Preparation method of cyclohexanone oxime

A technology of cyclohexanone oxime and cyclohexanone, which is applied in the field of preparation of cyclohexanone oxime, can solve the problems of reduced effective utilization rate of catalyst, complex process, easy adhesion, etc., achieve high solid-liquid separation efficiency, improve reaction efficiency, The effect of increasing the heat transfer rate

Active Publication Date: 2008-02-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is complicated and the production cost is high
[0008] To sum up, when the trickle bed is operated, on the one hand, there are higher requirements for the uniform distribution of the feed liquid, and on the other hand, there are higher requirements for the strength of the catalyst, and the catalyst must have a long life; The use of binders will block a part of the pores of the molecular sieve, resulting in a decrease in pore volume and specific surface area, which will eventually lead to a decrease in the effective utilization of the molecular sieve catalyst, and the reaction effect will decrease under the same catalyst concentration; The porous plate directly intercepts the catalyst, and there is no automatic backflushing syst

Method used

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  • Preparation method of cyclohexanone oxime
  • Preparation method of cyclohexanone oxime
  • Preparation method of cyclohexanone oxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] See Figure 1 for the reaction process. The effective volume of the reactor is 5 liters, the separation element is an inorganic ceramic membrane tube with 19 channels φ4, and the effective filtration area is 0.2m 2 , The slurry is forced to circulate by a circulation pump, the reaction raw materials and reaction products are continuously fed into and out of the reactor, the catalyst is added at one time, and the heat exchange through the jacket is used to maintain isothermal operation.

[0061] Concrete feed parameter, separation system parameter and reaction result are as follows:

[0062] Cyclohexanone = 620 g / h

[0063] Tert-butanol (about 15w% water) = 3000 g / h

[0064] 27.5w% hydrogen peroxide = 860 g / hour

[0065] Liquid ammonia = 180 g / h

[0066] Reaction temperature = 83±1°C

[0067] Reaction pressure = 0.3MPa (gauge pressure)

[0068] Slurry linear velocity in the ring pipe = 2 m / s

[0069] Catalyst concentration = 3% by weight

[0070] The average resid...

Embodiment 2

[0081] The reaction process is shown in Figure 1, and the specific feed parameters, separation system parameters and reaction results are as follows:

[0082] Cyclohexanone = 750 g / h

[0083] Tert-butanol (about 15w% water) = 3500 g / h

[0084] 27.5w% hydrogen peroxide = 995 g / hour

[0085] Liquid ammonia = 170 g / h

[0086] Reaction temperature = 76±1°C

[0087] Reaction pressure = 0.4MPa (gauge pressure)

[0088] Slurry linear velocity in the ring pipe = 2 m / s

[0089] Catalyst concentration = 2% by weight

[0090] The average residence time of the material in the reactor = 50 minutes

[0091] Filtration system recoil cycle = 30 minutes

[0092] Filtration system recoil time = 2 seconds

[0093] Its reaction result is as follows:

[0094] Cyclohexanone conversion = 97.3%

[0095] Hydrogen peroxide conversion rate = 98.6%

[0096] Reaction selectivity in terms of cyclohexanone = 99.1%

[0097] Effective utilization rate of hydrogen peroxide = 90.6%

[0098] Cyclohexa...

Embodiment 3

[0101] The reaction process is shown in Figure 1, and the specific feed parameters, separation system parameters and reaction results are as follows:

[0102] Cyclohexanone = 500 g / h

[0103] Tert-butanol (about 15w% water) = 2400 g / h

[0104] 27.5w% hydrogen peroxide = 725g / hour

[0105] Liquid ammonia = 130 g / h

[0106] Reaction temperature = 89±1°C

[0107] Reaction pressure = 0.2MPa (gauge pressure)

[0108] Slurry linear velocity in the ring pipe = 2 m / s

[0109] Catalyst concentration = 4% by weight

[0110] The average residence time of the material in the reactor = 78 minutes

[0111] Filtration system recoil cycle = 20 minutes

[0112] Filtration system recoil time = 2 seconds

[0113] Its reaction result is as follows:

[0114] Cyclohexanone conversion = 99.4%

[0115] Hydrogen peroxide conversion rate = 100%

[0116] Reaction selectivity in terms of cyclohexanone = 98.6%

[0117] Effective utilization rate of hydrogen peroxide = 87.0%

[0118] Cyclohexa...

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Abstract

The invention discloses a preparation process for cyclohexanone oxime which is characterized in that the process is carried out continuously and circularly in a loop reactor, wherein the loop reactor consists of a loop and a solid-liquid separating component and makes the reaction slurry comprising catalyzer, ammonia, cyclohexanone, hydrogen peroxide and solvent have an ammoximation reaction in the loop, then the reaction slurry is made a solid-liquid separation by a filtering element in the solid-liquid separating component in a cross-current way, the obtained clear liquid flows out along the radial direction of the filtering element and is reclaimed, the concentrated slurry continues to circulate in the loop.

Description

technical field [0001] The present invention relates to the preparation method of cyclohexanone oxime, more specifically, the present invention relates to the method for preparing cyclohexanone oxime by ammoximation of cyclohexanone. Background technique [0002] Caprolactam is a monomer raw material for the production of nylon 6 fiber and nylon 6 engineering plastics. At present, there are three process routes for industrial production of caprolactam: (1) Cyclohexanone-hydroxylamine production process, including traditional Raschig process, DSM / HPO process, BASF-NO reduction process, Inventa-NO reduction process, Allied cumene / phenol (2) Cyclohexane photonitrosation process of Japan Toray Company; (3) Toluene process of SNIA Company of Italy. Among them, the production capacity of the cyclohexanone-hydroxylamine route accounts for 91.3% of the total capacity of the world's devices. [0003] The production of caprolactam by the cyclohexanone-hydroxylamine route is based on...

Claims

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Application Information

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IPC IPC(8): C07C249/08C07C251/44B01J29/89
Inventor 李永祥吴巍孙斌闵恩泽
Owner CHINA PETROLEUM & CHEM CORP
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