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Method for recovery and purification of sulfoxide chloride in acyl chloride production

A technology of thionyl chloride and purification method, applied in the direction of sulfur and halogen compounds, etc., can solve the problems of unusable, low purity, etc.

Inactive Publication Date: 2013-03-27
YANTAI TAYHO ADVANCED MATERIALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The recovered thionyl chloride usually contains isophthaloyl chloride, isophthalic acid, N,N-dimethylformamide, sulfur monochloride, sulfur dichloride and other impurities, and the color is dark yellow , the active ingredient of thionyl chloride is about 90%. Due to its dark color and low purity, it cannot be used any longer.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 1 ton of reclaimed thionyl chloride in still 1, steam heating, the gas phase temperature of thionyl chloride reaches about 74 ℃ and reflux transfers to still 2, a small amount of heavy boiling point substances remain in still 1. Add 22 kilograms of sulfur powder and 28 kilograms of gac in the distillation still 2, heat and reflux for 8 hours, and the sulfur oxychloride steam temperature reaches 74 ℃ and transfers to the collecting still. The obtained thionyl chloride had a purity of 98.5%, and a total of 780 kg of finished products were collected.

Embodiment 2

[0019] Add 1.7 t of recovered thionyl chloride into distillation still 1, and heat it with steam. When the temperature of the thionyl chloride steam reaches about 74° C., it is refluxed and transferred to still 2. A small amount of heavy boiling point substances remain in still 1. Add 36kg of sulfur powder and 48kg of activated carbon to the distillation kettle 2, heat to reflux for 8h, and the temperature of the thionyl chloride vapor reaches 74°C and is transferred into the collection kettle. The obtained thionyl chloride had a purity of 98.5%, and a total of 1330 kg of finished products were collected.

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PUM

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Abstract

The invention relates to a method for recovery and purification of sulfoxide chloride in acyl chloride production, which comprises the following steps of: implementing primary purification by a distilling way; converting sulfur dichloride which is difficult to separate into sulfur chloride which is easy to remove by sulfur powder; and adsorbing other colored components by active carbon; and obtaining pure sulfoxide chloride which reaches three-level color degree. The method disclosed by the invention can effectively recover the sulfoxide chloride, and is high in recovery rate, good in quality, safe in process and easy in control; the purified sulfoxide chloride can reach 98.5% in purity and three-level color degree in color.

Description

technical field [0001] The invention relates to a method for recovering and purifying thionyl chloride in the production of acid chlorides. Background technique [0002] In the process of producing acid chlorides by the thionyl chloride method, excess thionyl chloride is usually used, and then recycled after the reaction is finished. The recovered thionyl chloride usually contains isophthaloyl chloride, isophthalic acid, N,N-dimethylformamide, sulfur monochloride, sulfur dichloride and other impurities, and the color is dark yellow , the active ingredient of thionyl chloride is about 90%. Due to its dark color and low purity, it cannot be used any longer. Therefore need to adopt a process to purify thionyl chloride so that it can be reused. Contents of the invention [0003] The technical purpose of the present invention is to provide a method for the recovery and purification of thionyl chloride in the production of acid chlorides, which can effectively recover thionyl ...

Claims

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Application Information

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IPC IPC(8): C01B17/45
Inventor 杨佳云马海兵史洪波
Owner YANTAI TAYHO ADVANCED MATERIALS CO LTD
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