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a catalyst cuber 2 @uio-66-nh 2 -cf 3 cooh and its preparation method and application

A uio-66-nh2-cf3cooh, uio-66-nh2 technology, applied in the field of catalysts, can solve the problems of the catalyst system cannot be recycled, the trifluoroacetic acid cannot be recovered, the utilization rate is reduced, etc., and can be easily filtered or recovered by centrifugal separation. , the amount of catalyst is less, the effect of improving the utilization rate

Active Publication Date: 2022-04-15
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Even so, the inventors have found that the current copper bromide catalyst still has the following problems in the process of synthesizing sulfonic acid esters: (1) copper bromide is discharged after being catalyzed as a metal salt, causing environmental pollution; (2) trifluoroacetic acid As an auxiliary catalyst, it cannot be recycled, resulting in waste; (3) The catalyst system cannot be recycled, and the utilization rate is reduced

Method used

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  • a catalyst cuber <sub>2</sub> @uio-66-nh <sub>2</sub> -cf <sub>3</sub> cooh and its preparation method and application
  • a catalyst cuber <sub>2</sub> @uio-66-nh <sub>2</sub> -cf <sub>3</sub> cooh and its preparation method and application
  • a catalyst cuber <sub>2</sub> @uio-66-nh <sub>2</sub> -cf <sub>3</sub> cooh and its preparation method and application

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Experimental program
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Embodiment 1

[0050] UiO-66-NH 2 The preparation comprises the following steps:

[0051] (1) ZrCl 4 (139mg, 0.6mmol) and CH 3 COOH (538μL, 9.4mmol) was dissolved in 15mL DMF solution, ultrasonically dispersed for 30min, after the solution was clarified, 2-aminoterephthalic acid (108mg, 0.6mmol) was added, and ultrasonically dispersed for 10min;

[0052] (2) Transfer the solution obtained after ultrasonic dispersion in step (1) to an autoclave, heat at 120°C for 24 hours, separate the reaction solution after completion, wash the obtained solid product three times with ethanol, and then heat it at 80°C Dry for 12h to get UiO-66-NH 2 95.0 mg, yield 89.7%.

Embodiment 2

[0054] UiO-66-NH 2 -CF 3 The synthesis of COOH comprises the following steps: get the UiO-66-NH prepared in Example 1 2 20.0 mg, placed in 10 mL of CF with a concentration of 6 mol / L 3 After stirring in COOH aqueous solution for 12 hours, the reaction solution was separated after completion, and the obtained solid product was washed with ethanol three times, and then dried at 80°C for 12 hours to obtain UiO-66-NH 2 -CF 3 COOH.

Embodiment 3

[0056] Catalyst CuBr 2 @UiO-66-NH 2 -CF 3 The preparation of COOH comprises the following steps: get the UiO-66-NH prepared by 10mg embodiment 2 2 -CF 3 COOH, add 8mL ethanol solution containing copper bromide (concentration: 5mg / mL), stir into a uniform turbid solution, soak for 12 hours, and centrifuge to obtain CuBr 2 @UiO-66-NH 2 -CF 3 COOH.

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Abstract

The invention relates to the technical field of catalysts, in particular to a catalyst CuBr 2 @UiO‑66‑NH 2 ‑CF 3 COOH and its preparation method and application. The method comprises: 1) UiO-66-NH 2 placed in CF 3 Soak in the aqueous solution of COOH, separate the reaction liquid after completion, wash the obtained solid product, and obtain UiO‑66‑NH after drying 2 ‑CF 3 COOH; 2) UiO-66-NH of step 1) 2 ‑CF 3 COOH, soak in copper bromide solution, separate the reaction solution after completion, wash the obtained solid product, and obtain CuBr after drying 2 @UiO‑66‑NH 2 ‑CF 3 COOH. Catalyst CuBr of the present invention 2 @UiO‑66‑NH 2 ‑CF 3 COOH has a high utilization rate, mild reaction conditions, and is environmentally friendly, which can effectively reduce the cost of catalysis.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a catalyst CuBr for synthesizing sulfonate esters 2 @UiO-66-NH 2 -CF 3 COOH and its preparation method and application. Background technique [0002] The information disclosed in the Background of the Invention is only intended to increase the understanding of the general background of the invention, and is not necessarily to be taken as an acknowledgment or any form of suggestion that the information constitutes the prior art that is already known to those skilled in the art. [0003] Metal-organic frameworks (MOFs) are organic-inorganic hybrid materials with intramolecular pores formed by the self-assembly of organic ligands and inorganic metal ions or clusters through coordination bonds. MOFs can control the pore structure and have a large specific surface area, so they have wider application prospects than other porous materials, such as adsorption separation, catalysis,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/30B01J31/22C07C303/26C07C309/73
CPCB01J31/30C07C303/26B01J31/1691B01J31/2243B01J2231/49B01J2531/48C07C309/73
Inventor 王建成郭俊毅阚璇董育斌
Owner SHANDONG NORMAL UNIV
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