Preparation and Characterisation of Charcoal Material Derived from Bamboo for the Adsorption of Sulphur Contaminated Water

London Journal of Research in Science: Natural and Formal
Volume | Issue | Compilation
Authored by Varinder Kaur , Baljinder Kaur, Karanjeet Kaur, Mandeep Kaur, Supreet Kaur
Classification: FOR Code: 069999
Keywords: bamboo, charcoal, cellulose, lignin, sulhur.
Language: English

Bamboo charcoal has a lot of positive qualities. The highly porous structure of the bamboo charcoal absorbs sulfur-based compounds. Sulfur powder and sulfur dioxide (SO2 ) often floated in air, produced acid rain and algal blooms and cause diseases. Bamboo charcoal has adsorption and filtration properties. In this study, Bamboo charcoal is created by: (a) Pyrolysing bamboo using aluminium foil, (b) in muffle furnace at temperature of 600 ̊C. The obtained charcoal from pyrolysing bamboo in muffle furnace is further purified by solvent-extraction. The resulted charcoal obtained by these two methods is then characterised by XRD and FTIR. In order to figure out the optimal adsorption condition and the intrinsic change of the bamboo charcoal, two chemicals (Sodium sulphate powder and Sodium persulphate) are adsorbed by bamboo charcoal. Bamboo charcoal which contained potassium, calcium and other minerals, could have adsorption and filtration of extractives, oil, and other substances.

               

Preparation and Characterisation of Charcoal Material Derived from Bamboo for the Adsorption of Sulphur Contaminated Water

Varinder Kaurα,  Baljinder Kaurσ, Karanjeet Kaurρ, Mandeep KaurѠ & Supreet Kaur¥

____________________________________________

ABSTRACT

Bamboo charcoal has a lot of positive qualities. The highly porous structure of the bamboo charcoal absorbs sulfur-based compounds. Sulfur powder and sulfur dioxide (SO2) often floated in air, produced acid rain and algal blooms and cause diseases. Bamboo charcoal has adsorption and filtration properties. In this study, Bamboo charcoal is created by: (a) Pyrolysing bamboo using aluminium foil, (b) in muffle furnace at temperature of 600 ̊C. The obtained charcoal from pyrolysing bamboo in muffle furnace is further purified by solvent- extraction. The resulted charcoal obtained by these two methods is then characterised by XRD and FTIR. In order to figure out the optimal adsorption condition and the intrinsic change of the bamboo charcoal, two chemicals (Sodium sulphate powder and Sodium persulphate) are adsorbed by bamboo charcoal. Bamboo charcoal which contained potassium, calcium and other minerals, could have adsorption and filtration of extractives, oil, and other substances.  

Keywords: bamboo, charcoal, cellulose, lignin, sulhur.

Author α σ ρ Ѡ ¥: Department of Chemistry, Guru Nanak Dev University, Amritsar-143005, Punjab, India.

  1. INTRODUCTION

Ecological or environment problems have become global in character and there is an urgent need worldwide to tackle these problems. Industrial activities have negative effect on the ecological system. Industrial waste water is often contaminated with various organic and inorganic compounds such as phenol, chromium, suspended solids, dissolved organic compounds, heavy metals and so on [1]. Heavy metals as one of the environmental pollutants are gradually becoming most dangerous without immediate detection because it takes long for the metals to accumulate in the body depending on the distance away from the point of discharge and thus, they pose health hazards to man and aquatic lives [2]. The majority of sulphur have came from industrial waste water, such as chemical fertilizers, processed meat, leather and other industries, city life sewage and farmland irrigation are also the main sources. Sulphur is a rich nutrient pollutant which after entering water can cause algal blooms and eutrophication of the water body. This polluted water may further pollutes the environment, disrupts the ecological balance and also harms human health through food chain channels and thus, lead to drinking-water toxicosis. This also causes sulphide formation of acid rain in the air and water and other substances reaction [3].

Treatment processes for metal contaminated wastewater include chemical precipitation, membrane filtration, reverse osmosis, ion exchange and absorption. Absorption has advantageous over other methods because it is sludge-free and is of low capital intensiveness. Activated carbon has been reported to have high and fast absorption capacities due to its well-developed porous structure and tremendous surface area [4]. In China, Bamboo planting is very large; it has a kind of short growth cycle and timber fast biomass resources [5]. Due to the increasing demand for carbon-based nano-materials in various emerging fields, renewable carbon resources such as plant biomass, plant extracts and hydrocarbons have been explored for the fabrication of carbon nanostructures. Bamboo has a carbon rich chemical structure and is cost effective [6]. Bamboo plants are identified as species of subfamily Bambusoideae, family Gramineae. They are distributed in many parts of the world and having more than 1200 species of 50 genera of bamboo. The chemical composition of bamboo is similar to that of wood. Therefore, the main constituents of bamboo culms are cellulose (45-55%), hemi-cellulose (20-25%) and lignin (22-30%), which amount to over 90% of the total mass. The minor constituents of bamboo are resins, tannins, waxes (0.5-0.7%) and inorganic salts. Compared with wood, however, bamboo has higher alkaline extractives, ash and silica contents [7]. Bamboos are the fastest growing plants in the world, due to a unique rhizome dependent system. These are of notable economic and cultural significance in South Asia, Southeast Asia and East Asia, being used for building materials, as a food source and as a versatile raw product. It has a higher specific compressive strength than wood, brick or concrete and a specific tensile strength than rivals steel. Bamboo charcoal is a natural, renewable environmental protection material and functional material.

