SUGARCANE BAGASSE CONVERSION TO HIGH …jestec.taylors.edu.my/Special Issue 1_SOMCHE_2014/SOMCHE 2014_… · cellulose-acetate addesive, nitrocellulose coating agent, and nitrocellulose

Journal of Engineering Science and Technology Special Issue on SOMCHE 2014 & RSCE 2014 Conference, January (2015) 35 - 46 © School of Engineering, Taylor’s University

35

SUGARCANE BAGASSE CONVERSION TO HIGH REFINED CELLULOSE USING NITRIC ACID, SODIUM HYDROXIDE AND HYDROGEN PEROXIDE AS THE DELIGNIFICATING AGENTS

S. SUPRANTO*, A. TAWFIEQURRAHMAN, D. E. YUNANTO

Department of Chemical Engineering, Gadjah Mada University, Jalan Grafika No. 2, Yogyakarta 55282, Indonesia

*Corresponding Author: [email protected]

Abstract

As a renewable material, Sugarcane-bagasse fiber waste, has a huge potential as raw material for production of the High Refined Cellulose (HRC) and the cellulose chemicals derivatives such as Carboxyl Methyl Cellulose -emulsifier, cellulose-acetate addesive, nitrocellulose coating agent, and nitrocellulose membrane filter. The objective of the study is to find out the optimal process conditions of the chemical conversion of the Sugarcane-bagasse fibre waste to the HRC. The experiments were carried out in a 1000 mL reactor capacity, equipped with stirrer and temperature controller. Three-steps atmospheric processes were involved, firstly using nitric acid solution at 80oC for 2 hours, following by the second step using sodium hydroxide at 80oC for 2 hours and finishing using hydrogen peroxide at 80oC, 30-300 min in the third step . The HRC quality was indicated by its cellulose content. The result shows that the HRC product with cellulose content of higher than 90% were succesfully performed using a three-steps of the sugarcane-bagasse fiber delignification process. The optimal process condition of the sugarcane-bagasse fiber conversion to the HRC were achieved at 80oC at atmospheric pressure with a combinations of the 3-5% HNO3 with ratio of HNO3 /bagasse of 15-20 mL/g and 2N NaOH with ratio of NaOH/bagasse of 15-20 mL/g and 10% H2O2 for 5 hours.

Keywords: High refined cellulose, Delignification process, Sugarcane-bagasse fiber.

36 S. Supranto et al.

Journal of Engineering Science and Technology Special Issue 1 1/2015

Nomenclatures Ca(OH)2 FeCl3 HCl HNO3 H2O2 H2SO4

KOH L/D NaOH Na2CO3

Calcium Hydroxide Ferry Chloride Hydrochloric Acid Sulphuric Acid Hydrogen Peroxide Nitric Acid Potassium Hydroxide Length to Diameter ratio Sodium Hydroxide Sodium Carbonate

Abbreviations

BPS C HRC

Badan Pusat Statistik Indonesia Celsius High Refined Cellulose

SCB Sugar Cane Bagasse

1. Introduction

1.1. Sugar cane bagasse

The photosynthesis process which converts carbon dioxide to organic compound is the most important step in the growth of biomass. Cellulose, carbohydrate and fatty oil are the main three components in biomass produced by photosynthesis process, so the plantation cellulose is one of the renewable chemical performed in carbon dioxide photosynthesis conversion. The cellulose in plantation fibre generally is the most dominant organic components in most biomass. In sugar cane bagasse (solid waste in cane sugar production) the cellulose content were reported as high as 35,3% [1], 32-44% [2], 35-50% [3], 32-44% [4], 45,5% [5], 47.5-51.1% [6], 40-41.5% [7] [8]. BPS, 2013 [9] reported that in 2012, Indonesia with the production of sugar cane as much as 2.6 million ton, there would be produced solid waste bagasse as much as 13 million ton. The solid waste bagasse from sugar production may be counted as a potential raw material for HRC production, which can be converted further to some end product, Cellulose acetate, Carboxyl Methyl Cellulose, viscose cellulose and other cellulose derivatives.

