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Study on extraction of bamboo fibres from raw

bamboo fibres bundles using different retting


techniques

Abstract:
Pure bamboo fibres have been extracted by using three different
retting techniques viz. chemical assisted natural retting(CAN),
acid retting and alkali retting. CAN and acid retted fibre bundles
were further scoured using various concentrations of sodium carbonate.
As the primary concern of this study was the end use of treated fibres for
textile application, therefore, lignin content, tensile strength, weight loss,
moisture content, whiteness and yellowness indices were measured.
Lignin content analysis of the fibre bundles obtained showed that there
was a remarkable reduction in lignin content after CAN retting.
Scanning electronic microscopy of the retted bamboo fibre bundles
showed removal of short elementary fibres from their surfaces in
appropriate amount which further improved their overall physical
properties of retted and scoured bamboo fibres.

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

2.1. Introduction
In textiles, market of natural bamboo fibre that is extracted directly from bamboo by
degumming process (retting), has risen due to its excellent properties like biodegradability,
antibacterial functions and anti-odor [1]. There are two ways to process bamboo to make the
plant into a fibre/fabric: mechanically [2] or chemically [3] as mentioned in earlier chapter.
Bamboo has emerged as a sustainable material for different uses like construction,
handicrafts, food. However, it is only recently that efforts have been made to produce textile
fibers from bamboo [4]. The worldwide research has been carried out on bamboo to study
the structure, properties and extraction methods of bamboo fibre [5]. For better penetration
of chemicals used in subsequent wet processing, separation of fibre bundles from the culm of
bamboo; need to undergo a process called retting. Retting is an essential stage for all types of
bast fibre extraction, especially in flax which is a combined effect of temperature, moisture,
bacteria or fungi and results in the fibrillation of the fibre bundle from gummy and
cementing non-cellulosic substances like hemicellulose, lignin and pectin [6].
Understanding the composition of bamboo is essential in order to establish the retting
process. The composition of bamboo is 45-55% cellulose, 20-30% lignin and 20-25%
hemicellulose, depending on the specific species [1]. The major limitation for use of bamboo
in textile industry is the presence of lignin and hemicellulose in it [7]. Therefore, these
compounds must be removed through a degumming process called retting. Retting for most
bast fibres occurs in the field with water, natural enzymes as well as sunlight and it takes
several weeks. Bamboo, however, cannot be field-retted because its fibres get rotten easily.
It requires chemical retting [6] or mechanical combing [8] and biological processes [9].
In this work, a possible bamboo retting system is developed and properties of retted
bamboo are also discussed. The extracted fibres were further characterized by calculating
weight loss, moisture content, whiteness & yellowness indices, lignin content measurement,
tensile strength and Scanning electron microscope (SEM).
2.2. Material and Experiments
2.2.1. Raw Bamboo (Figure 2.1a)
Raw bamboo (2-3 years old) was harvested from Botanical Garden, Guru Nanak Dev
University, Amritsar, India, and it was retted and extracted by following methods
2.2.2. Chemical assisted natural retting (CAN) (Figure 2.1b)
First of all, nodes of raw bamboo were detached and residual part was cleaved in
longitudinal direction to thin slabs with 15 - 20 cm in length and 1.5 - 2 mm in thickness by

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

the slicer. Finally, they were converted manually into fibre bundles. These bundles were then
immersed in Zn(NO3)2 solution using material to liquor ratio 1: 20 at 40 °C at neutral pH for
time period of 116 h in BOD incubator. Then they were boiled in water for one hour. The
concentrations of Zn(NO3)2 were 1%, 2% and 3% (owf).
2.2.3. Acid Retting (Figure 2.1c)
The bamboo fibre bundles with the same dimensions as mentioned above were
soaked in 1% HCl (owf) solution using material to liquor ratio 1 : 20 at room temperature for
45 min. Finally, they were washed with fresh water and dried under shadow.
2.2.4. Alkaline Retting (Figure 2.1d)
Alkaline retting was carried out by soaking the bamboo fibre bundles of same
dimensions as mentioned earlier in section 2.1.2, in 2 g/L Na2CO3 and 0.5% Lissapol D
solution using material to liquor ratio 1 : 20 at 80 °C for 45 min. Finally, they were washed
with fresh water and dried under shadow.