In this study, Bamboo charcoal is created by: (a) Pyrolysing bamboo using aluminium foil, (b) in muffle furnace at temperature of 600 ̊C. The obtained charcoal from pyrolysing bamboo in muffle furnace is further purified by solvent-extraction. The resulted charcoal obtained by these two methods is then characterised by XRD and FTIR. Bamboo charcoal has a lot of positive qualities. The highly porous structure of the bamboo charcoal absorbs sulphur based compounds. Sulphur powder and sulphur dioxide (SO2) often floated in air, produced acid rain and algal blooms and cause diseases. Bamboo charcoal has adsorption and filtration properties. In order to figure out the optimal adsorption condition and the intrinsic change of the bamboo charcoal, two chemicals (Sodium sulphate powder and Sodium per sulphate) are adsorbed by bamboo charcoal. Bamboo charcoal which contained potassium, calcium and other minerals, could have adsorption and filtration of extractives, oil, and other substances.  

1.1. Introduction of Bamboo Charcoal

Bamboo charcoal is the carbonaceous residue of bamboo left after heating organic matter (bamboo) in the absence of oxygen. Bamboo charcoal comes from pieces of bamboo plants, harvested after at least five years, and burned in ovens at temperatures ranging from 800 to 1200 ºC. This fine and tasteless black powder is an adsorbent for many toxins, gases and drugs without any specific action [8]. Bamboo charcoal has an extra-ordinarily large surface area and pore volume that gives it a unique adsorption capacity [9]. It benefits environmental protection by reducing pollutant residue. It is an environmentally functional material featuring excellent absorption properties [10]. Commercial food grade charcoal products range between 300 and 2000 m2/ g [11]. Charcoal has much higher adsorptivity than wood charcoal because bamboo charcoal has very high specific surface area, about 150-400 m2/ g, which is 2-3 times bigger than wood charcoal and can be used for a wide range of different purification and absorption applications, such as purifying drinking water, in air filters, gas masks, mattresses and pillow and for certain industrial purification uses [12].

1.2. Structure of Bamboo charcoal

Bamboo charcoal has micro porous structure and countless small cavities. Bamboo charcoal has about four times more cavities than wood charcoal because it has surface area of 300m2/g, which is 10 times more than wood charcoal. Cell wall mainly consists of cellulose, hemicellulose and lignin [13]. Bamboo charcoal being an outcome of pyrolyzing bamboo, is a sort of porous material with excellent adsorption and electromagnetic shielding (Figure 1.5). The surface area to weight ratio of bamboo charcoal is 600:1. This is because of the presence of C60 carbon molecule that is like a ball shape [14].

Figure 1.5: Micro-porous structure of Bamboo charcoal [13]

1.3.  Adsorption capacity of Bamboo charcoal

Adsorption capacity of bamboo charcoal is an important characteristics because bamboo charcoal forms a lot of pores after pyrolysed under high temperature, which is similar to wood charcoal. It has adsorption capacity with big specific surface area (for example, its specific surface area reaches 385 m2/g when it is carbonized at 700 ºC).  Its physical and chemical properties are very stable. It is not soluble in water and other solvents. It demonstrates high stability in various working conditions except with strong oxidant in high temperature (for example, oxygen in high temperature, ozone, chlorine and salt of dichromate). So bamboo charcoal can be used both in a wide range of pH and in many solvents.

In order to study bamboo charcoal’s capacity for adsorbing harmful gas, five kinds of representative harmful substances, that is methanol, ammonia, benzene, methylbenzene, and chloroform were chosen and the static method that measures the adsorption ratio of bamboo charcoal in airtight surroundings was applied to determine the adsorption effect of bamboo charcoal made at different carbonization temperature (300 ~1000 ºC) [15].

Table 1.1: Absorption capacity of bamboo charcoal towards harmful substances [15].

S.

No.

   Solvents

     Used

 Boiling   point             of Solvent (ºC)

Best Bamboo charcoal fit for absorption of solvent

Absorption rate of Bamboo charcoal to solvent (%)

1.

  Methanol

   (HCHO)

        21

Bamboo charcoal carbonized at  900ºC

   19.39

2.

   Benzene  

     (C6H6)    

      80.1

Bamboo charcoal carbonized at 500ºC

      10.08

3.

Methyl-   benzene

(C6H8)

       110

     (volatile)

Bamboo charcoal carbonized at  500ºC

    9.65

4.

