the industrial production in my country adopts the semi-continuous dehydration process of tank type. The disadvantages of this process are that chloral stays in the kettle for a long time, is highly oxidized by concentrated sulfuric acid, and the product yield is low, and the material needs to go through two vaporization and condensation processes, and the production energy consumption is high. Therefore invent a kind of continuous dehydration technology method of chloral hydrate, very beneficial to improve product yield and quality. Invention content: [0003] The purpose of the present invention is e...

Claims

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Application Information

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IPC IPC(8): C07C47/16C07C45/78
Inventor 何富春殷宏薛光才刘孝平杨光富王洪群戴锋成和武廖艳潘晖徐艳
Owner 荆州沙隆达控股有限公司
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