Preparation for supported type noble metal-based catalyst using core-shell structure MOF as reaction vessel and application of catalyst

A core-shell structure and reaction vessel technology, applied in the preparation of carbon-based compounds, organic compounds, physical/chemical process catalysts, etc., can solve the problems of few research reports and achieve simple preparation methods, not easy to lose, and high yield Effect

Active Publication Date: 2018-10-12
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many reports on MOFs as carriers to support nanoparticles and their application in catalysis, but in contrast, there are still few research reports on MOF-based core-shell structures.

Method used

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  • Preparation for supported type noble metal-based catalyst using core-shell structure MOF as reaction vessel and application of catalyst
  • Preparation for supported type noble metal-based catalyst using core-shell structure MOF as reaction vessel and application of catalyst
  • Preparation for supported type noble metal-based catalyst using core-shell structure MOF as reaction vessel and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Step 1: Dissolve 15 mg of palladium chloride and 77 mg of polyvinylpyrrolidone in a mixture of 85 mL of methanol and 15 mL of deionized water, and reflux at 70°C for 4 hours to obtain a Pd nanoparticle solution.

[0023] The second step: Weigh 30mg of terephthalic acid, 60mg of nickel nitrate and 40mg of zinc nitrate and dissolve them in a mixed solution of N,N-dimethylformamide (8mL) and ethylene glycol (5mL), after stirring for 1 hour, Transfer to a polytetrafluoroethylene reactor at a reaction temperature of 150°C. After reacting for 1.5 hours, add the Pd nanoparticle solution (3.5 mL) synthesized above, and react for 4 hours. Then cool, centrifuge, wash, activate, and dry to prepare Pd@Ni / Zn-MOF, noble metal Pd nanoparticles were successfully loaded in the cavity (mainly in the cavity) between the core-shell structure of the core-shell Ni / Zn-MOF.

[0024] Step 3: Weigh 20mg of catalyst Pd@Ni / Zn-MOF, 5mL of isopropanol, 0.5mmol of cinnamaldehyde, transfer to a high-p...

Embodiment 2

[0026] The first step: Weigh 16.6mg of polyvinylpyrrolidone and dissolve it in 45mL of ethanol, add 5.0mL of H 2 PtCl 6 (6.0mM) aqueous solution, condensed and refluxed for 3h to obtain a Pt nanoparticle solution.

[0027] The second step: Weigh 30mg of terephthalic acid, 50mg of nickel nitrate and 50mg of zinc nitrate and dissolve them in a mixed solution of N,N-dimethylformamide (10mL) and ethylene glycol (5mL), after stirring for 1 hour, Transfer to a polytetrafluoroethylene reactor, add the Pt nanoparticle solution (5mL) synthesized above, the reaction temperature is 140°C, the reaction time is 6 hours, then cooled, centrifuged, washed, activated, and dried to prepare Pt@Ni / Zn- MOF, noble metal Pd nanoparticles were successfully supported in the core (mainly in the core) of the core-shell structure Ni / Zn-MOF.

[0028] Step 3: Weigh 50mg of catalyst Pt@Ni / Zn-MOF, 5mL of isopropanol, 0.4mmol of cinnamaldehyde, transfer to a high-pressure reactor, feed hydrogen at 1.0MPa, s...

Embodiment 3

[0030] Step 1: Weigh 100mL of HAuCl 4 (0.01%) aqueous solution, condensation reflux, add the aqueous solution of sodium citrate (1%) of 4.5mL, after condensation reflux 20 minutes, drop to room temperature, add 20mL polyvinylpyrrolidone (0.5g) aqueous solution, stir 24 hours at room temperature, Au nanoparticle solution was obtained.

[0031] The second step: Weigh 30mg of terephthalic acid, 60mg of nickel nitrate and 40mg of zinc nitrate and dissolve them in a mixed solution of N,N-dimethylformamide (8mL) and ethylene glycol (5mL), after stirring for 1 hour, Transfer to a polytetrafluoroethylene reactor at a reaction temperature of 150°C. After 6 hours of reaction, add the Au nanoparticle solution (3.5 mL) synthesized above, stir at room temperature, and then centrifugally wash, activate, and dry to prepare Au@ Ni / Zn-MOF, noble metal Pd nanoparticles were successfully loaded outside the shell (mainly outside the shell) of the core-shell structure Ni / Zn-MOF.

[0032] Step 3:...

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Abstract

The invention discloses preparation for a supported type noble metal-based catalyst using a core-shell structure metal-organic framework (MOF) as a reaction vessel and an application of the catalyst,and belongs to the technical field of catalysts. Bimetal Ni / Zn-MOF with a core-shell structure is used as a carrier, noble metal nanoparticles can be encapsulated into a hollow cavity between a core and a shell by regulation and control, the inner core can be used as a carrier to uniformly disperse noble metal palladium nanoparticles, the outer shell can play a protective role to inhibit loss of the noble metal nanoparticles, and a Pd@Ni Zn-MOF with a multi-stage structure is constructed. Catalytic performance of the catalyst for selective hydrogenation of carbon-carbon double bonds and carbon-oxygen double bonds is studied under a hydrogen gas atmosphere. The preparation method disclosed by the invention is simple and easy to implement and has a high yield; the prepared catalyst carrier Ni Zn-MOF has a large specific surface area, thereby facilitating uniform dispersion of the noble metal nanoparticles; the prepared catalyst carrier Ni / Zn-MOF has rich pores, thereby facilitating diffusion of reaction substrates and products; and the prepared catalyst carrier Ni / Zn-MOF can play a role of molecular size selection, so that the catalyst has excellent catalytic activity and selectivity.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and relates to a nano-reactor with a core-shell structure (NiZn-MOFs) as a carrier to construct a loaded noble metal-based multi-level structure catalyst, which is applied to carbon-carbon double bonds and carbon Selective hydrogenation of oxygen double bonds. Background technique [0002] The selective catalytic hydrogenation of α-β unsaturated aldehydes is one of the important reactions in the synthesis of fine chemical products. It has been widely used in modern fine organic synthesis, especially in the preparation of drugs and their intermediates, food additives, spices, etc. . The method of catalytic hydrogenation can greatly reduce product cost, improve product quality, increase yield, shorten reaction time and reduce three-waste discharge, so it is widely valued by people. According to literature reports, the C=C hydrogenation selectivity of the catalyst Pd is relatively high. Bond hy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C45/62C07C47/228
CPCB01J31/1691B01J31/2239B01J35/006B01J35/0073B01J2231/645B01J2531/26B01J2531/847C07C45/62C07C47/228
Inventor 李建荣周阿武豆义波谢亚勃
Owner BEIJING UNIV OF TECH
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