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Noble metal/amino MOFs selective hydrogenation catalyst, preparation method and application thereof

A hydrogenation catalyst and noble metal technology, which is applied in the preparation of hydroxyl compounds, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve problems such as high surface energy, small size, and easy agglomeration , to achieve high selectivity and high stability

Inactive Publication Date: 2020-01-10
北京氦舶科技有限责任公司
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Problems solved by technology

[0003] Activity, selectivity, and stability are the most important performance indicators of catalysts. Single-atom noble metal catalysts have high activity and high selectivity, and are expected to be used in the selective hydrogenation of cinnamaldehyde to cinnamyl alcohol. However, the size of single-atom noble metal particles is small and the surface High energy, easy to agglomerate when loaded on the carrier, resulting in reduced catalytic activity and stability

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  • Noble metal/amino MOFs selective hydrogenation catalyst, preparation method and application thereof

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preparation example Construction

[0027] The preparation method of the supported noble metal / amino MOFs selective hydrogenation catalyst of the present invention comprises the following steps:

[0028] (1) Low-temperature liquid phase reduction to prepare single-atom noble metal sol;

[0029] (2) Load the single-atom noble metal sol in step (1) into the amino MOFs material to obtain a supported noble metal / amino MOFs selective hydrogenation catalyst.

[0030] Preferably, step (1) specifically includes the following steps: (1a) Slowly add the reducing agent solution to the noble metal precursor solution dropwise under the condition of -50-0°C, and after the dropwise addition, continue to complete the reaction to obtain a single atom Precious metal sol.

[0031] Preferably, the noble metal in step (1a) is Pt, and the noble metal precursor is a soluble salt of Pt, such as any one of H2PtCl4, H2PtCl6, K2PtCl6, Na2PtCl6, K2PtCl4 or Na2PtCl4 or a mixture of at least two .

[0032] Preferably, the concentration of...

Embodiment 1

[0056] Preparation of porous grade UiO66-NH2:

[0057] Weigh 0.8g of ZrCl4, 0.6g of 2-aminoterephthalic acid and dissolve in 200mL N,N-dimethylformamide to obtain a mixed solution; the mixed solution is sonicated for 5min, and then transferred to water with a Teflon cannula In a thermal reaction kettle, crystallize at 120°C for 24 hours to obtain the reaction product; after the reaction product is cooled to room temperature, wash with N,N-dimethylformamide solution and methanol solution three times respectively, and vacuum dry at 100°C for 12 hours to prepare Porous grade UiO-66-NH2.

Embodiment 2

[0059] Preparation of Supported Noble Metal / Amino MOFs Selective Hydrogenation Catalyst:

[0060] Configure 10mL 0.0001MH 2 PtCl 6 solution and 50mL0.001M hydrazine hydrate solution, H 2 PtCl 6 The solvent of the solution and the hydrazine hydrate solution is a mixture of water and ethanol with a volume ratio of 1:9.

[0061] H 2 PtCl 6 The solution and the hydrazine hydrate solution were placed in a high and low temperature box, and when the temperature dropped to -50°C, the hydrazine hydrate solution was slowly added dropwise to the H 2 PtCl 6 In the solution, after the dropwise addition, the reaction was continued at -50° C. for 2 h to obtain a single-atom Pt sol.

[0062] Weighed 1.95g of porous UiO66-NH2 into the above single-atom Pt sol, stirred for 10h, washed alternately with water and ethanol, and dried in vacuum at 100°C for 12h to prepare the supported noble metal / amino MOFs selective hydrogenation catalyst.

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Abstract

The invention specifically relates to a supported noble metal / amino MOFs selective hydrogenation catalyst, a preparation method and application thereof. The preparation method of the supported noble metal / amino MOFs selective hydrogenation catalyst comprises the following steps of: (1) preparing a monoatomic noble metal sol through low-temperature liquid phase reduction; (2) loading the monoatomicnoble metal sol in the step (1) into an amino MOFs material to obtain the supported noble metal / amino MOFs selective hydrogenation catalyst. The catalyst can be used in the selective hydrogenation ofcinnamaldehyde to prepare cinnamyl alcohol. The catalyst has the characteristics of high activity, high selectivity and high stability.

Description

technical field [0001] The invention belongs to the field of precious metal catalyzed organic compound synthesis, and in particular relates to a noble metal / amino MOFs selective hydrogenation catalyst, a preparation method and an application thereof. Background technique [0002] α, β-unsaturated aldehydes are selectively hydrogenated to α, β-unsaturated alcohols, which are important raw materials and intermediates in the production of fragrances, pharmaceuticals and other fine chemical products, and are also widely used in organic synthesis. Cinnamaldehyde is a typical representative of α, β unsaturated aldehyde, it has benzene ring, C=O double bond and C=C double bond, forms a conjugated system, because the bond energy of C=C bond (615KJ·mol- 1) Lower than the C=O bond (715KJ mol-1), the hydrogenation of the former is thermodynamically more favorable, making it difficult to selectively hydrogenate on the C=O bond without destroying C=C, hydrogenation selectivity poor. On...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28C07C29/141C07C33/32
CPCB01J31/28C07C29/141B01J2231/643B01J2531/48B01J2531/0205B01J35/399B01J35/393B01J35/23C07C33/32
Inventor 郭文雅关超阳郎嘉良赵刚黄翟
Owner 北京氦舶科技有限责任公司
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