1.2. Delignification processes

The first step in converting the plantation fibre to cellulose derivatives is called delignification, in which lignin as component of plantation fibre was removed, leaving the relatively pure cellulose in solid phase as HRC product. Supranto, 2011 [10] reported that sago fibre can be converted to nitrocellulose through delignification and nitration processes. Delignification process of sugar cane bagasse (SCB) prior to further processes has been found in some publication. Some different method of SCB delignification process has been reported. Acid process and alkaline processes were the two most popular.

Sugarcane Bagasse Conversion to High Refined Cellulose Using Nitric . . 37


1.2.1. Acid process

Deschamps et al., 1995 [11], in cattle feed production processing from SCB, used Phosphoric acid as much as 3% (w/w) to remove lignin, followed by alkali washing. Phosphoric acid process for lignin removal from SCB also reported by Gamez et al., 2006 [12]. Gomez et al. used Phosphoric acid concentration of 2-6%, time 0-300 min and temperature of 122oC to remove lignin from SCB. Chong et al., 2004 [13], reported that releasing lignin from SCB was successfully done by using nitric acid at variable concentration of 2-6%, reaction time up to 300 min and temperature of 100-128oC. Diluted sulphuric acid used for pre-treatment of SCB hydrolysis was reported by Cassia et al., 2010 [14]. Combination of acid concentration, temperature and residence time was simulated. Zhang et al., 2012,[15] used 1.2% HCl, reaction time of 30 min and 130oC in delignification process of SCB. They found that HCl was more effective than H2SO4 of FeCl3. Zhao and Liu, 2013 [16] used 0.05-0.4 % sulphuric acid and 60-90 weight% acetic acid in delignification process of SCB. The degree of delignification resulted were 53.7-79.7%.

Sulphuric acid process in removing lignin from SCB with acid concentration of 0.4-5% at 97-126oC was reported by Zhao et al., 2012 [17]. The model of kinetic behaviour of dilute acid hydrolysis of SCB has been introduced with determination coefficients (R) in the range of 0.95-0.995. Disruption of lignocellulose structure of SCB using dilute sulphuric acid in microwave heating at temperature of 130, 160 and 190oC with two heating time of 5 and 10 min have been investigated by Chena et al., 2011 [18]. The result shows that an increase in reaction temperature destroyed the lignocellulose structure of SCB. Chena et al., 2012 [19] reported that around 40-44% of bagasse was degraded in acid delignification process using dilute sulphuric acid solution at 180oC for 30 min in a microwave irradiation environment. Leibbrandt et al., 2011 [20] reported that lignin was successfully removed from SCB using process of delignification as pre-treatment process for bioethanol production from SCB using three different pre-treatment methods, i.e. dilute acid, liquid hot water and steam explosion, at various concentration. Mandal and Chakrabarty, 2011 [21] successfully used the acid hydrolysis process in the delignification and isolation process of nanocellulose from SCB with fibre to liquor ratio of 1:20 for 5 h at 50oC. Cardona et al., 2010 [22] resumed that delignification of SCB with dilute acids (sulphuric, hydrochloric or acetic, typically 1-10% weight) hydrolysed the hemicellulose fraction at moderate temperature (100-150oC). The usage of sulphuric acid, hydrochloric acid and acetic acid of 1-10%, and temperature of 100-150oC in SCB hydrolysing process for ethanol production also reported by Cheng et al., 2008 [23]. Combination of sulphuric acid and phosphoric acid for delignification of SCB reported by Geddes et al., 2010 [24]. A low level of phosphoric acid (1% w/w on dry bagasse basis, 160 C and above, 10 min) was shown to effectively hydrolyse the hemicellulose in sugar cane bagasse into monomers with minimal side reactions and to serve as an effective pre-treatment for the enzymatic hydrolysis of cellulose. Sulphuric was more effective than phosphoric at low concentrations.

