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A Novel Chemical Degumming Process for Ramie Bast Fiber

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DOI: 10.1177/0040517510373632

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 Textile Research Journal Article

A Novel Chemical Degumming Process for Ramie Bast Fiber

Xiu-Shan Fan, Zhong-Wen Liu and
Abstract A novel chemical degumming process Zhao-Tie Liu1
for ramie fiber was developed, using sodium car- Key Laboratory of Applied Surface and Colloid Chemistry
bonate solution with poly(vinyl alcohol) (PVA) as (Shaanxi Normal University), Ministry of Education,
an auxiliary surfactant and sodium triphosphate. Xi’an 710062, P. R. China and School of Chemistry &
Optimum performance for the degumming of ramie Materials Science, Shaanxi Normal University,
fiber was obtained with sodium carbonate con- Xi’an 710062, P. R. China
centration 30 g·L–1, PVA concentration 2.2 g·L–1,
sodium triphosphate concentration 6.0 g·L–1 and
Jian Lu
temperature 90 °C. The tensile properties of the
Key Laboratory of Applied Surface and Colloid Chemistry
ramie fibers degummed using Na2CO3 are compa-
(Shaanxi Normal University), Ministry of Education,
rable with fibers degummed using sodium hydrox-
Xi’an 710062, P. R. China
ide. This new mild, rapid degumming technique for
ramie fiber has a potential application in industry,
and is less environmentally polluting than the tradi-
tional method. The ramie fibers before and after
degumming were characterized by FT-IR, thermo-
gravimetric analysis, differential scanning calorime-
try, and scanning electron microscopy.

Key words ramie fiber, chemical degumming,

sodium carbonate, auxiliary surfactant, tensile
property

Introduction There are several types of degumming processes including

chemical and bacterial enzyme degumming [7–11]. In the
process of bacterial enzyme degumming, fungal or bacte-
Ramie is a member of the bast family, grown mainly in rial enzymes [12–15] attack the plant pectic materials while
temperate and tropical areas, and well known as “China
the stems are spread on the ground. The advantages of the
grass” in Western Europe and America due to the large
bacterial enzyme degumming process are its simplicity and
production in China [1]. As one of the most important nat-
low cost, but environmental factors such as temperature
ural fibers, the cellulose content of ramie is higher than in and moisture can easily affect degumming efficiency. The
other bast fibers such as hemp, flax and jute [2]. Ramie
main disadvantage of this process is the risk of fiber dam-
produces one of the strongest and longest plant fibers, and
age by cellulolytic enzymes secreted by the microbial flora
is lustrous with an almost silky appearance. Thus ramie fib-
acting on the fibers [16].
ers are used for clothing fabrics, industrial packaging, Another typical procedure is chemical degumming. In
twines, cordage, canvas, car outfits, etc. [3–5]. However,
this traditional degumming process, the gums, waxes and
the stem of ramie contains a large amount (20–30 wt%) of
other materials that remain coated on the processed bast
gummy matter comprising pectin and other non-cellulosic
fibers are removed by chemical means [17–20]. The deg-
materials. The gummy substance is commonly amorphous, umming of bast fibers is carried out on an industrial scale
with a degree of polymerization of 200–400 [6].
The removal of heavily coated, gummy material from
the cellulosic part of plant fibers is called “degumming”
1
and is necessary prior to industrial utilization of fibers. Corresponding author: email: ztliu@snnu.edu.cn

Textile Research Journal Vol 80(19): 2046–2051 DOI: 10.1177/0040517510373632 © The Author(s), 2010. Reprints and permissions:
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 A Novel Chemical Degumming Process for Ramie Bast Fiber X.-S. Fan et al. 2047 TRJ

