Volume 8, Issue 2, February – 2023 International Journal of Innovative Science and Research Technology

ISSN No:-2456-2165

Rice Husk Ash Extraction with Organic Acid

Leaching as the Pra-Treatment of Green Silica
Production for Sustainable Industry Purpose
Aulia Cahyani
Master Program of Chemical Engineering
Faculty of Engineering, Diponegoro University Semarang, Indonesia

Abstract:- Rice production in Indonesia has increased chemically, and thermochemically6. In general, the silica
in the last 3 years. This condition resulted an increase in separation process consists of removing inorganic
rice husk production as one of kind of its by-product. compounds (metal impurities) K, Ca, Na, Al, Mg, and Mn,
The high silica content encourages the potential of rice followed by the removal of organic compounds such as
husk to become the raw material for green silica cellulose, hemicellulose, and lignin contained in rice husks
production. The utilization of rice husk to produce silica [2].
can shift the production of commercial silica (TEOS
and LUDOX) due to the low cost of raw material, Rice husks treated with acid leaching produced the
production costs, and of couse- energy consumption. final silica purity of 92-93%. However, rice husk has a stiff
Treatments of different kind of organic acid (C4H6O6 texture, so in the acid leaching process, the acid solution is
and CH3COOH), variation of temperature (28oC, 75oC) challenging to diffuse to the inner layer of the husk, and the
in duration of process (1h, 2h) in acid leaching was operation process can only be carried out under certain
applied in this study. The parameters on this study are conditions. In the study by Steven, S. et al.,[3] it was
acid concentration and aging time on precipitation. The shown that soaking rice husks requires operating conditions
experimental result shows that the use of C4H6O6 and at a temperature of 200oC, a pressure of 6-8 bar, and
CH3COOH has been shown to reduce the levels of metal vigorous stirring to break up rice husk particles and bring
impurities, producing green-silica with 92.21% purity impurities out. While the structure of rice husk ash is more
on the best silica product (C4H6O6,28oC,2h) with an brittle, so the acid solution quickly diffuses, and acid
amorphous phase of 61,26%, increasing surface area leaching can be carried out at atmospheric pressure and low
and pore volume of silica to reach 154,570 m2/g and temperature9. Acid leaching carried out on rice husk ash
44,2513 cm3/g. The high silica yield was reached at produced silica purity up to 96.44% [3].
99,26%. The highest adsoption capacity of 756,4 mg/g,
824 mg/g, and 824 mg/g meet the quality standart of There is still metal impurity content which is one of
SNI no. 06-2477-1991 for silica product with good the factors for the low purity of silica products [4]. The
adsoption quality. The main analysis process using acid leaching treatment has attracted attention for its ability
Scanning Electron Microscopy with Energy Dispersive to remove mineral impurities and increase the purity of
X-Ray Spectroscopy (SEM-EDX), X-Ray Diffraction silica products [5]. However, the application of acid
(XRD), and Brunauer Emmet Teller-Surface Area leaching is generally still using strong acids such as nitric
Analyzer (BET-SAA). The obtained result suggest that acid (HNO3), sulfuric acid (H2SO4), and hydrochloric acid
appliying organic acid leaching unsing C4H6O6 can (HCl) [6]. This inorganic acid is commonly used as a metal
reduce impurities on silica product, producing component remover during the silica production process
mesopore-sized amorphous green silica with good [7]. However, the application of solid and hazardous
adsorption qualities an an alternative hazardous to chemicals can cause side effects on the human body and
good material in the implementation of environmentally the environment in the long-term production design [8].
friendly chemical on micro-scale cleaner production. The characteristics of organic acids, which have low
Keywords:- Acetic acid, Green silica, Impurities, Organic molecular weight, have potential as metal chelating agents.
acid leaching, Tartaric acid. Tartaric acid (C4H6O6) is an environmentally friendly
organic acid [9]. C4H6O6 not only functions as a
I. INTRODUCTION precipitating agent but also as a metal chelating agent [10].
At the same time, acetic acide (CH3COOH) is one type of
There have been many studies state that rice husk ash organic acid that can form complex bonds with several
contains a range of 88-95% silica content. With the metal ions [11]. Studies on carboxylic acid as a metal
combustion treatment, it was found that 94.95% silica complexing agent with tartaric acid as a chelating agent are
content in rice husks was found4. In another study, it was still minimal. Replacing the use of hazardous materials
shown that it was possible to isolate 93.67% of silica from with less hazardous materials is the implementation of
rice husks [1]. environmentally friendly chemistry in micro-scale cleaner
production. Thus, this study was conducted to analyze the
The technique of extracting silica from its source in effectiveness of organic acids as environmentally friendly
the form of rice husks can be carried out by various additives and is expected to be an alternative to dangerous
separation methods, such as hydrothermally, biologically, strong acids in producing high purity low-impurity silica

