Preparation of biochar from pyrolysis of soybean straw at different pyrolysis temperature for cadmium removal from wastewater and pyrolysis gas investigation

Chao Lv; Peng Liu; Song Cheng

doi:10.1016/j.arabjc.2024.105946

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09 2024

:17;

105946

doi:

10.1016/j.arabjc.2024.105946

Preparation of biochar from pyrolysis of soybean straw at different pyrolysis temperature for cadmium removal from wastewater and pyrolysis gas investigation

Chao Lv^{^a}, Peng Liu^{^b,⁎}, Song Cheng^{^c,⁎}

a School of Coal Engineering, Shanxi Datong University, Datong, Shanxi 037009, China

b School of Vanadium and Titanium, Panzhihua University, Panzhihua 617000, China

c College of Chemistry and Chemical Engineering, Henan Polytechnic University, Jiaozuo 454003, China

⁎Corresponding authors. tbagmo@126.com (Peng Liu), chengsong@hpu.edu.cn (Song Cheng)

Received: 2024-4-9, Accepted: 2024-8-1,

Disclaimer:
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.

Abstract

The Cd²⁺ adsorption performance of biochar derived from soybean straw pyrolysis at 400–600 °C is investigated. Langmuir model can accurately describe the Cd²⁺ adsorption data with adsorption amount of 47.30 mg/g with pH=5. Cd²⁺ adsorption kinetic process could be analyzed using Pseudo-second-order. Biochar has large Cd²⁺ wastewater treatment volume, based on column adsorption experiment. The π-electrons play an important role in Cd²⁺ adsorption, based on adsorption mechanism analysis. Biochar has good stability after three cycles. Biochar also has good application potential used in lithium ion battery anode with specific capacity of 132 mA g⁻¹. Besides, pyrolysis gas is recycled in the preparation process of biochar with heating value of the 12.10 MJ/Nm³. These results indicate that soybean straw waste is converted into sustainable adsorbent for Cd²⁺ wastewater treatment.

Keywords

Soybean straw

Pyrolysis

Cd2+

Adsorption

Energy storage

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1 Introduction

Cadmium is a kind of the toxic heavy metal in the water ecosystem, which has caused a serious of the environmental problem to the humans (Nosuhi and Nezamzadeh-Ejhieh, 2017; Guo et al., 2024). The sources of cadmium-containing wastewater include the production process of metal mining, smelting, electrolysis, pesticide, medicine, inorganic pigment manufacturing, and electroplating. The cadmium can generate reactive oxygen species, which damage DNA structure and restrain DNA repair. Therefore, cadmium wastewater must be removed from wastewater to eliminate its environmental hazards to environment (Shafiof and Nezamzadeh-Ejhieh, 2020). The wastewater treatment methods include the chemical precipitation, membrane filtration, electrochemical treatment and adsorption (SalehA et al., 2013; Khani et al., 2010; Mehrali-Afjani and Nezamzadeh-Ejhieh, 2020 ). Adsorption is one of the widely used methods for cadmium wastewater treatment owe to the advantages of simple process and environment-friendly (Qin et al., 2023; Yuan et al., 2023). Therefore, adsorption technology is used as the effective method for cadmium wastewater treatment (Su et al., 2019; Guan et al., 2024). The biochar, activated carbon and zeolite molecular sieve are common adsorbents that are widely applied in wastewater treatment (Wang et al., 2024). However, the price of the common adsorbents is relatively expensive, resulted in the high cost of wastewater treatment. Therefore, preparation adsorbent with low-cost for large-scale wastewater treatment is urgent.

