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Mohamed A. M. Elsayed. Novel Material for the Separation of Mixtures of Carbon Dioxide and Nitrogen. Supervisors : Prof. P. J. Hall & Dr. M. J. Heslop. Introduction. Naturally occurring carbonaceous material. Physical or chemical activation. Polymer precursor. Sol-gel process.

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Mohamed A. M. Elsayed

Novel Material for the Separation of Mixtures of Carbon Dioxide and Nitrogen

Supervisors : Prof. P. J. Hall & Dr. M. J. Heslop


Introduction

Naturally occurring carbonaceous material

Physical or chemical activation

Polymer precursor

Sol-gel process

POROUS CARBON

Pyrolysis

Fewer minerals impurities & controlled pore structure



OBJECTIVES

First stage

1- further developing and modifying resorcinol formaldehyde sol-gel synthesis procedure to make high surface area carbon xerogels with a controlled pore structure.

2- Studying factor affecting on the texture properties and characteristics of the produced material.

3- Further chemical impregnation to produce nitrogen-enriched carbon xerogels

4 - Using different techniques for characterization and analysis (BET, TPD, FTIR, TGA, XRD, SEM, etc…)

Second stage

1-Investigation of full binary isotherms for CO2 and N2 from composition and flow-rate transient times in chromatographic columns

2- Studying factor affecting on the selectivity of CO2 and N2.


Experimental

Drying

Pyrolysis

Resin synthesis

RF-xerogels

Carbon xerogels

Co2 gasification

Active carbon xerogels

Carbon characterization

N2 adsorption-desorption techniques


Result and discussion

Resin analysis

Ultimate and Proximate analyses using Elemental and Thermogravimetric analyzer respectively

R/F= 0.5 and R/C = 300 by mole PH=6 and R/W = 0.25 g/cm3


Thermogravimetric analysis of a dried resorcinol-formaldehyde gel


FTIR spectra for the synthesis resins with different type of catalytic species

nitrile

lactame

aromatic

-CH2-

amides & amines

-OH


Carbon catalytic species xerogelscharacterization by BET.

Effect of changing catalyst species and the catalyst ratios.

(b) MEA was used as a catalyst with different R/C ratio

(a) R/C= 300 by mole with different type of catalytic species


Characteristic pore properties of RF carbon xerogels catalytic species

a Specific surface area determined from the BET equation.

bTotal pore volume.

cMicropore volume determine by Horvath-Kawazoe equation.

dMesopore volume .

eMean pore diameter.


Pore size distribution of the RF carbon xerogels catalytic species

(a) R/C= 300 by mole with different type of catalytic species

(b) MEA was used as a catalyst with different R/C ratio

R/F=0.5 by mole and R/W=0.25 g/cm3


Effect of R/W on porous structure of carbon xerogels. catalytic species

(b) Total and micropores volume

(a) BET surface area and surface area of micropores

R/F=0.5, R/C= 100, PH=6 and MEA as a catalyst


Effect of pH on the on porous structure of carbon xerogels catalytic species

(b) Total and micropores volume

(a) BET surface area and surface area of micropores

R/F=0.5 R/C=100 by mole, R/W=0.25 g/cm3 and MEA as a catalyst.


Effect of degree of Burn-off. catalytic species

Variation of the BET surface area, pore volume and micropore volume with the burn off level of carbon xerogels gasified in CO2 at 900°C

R/F=0.5 R/C=100 by mole, R/W=0.25 g/cm3 and MEA as a catalyst.


(a) catalytic species

(b)

( c )

(d)

Structural characterization with scanning electron microscopyanalysis.

SEM images of cross-section of (a) and (b) samples synthesized under condition pH=6, R/C=300 and R/W=0.25 before and after pyrolysis respectively (c) and (d) carbon xerogels synthesized under condition pH=6, R/C=100 and R/W=0.25 with 0 % and 37% burn-off respectively. (All the samples were prepared using MEA as catalyst)


Conclusion catalytic species

Microporous carbons with high porosity and surface area can be prepared from Resorcinol-Formaldehyde resins

The samples evolve from micro-mesoporous solid (RF-Na2CO3: combination of types I and IV isotherms) with 24.2% micropore to an exclusively microporous material (RF-NH4HCO3: type I isotherm) with 98.7% micropore.

High surface area (> 2890 m2/g) can be obtained at high burn off levels (>75%).

It is possible to tailor the morphology of these materials by varying the initial pH of the precursor’s solution in a narrow range

FTIR study shows that samples prepared by MEA, DEA, MDEA and NH4HCO3 contain nitrogenated functional groups

These porous materials with these functional groups are being expected as suitable candidates for acidic gas capture like CO2 and SO2, which will be studied in the next stage.


Thank-You catalytic species

&

Questions


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