Research On The Synthesis And Application Of Char-forming Agent And Flame Retardant Intermediates

Along with the human's more and more attention to protect the ecological environment and their own health,green technology to synthesis flame retardant has received extensive attention.Intumescent flame retardant with excellent performance occupies an important position in the field of flame retardants,and its important component-charring agent has become a research hotspot;Because of its unique properties,some of brominated flame retardants has not been fully replaced by halogen-free flame retardant.This paper studies and synthesis triazine charring agent(poly-2-ethanolamino-4,6-ethylenediamino-1,3,5-triazine)and flame retardant intermediate(N-(allyl)-1,2,3,6-Tetrahydrophthalimide and 2,2',6,6'-tetrabromobisphenol A diallyl ether)by a green process,and simplify the process.The green synthesis progess of triazine charring agent:poly-2-ethanolamino-4,6-ethylenediamino-1,3,5-triazine was studied.Discuss factors such as reaction solvent,reaction temperature,reaction time,pH and so on by using the orthogonal experiment and single factor experiment,the optimum technological conditions were determined.This progess happened in three steps,The optimal reaction conditions was:the first step was happened at 0-5? for 6 h with the pH 6-7,then rise the temperature to 40-50?,react 7 h;the third step was happened at 100-105? for 10 h.Under the optimum conditions,the yield can reach up to 94.4%.ESI-MS and IR were used to characterize their chemical structures,matching with their target molecules.TG was used to detect on the thermal stability of poly-2-ethanolamino-4,6-ethylenediamino-1,3,5-triazine,the results show that it has good thermal stability.Synthesis the flame retardant intermediate:N-(allyl)-1,2,3,6-Tetrahydrophthalimide,and discuss factors such as reaction temperature,reaction time,the ratio of raw materials by using the orthogonal experiment and single factor experiment,the optimum technological conditions were determined.The first step was happened at 70? with reaction time 5 h,the ratio of raw materials(n(four hydrogen phthalimide):n(sodium hydroxide))was 1:1.5,yield up to 88.3%;the second step was happened at 80? with reaction time 8 h,the ratio of raw materials(n(intermediate(3-a):n(allyl chloride))was 1:2,yield up to 89.8%.ESI-MS,IR and 1H NMR were used to characterize their chemical structures,matching with their target molecules.The flame retardant intermediate:2,2',6,6'-tetrabromobisphenol A diallyl ether was synthesized only in water,and studied its reaction temperature,reaction time,the ratio of raw materials by single factor experiment,determined the progress can make a high yield of 98%only by one step.The optimal reaction condition was:The reaction was happened at 55? with reaction time 4.5 h,ally]chloride dosage was 0.136 mol,yield up to 98%,the product color was white.The application research of triazine charring agents shows that poly-2-ethanolamino-4,6-ethylenediamino-1,3,5-triazine which was based with ammonium polyphosphate have excellent water resistant property and excellent flame retardant effect.