Resource utilization method of cyclohexanone-oxime gas-phase rearrangement product residues
A cyclohexanone oxime and recycling technology, applied in the field of caprolactam preparation, can solve the problem that caprolactam cannot be recovered, and achieve the effect of improving the overall recovery rate
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Embodiment 1
[0030] Pass the residue and water through the solution containing 40g B 2 o 3 -Al 2 o 3 Fixed bed reactor with solid acid catalyst, the residue enters the reactor from the upper end of the reactor, water enters the reactor from the lower end of the reactor, the mass ratio of water to residue is 10:1, and the weight hourly space velocity of residue is 0.5h -1 , normal pressure reaction, the reaction temperature is 300 ° C, the obtained hydrolysis reaction solution is removed from the top of the reactor, and the secondary residue is removed from the bottom of the reactor. Then carry out negative pressure dehydration on the depolymerization reaction solution at a pressure of 20kPa and a temperature of 100°C to obtain a dehydrated product; carry out negative pressure distillation on the dehydrated product at an absolute pressure of 0.5kPa and a temperature of 150°C. Finally, fractions are collected to obtain the caprolactam product. The obtained caprolactam product was analyze...
Embodiment 2
[0032] Pass the residue and water through a 45g SiO 2 Fixed bed reactor with solid acid catalyst, the residue enters the reactor from the upper end of the reactor, water enters the reactor from the lower end of the reactor, the mass ratio of water to residue is 5:1, and the weight hourly space velocity of residue is 1h -1 , the reaction pressure is 80kPa, the reaction temperature is 320°C, the obtained hydrolysis reaction solution is removed from the top of the reactor, and the secondary residue is removed from the bottom of the reactor. Then carry out negative pressure dehydration on the depolymerization reaction solution at a pressure of 15kPa and a temperature of 80°C to obtain a dehydrated product; carry out negative pressure distillation on the dehydrated product at an absolute pressure of 0.8kPa and a temperature of 140°C. Finally, fractions are collected to obtain the caprolactam product. The obtained caprolactam product was analyzed, and the weight recovery rate of ca...
Embodiment 3
[0034] Pass the residue and water through a 50g SiO 2 -Al 2 o 3 Fixed bed reactor with solid acid catalyst, the residue enters the reactor from the upper end of the reactor, water enters the reactor from the lower end of the reactor, the mass ratio of water to residue is 3:1, and the weight hourly space velocity of residue is 1.5h -1 , the reaction pressure is 1MPa, the reaction temperature is 300°C, the obtained hydrolysis reaction solution is removed from the top of the reactor, and the secondary residue is removed from the bottom of the reactor. Then carry out negative pressure dehydration on the depolymerization reaction solution at a pressure of 15kPa and a temperature of 100°C to obtain a dehydrated product; carry out negative pressure distillation on the dehydrated product at an absolute pressure of 0.5kPa and a temperature of 130°C. Finally, fractions are collected to obtain the caprolactam product, and the remainder is secondary residue. The obtained caprolactam pr...
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