Extraction and Characterization of Bio-Silica from Sugar ...ijrar.org/download1.php?file=IJRAR19K5557.pdf · Therefore, in this study Sugar Cane Bagasse ash collected from Wonji sugar

© 2019 IJRAR September 2019, Volume 6, Issue 3 www.ijrar.org (E-ISSN 2348-1269, P- ISSN 2349-5138)

IJRAR19K5557 International Journal of Research and Analytical Reviews (IJRAR) www.ijrar.org 609

Extraction and Characterization of Bio-Silica from

Sugar Cane Bagasse Ash of Wonji Sugar Industry,

Ethiopia

1Mengistu Tadesse, 2Enyew Amare, 2H. C. Ananda Murthy, 2Eshetu Bekele*

1Lecturer, 2Assistant Professor, 2Associate Professor, 2Assistant Professor

1Department of Chemical Engineering, Adama Science and Technology University, P O Box 1888, Adama,

Ethiopia

2Department of Applied Chemistry, Adama Science and Technology University, P O Box 1888, Adama, Ethiopia

*Corresponding Author email. [email protected], [email protected]

Abstract: Bio-Silica is a potentially good replacement for commercial silica which is an extensively used

material throughout the world for different purpose. Therefore, in this study Sugar Cane Bagasse ash collected

from Wonji sugar industry, Ethiopia was used for the extraction of Bio-Silica. The Bagasse ash used is a pores

material, with 96.5% of particle less than 75µm in size and its bulk density was 0.026 g/cm3 characterization of

the Bagasse Ash by XRF resulted high SiO2 (71.5%) and Al2O3 (8.16%), while X-ray diffraction(XRD) analysis

showed its amorphous nature. Whereas scanning electron microscopy (SEM) analysis indicated a heterogeneous

and irregular shape of the pores. Moreover, thermal analysis (TGA/DTA) showed weight lost at 100 oC and

521.94 oC which related with loose of physical absorbed water and unburned organic carbon. For the extraction

of bio-silica from Bagasse Ash, Alkaline Fusion Method was used followed by hydrothermal treatment at 90 oC

for 20 h The Bulk density of extracted bio-silica was 0.019 g/cm3. The chemical composition analysis of

extracted Bio-Silica by XRF indicated high percentage of SiO2 (94.27%), and X-ray diffraction indicated

amorphous feature of Bio-Silica. overall the result confirmed that Bagasse Ash is a good source of Bio-Silica

and extraction of Bio-Silica from bagasse Ash using Alkaline Fusion Method followed by hydrothermal treatment

is promising method of recycling this solid waste so that to reduce the current environmental concern related to

dumping of Bagasse Ash in addition to obtaining the valuable Bio-Silica for different purposes.

Keywords: Bagasse Ash, Bio-Silica, Extraction, Alkaline Fusion

1. Introduction

Sugar cane is one of the commonly grown tropical and subtropical crops and is the main sugar crop worldwide.

Global sugar crop acreage is approximately 31.3 million hectares, among which sugar cane accounts for

approximately 70% (Xu et. al, 2019). It is commonly used to produce sugar and ethanol. For instance, sugar

production from sugar cane is one of the most significant economic products for Ethiopia (HVA, 2006). This

sector is expected to contribute a positive impact on the current economy of the country by exporting substantial

quantities of sugar to EU Countries and meeting steadily growing local sugar demand (UNEP and

AFREPREN/FWD, 2006). To meet this national target of the country, the sugar industry is one of the currently

running megaprojects in Ethiopia, in addition to the existing sugar industries (Berhane, 2007). This increasing

number of sugar industries gave rise to new problems related to dumping huge quantities of solid waste

byproduct such as Sugar Cane Bagasse Ash to the environment.

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Sugar cane Bagasse is an abundant fibrous waste product derived from sugar refining industry and readily

available for use with low costs (Ma et al., 2012). It is produced after the extraction of sugar juice from sugar

cane, which is approximately 50% of the sugar cane quality (Xu et. al, 2019). Bagasse is commonly used as a

fuel in cogeneration to produce steam and generate electricity. In this process, sugar cane bagasse ash remains as

the final waste in the sugar production chain. A ton of burnt bagasse may generate 25–40 kg of bagasse ash