Biochar is a kind of the carbonaceous porous material, which belongs to the by-product of the biomass pyrolysis, and has promising potential in cadmium wastewater treatment (Huang et al., 2020; Fu et al., 2019). Yin et al. (2023) prepared the Pennisetum sp. straw biochar for cadmium wastewater treatment with the cadmium adsorption amount of the 53 mg/g (Yin et al., 2023). Yin et al. (2019) prepared the Pennisetum sp. straw biochars modified by KMnO₄ for cadmium wastewater purification with the adsorption amount of the 45.18 mg/g (Yin et al., 2019). Zhang et al.(2020) prepared the biochar derived from Agaricus bisporus substrate for cadmium removal from wastewater with the adsorption amount of the 64.80 mg/g (Zhang et al., 2020). Liu et al. (2020) prepared the blue algae-derived biochar, which has promising potential in cadmium wastewater removal with the adsorption amount of the 135.70 mg/g (Liu et al., 2021). Yang et al. (2023) prepared the novel MgO-modifed biochar derived from rice straw for cadmium wastewater removal with the adsorption amount of the 441.1 mg/g (Yang et al., 2023). Besides, biochar can be well generated with good stability after use using simple regeneration method. These above results demonstrate that biochar is the sustainability adsorbents for cadmium removal from wastewater.

The biochar obtained from biomass pyrolysis is much cheaper than that of the commercial activated carbon (Kearns et al., 2014). The typical price of commercial activated carbon is about US $ 2890/ton (Ng et al., 2003). Some literatures have reported the preparation cost of the biochar, which is about the US $ 246/ton (Ahmad et al., 2014) and US $ 51–386/ton (Meyer et al., 2011). Besides, the regeneration process of biochar is simple after use (Panahi et al., 2020). Therefore, biochar is the sustainable low-cost adsorbent for pollution wastewater treatment.

In this work, the soybean straw (SS) is the by-product of the soybean harvest. The SS is a kind of agricultural waste that is used for preparation of biochar using pyrolysis technology at different pyrolysis temperature for cadmium removal from wastewater. The physicochemical properties of biochar are analyzed. The cadmium adsorption capacity of the biochar prepared from different temperature is analyzed. The involved cadmium adsorption mechanisms on biochar are systematically investigated. The heating value and gases composition of the pyrolysis gas obtained from biochar preparation process are investigated. Besides, the possible of the biochar used in lithium-ion battery is also analyzed.

2 Materials and methods

2.1

2.1 Preparation of biochar

The SS is crushed with the particle size of about 840 μm. The 15 g SS is put in the resistance tube furnace, which is heated at 400–600 °C. The oxygen in the pyrolysis system is removed using the N₂ before starting experiment. Pyrolysis gas is collected from biochar preparation process, and purified for use. After that, the purification pyrolysis gas is named as the bio-gas. The biochar is the residue in resistance furnace after cooling. Biochar produced from the temperature of 400–600 °C is named as BY, and Y is temperature.

2.2

2.2 Adsorption experiment

The influence of initial pH on Cd²⁺ adsorption is analyzed at pH of 2–6. The 0.1 g biochar is put in the 100 mL Cd²⁺ solution at different Cd²⁺ concentrations, which is used to investigate adsorption isotherm of biochar. Residual Cd²⁺ concentration is detected using the atomic absorption spectrometer after reaching adsorption equilibrium. In the adsorption kinetic experiment, 0.1 g biochar is mixed in 100 mL Cd²⁺ solution (200 mg/L) to investigate adsorption capacity of biochar over time with pH of 5.

Cd²⁺ adsorption amount (q_e or q_t) in above adsorption experiments are calculated as follows:

(1)

q_{e} = \frac{V (C_{o} - C_{e})}{M}

(2)

q_{t} = \frac{V (C_{o} - C_{t})}{M}

C_o is initial concentration. C_e and C_t are the equilibrium concentration and Cd²⁺ concentration over time, respectively. M is biochar mass. V is solution volume. Adsorption kinetics and isotherm models are listed in Tables 1-2 in the supporting material. The practical application of biochar is investigated in the column adsorption experiment.

Table 1 Basis property of biochar produced at 400–600 °C.

Sample	BET (m²/g)	C/%	H/%	N/%	O/%	H/C	O/C
B400 °C	50.17	69.81	2.25	0.54	27.4	0.032	0.39
B500 °C	126.32	75.14	2.13	0.92	21.81	0.028	0.29
B600 °C	190.56	76.33	1.96	0.78	20.93	0.026	0.27

Table 2 Kinetic parameters of Cd²⁺ adsorption on biochar produced at 400–600 °C.

