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Environment-friendly recovery method for ethyl chloride production by-product sulfur

An ethyl chloride, environment-friendly technology, applied in chemical instruments and methods, sulfur compounds, inorganic chemistry, etc., can solve the problems of high processing cost, high distillation temperature, and the impact of recovering ethyl chloride, and achieve ecological and environmental friendliness. Effect

Active Publication Date: 2019-04-02
扬州帮手科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Patent Publication No. CN103910337A discloses a treatment method of by-product sulfur in the ethyl chloride production process. The treatment method is to add liquid caustic soda, catalyst and emulsifier during treatment. The treatment cost is high, the treatment time is long, and the distillation temperature is high ( 60~110℃), which has a great impact on the subsequent recovery of ethyl chloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1, small test example:

[0042] Add 100 grams of crude sulfur to a 500ml four-necked flask equipped with a condenser, a thermometer and an air guide tube, add 350ml of clear water, crush it to 120 mesh with a high-shear pump, then use ordinary stirring instead, heat up and carry out steam distillation to zero The oil flows out, the temperature is lowered to 50°C, and chlorine gas is introduced for the primary oxidation reaction. After 15 grams of chlorine gas is introduced, the introduction of chlorine gas is stopped, and ozone is introduced for secondary oxidation reaction (0.01 g of catalyst DM can be added, and ozone is introduced for secondary oxidation reaction). Oxidation reaction), while adjusting the temperature to 70 ° C for hydrolysis. Stop feeding ozone after feeding 1 gram of ozone. After 7 hours of hydrolysis, lower the temperature to 30°C for suction filtration, rinse the filter cake twice with 10 grams of water, and finally dry it to obtain fi...

Embodiment 2

[0043] Embodiment 2, large-scale production example:

[0044]Add 1,000 kg of crude sulfur to a 5,000-liter shear force kettle, add 3,500 liters of clear water, crush it to 120 mesh with a high-shear force pump, then put it in a 5,000-liter processing kettle, and heat up for steam distillation until no oil flows out , lower the temperature to 50°C, feed chlorine gas for the primary oxidation reaction, stop feeding chlorine gas after feeding 15 kg of chlorine gas, and feed ozone for secondary oxidation reaction (you can add 0.1 kg of catalyst DM, and feed ozone for secondary oxidation reaction ), while adjusting the temperature to 70°C for hydrolysis. Stop feeding ozone after feeding 13 kilograms of ozone. After hydrolysis for 7 hours, lower the temperature to 30°C for suction filtration, wash the filter cake twice with 20 kg of water, and finally dry it to obtain finished sulfur.

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Abstract

The invention relates to an environment-friendly recovery method for an ethyl chloride production by-product sulfur, comprising the following steps: step 1), placing small-particle sulfur of a by-product of ethyl chloride production in a high-shearing kettle, adding water, and conducting pulverizing to form a powder of 120 mesh or more; step 2), placing a pulverized sulfur suspension in a treatment kettle for water steam distillation; step 3), introducing a primary oxidant for primary oxidation reaction, wherein the primary oxidant is chlorine; step 4) after the primary oxidation reaction, introducing a secondary oxidant for a secondary oxidation reaction, and at the same time, adjusting the temperature in the treatment kettle to carry out a hydrolysis reaction, wherein the secondary oxidant is ozone; and step 5), after the secondary oxidation reaction and the hydrolysis reaction, cooling the temperature of the suspension, and conducting suction filtration, washing the obtained filtercake by clear water, conducting drying through baking or melting, and conducting slicing, so as to obtain a finished product sulfur. According to the present invention, the recovery method for the ethyl chloride production by-product sulfur is extremely friendly to environment.

Description

technical field [0001] The invention relates to an environmentally friendly method for recovering sulfur, a by-product of ethyl chloride production, and belongs to the field of fine chemicals. Background technique [0002] Ethyl chloride is an important intermediate in the production of pesticides such as chlorpyrifos, triazophos, phoxim, diazinon, parathion, and pyrimiphos, which are highly efficient and low-toxic insecticides, and plays an important role in the production of pesticides. It is an absolutely indispensable pesticide intermediate. In order to realize that the production of ethyl chloride conforms to the concept of green environmental protection and the requirements of circular economy, the phosphorus pentasulfide distillation process is generally used in China to produce ethyl chloride. The basic process is: react phosphorus pentasulfide and absolute ethanol under the catalysis of pyridine to produce sulfide, sulfide is passed through chlorine for primary chl...

Claims

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Application Information

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IPC IPC(8): C01B17/027
CPCC01B17/0232C01B17/027
Inventor 常志良
Owner 扬州帮手科技有限公司
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