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Preparation method of nitrogen-rich ionic liquid polymer and application of nitrogen-rich ionic liquid polymer in catalytic hydrogenation reaction

A technology of ionic liquids and polymers, applied in the field of palladium catalysts, can solve problems such as unsatisfactory designability

Active Publication Date: 2021-10-08
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The excellent performance of nitrogen-doped catalysts in many fields such as oxidation, hydrogenation, and photocatalysis has attracted more and more attention to N-rich carbon materials. However, the common N-doping method is still through high-temperature calcination by N source and C source. Obtained, its degree of dispersion and designability are not ideal

Method used

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  • Preparation method of nitrogen-rich ionic liquid polymer and application of nitrogen-rich ionic liquid polymer in catalytic hydrogenation reaction
  • Preparation method of nitrogen-rich ionic liquid polymer and application of nitrogen-rich ionic liquid polymer in catalytic hydrogenation reaction
  • Preparation method of nitrogen-rich ionic liquid polymer and application of nitrogen-rich ionic liquid polymer in catalytic hydrogenation reaction

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Experimental program
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Effect test

Embodiment 1

[0031] Preparation of nitrogen-enriched ionic liquid polymer:

[0032] (1) By reacting imidazole and cyanuric chloride, the precursor trimidazole-triazine TIMT of synthesizing triimidazole triazine structure: imidazole (6g, 80mmol) and cyanuric chloride (3g, 16mmol) are dissolved in 40ml THF, in Mix in a three-necked flask, stir for 24 hours at 80°C under a nitrogen atmosphere, filter and wash with water, and dry to obtain 3.3 g of white precipitate, with a yield of 78.6%;

[0033] (2) Synthesis of ionic liquid with 4-vinylbenzyl chloride and trimidazole-triazine (TIMT): step (1) product TIMT (0.6g, 2.15mmol) and vinylbenzyl chloride (1.2g, 7.9mmol), DMSO 15ml As a solvent, stir for 48 hours under a nitrogen atmosphere at 80°C to obtain a dark brown liquid. After the reaction, wash with ethyl acetate three times to remove unreacted vinylbenzyl chloride and solvent DMSO, and dry the solid by centrifugation to obtain light yellow powder Cl-IL 1.4g, yield 88.6%;

[0034] (3) Cl...

Embodiment 2

[0037] Metal load: the PIL-Tf that the vacuum drying that embodiment obtains obtains 2 N 1g and enough chloropalladic acid were stirred in water at room temperature for 24 hours. Filtered, dried in vacuo, and the solid was reduced with excess sodium borohydride solution to give 2wt% Pd-PIL-TF 2 N.

[0038] Same as above, using PIL-Cl-IL, PIL-PF 6 -IL carries out metal loading, and ICP-MS test shows that the actual loading is 1.05wt% Pd-PIL-Tf 2 N, 1.05wt% Pd-PIL-Cl, 1.55wt% Pd-PIL-PF 6 catalyst.

Embodiment 3

[0040] In order to confirm the successful polymerization of polyionic liquids and determine the structure of the polymerized catalyst, the synthesized polyionic liquids were characterized by FT-IR. Three kinds of polyionic liquids after anion exchange (PIL-Tf 2 N, PIL-Cl, PIL-PF 6 ) infrared spectrum such as figure 2 shown.

[0041] Such as figure 2 As shown, the three catalysts are all at 2960-2840cm -1 There are obvious absorption peaks between the three catalysts and the monomers contain -CH 2 -structure. Compared with other catalysts, the monomer IL-Cl catalyst is at 3150cm -1 There is a relatively obvious absorption peak, here is the vinyl C-H stretching vibration peak, 840cm -1 There is an obvious peak at , which is the out-of-plane rocking vibration absorption peak of vinyl. None of the two peaks existed in the three polymerized catalysts, which proved that the free radical polymerization with AIBN as the initiator was successful. All three catalysts are at 1...

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Abstract

The invention belongs to the technical field of palladium catalysts, and discloses a preparation method of a nitrogen-rich ionic liquid polymer and an application of the nitrogen-rich ionic liquid polymer in a catalytic hydrogenation reaction. The trigeminal nitrogen-rich ionic liquid is synthesized on the basis of triimidazole tricyano, free radicals are adopted to initiate polymerization, the synthesized polyionic liquid is used as a carrier to load palladium nanoparticles as hydrogenation active sites, and SEM and TEM prove that the loaded Pd has good distribution. The different anions of the polyion liquid are researched, it is found that Tf2N<-> has the best promoting effect in the nitrobenzene hydrogenation reaction, good catalytic activity and selectivity can be obtained under the mild condition, and the catalytic activity is far higher than that of a PF6<-> and Cl<-> polyion liquid carrier.

Description

technical field [0001] The invention relates to the technical field of palladium catalysts, in particular to a preparation method of a nitrogen-rich ionic liquid polymer and its application in catalytic hydrogenation reactions. Background technique [0002] Palladium catalyst supported on carbon (Pd / C) is widely used in catalytic reactions such as industrial hydrogenation, oxidation and fuel cells. However, due to the limited resources and high price of palladium metal, people expect to design catalysts with low Pd loading and good catalytic effect, and a lot of research has been carried out to reduce the amount of Pd used. [0003] From the perspective of changing the physical structure of catalysts through synthesis design, it is a direction that people are working hard to design catalysts to make the active center contact with the substrate as much as possible. Changing the size of metal nanoparticles and synthesizing ultrafine nanoparticles not only make the active sites...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J31/06B01J35/00C07C209/36C07C211/46
CPCB01J31/0284B01J31/0298B01J31/06C07C209/36B01J2231/641B01J35/393C07C211/46
Inventor 宋红兵张子辰盖恒军肖盟黄婷婷
Owner QINGDAO UNIV OF SCI & TECH
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