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ISSN No:-2456-2165
from rice husk biomass. The experiment was conducted erlenmeyer, glass funnel, aluminium foil, hot plate, stirrer,
using the acid leaching treatment using 1 mol/L of tartaric pH indicator paper. The results of this study were analyzed
acid (C4H6O6) and 1 mol/L of carboxylic acid in the form using a Scanning Electron Microscope-Energy Dispersive
of acetic acid (CH3COOH). There are variations in X-Ray (SEM-EDX) JEOL JSM-6510LA, X-Ray
temperature and duration of the acid leaching process, Diffraction (XRD) SHIMADZU XRD-7000 at UPT
namely at conditions T = 28oC, 75oC, and t=1 and 2 hours. Laboratorium Terpadu, Universitas Diponegoro, Semarang,
The best operating conditions for acid leaching to produce and Brunauer Emmet Teller-Surface Area Analyzer (BET-
high-purity green silica products from rice husks have been SAA) Quantrachrome Nova 1300E at UPT Laboratorium
studied. In addition, a thermal process is carried out ashing Terpadu UPN Veteran Yogyakarta. The location of the
the raw material of rice husks in a muffle furnace under research was carried out at Laboratorium Dasar Teknik
high-temperature conditions. Na2SiO3 was obtained from Kimia, Universitas Diponegoro.
soaking rice husk ash (RHA) in 1 mol/L of alkaline NaOH
solution. Green silica products were analyzed using SEM- B. Parameter, Variations and Experimental Procedures
EDX, XRD, and BET-SAA to determine green silica The green silica is produced at several stages of the
surface morphology, crystallinity level, and pore process. The first stage is the preparation of rice husk raw
characteristics. materials. Fresh rice husks are washed using running
demineralized water to remove small particles such as
II. EXPERIMENTAL METHOD gravel that are carried along with rice husks. Next, the rice
husks were dried using a drying oven at 80oC for 6-8 hours.
A. Experimental Materials and Equipments The dried husks then entered the second stage, the
Materials involved in this research include fresh rice calcination/ashing process, using a muffle furnace at a
husks obtained from Penggilingan Padi dan Beras UD temperature of 700oC for 2 hours. The calcination results in
Maju Makmur, Trucuk, Klaten, Indonesia, were then black rice husk ash referred to as Rice Husk Ash (RHA).
washed and dried in an oven at 80oC for 6-8 hours. The The RHA particle size was reduced by using mortar-pestle.
demineralized water was obtained from CV. Indrasari, Some of the RHA entered the analysis stage as a control
Semarang, Indonesia, was used without further purification. sample. The data on the characteristics of the raw materials
1 mol/L C4H6O6 solution was prepared by dissolving were obtained. 10 grams of RHA were put into a beaker
75.043 grams of C4H6O6 per 500 mL of distilled water. 1 glass, then added 100 mL of 1 mol/L C4H6O6 solution and
mol/L glacial CH3COOH solution was obtained by diluting stirrer to enter the acid leaching stage. The solution was
60 mL concentrated CH3COOH into 1000 mL of distilled then heated on a hot plate at 75oC for 1 hour with a stirring
water. 1 mol/L NaOH was obtained by dissolving 40 grams speed of 500 rpm. Do the same for the acetic acid solution
of NaOH per 1000 mL of distilled water. All chemicals (CH3COOH) and other variations in temperature and
used have a pro-analyst grade level. duration of the process. The variation of acid leaching
temperature is 28oC and 75oC and the variation of acid
The equipment used in this experiment includes oven leaching duration is 1 and 2 hours .
(WTB 9010-0333 ED-56), muffle furnace (WISETHERM
F-03), digital balance, mortar-pestle, glass beaker,

Fig. 1: Green Silica Production Process Flowchart [13] [14][15][16]

f

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ISSN No:-2456-2165
The RHA solution then entered the first filtration important part to analys for some kind of adsorben product
stage, where the acid solution was separated from the RHA such silica.
residue with 10x10 cm fine filter paper. The dissolved
residue was then rinsed with demineralized water at III. RESULT AND DISCUSSION
T=80oC. RHA enters the alkaline extraction stage by being
contacted with 200 mL of 1 mol/L NaOH solution into a A. Potential Uses of C4H6O6 and CH3COOH in Green
500 mL erlenmeyer. The mixture was heated at 120oC for 2 silica Synthesis
hours with a stirring speed of 500 rpm. This is the process Impurities chelating process has an essential role in the
of forming sodium silicate (NaSiO3). The solution then production of green silica. Organic acids are non- corrosive
goes to filtration step 2 to separate the sodium silicate and more environmentally friendly. Acid leaching
formed from the RHA. The following process is the treatment with organic acids as chelating agents can reduce
precipitation of sodium silicate with an acid solution. 90 the levels of another elements than silicon, such as: Ca, Ni,
mL of NaSiO3 solution was given 1 mol/L C4H6O6 solution K, Mn, Fe, and Zn [17]. From its toxic properties, the
drop by drop until a clear precipitate was formed in silica application of organic acids is more efficient because they
hydrogel and stopped when pH=7. Test the acidity level of have lower toxic properties compared to mineral acids such
the sample with pH indicator paper. The silica gel was then as hydrochloric acid, sulfuric acid, and nitric acid [18].
rinsed with demineralized water at 80oC and then dried in C4H6O6 with the bond structure
an oven at 105oC for 6 hours. The flow of the green silica HOOC(CHOH)2COOH not only as a precipitating agent
production process can be seen in Fig. 1., use mortar-pestle but also as a chelating agent16. C4H6O6 contains a carboxyl
to reduce the silica particle size. The silica product is then group and a hydroxyl group that can act as a binding agent
weighed and ready to enter the product analysis stage. The for metal elements. C4H6O6 can potentially reduce the
silica product from this study was carried out in several levels of Cu2+ in the sample [8], chelating elements Fe2+
stages of analysis. The morphology and shape of the [9], and Fe3+ contained in water [19]. This is ecident from
surface of the silica particles were analyzed using the the experimental results of acid leaching using C4H6O6 at
principle of atomic bombardment using a Scanning an operating temperature of 28oC for 2 hours can reduce Cu
Electron Microscope (SEM). The percentage and levels from 1,53% to 0,06% and Al from 1,02% to 0,16%
identification of chemical compounds in the product were thereby reducing the formation of CuO and Al 2O3
determined through an Energy Dispersive X-Ray (EDX) compounds in green silica products (see Table 1.). The
analysis, and the crystallinity level of silica was analyzed application of C4H6O6 in acid leaching under these
by X-Ray Diffraction (XRD) using data interpretation of operating conditions has been shown to reduce the levels of
Match!3, the volume of adsorption isotherms and specific several metal elements, which can automatically increase
surface area of silica particles were evaluated by the the percentage of green silica purity obtained, which
Brunauer Emmet Teller (BET) and Barret Joyner Halenda reaches 92,21%, thus making the temperature of 28oC for 2
(BJH) method using the nitrogen gas adsorption principle, hours significantly the best condition of 1 mol/L solution of
with the degassing process under vacuum at 280oC for 180 C4H6O6 to increase the purity of green silica.
minutes. Data of characteristics pore can shown how the
porosity quality of green silica. Porosity become the

Chemical Components (% mass)

Compound CH3COOH C4H6O6
RHA
(28,1) (28,2) (75,1) (75,2) (28,1) (28,2) (75,1) (75,2)
Na2O 2.04 1.04 0.90 0.61 0.26 23.05 0.54 0.95 0.45
MgO 1.43 0.01 0.02 - - - - - -
Al2O3 1.03 0.12 0.21 0.20 0.18 0.10 0.41 0.07 0.09
SiO2 51.84 62.19 89.49 89.41 84.02 52.56 92.21 81.25 60.11
P2O5 0.08 - 0.08 0.04 - - - - -
K2O 2.00 0.07 0.21 0.07 0.10 0.11 0.12 0.16 0.08
CaO 1.39 0.01 0.05 0.02 0.01 - - 0.06 0.04
TiO2 1.10 - 0.03 - - - - - -
CuO 1.91 0.79 0.41 0.97 - 0.97 0.33 0.23 0.83
Table 1: Chemical Composition Of Green Silica By Edx

