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A R T I C L E I N F O A B S T R A C T
Keywords: Finding a way to efficiently utilize this bio-waste resource is a great challenge due to the depletion of traditional
Acid hydrolysis fossil fuels and the environmental impact associated to their use. Rice straw is considered as one of the main
Bio-energy cereal straws. It is produced in many countries every year in substantial amounts and it has a high ash content
Furans
and low protein content. Usually, rice straw is burned by farmers causing many adverse effects on the envi
Liquid-liquid extraction
Rice straw
ronment and public health. This research investigates the process synthesis of furfural production through the
Process simulation acid-hydrolysis of rice straws. Furfural is a strategic bio-renewable chemical and has gained attention due to its
possibility to produce biofuels and bio chemicals. Aspen Plus® simulation package is employed for process
simulation, sizing, and analysis. Results of simulations are validated against an experimental work. Optimization
through manipulation of several parameters including acid concentration, reaction temperature, acid/rice straw
ratio, catalyst concentration, and type of acid to maximize the furfural yield and reaction conversion. A complete
flow sheet is synthesized and sensitivity analysis is studied to reach an optimum process concerning environment
and economics. The amount of furfural obtained as a final product from the process represents a yield of 73% per
100 kg/hr of rice straw processed.
* Corresponding author.
E-mail address: dina.ahmed@bue.edu.eg (D. Kamel).
https://doi.org/10.1016/j.sajce.2021.08.002
Received 29 March 2021; Accepted 9 August 2021
Available online 10 August 2021
1026-9185/© 2021 The Authors. Published by Elsevier B.V. on behalf of Institution of Chemical Engineers. This is an open access article under the CC BY-NC-ND
license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
N. Sherif et al. South African Journal of Chemical Engineering 38 (2021) 34–40
Table 1 steps happen in series. Since it is difficult to generalize the effect of the:
Composition of rice straw using different standard methods (Yadav et al., 2016). Concentration of hydrolyzing agent, reaction time, reaction tempera
Components Determination Percentage mass ture, the particle size of biomass, and liquid to solid ratio on all ligno
method fraction cellulosic materials because they exhibit different characteristics ( P.
Cellulose TAPPI T 203cm-99 38.6 Yadav et al., 2016). The furans produced from the acid hydrolysis usu
Hemicellulose TAPPI T 203cm-99 26.4 ally have lower oxygen content than original biomass sugars, making
Glucan ASTM E 1758–01 38.82 them efficiently used as fuels. For such furans to be alike in properties
Xylan ASTM E 1758–01 19.7 further hydrogenation to larger hydrocarbons is needed to produce
Araban ASTM E 1758–01 2.6
Acetyl ASTM E 1758–01 1.1
5–hydroxymethyl furfural (HMF) (Marcotullio, 2011).
Lignin ASTM E 1758–01 15.8 Sarkar et al. (2012), studied the effect of the concentration of the
Moisture content ASTM D-1106 10.47 acid, the reaction time on the production of xylose which is the inter
Ethanol-benzene ASTM D-1107 3.8 mediate product before producing furfural and the kinetic model of this
extractives
reaction was developed to show the change in the production of xylose
Hot water extractives ASTM D-1111 5.7
Ash ASTM D-1102 10.5 with time. The rice straw to be hydrolyzed was obtained from Bankura,
India and it was dried employing air, grounded to a particle size of 0.5
mm, and kept at room temperature for later experiments. The compo
sitions of the cellulose, hemicellulose, and lignin were determined to be
Table 2
40.09 ± 0.02, 26.8 ± 0.02, and 18.9 ± 0.02 percentage of dry weight,
Elemental analysis of rice straw available in Egypt (Ali et al., 2017).
