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Synthesis of nitrocyclohexane

A technology for nitrocyclohexane and cyclohexane, applied in the preparation of nitro compounds, organic chemistry, etc., can solve problems such as poor selectivity, unsuitability for nitration, serious environmental pollution, etc., achieve less harsh reaction conditions, and improve resource utilization efficiency, the effect of simplifying the process

Inactive Publication Date: 2007-11-21
XIANGTAN UNIV
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AI Technical Summary

Problems solved by technology

However, this reaction system is very corrosive to equipment, and produces a large amount of waste acid and waste water containing organic compounds, causing serious environmental pollution and high treatment costs.
In addition, the selectivity of this method is poor, and there are many side reactions such as oxidation, hydrolysis, and hydroxylation, and it is especially not suitable for the nitration of acid-sensitive substrates.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: by cyclohexane: NO 2 = 2:1 molar ratio, first feed N 2 Purge the reaction system at a certain temperature for 5 minutes, then adjust the temperature to 300°C and use NO 2 Rebalance for 10 minutes. Cyclohexane is passed through NO from the reaction tube by a plunger type advection pump 2 The reaction liquid is vaporized in the preheating section and then enters the 440ml spherical reactor for reaction. The time is 1h, and the product is condensed by the water flow and enters the collection bottle. The reacted mixture is divided into two layers, the upper layer is an organic phase, and the lower layer is an aqueous phase. After the upper layer was analyzed by the internal standard of gas chromatography, the conversion rate of cyclohexane was calculated by using material balance to be 13.71%, and the selectivity of nitrocyclohexane was 70.04%.

Embodiment 2

[0016] Embodiment 2: step is with embodiment 1, and difference is, cyclohexane: NO 2 =0.8:1 molar ratio, reaction temperature 240°C. The conversion rate of cyclohexane was 53.21%, and the selectivity of nitrocyclohexane was 62.68%.

Embodiment 3

[0017] Embodiment 3: step is with embodiment 1, and difference is, by cyclohexane: N 2 o 3 =1:1 molar ratio, the conversion rate of cyclohexane is 57.01%, and the selectivity of nitrocyclohexane is 50.04%.

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Abstract

Synthesis of nitrocyclohexane is carried out by nitrofication reacting cyclohexane with NOX under protection of nitrogen and obtain final product. X is 1.5-2.5. It's simple, cheap and has friendly environment.

Description

technical field [0001] The present invention relates to the synthetic method of nitrocyclohexane. Background technique [0002] Nitroalkane has become an important raw material in the field of fine chemicals such as drugs, solvents, surfactants, emulsifiers and lubricants due to its unique physical and chemical properties and reactivity, and nearly 2,000 derivatives can be produced. If nitroalkanes are partially catalytically reduced to nitroso compounds, oximes (which can be rearranged into amides), or completely reduced to amines, it will provide a raw material basis for the creation of new functional products or materials. With the development of fine chemical industry, the demand for nitrogen-containing compounds will continue to increase, and the technological progress in the production of nitroalkanes will guarantee the development of related fields. [0003] The reaction of introducing a nitro group to a carbon atom of an organic molecule is called nitration. At pre...

Claims

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Application Information

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IPC IPC(8): C07C205/05C07C201/08
Inventor 罗和安尹笃林毛丽秋李光洪刘平乐
Owner XIANGTAN UNIV
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