The experimental results also show that the is supported by the statement [20] where CH3COOH
application of CH3COOH in the acid leaching process at a belongs to the bidentate ligand group so that it can act as a
temperature of 28oC for 2 hours can reduce Mg levels from complexing agent such as oxalic acid, ethanediol, and
1.26% to 0.01% and Ca levels from 1.28% to 0.04%, ethylenediamine. CH3COOH has a carboxylic group (-
thereby reducing the formation of MgO compounds and COOH) which can act as a connecting ligand that can
CaO in green silica products. In this operating condition, 1 connect metal centers [21] to reduce metal impurities in
mol/L CH3COOH also increased silica purity by 72.62%, silica, as well as with the characteristics of a relatively
from 51.84% to 89.49%. CH3COOH acts as a complexing cheap and easy- to-obtain cost [11], making CH3COOH
agent that forms bonds with metal elements in RHA. This

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ISSN No:-2456-2165
potential in optimizing the acid leaching process to improve silica. Detecting trace amounts of Cu, P, Ti, and Zn
the purity of green silica products. elements is possible from soil impurities in rice husks.
Meanwhile, the presence of Na content was caused by the
B. The Role of Thermal Process in Affecting The Particles reaction of the formation of sodium silicate during the
and Pores of Green Silica extraction process. Fig. 4. shows a photo of the surface
Energy Dispersive X-Ray (EDX) analysis was carried morphology of the green silica product resulting from acid
out to determine the chemical composition contained in the leaching with C4H6O6 at 28oC for 2 hours using SEM. With
silica product. The high percentage of impurities is the qualitative visualization, the silica material formed
cause of the low purity of the silica obtained30. In previous envelops the carbon, as shown in Fig. 4a). However, it is
studies, the data can be compared with silica synthesized still clear that some carbon aggregates with a size large
using inorganic acids. Differences or deviations in the enough in the range of 2.6 µm were found. It was found
percentage of impurity levels can be caused by several that the particle non-uniformity in silica morphology was
things, such as the incomplete smelting process of volatile caused by the process of reducing particle size using
compounds during calcination, as well as acid leaching manual milling and the possibility of forming aggregates in
operating conditions that are difficult to stabilize, causing a the product during drying process.
decrease in silica content. The elements O and Si are
present in the Si-O-Si and Si-OH groups contained in

Fig. 2: Morphology By Sem Analysis Of: A) Rha, B) Control, C) The Best Silica (C4h6o6,28oc,2h), D) The Best Silica
(Ch3cooh,28oc,2h) From 1000x Magnification

Calcination plays a vital role in the carbon oxidation C. Crystallinity Ratio of Green Silica Product
process. In this study, high levels of carbon were found in The crystallinity index of the best silica product from
the green silica product, as evidenced by the detection of the results of this study was calculated using the Segal
carbon in the surface morphology of the silica (see Fig. 1). method (see eq. 2), where the intensity value of the most
This is presumably because the decomposition process of substantial absorption spectra (It) became a function of the
volatile materials does not run perfectly during calcination, percentage of crystalline in the silica product (CI). CI=It-
causing oxidation to consume less carbon, so that the solids Ia/It (expressed in %) where CI shows the crystallinity
resulting from ashing still contain high levels of fixed index of the green silica product (expressed in %), which
carbon. This is probably one of the causes of the difficulty was synthesized using C4H6O6 at 28oC for 2 hours, and It
in achieving silica products with purity above 99%. is the total intensity of the most substantial absorption
Another cause is thought to be because the purity of silica peak. The results of XRD analysis showed that the
in RHA in this study was only 51.84%, whereas, in other strongest absorption peak of the best silica product was
studies, the percentage of silica was found to be much achieved at 869 counts. Substitute this value into equation
larger (73.85%-82.80%) [22][23]. However, adding an acid to obtain a silica crystallinity index of 38.74%. This
leaching treatment helped to obtain low-impurity green indicates that the best silica product from this study
silica with high pore volume characteristics, as shown in contains 61.26% amorphous silica. Based on the literature
Table 2. [24] the amorphous phase of silica is at 2<26o, for the
quartz phase is at 2=26o, the tridymite stage is at 2=31o,

