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a kind of in 2.24 (ncn) 3 Method for preparing aniline by catalytic hydrogenation reduction of nitrobenzene

A technology for nitrobenzene and aniline, which is applied in the field of In2.243 catalyzed hydrogenation and reduction of nitrobenzene to prepare aniline, can solve the problems of limited industrial application progress, difficult preparation of MoFs materials, complicated catalyst preparation process, etc., and achieves a short preparation period, The effect of stable structure and low cost

Active Publication Date: 2022-02-25
SHAANXI UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although these catalysts can efficiently catalyze the reductive hydrogenation of nitrobenzene to aniline at lower temperatures, the defects of the use of noble metals, the difficulty in preparing MoFs materials required for the dispersion of active components, and the complicated preparation process of the catalysts greatly limit this development. Industrial application progress of similar materials

Method used

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  • a kind of in <sub>2.24</sub> (ncn) <sub>3</sub> Method for preparing aniline by catalytic hydrogenation reduction of nitrobenzene
  • a kind of in <sub>2.24</sub> (ncn) <sub>3</sub> Method for preparing aniline by catalytic hydrogenation reduction of nitrobenzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] According to the In:N molar ratio of 1:18, weigh 1.5041g (5mmol) In(NO 3 ) 3 ·xH 2 O and 1.8910 g (15 mmol) of melamine were mixed fully and evenly in 15 mL of methanol, and then the solvent was evaporated to dryness by rotary evaporation at 50 ° C, and the resulting solid mixture was roasted at 650 ° C for 5 h in a nitrogen atmosphere, and cooled naturally to room temperature to obtain In 2.24 (NCN) 3 catalyst. Depend on figure 1 It can be seen that the XRD diffraction peaks of the obtained samples are similar to those of In 2.24 (NCN) 3 The powder standard diffraction peaks are consistent, indicating that the prepared sample is In 2.24 (NCN) 3 . In the diffraction peak area with 2θ value of 18-37.4°, the In 2.24 (NCN) 3 The average grain size is 117nm.

[0032] In a 100mL batch kettle, dissolve 100mg of nitrobenzene in 2mL of isopropanol, then add 100mg of In 2.24 (NCN) 3 The catalysts were fully mixed and reacted at 190°C for 2h under the condition of 3MPa...

Embodiment 2

[0034] In this example, the In prepared in Example 1 2.24 (NCN) 3 As a catalyst, in a 100mL batch kettle, dissolve 100mg of nitrobenzene in 2mL of isopropanol, and then add 100mg of In 2.24 (NCN) 3 The catalysts were fully mixed and reacted at 190°C for 1.5h under the condition of 3MPa hydrogen. After the reaction, it was detected by off-line chromatography (FuLi GC-9720), and the yield of the obtained aniline was 79.8%.

Embodiment 3

[0036] In this example, the In prepared in Example 1 2.24 (NCN) 3 As a catalyst, in a 100mL batch kettle, dissolve 100mg of nitrobenzene in 2mL of isopropanol, and then add 100mg of In 2.24 (NCN) 3 The catalysts were fully mixed and reacted at 190°C for 3h under the condition of 3MPa hydrogen. After the reaction, it was detected by off-line chromatography (FuLi GC-9720), and the yield of the obtained aniline was 99.9%.

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Abstract

The invention discloses an In 2.24 (NCN) 3 Catalytic nitrobenzene hydrogenation reduction prepares the method for aniline, and this method uses In 2.24 (NCN) 3 as catalyst, in H 2 Under the condition of 180-200 DEG C for 1-5 hours, the efficient catalytic reduction of nitrobenzene is realized, the conversion rate of nitrobenzene reaches 99.9%, and the selectivity of aniline reaches 99.8%. In which said In 2.24 (NCN) 3 The catalyst uses indium oxide, indium iodide, indium nitrate, and indium chloride as the indium source, and melamine and urea as the nitrogen source. Firstly, the indium source and the nitrogen source are fully mixed in the solvent, then evaporated to dryness, and roasted at high temperature And get. The preparation method of the catalyst used in the present invention has simple and safe operation steps, low cost, and a short preparation cycle. The catalyst is used in the reaction of nitrobenzene hydrogenation reduction to aniline, and realizes efficient catalytic conversion of nitrobenzene, and the structure of the catalyst It is stable and will not lose its activity after repeated recycling.

Description

technical field [0001] The invention belongs to the technical field of the application of catalysts and the preparation method of fine chemicals, in particular to an In 2.24 (NCN) 3 A method for preparing aniline by catalytic hydrogenation reduction of nitrobenzene. Background technique [0002] Aniline is the simplest primary aromatic amine. It is an important raw material and intermediate in the fine chemical process. It is widely used in rubber additives, medicine, dyes, pesticides, polyurethane production and other fields. For example, aniline can be used to produce rubber additives such as anti-aging agent A, anti-aging agent D, and accelerator M; it can also be used as an intermediate for pesticides such as triazophos, alachlor, hexazinone, and imidazoquinolinic acid; , It is also the raw material for the production of sulfonamides and the intermediate for the production of spices, plastics, varnishes, films, etc. The industrial production methods of aniline mainly ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/36C07C211/46B01J27/24B01J37/08
CPCB01J27/24B01J37/082B01J35/0013B01J35/006C07C209/36C07C211/46Y02P20/584
Inventor 何珍红王忠宇王宽刘昭铁王伟涛杨阳
Owner SHAANXI UNIV OF SCI & TECH
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