  Ammonia

      (NH3)

      -33.5

     (volatile)

Bamboo charcoal carbonized at  300ºC

     35.65

5.

Chloroform

    (CHCl3)

       61.2

     (volatile)

Bamboo charcoal carbonized at  300ºC

        40.68

  1. MATERIALS AND METHODS

2.1  Materials

2.1.1 Bamboo fiber bundles: Fibre bundles were extracted from Raw Bamboo [Botanical Garden of GNDU, Amritsar].

2.1.2 Chemicals used: All the chemicals used in this investigation are of AR grade and are purchased from Merck Ltd., Hi-media Labs, Bombay (India).

  • Acetone
  • Petroleum ether
  • Alcohol
  • Sodium sulphate
  • Sodium persulfate

2.2  Methods Used

2.2.1  Extraction of Fiber bundles

Raw culm of Bambusa vulgaris is harvested from Botanical Garden of Guru Nanak Dev University, Amritsar. The nodes of the raw bamboo (3 years old) are firstly separated. Then the remaining part is sliced in the longitudinal direction to the thin blocks with 10-15 cm in the length and 2-4 cm in the thickness by the slicer followed by the removal of its upper layer. Finally they are kept for drying at room temperature for four days.

Figure 2.1: Bamboo culms

Nodes of bamboo (3 years old) are separated.

Residual part is cleaved into longitudinal direction to thin blocks with 10-15 cm in length and 2-4 cm in thickness by slicer.

Then, finally they are kept for drying at room temperature as shown in the below figure.

IMG_20161213_143236411

Figure 2.2: Bamboo sliced culms

2.2.2  Preparation of Bamboo charcoal

2.2.2.1 Preparation of Bamboo charcoal using aluminium foil and spirit lamp

Bamboo bundles are wrapped with aluminium foil several times to protect it from air intact. A tiny hole is made at one side of the bamboo bundles wrapped with aluminium foil so as to prevent it from bursting. A wire-mesh is placed on the top of the spirit lamp and then position the aluminium wrapped bamboo on top of it. A spirit lamp is lighted up to dry the bamboo inside the foil. White smoke came out from this tiny hole and further turn in yellow colour with passage of time. When the colour of aluminium foil turns yellow, it indicates the completion of process. This yellow colour is caused by the bamboo tar [83]. Precaution parameter is that do not open the aluminium foil until it is cooled as heat can break the charcoal easily.  

Sequence:           

Step 1. Wrap the small bamboo bundles with aluminium foil several times so as to prevent it from air contact.

Step 2.  A tiny hole is made to the wrapped aluminium foil at one side to prevent it from bursting when the trapped air in it is expanded by the heat.

Step 3.  Place a wire mesh on top of the spirit lamp and position the aluminium wrapped bamboo on top of it.

Step 4.  Light up the spirit lamp to dry the bamboo inside the foil. White smoke came out from this tiny hole and further turn in yellow colour with passage of time.

Step 5. When the colour of aluminium foil turns yellow, it indicates the completion of process.

Rocess Sequence of Bamboo Charcoal

Figure 2.3: Process sequence for preparing of bamboo charcoal: (a) Bamboo bundles ; (b) Bamboo bundles wrapped with aluminium foil ; (c) Bamboo  bundles wrapped with aluminium foil with a tiny hole at a side ; (d) White smoke coming out from the tiny hole during pyrolysis step ; (e) Bamboo charcoal after pyrolysis.

2.2.2.2. Preparation of bamboo charcoal from bamboo using Muffle furnace

The dried bamboo culms are introduced into muffle furnace (SR NO: 096; MODEL NO: MF- 1450; TEMP MAX. 1450 °C) at constant temperature 600 °C for two hours, 90 min, 60 min, 45 min and 30 min. After that, it is kept for cooling at room temperature. The black mass so obtained after bamboo pyrolysis is then purified by solvent extraction using petroleum ether (non-polar solvent) and acetone (polar solvent) in the ratio of 1:1 for three number of runs in order to obtain pure form of bamboo charcoal. The solvent extraction is a method for separating a substance from a solution or mixture by dissolving it in another, immiscible solvents in which it is more soluble. The solvents used here are acetone (polar solvent) and petroleum ether (non-polar solvent) because they do not mix with the bamboo charcoal, so that when left undisturbed, they will form two separate layers.

Figure 2.4: Muffle furnace

Sequence:

Step 1.  Bamboo pyrolysis at 600 °C in muffle furnace with variation of time.

Step 2.  It is then kept for cooling at room temperature for 24 hours.

Step 3. Solvent extraction: The black mass obtained is purified by solvent extraction using petroleum ether and acetone as solvents in the ratio 1:1. This step is revised three times for obtaining a pure form of bamboo charcoal.