2.3. Optimization of Na2CO3 concentration for Scouring


The CAN, acid and alkaline retted bamboo fibers were treated with sodium carbonate
5-30 g/L, Lissapol-D 0.5 g/L and kept at 80 °C for 45 min with fiber to liquor ratio 1:20. The
concentrations of sodium carbonate were 5g/L, 10 g/L, 15 g/L, 20 g/L and 30 g/L. At the end
of scouring treatment, the fibers were neutralized with acetic acid After neutralizing, the
samples were rinsed successively with hot and cold water, detergent solution (70 °C, 5 min),
and finally rinsed in cold water and air-dried.
2.4. Testing
2.4.1. Tensile strength and weight loss
Breaking strength and breaking extension of bamboo were tested using an Instron
series IX fiber breaking strength machine in a constant 27 °C temperature and 65% relative
humidity using ASTM Method D-5035. Fiber weight loss was calculated using Eq. 1:
(1)

Where Wi is the initial weight of the raw bamboo fiber. Wf is the final weight of treated
bamboo fiber.
2.4.2. Moisture Content (T264-om-88)
After retting, scouring and drying, the fibres were weighed in a weighing bottle. The
weighed fibres were then dried for 2 hour in a preheated oven at 105 °C. After that the
samples were cooled in desicator and then replaced the stopper, followed by opening the

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

stopper for a moment to equalize the air pressure. The cooled samples were weighed again
and placed back to the oven for subsequent I hour. The cooling and weighing of these
samples were repeated as above for successive hourly periods until constant weight was
achieved.

Moisture content (M %) of bamboo fibers was calculated from equation (2) following as:

(2)

wi: Initial weight of the fibers


wf: Final weight of the fibers after drying
The colorimetric properties [10] of the retted fibers (D65 illumination, 10o observer) were
determined using a Spectraflash 600 colorimeter (Datacolor International).
2.4.3. Scanning electron microscopy
The deformation behavior of a single elementary retted bamboo fibre bundle was
investigated by scanning electron microscopy (SEM) using Quorum Q150RES (Supra 55-
CARLZEISS) equipment (EHT= 10.00 KV, Signal A= In Lens). All specimens with
longitudinal-section were coated with a thin layer of gold to avoid electrical charging.
2.4.4. Chemical analysis
The chemical composition of the original bamboo culm (without outmost layer) and
retted bamboo fibre bundles was analyzed for lignin contents by using TAPPI standard
T250-um-85.

2.5. Results and Discussion


2.5.1. Scanning electron microscopy
The surface properties of original & treated bamboo fibres were examined by SEM.
A large quantity of gum & lignin in untreated bamboo can be observed. As it can be seen in
Figures 2.1a, 2.1b, 2.1c & 2.1d, the natural bamboo fibre consists of numerous elementary
fibres. After natural retting, the number of elementary fibres is decreasing, meaning that the
technical bamboo fibre is getting finer. Moreover, the inner structure of bamboo fibre
becomes looser after treated with different retting techniques. As shown in all figures, clear
cracks can be observed for thus produced natural bamboo fibre, indicating that the fibre can
be easily separated into small bundles.

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

Soft fibres
Longitudinal
-section
Lignin

20µm 10 µm
Figure 2.1a. SEM images for side-view surfaces of Raw Bamboo fibre

Soft fibres/cells

100 µm Longitudinal-section

Figure 2.1b. SEM images for side-view surfaces of CAN retted bamboo fibre

Lignin

Soft cells
10 µm 20 µm

Figure 2.1c. SEM images for side-view surfaces of Acid retted bamboo fibre

Lignin
100 µm
Figure 2.1d. SEM images for side-view surfaces of Alkali retted
bamboo fibre
2.5.2. Optimization of Zn(NO3)2 concentration for CAN retting
Zinc nitrate was used to boost up the retting process of bamboo. The 1%
concentration of Zn(NO3)2 was selected in this study due to the better whiteness index
with improved physical and mechanical properties of fibers with 1% than other treated with
2% and 3% (owf) of Zn(NO3)2 (Table 2.1 & Figure 2.2). Finally, they were washed with
fresh water and dried under shadow.

