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High-thermostability ordered mesoporous carbon material and preparation method thereof

A technology of high thermal stability and mesoporous carbon, applied in the field of preparation of porous materials, can solve the problems of metal equipment corrosion and environmental pollution, and achieve the effects of reducing corrosion, cheap and easy-to-obtain raw materials, and high yield.

Inactive Publication Date: 2013-11-06
天津神能科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Dai's group expanded the range of conditions for material synthesis (C.D.Liang and S.Dai, J.Am.Chem.Soc., 2006, 128, 5316.), but used expensive phloroglucinol as a carbon source, and during the synthesis process It usually involves the use of liquid acid. The discharge of chloride ions has caused certain pollution to the environment. At the same time, liquid acid will also cause certain corrosion to metal equipment.

Method used

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  • High-thermostability ordered mesoporous carbon material and preparation method thereof
  • High-thermostability ordered mesoporous carbon material and preparation method thereof
  • High-thermostability ordered mesoporous carbon material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0021] 1) Dissolve resorcinol and surfactant F127 in a mixed system of 20g ethanol and 20g distilled water, stir vigorously to dissolve them all, then add 2.1g citric acid;

[0022] 2) After stirring for 2 hours, add 2.5g of 37% formaldehyde solution (the molar ratio of formaldehyde to citric acid is 3), and continue to stir to make it start to polymerize slowly to obtain the oligomeric resol resin / F127 complex;

[0023] 3) After the reaction was carried out for 2 hours, a light yellow clear and transparent solution was obtained, which was transferred to a 50ml reaction kettle and aged at 60°C for two days to obtain an elastic orange-red polymer / surfactant solid composite, which was carbonized at 600°C for 3h Finally, the ordered mesoporous carbon material was obtained with a specific surface area of ​​758m 2 g -1 , the total pore volume is 0.55cc / g, the micropore volume is 0.16cc / g, and the mesopore diameter is about 5.2nm.

Embodiment 2

[0025] Same as Example 1, the amount of citric acid in step 1) is reduced to 1.0g (the molar ratio of formaldehyde to citric acid is 6), other reaction conditions remain unchanged, the final mixed solution is transferred to a 50ml reaction kettle, 60°C After aging for two days, an elastic orange-red polymer / surfactant solid composite was obtained. After washing, drying, and carbonization at 600°C for 3 hours, an ordered mesoporous carbon material was obtained, with a specific surface of 770m 2 g -1 , the total pore volume is 0.52cc / g, the micropore volume is 0.15cc / g, and the mesopore diameter is about 5.6nm.

Embodiment 3

[0027] Same as in Example 1, reduce the amount of citric acid used in step 1) to 0.5g (the molar ratio of formaldehyde to citric acid is 15), keep other reaction conditions unchanged, transfer the final mixed solution into a 50ml reactor, and age at 60°C After two days, an orange-red polymer / surfactant solid composite was obtained, which was washed, dried, and carbonized at 600°C for 3 hours to obtain an ordered mesoporous carbon material with a specific surface of 736m 2 g -1 , the total pore volume is 0.54cc / g, the micropore volume is 0.13cc / g, and the mesopore diameter is about 5.2nm.

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Abstract

The invention relates to a high-thermostability ordered mesoporous carbon material and a preparation method thereof. The invention discloses an environment-friendly method for synthesizing a high-thermostability ordered mesoporous carbon material. In the method, a citric acid material is used as a catalyst to catalyze the polymerization of phenolic resin on one hand and reinforce the interaction between a carbon precursor and a surfactant through rich carboxyl functional groups. The used raw material is cheap and readily available and avoids corrosion to equipment, and the process is easy to operate. The ordered structure is obtained under mild reaction conditions that: the molar ratio of formaldehyde to citric acid is not less than 3; and the hydrothermal temperature is between 50 and 80 DEG C. The synthesized ordered mesoporous carbon material has a high thermostability and can keep ordered mesoporous structure after being carbonized at 1,000 DEG C. The prepared mesoporous carbon material has two-dimensional hexagonal mesopores, the specific surface area of the mesoporous carbon material can reach 612 to 851m<2>g<-1>, and the mesoporous carbon material has high aperture (5.2 nanometers) and high porous capacity (0.46 to 0.62cc / g). With the citric acid used in place of conventional hydrochloric acid as the catalyst for the polymerization of phenolic resin, the operation is easy; and the introduction of chlorine ions into a reaction system is avoided, which is favorable for use in some catalytic reactions. The ordered mesoporous carbon material has a high application value in fields of absorption, catalyst carriers, hydrogen storage materials, electrode materials for electrochemical capacitors, and the like.

Description

technical field [0001] The invention belongs to the field of preparation of porous materials. Especially an environmentally friendly method to prepare ordered mesoporous carbon materials with high thermal stability. Background technique [0002] Ordered mesoporous carbon materials have attracted great interest and widespread attention in the scientific community since their birth, and they have potential value in adsorption, catalyst support, hydrogen storage materials, and electrode materials for electrochemical capacitors. The hard template method (H.F.Yang.; Q.H.Shi.; X.Y.Liu.; S.H.Xie.; D.C. Jiang.; F.Q.Zhang, C.Z.Yu, B.Tu.; D.Y.Zhao.Chem.Commun., 2002, 2842) is widely It is applied to the synthesis of ordered mesoporous carbon materials, but the process of the template casting method is complicated, time-consuming and relatively high in cost. In recent years, organic-organic self-assembly methods have been developed to directly synthesize ordered mesoporous carbon mat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/00C01B31/02
Inventor 袁忠勇刘蕾
Owner 天津神能科技有限公司
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