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以4,4’-二氨基二苯甲烷为原料,通过乙酰化反应、烷基化反应、去乙酰化反应,合成了3,3’-二叔丁基-4,4’-二氨基二苯甲烷,采用FTIR证实了其分子结构。通过产率测定研究了各反应阶段的影响因素,确定最佳反应条件:乙酰化反应中,在反应温度215℃下,乙酸过量200%,产率达97%;烷基化反应中,以N,N’-二甲基甲酰胺(DMF)为溶剂,无水三氯化铝为催化剂,在25℃反应温度下,产率达92%;去乙酰化反应中,采用浓盐酸加热,冰浴析出法,产率达98%。通过向4,4’-二氨基二苯甲烷的苯环上引入大体积的叔丁基,提高双马来酰亚胺树脂单体在普通溶剂中的溶解能力,降低预聚体粘度,以便于双马来酰亚胺树脂应用传递模塑成型工艺(RTM)加工。
Using 4,4’-diaminodiphenylmethane as starting material, acetylation reaction, alkylation reaction and deacetylation reaction were carried out to synthesize 3,3’-di-tert-butyl-4,4’-diaminodiphenyl Methane, confirmed by FTIR its molecular structure. Through the determination of yield, the influencing factors of each reaction stage were studied, and the optimum reaction conditions were determined. In the acetylation reaction, the excess of acetic acid was 200% at the reaction temperature of 215 ℃ and the yield was 97%. In the alkylation reaction, , N’-dimethylformamide (DMF) as solvent and anhydrous aluminum trichloride as catalyst, the yield was 92% at the reaction temperature of 25 ℃. In the deacetylation reaction, Precipitation method, the yield of 98%. By introducing a large volume of tert-butyl onto the benzene ring of 4,4’-diaminodiphenylmethane, the ability of the bismaleimide resin monomer to dissolve in ordinary solvents is increased and the viscosity of the prepolymer is reduced to facilitate Bismaleimide resins should be processed using transfer molding (RTM).