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Capillary type efficient palladium-loaded zirconium based metal organic framework film microreactor, dynamic in-situ preparation method and application thereof

A technology of organic framework and micro-reactor, which is applied in the preparation of organic compounds, chemical instruments and methods, preparation of amino hydroxyl compounds, etc. It can solve the poor stability of ZIF-8 membrane and obtain membrane catalytic microreactor, which cannot realize the preparation of membrane catalysis layers and other issues to achieve the effect of solving poor stability

Active Publication Date: 2017-07-04
DALIAN UNIV OF TECH
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

However, this method cannot realize the preparation of Pd / UiO-66-NH in a quartz capillary microreactor 2 Membrane catalytic layer
Kong et al[APTES-assisted synthesis of ZIF-8films on the inner surface of capillaryquartz tubes via flow system.Materials Letters.2015(141):344-346.] first treated the inner surface of the quartz tube with APTES, and then prepared ZIF-8 by flow However, due to the poor stability of the ZIF-8 membrane, it is difficult to use it as a carrier for loading palladium nanoparticles in a microreactor and obtain a membrane catalytic microreactor
Therefore, at present, for the preparation of Pd / UiO-66-NH in capillary quartz tube microreactor 2 Membrane catalytic layer, to construct a high-efficiency capillary quartz tube membrane catalytic microreactor, has not yet been reported

Method used

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  • Capillary type efficient palladium-loaded zirconium based metal organic framework film microreactor, dynamic in-situ preparation method and application thereof
  • Capillary type efficient palladium-loaded zirconium based metal organic framework film microreactor, dynamic in-situ preparation method and application thereof
  • Capillary type efficient palladium-loaded zirconium based metal organic framework film microreactor, dynamic in-situ preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) UiO-66-NH on the capillary 2 Membrane synthesis

[0034] ①Select a capillary quartz tube with a length of 25cm and an inner diameter of 530μm as the microchannel. The cross-sectional topography of the capillary quartz tube is as follows Figure 1b ;

[0035] ②Prepare 20mL of 1mmol / L hydrochloric acid aqueous solution. At room temperature, with the help of a micro pump, continue to flow at a flow rate of 20μL / min for 30 minutes; then use deionized water to flow continuously at a flow rate of 20μL / min to wash away the acid until the capillary The pH at the outlet of the quartz tube is 7; prepare 20mL of 1mmol / L NaOH aqueous solution, and continue to flow at a flow rate of 20μL / min for 30min at 80℃ with the help of a micro pump; then use deionized water to flow continuously at a flow rate of 20μL / min , Wash away the lye until the pH at the outlet of the capillary quartz tube is 7, then air-dried at 100°C for later use;

[0036] ③ Measure 0.3 mL of 3-aminopropyltriethoxysilan...

Embodiment 2

[0046] (1) UiO-66-NH on capillary quartz tube 2 The synthesis of the membrane is the same as in Example 1;

[0047] (2)UiO-66-NH 2 Preparation of Pd Nanoparticles on Film

[0048] ①The preparation concentration is 0.02mmol / L H 2 PdCl 4 The HCl solution of 10mL, with the help of a micro pump, continues to flow at a flow rate of 20μL / min; the ambient temperature is 35°C. The flow time is 30 minutes, and then the residual palladium ions are dynamically treated and rinsed with deionized water at a flow rate of 20 μL / min at a temperature of 25°C;

[0049] ②Weigh 0.019g of NaBH 4 The solid is dissolved in 50mL deionized water and prepared into NaBH with a concentration of 10mmol / L 4 The aqueous solution, driven by a micro pump, flows continuously at a flow rate of 25 μL / min at room temperature for 4 hours, then rinses with deionized water and blast-dried at 80°C;

[0050] UiO-66-NH loaded with Pd nanoparticles 2 Membrane microreactor catalyzed NaBH 4 The application of reducing p-nitropheno...

Embodiment 3

[0052] (1) UiO-66-NH on capillary quartz tube 2 The synthesis of the membrane is the same as in Example 1;

[0053] (2)UiO-66-NH 2 Preparation of Pd Nanoparticles on Film

[0054] ①The preparation concentration is 2mmol / L H 2 PdCl 4 The HCl solution of 10mL, with the help of a micro pump, continues to flow at a flow rate of 20μL / min; the ambient temperature is 35°C. The flow time is 30 minutes, and then the residual palladium ions are dynamically treated and rinsed with deionized water at a flow rate of 20 μL / min at a temperature of 25°C;

[0055] ②Weigh 0.076g of NaBH 4 The solid is dissolved in 50mL deionized water to prepare NaBH with a concentration of 40mmol / L 4 The aqueous solution, driven by a micro pump, flows continuously at a flow rate of 25 μL / min at room temperature for 3 hours, then rinses with deionized water and blast-dried at 80°C;

[0056] UiO-66-NH loaded with Pd nanoparticles 2 Membrane microreactor catalyzed NaBH 4 The application of reducing p-nitrophenol is the s...

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Abstract

Belonging to the technical field of microreactors, the invention provides a capillary type efficient palladium-loaded zirconium based metal organic framework film microreactor, a dynamic in-situ preparation method and application thereof. The preparation method includes: introducing a 3-aminopropyltriethoxysilane chemical modification layer to an inner surface of a capillary quartz tube microreactor by dynamic method in advance; then under a continuum flow state, growing a UiO-66-NH2 zirconium based metal organic framework film layer of certain thickness; and finally, using impregnation-reduction method for continuous dynamic preparation of the UiO-66-NH2 zirconium based metal organic framework film palladium-loaded film microreactor. The invention establishes a simple and convenient new method for preparation of a film microreactor, the prepared palladium-loaded zirconium based metal organic framework film microreactor has the characteristics of continuous film layers and controllable thickness, uniformly distributed Pd nanoparticles and firm combination, and difficult fall. The film microreactor has excellent excellent catalytic efficiency in the reaction of catalyzing NaBH4 for reduction of nitrophenol organic matters, and can run stably for a long time.

Description

Technical field [0001] The invention belongs to the field of microreactors, and relates to a capillary type high-efficiency palladium-zirconium-based metal organic framework membrane microreactor, a dynamic in-situ preparation method and applications thereof. Background technique [0002] Hydrogenation reduction of nitro compounds is an important process in chemical production. Unsupported catalysts such as platinum and palladium are commonly used in catalytic hydrogenation. They are expensive, difficult to separate and recover, and easy to deactivate. They have a great impact on the service life of the catalyst and greatly limit its wide application in industry. Therefore, loading catalysts on various supports to prepare supported catalysts with excellent recovery performance has become a research hotspot in the catalysis of nitro compound hydrogenation reduction reactions. [0003] In recent years, the development of microreactors has attracted more and more attention from resea...

Claims

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Application Information

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IPC IPC(8): B01J19/00B01J31/22C07C213/02C07C215/76
CPCB01J19/0093B01J31/1691B01J31/1805B01J2219/00795B01J2219/00835B01J2231/641B01J2531/824C07C213/02C07C215/76
Inventor 张雄福李静吴飞超刘海鸥
Owner DALIAN UNIV OF TECH
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