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Significance of micropores for the removal of hydrogen sulfide from oxygen-free gas streams by activated carbon

  • Bin Liu and Songlin Zuo EMAIL logo
Published/Copyright: August 29, 2025
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High Temperature Materials and Processes
From the journal High Temperature Materials and Processes Volume 44 Issue 1

Abstract

Activated carbons are widely used adsorbents for hydrogen sulfide (H2S) removal in the field of gas stream purification in industry. Five commercially available wood-, coal-, and coconut shell-based activated carbons, prepared by phosphoric acid activation and steam activation, were chosen as adsorbents in an effort to elucidate the effect of the pore structure on H2S adsorption of activated carbons in an oxygen-free gas stream. The adsorption experiments were conducted in an adsorption column, and the breakthrough curves of the activated carbons were examined. The results showed that adsorption of H2S by activated carbon under oxygen-free conditions was dependent on the microporous structure, particularly micropores with sizes of <1 nm. The surface area of CS-3 is 1,792 m2·g−1. The H2S breakthrough capacities of WS-1, BS-1, CS-1, CS-2, and CS-3 were 0.006, 0.01, 0.018, 0.021, and 0.026 g·cm−3 under oxygen-free conditions. The adsorption experiments of the KOH- and CuO-loaded activated carbons further confirmed the significance of micropores with sizes of <1 nm for H2S removal. Also, it was found that pre-adsorption or co-adsorption of carbon tetrachloride led to poisoning of the activated carbon for H2S adsorption due to a remarkable reduction in the micropore volume. Therefore, steam-activated materials with highly developed micropore structures were favorable adsorbents for H2S removal because of their high adsorption capacities and reduced fire risk in an oxygen-free gas stream.

Keywords: activated carbon; micropores; hydrogen sulfide; adsorption

1 Introduction

Hydrogen sulfide (H2S) is an acidic and poisonous gas that is frequently found at various concentrations in industrial gas streams such as natural gas, fermentation gas, syngas, and coal-derived gas [1,2,3,4,5]. It is problematic in industrial processes because it poisons catalysts and readily corrodes metallic equipment and pipelines. Accordingly, removal of H2S from industrial gas streams is an indispensable step in areas such as semiconductor manufacture, high-quality oil and gas, and green catalysis [6]. Adsorption is the most commonly used method to remove H2S from gas streams containing concentrations typically below 100 ppm.

Activated carbon is the most widely used adsorbent for H2S in the purification of gas streams [7,8,9]. Generally, removal of H2S requires that the activated carbon be loaded with a catalyst, which is commonly an alkaline substance or metal oxide, because the pristine-activated carbon has poor adsorption capacity for H2S [10,11,12,13,14]. Moreover, extensive investigations have demonstrated that H2S removal by activated carbon involves complex physical and chemical processes. Therefore, the adsorption capacity of activated carbon for H2S depends not only on its physicochemical properties but also on the adsorption parameters [15,16,17]. In particular, in the presence of oxygen, H2S can be oxidized to S, SO3 2−, or SO4 2− species during adsorption by activated carbon impregnated with the catalyst [18,19,20], resulting in remarkably enhanced removal of H2S. Accordingly, air or oxygen is a key factor in the removal of H2S by activated carbon and, thus usually pumped into the gas stream for industrial desulfurization.

However, oxygen and air are not permitted even at quite low concentrations in some gas streams, including natural gas, gaseous carbon dioxide in the beverage industry, and supercritical gas. Under such oxygen-free conditions, the adsorption capacity of activated carbon for H2S is dramatically decreased even if catalyst-loaded activated carbon is used. Unfavorably, the H2S-saturated activated carbon readily ignites during replacement of used adsorbent due to rapid oxidation in air [21,22]. Consequently, the development of efficient H2S removal technology using activated carbon in oxygen-free conditions is desirable for industrial desulfurization. Based on the adsorption mechanism of activated carbon, it can be inferred that surface chemistry and pore structure determine the adsorption capacity for H2S under oxygen-free conditions. It is generally accepted that a basic surface greatly benefits the adsorption of acidic H2S [23,24,25]. However, the effect of pore structure has yet to be addressed in detail. This investigation focused on the effect of the micropore structure of activated carbon on the ability to remove H2S based on detailed structural analysis. The results demonstrated the significance of micropores of different sizes in the adsorption of gaseous H2S by activated carbon, providing new insight into the adsorption process.

