A kind of fe-zn bimetallic crystalline catalyst and its preparation method and application

A catalyst and bimetallic technology, applied in the field of porous coordination polymers, can solve the problems of uncontrollable MOFs assembly process, unpredictable synthesis process, poor catalyst stability, etc., and achieve a wide range of substrates, good selectivity and yield. rate, mild conditions

Active Publication Date: 2022-02-11
SHANGHAI INST OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a solution to the uncontrollable assembly process of most MOFs in the prior art, the structure is variable and the synthesis process is relatively unpredictable, and the catalyst prepared by the traditional method has poor stability, cumbersome preparation steps and low activity. The Fe-Zn bimetallic crystal state catalyst of technical problem such as and its preparation method and application

Method used

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  • A kind of fe-zn bimetallic crystalline catalyst and its preparation method and application
  • A kind of fe-zn bimetallic crystalline catalyst and its preparation method and application
  • A kind of fe-zn bimetallic crystalline catalyst and its preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: Preparation of bimetallic MOF1 crystalline catalyst

[0031] (1) According to Fe(NO 3 ) 3 9H 2 O and Zn(CCl 3 COO) 2 2H 2 O molar ratio is 1:2 weighing, add 40mL methanol, ultrasonic to make it mix evenly, the reaction solution is transferred to the oil bath and heated to reflux for 7h and then cooled to room temperature, filtered and washed with methanol to obtain the corresponding complex precursor, Molecular formula is Fe III 2 Zn II O(CCl 3 COO) 6 (CH 3 Oh) 3 ;

[0032] (2) According to H 2 BDC and Fe in (1) III 2 Zn II O(CCl 3 COO) 6 (CH 3 Oh) 3 The molar ratio of the complex precursor is 10:1. Weigh the H 2 BDC;

[0033] (3) H 2 BDC and the complex precursor were mixed in DMF (10ml) and n-propanol (0.5mL) under ultrasound or stirring to form a precursor solution, and stirred at room temperature for 30min;

[0034] (4) Transfer the precursor solution obtained in (3) into a hydrothermal kettle with a volume ratio of 1 / 3, and perfo...

Embodiment 2

[0037] Embodiment 2: Preparation of bimetallic MOF1 crystalline catalyst

[0038] (1) According to Fe(NO 3 ) 3 9H 2 O and Zn(CCl 3 COO) 2 2H 2 O molar ratio is 1:2 weighing, add 40mL methanol, ultrasonic to make it mix evenly, the reaction solution is transferred to the oil bath and heated to reflux for 7h and then cooled to room temperature, filtered and washed with methanol to obtain the corresponding complex precursor, Molecular formula is Fe III 2 Zn II O(CCl 3 COO) 6 (CH 3 Oh) 3 ;

[0039] (2) According to H 2 BDC and Fe in (1) III 2 Zn II O(CCl 3 COO) 6 (CH 3 Oh) 3 The molar ratio of the complex precursor is 5:1. Weigh the H 2 BDC;

[0040] (3) H 2 BDC and the complex precursor were mixed in DMF (10ml) and n-propanol (0.5mL) under ultrasound or stirring to form a precursor solution, and stirred at room temperature for 30min;

[0041] (4) Transfer the precursor solution obtained in (3) into a hydrothermal kettle with a volume ratio of 1 / 3, and perf...

Embodiment 3

[0042] Embodiment 3: Preparation of bimetallic MOF1 crystalline catalyst

[0043] (1) According to Fe(NO 3 ) 3 9H 2 O and Zn(CCl 3 COO) 2 2H 2 O molar ratio is 1:2 weighing, add 40mL methanol, ultrasonic to make it mix evenly, the reaction solution is transferred to the oil bath and heated to reflux for 7h and then cooled to room temperature, filtered and washed with methanol to obtain the corresponding complex precursor, Molecular formula is Fe III 2 Zn II O(CCl 3 COO) 6 (CH 3 Oh) 3 ;

[0044] (2) According to H 2 BDC and Fe in (1) III 2 Zn II O(CCl 3 COO) 6 (CH 3 Oh) 3 The molar ratio of the complex precursor is 10:1. Weigh the H 2 BDC;

[0045] (3) H 2 BDC and the complex precursor were mixed in DMF (10ml) and n-propanol (1mL) under ultrasound or stirring to form a precursor solution, and stirred at room temperature for 30min;

[0046] (4) Transfer the precursor solution obtained in (3) into a hydrothermal kettle with a volume ratio of 1 / 3, and perfo...

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Abstract

The present invention relates to a kind of Fe-Zn bimetallic crystal state catalyst and its preparation method and application, and this catalyst is made of Fe(NO 3 ) 3 9H 2 O and Zn(CCl 3 COO) 2 2H 2 O constitutes the precursor of the complex, and H 2 BDC is an organic bridging ligand, which is formed by assembly; its preparation method is to mix the mixed precursor and the organic bridging ligand to form a precursor solution, and perform a solvothermal reaction on the precursor solution, and the obtained solid substance is the target product ; The catalyst can be applied to catalyze C=N coupling reaction. Compared with the prior art, the crystalline material of the present invention has larger two-dimensional channels and coordination unsaturated sites, and has higher catalytic activity for the oxidative coupling reaction of imine compounds prepared by "one-pot method". , the highest catalytic efficiency reaches 98%.

Description

technical field [0001] The invention belongs to the technical field of porous coordination polymers, and relates to a Fe-Zn bimetallic crystal catalyst and its preparation method and application, in particular to a Fe III -Zn II Heteronuclear bimetallic crystalline catalyst and its preparation method and application. Background technique [0002] The transition metal-catalyzed "one-pot" C=N coupling reaction for the preparation of imines is a very classic and important method for the construction of aryl carbon-heterobonds, and is one of the most important processes in chemical changes. These reactions can be used to transform simple reaction precursors into structurally complex molecules, and transition metal-catalyzed coupling reactions are one of the most powerful means. The C=N coupling reaction catalyzed by the transition metal has mild conditions, wide application range, easy separation of products, good compatibility with substrates, and high yield. Although the co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J35/10C07C249/02C07C251/24
CPCB01J31/1691B01J31/2208B01J35/1004C07C249/02B01J2231/70B01J2531/0216B01J2531/26B01J2531/842C07C251/24
Inventor 张建勇邓维谭静怡史军霞崔鹏辉刘青
Owner SHANGHAI INST OF TECH
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