respectively. As for the acid hydrolysis step, the rice straw is diluted with
Proxanal Ultanal Sulfanal
H2SO4 at a temperature of 121 ◦ C and pressure of 15 psi, 1 g of rice straw
Element (wt Element (wt%,dry Element (wt%, dry
%) basis) basis)
was treated with almost 10 ml of H2SO4 having different concentrations
at different times of reaction. From this experiment, it was observed that
Moisture(wet 10 Ash 20 Pyritic 0
the maximum xylose was released at an acid concentration of 0.24
basis)
Fixed carbon(dry 20 C 39.2 sulfate 0 mol/L and a retention time of 30 min. Besides, it was noticed that the
basis) concentration of xylose showed an inversely proportional relationship
Volatile matter(dry 60 H 3.8 Organic 100 with time. As time increased the amount of produced xylose decreased;
basis)
this could be due to the breakdown of the sugar and the production of
Ash(dry basis) 20 N 0.3
Cl 0.9
inhibitors. Moreover, Gupta et al. (2016) collected the rice straw sam
ples from Saharanpur, India procured them, dried them in air, and
subjected it to mechanical size reduction by chopping to have a particle
size of 2–4 cm. All used chemicals were analytical grade produced by
Merk and Sigma. The rice straw hydrolysis was carried out at different
acid concentrations ranging from 0.1%− 0.6% v/v, to achieve the
maximum breakdown of hemicellulose to produce xylose the acid hy
drolysis was optimized at different temperatures (120 ◦ C, 140 ◦ C,
160 ◦ C) and at different retention times (60 min, 90 min, and 120 min)
the bath ratio was set to be 1:8 at the given conditions for all of the tested
Fig. 1. Formulation of furfural from pentoses (Karimia et al., 2006). samples.
Not only that but also, Yadav et al. (2016) collected rice straw from
testing committee standards gas chromatography-mass spectrometry India too, after the samples are dried they are stored in an air-tight
(GC–MS) method was used to obtain general quantification of some container for future use. The acid used in this hydrolysis was phos
saccharides within the rice straw and the results were as follows; 24.13 phoric acid, the experiments were performed in a rotating digester
mg glucose, 37.97 mg xylose, and 2.08 mg arabinose (Labib, 2017). consisting of two stainless steel cylindrical reactors inside it, each having
Moreover, according to Karimia et al. (2006) rice straw mainly contains capacity of one liter. And the optimum reaction conditions were found to
cellulose (32–47%), hemicellulose (19–27%), and lignin (5–24%). be: reaction temperature 160 ◦ C, reaction time 150 min., acid concen
Furthermore, the glucose content in cellulose (41–43.4%) and the xylose tration 8% (w/v), and liquid-solid ratio of 6.0 (volume-mass). At these
content in hemicellulose (14.8–20.2%). It was noted by Sashikala and conditions the amount of furfural produced is 4.85 g/L. The kinetics of
Ong (2007) that at harvest the moisture content of the rice straw is the hydrolysis reaction were studied by Hua et al. ( Hua et al., 2016) at
commonly greater than 60% on wet basis and it could decrease up to an operating temperature of 160–200 ◦ C and retention time of 3 h the
10–12% in dry weather conditions and that straw contains 90% cell furfural yield was 75% at optimum conditions. The rate constant k
wall, 3% silica, and 7% extractives. According to Gupta et al. (2016), the showed a clear agreement with the Arrhenius law from 160 to 200 ◦ C.
physicochemical composition of rice straw is as follows: 16.73% ash, The highest yields of xylose were obtained at 200 ◦ C, the activation
14.32% k.lignin, 18.83% pentosane, 63.2% hollocellulose, 7.82% energy for the reaction was 68.5 kJ/mol, and the pre-exponential factor
γ-cellulose, 40.15% α-cellulose, and 14.23 β–cellulose. As for Yadav was 1.82 ×105(mol dm− 3)0.5 min− 1.
et al. (2016), the main components of rice straw were determined using Furfural was identified as a top chemical that has opportunities from
several standard ways, the results are presented in Table 1. biorefinery carbohydrates due to the high level of attention in the
Furthermore, Ali et al. (2017) stated the elemental analysis of rice literature in recent years (Lee and Wu, 2021).
straw that gives data about the characteristics of the rice straw available The market price for furfural is at $1500/tonne (Valvand et al.,
in Egypt, the elemental analysis is provided in Table 2. 2018) whereas the market demand for furfural was estimated to reach
According to Fig 1, during the hydrolysis process, the acid releases 600-kilo tonnes annually by the year 2020 (Silva et al., 2017). The
protons that can break the heterocyclic ether bonds located between the adaptability of furfural to produce multiple products (Cai et al., 2014),
different sugar monomers in the polymeric chains of celluloses and and furfural currently being an existing commercial product with a
hemicelluloses. This break of bonds leads to the production of pentose well-established commercial production from renewable carbon has the
and hexose sugars. The furfural is produced in the dehydration step, by potential to be a primary building block in biorefineries (Bozell and
dehydrating the sugars to form such degradation products, these two Petersen, 2010). Furfural can be used to derive other value-added
chemicals such as industrial solvents, pharmaceutical products, food
35
N. Sherif et al. South African Journal of Chemical Engineering 38 (2021) 34–40
Table 3
Furfural production processes (Lee and Wu, 2021).
