Method for preparing methylcyclohexyl diisocyanate
A technology of methyl cyclohexyl diisocyanate and methyl cyclohexyl diamine, which is applied in the field of non-phosgene preparation of methyl cyclohexyl diisocyanate, can solve the problems of long process route, poor safety, complicated technology and the like, and achieves simplified process, Easy to operate, simple effect of exhaust gas treatment
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Embodiment 1
[0024] 300 ml o-dichlorobenzene solution containing 128.26 g (1 mole) of methylcyclohexyldiamine isomer mixture and 300 ml o-dichlorobenzene containing 396 g (1.34 mole) bis(trichloromethyl)carbonate The solutions were slowly added into 1000 ml three-neck flasks, and the temperature of the reaction system was controlled below 50 °C during the dropwise addition. After the dropwise addition, the temperature was raised to reflux for 3 hours. After the solvent was distilled off under reduced pressure, the distillate product at 126-131°C / 2 mmHg was collected by rectification. The content of methylcyclohexyl diisocyanate analyzed by GC is 96.8%.
Embodiment 2
[0026]Slowly add 300 ml of benzonitrile solution containing 128.23 g (1 mol) of methylcyclohexyldiamine isomer mixture to 300 ml of benzonitrile containing 396.2 g (1.34 mol) of bis(trichloromethyl)carbonate solution. During the dropwise addition, the temperature of the reaction system was controlled below 50 °C. After the dropwise addition was completed, the temperature was raised to reflux, and kept at this temperature for 3 hours under reflux. After distilling off the solvent, rectify and collect the distillate product at 125-130 ℃ / 2mmHg. GC analysis showed that the content of methylcyclohexyl diisocyanate isomer mixture was 96.1%.
Embodiment 3
[0028] Add 100 ml of benzonitrile in the reaction flask, heat up to 160 ° C, and dissolve 300 ml of benzonitrile containing 128.3 g (1 mole) of methylcyclohexyldiamine isomer mixture into 250 ml of benzonitrile containing 148.5 g (0.5 mole of ) The benzonitrile solution of bis(trichloromethyl)carbonate was added to the reaction flask at the same time. Add dropwise within 3.5 hours at 160-165°C, then add 250 ml of benzonitrile solution containing 148.6 g (0.5 mol) bis(trichloromethyl)carbonate dropwise at the same temperature, and keep warm for 3 hours after adding . After distilling off the solvent, rectification collected the distillate product at 122-132 ℃ / 1.5 mmHg. GC analysis showed that the content of methylcyclohexyl diisocyanate isomer mixture was 86.5%.
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