Synthesis process for aroamtic dithiol

A synthesis method and technology of dithiophenol are applied in the synthesis field of aromatic dithiophenol, can solve the problems of difficult industrialization, high production cost, environmental pollution and the like, and achieve the effects of avoiding pollution, saving costs and expanding the scope of application

Inactive Publication Date: 2002-08-21
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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Problems solved by technology

Due to the use of many toxic reagents in the preparation process, which causes environmental pollution, and the product needs post-...

Method used

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Embodiment

[0014] Chlorosulfonated Aromatic Compounds:

[0015] Take diphenyl ether, diphenylmethane, diphenyl sulfide, 1,4-diphenylbenzene, and 2,2-diphenylpropane as raw materials, and add them in batches to 48ml chlorosulfonic acid flasks at room temperature. After stirring for 3 hours, the reaction mixture was precipitated by adding water, and the chlorosulfonic acid product corresponding to the above-mentioned aromatic compound was isolated.

[0016] Synthesis of aromatic dithiophenols:

[0017] Weigh 2.2 to 2.9 grams of the chlorosulfonic acid products of the above-mentioned aromatic compounds, add 2.7 to 5.9 grams of zinc powder, 10 ml of water or 10 ml of absolute ethanol, 5 to 10 ml of concentrated sulfuric acid or 8 to 15 ml of concentrated hydrochloric acid as an acidic medium, and then in 70 Stir and reflux at ~90°C for 1.5 to 3 hours. After the reaction is completed, the reaction product is distilled off to obtain an aromatic dithiol product.

[0018]

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Abstract

The synthesis of aromatic dithiol includes the following steps: sulfochlorination of aromatic compound diphenyl ether, diphenyl methane, diphenyl sulfide and 1,4-diphenyl or 2,2-diphenyl propane; and the reaction between the sulfuryl chloride compound, zinc as reductant in sulfuric acid or hydrochloric acid medium system at 70-90 deg.c for 1.5-3 hr with the reactant moar ratio of sulfuryl chloride compound to zine powder to sulfuric acid or hydrochloride acid being 1 to 7-15 to 8-30. The process of the present invention has high product yield, no toxic solvent used and low cost, and the new aromatic dithiol products are used as fine chemical intermediate and synthesized material.

Description

technical field [0001] The invention relates to a method for synthesizing aromatic dithiols. technical background [0002] Aromatic dithiophenols are often used as intermediates of fine chemicals such as dyes, medicines, and pesticides. In addition, under the action of oxidizing agents, aromatic dithiophenols can generate cyclic oligomers, which can be processed at lower temperatures than the corresponding polymers, and can be processed without releasing any by-products. Ring-opening polymerization makes macrocyclic polymers potentially useful in many fields such as high-temperature hot-melt adhesives, coatings, and thermoplastic composites. [0003] At present, there are few varieties of aromatic dithiols, and the synthesis of aromatic dithiols reported in the literature adopts a two-step method. First, aromatic compounds are chlorosulfonated and then reduced to give aromatic dithiophenols. The reduction of aromatic compounds by chlorosulfonate...

Claims

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Application Information

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IPC IPC(8): C07C319/00C07C321/24
Inventor 孟跃中陈克张耀谋杜续生
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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