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Continuous production process of dinitrotoluene for synthesis of toluenediamine by low-pressure hydrogenation, catalyst and catalyst preparation method

A technology of dinitrotoluene and toluenediamine, which is applied in the fields of chemical recovery and organic chemistry, and can solve the problems of large investment in equipment, the need for additional solvents, and high reaction pressure

Inactive Publication Date: 2015-09-16
SEDIN ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to achieve the above-mentioned purpose, the present invention breaks through the shackles of conventional technical cognition that nickel-based catalysts need to add solvents and reaction pressures up to 2MPa in the hydrogenation reaction of dinitrotoluene, and through a large number of catalyst modification experiments, activity evaluation experiments and mechanism research The analysis screened and compared various nickel-based catalysts, and successfully developed a Raney nickel catalyst with activity similar to noble metal catalysts under the condition of low pressure 1MPa and no external solvent; and according to the catalytic performance of the developed Raney nickel catalyst, Strength and settling properties, through a large number of theoretical calculations and experimental research, a new process for the continuous production of toluenediamine by hydrogenation of dinitrotoluene was further developed; the invention of a new process for the hydrogenation of dinitrotoluene with Raney nickel catalyst It not only completely overcomes the shortcomings of the existing two industrial DNT hydrogenation technologies, but fundamentally solves the two industrial dinitrotoluene hydrogenation technologies such as Sweden and DuPont in the United States. The problems existing in the reaction with BASF technology require additional solvent, high reaction pressure and large investment in equipment

Method used

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  • Continuous production process of dinitrotoluene for synthesis of toluenediamine by low-pressure hydrogenation, catalyst and catalyst preparation method
  • Continuous production process of dinitrotoluene for synthesis of toluenediamine by low-pressure hydrogenation, catalyst and catalyst preparation method
  • Continuous production process of dinitrotoluene for synthesis of toluenediamine by low-pressure hydrogenation, catalyst and catalyst preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Mix 6μm nickel powder, 5μm aluminum powder and 8μm auxiliary metal powder with a mass fraction of Ni55wt%—Al40wt%—Fe5wt%, and place them in a crucible with a funnel at the bottom and inlaid with SiC. It is heated to 1600℃ and melted at a rate of min., and the alloy powder is obtained after 0.8MPa Ar gasification and atomization. The cooling rate is 1.0×10 6 K / s; Mix the alloy powder and NaOH powder in a mass ratio of 1:1, and add 3 times the volume of the alloy powder to the container at room temperature. The dropping acceleration keeps the material evenly wet but does not form a liquid phase; After the dropwise addition, the suspension was sonicated for 40 min under the conditions of 20kHZ and 70°C, and then washed with distilled water to obtain the catalyst, which was stored in water for later use. The specific process route and reaction conditions of the catalyst prepared in this example for hydrogenation of dinitrotoluene are as follows:

[0054] (1) Prepare the prepar...

Embodiment 2

[0059] Mix 5μm nickel powder, 7μm aluminum powder and 7μm auxiliary metal powder with a mass fraction of Ni53wt%—Al43wt%—auxiliary 4wt%, and place them in a crucible with a funnel at the bottom and inlaid with SiC. It is heated to 1550°C at a rate of ℃ / min to melt, and the alloy powder is obtained after being vaporized and atomized by 0.9MPa Ar. The cooling rate is 1.2×10 6 K / s; Mix the alloy and NaOH powder at a mass ratio of 1.1:1, and add 4 times the volume of the alloy powder to the container at room temperature. The dropping rate keeps the material evenly wet but does not form a liquid phase; After the addition, the suspension was sonicated for 35 min under the conditions of 30kHZ and 60°C, and then washed with distilled water to obtain the target catalyst, which was stored in water for later use. The specific process route and reaction conditions of the catalyst prepared in this example for hydrogenation of dinitrotoluene are as follows:

[0060] (1) Prepare the prepared Ra...

Embodiment 3

[0065] Mix 4μm nickel powder, 9μm aluminum powder and 6μm auxiliary metal powder with a mass fraction of Ni53wt%—Al45wt%—auxiliary 2wt%, and place them in a crucible with a funnel at the bottom and inlaid with SiC. It is heated to 1500℃ to melt at the rate of ℃ / min, and the alloy powder is obtained after vaporization and atomization with 1.0MPa Ar. The cooling rate is 1.3×10 6 K / s; Mix the alloy and NaOH powder in a mass ratio of 1:2, and add 5 times the volume of the alloy powder to the container at room temperature. The dropping rate keeps the material evenly wet but does not form a liquid phase; After the addition, the suspension was sonicated at 50kHZ and 60°C for 30min, and then washed with distilled water to obtain the catalyst, which was stored in water for later use. The specific process route and reaction conditions of the catalyst prepared in this example for hydrogenation of dinitrotoluene are as follows:

[0066] (1) Prepare the prepared Raney-Ni catalyst and DNT in a...

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Abstract

The invention discloses a process for continuously producing toluenediamine through low-pressure hydrogenation synthesis of dinitrotoluene. The process comprises the steps of preparing a fresh Raney nickel catalyst and dinitrotoluene into fresh catalyst slurry, and adding the fresh catalyst slurry into a hydrogenation reactor; respectively adding raw materials, namely, dinitrotoluene and hydrogen into the hydrogenation reactor to react, overflowing a liquid-phase reaction product into a clean reactor, pumping the liquid-phase product in the clean reactor into a catalyst thickener, enabling gases to enter a purge gas separator from the top, returning the thickened catalyst slurry to the hydrogenation reactor, delivering clear liquid into a filter for filtering to obtain a crude toluenediamine product. The process has the advantages of low equipment investment, low energy consumption and capability of synthesizing toluenediamine through dinitrobenzene hydrogenation under the conditions that no additional solvent is added and the low pressure is kept at about 1MPa.

Description

Technical field [0001] The invention belongs to a process for synthesizing toluene diamine, and in particular relates to a continuous production process for synthesizing toluene diamine by low-pressure hydrogenation of dinitrotoluene, and a method for preparing the used Raney nickel catalyst and the catalyst. Background technique [0002] Toluene diamine (TDA), also known as diaminotoluene, is an important chemical raw material and chemical intermediate, mainly used in the synthesis of polyurethane materials. In industry, toluene diamine is usually synthesized by hydrogenation of dinitrotoluene (DNT) in the presence of an organic solvent and a catalyst. At present, there are two main DNT hydrogenation technologies: the first is to use supported Pd / C and Pt / C The DuPont technology of Sweden and the United States of other precious metal catalysts has the advantages of low reaction pressure and high catalyst activity, but it has the disadvantages of difficult catalyst separation, ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/50
CPCY02P20/584
Inventor 李改英范辉王月玲
Owner SEDIN ENG
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