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Method for preparing nitrobenzene through catalysis of polyoxometallate

A polyoxometalate and catalytic preparation technology, which is applied in the field of polyoxometalate catalytic preparation of nitrobenzene, can solve problems such as environmental pollution, corrosion of reaction equipment and the like, achieve simple requirements for reaction equipment, reduce pollution, and mild reaction conditions controllable effect

Pending Publication Date: 2020-12-01
LINYI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the traditional nitration process mostly adopts the mixed nitration method of sulfuric acid and nitric acid. This method is mature and has high yield. Generation of waste acid
A large amount of waste acid will not only corrode the reaction equipment, but also pollute the environment after discharge

Method used

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  • Method for preparing nitrobenzene through catalysis of polyoxometallate
  • Method for preparing nitrobenzene through catalysis of polyoxometallate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiments of the present invention provide a method for preparing nitrobenzene by polyoxometalate catalysis, comprising the following steps:

[0031] a. Add 10ml of benzene, 1.6g of phosphotungstic acid polyoxometalate with Anderson structure, and 7.7mL of concentrated nitric acid with a concentration of 70% into the reaction kettle in turn, control the reaction temperature at 60 degrees, and react for 6 hours;

[0032] b. After the nitration reaction is finished, the liquid should be layered to obtain an organic phase and an aqueous phase, and the aqueous phase should be separated and removed after liquid separation; 20ml of water is added to the organic phase to wash off unreacted acid, and the aqueous phase should be separated and removed after liquid separation;

[0033] c. Add 20g of anhydrous sodium sulfate to the organic phase, filter out the desiccant after drying, the yellow organic phase liquid is the crude product of nitrobenzene, the crude product of nitrob...

Embodiment 2

[0035] Embodiments of the present invention provide a method for preparing nitrobenzene by polyoxometalate catalysis, comprising the following steps:

[0036] a. Add 10ml of benzene, 1.7g of silicotungstomolybdate polyoxometalate with Anderson structure, 7.7mL of concentrated nitric acid with a concentration of 70% and 0.64ml of concentrated sulfuric acid with a concentration of 98% into the reaction kettle in sequence, and control the reaction temperature to 80 degree, react for 2 hours;

[0037] b. After the nitration reaction is finished, the liquid should be layered to obtain an organic phase and an aqueous phase, and the aqueous phase should be separated and removed after liquid separation; 20ml of water is added to the organic phase to wash off unreacted acid, and the aqueous phase should be separated and removed after liquid separation;

[0038] c. Add 20g of anhydrous sodium sulfate to the organic phase, filter out the desiccant after drying, the yellow organic phase l...

Embodiment 3

[0040] Embodiments of the present invention provide a method for preparing nitrobenzene by polyoxometalate catalysis, comprising the following steps:

[0041] a. 10ml of benzene, 1.7g of borotungstomolybdate polyoxometalate with Anderson structure, 8.47mL of concentrated nitric acid with a concentration of 70% and 1.28ml of concentrated sulfuric acid with a concentration of 98% were successively added to the reaction kettle, and the reaction temperature was controlled to be 60 degree, react for 6 hours;

[0042] b. After the nitration reaction is finished, the liquid should be layered to obtain an organic phase and an aqueous phase, and the aqueous phase should be separated and removed after liquid separation; 20ml of water is added to the organic phase to wash off unreacted acid, and the aqueous phase should be separated and removed after liquid separation;

[0043] c. Add 20g of anhydrous calcium chloride to the organic phase, filter out the desiccant after drying, the yello...

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Abstract

The invention provides a method for preparing nitrobenzene by catalysis of polyoxometallate, which comprises the following steps: sequentially adding polyoxometallate, benzene, concentrated sulfuric acid and concentrated nitric acid into a reaction kettle, heating and stirring, after the nitration reaction is finished, layering the reaction liquid to obtain an organic phase and a water phase, separating to remove the water phase after liquid separation, adding a certain amount of water into the organic phase to wash off unreacted acid, separating to remove the water phase after liquid separation, adding a drying agent into the organic phase, drying, filtering out the drying agent, and purifying the organic phase liquid through reduced pressure distillation to obtain the nitrobenzene finished product, wherein the distillation residue is the polyoxometallate catalyst. Benzene is used as a raw material, nitric acid and sulfuric acid are used as mixed acid nitration reagents, one-pot reaction is adopted, operation is easy, reaction conditions are mild, the yield is high, polyoxometallate is used as a catalyst, the use amount of concentrated sulfuric acid in nitration reaction can be greatly reduced, recovery is convenient, pollution to the environment is reduced, safety and environmental friendliness are achieved, and environmental protection pressure is relieved.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for preparing nitrobenzene by polyoxometalate catalysis. Background technique [0002] Nitrification refers to a type of reaction in which one or more nitro functional groups are generated or introduced in organic compounds. In industrial production, nitrification plays an important role. The nitro compounds produced by the reaction are important chemical raw materials for medicines, dyes, pesticides, explosives and other products. At present, the traditional nitration process mostly adopts the mixed nitration method of sulfuric acid and nitric acid. This method is mature and has high yield. Generation of waste acid. A large amount of waste acid will not only corrode the reaction equipment, but also pollute the environment after being discharged. In order to overcome the above problems, it is particularly important to develop a green catalyst with high atom utilizati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C201/16C07C205/06
CPCC07C201/08C07C201/16C07C205/06
Inventor 孙运强余焓彭寅
Owner LINYI UNIVERSITY
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