Synthetic method of diphenyl sulfide

A synthetic method and technology of diphenyl sulfide, applied in the direction of sulfide preparation, organic chemistry, etc., can solve the problems of high production cost, difficulty in forming production capacity, low yield, etc., and achieve the effect of less waste water and lower cost

Inactive Publication Date: 2017-07-14
LIANYUNGANG ZHICHENG CHEM
View PDF4 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The disadvantage of the first two methods is that sulfur chloride is a golden yellow liquid, and when the purity is not high, it is often caused by the presence of SCl 2 It is orange or even slightly red, fumes in humid air, and has an unpleasant pungent smell. The treatment of the three wastes is very difficult, and the yield is too low
The raw material iodobenzene of the thir

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Synthetic method of diphenyl sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a four-neck flask equipped with a condenser, a water separator, a thermometer and a tail gas treatment device (tail gas produced by the absorption reaction of the sodium hydroxide solution), add 200g of benzene and 97g of aluminum trichloride, heat up to 50°C, and Under reflux, add sulfur 23.2g in batches, along with the addition of sulfur, the reflux temperature is higher and higher, as the reaction proceeds, the color of the reaction solution deepens to purple red, and then continues the heat preservation reaction for 7.5 hours. After the reaction is completed, cool to room temperature, and synthesize The material is slowly added dropwise into hydrochloric acid composed of 50g of 30% hydrochloric acid and 160g of water, and the reaction solution gradually becomes a brownish-yellow turbid liquid, and the addition is completed in about 1 hour; the layers are left to stand, and the upper organic layer is heated and precipitated to remove benzene to obtain diphenylsulfid...

Embodiment 2

[0021] In a four-neck flask equipped with a condenser, a water separator, a thermometer and a tail gas treatment device (tail gas generated by the absorption reaction of the sodium hydroxide solution), add 200g of benzene and 142.8g of ferric chloride, heat up to 50°C, and Under slight reflux, add sulfur 23.2g in batches, along with the addition of sulfur, the reflux temperature is getting higher and higher, as the reaction proceeds, the color of the reaction solution is deepened to purple red, and then the insulation reaction is continued for 6 hours. After the reaction is completed, it is cooled to room temperature, and the The synthetic material is slowly added dropwise to dilute hydrochloric acid composed of 50g of 30% hydrochloric acid and 160g of water, the reaction solution gradually turns into a brownish-yellow turbid solution, and the addition is completed in about 1 hour; standing for stratification, the upper organic layer is heated and precipitated to remove benzene ...

Embodiment 3

[0024] In a four-necked flask equipped with a condenser, a water separator, a thermometer and a tail gas treatment device (tail gas generated by the absorption reaction of the sodium hydroxide solution), add 200g of benzene and 97g of aluminum trichloride, heat up to 70°C, and Under reflux, add sulfur 23.2g in batches, along with the adding of sulfur, reflux temperature is more and more higher, along with reaction, reaction solution color is deepened to purple red, then continue insulation reaction 7.5 hours, then 30% in pickling reaction bottle Dilute hydrochloric acid composed of 50g of hydrochloric acid and 250g of water, slowly add the above-mentioned synthetic material dropwise, the reaction solution gradually turns into a brownish-yellow turbid solution, and the addition is completed in about 1.0h; let stand to separate layers, and then add water to wash until the water layer is neutral.

[0025] In this embodiment, 60.7 g of the product was finally obtained, with a conte...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a synthesis method of diphenyl sulfide. According to the method, the molar ratio of benzene, Lewis acid catalyst and sulfur is 3.0~3.6:1.0~3.0:1.0. After mixing benzene and catalyst, the temperature is raised to 50~70°C, sulfur is slowly added, and the hydrogen sulfide gas generated by the reaction is Pour into the sodium hydroxide solution, reflux until the reaction is complete after adding the sulfur, then cool to room temperature, and slowly add the synthetic material dropwise to 5-15% dilute hydrochloric acid for pickling, leave the upper layer organic layer after stratification Benzene is removed by heating and precipitating to obtain diphenyl sulfide, and benzene is recovered and used mechanically. The invention uses benzene and sulfur as raw materials, significantly reduces the cost, produces less waste gas and waste water, is environmentally friendly, and reaches the international standard. More than 98%, suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis method of diphenyl sulfide, which belongs to the field of organic chemistry. Background technique [0002] Diphenyl sulfide is an intermediate of pesticides, medicines, and dyes, and it is also used for the synthesis of 2,4-dichlorophenol, pesticide herbicides (benben, 2,4-D), insecticide ibifos (EPBP), and veterinary drug Dukesan And other catalysts can also be used in the synthesis of sulfur bis-dichlorophenol and so on. [0003] At present, there are mainly four preparation methods of diphenyl sulfide: 1) first mix benzene and aluminum trichloride, cool to a certain temperature, add dropwise the mixed solution of sulfur chloride and benzene under stirring, and hydrogen chloride will escape at the beginning of the reaction and a small amount of hydrogen sulfide to precipitate a yellow viscous aluminum trichloride complex. After the reaction is complete, diphenyl sulfide is obtained through a series of post-treatm...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C319/14C07C321/30
CPCC07C319/14
Inventor 刘必焕王耀良
Owner LIANYUNGANG ZHICHENG CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap