Preparation of Sugarcane Based Activated Carbon by One-step Method and Its Adsorption-desorption Performance of Toluene

doi:10.21203/rs.3.rs-3899560/v1

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Preparation of Sugarcane Based Activated Carbon by One-step Method and Its Adsorption-desorption Performance of Toluene

https://doi.org/10.21203/rs.3.rs-3899560/v1

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The sugarcane based activated carbon was prepared by one-step method using sugarcane bagasse as raw material and H₃PO₄ as activator, meanwhile in order to get the better preparation condition of the materials the dose of phosphoric acid addition, material liquid ratio, activation temperature, and activation time on the adsorption performance of activated carbon were discussed. This study investigated the effects of different preparation conditions on the adsorption and desorption performance of activated carbon through characterization such as BET, FT-IR, XRD, dynamic adsorption, and static adsorption, which has shown that when the phosphoric acid content was 30%, the solid-liquid ratio was 1:2, the activation temperature was 400 ℃, and the activation time was 30 minutes by one-step method, the carbon content reached 55.73%, but its specific surface area can reach 1037.7m² /g, the saturated adsorption capacity can reach 487.3mg/g, and the adsorption capacity was still above 80% after three regenerated, and the adsorption and desorption performance was the best.

Activated carbon

Bagasse

Toluene

One-step method

Volatile organic compounds (VOCs) are a general term for a class of organic compounds, most of which are not only toxic and irritating, but also have carcinogenic effects, and they can undergo photochemical reactions with nitrogen oxides, forming more harmful photochemical smog, causing secondary pollution and serious environmental air pollution ^[1–4]. At present, the treatment methods for VOCs include recycling and destruction ^[5], among which recycling technologies mainly include adsorption, absorption, condensation, membrane technology, etc. The activated carbon adsorption method ^[6–8] has been widely used due to its simple equipment, mature process and flexible operation.

Activated carbon is a carbon-based adsorption material composed of microcrystalline structure and amorphous carbon, with well-developed pore structure and generally high specific surface area and pore volume ^[9]. Sugarcane bagasse is the main byproduct in the sugar production process and is a type of agricultural and forestry biomass waste ^[10], which is usually treated through boiler combustion or direct treatment, causing environmental pollution and resource waste ^{[11, 12]}. Sugarcane bagasse, mainly composed of cellulose, hemicellulose, and lignin ^[13], is a carbon rich biomass waste with a carbon content of up to 44.17%, which can be used to prepare biomass activated carbon ^[14]. Zhao Haoran ^[15] reported that sugarcane bagasse still maintains a relatively complete fiber structure after carbonization, and there is abundant honeycomb like pores inside, making it a suitable carbon source for preparing activated carbon. Qin et al. used sugarcane bagasse as the raw material and further activated it to obtain activated carbon for methylene blue adsorption ^[16]. Xiaogang Luo ^[17] used sugarcane bagasse as raw material, after carbonization, impregnation and activation with ZnCl₂ at 600℃ for 2h, the S_BET of activated carbon was 916.1m²/g.

The traditional process for preparing activated carbon usually includes two steps: slow pyrolysis process and continuous activation process, which operate under CO₂ or steam atmosphere in the temperature range of 600–1000°C ^[18–20], or use chemical activators such as potassium hydroxide, phosphoric acid, and zinc chloride ^{[21, 22]}. The traditional two-step method usually requires higher temperature and longer time, while this study introduces a one-step method for simultaneous pyrolysis and activation processes in the presence of activators to reduce energy consumption and shorten processing time to reduce costs. The one-step method for preparing activated carbon can ensure the formation of rich pore structures in activated carbon powder by changing the preparation conditions that is a simpler, greener, and more convenient method for preparing activated carbon, which is an urgent process technology for VOCs adsorption processes. Phosphoric acid activation method consumes less energy compared to physical activation method and has less pollution compared to zinc chloride activation method, making it a relatively ideal process method. At the same time, the activation mechanism of bagasse activated carbon is elaborated in order to provide technical support for the industrialization of bagasse activated carbon. This is of great significance for achieving the sustainable development of the sugar industry and producing carbon materials with strong regeneration ability and higher application value.

2.1 Preparation of sugarcane based activated carbon

Dry the sugarcane bagasse, grind it, and pass it through a 60-mesh sieve; After soaking in distilled water for 2 hours, sonicate with distilled water multiple times to remove impurities, and dry at 100 ℃ for 10 hours.