Model	Parameters	B400 °C	B500 °C	B600 °C
Pseudo-first-order	qe.cal(mg/g)	20.84	24.92	27.97
Pseudo-first-order	K₁(1/min)	0.01554	0.02217	0.0205
	R²	0.8854	0.7373	0.8222
Pseudo-second-order	qe.cal(mg/L)	24.15	28.95	31.98
Pseudo-second-order	K₂(g/mg.min)	0.000787	0.00082	0.00079
	R²	0.9987	0.9975	0.9991
	h(mg/mg.min)	0.00036	0.00057	0.00064
Intraparticle diffusion	C(mg/g)	8.32	12.95	14.12
Intraparticle diffusion	K₃(mg/gmin^1/2)	0.653	0.657	0.746
	R²	0.917	0.951	0.910

3 Results and discussion

3.1

3.1 Physicochemical properties of biochar

Table 1 lists the basic property of biochar. Table 1 indicates that biochar has large C content at high temperature. This result indicates that biochar prepared from high temperature has high degree of aromaticity, indicating that high pyrolysis enhances the enrichment of C element. As Table 1 shown, the content of H and O decreases with increasing in pyrolysis temperature. Besides, O/C and H/C ratio also decrease with increasing in pyrolysis temperature. These results indicate that the biochar prepared from high temperature has large aromaticity and low polarity compared to low temperature (Sun et al., 2014).

Table1 also shows that biochar has large specific area with different temperature. The specific area of the biochar prepared form 600 °C is the largest than other pyrolysis temperature, indicating that temperature significantly influences the specific area of biochar. The pore and 2D annular structures are generally formed during the thermal decomposition of biomass as temperature increases.

Fig. 1 shows the chemical functional groups of the biochar. The —OH group is appeared at peaks of the 3420–3400 cm⁻¹ (Fig. 1). All the samples have the prominent peak at around 1600 cm⁻¹ band, which is the aromatic carbonyl/carboxyl C⚌O stretching. The oxygen-containing functional groups of biochar can bind with the metal ions, realizing the wastewater purification. The aliphatic chain of the CH₃— group is appeared at the peak of the 1380 cm⁻¹ (Zhao et al., 2015). The biochar has the —CH group at round 870 cm⁻¹ (Nowrouzi et al., 2017). However, the peaks intensity of the —OH and C⚌O group become weak at high temperature.

Chemical functional groups of biochar produced at 400–600 °C.

3.2

3.2 Influence of pH

Fig. 2 shows the influence of initial pH on Cd²⁺ adsorption. Fig. 2 indicates that the pH value significantly influences the adsorption performance of the biochar. The Cd²⁺ adsorption amount is low at pH=2–3. In a word, the Cd²⁺ adsorption on biochar is hindered (Omrani and Nezamzadeh-Ejhieh, 2020). However, the H⁺ concentration generally decreases with increasing in pH value. Therefore, Cd²⁺ adsorption capability generally increases with increasing in pH value. However, the precipitation is formed in the Cd²⁺ solution at pH>7.34 (Cheng et al., 2021). The solution with a certain of H⁺ concentration will contribute to Cd²⁺ adsorption on biochar. Besides, the precipitation of the Cd²⁺ can be hindered. Therefore, Cd²⁺ adsorption with the pH of 5 is feasible.

3.3

3.3 Adsorption kinetics

Adsorption kinetics models such as pseudo-first-order, pseudo-second-order and intraparticle diffusion model are used to describe the adsorption kinetics process (Yang et al., 2021). The fitting results of the Cd²⁺ adsorption data fitting the above adsorption kinetics models are listed in Table 2. As Table 2 shown, the biochar prepared from high temperature has large Cd²⁺ adsorption amount, which is larger than that low temperature. The pseudo-second-order model has the largest correlation coefficient (R²) than the pseudo-first-order and intraparticle diffusion models. Therefore, Cd²⁺ adsorption on biochar analyzed by the pseudo-second-order model is feasible. Besides, Cd²⁺ adsorption on biochar is influenced by chemisorption. Fig. 3 shows the fitting results using pseudo-second-order model. The intraparticle diffusion model is also used to fit Cd²⁺ adsorption data (Fig. S1). As Fig. S1 shown, the intercept of the fitting curve is not zero, indicating that the mass transfer rate of Cd²⁺ adsorption on biochar is different in initial and final adsorption stages. The fitting C values of biochar are in the range of the 8.32–14.12. This result indicates that rate-limiting step of Cd²⁺ adsorption on biochar is influenced by the intraparticle diffusion.

