Catalyst for reduction of nitro, nitroso, azo or/and azoxy compounds

A technology of azo and nitroso oxides, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, preparation of amino compounds, etc., can solve long production process, high operating costs, and production costs Improvement and other issues

Inactive Publication Date: 2005-06-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] The technical problem to be solved by the present invention is that the previous documents mainly use noble metal catalysts in the process of reducing nitro, nitroso, azo or / and hydrazo compounds, which increases the production cost, and azo or / and hydrazo compounds The compound needs to be hydrogenated after additional separation, the production process is long, the operation cost is high, or when the skeleton nickel catalyst is used, only pure raw materials can be used, and it cannot be reacted in the presence of strong alkali or strong organic base, which also makes the production process longer and the operation cost is high. Problem, to provide a new catalyst for the reduction of nitro, nitroso, azo and / or hydroazo compounds

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 0.3-liter autoclave, drop into the condensation reaction solution containing tetramethylammonium hydroxide (weight percentage is composed of: aniline 48.9%, 4-nitrosodiphenylamine 30.1%, 4-nitrodiphenylamine 7.0%, phenazine 0.35% %, azobenzene 7.6%, tetramethylammonium hydroxide 6.5%) 100 grams, 45 grams of aniline, 20 grams of water and 4 grams of modified skeleton nickel catalyst (dry basis). It was replaced three times with nitrogen and twice with hydrogen. Keep the hydrogen pressure in the kettle at 2.5 MPa, raise the temperature to 70° C., and react for 2 hours with a stirring speed of 300 rpm. The modified skeleton nickel catalyst contains boron, tungsten and tin, wherein the weight ratio of Ni:P:W:Sn is 100:0.15:0.1:0.05 relative to Ni. Cool after the reaction, remove the catalyst by filtration, and separate the water phase. The oil phase of the reaction liquid is analyzed by HPLC. The results are: 22.30% of 4-aminodiphenylamine, 0.26% of phenazine, 76.44% ...

Embodiment 2~5

[0029]According to each operation step and condition of embodiment 1, just change the composition of catalyst, its reaction result is listed in table 1.

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PUM

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Abstract

The invention relates to a catalyst for reducing nitro, nitroso, azo or / and azo compounds In the process, only precious metal catalysts can be used, which makes the production cost high, and the azo or / and azo compounds need to be additionally separated and then hydrogenated or when skeleton nickel catalysts are used, only pure raw materials can be used, not strong bases or strong organic bases. There is a problem with the reaction. The present invention supports at least one rare earth element selected from phosphorus, sulfur or boron and selected from the group consisting of tin, aluminum, titanium, bismuth, arsenic, chromium, molybdenum, tungsten, gallium, copper, or halogen by adopting a rare earth element supported on the framework nickel. The technical solution of at least one co-catalyst according to the invention solves this problem well, and can be used in the industrial production of reducing nitro, nitroso, azo or / and azo compounds.

Description

technical field [0001] The present invention relates to a kind of catalyst for reducing nitro, nitroso, azo or / and azo oxide compound, especially about being suitable for reducing nitro, nitroso, azo in the presence of strong base or strong organic base Catalysts for nitrogen and / or azo oxide compounds. Background technique [0002] Nitro or nitroso compounds can be reduced to amino compounds by hydrogenation, for example, 4-nitrodiphenylamine and 4-nitrosodiphenylamine can be reduced to 4-aminodiphenylamine by hydrogenation. Azo or / and azo oxide compounds can be reduced to amine compounds by hydrogenation, for example, azobenzene and / and azobenzene oxide can be reduced to aniline by hydrogenation. In the preparation process of 4-nitrodiphenylamine and 4-nitrosodiphenylamine, a large amount of by-product azobenzene or / and azobenzene oxide can be generated. The catalyst for hydrogenation of nitro, azo or / and azo oxide compounds can be reduced to ami...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755B01J23/76B01J25/02B01J27/00C07C209/02C07C209/36C07C209/38
Inventor 刘仲能侯闽渤吴晓玲朱海燕
Owner CHINA PETROLEUM & CHEM CORP
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