Synthesis of sicycle-ring hexyl di-thiophosphinic acid

Abstract

The invention discloses a synthetic method of dicyclohexyl dithiophosphinate. The method comprises: taking bromo cyclohexane as a raw material which is firstly reacted with a magnesium rod for obtaining a Grignard reagent, forming a linked phosphorus intermediate through the reaction between the acquired Grignard reagent and phosphorus thiochloride, obtaining a crude product of dicyclohexyl dithiophosphinate through steps of sulfurization and acidification, then gaining a pure product of dicyclohexyl dithiophosphinate through amine salt formation, recrystallization and acidification. Comparedwith the current methods, the method of the invention has the advantages of easy obtaining of materials, less synthesis steps, simple process, high yield and low toxicity.

Description

technical field [0001] The invention belongs to the synthesis method of compounds in organic chemistry, in particular to the synthesis method of dicyclohexyl dithiophosphinic acid. Background technique [0002] Dithiophosphinic acid compounds are a class of flotation agents widely studied in the metallurgical industry. Certain types of structures, such as Cynaex301, have good complexation, coordination and separation capabilities for lanthanide-actinides. There are many ways to synthesize dialkyl dithiophosphinic acid, such as the aryl-substituted structure, the benzene ring or the substituted benzene ring in AlCl 3 Catalyzed with P 2 S 5 Prepared by reaction; there are many synthetic methods for primary alkyl-substituted compounds, and intermediate secondary phosphine can be obtained from different reaction raw materials. The biphosphine intermediate reacts with sulfur and sodium sulfide to obtain a salt, which is acidified to give dithiophosphinic acid; the synthesis of...

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Problems solved by technology

However, the volatility and irritation of the secondary phosphine are relatively strong, so the toxicity is relatively high

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