by treating the coarse fibers with alkali solutions (such as
NaOH) containing wetting and reducing agents. Following
a soaking period, the fibers are boiled, neutralized and
washed several times. The fibers are then dried and treated
with softeners such as glycerol or wax to prevent them from
becoming brittle. The traditional chemical treatment of
fibers is believed to be heavily polluting and to cause seri-
ous environmental threats, in addition to requiring high
energy consumption [16]. Moreover, in the traditional deg-
umming process the strong alkali (NaOH) produces signif-
icant fiber damage that can affect subsequent processing.
With rising energy costs due to the scarcity of energy
resources, and deterioration of the environment beyond a
tolerable level, there is an urgent need to develop alterna-
tive, environmentally friendly processes for degumming
and processing bast fibers.
Despite its excellent properties and diverse applica-
tions, ramie fiber has failed to become a major textile crop,
mainly due to difficulties associated with processing of the
fiber. In the present study, ramie fiber was decorticated in
a solution of sodium carbonate together with polyvinyl
alcohol (PVA; Mw 85000–88000 g mol–1) and sodium tri-
phosphate. In this mildly alkaline solution the gummy
materials were easily removed, with much less environ-
mental pollution than results from traditional chemical
degumming. The properties and performance of the deg-
ummed fibers were evaluated in terms of weight loss and
other basic characteristics of the fiber. The tensile proper-
ties of ramie fiber degummed using sodium carbonate
were comparable with those of ramie fiber degummed with
sodium hydroxide.
Experimental
troscopy was performed using a Nicolet 870 spectrometer,
taking 32 scans for each sample. Fibers and KBr were care-
fully dried before disk preparation and subjected to FT-IR
analysis immediately after disk preparation. Scanning elec-
tron microscopy (SEM) observations on ramie and ramie
fibers were carried out using a Philips Quanta 200 instru-
ment. Differential scanning calorimetry (DSC) and ther-
mogravimetric analysis (TGA) were performed with a
model Q600SDT thermoanalyzer system. The heating/
cooling rates are 20 °C/min. Tensile properties were deter-
mined by universal material testing machine and the test
method used was according to the previous report [21].
Process for the degumming of ramie
Wet ramie (2.0 g) was boiled in sodium carbonate solutions
with a range of concentrations, with surfactant. Boiling was
continued for 6 h, and the solution was maintained at the
liquor:sample ratio 50:1. The degumming of ramie in
sodium hydroxide was carried out at 80 °C with the same liq-
uor/sample ratio for 2.5 h. The fiber was then washed thor-
oughly with distilled water, until the washings were neutral,
then dried.
Results and Discussion
Optimization of the reaction conditions
The effect of sodium carbonate concentration on weight loss
is shown in Figure 1. The ramie fiber weight loss increased
with increasing concentration of alkali from 0 to 30 g·L–1,
and remained essentially constant with further increase in
Na2CO3 concentration.

Materials
The ramie was supplied by Hu’nan Yuanjiang Mingxing
Co. Ltd. and cut into 3 cm lengths. Sodium carbonate,
PVA, and sodium triphosphate were obtained from Xi’an
Chemicals Co. Ltd. All chemicals were AR grade and were
used without further purification.

Characterization
The weight loss of the sample was determined by measur-
ing the differences in weight between the degummed and
the decorticated ramie, expressed as a percentage after the
sample reached constant weight by drying for 1 h at 100 °C.
The residue of gum was also determined by measuring the
difference in weight between the degummed ramie fiber
before and after treatment with NaOH.
For FT-IR analysis the fibers were pounded in a mortar Figure 1 The effect of sodium carbonate concentration on
cooled with liquid nitrogen and 1 mg of sample powder ramie weight loss.
was dispersed in 150 mg potassium bromide. FT-IR spec-
TRJ 2048 Textile Research Journal 80(19)

From these results it appears that the gummy materials

dissolved in the alkali solutions. At low concentration of
sodium carbonate the non-cellulosic materials began to
dissolve, and the gummy materials dissolved to an increas-
ing extent as the Na2CO3 concentration increased. When
the gummy materials were completely dissolved the weight
loss became independent of Na2CO3 concentration.
The weight loss of ramie fiber was investigated at tem-
peratures from 30 to 110 °C, at constant Na2CO3 concen-
tration (30 g·L–1). The results reveal (Figure 2) that the
weight loss of ramie fiber increased with increasing tem-
perature, and became constant above 90 °C.
This trend can be explained by increasing solubility of
the gummy materials in sodium carbonate solution with
increasing temperature. At higher temperature, the equi-
librium solubility of pectin in sodium carbonate solution
was reached, leading to temperature independent weight
loss. Figure 3 The relationship between weight loss and PVA
PVA acted as an anti-deposition agent in this procedure concentration.
and prevented the gummy materials from re-depositing on
the surface of the fibers. The optimum concentration of
PVA can be evaluated from the residue of gum. Figure 3
shows that the residue of gum decreased with increase of
the concentration of PVA up to 2.2 g·L–1.
At higher concentrations of PVA, the PVA coats the
surface of ramie, thus hindering interaction between
sodium carbonate and gummy materials. Thus the residue
of gum remains constant at higher PVA concentrations.
The penetrating agent (sodium triphosphate, in these
experiments) plays an important role in the degumming of
ramie fiber, because it can improve the interaction between
fiber and alkali solutions. Weight loss is shown as a function
of sodium triphosphate concentration in Figure 4. The

Figure 4 The relationship between weight loss and con-

centration of sodium triphosphate.

graph shows that the weight loss increased with increase of

Figure 2 The relationship between weight loss and tem-
perature at constant Na2CO3 concentration.
sodium triphosphate concentration up to 6.0 g·L–1, and
remained constant with further increase of sodium triphos-
phate concentration.
This trend may be due to the emulsifying and penetrat-
ing ability of sodium triphosphate. At high concentrations
of sodium triphosphate most of the gummy materials were
removed, and the weight loss became invariant at concen-
trations above 6.0 g·L–1.
 A Novel Chemical Degumming Process for Ramie Bast Fiber X.-S. Fan et al. 2049 TRJ

Figure 6 TG curves of (a) ramie, and (b) ramie fiber.

