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Method using hydrophobically modified core-shell catalyst ZIF-67@SiO2 in transfer hydrogenation of cinnamaldehyde to prepare cinnamyl alcohol

A ZIF-67, core-shell catalyst technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve problems such as structural instability, achieve low production cost, low price, and solve structural instability Effect

Inactive Publication Date: 2019-09-13
XIANGTAN UNIV
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Problems solved by technology

[0007] Aiming at technical problems such as the unstable structure of ZIFs materials in the reaction, the present invention provides a hydrophobically modified core-shell catalyst ZIF-67@SiO 2 Method for preparing cinnamyl alcohol by transfer hydrogenation of cinnamaldehyde

Method used

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  • Method using hydrophobically modified core-shell catalyst ZIF-67@SiO2 in transfer hydrogenation of cinnamaldehyde to prepare cinnamyl alcohol

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Example 1 ZIF-67-@SiO 2 Used to catalyze the transfer hydrogenation reaction of cinnamaldehyde

[0027] (1) ZIF-67-@SiO 2 resolve resolution

[0028] 1.1 Preparation of ZIF-67@SiO by rapid stirring method 2

[0029] 3.4mmol Co(NO 3 ) 2 ·6H 2 O was dissolved in an appropriate amount of methanol solution, and ultrasonically dispersed for 10 minutes. Dissolve 23.8mmol 2-methylimidazole in an appropriate amount of methanol, and ultrasonically disperse for 10min. Slowly drop the prepared 2-methylimidazole solution into the prepared Co(NO 3 ) 2 ·6H 2 O solution, stirred at room temperature for 24 hours, washed by centrifugation, and washed three times with appropriate amount of DMF and methanol respectively; after repeated washing and centrifuged, the resulting precipitate was vacuum-dried at 80°C to obtain the catalyst ZIF-67. Take 0.1g ZIF-67 and dissolve it in 133.3mL methanol under ultrasonic. Then use 0.1mol / L NaOH to adjust the pH of the ZIF-67 solution to 8...

Embodiment 2

[0037] ZIF-67@SiO2 Used to catalyze cinnamaldehyde reaction cycle experiment test

[0038] The catalyst after the reaction in Example 1 was centrifuged and washed with ethanol several times, dried in vacuum at 80°C for 12 hours, and the recovered catalyst was reacted at 180°C and 1Mpa nitrogen for 18 hours, and the number of cycles was as follows:

[0039] Cycles temperature / ℃ time / h Pressure / MPa Conversion rate of cinnamyl alcohol Cinnamyl Alcohol Selectivity 1 180 18 1 98.63 93.65 2 180 18 1 98.79 93.26 3 180 18 1 97.65 94.01 4 180 18 1 97.32 94.28

[0040] It can be seen from the above table that the catalyst obtained in the present invention is applied in the reaction of cinnamaldehyde hydrogenation to cinnamyl alcohol, which is very stable and has very good cycle performance. After being recycled for 4 times, the catalytic performance does not decline, and the follow-up experimental results show that , continue t...

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Abstract

The invention discloses a method using a hydrophobically modified core-shell catalyst ZIF-67@SiO2 in transfer hydrogenation of cinnamaldehyde to prepare cinnamyl alcohol. The method is characterized in that the hydrophobically modified core-shell catalyst ZIF-67@SiO2 is added to a reaction, for hydrogenation of cinnamaldehyde to prepare cinnamyl alcohol, in the presence of isopropanol, the reaction temperature is controlled to be 160-190 DEG C, the reaction time is controlled to be 12-18 h, and the reaction pressure is controlled to be 1-4 MPa. The catalyst has a low raw material price, and adopts non-noble metal, so the preparation cycle is short, and the production cost is low; and when the hydrophobically modified core-shell catalyst ZIF-67@SiO2 is used in the hydrogenation of cinnamaldehyde, the stability of a ZIFs material improved, the problem of unstable structure of the ZIFs is solved, the reusability of the catalyst is improved, and the hydrophobicity of the catalyst is also significantly improved, so the conversion rate of cinnamaldehyde and the selectivity of the target product cinnamyl alcohol are greatly increased.

Description

technical field [0001] The invention relates to the preparation of catalysts, in particular to a hydrophobically modified core-shell catalyst ZIF-67@SiO 2 A method for preparing cinnamyl alcohol by transfer hydrogenation of cinnamaldehyde. Background technique [0002] α,β-unsaturated aldehydes are important chemical raw materials and intermediates. Cinnamaldehyde is a typical representative of α,β-unsaturated aldehydes, and the hydrogenation of its conjugated double bonds C=C and C=O has attracted extensive attention. The selective hydrogenation of C=O yields cinnamyl alcohol, which is an important raw material and intermediate for medicines and spices, and the selective hydrogenation of C=C yields phenylpropanal, which is an important intermediate for the preparation of HIV and other medicines. As a typical representative of α, β-unsaturated aldehydes, the hydrogenation of cinnamaldehyde has important theoretical significance and industrial application prospects. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C33/32C07C29/141
CPCB01J31/1691B01J31/1815B01J2231/643B01J2523/845C07C29/141C07C33/32
Inventor 刘平乐崔海帅吕扬熊伟郝芳罗和安
Owner XIANGTAN UNIV
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