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
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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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