Process sequence of production of Bamboo Charcoal obtained by pyrolysing bamboo in muffle furnace

Figure 2.5: Process sequence of bamboo charcoal obtained by bamboo pyrolysis in muffle furnace: (a) Dried bamboo culms ; (b) Bamboo charcoal obtained after pyrolysis done in muffle furnace at 600 °C for 30 minutes ; (c) Bamboo charcoal obtained after pyrolysis done in muffle furnace at 600 °C for two hours.

2.2.2.3 Preparation of Artificial Sulphur contaminated water [16]

1.63 g, 2.38 g and 2.63 g amounts of sodium sulphate powder were weighed. These amounts of sodium sulphate powder were dissolved in 125 ml of water, respectively. Similarly, sodium per sulphate powder was weighed in amounts of 0.88 g, 1.63 g and 2.38 g. These amounts of sodium per sulphate powder were put into beaker which equipped with 125 ml water, respectively.

2.3  Characterisation of Bamboo charcoal

2.3.1  X-Ray Diffraction (XRD)                 

Crystallinity and crystal size of raw bamboo fibre bundles and pyrolysed bamboo fiber bundles are determined by PXRD technique in the Department of Chemistry, GNDU, Amritsar, using Rigaku Miniflex X-ray diffractrometer having CuKα source( λ = 1.54Ǻ ). Bamboo fibres are ground into powders as measuring samples. The obtained samples are scanned in the angle range i.e. 2 value of 20- 80° with an interval of 0.2°. The percentage of crystalline material in fibre sample is calculated as [17 85]:

  ×100

Where I002 is the maximum intensity of the (002) lattice diffraction (2 =22.1°) and Iam is the intensity at 2 = 15.7°. The standard size of crystallites is determined from following equation.

                    D(hkl)  =

Where (hkl) is the lattice plane, D(hkl) is the size of crystalline, K is the Scherrer constant (0.84), λ is the X-ray wavelength (0.94 nm), B(hkl) is the FWMH (full width half maximum of the measured hkl reflection, and 2 is the corresponding reflection angle [18].

2.3.2  Fourier Transform Infrared Spectroscopy                      (FTIR)

The functional groups components and consistency in the bamboo charcoal is determined by FTIR technique in the Department of Chemistry, GNDU, Amritsar using Varian 660 FT-IR having the spectral range from 400 to 4000 nm (at room temperature=20 °C) by mixing the sample into fine alkali halide powder (KBr) and then finally pulverized and put into a pellet-forming die.

2.4  Test Methods

2.4.1  Weight loss (%) 

The fiber weight loss is determined by ASTM Method D-5035 at a constant temperature 27 °C using below equation:

 

Where wi is the initial weight of the raw bamboo fiber and wf is the final weight of treated bamboo fiber.

2.4.2 Moisture Content (%)

The bamboo charcoal of dimensions 20mm×60mm×5mm are used to determine moisture content using oven-drying method in accordance with ASTM D 4442-84 using below equation:

 

Where wm is the weight of bamboo charcoal before oven-drying (g) and wo is the weight of bamboo charcoal after oven-drying (g). 

2.4.3 Adsorption behaviour of Bamboo Charcoal for sulphur containing solution [16 80]. 

Sodium sulphate powder is weighed in amounts of 1.63 g, 2.38 g and 2.63 g. These powder and 0.5 g of over dry bamboo charcoal are put into beaker which equipped with 125 ml water, respectively. It is stirred in a beaker for 20 min, 60 min and 80 min. Similarly, Sodium per sulphate powder is weighed in amounts of 0.88 g, 1.63 g and 2.38g. These powder and 0.5 g over dry bamboo charcoal are put into beaker which equipped with 125 ml water, respectively. It is stirred in a beaker for 40 min, 100 min and 120 min. Each bamboo charcoal is removed, dried and weighed, respectively [19].

  1. RESULTS AND DISCUSSION

3.1.  XRD analysis

Figure 3.1  showed the XRD patterns for bamboo fibres and bamboo charcoal; (a)  XRD of bamboo fibres, (b)  XRD of bamboo charcoal pyrolysed using aluminium foil, (c) XRD of bamboo charcoal pyrolysed in muffle furnace at 600 °C for 30 min, (d) XRD of bamboo charcoal pyrolysed  in muffle furnace at 600 °C for 45 min, (e) XRD of bamboo charcoal pyrolysed in muffle furnace at 600 °C for 60 min, and (f) XRD of bamboo charcoal pyrolysed in muffle furnace at 600 °C for 120 min. It is found that their patterns have similar diffraction peaks, but with different intensity. Additionally, their crystallinity degree has been calculated by dividing the crystallinity area by the total area formed by the curves in Figure 3.1. The crystallinity degree has been obtained 8.6%, 9.8%, 83.9%, 51%, 72.1% and 93.3% for bamboo fibres and pyrolysed bamboo charcoal using aluminium foil and in muffle furnace at 600 °C for 30 min, 45 min, 60 min and 120 min, respectively. Thus, when lignin and hemicelluloses, both of which are amorphous in nature are partially removed that leads to a improved packing of cellulose chains, crystallinity would be better with variation of time. According to the results obtained from XRD, the crystallinity index for bamboo charcoal obtained by pyrolysing bamboo in aluminium foil and pyrolysing bamboo in muffle furnace at 600 °C for 30 min, 45 min, 60 min and 120 min are 20.12 Ǻ, 28.31 Ǻ, 27.54 Ǻ, 31.34 Ǻ and 28.32 Ǻ, respectively.