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

Table 2.1: Physical and mechanical properties of bamboo fibre bundle with respect to ZnNO3
concentration

Concentration of Tenacity Whiteness Index Yellowness Index


ZnNO3 (owf) (g/den) (Hunter lab) (Hunter lab)
Untreated 2.8568 17.63 47.51
Zn(NO3)2 1% 1.8080 17.28 54.13

Zn(NO3)2 2% 1.7287 14.37 53.87


Zn(NO3)2 3% 1.7019 13.89 54.08

Figure 2.2. Physical and mechanical properties of bamboo fibre bundle with
respect to Zn(NO3)2 concentration

Table 2.2 shows the physical changes after different treatments. The removal of non-
cellulosic matter by retting process enhanced the fibre separation from the bulk. The process
also improved the ability of the fibres to absorb higher degree of moisture. Acid retting
process highly enhanced the fibre appearance as seen from its whiteness index value. The
drop in tenacity of the fibre was also comparatively low. Chemical assisted natural retting
caused highest loss in weight at the cost of maximum loss in tenacity (Figure 2.3a). The
maximum loss in lignin was caused by chemical assisted natural retting process. In CAN
retting, the natural microorganisms may start growing directly on the bamboo material. The
microbes take use of the gummy substances as a source of nutrition and grow on the plant
resources on a large scale. During growth in 116 h, enzymes may be secreted from the
microbes and catalyze the degradation of the gummy materials into small water soluble
molecules leading to the separation of fibres. Similar observations were made by Wang et al.

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

[11]. In the present study, Zn(NO3)2, has been used as booster or nutrient for natural
microorganisms to catalyze the degradation of gummy substances. By using CAN retting,
the interpenetrating network structure of bamboo gets broken into soluble molecules which
resulted in weight loss at the cost of loss in tenacity.
Alkali retting gave an intermediate effect on fibre appearance and strength of fibre.
Moisture content was also determined. The results showed that the difference of moisture
content of the acid treated and the alkali treated fibres was much lower than that of the
chemical assisted natural retted fibres. But physical fibre separation was achieved through
chemical assisted natural retting.

Table 2.2: Comparison of physical properties of CAN, Acid and Alkali retted fibres.

Type of Weight Moisture Whiteness Yellowness % Loss in


retting loss (%) content (%) Index Index Tenacity
Untreated 0 6.63 17.63 47.51 -

CAN 5.0 11.01 17.28 54.13 36.72%

Acid 4.0 8.50 29.24 36.88 10.81%

Alkali 4.1 8.70 21.20 51.08 23.91%

Figure 2.3a. Effect of CAN, Acid and Alkali retting on weight loss (%)
& loss in tenacity (%) of fibres

Properties of bamboo fibres depend on extraction conditions significantly. An


attempt has been made to produce textile fibre from bamboo [12]. The author stated that a
single bamboo fibre of 2 mm in length could be used in textile production in the form of a
fibre bundle. Lignin in bamboo fibre bundles is the main cause for yellow colour of fibres
and coarse fibre fineness. The bamboo single fibre of width 6–12 μm and the length 2–3 mm

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

was proposed for textile application. The structural morphology directly affected the fibre
properties, i.e. density, moisture regain, tenacity, dyeing and thermal properties, etc. [12].

Figure 2.3b. Effect of CAN, acid and alkali retting on whiteness &
yellowness indices of fibres

Figure 2.3c. Effect of CAN, acid and alkali retting on lignin content of
retted fibres

Natural bamboo fibres were chemically extracted by different retting techniques


during the present study. Reduced content of lignin, maximum weight loss and improved
moisture content of fibres in case of CAN retting is shown in Figure 2.3a and 2.3b. The
processing parameters or optimized condition for CAN retting was: - treatment in presence
of 1% (owf) Zn(NO3)2 using 1: 20 material to liquor ratio at 400C at neutral pH for 116 h in
BOD incubator. The fibres thus obtained had whiteness index 17.28, yellowness index
54.13, lignin and moisture 9% and 11% respectively. The acceptable limit for weight loss,
tenacity and yellowness indices depends on its area of application.