2 Experimental

2.1 Activated carbon adsorbents

Five commercially available activated carbons were selected as adsorbents. These included three coconut shell-based materials with different pore structures (three coconut carbon samples, named CS-1, CS-2, and CS-3, respectively), one bituminous-based activated carbon (bituminous carbon sample, named BS-1), and one wood-based activated carbon (wood carbon sample, named WS-1), which were all purchased from Purestar, China. CS-1, CS-2, CS-3, and BS-1 are manufactured by steam activation, and WS-1 is produced by phosphoric acid activation. All of the materials were crushed and sieved to obtain particles of 1.7–3.35 mm.

The activated carbons were modified by impregnating with a solution of Cu(NO3)2 or a KOH solution. The impregnated Cu2+ activated carbons were heat-treated in a N2 atmosphere at 450°C for 1 h to give 8% CuO-loaded activated carbons. The KOH-impregnated activated carbons were dried in an oven at 85°C. The resultant impregnated activated carbons were denoted as C-CuO and C-KOH.

2.2 Pore size analysis

Nitrogen adsorption–desorption tests were performed at 77 K using an adsorption analyzer (Autosorb IQ10, Quantachrome, USA). The surface area was calculated using the Brunauer–Emmett–Teller (BET) equation, and the total pore volume was obtained at a relative pressure of 0.99. The mesopore volume was obtained using the Barrett, Joyner, and Halenda method. The pore size distribution curves were analyzed using the quenched solid density functional theory (QSDFT) method in terms of the adsorption branch. The ratios of pore volumes of different sizes to the total pore volume were also evaluated based on the pore size distribution of the activated carbons.

2.3 Adsorption test

The breakthrough curves were tested in a vertical adsorption tube (24 mm × 230 mm). Nitrogen containing 1% v/v H2S was used as the gas stream for testing breakthrough curves, which was obtained by diluting raw 5% v/v H2S with nitrogen or carbon tetrachloride (CTC)-loaded nitrogen. The gas stream was calibrated and monitored to maintain a total flow rate of 1,450 ± 20 mL·min−1. All tests used the same carbon volume to keep the same contact time of 5 s. The stream flow was maintained until a breakthrough of 50 ppmv was indicated. The time elapsed from the start to the breakthrough was recorded. The H2S detector was provided by Handa Technology (HD-P900-H2S). The H2S breakthrough capacities (BTC) of the adsorbents were calculated by integrating the areas of the breakthrough curves, expressed as the amount (g) of H2S removed from the vapor stream per volume (cm3) of carbon. The saturated adsorption capacity (SAC) was calculated by increased weight, expressed as the amount (g) of H2S removed from the vapor stream per weight (g) of carbon.

BTC = ∫ 0 t v ⋅ ( C 0 − C t ) d t V = v C 0 t − ∫ 0 t v C t d t V ,

where BTC is the breakthrough capacity (g·cm−3), v is the flow rate (cm3·min−1), C 0 is the initial H2S concentration (ppmv), C t is the breakthrough concentration at time t (ppmv), and V is the volume of activated carbon (cm3).

2.4 Ignition temperature testing

The ignition temperatures of the activated carbons were determined according to the method described in the national testing standard of activated carbons (GB/T 7702.9-2008). The activated carbon was first placed in a vertical tube in an ignition point analyzer (FMX-K8, ZhongHuiTian Cheng, China) in direct contact with an air stream. The air stream was slowly heated until the activated carbon began to ignite. The temperatures of the carbon bed and the air entering the bed were recorded. The ignition temperature is defined as the point at which the carbon temperature suddenly rises above the temperature of the air entering the bed.

3 Results and discussion

3.1 Pore structures of activated carbons

Figure 1(a) shows the N2 adsorption/desorption isotherms of the activated carbons. It can be seen that CS-1, CS-2, and CS-3 all exhibited type I adsorption isotherms with no apparent hysteresis loop, indicative of predominantly micropore structures. The WS-1 and BS-1-activated carbons exhibited type IV adsorption isotherms, which had high adsorption capacity before the knee point in the curves and exhibited an obvious hysteresis loop. The results demonstrated that WS-1 and BS-1 had microporous/mesoporous structures. WS-1 was prepared by phosphoric acid activation, a chemical activation method, and therefore contained a high proportion of mesopores. The pore size distributions of these activated carbons are presented in Figure 1(b). A comparison of the pore size distribution curves indicated that the pores in CS-1, CS-2, and CS-3 were predominantly less than 3 nm, while WS-1 and BS-1 had a wide size distribution in the range of <15 nm, with the predominant pores of <2 nm. A further observation (the inset in Figure 1 (b)) demonstrated that the size of the predominant pores was <2 nm·min−1 CS-1, CS-2, and CS-3. Table 1 lists the pore parameters of the five activated carbons obtained in terms of their adsorption/desorption isotherms. As shown in Table 1, CS-2 and CS-3 had microporous structures but almost negligible mesopore volumes, and CS-1 had predominantly micropore structures with a minority of mesopores. BS-1 had developed micropore and mesopore structures. WS-1 is a type of porous carbon with a predominantly mesopore structure. Therefore, the five activated carbons possess different pore structures, depending on the raw materials and activation methods.