The peaks of the XRD of bamboo charcoal obtained by pyrolysing bamboo in muffle furnace are sharp, clear and higher than the broad peak of XRD of bamboo charcoal obtained by pyrolysing bamboo using aluminium foil. This confirms the good extent of graphitization in former than in latter. In case of latter and raw material, the XRD patterns are similar. This indicates that they have almost same crystallinity degree. Figure 3.1(c) and Figure 3.1(d) shows similar diffraction behaviour. This indicates that the structure of cellulose in molecule level is fully destructed and methoxy groups in lignin are dislocated. Figure 3.1(e) shows less number of peaks than previous XRD spectras because in this case, the conjugation of C=O bond with the aromatic rings takes place. Figure 3.1(f) shows clear three peaks at 16°, 23° and 28°. This indicates the full aromatization of carbon in bamboo charcoal.  

             

  2 (degree) 

Figure 3.1 (a):  XRD pattern of raw bamboo fibres                       

2 (degree)

Figure 3.1 (b): XRD of bamboo charcoal pyrolysed using Aluminium foil

           

2 (degree)

Figure 3.1 (c):  XRD of bamboo charcoal pyrolysed in muffle furnace at 600 °C for 30 min                   

2 (degree)

Figure 3.1 (d):  XRD of bamboo charcoal pyrolysed in muffle furnace at 600 °C for 45 min

 2 (degree)

Figure 3.1 (e):  XRD of bamboo charcoal pyrolysed in muffle furnace at 600 °C for 60 min

   

2 (degree)

Figure 3.1 (f):  XRD of bamboo charcoal pyrolysed in muffle furnace at 600 °C for 120 min

2 (degree)

Figure 3.1 (g): Comparison of XRD spectra of raw bamboo and bamboo charcoal obtained by pyrolysing bamboo  using muffle furnace at 600 °C with variation of time.

2 (degree)

Figure 3.1 (h): Comparison of XRD spectra of raw bamboo, bamboo charcoal obtained by pyrolysis   bamboo in aluminium foil and in muffle furnace at 600 ̊C for 120 min.

The peaks obtained from the XRD spectra of bamboo charcoal prepared by pyrolysing bamboo in muffle furnace are sharp, clear and higher than the less intense peaks of XRD of bamboo charcoal obtained by pyrolysing bamboo using aluminium foil. This confirms the good extent of graphitization in former than in latter. In case of raw bamboo, the XRD patterns show a single broad peak. This corresponds to asymmetric stretching (=C-O-C) of vibrational mode, which originates from lignin.

3.1.2  FTIR analysis

FTIR spectrum of bamboo

For bamboo the FTIR spectroscopy (Figure 3.2(a)) provides information on the chemical structure of the material. Band assignments for the spectrum of bamboo are summarized in Table 3.1, indicate that bamboo contains a number of atomic groups and structures (OH, CH2, C=O, C-O-C and so on).

Table 3.1: FTIR spectrum for bamboo [20]

S.No.

   Band position (cm-1)

          Assignment

1.

  3625

O-H (stretching)

2.

   2910

C-H (stretching)

3.

   2360

C=O (stretching)

4.

   1585

C=C (stretching)

5.

   1434

CH3, CH2 (asymmetric bending)

6.

    1371

CH3 (symmetric bending)

7.

      1280

=C-O-C (asymmetric stretching)

8.

      1115

C-O (stretching)

9.

       669

C-H (bending out of plane)

10.

       618

O-H (bending out of plane)

The position and shape of the band at 3625 cm-1 are compatible with the involvement of the hydroxyl groups in hydrogen bonding. Otherwise, the band should be located at significantly higher wave numbers and much sharper. This is because that the bamboo contains OH-ether hydrogen bonds which absorb infrared radiation at 3300 cm-1. Other spectral bands connected with the OH groups, which appeared at lower wave numbers than 3625 cm-1 , are those caused by O-H ( bending in plane ), C-O ( stretching ) and O-H (bending out of plane) absorptions. These bands are mainly related to the structure of hemicelluloses and cellulose in bamboo, in addition to the bands at 1140 cm-1, 1115 cm-1 and 980 cm-1, considering the fact that the FTIR spectroscopy of cellulose has the strongest and characteristic spectrum bands at 1058 cm-1 with shoulder bands at 1162 cm-1, 1122 cm-1 and 985 cm-1, which originate from the absorptions of C-O (stretching) and O-H (bending). The band at 1585 cm-1 denotes the presence on bamboo of a high concentration of primary hydroxyl groups. In the range from 1600 cm-1 to 1420 cm-1 are attributed to skeleton stretching vibration of aromatic rings, which are mainly concerned with lignin in bamboo. The band at 1280 cm-1 corresponds to asymmetric stretching (=C-O-C) of vibrational mode, which originates from lignin. The high intensity of the band at 1585 cm-1 shows that bamboo has a lot carbonyl groups and this indicates that the C=O groups are not involved in  conjugation with double bond or aryl group in bamboo.

