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Method for separating disulfur dichloride in preparation process of high-purity ethyl chloride

A technology of ethyl chloride and preparation process, applied in the field of separation and purification of organic compounds, can solve the problems of high production and operation cost, large amount of distillation residue, long production cycle, etc., and achieves reduction of waste water treatment cost and comprehensive economic benefits Huge and beneficial effect

Active Publication Date: 2017-01-25
湖北犇星农化有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the purity of ethyl chloride produced by this method is high, the purification of sulfide will result in a long production cycle and high production and operation costs; and the whole system has a large amount of distillation residue and is difficult to handle

Method used

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  • Method for separating disulfur dichloride in preparation process of high-purity ethyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The process of separating dichlorodisulfide is as follows figure 1 .

[0032] 1) Put 1000kg of crude chlorine in the rectification tower kettle, control the negative pressure at -0.098MPa, reflux ratio 4:2, and slowly raise the temperature with hot water. The size of the distillation tower is Ф400×6000mm, and the material is 316L stainless steel lined with fluorine. A digital display bimetal corrosion-resistant thermometer is installed in the tower kettle, which extends into the material.

[0033] 2) When the tower kettle temperature tower Total reflux at <55℃; when 55℃≦tower temperature≦70℃, collect yellow-red fractions as dichlorodisulfide (gas chromatographic detection content: 99.1%); when 70℃ <Temperature of tower bottom ≦83℃, the collected transitional fraction is returned to tower bottom; from the thermometer showing 83.1℃, that is 83℃ <The distillate collected when the tower kettle temperature≦93°C is refined ethyl chloride (gas chromatography detection content: 99....

Embodiment 2

[0037] 1) Put 1000kg of crude chlorine in the rectification tower kettle, control the negative pressure at -0.099MPa, reflux ratio 4:2, and slowly raise the temperature with hot water. The rectification equipment is the same as in Example 1.

[0038] 2) When the tower kettle temperature tower Total reflux at <55℃; when 55℃≦tower temperature≦70℃, collect yellow-red fractions as dichlorodisulfide (content: 99.2%); when 70℃ <Temperature of tower bottom ≦83℃, the collected transitional fraction is returned to the tower bottom; from the thermometer showing 83.2℃, that is when 83℃ <The distillate collected when the tower kettle temperature≦93°C is refined ethyl chloride (content: 99.67%).

[0039] 3) After the rectification is completed, the temperature is reduced to 40°C, and then a small amount of solid sulfur is filtered out, which is used as a by-product after refining; a small amount of residue is treated separately.

Embodiment 3

[0041] 1. Put 1000kg of crude chlorine in the rectification tower kettle, control the negative pressure at -0.1MPa, reflux ratio 4:2, and slowly heat up with hot water. The rectification equipment is the same as in Example 1.

[0042] 2. When the tower kettle temperature tower Total reflux at <55℃; when 55℃≦tower temperature≦70℃, collect yellow-red fractions as dichlorodisulfide (content: 99.4%); when 70℃

[0043] 3. After the rectification is completed, the temperature is reduced to 40°C, and then a small amount of solid sulfur is filtered out, which is used as a by-product after refining; a small amount of residual liquid is treated separately.

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Abstract

The invention provides a method for separating disulfur dichloride in the preparation process of high-purity ethyl chloride; crude ethyl chloride generated in the reaction of ethyl sulfide with chlorine is separated through a rectifying column, disulfur dichloride fraction is collected when column bottom temperature is 70 DEG C and below, and the fraction refined ethyl chloride is collected when column bottom temperature is 83-84 DEG C and above. According to the method provided herein, the crude ethyl chloride can be rectified and separated to obtain refined ethyl chloride with a content of > / =99.6% and the byproduct disulfur dichloride with a content of > / =99%; little sulfur and liquid residue are generated in the separation process, and the sulfur can be post-processed into byproducts for sale; the whole process is free of wastewater, and environmental pollution reduction and resource saving are achieved to maximum extent.

Description

Technical field [0001] The invention belongs to the field of organic chemistry, and specifically relates to a method for separating and purifying organic compounds containing phosphorus and sulfur. Background technique [0002] "Ethyl chloride" is a key intermediate for the production of the high-efficiency and low-toxic pesticide chlorpyrifos technical. The product meets the requirements of green chemical industry and circular economy. At present, the reaction mechanism of ethyl chloride is as follows: [0003] P 2 S 5 +4C 2 H 5 0H 2 →2(C 2 H 5 0) 2 PS-SH+H 2 S↑ (1) [0004] 2(C 2 H 5 O) 2 PS-SH+3Cl 2 →2(C 2 H 5 0) 2 PS-C1+S 2 Cl 2 +2HCl↑ (2) [0005] S 2 Cl 2 +Na 2 S=2NaCl+3S↓ (3) [0006] S 2 Cl 2 =Cl 2 ↑+3S↓ (4) [0007] A quantitative amount of phosphorus pentasulfide is reacted with anhydrous ethanol under the action of a catalyst to form ethyl sulfide, and the exhaust hydrogen sulfide produced is absorbed by liquid caustic so as to form sodium sulfide solution; then chlorine gas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/20C01B17/45
CPCC01B17/4538C07F9/20
Inventor 戴百雄熊传宗贺丛国龚仕望罗斌
Owner 湖北犇星农化有限责任公司
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