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Process for photo catalytic reduction preparation of m-nitroaniline

A technology of nitroaniline and m-dinitrobenzene, which is applied in the field of photocatalytic reduction to prepare m-nitroaniline, can solve the problems of excessive sulfur-containing waste water in waste gas, large discharge of waste residue and high corrosiveness, etc., and achieve reduction conversion rate and The effect of high yield, less discharge of three wastes, and easy manufacturing materials

Inactive Publication Date: 2005-07-06
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The iron powder method is not easy to stir evenly, has strong corrosion, serious equipment abrasion, waste residue and wastewater discharge, it is difficult to control the reduction end point, and the yield is low; the sulfide alkali method produces waste gas and sulfur-containing wastewater, which is difficult to treat; High pressure equipment, dangerous to operate, limited by high quality hydrogen source
It is also possible to prepare m-nitroaniline by aminolysis of m-chloronitroaniline, but it requires a high-pressure reactor, which is highly corrosive and expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1 Weigh 120mg m-dinitrobenzene and 250mg TiO 2 (P25 type, about 80% anatase type and 20% rutile type mixed crystal, average grain size 30nm), it is put into 120mL Pyrex glass cylindrical reaction flask, adds 80mL isopropanol, puts into magnetic stirring bottle, tightly cap the cork, start the magnetic stirrer, and after 1.5 hours of dark adsorption under magnetic stirring, pass nitrogen to exhaust oxygen for about 1 hour. Then turn on the 100W high-pressure mercury lamp to irradiate from the side of the reactor, finish the reaction after irradiating for 5 hours, and filter to remove TiO 2 Particles, the obtained filtrate was analyzed by high pressure liquid chromatography (HPLC), and the yield of m-nitroaniline was 79.8%, and the yield of by-product m-phenylenediamine was 3.5%.

Embodiment 2

[0016] Embodiment 2 except that catalyst is changed into A101 (substantially anatase TiO 2 , average grain size 210nm), isopropanol is changed to methanol, and the irradiation time is 9h, and other reaction conditions are the same as in Example 1. As a result, the yield of m-nitroaniline is 44.1%, and there is no by-product m-phenylenediamine.

[0017] Examples 3-7 were operated in the same manner as in Example 1, but the hole scavenger oxalic acid was added, and the solvent was changed to ethanol. Y1 is the yield of m-nitroaniline, and Y2 is the yield of m-phenylenediamine.

[0018] Table 1: Examples 3-7

[0019] Test No. m-dinitrobenzene TiO 2 Oxalic acid Solvent Lighting time Y1 Y2

[0020] (g) (g) (mg) (mL) (h) (%) (%)

Embodiment 3

[0021] Example 3 0.12 0.25 21 60 3 83.9 0

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Abstract

The invention discloses a method for reduction preparation of m-nitro aniline by photocatalysis. The lightcatalyzed reduction reaction can be carried out in photocatalysis reactor with temperature control apparatus, m-dinitrobenzene is solved by organic solvent with sacrificial electron donor with the mass ratio of m-dinitrobenzene to solvent between 1í†50 and 1í†500, said mixture and photocatalyst are added in the reactor with the concentration of photocatalyst in solvent between 0.2g / L and 8g / L, the solution is stirred to suspending liquid, then nitrogen is added for removing oxygen and the solution is irradiated for 2 hours to 12 hours by ultraviolet light at normal pressure to produce meta nitro aniline m-nitroaniline. The reduction reaction can be carried out at normal temperature without high temperature energy consumption device, and the initiation light can be natural sunlight.

Description

technical field [0001] The invention belongs to the synthesis method of organic compounds, and particularly proposes a method for preparing m-nitroaniline by photocatalytic reduction. Background technique [0002] m-Nitroaniline is an important and widely used intermediate for fine chemicals such as medicine, dyes, pigments, pesticides and auxiliaries. [0003] The existing synthetic method basically prepares m-nitroaniline by reducing m-dinitrobenzene in an acidic medium through iron powder, or prepares m-nitroaniline by reducing m-dinitrobenzene in an alkaline medium through alkali sulfide, or m-nitroaniline is prepared from m-dinitrobenzene by hydrogenation reduction in the presence of a catalyst. The iron powder method is not easy to stir evenly, has strong corrosion, serious equipment abrasion, waste residue and wastewater discharge, it is difficult to control the reduction end point, and the yield is low; the sulfide alkali method prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/36C07C211/52
Inventor 张天永张友兰由兰英
Owner TIANJIN UNIV
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