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Raney nickel catalyst for low-pressure hydrogenation of dinitrotoluene and its preparation method and application

A dinitrotoluene and catalyst technology, which is applied in the fields of Raney-type catalysts, amino compound preparation, physical/chemical process catalysts, etc., can solve the problems of large equipment investment, expensive catalysts, and high reaction pressure

Inactive Publication Date: 2016-04-06
TAIYUAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fundamentally solve two industrial dinitrotoluene hydrogenation technologies such as Sweden and DuPont technology in the United States. The catalyst is expensive, the catalyst is easily deactivated and the separation is difficult, and the reaction in the BASF technology requires additional solvents, high reaction pressure and equipment. big investment problem

Method used

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  • Raney nickel catalyst for low-pressure hydrogenation of dinitrotoluene and its preparation method and application
  • Raney nickel catalyst for low-pressure hydrogenation of dinitrotoluene and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Mix the 6μm nickel powder, 5μm Al powder and 8μmCr powder uniformly in the mass ratio of Ni55wt%-Al40wt%-Fe5wt%, and then place them in a crucible with SiC inlaid around and a leak at the bottom, and place the above crucible in a microwave oven In the Ar atmosphere of 0.8MPa, the temperature is increased to 1600°C at a rate of 80°C / min to melt, and then the molten alloy is sent to the atomization chamber through the funnel under the pressure of Ar gas, and is in the atomization chamber through the heat preservation nozzle Carry out the secondary cooling of gasification atomization and centrifugal atomization, the rotating disk speed of centrifugal atomization is 4000R / min, and the cooling rate is 1×10 6 K / s, then dried and sieved to obtain alloy powder with a particle size of 80-100 mesh;

[0045] (2) Mix the above-prepared alloy powder and sodium hydroxide solids and place them in a container. The mass ratio of sodium hydroxide and alloy powder is 1:1. Under normal tem...

Embodiment 2

[0050] (1) Mix the 3μm nickel powder, 7μm Al powder and 7μm iron powder uniformly in the mass ratio of Ni54wt%-Al42wt%-Fe4wt%, and then place them in a crucible with SiC inlaid around and a leak at the bottom. In a microwave oven, in an Ar atmosphere of 0.9MPa, the temperature is increased to 1550°C at a rate of 70°C / min to melt, and then the molten alloy is sent to the atomization chamber under the pressure of Ar gas, and is carried out in the atomization chamber through a heat preservation nozzle Two-stage cooling for gasification atomization and centrifugal atomization, the rotating disk of centrifugal atomization is 4500R / min, and the cooling rate is 1.2×10 6 K / s, then dried and sieved to obtain alloy powder with a particle size of 100-120 mesh;

[0051] (2) Mix the sodium hydroxide solid prepared above and alloy powder uniformly and place it in a container. The mass ratio of sodium hydroxide and alloy powder is 1.1:1. Under normal temperature conditions, add distilled water a...

Embodiment 3

[0055] (1) Mix 4μm nickel powder, 9μm Al powder and 6μmMo powder with a mass ratio of Ni53wt%-Al45wt%-Mo2wt%, and then place them in a crucible with SiC inlaid around and a leak at the bottom, and place the above crucible in a microwave oven In the Ar atmosphere of 1.0MPa, the temperature is increased to 1500°C at a rate of 60°C / min to melt, and then the molten alloy is sent to the atomization chamber under the pressure of Ar gas, and gas is carried out in the atomization chamber through the heat preservation nozzle. The two-stage cooling of chemical atomization and centrifugal atomization, the rotating speed of centrifugal atomization is 5000R / min, and the cooling rate is 1.3×10 6 K / s, then dried and sieved to obtain alloy powder with a particle size of 120-140 mesh;

[0056] (2) Mix the sodium hydroxide solid prepared above and alloy powder uniformly and place it in a container. The mass ratio of sodium hydroxide to alloy powder is 1.2:1. Add distilled water at a rate of 3ml / min...

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Abstract

A Raney nickel catalyst used for low-pressure hydrogenation of dinitrotoluenem. The catalyst is characterized by comprising, by mass, 80-90 wt% of nickel, 5-10 wt% of aluminium and 1.65-10 wt% of an auxiliary agent metal, wherein the nickel is in the form of a simple substance, the aluminium is in the form of the simple substance of an oxide and the auxiliary agent metal is in the form of the oxide. The catalyst is low in price and has an excellent performance of catalytic hydrogenation of the dinitrotoluenem (DNT) without an additional solvent and under a low-pressure condition of 1Mpa.

Description

Technical field [0001] The invention belongs to a Raney-Ni catalyst and a preparation method, and particularly relates to a low-pressure Raney-Ni catalyst used for the hydrogenation of dinitrotoluene to synthesize toluene diamine, and a preparation method and application thereof. Background technique [0002] Toluene diamine, also known as diaminotoluene (TDA), is an important chemical raw material and chemical intermediate. Its main purpose is to synthesize toluene diisocyanate (TDI). TDA is usually synthesized by hydrogenation of dinitrotoluene (DNT) in the presence of organic solvents and catalysts in industry, as shown in reaction formulas (1) and (2). At present, there are mainly two DNT hydrogenation technologies in the industry: the first is the Swedish and American DuPont technology, which uses a supported Pd+Pt / C precious metal catalyst. The catalyst has high hydrogenation activity, low reaction pressure (1MPa) and no reaction. Adding solvents and other advantages, but ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J25/02C07C211/50C07C209/36
Inventor 范辉李忠闫少伟崔晓曦
Owner TAIYUAN UNIV OF TECH
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