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Method for preparing caprolactam

A technology of caprolactam and cyclohexanone oxime, which is applied in the field of preparation of caprolactam, can solve the problems of catalyst surface coking, etc., and achieve the effects of improving production efficiency, reducing the risk of device shutdown, and reducing catalyst coking

Pending Publication Date: 2022-05-17
JIANGSU YANGNONG CHEM GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The main purpose of the present invention is to provide a method for preparing caprolactam, so as to improve the method for preparing caprolactam by gas-phase Beckmann rearrangement reaction in a fixed bed. The condensation and carbonization of cyclohexanone oxime in the feeding process will cause the surface of the catalyst to The problem of coking

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  • Method for preparing caprolactam
  • Method for preparing caprolactam
  • Method for preparing caprolactam

Examples

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preparation example Construction

[0029] In the method for preparing caprolactam provided by the application, the carrier gas is used to gasify cyclohexanone oxime to obtain a gasified product, and then the cyclohexanone oxime is transported in the gasified product to a multi-phase communication network under the action of the carrier gas. The gas-phase Beckmann rearrangement reaction occurs in the fixed-bed reactor. Due to the gasification of the carrier gas, the concentration of cyclohexanone oxime decreases at high temperature, so the non-toxicity that occurs during the single feeding process of cyclohexanone oxime is effectively controlled. Catalytic carbonization phenomenon, thereby effectively reducing catalyst coking and deactivation, prolonging catalyst service life, thereby reducing the risk of device shutdown caused by catalyst replacement, and improving the production efficiency of caprolactam.

[0030] Typically but not limitatively, the above n is 2, 3, 4, 5 or 6, for example.

[0031] In order to...

Embodiment 1

[0057] This embodiment provides a method for preparing caprolactam, the process flow diagram is as follows figure 1 shown, including the following steps:

[0058] (1) The cyclohexanone oxime methanol solution with a water content of 1% and a concentration of 20% are mixed and gasified in the falling film evaporator 201 to obtain a gasified product; wherein, the gasification temperature is 175° C. and the pressure is 0.25 MPaG, the molar ratio of nitrogen to cyclohexanone oxime is 15:1.

[0059] (2) The gasification is divided into the first gasification, the second gasification and the third gasification, the mass ratio of the three is 50:25:25, and the three gasifications are respectively passed into the reactor for gas-phase Beckmann rearrangement Reaction, the mass space velocity of cyclohexanone oxime is 1h -1 , the temperature in the reactor is 360°C, and the pressure is 0.25MPa, such as figure 1 As shown, the reactor includes a first fixed bed layer 101, a second fixe...

Embodiment 2

[0061] This embodiment provides a method for preparing caprolactam, which is different from Example 1 in that in step (2), the gasified product is divided into a first gasified product and a second gasified product, and the mass ratio of the two is 60 : 40, and the reactor comprises the first fixed bed and the second fixed bed, the catalyst of two fixed bed equal loads is the same as embodiment 1, the top of the first fixed bed is provided with the first gasification product inlet, the second The top of the two fixed beds is provided with a second gasification feeding port, and the first gasification is added to the first fixed bed from the first gasification inlet to react to form the first reaction product, and the first reaction product is combined with the gasification from the second gasification The second gasified product fed into the feeding port is mixed and enters the second fixed bed for reaction to generate a second reaction product, which is discharged from the rea...

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Abstract

The invention provides a method for preparing caprolactam. The method comprises the steps that gasified matter containing cyclohexanone-oxime and carrier gas is conveyed into a reactor, the reactor is filled with a catalyst, the cyclohexanone-oxime is subjected to a gas-phase Beckmann rearrangement reaction under the catalytic action of the catalyst to generate caprolactam, the reactor comprises n fixed bed layers which are communicated in sequence, and n is a natural number; each fixed bed layer is filled with a catalyst, n is greater than or equal to 2 and less than or equal to 6, and n is a natural number. According to the technical scheme of the invention, cyclohexanone-oxime is conveyed into the reactor with the plurality of communicated fixed bed layers under the carrying action of the carrier gas for gas-phase Beckmann rearrangement reaction, so that the problems of condensation and carbonization in the feeding process of cyclohexanone-oxime can be effectively controlled, thereby effectively reducing catalyst coking and improving the yield of cyclohexanone-oxime. The service time of the catalyst is prolonged, so that the device shutdown risk caused by replacement of the catalyst is reduced, and the production efficiency of caprolactam is improved.

Description

technical field [0001] The invention relates to the field of petrochemical technology, in particular to a method for preparing caprolactam. Background technique [0002] Caprolactam is the key raw material for the production of nylon, nylon fiber and industrial cord products. Industrially, caprolactam is generally produced from cyclohexanone oxime. The preparation of caprolactam from cyclohexanone oxime mainly adopts sulfuric acid catalyzed liquid phase Beckmann rearrangement and MFI structure molecular sieve catalyzed gas phase Beckmann rearrangement reaction process. The liquid-phase Beckmann rearrangement process of cyclohexanone oxime needs to consume a large amount of sulfuric acid and ammonia water, and produce a large amount of low-value ammonium sulfate by-product, which will also cause equipment corrosion and environmental pollution. The gas-phase rearrangement of cyclohexanone oxime does not produce ammonium sulfate by-product, has the advantages of no equipment c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D201/04C07D223/10
CPCC07D201/04C07D223/10Y02P20/52
Inventor 王根林李良善丁克鸿徐林王铖梅学赓刘鑫邢志远陈耀坤郭博博何成义王鑫宇
Owner JIANGSU YANGNONG CHEM GROUP