Preparation method of alkyl aromatic aldehyde
A technology of alkyl aromatic aldehyde and alkyl aromatic, applied in the field of preparation of alkyl aromatic aldehyde
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Embodiment 1
[0054] This example is used to prepare an alkylaromatic aldehyde reaction product mixture and to isolate the alkylaromatic aldehyde.
[0055] Add 33.3 g of C to a 100 ml zirconium autoclave 3 h 10 NCl-AlCl 3 Ionic liquid (C 3 h 10 NCl and AlCl 3 The molar ratio is 1:2) and 5.7 milliliters (0.0537 moles) of toluene, after replacing the air in the kettle with nitrogen, the partial pressure of carbon monoxide is raised to 3.0 MPa. , and reacted for 1.0 hour to obtain a reaction product mixture. Gas chromatographic analysis showed that the conversion rate of toluene was 56.4%, and the selectivity of p-methylbenzaldehyde was 88.0%. The selectivity of the alkyl aromatic aldehyde is calculated by the percentage content of the alkyl aromatic aldehyde after removing the unconverted alkyl aromatic compound in the product.
[0056] Add 5 milliliters of the reaction product mixture obtained above in a 100 milliliter conical flask, and add 20 milliliters of toluene and stir and mix ...
Embodiment 2
[0058] This example is used to prepare an alkylaromatic aldehyde reaction product mixture and to isolate the alkylaromatic aldehyde.
[0059] Prepare and separate tolualdehyde according to the method of Example 1, the difference is that when separating, add 5 milliliters of the reaction product mixture that embodiment 1 obtains in the Erlenmeyer flask of 100 milliliters, and add C 3 h 10 NCl, make the mixture C 3 h 10 NCl and AlCl 3 The molar ratio is 2:1. Then 20 ml of toluene was added, stirred and mixed for 10 minutes, the phases were separated at rest, and the upper and lower layers were separated using a separatory funnel. Analysis of the upper strata toluene solution with the internal standard method showed that the extraction rate of tolualdehyde was 80.5%. Then the filtrate was distilled at 120° C. and 0.02 MPa for 0.5 hour to obtain 0.34 gram of p-tolualdehyde.
Embodiment 3
[0069] This example is used to prepare an alkylaromatic aldehyde reaction product mixture and to isolate the alkylaromatic aldehyde.
[0070] Add 36.5 g of C to a 100 ml zirconium autoclave 6 h 16 NCl-AlCl 3 Ionic liquid (C 6 h 16 NCl and AlCl 3 The molar ratio is 1:2) and 5.7 milliliters (0.0537 moles) of toluene, after replacing the air in the kettle with nitrogen, the partial pressure of carbon monoxide is raised to 3.0 MPa. , and reacted for 1.0 hour to obtain a reaction product mixture. Gas chromatographic analysis showed that the conversion rate of toluene was 52.8%, and the selectivity of p-methylbenzaldehyde was 87.6%.
[0071] Add 5 milliliters of the reaction product mixture obtained above in a 100 milliliter Erlenmeyer flask, and add 20 milliliters of xylene and stir and mix for 10 minutes, static phase separation, and separate the upper extract phase and the lower raffinate phase with a separatory funnel. Analyze the product in the upper layer extraction pha...
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