Figure 1 N2 adsorption isotherms (a) and pore size distribution (b) of activated carbons.
Figure 1

N2 adsorption isotherms (a) and pore size distribution (b) of activated carbons.

Table 1

Porous parameters of the activated carbons

BET surface area (m2·g−1) Total pore volume (cm3·g−1) Micropore volume (cm3·g−1) Mesopore volume (cm3·g−1) Average pore size (nm)
WS-1 1,315 1.149 0.359 0.665 3.49
BS-1 1,100 0.818 0.369 0.381 2.97
CS-1 1,156 0.626 0.404 0.152 2.09
CS-2 1,371 0.645 0.590 0.032 1.87
CS-3 1,792 0.835 0.728 0.078 1.86

3.2 Effect of pore size on H2S adsorption

Figures 2 and 3 show the H2S breakthrough curves and SACs of the activated carbons. Figure 2 shows that the breakthrough times of WS-1, BS-1, CS-1, CS-2, and CS-3 are about 10, 27, 60, 72, and 95 min, respectively. Correspondingly, the H2S BTC values of WS-1, BS-1, CS-1, CS-2, and CS-3 were 0.006, 0.01, 0.018, 0.021, and 0.026 g·cm−3, respectively (Figure 2). The CS-3-activated carbon column exhibited the highest uptake ability toward H2S in an adsorption column, which was about 10 and 4.4 times that of WS-1 in terms of the breakthrough time and adsorption capacity. Based on the results shown in Table 1 and Figures 1 and 2, it is evident that the higher the micropore volume of activated carbons, the larger the adsorption capacity of H2S. This indicates that the micropores of activated carbons play a key role in removing H2S in the activated carbon adsorption column. Figure 4 shows that the adsorption capacity of activated carbons in a fixed bed increased almost linearly as the micropore volume increased, further confirming the significance of the micropores in the adsorption of H2S. Obviously, mesopores have a negligible contribution to the H2S uptake. Accordingly, although WS-1 and BS-1 had a much higher total pore volume than CS-1 and CS-2, they exhibited a much lower H2S adsorption capacity. Similarly, Table 1 and Figures 1 and 2 indicate that the surface area is not an exact parameter to evaluate the H2S adsorption capacity of activated carbons. Clearly, the breakthrough of H2S gas stream through an activated carbon column varied greatly dependent on the activated carbon species. WS-1 has the shortest breakthrough time of about 27 min and the least BTC value. In particular, the adsorption capacity of CS-3 toward H2S was about 4.4 times that of WS-1 in the fixed-bed adsorption process. This indicated that it had about 4.4 times the adsorption capacity. Moreover, we found that micropores played a key role in the adsorption of H2S. CS-3 had a much higher micropore volume (0.728 cm3·g−1) than that of WS-1 (0.359 cm3·g−1). Comparing CS-1, CS-2, and CS-3-activated carbons, which were all prepared by steam activation of coconut shell-based chars, it was found that the activated carbon with a higher micropore volume exhibited a longer breakthrough time.

Figure 2 H2S breakthrough curves of WS-1, BS-1, CS-1, CS-2 and CS-3.
Figure 2

H2S breakthrough curves of WS-1, BS-1, CS-1, CS-2 and CS-3.

Figure 3 SACs of WS-1, BS-1, CS-1, CS-2 and CS-3.
Figure 3

SACs of WS-1, BS-1, CS-1, CS-2 and CS-3.

Figure 4 Relationship between carbon porous properties and H2S adsorption capacity.
Figure 4

Relationship between carbon porous properties and H2S adsorption capacity.

Furthermore, it is noteworthy that although there was only a small difference in the micropore volumes of BS-1 and CS-1 (0.369 and 0.404 cm3·g−1, respectively), CS-1 exhibited a much longer breakthrough time of 60 min compared to the 30 min of BS-1. The calculated adsorption capacity of CS-1 was also much higher than that of BS-1. This comparison indicated that the micropore size exerted a significant effect on the adsorption of H2S by activated carbon. In order to elucidate the effect of micropore size on H2S adsorption, a regression analysis was conducted. Based on the pore size distribution determined using the QSDFT model, the total pore volumes of the five activated carbons were calculated, together with the volumes of pores with diameters below 1, 2, and 5 nm. All of the results are listed in Table 2.