Cd2+ adsorption data fitting the pseudo-second-order kinetic model.

3.4

3.4 Adsorption isotherms

Langmuir and Freundlich isotherm models are used to analyze the Cd²⁺ adsorption process. The Cd²⁺ adsorption parameters are calculated from adsorption isotherm data fitting adsorption isotherm model, which are listed in Table 3. Langmuir isotherm model better fits Cd^{2+ +} adsorption data compared to the Freundlich isotherm owe to large coefficients R² (Table 3). The Cd²⁺ adsorption amount of biochar produced at large temperature is large compared to biochar produced at low temperature, based on fitting results in Table 3. It might be explained that the biochar produced at large temperature has high BET surface area that contributes to Cd²⁺ adsorption. In addition, biochar has abundant surface chemical functional group and mineral component, which also contribute to Cd²⁺ removal. The fitting curve of the Cd²⁺ adsorption on biochar using Langmuir model is shown in Fig. 4. The Cd²⁺ adsorption capability of various of the biochar is summarized in Table S3. The biochar produced from SS has large Cd²⁺ adsorption capability compared to other biochar, demonstrating that SS biochar might be acted as an efficient adsorbent for Cd²⁺ removal from wastewater. B600 °C is acted as the candidate for further utilization and study due to large Cd²⁺ adsorption amount.

Table 3 Adsorption isotherm parameters of Cd²⁺ adsorption on biochar produced at 400–600 °C.

Isotherms	Parameters	B400 °C	B500 °C	B600 °C
	Q₀(mg/g)	33.91	39.18	47.30
Langmuir	K_L(L/mg)	0.0117	0.0155	0.0112
	R²	0.9935	0.9914	0.9967
	K_F((mg/g).(L/mg)^1/n)	5.6279	8.7501	6.9065
Freundlich	1/n	0.2713	0.3391	0.2925
	R²	0.9742	0.9579	0.9124

Cd2+adsorption data fitting the Langmuir model.

3.5

3.5 Recyclability of biochar

The reusability can be employed as an important parameter to investigate the practical application of biochar. The recyclability result of biochar is shown in Fig. S2. The Cd²⁺ adsorption amount of regenerated biochar decreases as cycle increases (Fig. S2). The Cd²⁺ adsorption capability is 22.91 mg/g at third cycle. The reason might be that biochar loses part of adsorption sites after regeneration, resulted in the decrease of Cd²⁺ adsorption amount (Herath et al., 2020). This result proves that biochar might be used as the recyclable adsorbent for Cd²⁺ removal from wastewater.

3.6

3.6 Adsorption mechanism

Fig. 5 shows the SEM-EDX images of B600 °C after Cd²⁺ adsorption. After Cd²⁺ adsorption, the surface of B600 °C appears grayish white particles, which are carbon, oxygen, calcium and cadmium, based on EDX analysis. This result proves that Cd²⁺ is adsorbed by B600 °C. XRD is used to analyze the adsorption status of Cd²⁺ on B600 °C. Fig. 6a shows that CdCO₃ is appeared on B600 after Cd²⁺ adsorption (Wang et al., 2015; Xu et al., 2013). The existence of the CdCO₃ indicates that the carbonate in B600 °C might react with Cd²⁺ to form the CdCO₃; which is one of the Cd²⁺ removal methods.

SEM-EDX images of B600 °C loaded Cd2+ (a-d).

XRD pattern of B600 °C after adsorption Cd2+ (a), FTIR of B600 °C before and after adsorption Cd2+ (b).