1.2.2. Alkaline process

Playne, 1984 [7] used alkaline process ( using NaOH, Ca(OH)2 and Na2CO3) combining with steam explosion at 200oC, 6.9 MPA and 5 min cooking time to remove lignin from SCB prior to pulp digesting process. Mandal and Chakrabart,



2011 [21] used 0.7% (w/v) sodium chloride solution, fibre to liquor ratio of 1:50, at pH4, adjusted by 5% acetic acid and maintained with buffer solution of pH4 while mixture was being boiled for 5 h to remove the lignin. After washing process, the residue was then boiled with 250 mL 5% (w/v) sodium sulphite solution for 5 h, followed by washing with distilled water to remove the lignin completely and hemicellulose partially. Sun et al., 2004 [25] investigated the delignification of SCB using various concentrations of alkali and alkaline peroxide yielded 44.7 and 45.9% as cellulose preparations process, which contained 6.0 and 7.2% associated hemicelluloses and 3.4 and 3.9% bound lignin, respectively.

Delignification with acidic sodium chlorite followed by extraction with alkali (10% KOH and 10% NaOH) gave cellulose yields of 44.7 and 44.2%, which contained 5.7 and 3.7% residual hemicelluloses and 1.6 and 1.5% remaining lignin, respectively. Sun et al., 2004 [26] used 0.5M NaOH and 05-3.0% H2O2 at pH 11.5 for 2 h under 55oC in delignification process of SCB. The successive treatments released 89% of the origin lignin in SCB. One-step process using alkaline hydrogen peroxide for SCB delignification process was investigated by Brienzo et al., 2009 [27]. With the operating condition used were H2O2 concentration from 2 to 6% (w/v), reaction time from 4 to 16 h, temperature from 20 to 60◦C, and magnesium sulphate absence or presence (0.5%,w/v), 88% of lignin in SCB removed.

Rabelo et al., 2011 [28] reported delignification process involving lime in alkaline hydrogen peroxide process prior to enzymatic hydrolysis of SCB. The experimental result shows that lignin removal using the peroxide process was higher than lignin removal using the lime process. Velmurugan and Muthukumar, 2011 [29] using the sono-assisted alkaline pre-treatment prior to SCB hydrolysis. The cellulose and hemicellulose recovery observed in the solid content was 99% and 78.95%, respectively and lignin removal observed during the pretreatment was about 75.44%. Combination of alkaline process and acid process in SCB delignification was reported by Teixeira et al., 2011 [30]. Their work evaluates the use of SCB as a source of cellulose to obtain whiskers. These fibers were extracted after SCB underwent alkaline peroxide pre-treatment followed by acid hydrolysis at 45◦C. The influence of extraction time (30 and 75 min) on the properties of the nanofibre was investigated. The results showed that SCB could be used as source to obtain cellulose whiskers and they had needle-like structures with an average length (L) of 255±55 nm and diameter (D) of 4±2 nm, giving an aspect ratio (L/D) around 64. More drastic hydrolysis conditions (75 min) resulted in some damage on the crystal structure of the cellulose. Gunam et al., 2011 [31] used sodium hydroxide process to remove lignin in SCB. Lignin removal of 32.11 % was reported as a result of alkaline delignification process using 6% sodium hydroxide at 50oC, with reaction time of 12 h.

Rezende et al., 2011 [32] reported that using sodium hydroxide process, 85% of lignin in SCB was successfully removed using 1% (m/v) NaOH. Soares and Gouvenia, 2013 [33] used alkaline delignification process of SCB using 0.5-1% NaOH. Lignin removal of 76% was achieved when SCB of 25% lignin content, was treated with alkaline delignification process using 1% NaOH. Asqher et al., 2013 [34] reported that lignin removal of 48.7% was achieved in alkali treatment process of SCB at 35oC, using 4% NaOH for 48 h. Two-step process for cellulose extraction from palm kernel cake involving H2O2 to separate hemicellulose, cellulose and lignin, was reported by Yan et al., 2009 [35]. Palm kernel cake was



pretreated in hot water at 180oC and followed by liquid oxidation process with 30% H2O2 at 60oC at atmospheric pressure. Through hot water treatment, hemicellulose in the palm kernel cake was successfully removed, leaving lignin and cellulose in solid phase. Lignin was removed to water soluble compounds in liquid oxidation step and almost pure cellulose was recovered.

1.3. Objective of the study

The objective of the study is to find out the optimal process conditions of the SCB conversion to HRC through a three-step delignification process.