Table 2

Analysis of different micropores

Pore range (nm) WS-1 BS-1 CS-1 CS-2 CS-3
Volume (cm3·g−1) Ratio (%) Volume (cm3·g−1) Ratio (%) Volume (cm3·g−1) Ratio (%) Volume (cm3·g−1) Ratio (%) Volume (cm3·g−1) Ratio (%)
<1 0.207 16.8 0.241 34.1 0.274 47.9 0.310 52.9 0.332 43.7
<2 0.382 31 0.258 36.5 0.378 66.1 0.382 65.2 0.495 65.1
<5 0.596 48.3 0.416 57.8 0.424 74.1 0.449 76.6 0.722 95.0
Total 1.234 0.707 0.572 0.586 0.76

To analyze the relationship between the pore volume and H2S adsorption capacity, the data were plotted, as shown in Figure 5. Figure 5 shows that the SAC was significantly increased as the volume of pores with a diameter less than 1 nm increased, with the best regression coefficient of 0.9527. The R 2 values were much lower for volumes of pores of sizes less than 2 and 5 nm, indicating that the volume of pores with a size of <1 nm was most strongly correlated with the H2S adsorption capacity. In addition, the slope of the curve for the volume of pores with a size of <1 nm versus SAC was greater than that of the other two, further confirming that the micropores with a size of <1 nm greatly contribute to H2S adsorption. The adsorption theory predicted that the favorable pores in a porous adsorbent for adsorption are those with sizes of approximately three times the molecular size of the adsorbate [26,27,28]. The molecular diameter of H2S is about 0.36 nm [29], so the most effective pore size for adsorbing H2S is approximately 1 nm, which is consistent with the above-mentioned results. Accordingly, it is certain that the volume of pores with sizes of <1 nm had the most important effect on H2S adsorption.

Figure 5 Relationship between the pore volume and H2S adsorption capacity.
Figure 5

Relationship between the pore volume and H2S adsorption capacity.

Additionally, it is noted that the micropore volume of BS-1 and WS-1 is approximate, and WS-1 has a higher surface area than BS-1, but BS-1 has a much longer breakthrough time and higher adsorption capacity toward H2S in a gas flow. This discrepancy is caused by their surface chemistry. WS-1 was prepared by phosphoric acid activation of wood sawdust, and thus, is characteristic of an acidic surface. BS-1 was fabricated by steam activation of coal, and thus, is of a basic surface. For the acidic H2S, the basic surface favors the uptake of H2S on the surface of activated carbons.

3.3 Effect of loaded activated carbon and pre-adsorption on H2S adsorption

Generally, H2S is not a single gas in the adsorption process, and many other substances are accompanied by the H2S adsorption process, like the biogas, natural gas, and NH3 [30,31,32]. Organic substances are important factors in adsorption. Previously, KOH and CuO were commonly used to improve the uptake of H2S by activated carbon because H2S adsorption could be remarkably promoted by providing basic surfaces for KOH-loaded activated carbons and active sites of chemically adsorbing H2S for the loaded CuO-activated carbons. Therefore, we further investigated the H2S adsorption ability of KOH or CuO-loaded CS-3. The N2 adsorption isotherms of CS-3, C-KOH, and C-CuO are shown in Figure 6, and their pore parameters are listed in Table 3. It is evident that the micropore volume of the activated carbon was remarkably reduced by almost 50% after loading KOH or CuO. Particularly, the pores with sizes of <1 nm were sharply reduced to a nearly negligible value. As a result, the H2S adsorption capacity was decreased from 6.5 g/100 g for CS-3 to 4.4 g/100 g for the KOH-loaded CS-3, and to 3.8 g/100 g for the CuO-loaded CS-3, as shown in Figure 7. Nevertheless, it should be noted that the H2S adsorption experiments in this study were conducted in an oxygen-free stream. In an oxygen-free atmosphere, the catalytic ability of KOH and CuO to convert H2S into S, SO3 2− or SO4 2− was inhibited in the process of removing H2S, which commonly works in an oxygen or air-containing stream [33,34,35].

Figure 6 N2 adsorption isotherms for CS-3, C-KOH, and C-CuO.
Figure 6

N2 adsorption isotherms for CS-3, C-KOH, and C-CuO.

