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Green method for nitrifying benzene with nitric acid to prepare nitrobenzen

A technology for mononitrobenzene and nitrobenzene, which is applied in the field of nitrifying benzene to prepare mononitrobenzene and nitrifying benzene with nitric acid, can solve problems such as catalyst stability to be improved, and achieves elimination of unsafe factors, convenient recovery, and high yield. rate effect

Inactive Publication Date: 2012-08-08
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent that has been published, using 65% nitric acid as the nitrating agent, silica-supported ammonium heteropolyacid shows good catalytic activity and one-substitution selectivity in the liquid phase nitration reaction, but the stability of the catalyst still needs to be improved

Method used

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  • Green method for nitrifying benzene with nitric acid to prepare nitrobenzen
  • Green method for nitrifying benzene with nitric acid to prepare nitrobenzen
  • Green method for nitrifying benzene with nitric acid to prepare nitrobenzen

Examples

Experimental program
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Effect test

Embodiment 1

[0030] The volume ratio of 150ml ethyl silicate is ethyl silicate:ethanol:water=1:2:2 to make a solution, heated at 70~80℃ for 30min; dissolve 8.64g phosphomolybdic acid and 1.892g cesium carbonate separately Add deionized water dropwise to the pre-heated ethyl silicate alcohol aqueous solution, continue to heat at 70~80℃, stir until the gel appears, after aging for 12h, dry at 100℃ for 3 hours, 300 o C was calcined for 4 hours to prepare the silica-supported cesium phosphomolybdate catalyst sample No. 1, in which the loading amount (based on the mass ratio of molybdenum trioxide to silica) was 20%.

Embodiment 2

[0032] Except that 8.64g of phosphomolybdic acid and 1.892g of cesium carbonate were dissolved in deionized water instead of 4.32g of phosphomolybdic acid and 0.946g of cesium carbonate in deionized water, the other operations were the same as in Example 1 to obtain a silica load Cesium phosphomolybdate catalyst sample No. 2, in which the loading amount (based on the mass ratio of molybdenum trioxide to silica) is 10%.

Embodiment 3

[0034] Except that 8.64g of phosphomolybdic acid and 1.892g of cesium carbonate were dissolved in deionized water, respectively, 12.96g of phosphomolybdic acid and 2.84g of cesium carbonate were dissolved in deionized water, and the remaining operations were the same as in Example 1, to obtain silica loading Cesium phosphomolybdate catalyst sample No. 3, in which the loading amount (based on the mass ratio of molybdenum trioxide to silica) is 30%.

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Abstract

The invention relates to a green method for nitrifying benzene with nitric acid to prepare nitrobenzen. The method takes silica-loaded cesium phosphomolybdate or cesium phosphotungstate as a catalyst, and employs nitric acid as a nitrating agent to nitrify benzene so as to prepare nitrobenzen. The method disclosed in the invention eliminates unsafe factors in generating polynitrobenzene, oxygen-containing compounds and other detonation matters, and has high yield, convenient catalyst recovery, reutilization and other environmental protection characteristics.

Description

Technical field [0001] The present invention involves a method of nitrate nitrate. Specifically, it involves a green method of nitrate nitrate nitrate benzene, which belongs to the field of organic synthetic technology. Background technique [0002] Nitrobene is an important chemical raw material or an important organic solvent.The nitrogenzene sulfonate can synthesize the nitrogenzene sulfonic chloride for intermediates such as dyes and medicines; chlorine chlorinated chlorine, and widely used in the production of dyes and pesticides.Linaine is also an intermediate of medicine, pesticides, fluorescent whitening agents, organic pigments, etc., and nitrozide is also the two very important intermediates developed in recent years. [0003] The traditional method of production method of nitrogen benzene is nitric acid-sulfuric acid mixing method proposed in 1934. The disadvantages are obvious. First, a large amount of sulfuric acid is required to produce a large amount of waste sulfu...

Claims

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Application Information

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IPC IPC(8): C07C205/06C07C201/08B01J27/19B01J27/188
Inventor 刘丽君尹汉东崔庆新
Owner LIAOCHENG UNIV
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