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Oxaamidination method of oxo-compound

A technology of carbonyl compounds and substances, which is applied in the field of ammoximation of carbonyl compounds, can solve the problems of decreased catalyst recovery rate, shortened catalyst stable operation time, and catalyst deactivation, so as to reduce catalyst deactivation, improve stable operation time, and prolong The effect of catalyst life

Inactive Publication Date: 2003-12-17
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
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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 embodiment is the process of cyclohexanone ammoximation to prepare cyclohexanone oxime, and the catalyst is titanium silicon (TS-1) molecular sieve raw powder.

[0028] The reactor has a volume of 150ml, magnetically stirred, and heated in an oil bath. The reaction raw materials and reaction products continuously enter and exit 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 in the reaction solution = 35ppm , The catalyst concentration is 1.8% by weight, the average residence time of the materials is 72min, the reaction temperature is 76±1°C, the reaction pressure is normal pressure, silica sol is added, and the addition is continuous. The reaction results are shown in Table 1, wherein the stable operation time of the catalyst is calculated as...

Embodiment 2

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

Embodiment 3

[0037] Repeat Example 1, the difference is: the reaction temperature is 83±1°C, the reaction pressure is 0.3Mpa, the 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 100 ppm. The reaction results are shown in Table 2, where the stable operation time of the catalyst is calculated as the single-pass operation time with a cyclohexanone conversion rate ≥ 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 a method for ammoximation of carbonyl compounds. Background technique [0002] Carbonyl compounds refer to compounds containing >C=O functional groups, such as aldehydes and ketones. The reaction between carbonyl compounds and hydroxylamine is the main method to synthesize corresponding oxime compounds. [0003] Taking the synthesis of cyclohexanone oxime as an example, cyclohexanone oxime is a key intermediate for the production of ε-caprolactam, and ε-caprolactam is an important organic chemical raw material, mainly used for synthetic fibers and engineering plastics (such as nylon-6) monomer. About 91% of caprolactam in industry is produced through the cyclohexanone oxime route, that is, the cyclohexanone-hydroxylamine process. This process is not only complicated, long production process, high equipment investment, but also because of the production or use of NO X , SO X There are serious corrosion and pollution proble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/04C07C251/44
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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