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Novel preparation method of p-fluoronitrobenzene

A technology of p-fluoronitrobenzene and p-nitrochlorobenzene, which is applied to the preparation of organic compounds, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of increasing fluoronitrobenzene Preparation costs, environmental hazards and other issues, to achieve the effect of avoiding solvent recovery process, simplifying production process, and high porosity

Active Publication Date: 2018-09-28
SHANGYU XIES CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, many organic solvents are often consumed in the process of preparing p-fluoronitrobenzene by the fluorination method, which not only increases the preparation cost of p-fluoronitrobenzene, but also has certain harm to the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A novel preparation method of p-fluoronitrobenzene, comprising the following steps:

[0025] (1) Durian shells are pulverized with a pulverizer, then the pulverized durian shell powder and ethanol are mixed, and the grinder is used to grind for 10 hours at a rotating speed of 580rpm. After drying, the durian shell powder is obtained; wherein, the durian shell powder and ethanol The mass ratio is 1:33;

[0026] (2) After mixing and grinding the durian shell powder and urea, place it in a porcelain boat, heat up to 700°C at a heating rate of 5°C / min, and process for 2 hours. After the treatment, the mixed powder is obtained; wherein, the durian shell powder The mass ratio to urea is 3:1.3;

[0027] (3) Tetrabutylammonium chloride is dissolved in deionized water to make a solution with a mass concentration of 4%; then add the mixed powder prepared above, stir and mix for 20min, then let it stand for 1h, filter, and the solid is at 80 Drying at ℃ to obtain the catalyst; ...

Embodiment 2

[0030] A novel preparation method of p-fluoronitrobenzene, comprising the following steps:

[0031] (1) Durian shells are pulverized with a pulverizer, then the pulverized durian shell powder and ethanol are mixed, and the grinder is used to grind for 20 hours at a rotating speed of 580rpm. After drying, the durian shell powder is obtained; wherein, the durian shell powder and ethanol The mass ratio is 1:45;

[0032] (2) After mixing and grinding the durian shell powder and urea, place it in a porcelain boat, heat up to 850°C at a heating rate of 15°C / min, and process for 4h. After the treatment, the mixed powder is obtained; wherein, the durian shell powder The mass ratio to urea is 9:1.3;

[0033] (3) Dissolve tetrabutylammonium chloride in deionized water to make a solution with a mass concentration of 8%; then add the mixed powder prepared above, stir and mix for 20-30min, then stand for 3h, filter, and solid drying at 100°C to obtain a catalyst;

[0034] (4) Mix p-nitr...

Embodiment 3

[0036] A novel preparation method of p-fluoronitrobenzene, comprising the following steps:

[0037] (1) Durian shells are pulverized by a pulverizer, then the pulverized durian shell powder and ethanol are mixed, and the grinder is used to grind for 12 hours at a rotating speed of 580rpm. After drying, the durian shell powder is obtained; wherein, the durian shell powder and ethanol The mass ratio is 1:35;

[0038] (2) After mixing and grinding the durian shell powder and urea, place it in a porcelain boat, heat up to 750°C at a heating rate of 8°C / min, and process for 2.5h. After the treatment, the mixed powder is obtained; among them, the durian shell The mass ratio of powder and urea is 5:1.3;

[0039] (3) Dissolve tetrabutylammonium chloride in deionized water to make a solution with a mass concentration of 5%; then add the mixed powder prepared above, stir and mix for 20-30min, then let it stand for 1-3h, and filter , the solid was dried at 85°C to obtain the catalyst; ...

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PUM

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Abstract

The invention discloses a novel preparation method of p-fluoronitrobenzene, and relates to the field of organic synthesis. The method concretely comprises the following steps of firstly crushing durian shells; adding ethanol; performing ball milling to prepare durian shell powder; then, mixing the durian shell powder with urea; performing sintering treatment at a certain temperature to obtain mixed powder; adding the mixed powder into a tetrabutylammonium chloride solution for stirring and still standing treatment; then, performing drying to obtain a catalyst; adding reaction raw materials ofpara-nitrochloro-benzene, potassium fluoride and the catalyst into a reaction kettle; performing sealing; performing reaction at a certain temperature; after the reaction is completed, performing water washing and layering treatment; performing organic layer rectification to obtain a target product. The method disclosed by the invention has the advantages that the operation is simple; a solvent isnot used in the reaction process; the cost is effectively reduced; the product yield is high.

Description

Technical field: [0001] The invention relates to the field of organic synthesis, in particular to a novel preparation method of p-fluoronitrobenzene. Background technique: [0002] p-Fluoronitrobenzene is an important intermediate for the preparation of medicines, pesticides, dyes, etc. "Ether" is synthesized with it as the main starting material, and its consumption is very large. Therefore, synthetic methods have received widespread attention. [0003] The methods for synthesizing p-fluoronitrobenzene are mainly nitration and fluorination. Compared with nitration, the raw materials of fluorination are simple and easy to obtain, the process operation is convenient, the product selectivity is good, and there is no need to separate isomers, so it is more commonly used. However, at present, many organic solvents are often consumed in the process of preparing p-fluoronitrobenzene by fluorination, which not only increases the preparation cost of p-fluoronitrobenzene, but also ...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/12B01J31/02
CPCB01J31/0239C07C201/12C07C205/12
Inventor 解卫宇柳衍森
Owner SHANGYU XIES CHEM IND
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