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Catalytic oxidation method of pyridine

A technology for oxidizing pyridine and pyridine, applied in directions such as organic chemistry, can solve problems such as complex production process, harmful emissions, etc., and achieve the effects of overcoming complex production process, simple production process and high selectivity

Active Publication Date: 2013-07-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Compared with the traditional method, the method provided by the present invention overcomes the problems of complex traditional production process, equipment corrosion, and harmful emissions, and adopts heteroatom molecular sieve modified by soluble zinc salt as the oxidation active component, without adding any inhibitor to the raw material. agent or initiator for green synthesis process

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  • Catalytic oxidation method of pyridine
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preparation example Construction

[0014] In the preparation method provided by the present invention, the solvent is selected from alcohols such as water or methanol, ethanol, n-propanol, isopropanol, tert-butanol, isobutanol or ketones such as acetone and methyl ethyl ketone or acetonitrile, Nitriles such as propionitrile and phenylacetonitrile or their mixtures, preferably acetonitrile, acetone, methanol, water or their mixtures, more preferably acetone, methanol and / or acetonitrile.

[0015] In the preparation method provided by the present invention, there is no special requirement on the order of addition. Pyridine may be added first, or oxidizing agent or solvent may be added first.

Embodiment 1

[0033] Pyridine, hydrogen peroxide, solvent and catalyst (the mol ratio of zinc nitrate and titanium silicon molecular sieve 0.2: 1) is 1: 2 according to the mol ratio of pyridine and hydrogen peroxide, solvent acetonitrile and catalyst mass ratio are 20: 1, pyridine and The catalyst mass ratio is 10:1, and the reaction is carried out at a temperature of 50° C. and a pressure of 1.5 MPa. After 2 hours of reaction, the conversion rate of pyridine was 23%, the effective utilization rate of hydrogen peroxide was 52%, and the selectivity of pyridine N-oxide was 63%.

Embodiment 2

[0035]Pyridine, hydrogen peroxide, solvent and catalyst (the mol ratio of zinc phosphate and titanium silicon molecular sieve 1: 1) are 1: 3 according to the mol ratio of pyridine and hydrogen peroxide, solvent acetone and catalyst mass ratio are 50: 1, pyridine and The catalyst mass ratio is 20:1, and the reaction is carried out at a temperature of 60° C. and a pressure of 2.5 MPa. After 2 hours of reaction, the conversion rate of pyridine was 35%; the effective utilization rate of hydrogen peroxide was 57%; the selectivity of pyridine N-oxide was 62%.

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Abstract

The invention discloses a catalytic oxidation method of pyridine. Under oxidation reaction conditions, pyridine, an oxidant, a solvent and a catalyst are mixed and subjected to a contact reaction so as to prepare pyridine-N-oxide. The method is characterized in that the catalyst is a soluble zinc salt modified heteroatom molecular sieve. Under the circumstance of comparable selectivity, the catalytic oxidation activity of the method is improved compared with the prior art.

Description

technical field [0001] The invention relates to a method for preparing pyridine N-oxide by catalytically oxidizing pyridine. Background technique [0002] Pyridine N-oxide is an important pyridine derivative. After the nitrogen atom is oxidized, it can no longer form positively charged pyridinium ions, which is conducive to the occurrence of aromatic electrophilic substitution reactions. After the substitution is completed, the oxygen on the nitrogen is removed, and the derivatives that cannot be obtained by the direct substitution of pyridine can be obtained. Therefore, pyridine oxide is a commonly used organic synthesis reagent, and is also a commonly used intermediate of pharmaceutical and chemical products. It can also be used as a new type of non-ionic surfactant, which can increase surface adsorption, reduce surface viscosity and stabilize foam. [0003] Due to the different mechanism of the preparation reaction, the preparation of pyridine N-oxide can be divided int...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/89
Inventor 林民史春风朱斌汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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