Solid-phase synthetic method of highly ordered mesoporous carbon material

A highly ordered, solid-phase synthesis technology, applied in the field of materials, can solve problems such as low efficiency, time-consuming, labor-intensive, and complicated

Inactive Publication Date: 2014-08-06
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The synthesis of mesoporous carbon materials by the hard template method is a complicated, non-environmentally friendly, time-consuming and laborious method due to the need for additional steps to synthesize and remove ordered mesoporous silicon, and is not suitable for large-scale mesoporous carbon materials. Synthesis of porous carbon materials
The organic-organic self-assembly method is generally synthesized by solvent evaporation-induced self-assembly process or solvothermal process, which are all carried out in dilute solution, and the synthesis efficiency is also low. The preparation of direct large-scale mesoporous carbon is also faced with insurmountable difficulties
So far, there is no very convenient method to directly synthesize mesoporous carbon materials, heteroatom-doped mesoporous carbons, metal carbides, and metal oxide mesoporous carbon composites.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] At room temperature, 0.62 g of triblock copolymer EO 106 PO 70 EO 106 Add to an agate mortar and grind to a fine powder. Then 0.62 g of resorcinol was added and ground for 5 minutes until powdered. Then 0.45 g of terephthalaldehyde was added in three batches, followed by careful grinding for 5 minutes and mixing as homogeneous as possible. The solid turned into a white to off-white pasty dough-like viscous solid during grinding, and the viscous solid from grinding was transferred to a corundum crucible. Put the newly prepared samples into ovens at 80°C and 100°C for heat treatment for 300 minutes respectively to obtain a hard bulk polymer composite material, remove it and grind it into powder, then place it in a tube furnace and protect it in an inert atmosphere calcination at 900°C for 360 minutes to obtain carbon mesoporous materials. This material has a pore diameter of 5.4nm and a pore volume of 0.55cm 3 / g, the specific surface area is 700m 2 / g, the pore sp...

Embodiment 2

[0025] At room temperature, add 0.81 g of cationic surfactant cetyltrimethylammonium bromide into an agate mortar and grind to fine powder; then add 0.42 g of resorcinol and grind for 5 minutes to powder. Then 0.49 g of terephthalaldehyde was added in three batches followed by careful grinding for 5 minutes and mixing as homogeneous as possible. During grinding, the solid turned into a white to off-white pasty dough-like sticky solid, which was transferred to a corundum crucible. Put the newly prepared samples into ovens at 80°C and 100°C for heat treatment for 300 minutes respectively to obtain a hard bulk polymer composite material, remove it and grind it into powder, then place it in a tube furnace and protect it in an inert atmosphere calcination at 900°C for 300 minutes to obtain carbon mesoporous materials. This material has a pore diameter of 5.4nm and a pore volume of 0.26cm 3 / g, the specific surface area is 420m 2 / g.

Embodiment 3

[0027] At room temperature, 1.5 grams of triblock copolymer Brij56 was added into an agate mortar and ground to a fine powder, then 1.50 grams of melamine was added and ground to make the mixture uniform. Then 0.54 g of resorcinol was added and ground for 5 minutes until powdered. Then 0.76 g of terephthalaldehyde was added in three batches, followed by careful grinding for 5 minutes, and the viscous solid obtained by grinding was transferred to a corundum crucible. The newly prepared samples were heat-treated in ovens at 80°C and 100°C for 300 minutes, respectively, to obtain bulk polymer composite materials. It was removed and ground into powder, then placed in a tube furnace, under the protection of an inert atmosphere, and fired at a high temperature of 600°C for 180 minutes, and finally a carbon mesoporous material was obtained. The material has a pore size of 3.3nm and a pore volume of 0.17cm 3 / g, the specific surface area is 310m 2 / g, the nitrogen content is 14.0wt...

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Abstract

The invention discloses a solid-phase synthetic method of a highly ordered mesoporous carbon material. The solid-phase synthetic method comprises the following steps: 1) mixing a structure-directing agent with a high molecular monomer used as a carbon source, and grinding for 5-180 min at 10-100 DEG C; 2), heating for 0.5-120 h at 40-380 DEG C; 3) under the protection of inert gases, rising the temperature to 500-2,100 DEG C at the temperature rising speed of 1-40 DEG C/min, and roasting for 2-10 h at high temperature. The functionalization mesoporous carbon material is synthetized through the organic-organic self-assembly between the high molecular monomer and the structure-directing agent and between the low polymer of the high molecular monomer and the structure-directing agent, and the mechanical grinding. The solid-phase synthetic method is simple to operate, efficient, and low in cost, and the prepared mesoporous carbon material has a highly ordered mesoporous channel, high specific surface area (500-2,500 m<2>/g and large pore volume (pore diameter of 2.5-20 nm and pore volume of 0.1-2.5 cm <3>/g).

Description

technical field [0001] The invention relates to the field of materials, in particular to a preparation method of mesoporous carbon materials. Background technique [0002] Highly ordered mesoporous materials have important application prospects in the fields of catalysis, adsorption, separation, mass transport, and chemical sensing. In recent years, the synthesis and application of mesoporous carbon materials have been developed rapidly. The reported methods for synthesizing ordered mesoporous carbon materials mainly include hard template method and soft template method. The hard template method, also known as the nano-casting method, is characterized by the use of ordered mesoporous silicon material templates. Carbon precursors are introduced into the silicon mesoporous channels, catalyzed or thermally polymerized, and finally the mesoporous silicon template is removed to obtain "reverse phase" Replicated mesoporous carbon materials. Through this method, a series of meso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B32/05
Inventor 孙予罕王桥炜孟岩牟一杰
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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