(Sales and Lima, 2010). Hence, In China, there may be 1.25–2 million tons of sugar cane bagasse ash produced

each year (Xu et. al, 2019). The estimated quantity of bagasse ash produced from the sugar industries in Ethiopia

may reached up to two million tons per annum (Ethiopian Sugar Corporation, 2016). This ash has negligible

costs and is easily overlooked in landfills, which can significantly cause severe environmental and human health

concerns unless it is properly managed. For instance, inhalation of dust from the disposing of Bagasse ash can

cause the chronic respiratory disease (Thomas et al., 2014). Moreover, improper land disposal of Bagasse ash in

a dry season is vulnerable to wind and increase the quantity of dust in the ambient air (Frias et al., 2011). On the

other hand, with proper design and implementation of recycling technologies the bagasse ash generated can be

used as a substitute for cement or sand in civil construction (Cordeiro et al., 2009), production of glass-ceramic

material (Teixeira et al., 2014), geopolymers (Noorul et al., 2016) and Fe2O3-SiO2 nano-composite to remove Cr

(VI) (Worathanakul et al., 2013). Moreover, it becomes a potential resource of low-cost precursors for the

production of high value-added silica/silicon materials for practical applications (Huabcharoen et al., 2017, Alves

et al., 2017, Xu et. al, 2019). For instance, recent studies indicated, depending on the recoverable Bio-Silica, the

bagasse ash can be used as filler reinforcement in natural rubber, zeolite synthesis, in tooth pastes as a cleansing

agent, as an anticaking agent in salts, in cosmetics, nanoparticles, coating of electronics and optical materials,

chromatograph column packing and so forth (Wang et al., 2016; Patcharin, et al., 2012). Moreover, the bio-silica

of bagasse ash has currently found attractive applications in photonics, sensing, biosensing, filtration,

microfabrication, protein separation, catalysis and drug delivery (Mukda, 2016). However, literatures have

indicated that Bio-Silica composition and consistency of bagasse ash depending on harvest dates and methods,

climatic conditions and sugarcane varieties, amount of cane washing, combustion temperature and duration,

purity of bagasse, ash fineness as well as efficiency of the milling plant which limits the use of bagasse ash as

obtained (Faria et al., 2012; Katare and Madurwar, 2017; Qing et al., 2019; Alves et al., 2017). Hence, it is

necessary to generate information about the bagasse ash composition and its application in different climatic

condition, Sugar cane varieties and processing conditions.

The extraction process of bio-silica from bagasse ash is one outmost factor which affect yield of bio-silica

produced. For instance, Sol-gel synthesis method is one of the conventional methods of silica synthesis from ash

through simultaneous hydrolysis and condensation reaction where a sol of sodium silicate, silicon alkoxide or

halide gels converted into a polymeric network of gel (Sapawe and Hanafi, 2018; Jal et al., 2004). The other

commonly used method of extraction has been pre-treatment with acids such as HCl followed by burning at

various temperatures (Worathanakul et al., 2009). Many researchers followed the procedures where Silica is

digested from ash using caustic soda as sodium silicate and then sulphuric acid to precipitate silica from sodium-

silicate. Finally, the purification and drying produce silica in white amorphous powder form (Costa Crusciol et

al., 2018, Brenda et al., 2016, and Kawu et al., 2013). However, the most commonly agreed method of bio-silica

extraction is still open for discussion among scientists and technologists (Alves et al., 2017). But alkali fusion

followed by precipitation method of extraction of Bio-Silica from biomass is more acceptable to many

researchers as it gave high yield of bio-silica with good quality (Alves et al., 2017 and Thuadaij and Mukda,

2016). Therefore, in this study extraction of bio-silica were made using alkaline fusion method followed by

hydrothermal treatment. Furthermore, the composition, morphology, crystallinity and particle size of the raw

bagasse ash and the extracted Bio-silica were characterized and the results were compared with ASTM standards

(ASTM 412-15a, 2016).

2. Materials and Methods

Instruments and Chemicals

Instruments used in the study includes, X-ray diffractometer (Schmaduze.7000, Korea), Thermal analyzer

(Schmaduze-60H, Korea), SEM(SEM/FIB-model Neon-40, India), digital electrical conductivity probe,

electronic balance, electrical oven, thermometer and a rotary shaker (L.E.D Orbit Shaker), AAS (Spectry-20 plus

Japan), Sieve Armfield CEN-MKII-00-A,pH- meter-pH scan10,Solid sample handling and Solid Mixer-arm field

CEN-MKII-11 UK, Muffle Furnace-AJEON.CO,LTD- Korea, and Magnetic Stirrer-(MS-300HS).




