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Clean preparation method of ethyl chloride with high purity

A technology of ethyl chloride and ethyl sulfide, applied in the field of clean preparation of high-purity ethyl chloride, can solve problems such as large waste water, environmental pollution, unpleasant and pungent odor, etc., and achieve resource saving and resource saving. Effect

Active Publication Date: 2014-01-08
HUANGGANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process produces a large amount of wastewater and unpleasant pungent odor during its alkaline hydrolysis and washing process; this not only increases the difficulty and production cost of wastewater treatment, but also will cause serious damage to the environment if the treatment is not up to standard or the discharge is not up to standard Pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Purification of ethyl sulfide: the crude product of ethyl sulfide, an intermediate product produced in the process of producing ethyl chloride with anhydrous ethanol and phosphorus pentasulfide as raw materials, is first sent to a thin film evaporator. Distill at high temperature to remove low-boiling impurities such as hydrogen sulfide gas, and then send it to a two-stage wiped-film molecular distillation device for the first-stage molecular distillation at a pressure of 10 Pa and a temperature of 70°C to obtain colorless ethyl Sulfide and brown-black raffinate, and then carry out second-stage molecular distillation on the brown-black raffinate at a pressure of 1 Pa and a temperature of 80°C to obtain light brown ethyl sulfide and black raffinate, which can be Used as flotation agent;

[0019] 2) Purification of ethyl chloride: send the colorless ethyl sulfide and the light brown ethyl sulfide obtained in step 1) together or separately into the chlorination kettle a...

Embodiment 2

[0021] 1) Purification of ethyl sulfide: the crude product of ethyl sulfide, an intermediate product produced in the process of producing ethyl sulfide with anhydrous ethanol and phosphorus pentasulfide as raw materials, is first sent to a thin film evaporator. Distill at high temperature to remove hydrogen sulfide gas and low-boiling impurities, and then send it to a two-stage wiped-film molecular distillation device for the first-stage molecular distillation at a pressure of 5pa and a temperature of 60°C to obtain colorless ethyl Sulfide and brown-black raffinate, and then carry out second-stage molecular distillation on the brown-black raffinate at a pressure of 10 Pa and a temperature of 70°C to obtain light brown ethyl sulfide and black raffinate, which can be Used as flotation agent;

[0022] 2) Purification of ethyl chloride: send the colorless ethyl sulfide and light brown ethyl chloride obtained in step 1) separately or together into the chlorination kettle and pass c...

Embodiment 3

[0024] 1) Purification of ethyl sulfide: the crude product of ethyl sulfide, an intermediate product produced in the process of producing ethyl chloride with anhydrous ethanol and phosphorus pentasulfide as raw materials, is first sent to a thin film evaporator, under 6650pa pressure, 40 ℃ Distill at high temperature to remove low-boiling impurities such as hydrogen sulfide gas, and then send it to a two-stage wiped-film molecular distillation device for the first-stage molecular distillation at a pressure of 10 Pa and a temperature of 70°C to obtain colorless ethyl Sulfide and brown-black raffinate, and then carry out second-stage molecular distillation on the brown-black raffinate at a pressure of 10pa and a temperature of 75°C to obtain light brown ethyl sulfide and black raffinate, which can be Used as flotation agent;

[0025] 2) Purification of ethyl chloride: send the colorless ethyl sulfide and light brown ethyl chloride obtained in step 1) separately or together into ...

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PUM

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Abstract

The invention discloses a clean preparation method of ethyl chloride with high purity. The method comprises the following steps: firstly, purifying a crude ethyl sulfide product by membrane distillation and molecular distillation in sequence to separate out impurities such as hydrogen sulfide gas, neutral oil and residues, then feeding the purified crude ethyl sulfide product into a chlorination process, thereby reducing byproducts in the chlorination process; filtering a crude ethyl chloride product obtained after chlorination, and then purifying the filtered crude ethyl chloride product by membrane distillation and molecular distillation in sequence to separate out impurities such as chlorine gas, hydrogen chloride and disulfur dichloride. The ethyl chloride produced by the method is high in purity, and no waste water is generated during the whole process, so that pollution to environment is minimized and resources are saved furthest.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a clean preparation method of high-purity ethyl chloride. Background technique [0002] Ethyl chloride is the abbreviation of O, O-diethylthiophosphoryl chloride, which is the main raw material for the preparation of important intermediates of organophosphorus pesticides. The traditional domestic production process is: use absolute ethanol and phosphorus pentasulfide as raw materials (absolute alcohol: phosphorus pentasulfide = 4.1:1 (molar ratio), in the presence of a catalyst, a chemical reaction occurs between 65 and 85 degrees to form brown Liquid O, O-diethyl dithiophosphate (referred to as ethyl sulfide) and hydrogen sulfide gas, hydrogen sulfide gas is absorbed by sodium hydroxide alkali solution to produce alkali sulfide solution; because P2S5 used as raw material contains P4S7, P4S5, P4S3 and other impurities, during the chemical reaction between P2S5 and absolut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/20
Inventor 田辉明
Owner HUANGGANG NORMAL UNIV
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