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Oxaamidination method of oxo-compound

A technology for carbonyl compounds and substances, applied in the field of ammoximation of carbonyl compounds, can solve the problems of catalyst deactivation, shortening of catalyst stable operation time, reduction of catalyst recovery rate, etc., so as to extend catalyst life, improve stable operation time, and reduce catalyst inactive effect

Inactive Publication Date: 2006-03-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In the above-mentioned ammoximation reaction of carbonyl compounds, due to the loss of silicon dissolution in the catalyst, it will cause the adverse effects of shortening the stable operation time of the catalyst and reducing the recovery rate of the catalyst. However, although the silicon dissolution of the molecular sieve caused by ammonia is the catalyst deactivation First and foremost factor, but adding acid solid as described in CN1345718A in the system, but can not solve catalyst deactivation problem as the silica gel of solid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] This example is the process of preparing cyclohexanone oxime by ammoximation of cyclohexanone, and the catalyst is titanium silicon (TS-1) molecular sieve raw powder.

[0028] The reaction kettle has a volume of 150ml, is stirred by magnetic force, and is heated by an oil bath. The reaction raw materials and reaction products are continuously fed into and out of the reactor, and the molecular sieve is intercepted in the reactor.

[0029] The process parameters are as follows H 2 o 2: cyclohexanone=1.10:1 (molar ratio), ammonia: cyclohexanone=1.70:1 (molar ratio), tert-butanol: cyclohexanone=3.30:1 (molar ratio), silicon content=35ppm in the reaction solution , the catalyst concentration is 1.8% by weight, the average residence time of materials is 72min, the reaction temperature is 76±1°C, the reaction pressure is normal pressure, and the silica sol is added continuously. The reaction results are shown in Table 1, wherein the stable operation time of the catalyst is ...

Embodiment 2

[0035] Repeat Example 1, except that toluene is used instead of tert-butanol as solvent, and an aqueous solution of ethyl orthosilicate (Beijing Chemical Reagent Company) is added, and the silicon content in the reaction solution is 1035 ppm. The reaction results are shown in Table 1.

Embodiment 3

[0037] Repeat Example 1, the difference is: 83 ± 1 ℃ of reaction temperature, reaction pressure 0.3Mpa, catalyst concentration is 2.0% by weight, H 2 o 2 The molar ratio to cyclohexanone is 1.08:1, and the silicon content in the reaction liquid is 100ppm. The reaction results are shown in Table 2, wherein the stable operation time of the catalyst is calculated as the single-pass operation time with the conversion rate of cyclohexanone ≥ 97%.

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Abstract

A process for oxaminating carbonyl compound features that under existance of Si-contained catalyst, the carbonyl compound, ammonia and hydrogen peroxide take part in liquid-phase reaction while a Si-contained liquid assistant is added to make the Si concentration reach 0.1-10000 ppm. Its advantages are long service life of catalyst and long running time.

Description

technical field [0001] The present invention relates to the ammoximation method of carbonyl compounds. Background technique [0002] Carbonyl compounds refer to compounds containing >C=O functional groups, such as aldehydes and ketones, and the reaction between carbonyl compounds and hydroxylamine is the main method for synthesizing corresponding oxime compounds. [0003] Taking the synthesis of cyclohexanone oxime as an example, cyclohexanone oxime is a key intermediate in the production of ε-caprolactam, and ε-caprolactam is an important organic chemical raw material, mainly used as a synthetic fiber and engineering plastics (such as nylon-6). monomer. About 91% of caprolactam in the industry is produced through the cyclohexanone oxime route, that is, the cyclohexanone-hydroxylamine process. This process is not only complex in process, long in production process, high in equipment investment, but also due to the production or use of NO X , SO X There are more seriou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C251/44C07C249/04
Inventor 吴巍孙斌李永祥程时标王恩泉张树忠
Owner CHINA PETROLEUM & CHEM CORP
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