Load type duplex metal/multi-metal catalyst for hydrogenation synthesis of metanilic acid from m-Nitrobenzenesulfonic acid and preparation method and application

A multi-metal catalyst, nitrobenzene sulfonic acid technology, applied in the direction of metal/metal oxide/metal hydroxide catalyst, sulfonic acid preparation, physical/chemical process catalyst, etc., can solve the problem of high catalyst, achieve high activity and Effects of stability, cost reduction, and simple preparation

Active Publication Date: 2016-07-27
HEBEI JIANXIN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Before the present invention was given, the prior art did not solve the problem that the catalyst could maintain a higher activity and stability during the reaction process of catalyzing the hydrogenation of m-nitrobenzenesulfonic acid to synthesize m-aminobenzenesulfonic acid

Method used

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  • Load type duplex metal/multi-metal catalyst for hydrogenation synthesis of metanilic acid from m-Nitrobenzenesulfonic acid and preparation method and application
  • Load type duplex metal/multi-metal catalyst for hydrogenation synthesis of metanilic acid from m-Nitrobenzenesulfonic acid and preparation method and application
  • Load type duplex metal/multi-metal catalyst for hydrogenation synthesis of metanilic acid from m-Nitrobenzenesulfonic acid and preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 3.5gAl 2 o 3 The carrier was poured into the flask, and then 100ml of a mixed solution of deionized water and glycerol at a ratio of 50:1 was added, and kept at a constant temperature of 90° C. in a water bath for 60 minutes under stirring. Then, 2 ml of 0.05 g / ml palladium nitrate solution and 1 ml of 0.05 g / ml platinum nitrate solution prepared in advance were added dropwise to the carrier, and kept at constant temperature for 2 hours. After the impregnation is completed, use lmol / mlNa 2 CO 3 The solution adjusts the pH value of the impregnating solution to 12, and maintains it for 100 minutes. Then the precipitate was transferred to a suction filter bottle for suction filtration, washed, dried at 80°C for 4h, calcined at 500°C for 4h, and finally reduced with H2 at 500°C for 1h to obtain Pd-Pt / Al 2 o 3 Catalyst, record catalyst A.

Embodiment 2

[0033] Weigh 3.5gAl 2 o 3 The carrier was poured into the flask, and then 100ml of a mixed solution of deionized water and glycerol at a ratio of 50:1 was added, and kept at a constant temperature of 90° C. in a water bath for 60 minutes under stirring. Then, 2 ml of 0.05 g / ml chloropalladium acid solution and 1 ml of 0.05 g / ml chloroplatinic acid prepared in advance were added dropwise to the carrier, and kept at constant temperature for 2 hours. After the impregnation is completed, use lmol / mlNa 2 CO 3 The solution adjusts the pH value of the impregnating solution to 12, and maintains it for 100 minutes. Then the precipitate was transferred to a suction filter bottle for suction filtration, washed, dried at 80°C for 4h, roasted at 500°C for 4h, and finally washed with H at 500°C. 2 After reduction for 1h, Pd-Pt / Al is obtained 2 o 3 Catalyst, record catalyst B.

Embodiment 3

[0035]Weigh 3.5g of the SiO2 carrier and pour it into a flask, then add 100ml of a mixed solution of deionized water and glycerol at a ratio of 50:1, and keep it in a water bath at 90°C for 60min under stirring. Then, 2ml of 0.05g / ml chloroplatinic acid solution and 1ml of 0.05g / ml cerium nitrate prepared in advance were added dropwise to the carrier, and kept at constant temperature for 2h. After the impregnation is completed, adjust the pH value of the impregnation solution to 12 with 1mol / ml Na2CO3 solution, and keep it for 100min. Then the precipitate was transferred to a suction filter bottle for suction filtration, washed, dried at 80°C for 4h, roasted at 500°C for 4h, and finally washed with H at 500°C. 2 After reduction for 1h, the corresponding Pt-Ce / SiO can be obtained 2 Catalyst, record catalyst C.

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Abstract

The invention relates to a load type duplex metal / multi-metal catalyst for hydrogenation synthesis of metanilic acid from m-Nitrobenzenesulfonic acid and a preparation method and application thereof. The catalyst comprises a carrier and two or more metal components loaded on the carrier, wherein at least one metal component is selected from active components of Pd and Pt precious metal, the other metal components are selected from auxiliary components with one or more base metals of K, Ca, Mg, La and Ce. The load type duplex metal / multi-metal catalyst is easy to prepare, low in load amount, convenient to regenerate, and capable of being applied to hydrogenation synthesis of metanilic acid from m-Nitrobenzenesulfonic acid, and has the high reaction activity and stability. The catalyst can also be used for the catalysis hydrogenation reaction process of other unsaturated organic compounds with sulfur-containing impurities, the production process is simplified, and the remarkable economic benefits and environmental benefits are achieved.

Description

technical field [0001] The invention relates to a supported bimetallic / multimetallic catalyst for hydrogenation of m-nitrobenzenesulfonic acid to synthesize m-aminobenzenesulfonic acid, a preparation method and application thereof, and belongs to the technical field of catalysts. Background technique [0002] Aminobenzenesulfonic acid is an important intermediate widely used in medicine, vat dyes, azo dyes, sulfur dyes and reactive dyes. M-aminobenzenesulfonic acid is mainly obtained by reduction of m-nitrobenzenesulfonic acid. At present, in the industry, the reduction of m-nitrobenzenesulfonic acid by iron powder is the main method for producing m-aminobenzenesulfonic acid. Patent CN200410054184.6 has a detailed description of the reduction method of iron powder. This method has low requirements on the purity of raw materials and is easy to control production , few by-products and low cost, etc., but it will produce a large amount of waste water and amine-containing iron ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J23/63C07C303/22C07C309/46
CPCB01J23/44B01J23/58B01J23/63C07C303/22C07C309/46
Inventor 李小年张群峰朱秀全
Owner HEBEI JIANXIN CHEM IND CO LTD
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