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

2.5.3. Optimization of Na2CO3 concentration


During scouring, Na2CO3 solution easily penetrate into fibres and so efficiently
reduce noncellulosic substances as it can softly break off the connectivity in between
noncellulosic (like lignin and gummy material) and cellulosic components. In order to obtain
the optimum sodium carbonate concentration for scouring, the pretreated (natural, acid &
alkali retted) bamboo fibres were treated with different sodium carbonate concentration viz.
5 g/L, 10 g/L, 15 g/L, 20 g/L 30 g/L and the solution was made with Lissapol D 0.5% (owf),
fibre to liquor ratio 1:20 and treated at 80 °C for 45 min followed by washing and finally
dried in open. After the treatment, the weight loss, moisture content, physical and
mechanical properties were tested to estimate the effect of sodium carbonate concentration.

2.5.4. Effect of Na2CO3 concentration on physical and mechanical properties


2.5.4.1. Effect of Na2CO3 concentration on weight loss of chemical assisted natural
retting, acid and alkali retted bamboo fibres

Table 2.3: Effect on weight loss of CAN, acid & alkali retted bamboo fibres

Concentration of Weight Loss (%)


Sodium carbonate pH of bath CAN retted Acid retted Alkali retted
(gpL) Fibre Fibres fibres
5 10.74 2.7 3 2.1
10 10.95 8.5 5.6 2.3
15 11.02 9.0 7.5 3.0
20 11.05 9.5 7.9 3.5
30 11.10 9.9 8.3 5.2

Table 2.3 & Figure 2.4 show that the weight loss value increased up to 10g/L, but
slightly decreased in natural retting when the concentration of sodium carbonate was
between 20g/L and 30g/L, and highly decrease in case of acid & alkaline retting. Minimum
loss in lignin was found in case of alkali retting which is the clear indication of less removal
of non-cellulosic material and resulting in less weight loss in comparison of CAN & acid
retting.
Alkali acts as a solubilising agent for lignin and hemicellulose and the later acts as a
cementing material for the cells of cellulose fibres. Rise in concentration of alkali caused rise
in the amount of hemicellulose removed. The open structure of CAN retted fibres was more
accessible for alkali (Na2CO3) which in turn caused high weight loss.

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

Figure 2.4. Effect on weight loss (%) of CAN, acid & alkali retted
bamboo fibres

2.5.4.2. Effect of Na2CO3 concentration on moisture content of natural, acid and alkali
retted bamboo fibres
Moisture content plays an important role in production of natural materials. It
directly affects the built-up process, manufactured goods properties as well as their
excellence. The result presented in Table 2.4 & Figure 2.5 exhibited that extracted fibres
from the acid and alkaline retting technique showed overall lower moisture contents than
natural retted fibres.

Table 2.4: Effect on Moisture Content (%) of CAN, acid & alkali retted bamboo fibres
Concentration of Sodium Moisture content (%)
Carbonate (gpL) CAN retted fibres Acid retted fibres Alkali retted fibres
5 6.2 4.2 5.7
10 7.14 5.7 6.3
15 7.84 7.0 7.14
20 8.1 7.8 7.89
30 8.3 8.1 7.93

It also shows that the moisture content value increased up to 15g/L, but slightly
decreased in natural & acid retting when the concentration of sodium carbonate was
between 20g/L and 30g/L, and highly decrease in case of alkaline retting.