Figure 3.2 (a):  FTIR spectrum of raw bamboo. 

Figure 3.2 (b):  FTIR spectrum of bamboo charcoal, pyrolysed in aluminium foil.

Compared with FTIR spectrum of bamboo, for that of the product from bamboo pyrolysed in aluminium foil (Figure 3.2(b)), the bands at 3324 cm-1 and 1121 cm-1 become sharper and the band at 2360 cm-1 becomes single. The intensity of the band decreases at 2900 cm-1. This is due to that a large number of hydroxyl bonds are lost in bamboo by heating at such temperatures. Also, hemicelluloses in bamboo is partly decomposed into fractions, part of which escapes from bamboo.

Figure 3.2 (c): FTIR spectrum of bamboo charcoal, pyrolysed in muffle furnace at 600 °C for 30 min.

(Figure 3.2(c)) The structure of cellulose in molecule level is fully destructed and methoxy groups in lignin are dislocated. The intensity of the characteristic bands at 1160- 980 cm-1 of cellulose in bamboo is weak followed by the disappearance of the band at 1329 cm-1. This indicates that the decomposition of cellulose in bamboo is almost complete. The decrease of the band at 897 cm-1 is due to the complete destruction of pyranoid rings in cellulose. The band at 1375 cm-1 disappears because the methyl groups in bamboo are almost lost by heating. But the bands from 1600-1450 cm-1, which are related to aromatic nuclei in lignin, keep stable. Therefore, it is confirmed that the basic net structure in lignin is not destructed.

Figure 3.2 (d): FTIR spectrum of bamboo charcoal, pyrolysed in muffle furnace at 600 °C for 45 min.

The net structure of lignin is completely collapsed (Figure 3.2(d)), followed by that the more positions in aryl groups are substituted, based on the disappearance of the band at 1510 cm-1, which originates in the skeletal vibration, as well as the change of the relative intensity of a trio-bands at 780 cm-1, 810 cm-1 and 780 cm-1.

Figure 3.2 (e):  FTIR spectrum of bamboo charcoal, pyrolysed in muffle furnace at 600 °C for 60 min.

(Figure 3.2(e)) The band at 870 cm-1 becomes stronger where the bands at 810 cm-1 and 780 cm-1 become weaker with increase in time. The stretching band of C=O groups disappears and the band near 1600 cm-1 becomes broader attributed to the conjugation of C=O bond with the aromatic rings. The stretching band of CH groups disappears.

Figure 3.2 (f): FTIR spectrum of bamboo charcoal, pyrolysed in muffle furnace at 600 °C for 120 min.

The bamboo carbonization at 600 °C for 120 min (Figure 3.2(f)) indicates the full aromatization of carbon in bamboo charcoal. The decrease of the intensity of the band near 1600 cm-1 is due to the lower content of oxygen. The band at 2360 cm-1 becomes double and the band at 2919 cm-1 becomes sharp. From 1650-1320 cm-1, the bands become strong and sharp.

For bamboo the FTIR spectroscopy provides information on the chemical structure of the material. Band assignments for the spectrum of bamboo indicate that bamboo contains a number of atomic groups and structures (OH, CH2, C=O, C-O-C and so on). The FTIR spectra of bamboo charcoal pyrolysed using aluminium foil shows that the intensity of the band at 2900 cm-1 decreases. This is due to that a large number of hydroxyl bonds are lost in bamboo by heating at such temperatures. Also, hemicelluloses in bamboo is partly decomposed into fractions, part of which escapes from bamboo. The FTIR spectra of bamboo charcoal pyrolysed in muffle furnace at 600 °C for 120 min indicate the full aromatization of carbon in bamboo charcoal.

 

3.1.3  Weight loss (%)

(a) Weight loss (%) of Bamboo charcoal pyrolysed using aluminium foil.

Table 3.2: Weight loss (%) of raw bamboo and bamboo charcoal obtained by pyrolysis using muffle furnace.

S.no.

Material          

   Weight loss (%)

1.

Raw bamboo

      42.33

2.

Bamboo charcoal obtained by pyrolysis using aluminium foil

      69.61

(b) Weight loss (%) of Bamboo charcoal obtained by pyrolysis in muffle furnace at 600 °C with variation of time.

Table 3.3: Weight loss (%) of bamboo charcoal after pyrolysis in muffle furnace with variation of time.

S.no.

 Pyrolysis Time- period (min)

Weight loss (%)

1.

