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Cyclodextrin-based aza-ordered mesoporous carbon preparation method and application

A cyclodextrin and ordered mesoporous technology, which is applied in the field of preparation of aza-ordered mesoporous carbon, achieves the effect of easy-to-obtain raw materials, large specific surface area, and regular and orderly morphology

Inactive Publication Date: 2016-10-12
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, it is still very challenging to construct nitrogen-doped ordered mesoporous carbon materials that can directly catalyze organic reactions.

Method used

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  • Cyclodextrin-based aza-ordered mesoporous carbon preparation method and application
  • Cyclodextrin-based aza-ordered mesoporous carbon preparation method and application
  • Cyclodextrin-based aza-ordered mesoporous carbon preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of cyclodextrin-based aza-ordered mesoporous carbon, the steps are as follows:

[0028] 1) Add 1.14g of β-cyclodextrin and 0.57g of melamine to 5mL of 2.7wt% sulfuric acid solution respectively, and stir at room temperature to obtain a mixed solution;

[0029] 2) Add 1g of SBA-11 to the above mixture, stir evenly, raise the temperature to 110°C, keep for 5h, then raise the temperature to 180°C, keep for 5h to obtain a black solid a;

[0030] 3) Add 0.73g of β-cyclodextrin and 0.37g of guanidine sulfamate into 5mL of 1.8wt% sulfuric acid solution, stir well, add the above black solid a, raise the temperature to 110°C, keep it for 5h, then raise the temperature to 180°C , kept for 5h to obtain black solid b;

[0031] 4) Put the above black solid b in a nitrogen-protected tube furnace and raise it to 600°C at 1°C / min, keep it for 3h, then rise it to 900°C at 5°C / min, keep it for 2h, cool to room temperature, and then grind it into powder, add 10mL of...

Embodiment 2

[0040] A preparation method of cyclodextrin-based aza-ordered mesoporous carbon, the steps are as follows:

[0041] 1) Add 1.14g of β-cyclodextrin and 0.11g of guanidine sulfamate to 5mL of 2.7wt% sulfuric acid solution respectively, and stir at room temperature to obtain a mixed solution;

[0042] 2) Add 1g of SBA-15 to the above mixture, stir evenly, raise the temperature to 100°C, keep it for 10h, then raise the temperature to 160°C, keep it for 10h to get a black solid a;

[0043] 3) Add 0.73g of β-cyclodextrin and 0.07g of guanidine sulfamate into 5mL of 1.8wt% sulfuric acid solution, stir well, add the above black solid a, raise the temperature to 100°C, keep it for 10h, then raise the temperature to 160°C , kept for 10h to obtain black solid b;

[0044] 4) Put the above black solid b in a nitrogen-protected tube furnace and raise it to 600°C at 1°C / min, keep it for 3h, then rise it to 900°C at 5°C / min, keep it for 2h, cool to room temperature, and then grind it into P...

Embodiment 3

[0050] A preparation method of cyclodextrin-based aza-ordered mesoporous carbon, the steps are as follows:

[0051] 1) Add 1.14g of β-cyclodextrin and 0.11g of dicyandiamide into 5mL of 2.7wt% sulfuric acid solution respectively, and stir at room temperature to obtain a mixed solution;

[0052] 2) Add 1g of MCM-48 to the above mixture, stir evenly, raise the temperature to 80°C, keep it for 10h, then raise the temperature to 140°C, keep it for 10h to get a black solid a;

[0053] 3) Add 0.73g of β-cyclodextrin and 0.07g of dicyandiamide into 5mL of 1.8wt% sulfuric acid solution respectively, stir evenly, add the above black solid a, raise the temperature to 80°C, keep it for 10h, then raise the temperature to 140°C, Keep for 10h to obtain black solid b;

[0054] 4) Put the above black solid b in a nitrogen-protected tube furnace and raise it to 600°C at 1°C / min, keep it for 3h, then rise it to 900°C at 5°C / min, keep it for 2h, cool to room temperature, and then grind it into ...

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Abstract

A cyclodextrin-based aza-ordered mesoporous carbon preparation method comprises the following steps that 1, beta-cyclodextrin and a nitrogen source are added into a sulfuric acid solution, and stirred under room temperature; 2, a template agent is added and stirred to be uniform, and two-time heating and heat preservation are performed to obtain a black solid a; 3, beta-cyclodextrin and a nitrogen source are added into a sulfuric acid solution and stirred to be uniform, then, the black solid a is added, the heating and heat preservation process is repeatedly executed, and a black solid b is obtained; 4, the black solid b is roasted in the nitrogen atmosphere, then, a HF acid or NaOH water solution is used for removing the template agent, filtering is performed, a filter cake is dried, and nitrogen-doped ordered mesoporous carbon is obtained. The method has the advantages that the raw materials are cheap and easy to obtain, the specific area of the obtained nitrogen-doped ordered mesoporous material is large, the morphology is in order, the aperture is large, the nitrogen-doped ordered mesoporous carbon can be used as a non-metal catalyst for selective oxidation of ethylbenzene and benzyl alcohol, the ethylbenzene conversion rate can reach 98.7%, and the benzyl alcohol can also reach 88.9%.

Description

technical field [0001] The invention relates to the preparation of aza-ordered mesoporous materials, in particular to a preparation method and application of cyclodextrin-based aza-ordered mesoporous carbon. technical background [0002] Ordered mesoporous carbon has always been the focus of research and development because of its large specific surface area, controllable pore size, good electrical conductivity, hydrothermal stability, and acid and alkali resistance. Its applications in energy storage, adsorption separation, catalysis and electrochemistry are endless, see: Zhang P.-F.; Yuan J.-Y.; FellingerT.-P.; Antonietti M.; LiH.-R .; Wang Y.; Angew. Chem. Int. Ed., 2013, 52, 6028-6032. Qu Y.-H.; Zhang Z.-A.; Zhang X.-H.; Ren G.-D. ; Lai Y.-Q.; Liu Y.-X.; Li J.; Carbon, 2015, 84, 399-408. Alsbaiee A.; Smith B.-J.; Xiao L.-L.; Ling Y.-H .; Helbling D.-E.; Dichtel W.-R.; Nature, 2016, 529, 190-194. Xia K.-S.; Gao Q.-M.; Wu C.-D.; Song S.-Q. ; Ruan M.-L.; Carbon, 2007, 45...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10C07C51/285C07C63/06C07C45/29C07C49/78
CPCC07C45/29C07C51/285B01J27/24B01J35/618B01J35/617B01J35/647C07C63/06C07C49/78
Inventor 刘育田军陈湧王丽华
Owner NANKAI UNIV
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