Method for continuously producing diphenyl sulfide in pipelined mode

Abstract

The invention discloses a method for continuously producing diphenyl sulfide in a pipelined mode. The method comprises the following steps: preparing benzene, a lewis acid catalyst and sulfur into rawmaterials, pumping the raw materials into a pipelined reactor through a metering pump to perform heating reaction, performing gas-liquid-phase separation on reaction liquor which flows out from the pipelined reactor after cooling; adding a reducing agent into a liquid phase obtained by gas-liquid-phase separation to perform reflow reaction, performing liquid separation on the product obtained byreflux reaction, performing normal-pressure distillation after washing an oil phase with deionized water, collecting fraction being 80-84 DEG C, wherein the fraction is benzene; distilling under reduced pressure, and collecting fraction being 80-90 DEG C, wherein the fraction is thiophenol; and collecting the fraction which is 160-170 DEG C, wherein the fraction is diphenyl sulfide. The method forproducing diphenyl sulfide has the characteristics of being capable of realizing continuous production, proper in reaction condition, low in production cost, considerable in yield, less in three wastes and the like.

Description

technical field [0001] The invention relates to a method for synthesizing organic compound diphenyl sulfide. Background technique [0002] Diphenyl sulfide is an important intermediate of pesticides, medicines and dyes. [0003] The literature (Applied Organometallic Chemistry, 32(5), 2018) reports a method for preparing diphenyl sulfide, dissolving halobenzene and sulfur in DMSO, adding potassium hydroxide, and reacting at 130°C. When chlorobenzene is the raw material, the yield of diphenyl sulfide is 28%, that of bromobenzene is 65%, and that of iodobenzene is 69%. This method uses chlorobenzene as a raw material, then the yield is low, and bromobenzene and iodobenzene are used as raw materials, and the cost is too high, so it is not suitable for industrial production. [0004] Literature (Organic Syntheses, 14,36-7; 1934) prepared diphenyl sulfide with benzene and disulfide dichloride under the catalysis of aluminum trichloride, the yield was 83%, but the method used th...

AI Technical Summary

Problems solved by technology

However, the reaction conditions of this method are too harsh, and the catalyst is easily poisoned and deactivated by the hydrogen sulfide generated by the reaction, so it is not suitable for industrial production.

[0006] The patent (CN106946752) mixes benzene and anhydrous aluminum chloride in a reactor and stirs, slowly adds sulfur under slight reflux, and continues the reflux reaction for 8 hours after adding, the reaction of benzene, anhydrous aluminum chloride (Lewis acid catalyst) and sulfur The molar ratio is 3.0~3.6:1.0~3.0:1.0; after the reaction, diphenyl sulfide is obtained by acid washing and distillation, and the reaction yield is 90%. This method does not explain the remaining 10% sulfur-containing products, and the reaction Long time, cumbersome operation, not suitable for continuous production

[0007] Therefore, the existing process for preparing diphenyl sulfide has the disadvantages of low yield, many wastes, and incapable of continuous production.

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