2. Material and Method

2.1. Materials

Locally available SCB from Yogyakarta Sugar Industry was collected, sorted and cleaned. SCB was dried in sunlight and cut into small pieces about 1 -2 cm. The cut SCB was grinded and the fraction passing 60 meshes was selected for raw material of delignification process. The cellulose content in the SCB was around 29.4%. Other reagent used (nitric acid, sodium hydroxide and hydrogen peroxide) were technical grade.

2.2. Methods

Three-step of SCB delignification was chosen, a combination of acid process, alkaline process and oxidation process. Variation of Nitric acid and NaOH concentration were chosen as referred to acid delignification process reported by Chong et al., 2004 [13]. They used nitric acid concentration of 2-6% and removed the lignin from SCB successfully, and alkaline delignification process reported by Soares and Gouvenia, 2013 [33] that used of 0.5-1% NaOH resulted in the lignin removal of 76% . The atmospheric pressure and temperature less than 100oC, were chosen, referred to Yan et al. work, 2009 [35], they extracted cellulose from palm kernel cake involving the use of 30% H2O2 at 60oC at atmospheric pressure. The oxidation process was varied from 8-12% H2O2, with reaction time of 1-5h, developed from the experimental oxidation process condition done by Brienzo et al., 2009 [27]. They used H2O2 concentration from 2 -6%, reaction time from 4-16 h, temperature from 20 – 60oC and magnesium sulphate of 0.5% (w/v), resulted in more than 88% lignin in SCB was removed.

The experiments were carried out in a 1000 mL reactor capacity, equipped with stirrer and temperature controller. Three-steps atmospheric processes were used, firstly using nitric acid solution at 80oC for 2 hours, following by the second step using sodium hydroxide at 80oC for 2 hours and finishing using hydrogen peroxide at 80oC, 30-300 min in the third step . The detail process diagram of the delignification process was shown in the following Fig. 1.



Fig. 1. Diagram of the Experimental Procedure of SCB Conversion to HRC.

2.3. Data analysis

The HRC quality was indicated by cellulose content in HRC product. Cellulose content in SCB and HRC were analyzed using method described by Kulić and Radojičić, 2011 [36]. This method is based on insolubility of cellulose in water and its resistance to action of dilute acids and bases. The sample was degraded with a mixture of nitric acid and acetic acid and boiled in apparatus that contained a Liebig's condenser. The solution was then filtered through a Büchner funnel. Then the filter paper containing an insoluble residue was dried in oven and measured. Analysis was done at “Pusat Studi Pangan dan Gizi” Gadjah Mada University.

The effect of process condition to HRC product quality were interpreted using graphical method using interpolation and second order polynomial correlation. The optimal process condition was determined graphically, indicated by the region or area in which the variation of process condition would result in highest cellulose content in HRC was achieved.

3. Results and Discussion

3.1. Effect of HNO3 concentration and ratio HNO3/SCB on HRC quality

Figure 2 shows the effect of varying HNO3 concentration on HRC quality. The correlation formula between HNO3 concentration (x) with the HRC quality indicated by its cellulose content (z), was represented by second order polynomial with correlation constant (R2) of 0.9459 as shown in Fig. 2. Increasing the HNO3 concentration from 2 to 5 % will result on increasing the cellulose content in



HRC, but further increase in HNO3 concentration result on lowering the cellulose content in HRC product. HNO3 concentration of 5 % was taken as the optimal HNO3 concentration.

Fig. 2. The Effect HNO3 on HRC Quality, with SCB Fixed of 30 g,

Duration Time of 2 h and Temperature 80oC, 2 N NaOH and 8% H2O2.

Figure 3 show the effect of varying HNO3/SCB ratio on HRC quality. The correlation formula between HNO3 / SCB ratio (r) with the HRC quality indicated by its cellulose content (z) , was represented by second order polynomial with correlation constant (R2) of 0.9849 as shown in Fig. 3. Increasing the HNO3/SCB ratio higher than 20 mL/g caused a reduction in the HRC cellulose content. The use of HNO /SCB ratio of 15 to 20 mL/g has no significance effect on HRC cellulose content. However solid-liquid mixing with HNO3/SCB ratio of 20 mL/g seem to be better. The optimal process condition of the 1st step delignification process was concluded as 3-5% HNO3 and 15-20 mL/g ratio of HNO3/SCB.