Process Temperature ( ◦ C) Pressure (bar) Catalyst Feed stock Furfural yield (%) Ref.
additives, and monomer (Machado et al., 2016) further highlighting its using an acid. Filtration of the solids residues from the filtrate is done to
versatility. avoid the fouling, corrosion and blockage in any of the following units.
Lee and Wu summarised in their review paper (Lee and Wu, 2021) on The stream is then heated to be prepared for the hydrolysis in the batch
furfural production, the various industrial processes to produce furfural reactor, after the reaction is done the effluent stream is cooled to be
from different feed stock in Table. 3. The highest yield is obtained ready for the liquid-liquid extraction.
through the Dupont process using corn cobs as a feed stock, and sul The separating agent is fed to the extractor along with the material
phuric acid as a catalyst. It should be highlighted that none of the stream and the required material is obtained, subsequently the material
available commercial processes uses rice straw as a feed stock, so this stream is fed to several/one distillation columns to ensure the proper
was the main drive to conduct our research work. separation of the required material (furfural) from any additional
This research aims to synthesize an optimum process for the indus products (separating agent, water and any other contaminants).
trial synthesis of furfural from rice straw bio-waste based on the The process flowsheet proposed in this work to convert rice straw
currently available experimental data. Most of the current research is waste into furfural is shown in Fig. 2. As shown in the figure, rice straw is
focused on optimization of the variables (reaction type, conditions, first washed and dried using hot air, and then is fed into a size reduction
retention time, and concentration of acid used) to produce furfural from machine in order to obtain a practical mixture for further processing.
rice straw on the laboratory scale, thus, the scope of this research is to Then, in a number of treatment operations, rice straw is treated to be
construct a full process flow diagram (PFD) using Aspen Plus software prepared for hydrolysis with acid in a batch reactor, the products go
package for an optimum furfural synthesis process. through cooling and separation to obtain the final product of furfural.
2. Methodology for furfural process synthesis 2.2. Developing the aspen plus model
2.1. Process synthesis Aspen Plus® simulation software is used to perform the modeling of
furfural production from rice straw bio-waste. The detailed steps for
The acid hydrolysis of rice straw in the laboratory proceeds through a developing the model are presented in the algorithm in Fig. 3. Aspen
number of experimental operations in order to yield furfural or chem Plus, as one of the famous energy industry’s leading process simulation
icals. These operations represent the basis for process synthesis. The first platforms for process optimization in design and operations, is used by
experimental step in the production is to wash and dry the rice straw, top oil and gas producers, refineries, and engineering companies.
this step is followed by mechanical size reduction of the straws. After
that, the rice straw is subjected to heat for pre-treatment in a heater
36
N. Sherif et al. South African Journal of Chemical Engineering 38 (2021) 34–40
37
N. Sherif et al. South African Journal of Chemical Engineering 38 (2021) 34–40
3.1. Reactor simulation furfural, such as Butylbenzene which has a boiling point of 183 ◦ C, and
pentylbenzene which has a boiling point of 205 ◦ C (Haan, 2011). It is
Based on Ali et al. (Ali et al., 2017) the yield reactor is used to better to use pentylbenzene in such case as the larger the difference
simulate the pre-treatment step and the required yield of the compo between the boiling point of furfural and the extraction solvent the
nents are entered. The yields of xylose, arabinose, glucose, and water are better the separation’s efficiency in the distillation column to extract
average values obtained from the ranges mentioned by Karimia et al. furfural, this gives enough time and temperature for all furfural to
(2006). The reaction temperature is set to be 121 ◦ C as according to vaporize leaving the extraction solvent (pentylbenzene) behind. The
Sarkar et al. (2012) this temperature and at 15 psi the highest yields of pressure and temperature of the extraction process are selected so that
xylose are obtained. The yields specified were; xylose 20.2%, glucose both streams are in their liquid state, experiments showed that out of a
43%, arabinose 4.5%, water 32.3%, and sulfuric acid was the inert temperature range less than or equal to 200 ◦ C, a temperature of 20 ◦ C
component. The stream exiting the yield reactor where pre-treatment showed better results. Besides, out of a pressure range less than 25 bar,
occurred is heated to 200 ◦ C to be ready for the reaction in the batch the ambient pressure (1 bar) was the most favorable. A feed to solvent
reactor. The reactor in simulation is selected to be isothermal along the ratio ranging from 1:2 to 2:l by weight could be used.
