Effect of Fe3O4 coated bacterial consortium IQMJ-5 on the desulfurization of the organosulfur portion of Pakistani coal and its chemical characteristics

doi:10.21203/rs.3.rs-2960716/v1

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Effect of Fe3O4 coated bacterial consortium IQMJ-5 on the desulfurization of the organosulfur portion of Pakistani coal and its chemical characteristics

https://doi.org/10.21203/rs.3.rs-2960716/v1

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Coal is an abundant and inexpensive source of energy with immense application in different industrial sectors. However, its extensive utilization has resulted in several kinds of sulfur-related environmental issues. To tackle such issues, indigenously isolated Fe₃O₄-coated bacterial consortium IQMJ-5 cells were applied for the desulfurization of a Pakistani coal. The coated cells were allowed to desulfurize the coal in a shake flask experiment. To assess the desulfurization capabilities, both the pre- and post-desulfurized coal were characterized by different chemical and analytical techniques. The total sulfur content identified in the coal sample was about 4.50%. The results of the analysis showed that after treatment an increase in the carbon content and heating value of the coal sample was detected. Moreover, an amount of about 54.46% and 66.6% of organic and total sulfur, respectively were removed after biodesulfurization. The obtained results clearly suggest that the consortium can be a potential candidate for reducing sulfur-related environmental pollutants of fossil fuels at a more advanced commercial scale.

Biodesulfurization

Coal

Consortium

Iron oxide Nanoparticles

Coal is globally known as the low-cost and most abundant fossil fuel source of energy with extensive industrial, domestic, and other commercial applications (Rehman et al., 2021). It is physically and chemically defined as a combustible and heterogeneous sedimentary rock made of both organic and inorganic constituents. Inorganically, coal contains different kinds of ash-forming substances, dispersed in the coal matrix. On the other hand, the organic part is made of carbon, hydrogen, and oxygen, with a smaller amount of nitrogen and sulfur (Adekola et al., 2012). It is currently fulfilling about 30% and 42% of the global energy and electricity requirements, respectively, and is still predicted to perfume an active role in the fulfillment of the global energy requirement for the upcoming 2 to 3 decades (Xia et al., 2015).

However, its extensive utilization for electricity generation as well as for other industrial purposes has caused several environmental problems (Santelli et al., 2008). Specifically, the sulfur released during the combustion of coal combines with oxygen in the atmosphere and generates sulfur dioxide, causing ash creation, acid rain, and air pollution (Li et al., 2022).

The amount of sulfur in different types of coal varies significantly and, in most coal, the amount usually falls in between 0.5–5% (Chou, 2012). The sulfur in coal mostly exists in inorganic and organic forms. The inorganic form is differentiated into pyritic and sulfate forms, both of which exist as mineral matter in coal. The organic sulfur is bonded to the macromolecular structure of coal by means of a covalent bond between C-S atoms. The presence of such a covalent bonding is responsible for the difficulty in the removal of the organosulfur portion of coal. This property has made it difficult for researchers to directly identify and quantify the organic sulfur of coal (Zhang et al., 2016).

To address the sulfur-related environmental issue, many researchers have contributed significantly to the field of greener forms of energy (Tahir et al., 2018) but coal still remains the backbone of energy in most parts of the world. Another useful strategy for protecting the quality of urban air is to limit and ban the excessive use of coal and its goods. However, this strategy also failed in gaining wide acceptance as it merely serves as a temporary solution (Liu et al., 2020). Thus, to have coal with little or zero sulfur level, the presence of a technique with the capability of removing sulfur and must be cost-effective is a need of time (Etemadifar et al., 2014). Therefore, desulfurization emerges as the preferred strategy for the reduction or complete removal of sulfur moieties from coal. Currently, three different strategies such as physical, chemical, and biological are available for the desulfurization of coal.

