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Process for photo catalytic reduction preparation of lentine

A technology of m-phenylenediamine and photocatalysis, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of large environmental pollution, high requirements, and serious corrosion, and achieve low discharge of three wastes. , Avoid high temperature oxidation, easy to manufacture materials

Inactive Publication Date: 2006-08-16
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The common production method of m-phenylenediamine is the reduction method of m-dinitrobenzene, and iron powder or alkali sulfide can be used, but these methods will produce a large amount of three wastes, such as waste residue and waste liquid, which will cause serious environmental pollution and serious corrosion
In addition, there is a catalytic hydrogenation reduction method. This method has high requirements for production equipment and process control, and requires excellent catalysts. It is generally carried out under high temperature and high pressure conditions, and the operation is dangerous and the conditions are relatively harsh.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 Weigh 80mg m-dinitrobenzene and 0.32g TiO 2 Powder (P25 type, containing about 80% anatase type and 20% rutile type, average particle size 30nm), put it into a 120mL Pyrex glass reactor, add 80mL methanol solution, put into a magnetic stirrer, cap the bottle tightly , start the magnetic stirrer, and after dark adsorption for 1.5h under magnetic stirring, pass nitrogen to exhaust oxygen for about 1h. 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 resulting filtrate was analyzed by high pressure liquid chromatography (HPLC), and the yield of m-phenylenediamine was 43.1%, and the yield of m-nitroaniline was 42.8%.

Embodiment 2

[0016] Example 2 Except that the Pyrex reactor in Example 1 was replaced by a quartz glass reactor with the same structure, other reaction conditions were the same as in Example 1, and the yield of m-phenylenediamine was 57.2%.

Embodiment 3

[0017] Example 3 Except that 80 mL of ethanol solvent was used instead of 80 mL of methanol solvent, other conditions were the same as in Example 1. As a result, the yield of m-phenylenediamine was 22%, and the yield of m-nitroaniline was 24.6%.

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Abstract

The invention discloses a method for reduction preparation of m-phenylenediamine by photocatalysis. The process comprises the following steps: solving m-dinitrobenzene with organic solvent in photocatalysis reactor allowing over 300nm ultraviolet light to pass, adding photocatalyst with adding proportion of 0.2g to 9g / L(sol), adding nitrogen for removing oxygen, and irradiating for 1.5 hours to 8 hours by ultraviolet light at normal pressure. In the invention, the reduction reaction can be carried out at normal temperature or under ultraviolet radiation, initiation light can be ultraviolet light or sunlight, nano photocatalyst can be titanium dioxide or zinc oxide, etc. and reducing medium is proper solvent which can be reclaimed. The invention can prevent high oxidation and coking of m-phenylenediamine.

Description

technical field [0001] The invention belongs to the synthesis method of organic compounds, and particularly proposes a method for preparing m-phenylenediamine through photocatalytic reduction. Background technique [0002] m-Phenylenediamine is an important intermediate for fine chemicals such as medicines, dyes, pigments, pesticides, auxiliaries, etc. An important component of the color developer, etc., with a large amount and a wide range of uses. [0003] The commonly used production method of m-phenylenediamine is m-dinitrobenzene reduction method, which can use iron powder or alkali sulfide, but these methods will produce a large amount of three wastes, such as waste residue and waste liquid, causing serious environmental pollution and serious corrosion. In addition, there is a catalytic hydrogenation reduction method, which has high requirements on production equipment and process control, and requires excellent catalysts. It is general...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/51C07C209/36
Inventor 张天永张友兰由兰英
Owner TIANJIN UNIV
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