Research On Preparation Of Flame Retardant Epoxy Containing-Phosphorus

3-Chloro-1,2-propanediol(3-MCPD) was synthesized with glycerol and hydrochloric acid as raw materials by the catalyst of acetic acid. The effects of mole ratio, reaction temperature, reaction time, the amount of catalyst used on the yield of ionone were investigated to obtain the optimal reaction conditions. The optimum condition of the reaction:n(HCl): n(glycerol)=3.2:1, the amount of catalyst is 0.3%, reaction time is 12 h, the reaction temperature is 100℃. Repeatability of the experiment is made and it demonstrates that 3-MCPD can work steadily and obtain correct and reliable result. the average yield of 3-MCPD was 60.9%.3-MCPD was synthesized with Epichlorohydrin and water as raw materials by the catalyst of sulfuric acid. Through the central composite design experiments to study the synthetic technology of it and investigating the influence of synthetic reaction that ratio of reactants, content of catalyst, reactive temperature and time was also related to the experiment. The optimum conditions:n(H2O):n(ECH)=4.5:1, the amount of catalyst is 0.2%, reaction time is 3h, the reaction temperature is 100℃. Through the cycle first fraction, the average yield of 3-MCPD was 89.6%.NaOH and 3-MCPD were mixed together in the organic solvent XY-3 to produce glycidol. The catalyst-1 dosage was 0.5% (total weight percentage of total reactants), reaction temperature 30℃, n(NaOH):n(3-MCPD)=1.04:1, feeding time is 3h, holding time is 2h. Products epoxy value reached 1.27 eq/100g, the yield reached 56.9%.With glycidyl and phosphorus oxychloride as raw materials and toluene as solvent, the triethylamine as the acid conditions of low temperature prepared by direct esterification glycidyl phosphate (TGP) in the process. Obtained through factor screening experiment of the reaction 4 main factors:mole ratio, the amount of acid binding agent, reaction temperature, holding time. Through orthogonal design experiments to determine the optimum conditions:n (GLY):n(POCl3)=3.4:1, n(TEA):n(POCl3)=4.2:1, reaction temperature is 4℃, holding time 18 h. The product is colorless and transparent, the epoxy value is more than 1.0 eq/100g, the moisture of 0.064%. By IR and NMR characterization of the compounds identified three glycidyl phosphate (TGP). Triethylamine hydrochloride reaction with sodium hydroxide solution, by atmospheric distillation, collecting between 80～90℃fractions, recycling acid binding agent triethylamine.