The physical and physicochemical techniques employ rigorous grinding of coal and remained successful in the removal of only pyritic forms of sulfur. However, such practices can reduce the productivity of coal (Cardona & Marquez, 2009). On the other hand, chemical techniques can reduce the amount of both organic and inorganic sulfur in coal. However, such techniques have several limitations including the expensive operating condition, can alter the structural integrity of coal, and results in the production of harmful byproducts (Aytar et al., 2008). Biological desulfurization involving microorganisms has gained much attention as an alternative and eco-friendly technique. The desulfurization of coal by microbial means is more advantageous than all of the above-said techniques (Handayani et al., 2016). Biodesulfurization (BDS) is a relatively novel technology operating at ambient environmental conditions along with the minimum release of unwanted by-products. Therefore, BDS is regarded as a promising technology for lowering the amount of sulfur in coal along with a minimum impact on the quality of the environment (Kumar et al., 2018).

Previously, our research team isolated a DBT desulfurizing bacterial consortium IQMJ-5 and optimized its environmental parameters (Khan et al., 2022a). Further, the consortium was immobilized with magnetic iron oxide (Fe₃O₄) nanoparticles and has exhibited promising results (Khan et al., 2022b). Thus, in the present research work, the Fe₃O₄-coated consortial cells were employed for the desulfurization of organosulfur moieties of Pakistan coal. The BDS potential of the consortium was assessed by conducting different chemical analyses before and after the biotreatment. The desulfurization was further evaluated through XRD, FTIR, and SEM/EDS analyses.

Microbes, Media, and growth conditions

The bacterial consortium IQMJ-5 used in the present research study was previously isolated from the hydrocarbon-contaminated soil sample in the Environmental Microbiology Lab, Department of Microbiology, Faculty of Biological Sciences, Quaid I Azam University, Islamabad, Pakistan (Khan et al., 2023). The isolated consortium was preserved in 50% glycerol and subsequently stockpiled in a -20 ^ºC freezer. Minimal Salt Medium (MSM) lacking a sulfur source, was sterilized by autoclave for 15 minutes at 121°C and 15 psi pressure and employed for the desulfurization experimentation. MSM per liter of distilled water contained different components including 1M phosphate buffer (2.65 g: KH₂PO₄ and 4.33 g + Na₂HPO₄, 0.525 g and pH 7.2): NH₄Cl, 0.203 g: MgCl₂.6H₂O, 0.022 g: CaCl₂.2H₂O, 0.005 g: yeast extract, and 2g: glycerol as carbon source.

Coal sample

The coal sample was collected randomly by hand from Cherat coal mines located in the Khyber Pakhtunkhwa province of Pakistan. The sample needed for different types of chemical analysis and desulfurization experimentation was initially air-dried and subsequently grounded and sieved for a size of about 250 µm. The inherent moisture present in coal was removed by placing the sample in a desiccator at 40°C for 4 h.

Characterization of Coal sample

The proximate analysis is used to find out the content of moisture, volatile matter, fixed carbon, and ash content in a coal sample. This analysis combines different types of ASTM standards including 3173, 3174, and 3175 applied for the determination of moisture, ash content, and volatile matter, respectively. Whereas the amount of fixed carbon was determined by subtracting the sum of the above three from that of the initially weighted percentage of the coal sample. The chemical characterization of the raw, de-pyritized, and biotreated coal was conducted with Scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS) analysis. The calorific value was determined by an Oxygen bomb analyzer.

De-pyritization of Coal

About six grams of coal sample was de-pyritized in a mixture of nitric acid (HNO₃) and distilled water (15% HNO₃). The slurry was stirred continuously at about 120 rpm for 5 h in a shaker incubator. The slurry was next separated by filtering through filter paper and washed with distilled water until the filtrate achieved neutral status. The filtrate was dried at 40 ˚C for 4 h and stored for future experimentation.

BDS of Coal

A lab-scale shake flask experiment was designed to find out the desulfurization capability of the bacterial consortium IQMJ-5. The experiment was performed in 250 ml Erlenmeyer flasks having about 150 mL MSM media. About 4% of the coal sample (w/v) with a particle size of 250 µm (60 mesh) was initially sterilized in a laminar flow hood under ultraviolet (UV) light. The UV sterilization procedure was performed to preserve the physicochemical properties of coal. An inoculum of 1% (v/v) was added in the medium and the desulfurization experiment was carried out for about 14 days in a shaker incubator at 25 ˚C with 100 rpm rotational speed. After completion of the experiment, the mixture was filtered and rinsed with distilled water to make the sample free of cells. The biotreated coal was dried in a desiccator at 40 ˚C for 4 h for further analysis.