30

92.88

2.

 45

93.26

3.

  60

93.37

4.

 90

93.59

5.

  120

93.88

To optimized the time period of pyrolysis treatment, time variations was studied as shown in Table 3.3 (30 min, 45 min, 60 min, 90 min and 120 min). Maximum weight loss (%) was found in case of 120 min time period. Further, this optimized time period for pyrolysis method was compared with weight loss (%) in case of Bamboo charcoal pyrolysed using aluminium foil as shown in Table 3.2. Again, weight loss (%) was minimum in case of latter one. This occurs because of the removal of non-cellulosic substances in larger amount than in case of latter one.

3.1.4 Moisture Content (%)

(a) Moisture content (%) of Bamboo charcoal pyrolysed using aluminium foil

Table 3.4: Moisture content (%) of raw bamboo and bamboo charcoal obtained by pyrolysis using muffle furnace

S.no.

Material          

Moisture content (%)

1.

Raw bamboo

      75.68

2.

Bamboo charcoal obtained by pyrolysis using aluminium foil

      40.80

(b)  Weight loss (%) of Bamboo charcoal obtained by pyrolysis in muffle furnace at 600 °C with variation of time.

Table 3.5: Moisture content (%) of bamboo charcaol after pyrolysis in muffle furnace with variation of time.

S.no.

 Pyrolysis Time- period (min)

Moisture content (%)

1.

30

25.33

2.

45

22.36

3.

60

19.18

4.

 90

17.56

5.

120

15.87

To optimize the time period of pyrolysis treatment, time variations was studied as shown in Table 3.5 (30 min, 45 min, 60 min, 90 min and 120 min). Minimum moisture content (%) was found in case of 120 min time period. Further, this optimized time period for pyrolysis method was compared with moisture content (%) in case of Bamboo charcoal pyrolysed using aluminium foil as shown in Table 3.4. Again, moisture content (%) was minimum in case of former one.

3.1.5  Adsorptivity test analysis

Based on the above test, the results of adsorption are obtained and listed in Table 3.6, Table 3.7 and Table 3.8.

Table 3.6: Adsorption results of Raw Bamboo.

S.No.

Concentation of Sulfur Solution in water (%)

            Na2SO4

       (Sodium sulphate)

Concentration of Sulfur Solution in water (%)

Na2S2O8

(Sodium persulphate)

        Stir time ( min)

Stir time ( min)

    20

   60

   80

  40

  100

  120

1.

0.63

0%

0.02%

0.02%

0.09

0.12%

0.05%

0.32%

2.

0.24

0.02%

0.03%

0.05%

0.16

0.08%

0.10%

0.05%

3.

0.26

0.01%

0.20%

0.11%

0.24

0.15%

0.03%

0.09%

Based on Table 3.6, when the concentration of sodium sulphate in water is 0.63%, the adsorption of sulphur components by raw bamboo does not occurs for the stir time of 20 min but when the stir time approaches to 60 min, it shows 0.02% adsorption. No affect on adsorption rate occurs with increase in stir time of 80 min. This is because the adsorption gaps in the bamboo have been exhausted and equilibrium has been attained. For 0.24% concentration of sodium sulphate, the adsorption increases with increase of the stir time but for 0.26% concentration of sodium sulphate, the adsorption first increases and then decreases with increase in stir time. This is due to the attainment of saturation point by the pores available which causes decrease in adsorption with increase in stir time.

When the concentration of sodium per sulphate in water is 0.09%, it shows adsorption of 0.12% for the stir time of 40 min but increase of stir time to 100 min leads to decrease in adsorption. With further increase in stir time causes increase in adsorption (0.32%) of sulphur components by bamboo. When the concentration of sulphur solution increases in water from 0.12- 0.24%, it results in decrease in adsorption with increase in stir time.

Table 3.7: Adsorption results of Bamboo charcoal obtained by pyrolysis using aluminium foil.

S.No.

Concentation of Sulfur Solution in water (%)

Na2SO4

(Sodium sulphate)

Concentration of Sulfur Solution in water (%)

Na2S2O8

(Sodium persulphate)

Stir time ( min)

Stir time ( min)

20

60

80

40

100

120

1.

0.63

-0.07%

0.05%

0.05%

0.09

0.24%

0.10%

0.56%

2.

0.24

0.08%

0.18%

0.27%

0.16

0.20%

0.14%

0%

3.

0.26

0.08%

0.56%

0.28%

0.24

0.25%

0.08%

0.19%

Based on Table 3.7, when the concentration of sodium sulphate in water is 0.63%, the adsorption of sulphur components by bamboo charcoal obtained by pyrolysis bamboo using aluminium foil, does not occurs for the stir time of 20 min but when the stir time approaches to 60 min, it shows 0.05% adsorption. No affect on adsorption rate occurs with increase in stir time of 80 min. This is because the adsorption gaps in the bamboo have been exhausted and equilibrium has been attained. For 0.24% concentration of sodium sulphate, the adsorption increases with increase of the stir time but for 0.26% concentration of sodium sulphate, the adsorption first increases and then decreases with increase in stir time. This is due to the attainment of saturation point by the pores available which causes decrease in adsorption with increase in stir time.