Take an appropriate amount of pretreated sugarcane bagasse and mix it with different mass fractions of phosphoric acid in different material liquid ratios, soak for 12 hours, and then dry at 80 ℃. Place the dried sample in a tube furnace at 200 ℃ for 2 hours and activate it at different temperatures for different times. After the sample cools down, clean it with distilled water to a pH of 6–7. Dry it at 80 ℃ and grind it for storage.

2.2 Material characterization

X-ray diffraction (XRD, Empyrean sharp shadow) analysis was used to determine the image and crystal structure of the prepared material. The adsorption analyzer performs adsorption and desorption (BET, iPore400) within the range of 77K and N₂ relative pressure P/P₀ = 10^− 6-1, and calculates the specific surface area, pore volume, and pore size. Use scanning electron microscopy (SEM, JSM-7800F) to observe the surface morphology and size structure of the sample. Analyze the types and content of functional groups in the sample using Fourier transform infrared spectroscopy (FT-IR, Thermo Fisher IS5).

2.3 Absorption and desorption experiment

Static adsorption and desorption experiment

The static adsorption capacity of toluene was determined gravimetrically in a vacuum dryer. Put the sample into a toluene vacuum dryer, take it out after adsorption for 48 hours, weigh it multiple times until the sample no longer changes, record the changes of the sample before and after adsorption, and calculate the static saturated adsorption capacity of toluene. Put the saturated sample into an air drying oven for desorption, weigh it, and then put it into a toluene vacuum drying oven again for multiple adsorption-desorption cycles.

Dynamic adsorption and desorption experiment

This study utilized the CEL-GPPCM microreactor system to conduct dynamic adsorption and desorption experiments on toluene. Place the sample in an adsorption tube, and the gas chromatograph automatically injects the sample every 10 minutes to analyze the gas concentration and calculate the toluene adsorption amount. Raise the temperature of the reaction furnace and introduce nitrogen gas to desorb the sample until the sample concentration stabilizes, and then calculate the desorption rate.

3.1 Phosphoric acid addition

The XRD patterns of different phosphate additions are shown in Fig. 1, with two peaks at approximately 24° and 44°, corresponding to the (002) and (100) crystal planes of the graphite structure, indicating that the material has been graphitized. This may be due to the high heat treatment temperature during the preparation of amorphous carbon, resulting in partial graphitization of the material, which belongs to partially graphitized amorphous carbon. The peak that appears around 26℃ is the SiO₂ peak generated during the preparation process.

N₂ adsorption–desorption isotherms of activated carbon with different amounts of phosphoric acid are shown in Fig. 2, showing that the prepared material shows type I and type IV binding isotherms. The rapid adsorption in the low-pressure region belongs to type I, and the adsorption in the middle and high-pressure region belongs to type IV, and the H₄ type hysteresis loop appears. This can be attributed to the existence of a narrow mesoporous structure of the adsorbent studied, which is a micro mesoporous material. In addition, the differences in the performance of several samples in areas with relatively low pressure (P /P0 < 0.2) are not significant, while the size of hysteresis loops varies, indicating that the main difference between different samples is the degree of mesoporous development. In Table 1, the saturated adsorption capacity of toluene shows a trend of first increasing and then decreasing with the mass fraction of phosphoric acid, with the highest adsorption capacity at AC-30%. It can be seen that AC-30% has the most developed pore structure and adsorption capacity, with a specific surface area of 826m²/g, pore volume of 0.496cm³/g, average pore size of 2.4nm, and saturated adsorption capacity of 438.9mg/g.

Table 1

Pore structure parameters of activated carbon with different amounts of phosphoric acid
Adsorbents	Surface area(m²/g)	Pore volume(cm³/g)	Average pore size(nm)	Adsorption quantity(mg/g)
AC-20%	675.2	0.414	2.46	372.1
AC-30%	826.0	0.496	2.4	438.9
AC-40%	748.0	0.478	2.56	424.9
AC-50%	709.4	0.453	2.56	391.7

3.2 solid-liquid ratio

The materials prepared in Fig. 3 still have the combination isotherm of type I and type IV, and the hysteresis loop of type H₄ appears, and the size of the hysteresis loop is different, indicating that different solid-liquid ratio has a certain impact on the pore structure, but it is still a micro mesoporous material. The prepared material shows the best performance when the solid-liquid ratio is 1:2 in Table 2. Its specific surface area can reach 826m²/g, pore volume is 0.496cm³/g, average pore size is 2.4nm, and saturated adsorption capacity is 442.1mg/g.

