A preparation method of nitrogen-doped carbon nanomaterial and its application in hydrogenation reaction of nitrobenzene

A nanomaterial, nitrogen-doped carbon technology, applied in the preparation of organic compounds, the preparation of amino compounds, chemical instruments and methods, etc., can solve the problems of corrosion equipment and storage hazards, high production costs, and high production equipment and process control requirements. problem, to achieve the effect of low raw material price, short time consumption, and improved catalytic performance

Active Publication Date: 2021-03-16
JILIN INST OF CHEM TECH
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Problems solved by technology

[0007] In view of this, the present invention provides a green metal-free, low-cost, simple process, stable product performance, high catalytic efficiency and recyclable carbon nanomaterials derived from nitrogen-rich covalent organic framework materials. Preparation method , and its application in the hydrogenation reaction of nitrobenzene, and the technical solution of the present invention solves the hidden dangers of high production cost, corrosion equipment and storage hazards in the existing catalytic nitrobenzene hydrogenation reaction, and the control of production equipment and processes Demanding deficiency

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  • A preparation method of nitrogen-doped carbon nanomaterial and its application in hydrogenation reaction of nitrobenzene
  • A preparation method of nitrogen-doped carbon nanomaterial and its application in hydrogenation reaction of nitrobenzene
  • A preparation method of nitrogen-doped carbon nanomaterial and its application in hydrogenation reaction of nitrobenzene

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[0038] The embodiment of the present invention discloses a method for preparing nitrogen-doped carbon nanomaterials derived from nitrogen-rich covalent organic framework materials. : 1.5 was dissolved in 36mL dimethyl sulfoxide solution, the solution mixture was transferred to the reaction kettle at 165°C for 72h, cooled naturally, the product was filtered with suction, washed several times with absolute ethanol, acetone, tetrahydrofuran, and dichloromethane successively, and dried to obtain The white powder is then subjected to high-temperature carbonization in a tube furnace to obtain carbon nanomaterial CC-X (X represents the carbonization temperature).

[0039] On the basis of the above-mentioned CC-X catalyst provided by the present invention, the applicant has carried out research on using CC-X catalysts with different carbonization temperatures to catalyze the hydrogenation reaction of nitrobenzene. The steps of the catalytic reaction are as follows:

[0040] Add cataly...

Embodiment 5

[0049] All use CC-700 as catalyst in embodiment 5,9,10, the consumption that adds hydrazine hydrate is also the same, but the temperature of reaction is different, other catalytic reaction conditions are all the same. It can be seen from the experimental data that the conversion of nitrobenzene is beneficial to the increase of the reaction temperature. In Example 5, the reaction temperature is 100° C., and the conversion rate of nitrobenzene is 96%. But the reaction temperature is too high. In Example 10, the conversion rate of nitrobenzene drops to 35%, which may be related to the evaporation of solvent ethanol and reducing agent hydrazine hydrate.

[0050] In Examples 9, 11, and 12, CC-700 was used as a catalyst, and the same amount of hydrazine hydrate was added as a reducing agent. The reaction temperature was 80°C, but the solvents added were different. After 4 hours of reaction, ethanol was used as a solvent for the reaction of nitro Both the conversion of benzene and th...

Embodiment 13

[0051] In Examples 13, 14, and 15, except that the amount of catalyst CC-700 added is different, other catalytic reaction conditions are the same. It can be seen from the experimental data that the amount of catalyst CC-700 added in Example 13 is the largest, the yield of aniline is also the highest, the catalytic effect is good, and the utilization rate of the catalyst is 15mmol g -1 h -1 . In Example 15, the amount of catalyst CC-700 added is the least, and the yield of aniline is also the lowest, but the utilization rate of the catalyst is 30mmol·g -1 h -1 , is the highest among the three examples.

[0052] In Examples 5, 15, and 16, the catalytic reaction conditions are the same, only the reaction time is different. It can be seen that the yield of aniline has been significantly improved with the increase of the reaction time.

[0053] in addition, figure 1 It is a line graph showing the change of aniline output with reaction time when catalyzing the hydrogenation rea...

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Abstract

A preparation method of nitrogen-doped carbon nanomaterials and its application in nitrobenzene hydrogenation reaction. The invention discloses a preparation method of nitrogen-doped carbon nanomaterials derived from nitrogen-rich covalent organic framework materials, Nitrogen-doped carbon nanomaterials were obtained by high-temperature carbonization of nitrogen-rich covalent organic framework materials, which were used to catalyze the hydrogenation reaction of nitrobenzene. The preparation method of the precursor of the nitrogen-doped carbon nanomaterial is simple, the process of preparing the nitrogen-doped carbon nanomaterial is simple and time-consuming, the selectivity of catalyzing the hydrogenation of nitrobenzene to generate aniline is high, and the utilization rate of the catalyst is high, which can be used in Industrialized mass production.

Description

technical field [0001] The invention relates to the technical field of synthesis of chemical catalytic materials, in particular to a preparation method of a nitrogen-doped carbon nanomaterial derived from a nitrogen-rich covalent organic framework material and its application in the hydrogenation reaction of nitrobenzene. Background technique [0002] Nitrobenzene compounds widely exist in industrial wastewater as pollutants, which have aroused urgent concern for human health and environmental protection. As the reduction product of nitroaromatic compounds, aniline is an important intermediate for the synthesis of dyes, pesticides, drugs and chelating agents, and has broad application prospects. [0003] The catalytic hydrogenation method prepares aniline compounds by reducing nitrobenzene, which is currently the main method for preparing aniline compounds. Traditional catalysts mainly include nickel-based catalysts, palladium-based catalysts, iron-based catalysts, and copp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J37/08C07C209/36C07C211/46
CPCB01J27/24B01J37/084C07C209/325C07C211/46
Inventor 高文秀邢树宇吕杰琼谢晖娄大伟王集思张志会
Owner JILIN INST OF CHEM TECH
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