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Pd-heterocyclic aromatic hydrocarbons Schiff base electrochemically polymerized-self-assembled-doped thin film and preparation method thereof

A technology of heterocyclic aromatic hydrocarbons and Schiff bases, applied in the field of heterogeneous catalysts, can solve the problems of poor circulation and stability of catalytic membranes, low catalytic yield of catalytic membranes, etc., and achieve enhanced catalytic activity and recycling ability, orderly arrangement, The effect of structural stability

Inactive Publication Date: 2016-07-13
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved in the present invention is that the catalytic film prepared in the prior art may have low catalytic yield, or the cycle and stability of the catalytic film are relatively poor. In order to solve the above problems, the present invention provides a Pd-heterocyclic aromatic hydrocarbon Schiff base electrochemical polymerization-self-assembly-doped thin film and its preparation method

Method used

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  • Pd-heterocyclic aromatic hydrocarbons Schiff base electrochemically polymerized-self-assembled-doped thin film and preparation method thereof
  • Pd-heterocyclic aromatic hydrocarbons Schiff base electrochemically polymerized-self-assembled-doped thin film and preparation method thereof
  • Pd-heterocyclic aromatic hydrocarbons Schiff base electrochemically polymerized-self-assembled-doped thin film and preparation method thereof

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Embodiment 1

[0061] The Pd-heterocyclic aromatic hydrocarbon Schiff base electrochemical polymerization-self-assembly-doped film provided by the present invention is a compound of the following formula; wherein 0<n≤10, n is an integer;

[0062]

[0063] Among them, R 1 = S, N, O; R 2 = S, R 3 = CHO, COCH 3 , H, CH 2 Br, CH 3 , CH 2 CH 3 , (CH 2 ) 5 CH 3 , (CH 2 ) 7 CH 3 , OCH 3 , Br; R 2 = N, R 3 = CHO, C 3 h 6 , NH 2 , H, CH 3 , Br; R 2 =O, R 3 = CHO, H, CH 2 Br, CH 3 , OCH 3 , Br; heterocyclic aromatic hydrocarbons for electrochemical doping can also be

[0064] The preparation method of Pd-heterocyclic aromatic hydrocarbon Schiff base electrochemical polymerization-self-assembly-doped film comprises the following specific steps:

[0065] a. Hydrophilic treatment of the substrate: ITO conductive glass is ultrasonically treated in acetone, ethanol and deionized water for 15-30 minutes, and then heated in an alkaline cleaning solution at 40-60°C for 0.5-2 hour...

Embodiment 2

[0084] The preparation method of the Pd-heterocyclic aromatic hydrocarbon Schiff base electrochemical polymerization-self-assembly-doped film in this example is as follows:

[0085] a. Hydrophilic treatment of the substrate: ITO conductive glass was ultrasonically treated in acetone, ethanol and deionized water for 15 minutes, and then heated in an alkaline cleaning solution at 40°C for 0.5 hours to generate silanol groups on the surface of the substrate. Rinse with secondary deionized water while hot, and dry;

[0086] b. Silanization of the hydrophilic substrate: the hydrophilic treated substrate (1×2.5cm 2 ), 3-aminopropyltriethoxysilane (1.0mmol) and anhydrous toluene (10mL) were respectively added into a round bottom flask, heated to 65°C in an oil bath, reacted at constant temperature for 18 hours, and cooled to room temperature after the reaction was completed. Take out the silanized substrate, wash it twice with toluene, acetone, ethanol and water in turn, if it is no...

Embodiment 3

[0097] The preparation method of the Pd-heterocyclic aromatic hydrocarbon Schiff base electrochemical polymerization-self-assembly-doped film in this example is as follows:

[0098] a. Hydrophilic treatment of the substrate: ITO conductive glass was ultrasonically treated in acetone, ethanol and deionized water for 16 minutes, and then heated in an alkaline cleaning solution at 41°C for 0.6 hours to generate silanol groups on the surface of the substrate. Rinse with secondary deionized water while hot, and dry;

[0099] b. Silanization of the hydrophilic substrate: the hydrophilic treated substrate (1×2.5cm 2 ), 3-aminopropyltriethoxysilane (1.1mmol) and absolute ethanol (11mL) were respectively added into a round bottom flask, heated to 66°C in an oil bath, and reacted at a constant temperature for 19 hours, and cooled to room temperature after the reaction was completed. Take out the silanized substrate, rinse it with ethyl acetate, petroleum ether, ethanol and water three ...

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Abstract

The invention provides a Pd-heterocyclic aromatic hydrocarbons Schiff base electrochemically polymerized-self-assembled-doped thin film, which is a compound shown in the formula, wherein n is more than 0 and less than or equal to 10 and n is an integer. Compared with the prior art, the Pd-heterocyclic aromatic hydrocarbons Schiff base electrochemically polymerized-self-assembled-doped thin film is prepared by utilizing an electrochemical polymerization, self-assembling and doping combined method; and a catalytic thin film, which is relatively orderly arrayed and has a relatively stable structure, is prepared by regulating and controlling a microscopic shape and the structure of the catalytic thin film, and arrangement of catalyst molecules, so that the catalytic activity and the recycling capability of heterogeneous catalysts are enhanced.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalysts, in particular to a Pd-heterocyclic aromatic hydrocarbon Schiff base electrochemical polymerization-self-assembly-doped thin film and a preparation method thereof. Background technique [0002] The ordered arrangement of the self-assembled catalytic film has a significant impact on the activity and selectivity of the catalyst, and its active sites are connected to the surface of the carrier through covalent bonds, so the catalyst has high stability and recycling ability. However, the design and assembly of molecules is a complex molecular assembly process. Small changes in the structure during the assembly process and changes in the conditions during the preparation process may affect the catalytic activity, stereoselectivity and service life of the catalyst. The selection of heterogeneous catalysts and the catalytic mechanism still need to be further explored, so the design and pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C15/14C07C1/32
CPCB01J31/22B01J2231/4211B01J2531/824C07C1/32C07C2531/22C07C15/14
Inventor 李铁生刘辉薛小侠吴养洁许文俭
Owner ZHENGZHOU UNIV