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ISSN No:-2456-2165
and the cristobalite phase is at 2=33o. Silica calcined at a condition because under these conditions, tridymite will
temperature range of 600-800oC has an amorphous phase. transform into cristobalite [25].
Calcination temperature that is too high is not the best

Ratio
Acid
CI (%) Amorphous (%)
C4H6O6 38,74 61,26
CH3COOH 72,82 27,18
Table 2: Chemical Composition Of Green Silica By Edx

The XRD results show that the green silica product product from 1000x magnification which shows an
has an amorphous phase, and cristobalite is supported by irregular silica structures. It indicates that the best silica
the results of the crystallinity calculation using the Segal product contain amorphous phase.
method, as well as the surface morphology of the silica

Fig. 3: Phase Profile By Xrd On The Best Green Silica

D. The Testing of Best Silica Product on Moisture Green silica is formed from siloxane (Si-O-Si) and
Adsorption Process silanol (Si-OH) [27] groups which act as active sites. The
The amount of mass of silica products and water silica sample's active site begins in the thermal process at a
molecules that can be adsorbed to the saturation limit is a temperature of 400oC. The active site synthesized with
function of the adsorption capacity of silica. Based on the CH3COOH at 28oC for 60 minutes worked well, as
data in Fig. 4, it shows that the highest water molecule indicated by the high adsorption capacity of silica against
adsorption capacity is obtained by silica synthesized with water molecules. The acid leaching treatment increased the
CH3COOH at 28oC for 60 minutes, which is 825.6 mg/g, porosity of SiO2 [28]. Data support that all silica treated
followed by silica synthesized by CH3COOH at 28oC for with acid leaching had a moisture absorption capacity of
120 minutes at 824.4 mg/g which increased by 0.14%. The 47.6%-78.78% higher than the control sample. This is
lowest moisture adsorption capacity was obtained from the because it has a high pore void space, thereby increasing
control silica sample without acid leaching treatment, the moisture adsorption capacity, and is supported by the
which was 395.2 mg/g [26]. The silica quality standard results of the silica adsorption test on nitrogen gas which
based on SNI No. 06-2477-1991 has a minimum silica shows a pore volume value of 44.2513 cm3/g, where the
absorption capacity of 750 mg/g. Therefore, four samples higher the pore volume of a material, the higher pore
of green silica from the research meet the quality standards, volume of material will be the higher the adsorption power
which have adsorption capacities of 756.4 mg/g, 761,1 as expressed in figure 4.
mg/g, 824.4 mg/g, and 825 mg/g, respectively.

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Fig. 4: Moisture Adsorption Of Best Silica Product

q
Silica synthesized from rice husk ash without acid showed that additional treatment with acid leaching (C4H6O6,
leaching treatment had a surface area of 116 m2/g with a pore 28oC, 2h) increased the surface area and pore volume of
3
volume of 0,23 cm /g. The results of the BET-SAA analysis green silica.

Variables
Method
Surface Area (m2/g) Pore Volume (cc/g) Pore Diameter (Á)*
Adsorption 114,205 0,649 288,768
Desorption 242,20 0,736 126,279
BET 154,570 44,2513 -
Table 3: Saa Analysis Of Best Silica Product

Based on the literature, the amorphous silica product is ACKNOWLEDGMENT

of good quality if it has a specific surface area of more than
100 m2/g [29]. The data presented in Table 4. shows that The authors expresses the deepest gratitude to
the best green silica product (C4H6O6,28oC,2h) belongs to Chemical Engineering Laboratory (E Building, 1st Floor)
the mesopore category with a pore size range between 2-50 Diponegoro University for providing places and
nm and includes a product with good quality because it has experimental equipment for this research and Ir. Arif
a surface area of 154,570 m2/g with a pores volume of Widiyanto, IPM. who has provided financial support
44,2513 cm3/g, using the Brunauer Emmet Teller method throughout the research and analysis process.
so that in terms of pore characteristics, the silica product
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