icci project number: 91-1/1.1a-2 - isgs

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FINAL TECHNICAL REPORT September 1st, 1991 to August 31st, 1992 Project Title: Principal Investigator: Co- Principal Investigator: Other Investigators: Acknowledgement: Project Monitor: Synthesis of Adsorbent Carbons from IlliI10is Coals Frank Derbyshire, UK, Center for Applied Energy Research Marit Jagtoyen, UK, Center for Applied Energy Research Danny Turner, Harry Ni, Chris Toles, Bob Rathbone; Mark Stewart and Vincent Verheyen UK, Center for Applied Energy Research Franklin Honea, CRSC ABSTRACT This research program has investigated the utility of Illinois coals as precursors for the synthesis of activated carbons by chemical activation, using a combination of coal cleaning by column flotation, followed by reaction with phosphoric acid or potassium hydroxide. With phosphoric acid activation, carbons with surface areas around 800 m2g-1 are produced at HTT to about 500°C. The carbons are dominantly microporous, with low mesopore surface areas. Above 500°C, the specific surface area decreases, when the acid may be converted to an inactive fonn. Extending the reaction time at high HIT can increase the micropore surface area. Increasing HTT increases the carbon ash content, commensurate with a reduction in yield, and reduces the organic sulfur and hydrogen contents. The carbon properties are strongly dependent upon the ratio of reagent to precursor. Increasing the ratio to about 1.0 increases both the micropore and mesopore surface areas. Further increase lowers the micropore surface area. The reduction can be attributed to increases in ash content. Increasing the ratio also promotes the removal of hydrogen and organic sulfur. The adjustment of the low HIT reaction parameters, over the ranges studied, appear to offer little prospect for significantly modifying the final carhon properties. The surface area of KOH carbons increases steadily with increasing HTT, attaining a value of about 1600 m2g-1 at HTT=800-900°C. The carbons are also highly microporous. The effect of KOH: coal ratio is also important to surface area development. A sharp increase in surface area is obtained by increasing the ratio at low values. At higher ratios, there is a reduction in specific surface area which can be accounted for increased carbon ash content. Activation with H3P04 and KOH produces some similar changes including partial dissolution of the coal structure at low HIT, and the removal of sulfur and hydrogen. The gaseous products could provide sources of H2 (KOH activation), and S (phosphoric acid activation). The liquids could be used as low-sulfur fuels or as a source of phenolics. Standard test methods have shown that these microporous carbons are suitable for the adsorption of small molecules but, not for the adsorption of large molecules such as color bodies. The KOH activated carbons are able to adsorb phenol to a similar extent as a commercial water treatment carbon. The acid activated carbons are much less effective. Further study is recommended. 1/

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FINAL TECHNICAL REPORT

September 1st, 1991 to August 31st, 1992

Project Title:

Principal Investigator:

Co- Principal Investigator:

Other Investigators: Acknowledgement:

Project Monitor:

Synthesis of Adsorbent Carbons from IlliI10is Coals

Frank Derbyshire, UK, Center for Applied Energy Research

Marit Jagtoyen, UK, Center for Applied Energy Research

Danny Turner, Harry Ni, Chris Toles, Bob Rathbone; Mark Stewart and Vincent Verheyen UK, Center for Applied Energy Research

Franklin Honea, CRSC

ABSTRACT

This research program has investigated the utility of Illinois coals as precursors for the synthesis of activated carbons by chemical activation, using a combination of coal cleaning by column flotation, followed by reaction with phosphoric acid or potassium hydroxide.

With phosphoric acid activation, carbons with surface areas around 800 m2g-1 are produced at HTT to about 500°C. The carbons are dominantly microporous, with low mesopore surface areas. Above 500°C, the specific surface area decreases, when the acid may be converted to an inactive fonn. Extending the reaction time at high HIT can increase the micropore surface area. Increasing HTT increases the carbon ash content, commensurate with a reduction in yield, and reduces the organic sulfur and hydrogen contents. The carbon properties are strongly dependent upon the ratio of reagent to precursor. Increasing the ratio to about 1.0 increases both the micropore and mesopore surface areas. Further increase lowers the micropore surface area. The reduction can be attributed to increases in ash content. Increasing the ratio also promotes the removal of hydrogen and organic sulfur. The adjustment of the low HIT reaction parameters, over the ranges studied, appear to offer little prospect for significantly modifying the final carhon properties.

The surface area of KOH carbons increases steadily with increasing HTT, attaining a value of about 1600 m2g-1 at HTT=800-900°C. The carbons are also highly microporous. The effect of KOH: coal ratio is also important to surface area development. A sharp increase in surface area is obtained by increasing the ratio at low values. At higher ratios, there is a reduction in specific surface area which can be accounted for increased carbon ash content.

Activation with H3P04 and KOH produces some similar changes including partial dissolution of the coal structure at low HIT, and the removal of sulfur and hydrogen. The gaseous products could provide sources of H2 (KOH activation), and S (phosphoric acid activation). The liquids could be used as low-sulfur fuels or as a source of phenolics.

Standard test methods have shown that these microporous carbons are suitable for the adsorption of small molecules but, not for the adsorption of large molecules such as color bodies. The KOH activated carbons are able to adsorb phenol to a similar extent as a commercial water treatment carbon. The acid activated carbons are much less effective. Further study is recommended.

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ICCI Project Number: 91-1/1.1A-2
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