B600 °C before and after adsorption Cd²⁺ is analyzed by the FTIR spectrum (Fig. 6b). As Fig. 6b shown, the aromatic structure of —CH of the B600 °C is appeared at peak of the 874–796 cm⁻¹. The —CH group is a kind of the weak cation-π binding agent, which could bind with the Cd²⁺, resulted in the formation of the Cd-π (Xie et al., 2014). The peak intensity of 874–796 cm⁻¹ is weaker after adsorption compared to before Cd²⁺ adsorption, resulted in the formation of the Cd-π on B600 °C after Cd²⁺ adsorption. The CH₂ group is appeared at peak the 1390 cm⁻¹. However, the peak location has changed after adsorption. Besides, peak position of C⚌C/C⚌O group also has changed after adsorption. The above results demonstrate that it is existence of the Cd²⁺-π interaction during adsorption process owe to high graphitization degree of the B600 °C.

B600 °C also has inorganic salt ions (magnesium, calcium and potassium ions). Therefore, it is existence of ion exchange between Cd²⁺ and inorganic salt ions during adsorption process. Therefore, ion exchange could also realize Cd²⁺ removal from wastewater. The Mg²⁺, Ca²⁺ and K⁺ concentrations in the Cd²⁺ adsorption process are 2.94, 2.68 and 0.35 mg/L, respectively, demonstrating that ion exchange occurs during Cd²⁺ adsorption process.

XPS spectrum is used to investigate Cd²⁺ adsorption behavior on biochar. As Fig. 7 shown, O 1 s spectrum has three peaks. The C⚌O, C—O and O—C⚌O groups are corresponded to the peaks of the 531.46, 532.54 and 533.69 eV, respectively (Wang et al., 2018). However, the peak area and binding energy of C⚌O, C—O and O—C⚌O groups change after Cd²⁺ adsorption. Peak area of C—O and O—C⚌O decreases from 41.76 % and 29.02 % to 36.49 % and 23.21 % after Cd²⁺ adsorption, respectively. The analysis result shows that the oxygen-containing functional groups involve into Cd²⁺ adsorption (Zhang et al., 2017). The spectrum of Cd3d is used to analyze the binding energy of Cd²⁺ adsorption on biochar, which have four peaks. The analysis result indicates that the existence form of the cadmium is presented as Cd²⁺ (43.78 %) and Cd-O (56.22 %).

The wide scan XPS spectrum (a) and C 1 s XPS spectra before and after Cd2+ adsorption (b-c), XPS survey spectra along with the spectra of Cd3d (d) after adsorption.

3.7

3.7 Column adsorption experiment

The practical application of the B600 °C is investigated in the column adsorption experiment. The Cd²⁺ solution with 1 mg/L is employed as simulated wastewater to explore column adsorption performance of B600 °C. Single bed volume (BV) of column adsorption is 20 mL. Fig. S3 shows the corresponding breakthrough curve. As Fig. S3 shown, the effective treatment volume of Cd²⁺ is 820 mL. This result indicates that B600 °C has potential in the long-term application.

3.8

3.8 Application biochar in energy storage

The rate performance of B600 °C is used to investigate the energy storage potential used in lithium ion batteries at different current densities of 50–2000 mA g⁻¹ (Fig. S4). The initial charge and discharge is 41.59 %, based on analysis result. The specific capacity of B600 °C at 50–2000 mA g⁻¹ is 132, 102, 82, 53, 32, 19 and 159 mA g⁻¹, respectively. Table 1 shows that the N content of B600 °C is large. This result indicates that N of the B600 °C can form pyridine- and pyrrolic-type nitrogen-doped atoms. The formed nitrogen-containing structure of the biochar contributes to lithium storage, and improves the specific capacity, based on theoretical calculation. These structural advantages greatly improve the electrochemical performance of B600 °C. Therefore, B600 °C shows promising application potential in energy storage.