Table 2

Pore structure parameters of activated carbon with different solid-liquid ratios
Adsorbents	Surface area(m²/g)	Pore volume(cm³/g)	Average pore size(nm)	Adsorption quantity(mg/g)
AC-1:1	547.4	0.352	2.58	357.9
AC-1:2	826.0	0.496	2.4	442.1
AC-1:3	692.1	0.451	2.6	380.5
AC-1:4	529.5	0.412	2.78	335.1

3.3 Activation temperature

The XRD patterns of activated carbon at different activation temperatures show that the amorphous carbon prepared at different temperatures is still partially graphitized, indicating that temperature has a significant impact on pore structure, but has a smaller impact on crystal structure as shown in Fig. 4. When the activation temperature is 400 ℃, the prepared material exhibits a combined isotherm of type I and type IV, and exhibits a standard H₄ hysteresis loop; When the activation temperature is 600 ℃, a type II or III isotherm appears, indicating that the pore structure collapses due to excessive temperature in Fig. 5, which belongs to non-porous or macroporous materials.

The prepared activated carbon expresses the best effect when the activation temperature is 400 ℃ in Table 3 and Fig. 6, with a specific surface area of 826m²/g, pore volume of 0.496cm³/g, average pore size of 2.4nm, and the maximum saturated adsorption capacity of 438.9mg/g at 400 ℃. When the temperature is 400 ℃, the adsorption performance is the best, and the longest adsorption penetration time is shown in Fig. 7 and Table 4, reaching adsorption saturation at 150 minutes.

Table 3

Pore structure parameters of activated carbon at different activation temperatures
Adsorbents	Surface area(m²/g)	Pore volume(cm³/g)	Average pore size(nm)	Adsorption quantity(mg/g)
AC-300	301.6	0.235	3.12	205.2
AC-400	826.0	0.496	2.4	431.0
AC-500	395.6	0.265	2.68	200.9
AC-600	73.6	0.109	5.9	93.3
AC-700	89.8	0.118	6.18	87.7

Table 4

Dynamic adsorption data table
Adsorbents	Breakout time(min)	Saturation time(min)	Adsorption capacity (mg/g)
AC-300	10	90	205.2
AC-400	70	150	431.0
AC-500	10	80	200.9

3.4 Activation time

XRD patterns of different activation times are shown in Fig. 8, which shows that amorphous carbon prepared at different activation times has little difference in crystal structure, and the impurity peaks are the least when the activation time is 30min.

The infrared spectrum of activated carbon prepared with activation time of 30min and 60min is shown in Fig. 9, which shows that the absorption peak attributed to OH is formed at 3429cm^− 1, the stretching vibration absorption peak of -CH₃ at 2918cm^− 1, and the chelating carbonyl absorption peak at 1594cm^− 1. 1173cm^− 1 is a C-O stretching vibration. With the increase of activation time, the peak height of C-O absorption increased, indicating that the content of C-O in AC-60min was higher than that in AC-30min.

N₂ adsorption–desorption isotherms of activated carbon at different activation temperatures are presented in Fig. 10, and their specific areas and pore volumes are listed in Table 5. As presented in Fig. 10, the N₂ adsorption–desorption isotherms with a type I in the relative pressure range of 0-0.4, with a type IV with a H₄ hysteresis loop in the relative pressure range of 0.4–1.0, which shows that the adsorbents have microporous and slit like mesoporous structures. When the activation temperature is 30min, the pore structure is the most developed, the specific surface area is 1037.7 m²/g, the pore volume is 0.568cm³/g, and the average pore size is 2.18nm.

Table 5

Pore structure parameters of activated carbon at different activation times
Adsorbents	Surface area(m²/g)	Pore volume(cm³/g)	Average pore size(nm)
AC-15min	984.4	0.562	2.28
AC-30min	1037.7	0.568	2.18
AC-45min	868.7	0.518	2.38
AC-60min	826.0	0.496	2.4

It was found that the maximum saturated adsorption capacity of activated carbon is 487.3mg/g when the activation time is 30 minutes in Fig. 11. The adsorption penetration time is the longest when the activation time is 30 minutes as shown in Fig. 12, and toluene can be completely adsorbed within 70 minutes, gradually reaching adsorption saturation within 70–150 minutes.