Table 3

Porous properties of CS-3, C-KOH, and C-CuO

BET surface area (m2·g−1) Total pore volume (cm3·g−1) Micropore volume (cm3·g−1) Pore volume below 1 nm (cm3·g−1)
CS-3 1,792 0.835 0.728 0.332
C-KOH 1,216 0.809 0.389 0.0748
C-CuO 972 0.607 0.361 0.0591
Figure 7 Adsorption capacities of CS-3, C-KOH, and C-CuO.
Figure 7

Adsorption capacities of CS-3, C-KOH, and C-CuO.

Considering that the gas stream usually contains organic substances other than H2S, we tested the effect of CTC on the adsorption of H2S by activated carbon. Surprisingly, the breakthrough time was sharply decreased to almost zero when CS-3 pre-adsorbed gaseous CTC or the adsorption was conducted with a gaseous mixture of CTC and H2S. We described this phenomenon as the poisoning of activated carbon for H2S adsorption. This was due to the adsorbed CTC that can occupy to some degree the micropores with sizes of less than 1 nm because the molecular size of CTC was 0.59 nm [36]. This poisoning phenomenon further illustrates the importance of micropores of smaller sizes in the H2S adsorption process. Therefore, it can be predicted that the organic substances of the smaller molecular dimensions contained in the H2S stream produce an obvious detriment on the H2S adsorption (Figure 8).

Figure 8 The effect of CCl4 on H2S adsorption.
Figure 8

The effect of CCl4 on H2S adsorption.

3.4 Risk of spent carbon fire

In the industrial process, fire risk is another important issue to be considered in the process of activated carbon for H2S removal. We therefore tested the ignition temperatures of WS-1, BS-1, and CS-3 microporous activated carbons and the KOH- and CuO-loaded activated carbons, C-KOH and C-CuO, as shown in Table 4. It was found that loading KOH or CuO led to an obvious decrease in the ignition temperature. This may be due to catalytic oxidation of carbon by air or oxygen in the presence of KOH or CuO. Clearly, the BS-1 and CS-3 microporous activated carbon materials were safer and exhibited an outstanding advantage in the large-scale industrial process.

Table 4

Safety parameters of CS-3, BS-1, C-KOH, and C-CuO

Samples Ignition temperature (°C) Spent carbon fire
CS-3 407 No
BS-1 459 No
WS-1 394 No
C-KOH 232 Burn directly
C-CuO 360 Burn directly

4 Conclusions

The five activated carbon materials were prepared by phosphoric acid activation and steam activation from coal, coconut shell, and wood. Their breakthrough curves and H2S adsorption capacities were examined using an adsorption column in an oxygen-free stream. The micropore volume of CS-3 is 0.728 cm3·g−1 and the average pore size is 1.86 nm. The H2S breakthrough capacity of coconut shell-based steam-activated carbon was 0.026 g·cm−3 under oxygen-free conditions. The results showed that the micropores with sizes of <1 nm were the main contributors to the uptake of H2S, with mesopores having nearly negligible contribution. The adsorption experiments of the KOH- and CuO-loaded activated carbons and pre-adsorption experiments of tetrachloride further confirmed the significance of the micropores with sizes of <1 nm. In addition, the steam-activated carbons exhibited higher safety due to a higher ignition temperature. The loading of KOH and CuO apparently reduced the ignition temperature of the activated carbons.

Acknowledgments

This study was performed in the framework of the research work in the State Key Laboratory of Chemistry and Utilization of Agriculture and Forestry Biomass in China.

  1. Funding information: This study was funded by the National Key Research and Development Program of China (No. 2019YFB1503804).

  2. Author contributions: Bin Liu, conceptualization, methodology, formal analysis, software, data curation, resources, writing – original draft, writing – review and editing, and visualization. Songlin Zuo, writing – original draft, writing – review and editing, methodology, supervision, and funding acquisition. The manuscript was written through the equal contributions of all authors. All authors read and approved the final manuscript.

  3. Conflict of interest: The authors state no conflict of interest.

  4. Compliance with ethical standards: We declare that accepted principles of ethical and professional conduct have been followed.

  5. Consent to participate: Not applicable.

  6. Consent to publish: Not applicable.

  7. Data availability statement: The datasets used in the current available from the corresponding author on reasonable request.

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Received: 2025-03-26
Revised: 2025-06-17
Accepted: 2025-06-17
Published Online: 2025-08-29

© 2025 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/htmp-2025-0085
Keywords for this article
activated carbon; micropores; hydrogen sulfide; adsorption
Creative Commons
BY 4.0

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