Supercritical phenthiol synthesis method by using hydrogen sulfide

The invention relates to a phenthiol synthesis method, in particular to a method comprising the following steps that in a high-pressure reaction vessel, hydrogen sulfide takes a contact reaction with chlorobenzene in a supercritical state, wherein the mol ratio of the chlorobenzene to the hydrogen s...

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Bibliographische Detailangaben
Hauptverfasser: LYU XUEHAO, WANG PENG, FAN BIN, YU LIZHI
Format: Patent
Sprache:chi ; eng
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Zusammenfassung:The invention relates to a phenthiol synthesis method, in particular to a method comprising the following steps that in a high-pressure reaction vessel, hydrogen sulfide takes a contact reaction with chlorobenzene in a supercritical state, wherein the mol ratio of the chlorobenzene to the hydrogen sulfide is 1:1 to 1:10, the reaction temperature is 100 DEG C to 200 DEG C, the reaction pressure is 9 to 25 MPa, and the reaction time is 1 to 10 hours; after the reaction is completed, water is used for washing a reaction mixture; an oil phase is collected; reduced pressure distillation is performed; fraction (10mmHg, 47 to 49 DEG C) is collected; the phenthiol is obtained. 本发明涉及合成苯硫酚的方法,具体涉及在高压反应器中,使硫化氢在超临界状态下与氯苯接触反应,氯苯与硫化氢的摩尔比为1∶1~1∶10,反应温度为100℃~200℃,反应压力为9~25MPa,反应时间为1~10小时,在反应结束后,用水洗涤反应混合物,收集油相,减压精馏,收集(10mmHg,47-49℃)馏分,即为得到苯硫酚。