3.9

3.9 Pyrolysis gas investigation

The composition and lower heating value (LHV) of bio-gas are analyzed to investigate the application potential of the pyrolysis gas. The gases composition and LHV of bio-gas are presented in the Fig. 8. As shown in Fig. 8a, the bio-gas has high percentage of the CO₂ at 400–500 °C. However, the CO₂ percentage of the bio-gas is decrease with increasing in temperature. This result demonstrates that the generation process of the CO₂ is restrained at high temperature. The CO content of bio-gas is decrease before 500 °C. However, the CO content of bio-gas increases after 500 °C, proving that high temperature contributes to CO generation. Fig. 8a indicates that bio-gas has low H₂ content at low temperature, and high H₂ content at high temperature, indicating that low temperature doesn’t contribute to the production of H₂. The CH₄ content of the bio-gas is decrease after 500 °C with content of 16.02 %. Fig. 8b indicates that the LHV of bio-gas is increase as temperature increases with the maximum LHV of the 12.10 MJ/Nm³. The bio-gas has large LHV, which has promising application potential in industry.

The composition (a) and lower heating value (LHV) (b) of bio-gas produced at 400–600 °C.

4 Conclusion

The biochar is prepared from soybean straw pyrolysis at different pyrolysis temperature, which has large Cd²⁺ adsorption amount. The physicochemical properties such as pore structure and chemical functional groups of the biochar are investigated. The pseudo-second-order model can be used to describe Cd²⁺ adsorption kinetic process. Cd²⁺ adsorption amount is 47.30 mg/g based on Langmuir model calculation. Cd²⁺-π interaction has significantly influenced on Cd²⁺ adsorption process, based on the adsorption mechanism analysis. Biochar has good recyclability, which still has the high Cd²⁺ adsorption capacity after regeneration. The column adsorption analysis results indicate that biochar has the great potential in Cd²⁺ wastewater treatment. Bio-gas obtained from pyrolysis process has large LHV with 12.10 MJ/Nm³. Besides, biochar has the potential of the energy storage with the specific capacity of 132mA g⁻¹.

Funding

The authors would like to express their gratitude to the Specialized Research Fund for the Fundamental Research Program of Shanxi Province(202403021211071), Science and Technology Plan Project of Datong City (2020139), Basic research project of Shanxi Datong University(2022Q36), Natural Science Foundation of Henan Province (232300420298), Panzhihua Directed Science and Technology Planning Projects (2022ZD-G-4), and Scientific Research Fund of Panzhihua University (XJ2022001301) for financial support.

Ethical approval.

Not applicable.

CRediT authorship contribution statement

Chao Lv: Writing – original draft, Investigation, Formal analysis, Conceptualization. Peng Liu: Writing – original draft, Supervision, Funding acquisition, Formal analysis. Song Cheng: Writing – original draft, Funding acquisition, Formal analysis, Data curation, Conceptualization.

Declaration of competing interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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[Google Scholar]
Zhao Y., Feng D., Yu Z., Huang Y., Sun S., . Effect of pyrolysis temperature on char structure and chemical speciation of alkali and alkaline earth metallic species in biochar. Fuel Process. Technol.. 2015;141:54-60.
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Appendix A

Supplementary data

Supplementary data to this article can be found online at https://doi.org/10.1016/j.arabjc.2024.105946.

Appendix A

Supplementary data

The following are the Supplementary data to this article:

Supplementary Data 1

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[Google Scholar]

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[Google Scholar]

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[Google Scholar]

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[Google Scholar]

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[Google Scholar]

Preparation of biochar from pyrolysis of soybean straw at different pyrolysis temperature for cadmium removal from wastewater and pyrolysis gas investigation

Abstract

Keywords

Soybean straw

Pyrolysis

Cd2+

Adsorption

Energy storage

1 Introduction

2 Materials and methods

2.1 Preparation of biochar

2.2 Adsorption experiment

3 Results and discussion

3.1 Physicochemical properties of biochar

3.2 Influence of pH

3.3 Adsorption kinetics

3.4 Adsorption isotherms

3.5 Recyclability of biochar

3.6 Adsorption mechanism

3.7 Column adsorption experiment

3.8 Application biochar in energy storage

3.9 Pyrolysis gas investigation

4 Conclusion

Funding

CRediT authorship contribution statement

Declaration of competing interest

References

Appendix A

Supplementary data

Appendix A

Supplementary data

Supplementary Data 1

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