The Development And Utilization Of Sodium Salt Of Diethyl Phosphate For The Preparation Of Useful Organic Phosphate

Organic phosphate is an extremely useful important fine chemical, and including many varieties. It has a wide application in plasticizers, flame retardants, catalysts, insecticides, antioxidants, defoamers and water treatment agent. And it occupies an important position in the national economy.In this paper, useful organic phosphate products were synthesized by phase transfer catalysis method which was used by many research scholars. It has the advantages of increasing reaction rate, mild reaction conditions, simple operations, high yields, clean technology and low toxicity and so on.Sodium salt of diethyl phosphate derived from the by-product of fluorescent brightener ER in Daqing New Century Fine Chemical Co., Ltd was used as raw materials. Because of complex composition of industry wastes, it has been purified firstly. Then we studied three reactions separately, such as sodium of diethyl phosphate with thionyl chloride, in the phase transfer catalysis sodium of diethyl phosphate with substituted benzyl chlorides and diethyl sulfate. The resulting compounds of three reactions are obtained in better yield by applying this phase transfer catalysis method.In the preparing tetraethyl pyrophosphate from sodium of diethyl phosphate and thionyl chloride, the optimized reaction conditions was obtained by orthogonal experimental design, then we repeated several experiments at the optimized reaction conditions, and the results are basically stable. The synthesized product was characterized by refractive index, MS, IR,1H NMR and 31P NMR. The possibly mechanism of this reaction was explored.In phase transfer catalysis, substituted benzyl diethyl phosphates and triethyl phosphate were synthesized from sodium of diethyl phosphate and substituted benzyl chlorides, diethyl sulfate separately. The effects of the raw material molar ratio, reaction temperature, catalyst structure and amounts on the yield of the benzyl diethyl phosphates were investigated and the possibly mechanism of this reaction was explored. At the same time, the effect of electron-donating substituting groups and electron-withdrawing substituting groups on substituted benzyl diethyl phosphates has been studied. The structures of all target products generated were confirmed by refractive index, MS, IR, and ~1H NMR. Through the ultraviolet - visible spectrophotometry, the content of triethyl phosphate is measured above 99%.