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For gas separation and purification, high surface area and adequate pore size distribution
are of great importance. Yet in the case of gases like green house gases (CO2, CO, N2O,
CH4), or SO2, H2S etc., chemical or thermal activation is required to improve the
adsorption capacity. However, this way of improving adsorption capacity is associated
with changes in the porous structure of the adsorbent. Here the effect of heat treatment
and KMnO4 impregnation on the textural and structural properties of a new Precipitated
Silica Structure (PSS), synthesised from water glass and inorganic calcium and
Fig.3a. Showing nitrogen physisorption isotherms of pure PSS
magnesium salts are presented. The effect of various routes of KMnO4 impregnation on and PSS calcined at different temperatures
the pore systems and the resulting H2S capacity were also considered.

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ÎThe dried pellets of PSS were heat treated under air for 4 hours at 400üC, 600üC and
800üC, respectively, and then removed from the furnace to cool in ambient conditions.
Î Virect (I) and post (II) impregnation routes at 8 and 13% by weight of KMnO4 and
NaHCO3 were successfully employed to prepare impregnated samples.
ÎThe nitrogen adsorption was measured at liquid nitrogen temperature 77K (-196°C)
using a Micromeritics ASAP 2000 volumetric adsorption analyser. The textural properties
were estimated from The BET standard equation ,the t-plots and density functional Fig.3b Showing NLDFT pore-size distribution curves of pure PSS
theory (VFT) method for Pore Size Vistribution. and PSS calcined at 400°C, 600°C and 800°C

Î The H2S concentration of ~12 ppm at 23 °C and 50% RH was flow through
impregnate samples of ~50g each loaded into the four columns forming 52mm high
beds. The flow was 1.8m3h-1 and 0.9m3h-1 for 0.2s and 0.4s contact time, respectively.

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Fig.4a showing nitrogen isotherms for pure PSS and samples

impregnated according to route I and II with different amount of
KMnO4 and NaHCO3. PSS60 is pure PSS dried at 60°C and 50% RH

à
à Fig.1 showing TGA/DTG curve for pure PSS
Setup of challenge test of H2S uptake

Setup of challenge test of H2S uptake

Fig.2 showing XRD patterns of pure PSS dried at

105°C and heat treated at 600 and 800°C for 4h

Fig.5a showing H2S concentration up- and downstream

of the impregnated PSS at 0.4 s contact time Fig.4b Showing NLDFT pore-size distribution curves of pure PSS and
samples impregnated with different amount of KMnO4 and NaHCO3.

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Fig.5b Showing efficiency profiles and H2S Uptake
capacity in [wt %] at 0.4s contact time
Î ùhen PSS heated at 400oC, the SBET surface area decreased accompanied by an
increased in pore volume and pore size. ùhen heated at 600 and 800oC both BET surface
area and a total pore volume decrease as well as the shift of pore size toward larger size.
At 800oC the amorphous PSS transformed into cristobalite and lost its porosity.
Î Virect (I) and post (II) impregnation routes at 8 and 13% by weight were successfully
employed to prepare impregnated samples. Regardless of the impregnation method and
amount the complete pore size distribution (1-30nm) was retained even if the incremental
pore volume was reduced.
ÎThe H2S uptake seems to be inversely proportional to the BET surface area and the total
pore volume with best results found for a 13% direct impregnated sample. A longer
contact time for H2S uptake was also found beneficial.