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

Figure 2.5. Effect on Moisture Content (%) of CAN, acid


& alkali retted bamboo fibres

2.5.4.3. Effect of Na2CO3 concentration on whiteness index of natural, acid and alkali
retted bamboo fibres
The retted bamboo fibres were treated using various concentrations of stock solution
of sodium carbonate viz. 5 g/L, 10 g/L, 15 g/L, 20 g/L, 30 g/L and in the presence of
Lissapol D 0.5% (owf), fibre to liquor ratio 1: 20 and treated at 80 °C for 45 min followed by
washing and finally dried in open. After that the samples were tested for improvement in
whiteness.
Table 2.5: Effect on Whiteness Index of CAN, acid & alkali retted bamboo fibres

Sodium Carbonate Whiteness Index


Concentration (g/L) CAN retted fibres Acid retted fibres Alkali retted fibres
Control 17.28 29.24 21.20
5 14.91 12.00 7.86
10 9.23 8.95 4.95
15 7.19 8.70 4.41
20 5.07 4.71 4.07
30 4.91 0.11 2.26

Figure 2.6. Effect on Whiteness Index of CAN, acid & alkali


retted bamboo fibres

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

It is found (Table 2.5 & Figure 2.6) that with increase in concentration of stock
solution, the whiteness of the sample is decreased up to 20 g/L. Further increase showed an
increasing effect on whiteness in case of natural and alkaline retting, but a steep fall has been
observed in case of acid retting. Increasing concentration of alkali causes breakdown of
some chemical linkages present in bamboo and this involves sometimes scission of the
occasional bonds between lignin and cellulose/hemicellulose chain and methoxyl splitting
from the lignin constituents which ultimately lead to the formation of orthoquinones and
other chromophores which causes yellowing and decreases whiteness of fibres.

2.5.4.4. Effect of Na2CO3 concentration on yellowness index of natural, acid and alkali
retted bamboo fibres
The yellowness indices of treated samples were measured at different concentrations
of sodium carbonate and the results are shown in Table 2.6 & Figure 2.7. From both the
table and figure, it is clear that all three processes of retting followed by treatment with
different concentrations of sodium carbonate have a major drawback of yellowing in alkaline
baths.
Table 2.6: Effect on Yellowness Index of CAN, acid & alkali retted bamboo fibres

Sodium Carbonate Yellowness Index


Concentration (g/L) CAN retted fibres Acid retted fibres Alkali retted fibres
0 54.13 36.88 51.08
5 59.17 48.73 53.56
10 63.21 53.40 56.39
15 63.97 58.81 62.81
20 65.34 60.92 65.30
30 67.88 66.38 67.02

Figure 2.7. Effect on Yellowness Index of CAN, acid & alkali


retted bamboo fibres
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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

2.5.4.5. Effect of Na2CO3 concentration on tenacity of natural, acid and alkali retted
bamboo fibres
The average tenacity of natural bamboo fibres after different treatments have been illustrated
in Table 2.7 & Figure 2.8. With the increase in the treatment intensity, the values of average
tenacity initially decreased upto 15gpL. The reduction in tenacity is due to removal of non-
cellulosic material. But the concentration higher than 15g/L found to be less effective. Initial
loss was due to removal of non cellulosic mater. Further increase in alkali concentration
must have opened the micro level structure led to symmetrical distribution of load.

Table 2.7: Tenacity (g/den) of CAN, acid & alkali retted bamboo fibres

Sodium Carbonate Tenacity at maximum (g/den)


Concentration (g/L) Natural retting Acid retting Alkali retting

0 1.808 2.5479 2.174

5 1.446 2.0266 1.6335

10 1.464 1.8019 1.2602

15 1.4063 1.4962 1.2571

20 1.6005 1.9941 1.8989

30 1.7955 1.978 1.9700

Figure 2.8. Tenacity (g/den) of CAN, acid & alkali retted bamboo fibres

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Chapter 2: Study on extraction of bamboo fibres from raw bamboo fibres bundles using different retting
techniques

2.6. Conclusion
In this study, the CAN, acid and alkaline retting methods were used to extract
bamboo fibres bundles from raw bamboo fibre bundles and the effect of different
concentrations of sodium carbonate on physical properties of fibres. CAN retting technique
has been found the effective pretreatment in wet processing of bamboo fibres. After CAN
retting, the fibres were found to be much cleaner and finer. Maximum physical fibre
separation was achieved through chemical assisted natural retting. It is also clear from the
major loss in weight

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Xiaojun, H.; Xushan, G. Textile Res. J. 2010, 80, 333.
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