Synthesis method for reactive phosphorus flame retardant n-butyl phosphinic acid benzene methyl ester

Abstract

The invention discloses a synthesis method for reactive phosphorus flame retardant n-butyl phosphinic acid benzene methyl ester. The method comprises the steps of: firstly adding diethylene glycol diethyl ether, tetrabutylammonium bromide and n-butyl chloride into a three-neck flask, adding a sodium hydroxide solution under room temperature, introducing nitrogen, heating the mixed solution to 60DEG C, adding yellow phosphorus, cooling the reaction system rapidly, carrying out reaction for 4h, and conducting standing and liquid separation; then adding hydrogen peroxide, hydrochloric acid and benzyl alcohol into the lower layer solution, and separating water at the end of reaction; conducting pressure reduced distillation to remove excess benzyl alcohol, and collecting fractions, thus obtaining the n-butyl phosphinic acid benzene methyl ester. The synthesis method provided by the invention has the characteristics of easily available synthesis raw materials, simple process, no excessive byproducts, high efficiency, and no obvious environmental pollution.

Description

[0001] technical field [0002] The invention relates to a method for synthesizing a flame retardant, in particular to a method for synthesizing a reactive phosphorus-based flame retardant. [0003] Background technique [0004] At present, most of the synthetic techniques of phosphinic esters are to add phosphinic acid hydrate to branched olefins and synthesize under the condition of peroxide as catalyst, but the yield is very low. In addition, the synthetic technique of dihalide is a very difficult process. The complex process also includes some uncertain factors to generate many unknown products, and the experimental operation is cumbersome, or requires the use of expensive organic solvents, and the reaction yield is low, and the product purity is not high. [0005] Contents of the invention [0006] The object of the present invention is to provide a method for synthesizing the reactive phosphorus-based flame retardant n-butyl benzylphosphinate, which has simple proc...

AI Technical Summary

Problems solved by technology

[0004] At present, most of the synthetic techniques of phosphinic esters are to add phosphinic acid hydrate to branched olefins and synthesize them under the condition of peroxide as a catalyst, but the yield is very low. In addition, the synthetic technique of dihalides is a very difficult process. Complicated process, including some uncertain factors to generate many unknown products, and the experimental operation is cumbersome, or requires the use of expensive organic solvents, and the reaction yield is low, the product purity is not high, etc.