reaction process at 200 ◦ C and the retention time was 3 h according to The stream obtained from the filter is cooled down from 200 ◦ C to
Hua et al. (2016). 20 ◦ C to be ready for the Liquid–Liquid (L–L) extraction process, also a
The reaction yielded 12.92 kg/hr of furfural, 39.57 kg/hr of water stream with a flow rate of 200 kg/hr of pentylbenzene is fed to the
and there are remaining amounts of glucose, sulfuric acid, and arabinose extraction process. The number of stages of the extraction unit was set to
which were not used up in the chemical reaction. Since the streams 10 stages.
entering and leaving the reactor are slurry then a filter is needed as the The top stream contained almost all of the arabinose, glucose, Sul
presence of any solid/slurry matter in the streams might cause problems phuric acid, and water. While, the bottom product stream contained
to the rest of the flowsheet’s equipment (distillation columns and liquid- pentylbenzene, furfural, and a small amount of water. The bottom
liquid extractor). The filter was modeled to be a solid separator. The product had a temperature of 24 ◦ C, thus it was heated to 180 ◦ C to
products from the filter were divided into two streams; a stream con vaporize the remaining water.
taining furfural and water and a stream containing all of the other by-
products.
3.3. Distillation towers
3.2. Liquid–liquid extraction The heated stream enters the distillation column which consists of 15
stages, with a total condenser. The specified operating specifications
It is difficult to obtain furfural from a furfural aqueous mixture by were the distillate rate and the reflux ratio. Both specs values were
distillation because furfural forms azeotropes with water in the total altered to reach the optimum furfural yield. The optimum value for the
aqueous product, thus, liquid-liquid extraction is used. According to distillate rate and the reflux ratio are 0.06 kmol/h, and, 3 respectively.
Haan (2011), to produce furfural a water immiscible furfural solvent The top product from the distillation column was water which could
such as diethylbenzene, dipropylbenzene, dimethylethylbenzene, be treated for later use and the bottom product was the pentylbenzene
butylbenzene, pentylbenzene, tetralin and isophorone could be used. and the furfural together.
Even though methylbenzene was found to be selective to extract The bottom product from distillation column 1 was at 188 ◦ C and was
furfural from the liquid aqueous phase comprising furfural along with directly fed to distillation column 2 to separate furfural from pentyl
one or more organic acids, the fact that it has a boiling point of 111 ◦ C benzene and to obtain it as a top product alone. The distillation column
makes it expensive to be recycled as it has a boiling point lower than that was set to 30 stages to enhance the separation efficiency between the
of furfural 162 ◦ C. The favored aromatic hydrocarbon compounds that two products. Also, the operating specifications specified were the reflux
include alkyl benzene are those who have an alkyl side chain that con ratio and the distillate rate same as distillation column 1, and a range of
tains at least 2 carbon atoms and have a higher boiling point than that of values was used until the optimum combination was reached at a
Table 5
Mainstream components and flow rates .
Components in the Feed to Feed to L-L Feed to 1st distillation Feed to 2nd distillation Furfural product Pentyl benzene
streams reactorkg/h extractorkg/h columnkg/h columnkg/h streamkg/h product kg/h
Xylose 20.2 – – – – –
Glucose 43 – – – – –
Arabinose 4.5 – – – – –
Water 32.3 39.57 1.42 0.41 – –
Sulfuric acid 23.43 23.43 5.3 2.97 – 2.97
Furfural – 12.92 12.91 12.7 9.47 2.57
Pentylbenzene – 200 200 199.7 4.66 194.6
38
N. Sherif et al. South African Journal of Chemical Engineering 38 (2021) 34–40
Table 6 targets after heat integration are 401.6 cal/s and 1780.22 cal/s for
Comparison between experimental data and design data. heating and cooling, respectively. The hot pinch temperature and cold
Parameter Experimental data Simulation results pinch temperature are 131 ◦ C and 121 ◦ C, respectively.
As for the heat exchanger network, the pinch temperatures were used
Reaction temperature 200 C◦
200 ◦ C
Reaction pressure 1 bar 1 bar to divide the network into two regions above the pinch and below the
Residence time 3h 3h pinch. There are 4 streams to be heated and cooled within the process; 1
Furfural yield 75% (under optimal conditions) 73% hot stream and 3 cold streams, their data are presented in Table 7. The
hot stream is available above the pinch along with two other cold
streams. The hot stream will be used to heat the two cold streams, the
Table 7 Cph is greater than the Cpc which violates the Cp rule thus the hot stream
Heat integration data. will be split to follow the rule. The rest of the hot stream available below
Stream Supply temperature ( ◦ C) Target temperature ( ◦ C) Enthalpy (cal/s) the pinch will integrate heat with the two available cold streams and will
need further external energy to be cooled.
