Cyclic oxidation method and cyclic oxidation device for preparing epsilon-caprolactone

Abstract

The invention provides a cyclic oxidation method and a cyclic oxidation device for preparing epsilon-caprolactone. A reactor adopts a fixed bed with a jacket or adopts a tubular reactor, and is filledwith a solid acid. A hydrogen peroxide reaction liquid, a cleaning liquid and a cyclohexanone solution sequentially flows through the reactor in sequence to complete a synthesis reaction of epsilon-caprolactone, the cleaning liquid flows through the reactor finally to complete regeneration, and a next cycle is started. A novel solid peroxy acid oxidation technology used in the invention makes residual water and a sulfuric acid catalyst simply washed off by using an anhydrous solvent, and the used solid organic peroxy acid can be recycled after being washed with a simple solvent washing, so peroxy acid and water residues are avoided, the energy consumption and danger are reduced, and the product quality can be guaranteed.

Description

technical field [0001] The invention relates to the technical field of ε-caprolactone production, in particular to a cyclic oxidation method and equipment for preparing ε-caprolactone. Background technique [0002] The most well-established ε-caprolactone is usually prepared by the Bayer-Williger reaction of cyclohexanone with peroxyacids. The method for preparing peroxyacids at low cost in industry is to react aqueous hydrogen peroxide solution with organic acids under the catalysis of sulfuric acid to prepare corresponding peroxyacids. However, the catalyst sulfuric acid residue in this process is unfavorable to the subsequent reaction, and a large amount of water in the system must be removed. Therefore, rectification of the peroxyacid aqueous solution is required to remove water, and there is a large safety hazard. In another process using weak acid catalysis to prepare peroxyacid, the removal of water still needs to be carried out with water-carrying agent and vacuum d...

AI Technical Summary

Problems solved by technology

However, the catalyst sulfuric acid residue in this process is unfavorable to the subsequent reaction, and a large amount of water in the system must be removed, so the peroxyacid aqueous solution is required to remove water by rectification, and there is a large potential safety hazard

In another process using weak acid catalysis to prepare peroxyacid, the removal of water still needs to be carried out with water-carrying agent and vacuum distillation, which increases the energy consumption of the system and the water is not easy to remove.

In addition, the residual peroxyacid after the peroxyacid oxidation of cyclohexanone must be removed to ensure the safety of the subsequent rectification system, so the energy consumption and risk factor of the entire process are relatively high

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