XRD analysis

X-ray diffraction (XRD) analysis was conducted to find out the mineralogical constituents of the de-pyritized and biotreated coal samples. The measurements were performed with an X-ray diffractometer (D8 advance, Bruker X-ray Diffractometer, Germany) with Cu Ka (1.5406) radiation in the 2θ range and 4^°/min scanning range. The initial angle of the diffraction data for the sample was set at 10^° and the end angle at 70^°.

FTIR analysis

The changes in the functional groups of the coal samples (both de-pyritized and biotreated coal samples) were analyzed with an FTIR spectrophotometer (Perkin Elmer). A ratio of 1:100 ofcoal samples and potassium bromide (KBr) were mixed and grounded in a mortar under pressure for a certain period. The overall number of scans taken was 20 with a 4 cm^− 1 spectral resolution and the changes in the functional groups were observed in the spectral region of 400–4000 cm^− 1.

Characterization of Coal after BDS

The variation in different properties of the coal samples (raw, de-pyritized, and biotreated) was investigated and are shown in the Table. 1. The results showed that the fixed carbon content of the coal greatly increased from 56.48 to 64.33% after biotreatment. A similar increase in the ash content of the coal was also reported after BDS treatment. The results further indicated that after biotreatment with the consortium IQMJ-5, an increase of about 643.31 kcal/kg in the calorific value of the coal sample was experienced.

Table 1

Different Characterization of the coal sample
Proximate analysis %	Raw	De-pyritized	Treated
Moisture	1.496	1.297	1.402
Volatile matter	14.03	15.736	16.180
Fixed carbon	56.48	58.062	64.33
Ash content	27.962	24.875	17.684
Chemical characterization %
C	69.29	76.855	81.90
O	13.89	12.54	11.706
S	4.5	3.305	1.505
Al	2.75	1.49	1.58
Si	3.458	2.245	2.4775
K	0.649	0.285	0.434
Fe	5.461	3.273	0.255
Heating value (kcal/kg)
	6272.23 kcal/kg	6778.32 kcal/kg	7421.63 kcal/kg

XRD analysis of the Coal sample

Figure 1. Indicated the XRD spectra of the de-pyritized and biotreated coal samples. The results in the figure detected peaks in the XRD spectra of de-pyritized coal samples representing different types of minerals including Kaolinite [Al₂Si₂O₅(OH)₄)], jarosite (Fe₃(SO₄)₂(OH)₆, Illite, quartz (SiO₂), gypsum (CaSO₄.2H₂O), and calcite (CaCO₃), along with the inorganic sulfur-containing minerals like melanterite (FeSO₄.6H₂O) and rozenite (FeSO₄.4H₂O) (Fig. 1). After BDS, a peak of melanterite at a 2θ value of 16.08^° was completely removed whereas peaks corresponding to rozenite present at a 2θ value of 42.62^° and 58.52^° were greatly reduced. A peak of melanterite at a 2θ value of 50.67^° was replaced by rozenite [Fig. 1. (right)]

FTIR analysis

The results of the FTIR spectral analysis of both de-pyritized and biotreated samples of coal are shown in Fig. 2. The results indicated several peaks at wavenumber 588.86, 595.73, and 612.66 cm^− 1 in the biotreated coal sample that corresponds to SO₄ functional group thereby confirming the BDS of organosulfur constituents of coal.

In addition, the emergence of a peak at wavenumber 1518.42 cm^− 1 in the biotreated sample was a distinction of the C = C functional group which displays an increase in the concentration of carbon.

SEM/EDS analysis

EDS analysis of the coal was conducted before and after BDS and is shown in Fig. 3. The results exhibited that the peak corresponding to the sulfur atom was significantly reduced in the biotreated sample relative to that of the de-pyritized sample. In addition, the results of the chemical analysis in Table. 2. confirmed that the consortium remained successful in removing about 54.46% of the organic sulfur in coal.

