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Raney nickel catalyst used for low-pressure hydrogenation of dinitrotoluenem, preparation method and application thereof

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

Inactive Publication Date: 2014-08-13
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 used for low-pressure hydrogenation of dinitrotoluenem, preparation method and application thereof
  • Raney nickel catalyst used for low-pressure hydrogenation of dinitrotoluenem, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Mix nickel powder, 5 μm Al powder, and 8 μm Cr powder with a particle size of 6 μm in a mass ratio of Ni55wt%-Al40wt%-Fe5wt%, and then place them in a crucible inlaid with SiC and with a leak at the bottom. In a microwave oven, under an Ar atmosphere of 0.8MPa, the temperature is raised 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 sprayed through the heat preservation nozzle. The chamber is used for secondary cooling of gasification atomization and centrifugal atomization. 6 K / s, then dried and sieved to obtain alloy powder with a particle size of 80-100 mesh;

[0045] (2) Mix the alloy powder and sodium hydroxide solid prepared above and place it in a container, the mass ratio of sodium hydroxide and alloy powder is 1:1, and distilled water is added dropwise at a rate of 5ml / min under normal temperature conditions Make it into a container, add water at ...

Embodiment 2

[0050] (1) Mix nickel powder, 7 μm Al powder, and 7 μm iron powder with a particle size of 3 μm nickel powder and 7 μm iron powder in a mass ratio of Ni54wt%-Al42wt%-Fe4wt%, and then place them in a crucible inlaid with SiC and with a leak at the bottom. In a microwave oven, under an Ar atmosphere of 0.9MPa, the temperature is raised 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 sprayed in the atomization chamber through the heat preservation nozzle. The secondary cooling of gasification atomization and centrifugal atomization treatment is carried out. The rotation speed of the rotary disc 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) Place the sodium hydroxide solid and alloy powder prepared above in a container evenly after being mixed, the mass ratio of so...

Embodiment 3

[0055](1) Mix nickel powder, 9 μm Al powder, and 6 μm Mo powder with a particle size of 4 μm nickel powder and 6 μm Mo powder in a mass ratio of Ni53wt%-Al45wt%-Mo2wt%, and then place them in a crucible inlaid with SiC around and with a leak at the bottom. In a microwave oven, under an Ar atmosphere of 1.0MPa, the temperature is raised 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 is sprayed in the atomization chamber through the heat preservation nozzle. The secondary cooling of gasification atomization and centrifugal atomization treatment is carried out. The rotation speed of the rotary disc 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) Place the sodium hydroxide solid and alloy powder prepared above in a container evenly after being mixed, the mass ratio of ...

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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 thereof, in particular to a low-pressure Raney-Ni catalyst used for hydrogenation of dinitrotoluene to synthesize toluenediamine, 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, and its main use is to synthesize toluene diisocyanate (TDI). TDA is usually synthesized industrially by hydrogenation of dinitrotoluene (DNT) in the presence of an organic solvent and a catalyst, as shown in reaction formulas (1) and (2). At present, there are two main DNT hydrogenation technologies in the industry: the first one is Sweden and the DuPont technology in the United States, which uses supported Pd+Pt / C noble metal catalysts. The catalyst has high hydrogenation activity, low reaction pressure (1MPa) and no need for reaction. Adding solvent and other ad...

Claims

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Application Information

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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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