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Ammoximation reaction of ketone or aldehyde

A technology of ammoximation reaction and aldoaminoxime, which is applied in the field of ammoximation reaction of ketones or aldehydes, can solve the problems that the efficiency is greatly affected by the concentration of the catalyst, difficult large-scale operation, and slow separation rate, etc., so as to reduce energy consumption , Prolong the regeneration cycle and improve the efficiency

Active Publication Date: 2010-06-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method provided by EP0496385 is difficult to carry out large-scale operation; the separation rate of the method provided by CN1432560A is relatively slow; the efficiency of membrane separation in the method provided by CN1324684A is greatly affected by the catalyst concentration

Method used

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  • Ammoximation reaction of ketone or aldehyde
  • Ammoximation reaction of ketone or aldehyde
  • Ammoximation reaction of ketone or aldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] For the reaction process, see figure 1 . The volume of the reactor is 500 liters, the diameter of the hydrocyclone is 10mm, 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.

[0066] Concrete feed parameter, separation system parameter and reaction result are as follows:

[0067] Cyclohexanone = 46 kg / hour

[0068] Hydrogen peroxide containing 27.5% by weight of hydrogen peroxide = 65 kg / hour

[0069] Tert-butanol (about 15w% water) = 120 kg / h

[0070] Liquid ammonia = 9 kg / hour

[0071] Reaction temperature = 83±1°C

[0072] Reaction pressure = 0.3MPa (gauge pressure)

[0073] Catalyst concentration = 3.2% by weight

[0074] The average residence time of the material in the reactor = 72 minutes

[0075] Filtration system recoil cycle = 30 minutes

[0076] Filtration system recoil time = 3 seconds

[0077] Slurry inlet pressur...

Embodiment 2

[0087] Reaction flow see figure 1 , other conditions were the same as in Example 1, and the fluxes of solid-liquid separation membranes under different catalyst concentrations of 0, 1.1, 3.2, 5.1, 8.3, and 9.8% by weight were investigated. The experimental results are shown in Table 1.

Embodiment 3

[0108] This example illustrates that the method provided by the present invention adopts the mode of two reactors connected in series. For the reaction process, see image 3 . The volumes of the two reactors are 500 liters respectively, and the two reactors are operated in series. The slurry in the first reactor enters the second reactor through the pressure difference, and the separation system after the second reactor is the same as in Example 1, and the type and size of the ceramic membrane and the hydrocyclone are the same as in Example 1.

[0109] Concrete feed parameter, separation system parameter and reaction result are as follows:

[0110] First Reactor (1)

[0111] Cyclohexanone = 46 kg / hour

[0112] Hydrogen peroxide containing 27.5% by weight of hydrogen peroxide = 62.8 kg / hour

[0113] Tert-butanol (about 15w% water) = 120 kg / h

[0114] Liquid ammonia = 9 kg / hour

[0115] Reaction temperature = 83±1°C

[0116] Reaction pressure = 0.3MPa (gauge pressure)

...

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Abstract

The invention relates to an ammoximation method of ketone or aldehyde, which comprises the step of making ketone or aldehyde, ammonia and peroxide take the ammoximation reaction in a reaction vessel in the existence of titanium silicon catalysts and reaction solvents. The invention is characterized in that in the method, the reaction pulp carries out the multi-stage liquid-solid separation through a hydraulic cyclone and an inorganic membrane or a metal sintering pipe, and the separated titanium silicon catalysts are sent back to the reaction vessel for recycled use. The method improves the solid-liquid separation efficiency, prolongs the regeneration period of separation assemblies, improves the permeation flux of separation components, and lowers the energy consumption and the investment of a solid-liquid separation system.

Description

technical field [0001] The present invention relates to a method for preparing ketoxime or aldoxime by ammoximation reaction of ketone or aldehyde, and more particularly relates to the preparation of ketoxime or aldehyde by ammoximation reaction of ketone or aldehyde including the separation process of reaction product and catalyst Oxime method. Background technique [0002] Ketoxime or aldoxime is an important chemical raw material intermediate. Taking cyclohexanone oxime as an example, cyclohexanone oxime is an intermediate for the preparation of caprolactam, and caprolactam is a monomer and an important chemical raw material for the production of nylon 6. [0003] The preparation of cyclohexanone oxime is a key step in the production of caprolactam by cyclohexanone-hydroxylamine method. According to different preparation processes of hydroxylamine, there are hydroxylamine sulfate method (HSO), nitric oxide reduction method (NO method) and hydroxylamine phosphate method ...

Claims

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Application Information

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IPC IPC(8): C07C249/08C07C251/32B01J29/89
Inventor 李永祥吴巍杨克勇孙斌闵恩泽
Owner CHINA PETROLEUM & CHEM CORP
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