Chemicals used throughout the experiment were analytical grade and includes, Hydrochloric acid (HCl), Sodium

hydroxide (NaOH, 98% lab Reagen), Calcium Chloride dihydrate (CaCl2.2H2O), Magnesium Sulphate Hepta

Hydrate (MgSO4.7H2O), Disodium salt of EDTA, Acetic Acid, Aluminum Oxide (Al2O3), Sodium Carbonate

(Na2CO3) (AviChem industries, Mumbai, India) and Distilled water.

Sample Collection, Preparation and Characterization of Raw Bagasse Ash

The raw bagasse ash was collected from Wonji Sugar Industry, Ethiopia, washed to remove different impurities,

especially salt and organic compounds and sun-dried for 2 days in laboratory. The dried bagasse ash was

powdered, sieved with 75µm mesh and kept in the desiccator for further use. A portion of the raw Bagasse ash

(RBA) was soaked in hydrochloric acid at 60 oC for 24 hrs to change metallic oxide to water soluble metallic

chloride. The metallic chloride solution was filtered, placed in oven at 100 oC, dried, powdered, sieved and

stored in a vacuum desiccator for the extraction of bio-silica (Gupta et al., 2002) (Fig 1). Initial characterization

of the RBA was carried out using XRD, whereas, the compositional analysis of RBA was determined using XRF

and the thermal stability analysis of RBA was made by using TGA/DTG instrument.

Extraction of Bio-Silica from Bagasse Ash

The extraction of Bio-Silica was undertaken using the method described in (Alves, Reis, Rovani, & Fungaro,

2017) and (Thuadaij, 2016), in which bagasse Ash fused with NaOH followed by hydrothermal treatment (Figure

1).

1 g of Bagasse Ash was mixed with 1.3 g of NaOH in capsule and titrated to obtain a homogenized mixture. The

mixture was then calcined at 600 oC for 1h. After cooling to room temperature, the fused product was ground and

mixed with 100 ml distilled water to form suspension. The suspension was stirred for 24 h (120 rpm) at room

temperature and resulting slurry was submitted to hydrothermal treatment at 90 oC for 20 h. The reaction product

was filtered with a quantitative filter paper Whatman No. 41 and the filtered liquid (sodium silicate solution) was

titrated with 3M Acetic Acid until pH reached 7. The resulting gel mixture was aged at 80oC for 1 h. The gel was

washed twice with 100mL of distilled water, filtered (sodium acetate solution), and separated from solid (silica

gel). The silica gel was dried at 135oC for 24h and kept in plastic container for characterization.

Fig. 1. Flow Diagram for Extraction of Bio-Silica from Bagasse Ash

Characterization

Particle Sze and Bulk density determination

Particle size distribution was measured based on the principle of laser diffraction, which is capable of measuring

particle sizes between 20nm and 2000µm according to Malvern Master Sizer Manual in Adama Science and

Technology University, Chemical Engineering Department Mechanical Unit Operation Laboratory Manual

(Ríos-Parada et al., 2017).




Composition Analysis Bagasse ash prepared following the aforementioned procedure was taken into Geological Survey of Ethiopia for

chemical analysis. LIBO2 FUSION, HF attack, gravimetric, colorimeteric and AAS analytical method was used

in order to assess its chemical composition.

X-ray diffraction Analysis

XRD analysis of both Raw Bagasse Ash and extracted Bio-Silica powder samples was conducted using XRD-

7000, Shimadzu, Korea diffractometer with Cu-Kα radiation (40 kV and 100 mA) for phase identification.

Scanning Electron Microscope Analysis

The surface morphology of Raw Bagasse Ash was determined using SEM at scanning rate of 0.06° s−1, and 2θ

range between 5–80° (Nova NanoSEM450, FEI Korea). The sample was applied on carbon tape, and measured

at working distance of 8mm. The sample preparation and analysis were done as per standard operating

procedures of NovaSEM450,FEI SEM whish was operated at 15kv and a current of 10A under 1000X

magnifications (Hegazy et al., 2014).

Thermal Analysis

Thermogravimetric analysis (TGA) was also performed for the Raw Bagasse Ash (RBA), hydrochloric acid

treated (HBA) and extracted Bio-Silica (B-SiO2) with a heating rate of 10 °C min−1, using an SDT 2960

simultaneous DSC–TGA Instruments.

