Synthesis Of Tetrakis-(2,4-di-butylphenyl)-4,4'-biphenylene Diphosphonite

Tetrakis-(2,4-di-butylphenyl)-4,4'-biphenylene diphosphonite is a kind of excellentphosphite antioxidant. By analyzing the molecule structure of the substance, two-step methodwas studied out to synthesize it in this paper. The route of synthesis is as follows: biphenyl andPCl3 as the raw materials, and the intermediate was synthesized with the catalyst PCl3, then theintermediate reacted with 2,4-di-butylpheno in the xylene, at last the P-EPQ was come intobeing. According to lots of experiments and the influence of the react temperature, time, ratio ofmaterials, bondage agents, the kinds of the solvents on the synthesis of the intermediate andfinal productions, the optimum factors was summarized.The results showed that the temperature of the water bath is 85℃, n(PCl3): n(AlCl3):n(biphenyl)=6: 2.2: 1, react time is 6h, the A substance as disconnect agents, the xylene as thesolvent, the disconnect temperature is 85℃, A was added with n(M): n(AlCl3)=1.0: 1.0, after60min, the yield of the intermediate can reach to 84.5%. In process of the esterification reaction,reaction temperature is 30℃, the amount of the solvent is 110ml, n(2,4-di-butylpheno):n(bondage agent): n(intermediate) is 4.4: 4.8: 1, reaction time is 90min, the solvent wasdecompression distilled off after reaction, and refining with methyl alcohol, then the purerproduction was obtained, the maximum yield can reach to 36.4%. The intermediates and finalproductions were analyzed by the means of melting point, IR spectrum, element analysis,finally their structures were ascertained.