When the concentration of sodium per sulphate in water is 0.09%, it shows adsorption of 0.24% for the stir time of 40 min but increase of stir time to 100 min leads to decrease in adsorption that is 0.10%. With further increase in stir time causes increase in adsorption (0.56%) of sulphur components by bamboo. When the concentration of sulphur solution increases in water from 0.12- 0.24%, it results in decrease in adsorption with increase in stir time.

Table 3.8: Adsorption results of Bamboo charcoal obtained after pyrolysis in muffle furnace at 600 °C for 120 min.

S. No.

Concentation of Sulfur Solution in water (%)

Na2SO4

(Sodium sulphate)

Concentration of Sulfur Solution in water (%)

Na2S2O8

(Sodium persulphate)

Stir time (min)

Stir time ( min)

20

60

80

40

100

120

1.

0.63

-0.09%

0.03%

0.03%

0.09

0.22%

0.09%

0.54%

2.

0.24

0.06%

0.16%

0.25%

0.16

0.19%

0.12%

0%

3.

0.26

0.06%

0.53%

0.25%

0.23

0.22%

0.06%

0.18%

Based on Table 3.8, when the concentration of sodium sulphate in water is 0.63%, the adsorption of sulphur components by raw bamboo does not occurs for the stir time of 20 min but when the stir time approaches to 60 min, it shows 0.03% adsorption. No affect on adsorption rate occurs with increase in stir time of 80 min. This is because the adsorption gaps in the bamboo have been exhausted and equilibrium has been attained. For 0.24% concentration of sodium sulphate, the adsorption increases with increase of the stir time but for 0.26% concentration of sodium sulphate, the adsorption first increases (0.53%) and then decreases (0.25%) with increase in stir time. This is due to the attainment of saturation point by the pores available which causes decrease in adsorption with increase in stir time.

When the concentration of sodium per sulphate in water is 0.09%, it shows adsorption of 0.22% for the stir time of 40 min but increase of stir time to 100 min leads to decrease in adsorption that is 0.09%. With further increase in stir time causes increase in adsorption (0.54%) of sulphur components by bamboo. When the concentration of sulphur solution increases in water from 0.12- 0.24%, it results in decrease in adsorption with increase in stir time.

The Sodium sulphate’s optimal adsorption condition is the concentration of 2.62 g/125 g for the stir time of 60 min and that of the Sodium persulfate’s optimal adsorption condition is the concentration of 0.88 g/125 g for the stir time of 120 min.

  1. CONCLUSION

Bamboo is known to be one of the most popular bio resources and its charcoal has an effective adsorbent property as desulphurisation characteristics from sulphur solution as well as for removal of humidity along with odours. In this work, bamboo charcoal is prepared using two different methods, (A) By pyrolysing bamboo using aluminium foil. In this case, the weight loss (%) of bamboo charcoal is 69.61%; moisture content (%) is 40.80% and the Sodium sulphate’s optimal adsorption condition is the concentration of 2.63 g/125 g for the stir time of 60 min and that of the Sodium per sulphate’s optimal adsorption condition is the concentration of 0.88 g/125 g for the stir time of 120 min. Second method is (B) By pyrolysing the bamboo pieces at 600 °C followed by purification by solvents. In this case, the weight loss (%) is 93.88%; moisture content (%) is 15.87% and the Sodium sulphate’s optimal adsorption condition is the concentration of 2.63g/125 g for the stir time of 60 min and that of the Sodium per sulphate’s optimal adsorption condition is the concentration of 0.88 g/125g for the stir time of 120 min, for the bamboo charcoal prepared in muffle furnace at 600 °C for 120 min. The XRD pattern of bamboo charcoal shows two intense peak at 25° and 44° which are assigned for (002) and (001) reflection respectively and confirms the good extent of graphitization. FT-IR spectra of bamboo charcoal carbonized at different interval of time can be applied to determinate the decomposition temperature of hemicelluloses, cellulose and lignin in bamboo. The following conclusion can be drawn:

For bamboo charcoal pyrolysed using aluminium foil, hemicelluloses in bamboo is decomposed and a large amounts of hydroxyl groups are dislocated from hemicellulose and cellulose, and then produce water to escape.

For bamboo charcoal pyrolysed in muffle furnace at 600 °C, the net structure of lignin completely collapses, followed by that the more positions in aryl groups are substituted, based on the disappearance of the band at 1510 cm-1, which originates in the skeletal vibration, as well as the change of the relative intensity of a trio-bands at 780 cm-1, 810 cm-1, and 780 cm-1.

Thus from the experimental observations it can be analysed that  bamboo can act as adsorbent for removal of sulphur from contaminated water.

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