3. Results and Discussion

Particle size and Bulk density of Bagasse Ash and Bio-Silica

Particle size is one of the important factors that play a vital role in recycling of solid waste by converting into

other valuable products like Bio-Silica or for re-using of the waste. According to the standard derived diameter

of spherical particles, out of total shows that the bagasse ash is fine particle in which 96.5% of the particles size

was less than 75μm (Figure 2). This result indicated, the particle size of Bagasse Ash was average and

comparable with previously reported value (Wang et al., 2016; Madu & Lajide, 2013; Sdiri et al., 2014). The

material can be used as an adsorbent due to its large surface area (Madu & Lajide, 2013). Moreover, previous

studies showed a positive correlation between bagasse ash fineness and silica content of the bagasse ash (Xu et.

al, 2019; Jha & Singh, 2017; Bahurudeen et al., 2015).

Fig. 2. Grain size distribution for bagasse ash with 50g total mass.

The bulk density of Bagasse Ash and extracted Bio-Silica were found to be 0.026 g/cm3 and 0.019 g/cm3,

respectively (Table 1). These values are in agreement with the previously reported values ( Alves et al., 2017).

The bulk density of both samples was lower than 1.3 g cm−3, indicated that this industrial byproduct and the

extracted Bio-Silica are classified as lightweight materials (ASTM 412-15a, 2016).

y = 0.0011x + 96.909R² = 0.8034

96.5

97

97.5

98

98.5

99

99.5

0 500 1000 1500 2000 2500

% o

f p

arti

cle

s p

asse

d in

sie

ve a

nal

ysis

Mesh Size




Table 1. Bulk density of Bagasse Ash and Bio-silica

Sample Bulk density

(g/cm3)

Bagasse ash 0.026

Bio-silica 0.019

Chemical Composition Analysis of RBA and Bio-SiO2

The chemical composition of Bagasse Ash and extracted Bio-Silica is shown in Table 2. The major

compositions of Bagasse ash are SiO2 (71.5%) followed by Al2O3 (8.16%) and similarly the extracted bio-silica

comprised of SiO2 (94.27 %) and Al2O3 (1.43 %). Bagasse Ash also contains high amounts of iron oxide and

calcium oxide and very minor quantity of TiO2 and MnO. However, these oxides were extremely reduced in

extracted bio-silica (Table 2). This was a good indicator of the alkaline fusion extraction method is simple and

best method to obtain pure bio-silica from bagasse ash. The Bagasse Ash also contains 1.6% Na and 5.8% K

which will stabilize charges in adsorbent like zeolite framework (Table 2). The observed composition of bagasse

ash with respect to SiO2 is higher than previously reported values (ranged from 58.6-69.2) (Sales and Lima,

2010; Moraes et al., 2016; Ríos-Parada et al., 2017), but lower than the amount reported by Cordeiro and Kurtis

(2017), which is 80.8 in weight percent of bagasse ash. However, the observed values of bagasse ash was

comparable with literature values reported by(Alves et al., 2017) and (Thuadaij, 2016), in which sugarcane

bagasse ash from Buriram, India were used for extraction of Bio-silica for synthesis of zeolite A. Moreover, the

obtained silica content of the bagasse ash (94.3%) is relatively higher than the amount of bio-silica extracted

from sugarcane bagasse ash (92.5%) using Sol-gel method by Sapawe and Hanafi, (2018) and other solid waste

that are considered as a good source of SiO2 such as Portland cement and blast furnace slag as can be inferred

from Figure 3, and its composition is closer to fly ash (Kamoche et al., 2009). Moreover, it is comparable as

compared to the other commonly used biomass source of SiO2 materials such as rice husk ash (90–98%) as

reported by Adam et al. (2006).

Table 2. Chemical Composition of Bagasse Ash and Extracted Bio-SiO2

Composition RBA (wt%) Bio-SiO2

SiO2 71.50 94.27

Al2O3 8.16 1.43

Fe2O3 5.12 0.80

CaO 1.68 <0.01

MgO 1.24 <0.01

Na2O 1.60 0.04

K2O 5.80 1.16

MnO <0.01 0.12

P2O5 0.68 0.18

TiO2 0.34 <0.01

H2O 1.23 1.30

LOI

SiO2 /Al2O3

Na2O /SiO2

3.59

14.9

0.023

1.70




Fig. 3. Ternary diagram of bagasse ash relative to other SiO2 source wastes and material as adopted from da

Silva et al., (2012).

Table 3 shows the comparison of bagasse ash with ASTM C-618 standard for the extraction of bio-silica from

silica source for different application. Based on the result obtained, the raw Bagasse ash under study can be

classified as F-class medium grade according to ASTM C-618. That fulfills the requirement for the extraction of

bio-silica for different applications. It contained lower content of organic carbon and sulfur content than the

standard set by ASTM C-618. For instance, fly ash which is exhibiting a relatively similar chemical composition

has been used as an admixture in concrete making. So that the bagasse ash can also be used as a source of bio-

silica for the same application after thorough investigation and material standardization.

