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Preparation method of ethyl chloride

A technology of ethyl chloride and ethyl sulfide, which is applied in the field of preparation of ethyl chloride, can solve the problems of high production and operation costs, large amount of distillation residual liquid, long production cycle, etc., and achieve waste water treatment cost reduction, comprehensive Huge economic benefits and resource saving effects

Inactive Publication Date: 2015-08-05
湖北犇星新材料股份有限公司
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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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1. Vulcanization: Take 600kg of phosphorus pentasulfide and react with 497kg of absolute ethanol under the pyridine catalyst to form ethyl sulfide; among them, the weight ratio of absolute ethanol to pyridine is 1000:1.5.

[0030] 2. Chlorination: pass chlorine gas into ethyl sulfide to produce crude chlorine, wherein the amount of chlorine gas is 71-73% of the mass of phosphorus pentasulfide, and the reaction time is 6-8 hours. When the density of the reaction solution reaches 1.275~1.285g / cm 3 (20°C), the reaction ended. The hydrogen chloride produced by the reaction is absorbed by water to obtain hydrochloric acid.

[0031] 3. Pass the hydrogen sulfide produced by the sulfidation reaction into the crude chlorine to remove the disulfur dichloride impurity, control the negative pressure at -0.03MPa, the temperature at 35°C, and the reaction time for 3h to obtain the crude ethyl chloride and fine sulfur, When the temperature drops below 8°C, after 0.5-1 hour of heat p...

Embodiment 2

[0034] 1. Vulcanization: Take 650kg of phosphorus pentasulfide and react with 538kg of absolute ethanol under the pyridine catalyst to form ethyl sulfide; among them, the weight ratio of absolute ethanol to pyridine is 1000:1.5.

[0035] 2. Chlorination: pass chlorine gas into ethyl sulfide to produce crude chlorine, wherein the amount of chlorine gas is 71-73% of the mass of phosphorus pentasulfide, and the reaction time is 6-8 hours. When the density of the reaction solution reaches 1.275~1.285g / cm 3 (20°C), the reaction ended. The hydrogen chloride produced by the reaction is absorbed by water to obtain hydrochloric acid.

[0036] 3. Pass the hydrogen sulfide produced by the sulfidation reaction into the crude chlorine to remove the disulfide dichloride impurity, control the negative pressure at -0.02MPa, the temperature at 45°C, and the reaction time of 2.5h to obtain crude ethyl chloride and fine sulfur , when the temperature drops below 8°C, after 0.5-1h of heat preser...

Embodiment 3

[0039] 1. Vulcanization: Take 600kg of phosphorus pentasulfide and react with 495kg of absolute ethanol under the pyridine catalyst to form ethyl sulfide. The weight ratio of absolute alcohol to pyridine is 1000:1.5.

[0040] 2. Chlorination: pass chlorine gas into ethyl sulfide to produce crude chlorine, wherein the amount of chlorine gas is 71-73% of the mass of phosphorus pentasulfide, and the reaction time is 6-8 hours. When the density of the reaction solution reaches 1.275~1.285g / cm3 (20°C), the reaction ended. The hydrogen chloride produced by the reaction is absorbed by water to obtain hydrochloric acid.

[0041] 3. Pass the hydrogen sulfide produced by the sulfidation reaction into the crude chlorine to remove the disulfide dichloride impurity, control the negative pressure at -0.025MPa, the temperature at 40°C, and the reaction time for 3h to obtain the crude ethyl chloride and fine sulfur, When the temperature drops below 8°C, after 0.5-1h of heat preservation, the...

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Abstract

The invention relates to a preparation method of ethyl chloride. The method comprises the following steps: 1, carrying out a sulfuration reaction on phosphorus pentasulfide and anhydrous ethanol under the action of a catalyst to obtain ethyl sulfide and hydrogen sulfide; 2, carrying out a chlorination reaction on ethyl sulfide and chlorine to generate crude chlorine; and 3, introducing hydrogen sulfide obtained after the sulfuration reaction into the crude chlorine, and reacting to obtain ethyl chloride and sulfur. The preparation method has the following advantages: hydrogen sulfide is adopted to remove disulfur dichloride in crude chlorine, so the consumption of an alkali liquid is reduced, and generated tail gas hydrogen chloride can be absorbed by water to prepare hydrochloric acid as a byproduct; obtained sulfur is sandy in shape, and can be directly sold as a raw material without treatment; and no wastewater is generated in the whole preparation process, so environmental pollution is maximally reduced, and the cost is saved.

Description

technical field [0001] The invention relates to a preparation method of ethyl chloride, which belongs to the technical field of preparation of pesticide intermediates. 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] 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 solution; then chlorine gas is passed into ethyl sulfide, and obtaine...

Claims

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Application Information

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IPC IPC(8): C07F9/20C01B17/02
Inventor 戴百雄郑强宫庭徐善武龚仕望张建广罗斌
Owner 湖北犇星新材料股份有限公司
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