Table 2

EDS results of 4 spectra of the coal sample showing sulfur removal rate
K coal sample	Weight of sulfur (in %)
K coal sample	De-pyritized coal	Biotreated coal
Spectrum 1	3.10	1.46
Spectrum 2	3.53	1.74
Spectrum 3	3.08	1.44
Spectrum 4	3.51	1.38
Total	13.22	6.02
Average	3.305	1.505
% Removed after analysis		54.46%

The removal rate of total, pyritic, and organic Sulfur

The percent by weight removal of total sulfur (S_t), pyritic sulfur (S_p), and organic sulfur (S_o) after de-pyritization and BDS has been revealed in Table. 3. The results indicated that after the de-pyritization step, about 100% of Sp and 26.7% of S_t were removed. On the other hand, after BDS about 54.46% and 66.6% of S_o and St, respectively were removed.

Table 3

The percent by weight of total (S_t), pyritic (S_p), and organic sulfur (S_o) removal
K coal forms (in %age)	S_t	S_p	S_o	% Desulfurization
Raw coal	4.50	1.2	3.305	----
After de-pyritization with HNO3	3.305	0.0	3.305	26.7% S_t, 100% S_p, 0% S_o
After biodesulfurization	1.505	0.0	1.505	66.6% S_o, 0.0% S_p, 54.46% S_o,

Up till now, the different kinds of BDS technologies failed in achieving a substantial reduction in the organosulfur content of coal while minimally affecting its carbon skeleton (Marinov et al., 2010). BDS is reported to be affecting not only the sulfur functionalities but also the organic matrix in coal (Gonsalvesh et al., 2013). This has ultimately resulted in the reduction of the other useful characteristics of coal, an undesirable property of the BDS process (Mishra et al., 2014). In the present research study,the Fe₃O₄-coated consortial cells were applied for the BDS of a high organosulfur-containing cherat coal sample. The consortium remained successful in achieving a significant reduction of about 66.6% of the total sulfur from the coal sample.

Similarly, the consortium remained effective in the desulfurization of about 54.46% of the organic sulfur content of coal. Previously, different researchers have contributed significantly to the field of BDS harnessing different types of bacterial and fungal strains. Singh et al., (2012) have examined the desulfurization of Indian and Indonesian coals with bacterial strains such as Pseudoxanthomonas sp and Ralstonia sp. After biotreatment, about 34.16% and 20.22% of the total sulfur in Indonesian coal was removed by Pseudoxanthomonas sp and Ralstonia sp, respectively. Whereas, about 41.84% and 45.5% of the total sulfur in Vastan lignite of Gujarat (India) were removed by the respective bacterial strains. Etemadzadeh et al., (2016) have used a newly isolated bacterial specie Fusarium oxysporum FE in their desulfurization studies. They remained successful in achieving about 34.21% of total sulfur removal from coal collected in Isfahan. In yet another study, Liu et al., (2017a) used two types of bacterial species such as Acidithiobacillus ferroxidans and Pseudomonas sp NP22 isolated from native coal mine sites for the desulfurization of low-quality lignite coal. A maximum amount of 56% of the organic sulfur and 46% of total sulfur were removed with Pseudomonas sp NP22 bacterial strain.

Aytar et al., (2014) used the fungal strain Alternariasp.CF1 to desulfurize a higher amount of sulfur and ash containing low-grade lignite. After BDS about 38% and 52% of the organic sulfur and total sulfur, respectively were removed when incubated for about 12 days. In yet another fungal-mediated desulfurization study, about 47% of total sulfur removal was obtained from Yihai coal with Aspergillus sp. DP06 (Liu et al., 2017b). In comparison to the aforementioned studies, a multifold increase in desulfurization activities has been achieved under ambient environmental conditions in the present study. The higher desulfurization activity of the consortium could be attributed to the genetic makeup, better adaptation ability, effective membrane transportation potential, and well-established 4S pathway. Therefore, it could be interesting to know that the consortium presents an excellent commercial potential for the desulfurization of coal and making energy production more sustainable and greener.

