Production device and production method of caprolactam

A caprolactam, production device technology, applied to the preparation of lactam, separation/purification of lactam, chemical instruments and methods, etc., can solve the problem of low conversion rate of cyclohexanone oxime, easy deactivation of catalyst, catalyst replacement and device shutdown risk, etc.

Pending Publication Date: 2020-12-15
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0023] The purpose of the present invention is to overcome the low conversion rate of cyclohexanone oxime existing in the prior art, the difficulty in separating the remaining cyclohexanone oxime, and the catalyst in the fixed bed is easily deactivated, resulting in the r

Method used

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  • Production device and production method of caprolactam
  • Production device and production method of caprolactam
  • Production device and production method of caprolactam

Examples

Experimental program
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Embodiment approach

[0089] According to a preferred embodiment provided by the present invention, the production device of the caprolactam, such as figure 1 As shown, it includes: cyclohexanone oxime evaporation gasification system 4, mist separation system, fluidized bed reaction system, moving bed reaction system 13 connected in series;

[0090] The device also includes a reaction solvent recovery circulation system and a carrier gas recovery circulation system, the reaction solvent recovery circulation system is used to recover the solvent, and the carrier gas recovery circulation system is used to recover the carrier gas;

[0091] The cyclohexanone oxime evaporation gasification system 4 is provided with a carrier gas inlet 1, an ethanol inlet 2 and a cyclohexanone oxime inlet 3; the ethanol inlet 2 includes a first ethanol inlet and a second ethanol inlet, and the first ethanol The inlet and the carrier gas inlet 1 are set to the same inlet so that part of the ethanol and the carrier gas are...

specific Embodiment approach

[0130] The present invention has a wide selection range for the content of silicon and oxygen in the molecular sieve. In a specific embodiment, based on the total amount of molecular sieve, in the molecular sieve, the content of silicon, oxygen and metal The sum of the contents of the elements is 100%.

[0131] According to a preferred embodiment of the present invention, based on the total amount of molecular sieves, the content of the metal elements in the molecular sieves is 6-90 μg / g, preferably 30-80 μg / g. Specifically, for example, 30 μg / g, 35 μg / g, 40 μg / g, 45 μg / g, 50 μg / g, 55 μg / g, 60 μg / g, 70 μg / g, 75 μg / g, 80 μg / g, and among these values Any value in the range formed by any two of . In this preferred embodiment, the catalytic performance of the catalyst is better, which is more conducive to improving the conversion rate of cyclohexanone oxime and the selectivity of caprolactam. In the present invention, if the content of the metal element is too much, it is possib...

preparation example 1

[0261] Preparation example 1 (spray molding)

[0262] (1) 482kg content is that the ethanol of 95% by weight and the tetrapropyl ammonium hydroxide aqueous solution that 302kg content is 22.5% by weight are added respectively to 2M 3 In the stainless steel reaction kettle, stir, then add 347kg orthosilicate ethyl ester, continue to stir, then add 332kg water and 38.6 grams of Fe(NO 3 ) 3 9H 2 O, continue stirring for 4 hours at room temperature to obtain a colloidal mixture; wherein, SiO 2 The molar ratio of ethyl orthosilicate: ethanol: tetrapropylammonium hydroxide: water is 1:10:0.2:20; 2 The weight ratio of tetraethyl orthosilicate in terms of metal elements to the metal source in terms of metal elements is 18666:1;

[0263] (2) The above-mentioned colloidal mixture is subjected to ethanol-hydrothermal system crystallization, and the conditions of the crystallization include: first crystallize at 70°C for 1 day, and then crystallize at 100°C for 2 days; obtain crystall...

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Abstract

The invention relates to the field of caprolactam production, in particular to a caprolactam production device and method, and the device comprises a cyclohexanone-oxime evaporation and gasification system, a mist separation system, a fluidized bed reaction system and a moving bed reaction system which are connected in series; the device further comprises a reaction solvent recycling system and acarrier gas recycling system. The method comprises the following steps: (1) evaporating and gasifying carrier gas, ethanol and cyclohexanone-oxime in a cyclohexanone-oxime evaporation and gasificationsystem; (2) feeding a gas-phase material flow obtained in the step (1) into a mist separation device to gasify cyclohexanone-oxime which is not completely gasified in a cyclohexanone-oxime evaporation and gasification system; (3) feeding the material flow obtained in the step (2) into a fluidized bed reaction system and a moving bed reaction system in sequence for gas-phase Beckmann rearrangementreaction; and (4) recovering ethanol and carrier gas in the material flow obtained in the step (3). By adopting the device and the method, the high conversion rate of cyclohexanone-oxime can be obtained, the problem of catalyst discharge is avoided, and the production is not interrupted.

Description

technical field [0001] The invention relates to the field of caprolactam production, in particular to a caprolactam production device and production method. Background technique [0002] Caprolactam is the main raw material for the production of three series of products: nylon, industrial cord and nylon engineering plastics. Its demand has been relatively high, and it is generally prepared through the Beckmann rearrangement reaction of cyclohexanone oxime. At present, the liquid phase rearrangement process using concentrated sulfuric acid or oleum as a catalyst is usually used in industry. The caprolactam produced by this process accounts for about 90% of the world's total production of caprolactam, but this process needs to consume a large amount of sulfuric acid and ammonia water. For every ton of caprolactam produced, 1.3-1.8 tons of ammonium sulfate will be produced as a by-product. The production cost is relatively high, and the use of sulfuric acid will also cause prob...

Claims

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Application Information

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IPC IPC(8): C07D201/06C07D201/16C07D223/10
CPCC07D201/06C07D201/16C07D223/10Y02P20/52
Inventor 程时标沈飞王韩张新平王洪营蒋肇斌胡志敏张忠光唐席
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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