Method for preparing spherical bimetallic MCo-MOFs catalytic material through microwave-ultrasonic wave synergistic assistance

A catalytic material and bimetallic technology, which is applied in chemical instruments and methods, catalytic reactions, catalyst activation/preparation, etc., can solve the problem of spherical bimetallic MCo-MOFs catalytic materials, which are difficult to obtain regular, orderly and three-dimensional Material, catalytic diolefin epoxidation performance is not ideal, etc., to achieve the effect of fast heating speed, fast reaction and good fluidity

Active Publication Date: 2021-03-09
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the ZnCo-MOF material prepared by this patent is to add metal cobalt salt, aromatic carboxylic acid, acetic acid, metal zinc salt and water into the container, mix and stir, then evaporate to dryness to obtain dry glue, and then grind it into dry glue powder. The rubber powder is subjected to a crystallization reaction, and finally the product is purified and dried to obtain a bimetallic functionalized ZnCo-MOF catalytic material; in the process of crystallizing the dry rubber powder, the system is a solid-phase synthesis and has poor fluidity. What is obtained is a layered stacked material, it is difficult to obtain a regular, orderly, three-dimensional material, and the catalytic performance of diolefin epoxidation is not ideal, so it can be seen that there are still great difficulties in preparing regular spherical bimetallic materials according to the prior art
[0006] At present, there is no report on the preparation method of spherical bimetallic MCo-MOFs catalytic materials assisted by microwave and ultrasonic synergy

Method used

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  • Method for preparing spherical bimetallic MCo-MOFs catalytic material through microwave-ultrasonic wave synergistic assistance
  • Method for preparing spherical bimetallic MCo-MOFs catalytic material through microwave-ultrasonic wave synergistic assistance
  • Method for preparing spherical bimetallic MCo-MOFs catalytic material through microwave-ultrasonic wave synergistic assistance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1) First weigh 12mmol of cobalt acetate, 1.2mmol of zinc nitrate and 12mmol of terephthalic acid into a round-bottomed flask of 6.84mol of water, mix well and place in a microwave-ultrasonic integrated reactor. Set the microwave power to 100W and the ultrasonic power to 100W. 500W, reaction temperature 80℃, microwave and ultrasonic synergistic reaction for 2h, bimetallic Zn 0.1 Co-MOFs precursor solution;

[0038] 2) Transfer the precursor reaction solution obtained in step 1) into a polytetrafluoroethylene lining, then place the lining in a stainless steel reactor, then seal the reactor, and place the reactor in a rotary crystallization reactor, Set the rotational speed to 150r / min, the crystallization temperature to 200°C, and the crystallization time to 3h, and perform rotational hydrothermal crystallization treatment to obtain bimetallic Zn 0.1 Crude Co-MOFs;

[0039] 3) The product obtained in step 2) is sequentially washed with DMF and ethanol (85° C.), suction ...

Embodiment 2

[0041] 1) First weigh 9mmol of cobalt nitrate, 1.8mmol of bismuth nitrate and 9mmol of terephthalic acid into a round-bottomed flask with 4.5mol of water, mix well and place in a microwave-ultrasonic integrated reactor, set the microwave power to 300W, ultrasonic The power is 400W, the reaction temperature is 80°C, and the microwave and ultrasonic waves are synergistically reacted for 1h to obtain bimetallic Bi 0.2 Co-MOFs precursor solution;

[0042] 2) Transfer the precursor reaction solution obtained in step 1) into a polytetrafluoroethylene lining, then place the lining in a stainless steel reactor, then seal the reactor, and place the reactor in a rotary crystallization reactor, Set the rotational speed to 150r / min, the crystallization temperature to 200°C, and the crystallization time to 4h, and perform rotational hydrothermal crystallization treatment to obtain bimetallic Bi 0.2 Crude Co-MOFs;

[0043] 3) The product obtained in step 2) was sequentially washed with DM...

Embodiment 3

[0045] 1) First weigh 12mmol of cobalt acetate, 3.6mmol of tin chloride and 12mmol of terephthalic acid into a round-bottomed flask with 4.44mol of water, mix well and place in a microwave-ultrasonic integrated reactor, set the microwave power to 200W, ultrasonic The power is 600W, the reaction temperature is 70℃, and the microwave and ultrasonic synergistic reaction is 3h, and the bimetallic Sn 0.3 Co-MOFs precursor solution;

[0046] 2) Transfer the precursor reaction solution obtained in step 1) into a polytetrafluoroethylene lining, then place the lining in a stainless steel reactor, then seal the reactor, and place the reactor in a rotary crystallization reactor, Set the rotational speed to 150r / min, the crystallization temperature to 200°C, and the crystallization time to 1h, and perform rotational hydrothermal crystallization treatment to obtain bimetallic Sn 0.3 Crude Co-MOFs;

[0047] 3) The product obtained in step 2) was sequentially washed with DMF and ethanol (8...

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Abstract

The invention discloses a method for preparing a spherical bimetallic MCo-MOFs catalytic material through microwave-ultrasonic synergistic assistance, which comprises the following steps: firstly, preparing a spherical bimetallic MCo-MOFs precursor through synergistic assistance of a metal salt I (metal cobalt salt), a metal salt II and aromatic dicarboxylic acid in a microwave-ultrasonic combinedmode; and further the precursor solution is crystallized through a hydrothermal rotation method to prepare the spherical bimetallic MCo-MOFs catalytic material. The method is simple in process, low in cost, convenient to operate and high in yield, and the prepared product is uniform in particle size, controllable in form and high in catalytic activity.

Description

technical field [0001] The invention relates to a method for preparing a spherical bimetallic MCo-MOFs catalytic material assisted by microwave and ultrasonic waves, and belongs to the technical field of catalytic material preparation. Background technique [0002] Microwave is electromagnetic radiation with a frequency in the range of 30-0.3GHz. The frequency of microwaves is close to the rotational vibration frequency of chemical functional groups, which can activate groups, initiate free radical polymerization, and promote chemical reactions. Ultrasound is a sound wave with a frequency range higher than 20KHz, which has the characteristics of good directionality and strong penetrating power. When ultrasonic wave acts on the reaction liquid as a mechanical wave, it breaks the air bubbles generated during the ultrasonic process so that the reactants undergo physical or chemical changes in the liquid medium, and its periodic fluctuations will cause compression and thinning ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J35/08B01J37/10B01J37/34C07D301/06C07D303/04
CPCB01J37/343B01J37/346B01J37/10B01J35/08B01J31/1691B01J31/2239C07D301/06C07D303/04B01J2231/72B01J2531/26B01J2531/845B01J2531/54B01J2531/42B01J2531/48Y02P20/52
Inventor 鲁新环杨璐张海福周丹夏清华
Owner HUBEI UNIV
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