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Process for preparing cyclohexone by catalyzing oxidating cyclohexol

A technology of catalytic oxidation and cyclohexanol, which is applied in the direction of oxidation preparation of carbonyl compounds, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as environmental pollution, product post-processing difficulties, equipment corrosion, etc., and achieve low reaction temperature , The effect of low reaction equipment requirements and low reaction energy consumption

Inactive Publication Date: 2006-06-28
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome a series of problems such as the use of strong corrosive and toxic metal oxides as catalysts in the existing cyclohexanone preparation technology, which can easily cause equipment corrosion, product post-processing difficulties and environmental pollution, the invention provides a Catalytic oxidation cyclohexanol prepares the method for cyclohexanone, with H 2 o 2 As the oxidizing agent, the ammonium salt of phosphomolybdenum vanadium heteropolyacid is used as the catalyst to catalyze the oxidation of cyclohexanol to prepare cyclohexanone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 50ml three-necked flask equipped with mechanical stirring and a reflux condenser, add 2 grams (20 mmol) of cyclohexanol, 30% H 2 o 2 Oxidant 6.8 grams (60mmol), 4.0ml acetone, heat up to 80 ℃, add the phosphorus molybdenum-vanadium heteropolyacid hexadecylpyridinium salt of 0.1g [(C 16 h 33 C 5 h 5 N) 4 PMo 11 VO 40 ] Catalyst, stirring reaction 7 hours. The catalyst was removed by cooling and filtering, and the reaction liquid was determined by gas chromatography. The conversion rate of cyclohexanol was 47.6%, and the yield of cyclohexanone was 100% (based on the reacted cyclohexanol raw material).

Embodiment 2～5

[0025] Adopt different acetone consumption to replace the acetone consumption described in embodiment 1, other conditions are the same as embodiment 1, and its test result is listed in table 1.

[0026]

Embodiment 6

[0028] In a 50ml three-necked flask equipped with mechanical stirring and a reflux condenser, add 2 grams (20 mmol) of cyclohexanol, 30% H 2 o 2 Oxidizing agent 10 grams (88mmol), 2.5ml acetone, heat up to 80 ℃, add the phosphorus molybdenum-vanadium heteropolyacid hexadecylpyridinium salt of 0.3g [(C 16 h 33 C 5 h 5 N) 4 PMo 11 VO 40] Catalyst, stirred and reacted for 7 hours. The catalyst was removed by cooling and filtration, and the reaction liquid was determined by gas chromatography. The conversion rate of cyclohexanol was 60.2%, and the yield of cyclohexanone was 82.4% (based on the reacted cyclohexanol raw material).

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PUM

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Abstract

The invention relates to a method to make cyclohexanone by catalytic oxidation cyclohexanol that includes H2O2 as oxidant. The catalyst is Q3+xPMo12-xVxO40, of which x=1-3, Q represents quaternary ammonium positive ion or MH4+. The invention avoids using noble metal as catalyst, has low reaction temperature, low reaction powder consumption. The invention almost has no pollution, and has good economic and social benefits.

Description

(1) Technical field [0001] The present invention relates to a kind of preparation method of cyclohexanone, particularly a kind of 2 o 2 It is an oxidizing agent, and the ammonium salt of phosphomolybdenum vanadium heteropolyacid is used as a catalyst to catalyze the method for preparing cyclohexanone by oxidizing cyclohexanol. (2) Background technology [0002] Cyclohexanone is an important organic chemical and pharmaceutical raw material. Its most important application is to prepare caprolactam, the raw material for nylon-6, and adipic acid, the raw material for nylon-66. In the process of preparing cyclohexanone by oxidative dehydrogenation of cyclohexanol, traditional catalysts mostly use inorganic and organic oxidants such as oxidizing heavy metal oxides and salts such as chromium trioxide, potassium permanganate, potassium dichromate, etc. Although oxidants have strong oxidizing properties and can oxidize various substrates, the catalysts are highly corrosive and toxi...

Claims

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Application Information

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IPC IPC(8): C07C45/29B01J27/18C07C49/403
Inventor 施介华李祥
Owner ZHEJIANG UNIV OF TECH
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