Optimization Of The Process Route For The Synthesis Of Triphenylphosphine By The Friedel-Crafts Reaction

Triphenylphosphine(triarylphosphine abbreviated to: PPh3)is a kind of important chemical reagent and ligand of homogeneous catalyst,and is also the base material of rhodium phosphine complex catalyst..For example,Wilkinson catalyst,Wittig reagent,Rydon reagent,etc.PPH3 is also widely used in dye processing,such as used as a light enhancer,color film imaging antioxidant,polymer polymerization,polyepoxidation stabilizer and as analytical reagent.PPH3 as a basic chemical raw material,with the development of organic synthesis technology,the new use of PPH3 is also constantly expanding,the demand is increasing year by year,the United States and Europe and other developed countries are building new production equipment to expand the capacity of PPH3.At present,the domestic industrial production of PPH3 manufacturers are not many.The purity of PPH3 produced by Anhui Jinshan Chemical Technology Co.,Ltd.ranks at the top,reaching 99.7%.Due to the low yield of PPH3 and the difficulty in recycling the waste residue produced in the production process,it is of great economic and practical value to improve the synthesis process of PPH3.This paper discusses the five kinds of common method to synthesize triphenylphosphine.Based on the analysis of PPH3 yield,economic cost and operation safety,an optimal synthesis scheme of PPH3 by Friedel-Crafts method was proposed.Results In the process of synthesis of PPH3 by Ferridel-Crafts method,the yield of PPH3 by two-step synthesis of phosphine trichloride and reduction of triphenyl phosphine sulphide is obviously better than that by one-step synthesis of phosphine trichloride and reduction of triphenyl phosphine sulphide.PPH3 was synthesized by the process of synthesis of thiophosphorus trichloride-synthesis of triphenyl phosphine-synthesis of PPH3.After the product was refined,the structure of the product was analyzed by melting point determination,infrared spectrum analysis and hydrogen nuclear magnetic resonance spectroscopy,and the intermediate product was determined as PPH3 and the final product was determined as PPH3.Through factor analysis,the optimal process was determined as follows: using phosphorus trichloride and sulfur as raw materials,using aluminum powder as catalyst,reaction at 120? to 130? for 3 hours to synthesize phosphorus trichloride;Triphenyl phosphosine was synthesized from thiophosphorus trichloride with excessive benzene using aluminum chloride as catalyst,and reacted at 120? to 130? for 8 hours to synthesize triphenyl phosphosine sulfur.PPH3 was reduced by zinc particles at 340?to 350? for 2 hours.The reduced product was PPH3.After the index detection of the synthetic product PPH3,all the test indexes meet the standard of industrial triphenylphosphine.