Both the pre- and post-biotreated coal samples were further analyzed for different types of chemical characteristics. These analyses have shown that the BDS treatment resulted in the alteration of the chemical characteristics of coal assuming a possible occurrence of an association between the BDS and the chemical characteristics of coal. The BDS process resulted in an increase in the amount of fixed carbon and a decrease in the ash content of the coal sample. The decrease in ash content was assumed to have resulted from the bacterial action of dissolving several types of coal minerals. Such reduction in ash content is regarded advantageous from the environmental point of view mainly due to the lower production of heavy metals. As a result of the biotreatment of coal with the consortium IQMJ-5, not only the organic sulfur fraction of coal was reduced but also many of the unwanted or noxious metals present in the coal samples were also altered positively. The results obtained in the present research work are greatly in accordance with that of the studies conducted previously (Acharya et al., 2004; Kumar et al., 2018, 2019; Yang et al., 2016). The ultimate analysis was conducted to find out the percentage by weight of different elements such as carbon, oxygen, hydrogen, sulfur, and nitrogen in coal samples. Such findings are valuable in determining the amount of air needed for combustion (Kavsek et al., 2013). The results of the ultimate analysis indicated that an increase in the concentration of carbon and oxygen was detected in the biotreated coal samples, and such findings were in accordance with the previous results reported by Kumar et al., (2019).

Similarly, the calorific or heating value of coal is also a significant factor when the combustion properties of the coal are considered. In most cases, after microbial treatment, the calorific value of coal decreases due to the loss of some parts of the carbon resulting from the cleavage of the bond between carbon atoms (Li et al., 2010). However, in the present research work, an increasing trend in the calorific value of the biotreated coal sample was recorded. An increasing value of about 643.31 kcal/kg was detected after the BDS of the coal sample. The possible reason for such an increase is the additional enrichment of the coal with organic matter that has probably stemmed from a decrease in the amount of mineral matter. Previously, Aytar et al., (2008) experienced a decrease in theconcentration of sulfur and several other mineral matters after the BDS process. This in turn has made the coal highly concentrated by increasing the organic matter content and thus resulted in a higher calorific value. In another study, Liu et al., (2017a) gained an increased value of about 187 cal/g in the calorific value of coal after BDS with Pseudomonas sp. NP22, an amount much lower than obtained with that of IQMJ-5 bacterial consortium in the present research study.On the other hand, Akhtar et al., (2016) have used the bacterium Rhodococcus spp. Eu-32 and obtained a conserved amount of calorific value after biotreatment.

The indigenously isolated consortium IQMJ-5 was for the first time employed to desulfurizea coal sample collected from cherat coal mines located in Khyber Pakhtunkhwa province of Pakistan. The consortium showed promising desulfurizing results by removing about 66.6% of the total sulfur and about54.46% of the organic sulfur fromthe coal sample. The sulfur reduction rate was also detected in the results of FTIR and XRD analysis. The different types of chemical characteristics like fixed carbon, the concentration of elemental carbon, and the calorific values of the coal sample were increased after biotreatment. Similarly, a decreasing pattern in the ash content was detected. From the promising results of all the above analysis, it can be concluded that the indigenously isolated bacterial consortium IQMJ-5 is the most suitable candidate to accomplish the BDS of coal at the pilot scale or more advanced commercial scale.

Acknowledgment

The author acknowledges the support offered by the Higher Education Commission of Pakistan for providing a Ph.D. fellowship named “MS Leading to Ph.D. under Aghaz-e-Haqooq-e-Baluchistan Package”. The authors are also thankful to the Higher Education Commission of Pakistan for providing the funding facility under the research project titled “ National Research Program for university (NRPU) with project ID 4568.

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Effect of Fe3O4 coated bacterial consortium IQMJ-5 on the desulfurization of the organosulfur portion of Pakistani coal and its chemical characteristics

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Abstract

Figures

Introduction

Material and Methods

Microbes, Media, and growth conditions

Coal sample

Characterization of Coal sample

De-pyritization of Coal

BDS of Coal

XRD analysis

FTIR analysis

Results

Characterization of Coal after BDS

XRD analysis of the Coal sample

FTIR analysis

SEM/EDS analysis

The removal rate of total, pyritic, and organic Sulfur

Discussion

Conclusion

Declarations

Acknowledgment

References

Additional Declarations

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