Novel method for synthesizing 4,4'-diaminodiphenyl-methane compound
A technology of diaminodiphenylmethane and compound, which is applied in the field of polymer material synthesis, can solve the problems of high temperature requirements, equipment corrosion and high energy consumption, achieve obvious economic and social benefits, mild reaction conditions and simple processing technology. Effect
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example 1
[0033] Add 5g of the catalyst prepared above into a 500ml three-neck flask equipped with a thermometer, reflux device and stirring, add 150g of water, 48.3g (0.4mol) of o-ethylaniline, 50g of toluene, start stirring and raise the temperature to 40°C, and start adding the concentration 16.2g (0.2mol) of 37% formaldehyde aqueous solution was added dropwise for 30 minutes. After the formaldehyde was added dropwise, the temperature was raised to 80°C and the reaction was maintained for 2 hours. Add 30g of toluene after completion of the reaction, stir for 3 minutes, then filter, the filtrate is allowed to stand for stratification to separate the oil layer, the filter cake is washed with a small amount of toluene, the resulting washing liquid is combined with the oil layer, washed twice with hot water, and evaporated under reduced pressure. Toluene and unreacted o-ethylaniline were removed to obtain 47.8 g of brown-yellow viscous liquid. The content of 3,3'-diethyl-4,4'-diaminodiph...
example 2
[0035] Add 5g of the catalyst prepared above into a 500ml three-necked flask equipped with a thermometer, reflux device and stirring, add 150g of water, 59.6g (0.4mol) of 2,6-diethylaniline, and 60g of xylene, start stirring and raise the temperature to 40°C , began to drop 16.2g (0.2mol) of formaldehyde solution with a concentration of 37%, and the dropwise addition took 30 minutes. After the dropwise addition of formaldehyde, the temperature was raised to 90°C and the reaction was maintained for 2.5 hours. After the reaction, add 30g of xylene, stir for 3 minutes, then filter, and the filtrate is allowed to stand for stratification to separate the oil layer. The filter cake is rinsed with 20g of xylene. The resulting washing liquid is combined with the oil layer and washed twice with hot water, and the oil layer is cooled and crystallized. , centrifugal filtration, and vacuum drying to obtain 58.2 g of off-white crystals. The melting point of the product is 87-91°C, the cont...
example 3
[0037] Add 5g of the catalyst prepared above into a 500ml three-neck flask equipped with a thermometer, reflux device and stirring, add 150g of water, 37.2g (0.4mol) of aniline, and 50g of toluene, start stirring and raise the temperature to 40°C, and start to add dropwise the concentration of 37% 16.2 g (0.2 mol) of formaldehyde aqueous solution was added dropwise for 30 minutes. After the formaldehyde was added dropwise, the temperature was raised to 85° C. and the reaction was maintained for 1 hour. After the reaction, add 30g of toluene, stir for 3 minutes, then filter, the filtrate is allowed to stand and separate the oil layer, and the filter cake is washed with 20g of toluene. Filter and dry in vacuo to obtain 36.9 g of off-white crystals. The melting point of the product is 88-91°C, the content of 4,4'-diaminodiphenylmethane is 98.75% and the yield is 93.18% according to high performance liquid chromatography analysis.
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