Fig. 3. The Effect HNO3 /SCB Ratio on HRC Quality, with SCB Fixed of

30 g, Duration Time of 2 h and Temperature 80oC, 2 N NaOH and 8% H2O2.

z = -0.4192x2 + 3.1824x + 81.73

R² = 0.9459

40

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0 2 4 6 8 10 12

Ce

llu

lose

co

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RC

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%

HNO3 (x), %

z = -0.1079r2 + 3.2545r + 66.108

R² = 0.9849

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10 15 20 25 30 35

Ce

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HNO3/bagasse (r), mL/g



3.2. Effect of NaOH concentration and ratio NaOH/SCB on HRC quality

Figures 4 and 5 show the effect of varying NaOH concentration and NaOH/SCB ratio on HRC quality. The correlation formula between NaOH concentration (y) and NaOH/SCB ratio (r) with the HRC quality indicated by its cellulose content (z) , was represented by 1st and 2nd order polynomial with correlation constant R2 (R2) of 0.9957 and 0.9958 respectively, as shown in Figs. 4 and 5.

Fig. 4. The Effect NaOH on HRC Quality, with SCB Fixed of 30 g,

Duration Time of 2 h and Temperature 80oC, 5% HNO3 and 8% H2O2.

Fig. 5. The Effect NaOH /SCB Ratio on HRC Quality, with SCB Fixed of

30 g, Duration Time of 2 h and Temperature 80oC, 5% HNO3 and 8% H2O2.

The optimal process condition of the 2st step delignification process was concluded as 2 N NaOH and 15-20 mL/g ratio of NaOH/SCB.

z = 2.314y + 86.938

R² = 0.9957

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0.5 1 1.5 2 2.5 3

Ce

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, %

NaOH (y), N

z = -0.0573r2 + 1.9398r + 75.404

R² = 0.9992

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10 15 20 25 30 35Ce

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3.3. The effect of H2O2 concentration and 3rd step time process

duration on HRC quality

Figures 6 and 7 show the effect of simultaneous varying H2O2 concentration and 3rd step time process duration on HRC quality, presented as a graphical surface response. The correlation formula between H2O2 concentration and time process duration was presented on 3D picture in Fig. 6 and 2D plotting in Fig. 7.

Fig. 6. The Effect of Simultaneous Varying H2O2 Concentration and

3rd Step Time Process Duration on HRC Quality, Presented in 3D Picture.

Fig. 7. The Effect of Simultaneous Varying H2O2 Concentration and

3rd Step Time Process Duration on HRC Quality, Presented in 2D Picture.

46

81012

4045505560657075808590

60

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36

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,%

Time, min

85-90

80-85

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Time, min

85-90

80-85

75-80

70-75

65-70

60-65

55-60

50-55

45-50

H2

O2

, %



The optimal process condition of the 3st step delignification process was concluded as 300 min and 10 % H2O2.

4. Conclusions

An investigation has been made of the effects of HNO3, NaOH and H2O2 in three-step delignification process of SCB on HRC product quality. The delignification process consisted of 3 steps, using HNO3, NaOH and H2O2 respectively. The result show that The optimal process condition of the sugarcane-bagasse fiber conversion to the HRC with cellulose content of 90% were achieved in three-step delignification processes in atmospheric processes, at 80oC with a combinations of 3-5% HNO3 with ratio HNO3 /bagasse of 15-20 mL/g and 2N NaOH with ratio NaOH/bagasse of 15-20 mL/g and 10% H2O2 in 5h process. HRC with 90% cellulose or higher may be converted further to some end product, such as Cellulose acetate, Carboxyl Methyl Cellulose, Viscose cellulose and other cellulose chemical derivatives form of useful products.

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SUGARCANE BAGASSE CONVERSION TO HIGH …jestec.taylors.edu.my/Special Issue 1_SOMCHE_2014/SOMCHE 2014_… · cellulose-acetate addesive, nitrocellulose coating agent, and nitrocellulose