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Cross-linking norbornene copolymer composite carbon black three-dimensional network immobilized platinum nano catalyst as well as preparation method and application thereof

A norbornene and three-dimensional network technology is applied in the field of cross-linked norbornene copolymer composite carbon black three-dimensional network immobilized platinum nanocatalyst and its preparation, and can solve the problems of difficult separation and recovery, high use cost, loss of metal platinum and the like , to achieve strong lipophilicity, prolong service life and good effect.

Active Publication Date: 2019-10-18
HUBEI ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The product of the present invention can overcome the problems in the prior art that various platinum salt homogeneous catalysts for nitrogen methylation reactions are difficult to separate and recover after reaction, resulting in serious loss of metal platinum, resulting in high use costs and environmental pollution problems

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  • Cross-linking norbornene copolymer composite carbon black three-dimensional network immobilized platinum nano catalyst as well as preparation method and application thereof
  • Cross-linking norbornene copolymer composite carbon black three-dimensional network immobilized platinum nano catalyst as well as preparation method and application thereof
  • Cross-linking norbornene copolymer composite carbon black three-dimensional network immobilized platinum nano catalyst as well as preparation method and application thereof

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specific Embodiment approach

[0053] The active component of the PNBI / CB-Pt catalyst provided by the embodiments of the present invention is platinum, the carrier is a cross-linked copolymerized norbornene / carbon black three-dimensional network, and the platinum is a nanostructure; at the same time, the active component platinum is in the PNBI / CB-Pt catalyst The relative content is 0.0849mmol / g~0.0872mmol / g, such as 0.0849mmol / g, 0.0851mmol / g, 0.0862mmol / g, 0.0865mmol / g, 0.0872mmol / g, etc.

[0054] Among them, the carrier is a cross-linked copolymerized norbornene / carbon black three-dimensional network, and the cross-linked norbornene copolymer / carbon black three-dimensional network is composed of three differently substituted norbornene monomers, after polymerization, activated carbon powder is added, and then cross-linked form.

[0055] The embodiment of the present invention also provides a preparation method of PNBI / CB-Pt catalyst, including three major steps:

[0056] 1) Preparation of norbornene cop...

Embodiment 1

[0064] 1) Preparation of norbornene copolymer: according to the ratio of three monomers 1:1:1, take the first norbornene monomer 345.44mg, the second norbornene monomer 311.38mg, the third norbornene monomer Body 431.53mg, and initiator Grubbs-I820mg were added to 50mL of anhydrous dichloromethane, and stirred at room temperature for 2h under an argon atmosphere. Add 10 ml of vinyl ether, quench for 10 min, concentrate the mixed system by rotary evaporation, slowly pour it into ether, filter, wash the precipitate with ether, and dry to obtain a norbornene copolymer. According to the integral ratio of the characteristic peaks of the NMR spectrum, the proportion of the monomer structure can be calculated to be about 1:1:1.

[0065] 2) Preparation of norbornene copolymer / carbon black / platinum: add activated carbon black and mix, wash several times, filter, place under vacuum line to remove residual solvent, and obtain the required polynorbornene carbon black network (PNBICB) . ...

Embodiment 2

[0069] 1) Preparation of norbornene copolymer: according to the ratio of the three monomers 1:0.75:0.75, take the first norbornene monomer 345.44mg, the second norbornene monomer 311.38mg, the third norbornene monomer Compound 431.53mg, and initiator Grubbs-I 820mg were added to 50mL of anhydrous dichloromethane, and stirred at room temperature for 2h under an argon atmosphere. Add 10ml of vinyl ether, quench for 10 minutes, concentrate the mixed system by rotary evaporation, slowly pour it into ether, filter, wash the precipitated precipitate with ether, and dry to obtain a norbornene copolymer. Its nuclear magnetic spectrum is as follows: Figure 5 As shown, the monomer structure ratio can be calculated from the integral ratio of the characteristic peaks of the NMR spectrum to be about 1:0.75:0.75.

[0070] 2) Preparation of norbornene copolymer / carbon black / platinum: add activated carbon black and mix, wash several times, filter, place under vacuum line to remove residual s...

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Abstract

The invention belongs to the technical field of catalysts and in relates to a cross-linking norbornene copolymer composite carbon black three-dimensional network immobilized platinum nano catalyst aswell as a preparation method and application thereof. The catalyst has an active component of platinum, and a carrier of a composition of a cross-linking norbornene copolymer and carbon black, and platinum is of a nano structure. The catalyst is high in catalysis activity, and is high in product yield when being used for catalyzing a nitrogen methylation reaction; in addition, the metal platinum exists in a nanoparticle state in the PNBI / CB / Pt catalyst, so that the metal platinum can be uniformly dispersed, and the catalysis performance can be further improved; furthermore, the carrier for immobilizing platinum is a cross-linking copolymer / carbon black three-dimensional network, the copolymer forming the cross-linking copolymer / carbon black three-dimensional network has good lipophilicity,so that the catalyst is applicable to reactions in organic solvents; and finally the catalysis material is insoluble in common solvents and has a good effect in immobilizing nano-grade platinum metals, so that the service life of the PNBI / CB / Pt catalyst can be prolonged.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a cross-linked norbornene copolymer composite carbon black three-dimensional network-immobilized platinum nano-catalyst and a preparation method and application thereof. Background technique [0002] Methylamine, dimethylamine, formamide, etc. formed by nitrogen methylation reaction can not only be used as reaction reagents in the laboratory, but also can be used as raw materials in the synthesis of fertilizers, fungicides, artificial leather, and polymers in chemical production . Therefore, the nitrogen methylation reaction of imine compounds plays an important role in laboratory synthesis and chemical industry. The selection of catalysts for the nitrogen methylation reaction is the most challenging field, and most of the catalysts used in this reaction are homogeneous organic catalysts and metal catalysts, and the application of heterogeneous catalysts is rare. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C209/60C07C211/48
CPCB01J31/06C07C209/60B01J2231/346C07C211/48
Inventor 李博解蔡爽朱磊魏鹏任李伟汪连生
Owner HUBEI ENG UNIV