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Process for photo catalytic reduction preparation of p-chloroaniline

A technology of p-chloroaniline and photocatalysis, applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of dangerous operation, strong corrosiveness, and excessive discharge of waste residue and wastewater, and achieves reduction conversion rate and The effect of high yield, stable chemical properties and less discharge of three wastes

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

AI Technical Summary

Problems solved by technology

The iron powder method is not easy to stir evenly, is highly corrosive, has serious equipment abrasion, discharges a lot of waste residue and wastewater, and has a low yield; Limited by high quality hydrogen source

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 630 mg of p-chloronitrobenzene dissolved in 10 mL of formic acid and 90 mL of isopropanol into a jacketed Pyrex reactor with a magnetic stirrer, and add 640 mg of P25 TiO 2 (about 80% anatase type, 20% rutile type, average particle size 30nm) catalyst powder to form a suspension system. After exhausting oxygen with nitrogen, dark adsorption was carried out for 1.5 h under magnetic stirring, and the suspension was irradiated under a high-pressure mercury lamp (100W), and reacted under magnetic stirring and continuous nitrogen flow. After 4 hours of irradiation, the reaction was terminated, and the TiO was removed by filtration. 2 Particles, the obtained filtrate was analyzed by high pressure liquid chromatography (HPLC), and the yield of p-chloroaniline was 98%.

Embodiment 2

[0016] Embodiment 2 except using powder A101 type TiO 2 (basically anatase type, average particle size 210nm) catalyst instead of P25 type TiO 2 Except, other conditions are the same as in Example 1, and the result is 69% p-chloroaniline yield.

Embodiment 3

[0017] Embodiment 3 except using powder R101 type TiO 2 (basically rutile type, average particle size 185nm) catalyst instead of P25 type TiO 2 Except that other conditions are the same as in Example 1, the result is that the yield of p-chloroaniline is 15%.

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PUM

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Abstract

The invention provides a method for reduction preparation of p-chloroaniline by photocatalysis. The process comprises the following steps: solving p-chloronitrobenzene with organic solvent in photocatalysis reactor allowing over 300nm ultraviolet light to pass with the mass ratio of p-chloronitrobenzene to solvent between 1í†40 and 1í†225, adding hole scavenger and photocatalyst with the volume ratio of hole scavenger to organic solvent between 1í†3 and 1í†18 with the concentration of photocatalyst in organic solvent between 0.5g / L and 10g / L, adding nitrogen for removing oxygen, and irradiating for 3 hours to 6 hours by ultraviolet light at normal pressure. The reduction reaction can be carried out at normal temperature without high temperature energy consumption device, initiation light can be ultraviolet light or sunlight, and nano photocatalyst can be titanium dioxide or zinc oxide, etc. The invention has higher reduction conversion and yield.

Description

technical field [0001] The invention belongs to the production method of organic compounds, and particularly proposes a method for preparing p-chloroaniline through photocatalytic reduction. Background technique [0002] p-Chloroaniline is an important intermediate for fine chemicals such as pharmaceuticals, dyes, pigments, and pesticides, and has a wide range of uses. [0003] The existing synthetic method is basically to prepare p-chloroaniline by reducing p-chloronitrobenzene through iron powder in acidic medium, or prepare p-chloroaniline by reducing p-chloronitrobenzene through alkali sulfide, or prepare p-chloroaniline by reducing p-chloronitrobenzene in an acidic medium. Preparation of p-chloroaniline by hydrogenation reduction in the presence of catalyst. The iron powder method is not easy to stir evenly, is highly corrosive, has serious equipment abrasion, discharges a lot of waste residue and wastewater, and has a low yield; Limit...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C211/52
Inventor 张天永张友兰由兰英
Owner TIANJIN UNIV
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