H1 200 20 9641.57
C1 25 121 1237.31
Fig. 5 presents the optimum heat exchanger network for the furfural
C2 121 200 2316.41 synthesis process. This optimized HEN enhanced the energy recovery
C3 24 180 4709.03 within the system; 95% of heating and 81% of the cooling duties.
6. Conclusion
distillate rate of 0.13 kmol/h and a reflux ratio of 3. Table 5 presents the
data for the main streams in the model.
In conclusion, the production of furfural from biomass is a worthy
process and needs much more attention to employ the rice agricultural
4. Model validation against the experimental data wastes economically and environmentally. The work presented in this
research also contributes to creating other sources of fuel other than
The amount of furfural obtained as a final product from the process is fossil fuels. The conversion process of rice straw to furfural was studied
9.47 kg/hr and mass fraction of 0.658, referring to the amount of by many researchers globally, thus, a huge library and amount of in
furfural produced from the batch reactor, almost 73% of it is obtained as formation for the lignocellulose content, the carbohydrates composition,
a final product. Moreover, 46% of the xylose fed to the batch reactor at and the water content were utilized to reach an optimum industrial
20.2 kg/hr was converted to furfural. In terms of molar flowrates, synthesis model.
0.1345 kmol/hr of xylose produced 0.098 kmol/hr of furfural, thus the The reaction kinetics used for the reaction were; the activation en
yield of furfural is 72%. Validation of the obtained results is done by ergy (E) is 68.5 kJ/mol, temperature (To) is 200 ◦ C, the order of reaction
comparing them to previous studies as presented in Table 6; the yield of (n) is 1, the pre-exponential factor (A) is 1.82 × 105 (mol dm− 3)0.5
furfural obtained ( Hua et al., 2016) is 75% under optimal conditions. min− 1, the rate constant (k) is 3.0025 * 10− 4 min-1. Since furfural forms
an azeotrope mixture with water, it is difficult to be extracted from it by
5. Optimization of the process through heat integration simple distillation, thus, liquid-liquid extraction is used. A solvent is
used (pentylbenzene) at a flow rate of 200 kg/hr in the extraction col
In this process, there is one hot stream and three cold streams, heat umn to obtain furfural from the mixture it formed with water. The final
integration is utilized to reduce the usage of external cooling or heating stream contained an amount of 9.47 kg/hr of furfural, with an overall
utilities. The overall heating and cooling utilities before heat integration recovery percentage of 73%.
were 9641.57 cal/s and 8262.75 cal/s, respectively. The minimum Validation of the plant model against the experimental results
temperature driving force (ΔTmin) was investigated through Aspen en showed an acceptable agreement. Optimization through heat integra
ergy analyzer software from the range of 5 ◦ C till 15 ◦ C, it was found that tion was performed using pinch analysis to save energy from within the
the most energy saved was at ΔTmin = 5 ◦ C. Although most of the energy process and decrease the cost of purchasing external utilities, the process
is recovered at ΔTmin = 5 ◦ C, a higher pinch temperature of 10 ◦ C is used had 4 streams; 1 hot and 3 cold streams the energy targets after
because ΔTmin = 5 ◦ C is only used in the clean industry. The energy
39
N. Sherif et al. South African Journal of Chemical Engineering 38 (2021) 34–40
integration are 146.6 cal/s and 1525.55 cal/s for heating and cooling, torrefied biomass pellets. Energy conversion management. Volume 161, 205–214.
https://doi.org/10.1016/j.enconman.2018.02.003.
respectively.
Hua, D., Wu, Y.L., Liu, Y.F., Chen, Y., Yang, M.D., Lu, X.N., Li, J., 2016. Preparation of
furfural and reaction kinetics of xylose dehydration to furfural in high-temperature
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Declaration of competing interest 4816–4838. https://doi.org/10.1039/C4GC01160K.
Machado, G., Leon, S., Santos, F., Lourega, R., Dullius, J., Elizabete, M., Eichler, P., 2016.
Literature review on furfural production from lignocellulosic biomass. Natural
The authors declare that they have no known competing financial Resources. Volume 7, 115–129. https://doi.org/10.4236/nr.2016.73012.
interests or personal relationships that could have appeared to influence Marcotullio, G., 2011. The Chemistry and Technology of Furfural Production in Modern
Lignocellulose-Feedstock Biorefineries. PhD, thesis, Delft University of Technology,
the work reported in this paper.
Delft.
Mariscal, R., Maireles_Torres, P., Ojeda, M., Sadaba, I., Granados, M., 2016. Furfural:a
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