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Method for separating dichlorodisulfide during preparation of high-purity ethyl chloride

A technology for 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: 2018-03-20
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 dichlorodisulfide during preparation of high-purity ethyl chloride

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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 still of the rectification tower, control the negative pressure at -0.098MPa, reflux ratio 4:2, and slowly raise the temperature with hot water. The size of the rectification 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) Total reflux when the temperature of the tower kettle is less than 55°C; when 55°C≦the temperature of the tower kettle≦70°C, the yellow-red fraction is collected as dichlorodisulfide (content detected by gas chromatography: 99.1%); when 70°C

Embodiment 2

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

[0038] 2) Total reflux when the temperature of the tower kettle is less than 55°C; when 55°C≦the temperature of the tower kettle≦70°C, collect the yellow-red fraction as dichlorodisulfide (content: 99.2%); when 70°C

[0039] 3) After the rectification is completed, cool down to 40°C, then filter out a small amount of solid sulfur, and use it as a by-product after refining; a small amount of raffinate will be treated separately.

Embodiment 3

[0041] 1. Put 1000kg of crude chlorine in the still of the rectification tower, control the negative pressure at -0.1MPa, reflux ratio 4:2, and slowly raise the temperature with hot water. Rectification equipment is with embodiment 1.

[0042] 2. When the temperature of the tower kettle is less than 55℃, full reflux; when 55℃≦the temperature of the tower kettle≦70℃, collect the yellow-red fraction as dichlorodisulfur (content: 99.4%); when 70℃

[0043] 3. After the rectification is completed, cool down to 40°C, then filter out a small amount of solid sulfur, and use it as a by-product after refining; a small amount of raffinate will be 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 in particular relates to a method for separating and purifying phosphorus and sulfur-containing organic compounds. Background technique [0002] "Ethyl chloride" is a key intermediate for the production of high-efficiency and low-toxic pesticide chlorpyrifos technical, and the product meets the requirements of green chemical industry and circular economy. Currently, 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] The quantitative phosphorus pentasulfide reacts with absolute ethanol under the action of a catalyst to form ethyl sulfide, and the generated tail gas hydrogen sulfide is absorbed by liquid caustic soda to form sodium sulfide...

Claims

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Application Information

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Patent Type & Authority Patents(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