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Green synthesis method for preparing nitroalkanes by oxime oxidation

A green synthesis technology of nitroalkanes, applied in the preparation of nitro compounds, organic chemistry, etc., can solve the problems of short life, low catalyst activity, low yield, etc.

Active Publication Date: 2017-05-10
SUZHOU YACOO SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These experimental methods for direct oxidation of oximes to nitroalkanes are difficult to reuse due to low yield, low catalyst activity and short life.

Method used

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  • Green synthesis method for preparing nitroalkanes by oxime oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1, embodiment 2 and embodiment 3 are catalyst reuse experiments.

[0018] Example 1:

[0019] After mixing 73g of acetone oxime and 160g of methanol through a mixer, use metering pump A, 97g of hydrogen peroxide (content is 70%), and use metering pump B to continuously add 3g of V-ZSM-5 catalyst (the ratio of silicon to metal is 30), sodium carbonate In a 0.003g reactor, the temperature is 60°C and the pressure is 0.01MPa. The reaction clear liquid separated by the membrane is rectified to obtain 2-nitropropane 85.9g after precipitating, and the yield is 96.5%, and the purity is 99.2%. The unreacted oxime and solvent are recovered and returned to continue the oxidation reaction. V- ZSM-5 catalyst yielded 2.87 g after filtration.

Embodiment 2

[0021] Repeat the experiment with the V-ZSM-5 catalyst recovered above according to the above experiment ratio, and reuse it 8 times, and the yield is all above 95%. In the 9th experiment, the conversion rate dropped to 92%. In the 10th experiment, the conversion rate dropped to 87%.

Embodiment 3

[0023] Butanone oxime 87g and tert-butanol 74g are mixed with metering pump A after mixer, hydrogen peroxide (content is 27.5%) 125g use metering pump B, add continuously to have Zr-V-ZSM-5 catalyzer (silicon metal ratio 50) 14g, potassium bicarbonate 0.3g in the reactor, temperature 65 ℃, pressure 0.05MPa, the reaction clear liquid separated by the membrane was rectified to obtain 2-nitrobutane 99.9g after precipitation, yield 97% , the purity is 99%, and the unreacted oxime and solvent are recovered and returned to continue the oxidation reaction.

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Abstract

The invention belongs to the field of organic chemical industries, and provides a green synthesis method for preparing nitroalkanes by oxime oxidation. At the temperature of 55 to 120 DEG C and under the pressure of 0 to 1.0 MPa, oxime, a solvent and hydrogen peroxide are reacted for 20 to 200min in the presence of certain amounts of nanoporous skeleton metal hybrid catalysts and cocatalysts, a reaction liquid is subjected to membrane separation, the catalysts can be repeatedly used for more than 7 times, and distilled to obtain nitroalkane products, the purity of the products is not less than 99%, and the yield of the products is not less than 95%. Furthermore, the green synthesis method for preparing nitroalkanes by the oxime oxidation disclosed by the invention is a green synthesis method of nitroalkanes, and suitable for large-scale industrialized production.

Description

technical field [0001] A green synthesis method for preparing nitroalkanes by oxidation of oximes. The invention relates to a green synthesis method of nitroalkane, in particular to an oxidation reaction. [0002] technical background [0003] Nitroalkanes are mainly used as raw materials for organic synthesis, solvents and explosives, and nearly 2,000 derivatives can be produced. Its use involves various industries of the national economy such as medicine, pesticide, explosives, dyes, reagents, solvents, surfactants, extractants, emulsifiers and lubricants ("Fine and Specialty Chemicals" 2005, Volume 13, No. 1, pp. 27-30). Condensation of nitroalkanes and aldehydes, followed by reduction treatment, can produce many widely used aminoalcohol products, which is one of the most industrially applicable aspects of nitroalkanes ("Natural Gas Chemical Industry", Volume 31, 2006, 64 -66 pages). [0004] There are three main industrial production methods of nitroalkanes: gas phase...

Claims

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Application Information

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IPC IPC(8): C07C201/06C07C205/02C07C205/05C07C205/04
CPCC07C201/06C07C205/02C07C205/05C07C205/04
Inventor 朱红军楚庆岩宋广亮刘睿何广科黄诚
Owner SUZHOU YACOO SCI CO LTD
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