Table 3. RBA comparison and standardization for extraction of bio-Silica

Properties BA % ASTM C618 requirement %

SiO2+Al2O3+ Fe2O3 84.78 70 (minimum)

SO3 - 5 (maximum)

LOI 3.59 6 (maximum)

X-ray diffraction Analysis

XRD analysis of RBA, HBA and B-SiO2 indicated the amorphous nature of the samples with low content of

inorganic constituents (Figure 4). There was a significant change in the diffraction pattern of the XRD of RBA

and HBA which may be due to the conversion of metallic oxides into the soluble chloride form of the metals

(citation???). However, insignificant peaks differences were observed in B-SiO2 as compared to the RBA. The

changes observed under acid treatment might be due to the formation of crystalline materials. Similarly early

reported findings for sugarcane waste showed when an organic material with a high percentage of silicon is

burned, it can generate amorphous or crystalline silica depending on the time and temperature conditions; for

instance high temperatures (800−1000 °C) generate crystalline silica (Le Blond et al., 2010)., In which the

amorphous silica present in Bagasse Ash is converted to crystalline silica,polymorphs, such as quartz, cristobalite

and tridymite at a temperature greater than 800 oC, while quartz in a crystalline form is formed in the case of

RBA(Figure 4).




Fig. 4. XRD diffraction patterns for raw Bagasse Ash (RBA), HCl treated Bagasse Ash (HBD) and

Extracted Bio-silica (B-SiO2).

The obtained values are matched well with literature result reported previously (Nyankson et al., 2018; Le

Blond et al., 2010). The crystalline phase of silica is one of the reasons for the peaks of quartz and mullite around

26 for RBA and HBA is due to presence of SiO2 components in both quartz and mullite crystals(Treacy &

Higgins, 2007).

SEM Analysis SEM analysis of bagasse ash was performed after treated by hydrochloric acid (Figure 5). Shape and the pore

size on surface of bagasse ash were not uniform but heterogeneous and irregular in shape. In particular, the larger

sized pores were rough with a lot of cracks which indicated binding site. This was a good indicator of the

development of surface porosity and readiness of the waste to interact with other material after acid treatment.

Moreover, the morphology of the bagasse ash observed in the study is similar with previously reported values

(Fungaro et al., 2014). Sizes between 5 and 500 μm and a high roughness were observed in the SEM image of

HBA (Figure 5), which are associated with the release of organic matter during the digestion process with HCl.

The morphologies obtained from the HBA sample are similar to those observed by Faria et al.(2012).




Fig. 5. SEM image of acid treated Bagasse Ash(HBA)

Thermal Analysis

Figure 6 displays the thermogravimetric and differential thermal curves for RBA, HBA and B-SiO2. The

thermogram of HBA presented a weight loss up to 100 oC which corresponds to the loss of physically adsorbed

water from the surface and the second step (521.94∘C) was related to the loss of the unburnt organic structure.

Similarly for sample without acid treatment mass loss was described 370.16 oC and 460.15oC that is related to

the loss of physically adsorbed water from the surface (García et al., 2015; Sales & Lima, 2010) and the

exothermic peak at 500 oC (DTA) reveals the existence of organic residues. Thus, the treatment up to 550 oC

removes all undesired organic compounds to extract the bio-silica from bagasse ash. These results are in good

agreement with report of ( Alves et al., 2017).

a)




Fig. 6. Thermal analysis of raw bagasse ash (RBA), acid treated (HBA), and extracted (B-SiO2) Bagasse

Ash: a) Thermogravimetric analysis (TGA) and b) differential (DTA).

Conclusion

This work explored the economical way of extraction of bio-silica from bagasse ash from sugar industries.

Moreover, the study confirmed, the Bagasse ash of Wonji sugar industry waste is rich in SiO2 and an important

precursor for bio-silica for further applications. Micrograph characterization results showed that acid treated

bagasse ash was porous, heterogeneous and irregular shape material. Overall, this study confirms that the

Bagasse Ash of sugar industries is a good source of pure amorphous Bio-Silica which can economically

extracted using Alkaline Fusion Method followed by hydrothermal treatment.

Acknowledgements We acknowledge Adama Science and Technology University for supporting this project, as well as Wonji

Sugar Factory for providing the bagasse Ash sample.

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