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Method and equipment for preparing caprolactam from cyclohexanone oxime

A technology of cyclohexanone oxime and caprolactam, which is applied in the field of preparing caprolactam, can solve the problems of uneven bed temperature, high operation cost, short operation period and the like, and achieves the effects of reducing temperature rise, eliminating coking and increasing relative content

Active Publication Date: 2009-05-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the disadvantages of large reaction temperature rise, uneven bed temperature, easy coking, short operation period, high operation cost, etc., and it is difficult to implement in industry

Method used

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  • Method and equipment for preparing caprolactam from cyclohexanone oxime
  • Method and equipment for preparing caprolactam from cyclohexanone oxime
  • Method and equipment for preparing caprolactam from cyclohexanone oxime

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Experimental program
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Effect test

Embodiment 1

[0046] Three fixed-bed reactors are connected in series as a multi-stage series reactor, and φ10, φ3 inert ceramic balls and 25kg of catalyst are respectively loaded from bottom to top, and the total catalyst loading capacity is 75kg. Nitrogen is used as the carrier gas, and the flow direction of the carrier gas and reaction raw materials is downward. Purge the system with nitrogen until the oxygen content is less than 0.3 %, and pressurized to a reaction pressure of 0.28MPa (g), start the circulating carrier gas compressor, and control the total flow of circulating nitrogen entering the reactor to be 410Nm 3 / h. After the system is stable, start the carrier gas heater to heat the carrier gas to 380-400°C. Add circulating methanol solvent to the circulating carrier gas at a flow rate of 75kg / h, and continuously inject 0.63L / h deionized water from the inlet of the first reactor. Divide into 3 equal parts, enter the inlet pipelines of three reactors respectively, mix with th...

Embodiment 2

[0048] According to the same method of embodiment 1, the feed flow rate of cyclohexanone oxime is increased to 150Kg / h by 75kg / h, and the water injection rate is increased to 1.2L / h by 0.63L / h, and other conditions are the same as embodiment 1, corresponding The changes of space velocity, total nitrogen oxime ratio, alcohol oxime ratio and reaction results are summarized in Table 1.

Embodiment 3

[0050] According to the same method of embodiment 1, the feed flow rate of cyclohexanone oxime is reduced to 45Kg / h by 75Kg / h, other conditions are identical with embodiment 1, the change of corresponding space velocity, total nitrogen oxime ratio, alcohol oxime ratio and The reaction results are summarized in Table 1.

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Abstract

The invention relates to a method for preparing caprolactam with cyclohexanone-oxime, and a device used in the method. The method includes the steps as follows: after being heated, inert supporting gas containing a solvent is continuously put into a supporting gas intake of a first-class reactor of a multi-stage series reactor provided with a catalyst. Cyclohexanone- oxime is directly divided into two parts which then enter all stages of the multi-stage series reactor, thereby ensuring that reaction effluents are cooled. The supporting gas is separated and recycled to the supporting gas intake of the first-class reactor, and then products from a liquid phase reaction are separated and purified.

Description

technical field [0001] The invention relates to a method for preparing caprolactam from cyclohexanone oxime and equipment used in the method. More specifically, the present invention relates to a method for preparing caprolactam by gas-phase Beckmann rearrangement reaction of cyclohexanone oxime and the equipment used in the method. Background technique [0002] The conversion of cyclohexanone oxime to caprolactam through liquid-phase Beckmann rearrangement reaction is a technology commonly used in industry at present, and the catalyst is mostly concentrated sulfuric acid or oleum. The selectivity of the method to caprolactam can reach more than 98.5%. The caprolactam produced by this method accounts for about 90% of the caprolactam production in the world. The biggest disadvantage of this method is that a large amount of low-value ammonium sulfate is produced by-product, followed by serious equipment corrosion and environmental pollution. [0003] Aiming at the shortcomi...

Claims

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Application Information

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IPC IPC(8): C07D201/04C07D223/10
Inventor 杨克勇付锦晖孙斌程时标张树忠吴巍
Owner CHINA PETROLEUM & CHEM CORP
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