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

Abstract

The invention discloses a synthesis method for reactive phosphorus flame retardant ethyl phosphinic acid n-butyl ester. The method includes the steps of: firstly preparing toluene and tetrabutylammonium bromide into a solution, conducting heating, adding white phosphorus, stirring the materials evenly, performing cooling, introducing nitrogen, adding bromoethane, adding a sodium hydroxide solution, carrying out heat preservation reaction, adding water, conducting stirring and heating to room temperature, and performing standing so as to obtain a clarified two-phase solution; then conducting liquid separation, adding hydrogen peroxide, hydrochloric acid and n-butanol into the lower layer solution, performing heating, separating the produced water with a water segregator, carrying out heat preservation reaction, then raising the temperature, and carrying out heat preservation reaction; and finally conducting pressure reduction distillation to remove excess n-butanol, and collecting 75DEG C / 39.9Pa fractions, thus obtaining ethyl phosphinic acid n-butyl 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 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. 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 a reactive phosphorus-based flame retardant n-butyl ethylphosphinate, which has a simp...

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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.