Through the above experiments and analysis, the optimum preparation conditions of activated carbon are as follows: phosphoric acid content 30%, solid-liquid ratio 1:2, activation temperature 400℃, activation time 30min. Table 6 shows the organic element analysis of the optimal activated carbon, which shows a carbon content of 55.73%, mainly due to incomplete carbonization and activation, resulting in lower carbon content.

Table 6

Organic element content table of the BAC
Adsorbents	C (%)	H (%)	S (%)	N (%)
BAC	55.73	2.701	0.168	0.58

As can be seen from Fig. 13, as the number of cycles increases, the saturated adsorption capacity of activated carbon decreases, and the time required for complete desorption increases successively. After three sorption and desorption experiments, activated carbon can still have good adsorption properties.

Figure 14 shows the adsorption capacity of BACs that have reached adsorption saturation after desorption for 2 hours at 50 ℃, 80 ℃, and 120 ℃, followed by three cycles. It can be seen that with the increase of desorption temperature, the saturated adsorption capacity increases gradually, and with the increase of regeneration times, the saturated adsorption capacity decreases gradually. The reason is that toluene blocks some micropores, making it difficult to desorb, resulting in a decrease in its adsorption capacity, while as the temperature increases, the movement of toluene molecules becomes stronger, making it easier to detach from the pores. When the desorption temperature is 120 ℃, after three adsorption and desorption cycles, the regeneration adsorption capacity can still reach over 80%, indicating good regeneration performance.

This article uses H₃PO₄ as an activator to prepare sugarcane based activated carbon. The optimal preparation conditions for sugarcane based activated carbon were obtained by using different amounts of phosphoric acid, material liquid ratio, activation temperature, and activation time. The adsorbent was characterized by BET, XRD, and FT-IR, and its performance was studied through static and dynamic adsorption.

When the phosphoric acid addition amount is 30%, the material liquid ratio is 1:2, the activation temperature is 400 ℃, and the activation time is 30 minutes, the prepared sugarcane based activated carbon has the most developed pore structure and superior adsorption performance, with a specific surface area of 1037.7m²/g, a pore volume of 0.568cm³/g, and an average pore size of 2.18nm, The breakthrough time of adsorption is 80 minutes, the saturation time of adsorption is 170 minutes, and the saturation adsorption amount is 487.3mg/g. Among them, the activation temperature is the most important factor affecting the pore structure of activated carbon. This study completes the carbonization-activation process through programmed heating, achieving the preparation of sugarcane based activated carbon with superior adsorption performance and strong regeneration ability at lower activation temperatures and times, reducing costs and energy consumption, which is of great significance for industrial production of carbon materials with high application value.

Contributions

Wenshan Sun: Investigation, Writing – original draft, Data curation. Yongqiang Wang: Writing – review & editing, Supervision. Lihong Yin: Formal analysis, Investigation. Xiubiao Ma: Formal analysis, Conceptualization. Yuxian Qian: Formal analysis, Data curation.

Competing interests

No competing interests.

Funding

This research was supported by the Natural Science Foundation of Shandong Province [ZR2019MEE112] and the Key Basic Research and Development Program of Shandong Province [2020CXGC011201].

Author Contribution

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Bai L, Su X, Lin J, et al. Experimental study on preparation of bagasse based activated carbon by microwave [J]. Jiangsu Agricultural Sciences, 2019, 48(1): 268–271,277. https://doi.org/10.15889/j.issn.1002-1302.2020.01.050
Boujibar O, Souikny A, Ghamouss F, et al. CO₂ capture using N-containing nanoporous activated carbon obtained from argan fruit shells[J]. Journal of Environmental Chemical Engineering, 2018, 6(2): 1995–2002. https://doi.org/10.1016/j.jece.2018.03.005
Cao L, Huang X, Song W, et al. Study on the binary adsorption process of VOCs Gas on activated carbon [J]. Environmental Science and Technology, 2012,35 (5): 160–163. https://doi.org/10.3969/j.issn.1003-6504.2012.05.035
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No competing interests reported.

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Preparation of Sugarcane Based Activated Carbon by One-step Method and Its Adsorption-desorption Performance of Toluene

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Abstract

Figures

1 Introduction

2 Experimental

2.1 Preparation of sugarcane based activated carbon

2.2 Material characterization

2.3 Absorption and desorption experiment

3 Results and discussion

3.1 Phosphoric acid addition

3.2 solid-liquid ratio

3.3 Activation temperature

3.4 Activation time

4 Conclusions

Declarations

Competing interests

Funding

Author Contribution

References

Additional Declarations

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