Figure 5 FT-IR spectra of (a) ramie, and (b) ramie fiber.

FT-IR analysis
Ramie is a mixture of ramie fiber, hemicellulose, lignin, gum
and other components. Pectin is a heterogeneous group of
acidic structural polysaccharides that have complex structure.
After degumming the residue is nearly pure ramie fiber. It is
commonly recognized that ramie fiber consists of linear mac-
romolecules formed by β-D-anhydroglucose units linked by
1,4-glucosidic bonds [22] The IR spectra of ramie before and
after degumming are shown in Figure 5.
The spectrum of the ramie fiber (curve b) exhibited O–
H stretching absorption around 3403 cm–1, C–H stretching
around 1645 cm–1 and 2900–3000 cm–1, and C–O–C
stretching around 1063 cm–1 and 1105 cm–1.
These absorption bands are consistent with those of a
typical cellulose backbone [23]. In the structure of ramie, Figure 7 DSC curves of (a) ramie, and (b) ramie fiber.
there are many other non-cellulose substances such as
hemicellulose, pectin and lignin which contain chemical
bonds such as O–H, C–O–C, C–H etc, thus the corre-
sponding intensities in the spectrum of ramie are higher as may be due to the different complexity of the two materials.
compared with that in ramie fiber. From the spectra of Ramie is a mixture and ramie fiber is nearly a pure sub-
ramie fiber we can draw conclusion that the mainly non- stance, and the hemicellulose, lignin and gum in ramie
cellulose substances were removed from ramie. decomposed at lower temperatures than the cellulose.
The main weight loss region for ramie was 250 to 390 °C,
while the principal weight loss region for ramie fiber was 280
Thermal analysis to 390 °C. Thus the onset temperature of weight loss for
Weight loss curves and DSC data for ramie and ramie fiber ramie was lower than that of the ramie fiber (Figure 7).
are shown in Figures 6 and 7, respectively. Figure 6 shows The differences in the temperature ranges of weight
similar weight loss trends for the two materials during loss of ramie and ramie fiber are due to the different struc-
decomposition. However, there were differences in the tures of ramie and ramie fiber. The non-cellulosic material
weight loss region between ramie and ramie fiber. decomposed at low temperatures, leaving residual ramie
From room temperature to 150 °C the percentage weight fiber, thus the residues decomposed for the most part at
loss of ramie decreased faster than that of ramie fiber. This the same temperature.
TRJ 2050 Textile Research Journal 80(19)
Figure 8 SEM micrographs of ramie (a, 300×) and ramie fiber (b, 3000×, Na2CO3; c, 1200×, NaOH).
Surface morphology
SEM micrographs of ramie and ramie fiber (produced by
Na2CO3 and NaOH) are shown in Figure 8. The surface of
ramie (Figure 8a) was rough and coarse, and treatment with
sodium carbonate solution removed the encrusting materi-
als, resulting in fibers with smooth surface (Figure 8b). Fig-
ure 8c shows the photo of ramie treated by NaOH, which
also shows a smooth surface. It means that the possibility of
ramie degumming in Na2CO3 solution was as feasible as
the traditional method using NaOH solution.
The main component of the gummy substances is pec-
tin, which behaves as an intercellular adhesive. Pectin is a
very complex polysaccharide in which glycosidic linkages
can form fragments of lower molecular weight upon treat-
ment with alkali. The lower molecular weight materials can
easily dissolve in weak, hot alkali solution, so that after
washing the ramie fibers remained.
Tensile properties
The tensile properties of ramie degummed in NaOH and
Na2CO3 solution are given in Table 1.
Table 1 Tensile properties of ramie degummed in NaOH
and Na2CO3.
Medium Stress (cN/dtex) Residue of gum (%)
NaOH 3.96 1.21
4.12
3.89
Na2CO3 4.23 1.27
4.06
4.26
The stress of ramie fiber degummed in sodium carbonate
solution were greater than the corresponding properties of
ramie degummed in NaOH, and there was almost the same
amount of gum residue from the two methods of treatment.
This may be due mainly to the alkalization differences
between NaOH and Na2CO3. NaOH is a strong alkali, and
in the process of degumming with NaOH the fibers are dam-
aged to a greater extent than in treatment with Na2CO3.
Thus, the ramie that was degummed with NaOH solution
had poorer tensile properties.
Conclusion
The biomass of ramie can be successfully degummed in
sodium carbonate solution with PVA and sodium triphos-
phate. The process is mild compared to the traditional
chemical degumming process. The tensile properties of the
degummed ramie fiber were comparable to those of ramie
degummed using sodium hydroxide, which is traditionally
used. Thus, this mild, rapid degumming technique with
NaCO3 for the biomass of ramie has potential application
in industry, and further work is ongoing.
Acknowledgments
The authors gratefully acknowledge the financial support
of the Specialized Research Fund for the Doctoral Pro-
gram of Higher Education (20070718003) and the Natural
Science Foundation of Shaanxi Province (2007B07).
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