Separation and purification method for acetaldehyde oxime
A purification method and technology of acetaldehyde oxime, which is applied in the field of separation and purification of acetaldehyde oxime, can solve the problems that acetaldehyde oxime and cyclohexanone cannot be separated, and achieve the effects of high purity and yield, cost reduction and simple operation
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Embodiment 1
[0032] 1) Add cyclohexanone oxime and 70% mass concentration sulfuric acid (catalyst) to the reaction kettle, add anhydrous acetaldehyde dropwise in a low-temperature cold bath (4-10° C.), acetaldehyde: cyclohexanone oxime: 70% mass Concentration of sulfuric acid (molar ratio) = 1.5:1:0.01, after the anhydrous acetaldehyde is added dropwise, continue to stir and react at normal temperature and pressure for 2 hours to obtain the acetaldehyde oxime reaction solution, after the reaction is completed, immediately neutralize it with NaOH solid, Adjust the reaction solution pH=7;
[0033] 2) Add the above preparation reaction liquid to toluene and carry out rectification under reduced pressure. The molar ratio of toluene to acetaldehyde oxime is 2:1. The vacuum degree is 0.060-0.065Mpa, and the tower top temperature is 66-71°C to obtain acetaldehyde The mixed solution of toluene and acetaldehyde oxime with a mass fraction of 20%, continue to collect the fraction with a vacuum degree...
Embodiment 2
[0037] 1) Add cyclohexanone oxime and 70% mass concentration sulfuric acid (catalyst) to the reaction kettle, add anhydrous acetaldehyde dropwise in a low-temperature cold bath (4-10° C.), acetaldehyde: cyclohexanone oxime: 70% mass Concentration of sulfuric acid (molar ratio) = 1.5:1:0.01, after the anhydrous acetaldehyde is added dropwise, continue to stir and react at normal temperature and pressure for 2 hours to obtain the acetaldehyde oxime reaction solution, after the reaction is completed, immediately neutralize it with NaOH solid, Adjust the reaction solution pH=7;
[0038] 2) Add the above preparation reaction liquid to toluene and carry out rectification under reduced pressure. The molar ratio of toluene to acetaldehyde oxime is 4:1, and the vacuum degree is 0.060-0.065Mpa. The mixed solution of toluene and acetaldehyde oxime with a mass fraction of 20%, continue to collect the fraction with a vacuum degree of 0.06-0.065Mpa and a tower top temperature of 83-90°C to ...
Embodiment 3
[0042] 1) Add cyclohexanone oxime and 70% mass concentration sulfuric acid (catalyst) to the reaction kettle, add anhydrous acetaldehyde dropwise in a low-temperature cold bath (4-10° C.), acetaldehyde: cyclohexanone oxime: 70% mass Concentration of sulfuric acid (molar ratio) = 1.5:1:0.01, after the anhydrous acetaldehyde is added dropwise, continue to stir and react at normal temperature and pressure for 2 hours to obtain the acetaldehyde oxime reaction solution, after the reaction is completed, immediately neutralize it with NaOH solid, Adjust the reaction solution pH=7;
[0043]2) Add the above prepared reaction solution to toluene and carry out rectification under reduced pressure. The molar ratio of toluene to acetaldehyde oxime is 8:1. The vacuum degree is 0.060-0.065Mpa, and the tower top temperature is 66-71°C to obtain acetaldehyde oxime The mixed solution of toluene and acetaldehyde oxime with a mass fraction of 19% continues to collect fractions with a vacuum degre...
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