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A kind of uio-66-nh2 composite catalyst supporting transition metal copper and its preparation method and application

A technology of uio-66-nh2 and composite catalysts, which is applied in the direction of physical/chemical process catalysts, catalytic reactions, organic compounds/hydrides/coordination complex catalysts, etc., can solve problems such as thinness, and achieve cost reduction and economic reduction The effect of less cost and usage

Active Publication Date: 2018-08-10
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the research of scientists mainly focuses on the loading of precious metals such as gold, silver, platinum, palladium, ruthenium, etc., while the research on the loading of cheap transition metals is relatively thin.

Method used

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  • A kind of uio-66-nh2 composite catalyst supporting transition metal copper and its preparation method and application
  • A kind of uio-66-nh2 composite catalyst supporting transition metal copper and its preparation method and application
  • A kind of uio-66-nh2 composite catalyst supporting transition metal copper and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Metal Organic Framework UiO-66-NH 2 preparation of

[0040] Concrete preparation steps are as follows:

[0041] Take ZrCl 4 (139.9mg, 0.60mmol) and CH 3 COOH (538μL, 9.4mmol) was dissolved in 15mL DMF solution, sonicated for 30min, after the solution was clarified, 2-aminoterephthalic acid (108.6mg, 0.60mmol) was added, and sonicated for 10min, the solution was transferred to an autoclave, Heating at 120°C for 24 hours, after the reaction is complete, centrifuge, wash and activate to obtain UiO-66-NH 2 Metal organic framework material 95.0mg, yield 89.7%.

[0042] For the UiO-66-NH prepared in this example 2 For characterization, IR, fluorescence such as figure 1 , 2 shown.

Embodiment 2

[0043] Example 2: Cu(Ⅱ)@UiO-66-NH 2 preparation of

[0044] Take UiO-66-NH 2 10.0 mg, placed in 2 mL of Cu(OAc) with a concentration of 0.02 mol / L 2 After soaking in the ethanol solution for 1 hour, centrifuge, soak and wash with ethanol three times, and dry at 80°C for 12 hours to obtain Cu(Ⅱ)@UiO-66-NH 2

[0045] Characterization of Cu(Ⅱ)@UiO-66-NH by fluorescence, IR, XPS and SEM 2 , see the results respectively figure 2 , 3 , 4 and 5.

Embodiment 3

[0046] Example 3: Cu(0)@UiO-66-NH 2 Preparation of composite catalyst

[0047] The Cu(Ⅱ)@UiO-66-NH prepared in Example 2 2 N 2 Add 10mL of ethanol and 50mL of dichloromethane under protection, stir to form a uniform turbid liquid, maintain the reaction system at 0°C and add 2mL of NaBH with a concentration of 7.5mg / mL dropwise 4 aqueous solution, after the dropwise addition, the ice bath was removed, the reaction system was gradually raised to room temperature, continued to stir for 0.5 hours, and centrifuged to obtain Cu(0)@UiO-66-NH 2 .

[0048] Characterization of Cu(0)@UiO-66-NH by fluorescence, IR, XPS, SEM and TEM 2 , see the results respectively figure 2 , 6 , 7, 8 and 9.

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Abstract

The invention discloses a composite catalyst Cu(0)@UiO-66-NH2. The preparation method of the composite catalyst consists of: firstly, synthesizing a metal organic framework UiO-66-NH2; then, soaking the UiO-66-NH2 material in a copper acetate ethanol solution for 1h at room temperature, then conducting ethanol washing and drying to obtain a Cu(II)@UiO-66-NH2 composite metal organic framework material; and finally, reducing the Cu(II)@UiO-66-NH2 composite metal organic framework material with an aqueous solution of sodium borohydride so as to obtain the composite catalyst Cu(0)@UiO-66-NH2. The catalyst can effectively catalyze styrene reduction reaction without reaction of a transition metal as the catalyst, realizes heterogeneous catalysis, also can be reused more than five times, and the catalyst can be easily recovered, thus improving the utilization rate of the catalyst and reducing the cost. At the same time, the composite catalyst provided by the invention has the advantages of mild reaction temperature, shorter reaction time, small catalyst dosage, and no other additive, and is beneficial to industrial popularization and application.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, in particular to UiO-66-NH loaded with transition metal copper 2 Composite catalyst and its preparation method and application. Background technique [0002] In recent years, coordination-driven organic-inorganic hybrid materials have attracted extensive and in-depth research, and have gradually become a class of promising materials in the fields of adsorption, catalysis, sensing, and biology. With the in-depth research on one type of organic-inorganic hybrid materials - multi-metal organic frameworks (MOFs), it is found that MOFs, as a porous crystal material, can confine various metal nanoparticles in its The pores of MOFs can be conveniently used for catalytic reactions after the guests containing catalytic active sites are introduced into the pores of MOFs. transmission. [0003] As a classic chemical reaction, the reduction reaction of carbon-carbon double bond has been relat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28C07C5/05C07C15/073
CPCB01J31/28B01J2231/645B01J2531/48C07C5/05C07C15/073
Inventor 董育斌王建成胡玉红陈功军
Owner SHANDONG NORMAL UNIV
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