Method for hydrogenation preparation of 4-amino-3-fluorophenol from o-fluoro-nitrobenzene and device therefor

A technology for o-fluoronitrobenzene and fluorophenol, which is applied in the field of nitrobenzene hydrogenation to produce 4-aminophenol, can solve problems such as difficult separation of catalysts, and achieve the effects of reducing reaction costs and improving economic benefits

Inactive Publication Date: 2005-07-06
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These catalytic hydrogenation reactions reported above are all carried out in solutions containing surfactants and / or water-soluble solvents. After the reaction, the catalyst is difficult to separate from the reaction system and can be recycled.

Method used

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  • Method for hydrogenation preparation of 4-amino-3-fluorophenol from o-fluoro-nitrobenzene and device therefor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Such as figure 1 Shown, the 500ml stainless steel reactor 13 that has magnetic stirrer 11 is arranged in the oil bath 14, and reactor 13 is provided with air inlet and exhaust hole, is provided with the liner 12 of polytetrafluoroethylene material in it, On the gas line between the hydrogen source 1 and the reactor 13, a shut-off valve 3, a pressure gauge 4, a pressure regulator 5, a purification tank 7, a filter 8, a mass flow meter 9 and a one-way valve 10 are arranged; 2 and the gas pipeline between the reactor 13 are provided with a shut-off valve 3, a pressure reducing valve 6 and a purification tank 7; on the exhaust pipeline connected with the reactor 13 vent hole, a pressure gauge 4 and 15 are arranged to be soap scum flow meter.

[0018] In reactor 13, add 10.8 gram o-fluoronitrobenzene respectively, 173ml deionized water, 7.7ml absolute ethanol, 10.4 gram vitriol oil, 0.426 gram platinum loading is 2wt.%Pt-C catalyst, and reaction temperature is 90 °C, the p...

Embodiment 2

[0020] Reaction temperature is changed into 80 ℃ and other conditions are identical with example 1, and other steps are with example 1.

Embodiment 3

[0022] Reaction temperature is changed into 100 ℃ and other conditions are identical with example 1, and other steps are with example 1.

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Abstract

The invention relates to hydrogenation preparation of 4-aminophenol from nitrobenzene, especially a method for hydrogenation preparation of 4-amino-3-fluorophenol from o-fluoro-nitrobenzene and device therefore. The reaction is carried out in autoclave with acid medium at 50í½300C.,0.1í½10.0MPa, and the stirring rate is 100í½900 r / min, and the catalytically hydrogenated product is separated, distilled, filtered, and dried to prepare the product. O-fluoro nitrobenzene can be converted into 4-amino-3-fluobenzene by said method with conversion approaching 100%. 4-amino-3-fluobenzene is colourless crystallisate with selective around 92% and purity up to 99%. The catalytic process in the invention can be used for heterogeneous catalysis process of hydrogenation preparation of aminophenol from o-fluoro nitrobenzene and its substituted nitrobenzene.

Description

technical field [0001] The present invention relates to hydrogenation of nitrobenzene to 4-aminophenol, in particular to a method and device for hydrogenation of o-fluoronitrobenzene to 4-amino-3-fluorophenol. Background technique [0002] J.Chem.Soc.1964, p.473; U.S. Patents USP4885389, 3654365, 4307249, 6403833, 5545754, 3715397; European Patents EP0041837, 0211545, 0289297; CN1061808, CN1087623, CN1077707, CN1105983, CN1237575, CN1121708 have only U.S. Patent 5545754 and Japanese Patent Publication Ping-182456 and Show-5373557 to report that Pt-C catalyst is used for the hydrogenation of o-fluoronitrobenzene to prepare 4-amino-3-fluorine The catalytic hydrogenation process of substituted phenols, but the role of co-catalyst was not reported. In addition, the Pt content of the catalyst used was as high as 5wt.%. Other patents only relate to the catalyst and process for producing p-aminophenol from nitrobenzene. CN1237575 describes the preparation of p-aminophenol by liqu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/00C07C215/76
Inventor 丁云杰潘振栋罗洪原吕元
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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