Synthesis Research Of Triazine Flame Retardant

Tris(2,4,6-tribromophenoxy)-triazine is an excellent performance flame retardant which contained bromine and nitrogen. This text studies the tris(2,4,6-tribromophenoxy)-triazine synthetic reaction system and conditions that tribromophenol and cyanuric chloride as raw materials, and characterize it's physical and chemical property.This experiment discuss the synthesis condition of tris(2,4,6-tribromophenoxy)-triazine with acetone, ethyl acetate, mixture of water and dichloromethane as the solvent. (1)Reaction steps in acetone solution as follows: the reaction ratio of raw materials is nsodium hydroxide∶ntribromophenol∶ncyanuric chloride =3.2∶3.1∶1; drop cyanuric chloride solution into the tribormophenol sodium salt solution; reacts at refluxing temperature for 3 h; the melting point of product is 230℃and yield is 98%. (2)Reaction steps in ethyl acetate solution as follows: the reaction ratio of raw materials is nsodium hydroxide∶ntribromophenol∶ncyanuric chloride =3.2∶3.1∶1 ; drop cyanuric chloride solution into the tribormophenol sodium salt solution; reacts at refluxing temperature for 3 h; the melting point of product is 230℃and yield is 94%. (3)Reaction steps in water and dichloromethane mixed solution with phase catalyst as follows: the reaction ratio of raw materials is nsodium hydroxide∶ntribromophenol∶ncyanuric chloride =3.1∶3.05∶1; drop cyanuric chloride solution into the tribormophenol sodium salt solution; reacts at 10℃for 1 h and then at refluxing temperature for 1.5 h; the melting point of product is 229℃and yield is 94%. (4)When the optimization process is determined, the product's physical-chemical property need characterization:the whiteness of product is 98; elemental analysis indicates that the bromine content is 66.81%, the nitrogen 3.82%, the carbon 22.93%, the hydrogen 0.71%, all these prove the purity of product access 99%; TG analysis indicates that the temperature is 287℃when the weight of product losing 1%, the decomposition temperature is 405℃, all these prove that it meet the application requirement of flame retardant; IR analysis indicates that the spectrum of product is the same with the standard; the 1H-NMR and 13C-NMR indicates that the product contains 6 hydrogen and 5 chemical equivalent of cabon; the IR and NMR spectrum ascertain that the product is Tris- (2,4,6-tribromophenoxy)-triazine.