Amorphous alloy catalyst for hydrogenating dinitrotoluene and application of amorphous alloy catalyst

A technology of dinitrotoluene and amorphous alloys, which is applied in the field of preparation of supported Ni-B amorphous alloy hydrogenation catalysts, can solve problems affecting catalyst hydrogenation performance, achieve low price, strong interaction, The effect of good hydrogenation performance

Inactive Publication Date: 2012-07-18
TAIYUAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above results show that in the preparation of supported Ni-B amorphous alloy catalysts, the conventional impregnation

Method used

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  • Amorphous alloy catalyst for hydrogenating dinitrotoluene and application of amorphous alloy catalyst
  • Amorphous alloy catalyst for hydrogenating dinitrotoluene and application of amorphous alloy catalyst
  • Amorphous alloy catalyst for hydrogenating dinitrotoluene and application of amorphous alloy catalyst

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0034] Example 1

[0035] (1) The concentration of 20ml is 0.6mol / L Ni(CH 3 COO) 2 ·4H 2 The aqueous solution of O was added dropwise to 40 ml of ethanol solution with a concentration of 1.5 mol / L tetraethyl orthosilicate, and 1 ml of acetic acid was added at the same time. The mixed solution was placed in a water bath at 60° C. and slowly stirred until it gelled.

[0036] (2) Dry the gel in an oven at 110℃ for 11h, then grind the gel to below 200 mesh, and then calcinate in a muffle furnace at 500℃ for 5h to obtain NiO / SiO 2 Forebody.

[0037] (3) Put 1mol / L KBH in an ice water bath 4 Solution, pass the 2.0mol / L NaOH solution to KBH 4 Adjust the pH of the solution to 7, press KBH 4 / Ni=4 (molar ratio), added dropwise to the calcined NiO / SiO at a rate of 3ml / min 2 After the dripping is completed, continue to stir until no bubbles are generated. First wash with distilled water to neutrality, and then wash with ethanol 5 times. The obtained composition is Ni-13.7wt%, B-15.5wt%, SiO 2 -7...

Example Embodiment

[0040] Example 2

[0041] (1) Change 15ml concentration to 1mol / L NiCl 2 The aqueous solution was added dropwise to 80ml of ethanol solution with a concentration of 1.3mol / L tetraethyl orthosilicate, and 2ml of acetic acid was added at the same time. The mixed solution was placed in a 60°C water bath and slowly stirred until it gelled.

[0042] (2) Dry the gel in an oven at 110°C for 9 hours, then grind the gel to below 200 mesh, and then calcinate in a muffle furnace at 550°C for 6 hours to obtain NiO / SiO 2 Forebody.

[0043] (3) Put 1.2mol / L KBH in an ice water bath 4 Solution, pass the 2.0mol / L NaOH solution to KBH 4 Adjust the pH of the solution to 7, press KBH 4 / Ni=4 (molar ratio), added dropwise to the calcined NiO / SiO at a rate of 4ml / min 2 After the dripping is completed, continue to stir until no bubbles are generated. First wash with distilled water to neutrality, and then wash with ethanol for 3 times. The composition obtained is Ni-10.2wt%, B-11.5wt%, SiO 2 -78.3wt% of th...

Example Embodiment

[0045] Example 3

[0046] (1) Set the concentration of 10ml to 0.7mol / L Ni(NO 3 ) 2 The aqueous solution was added dropwise to 70ml of ethanol solution with a concentration of 1.3mol / L tetraethyl orthosilicate, and 3ml of acetic acid was added at the same time. The mixed solution was placed in a 60°C water bath and slowly stirred until it gelled.

[0047] (2) Dry the gel in an oven at 110°C for 15h, then grind the gel to below 200 mesh, then calcinate in a muffle furnace at 450°C for 7h to obtain NiO / SiO 2 Forebody.

[0048] (3) Put 1.2mol / L KBH in an ice water bath 4 Solution, pass the 2.0mol / L NaOH solution to KBH 4 Adjust the pH of the solution to 7, press KBH 4 / Ni=3 (molar ratio), added dropwise to the calcined NiO / SiO at a rate of 4ml / min 2 After the dripping is completed, continue to stir until no bubbles are generated. First wash with distilled water to neutrality, then wash with ethanol 4 times and then 3 times with ethanol. The obtained composition is Ni-5.2wt%, B-5.7wt %, ...

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Abstract

An amorphous alloy catalyst for hydrogenating dinitrotoluene comprises the following components according to catalyst composition: 5-30.0wt% of Ni, 5-30.0wt% of B, 0-5wt% of auxiliary and 40-90wt% of SiO2. The amorphous alloy catalyst is prepared by adopting a preparation method comprising the following steps of: dropwise adding a mixed aqueous solution containing soluble nickel salt and soluble salt of the auxiliary to an ethanol solution of tetraethoxysilane, and simultaneously, adding acetic acid and forming gel in a water bath; drying and grinding the gel, and then roasting the gel to obtain an NiO/SiO2 precursor; adjusting the pH value of 0.5-2.5 mol/L of KBH4 solution and adding the KBH4 solution to NiO/SiO2 according to the mol ratio of KBH4 to Ni being (1-5): 1, and then washing to obtain the catalyst. The catalyst provided by the invention is used for the reaction of synthesizing toluene diamine (TDA) by catalytically hydrogenising dinitrotoluene DNT; and the technical conditions of the application of the catalyst are as follows: the reaction temperature ranges from 80 to 150 DEG C; the reaction pressure is 0.8-1.2 MPa; methanol or ethanol is taken as a solvent; the initial concentration of the dinitrotoluene DNT is 2-20wt%; and the concentration of the catalyst is 0.1-5wt%. The amorphous alloy catalyst is low in cost, good in selectivity and high in conversion ratio.

Description

technical field [0001] The invention belongs to a method for preparing a catalyst, in particular to a method for preparing a supported Ni-B amorphous alloy hydrogenation catalyst. Background technique [0002] Toluenediamine (TDA), also known as diaminotoluene, is an important chemical raw material and chemical intermediate. In industry, it is usually synthesized by hydrogenation of dinitrotoluene (DNT) in the presence of an external organic solvent and a catalyst. Catalysts are generally supported noble metal Pd / C and Pt / C catalysts (Sweden, DuPont technology in the United States, working pressure 1Mpa) and Raney-Ni based catalysts (Germany BASF technology, working pressure 2Mpa). Although noble metal catalysts such as supported Pd / C and Pt / C have the advantages of high reactivity and low working pressure, the cost of the catalyst is high, and it is easy to deactivate due to carbon deposition or poisoning; while the Raney-Ni catalyst is cheap, but its The reaction pressure...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J23/89B01J23/883B01J23/83B01J23/887C07C211/51C07C209/36
Inventor 李忠闫少伟崔晓曦范辉郑华艳梁川
Owner TAIYUAN UNIV OF TECH
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