Method for preparing carbon aerogel desulfurizing agent

A technology of carbon airgel and desulfurizer, which is applied in chemical instruments and methods, selection of absorbent solid gas purification, and other chemical processes, can solve the problem of destroying the airgel pore structure and distribution, low efficiency, and relatively Issues such as reduced surface area and pore volume

Inactive Publication Date: 2009-03-04
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Literature (R.W.Pekala, Organic aerugls from the polycondensation of resorcinol with formaldehyde, Journal of Materials Science, 24 (1989) 3221-3227) and U.S. Patent No. 4,873,218, US4997, 804 disclose a kind of use resorcinol and formaldehyde as raw material preparation The method of low-density organic aerogels limits its industrial production due to the price of resorcinol
[0004] In the process of synthesis, there are such problems: due to the existence of capillary tension, the structure of the gel network collapses during drying and carbonization, which destroys the pore structure and distribution of the airgel, and the specific surface area and pore volume are reduced due to shrinkage. reduction of
[0005] Currently, research and development of the H 2 There are many kinds of S removal methods, such as wet desulfurization and dry desulfurization, etc. Chinese patent (ZL9410271.1) discloses a columnar activated carbon to remove H 2 S method, but the efficiency is not high; Chinese patent (application number: 200610056702.7) discloses a kind of impregnated activated carbon adsorption H 2 S method
However, it has not been found that carbon aerogel is used as a desulfurization agent to remove H2S.

Method used

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  • Method for preparing carbon aerogel desulfurizing agent
  • Method for preparing carbon aerogel desulfurizing agent
  • Method for preparing carbon aerogel desulfurizing agent

Examples

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Embodiment 1

[0027] Phenol, formaldehyde, melamine, and commercial grade silica sol were mixed in a molar ratio of 1:2:0.4:4 to prepare a precursor solution, with a solid content of 40g / 100ml. Add 0.1mol / L NaOH to adjust the pH value to 9, carry out sol-gel reaction at 85°C, and continue aging for 4 days to obtain a composite hydrogel. Replace with absolute ethanol, and then dry in a mixed solution of absolute ethanol and petroleum ether at 250°C and 10MPa in a supercritical state for 4h. Then, under the protection of inert gas, it was carbonized at 800°C for 3h. Then soak it in HF acid solution to remove the inorganic template agent, adjust its pH value to neutral with deionized water, and dry under normal pressure to obtain carbon airgel. Finally, the carbon airgel was mixed with 8% Na 2 CO 3 The solution was impregnated with an equal volume, and dried at 130°C for 24 hours to obtain a carbon airgel desulfurizer. Its BET specific surface area is 650m 2 / g, the pore volume is 2.3cm ...

Embodiment 2

[0029] Phenol, formaldehyde, melamine, and commercial grade silica sol were mixed in a molar ratio of 1:2:0.8:4 to prepare a precursor solution, with a solid content of 40g / 100ml. Add 0.1mol / L NaOH to adjust the pH value to 9, carry out sol-gel reaction at 85°C, and continue aging for 4 days to obtain a composite hydrogel. Replace with absolute ethanol, and then dry in a mixed solution of absolute ethanol and petroleum ether at 250°C and 10MPa in a supercritical state for 4h. Then, under the protection of inert gas, it was carbonized at 800°C for 3h. Then soak it in HF acid solution to remove the inorganic template agent, adjust its pH value to neutral with deionized water, and dry under normal pressure to obtain carbon airgel. Finally, the carbon airgel was mixed with 8% Na 2 CO 3 The solution was impregnated with an equal volume, and dried at 130°C for 24 hours to obtain a carbon airgel desulfurizer. Its BET specific surface area is 756m 2 / g, the pore volume is 3.1cm ...

Embodiment 3

[0031]Phenol, formaldehyde, melamine, and commercial grade silica sol were mixed in a molar ratio of 1:2:1.2:4 to prepare a precursor solution, with a solid content of 40g / 100ml. Add 0.1mol / L NaOH to adjust the pH value to 9, carry out sol-gel reaction at 85°C, and continue aging for 4 days to obtain a composite hydrogel. Replace with absolute ethanol, and then dry in a mixed solution of absolute ethanol and petroleum ether at 250°C and 10MPa in a supercritical state for 4h. Then, under the protection of inert gas, it was carbonized at 800°C for 3h. Then soak it in HF acid solution to remove the inorganic template agent, adjust its pH value to neutral with deionized water, and dry under normal pressure to obtain carbon airgel. Finally, the carbon airgel was mixed with 8% Na 2 CO 3 The solution was impregnated with an equal volume, and dried at 130°C for 24 hours to obtain a carbon airgel desulfurizer. Its BET specific surface area is 844m 2 / g, the pore volume is 3.9cm 3...

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Abstract

The invention provides a preparation method for a carbon aerogel desulfurization agent. The invention utilizes phenyl hydroxide, methanal and melamine as polymer precursors and utilizes nano-scale silica sol as an inorganic template. The precursors are mixed at a certain proportion and carry on sol-gel reaction; and pure carbon aerogel is produced after the processes of drying, high-temperature carbonizing and template removing. The invention has the advantages of mild preparation condition and conventional production device, and is suitable for large scale industrial production. The desulfurization agent produced by the method of the invention has large breakthrough sulfur capacity and saturated sulfur capacity, thereby being adopted in H2S removing process in oil and gas, synthesis gas, and the tail gas in sewage treatment plants.

Description

technical field [0001] The present invention relates to a H 2 The S desulfurizer specifically relates to a preparation method of a carbon airgel desulfurizer. technical background [0002] h 2 S is a poisonous and harmful gas, which is mainly produced in various industrial production processes, such as gas manufacturing, ammonia synthesis industry, and coal gas production. Sewage treatment and petrochemical industry, etc. With the development of industry, purification and desulfurization becomes more and more important. This process directly affects the poisoning of the catalyst, resulting in a sharp drop in production efficiency, product quality and environmental degradation. For example, when coal, oil and natural gas are used as main raw materials to produce products such as ammonia, methanol, and methanation gas, sulfides (mainly H 2 S, COS, CS 2 etc.) is the main cause of catalyst poisoning and deactivation; in addition, containing H 2 SO produced by the combusti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/30C10K1/32
Inventor 张睿陈亮陈庆军龙东辉卢丰梁晓怿乔文明凌立成
Owner EAST CHINA UNIV OF SCI & TECH
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