preparationandcharacterizationof naturalbamboofiber

PBM • Natural Bamboo Fiber

Vol.5, No.2, 2020

Preparation and Characterization ofNatural Bamboo Fiber

Kaixuan Li1, Qingxian Miao1,*, He Zhao1, Jiawei Yang1,Haitao Cheng2, Lihui Chen1,*

1. College of Material Engineering, Fujian Agriculture and Forestry University, Fuzhou, Fujian

Province, 350100, China

2. International Centre For Bamboo and Rattan, Beijing, 100102, China

Abstract: In this study, natural bamboo fiber was prepared combining

chemical pretreatment with mechanical disc refining, opening, and carding.

An orthogonal experiment was designed based on four factors and three

levels; thereafter, the manufacturing process was optimized. The length,

diameter, tensile strength, and elastic modulus of the bamboo fiber were

determined, and the crystallinity and morphology of the fiber were analyzed

using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The

results showed that the optimum parameters for the chemical pretreatment

were a cooking temperature of 130℃ , heating time of 2 h, NaOH dosage of

2%, and Na2SO3 dosage of 10%. The cooking yield of bamboo chips was

89.5%, and the carding yield of natural bamboo fiber was 43.0% under the

optimum conditions. The length, diameter, tensile strength, and elastic

modulus of the obtained fiber were 36.71 mm, 0.285 mm, 407 MPa, and 27.7

GPa, respectively. XRD analysis and SEM observations showed that the

technology used in this study can produce bright and compact natural

bamboo fibers with high crystallinity.

Keywords: natural bamboo fiber; chemical pretreatment; disc refining;

sulfonic acid group; yield

DOI: 10.12103/j.issn.2096-2355.2020.02.004

1 Introduction

In recent years, the development and utilization of natural fibers has attracted

considerable attention [1-3]. Natural fibers can be prepared with bamboo, sisal, flax,

ramie, banana, and other resources [4-7]. Compared with other natural fibers, bamboo

Received: 19 February 2020; accepted: 17 March 2020.

Kaixuan Li, master candidate;

E-mail: [email protected]

*Corresponding author:

Qingxian Miao, professor;

research interest: pulping and

papermaking engineering;

E-mail: miaoqingxian@163.

com

*Corresponding author:

L ihu i Chen , p ro fes so r ;

research interest: plant fiber

chemistry & new materials;

E-mail: [email protected]

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Vol.5, No.2, 2020


fibrils have the advantages of high aspect ratio and

high specific strength. Bamboo is a type of fast-

growing grass plant that is widely cultivated in China

and is considered to be a promisingly renewable and

sustainable fiber resource [8]. Bamboo fiber can be

divided into two types according to different

preparation methods [9]. The first kind of bamboo fiber

is natural bamboo fiber, which is produced using

mechanical or physical methods combined with mild

chemical treatment. The other type of bamboo fiber is

viscose fiber, which is prepared by using intense

chemical treatment that includes alkaline cooking and

multi-stage bleaching. These two types of fiber differ in

morphology, crystallinity, and thermal stability [10].

Natural bamboo fiber has a higher yield, higher

cellulose crystallinity, and higher thermal stability than

viscose bamboo fiber. Natural bamboo fiber can be

regarded as the more real environment-friendly natural

fiber because it requires very few use of chemicals

during production. Thus, natural bamboo fiber can be

applied in the fields of textiles, composite materials,

pipelines, and mattresses, among others.

Nowadays, the preparation of natural bamboo fiber

involves mild chemical pretreatment of bamboo chips,

mechanical grinding, a second stage of chemical

treatment, mechanical opening, mechanical carding,

and final drying [11]. Studies have focused on further

refining natural bamboo fiber by subsequent biological

treatment [12-13]. Differences in length, diameter, yield,

and mechanical properties of natural bamboo fibers are

apparent using different manufacturing technologies [14-16].

Natural bamboo fiber can be extracted with a low

efficiency by partial removal of hemicellulose and

lignin with a steam explosion technique [17]. Natural

bamboo fiber can also be obtained by the partial

removal of lignin and hemicellulose by chemical

pretreatment with alkali or acid. The natural bamboo

fiber was prepared by soaking the bamboo in 1%

NaOH solution at 70℃ for 10 h following the

mechanical treatment. The obtained natural bamboo

fiber with a diameter of 230 µm and fiber strength of

395 MPa was more suitable for preparing composite

materials than the bamboo fiber extracted using the

steam explosion method [18-19]. However, some

disadvantages, including a long manufacturing process,

low production efficiency, and high cost, restrict the

application of natural bamboo fiber. Therefore, it is

particularly urgent and important to develop an

efficient manufacturing technology for natural bamboo

fiber.

In this study, natural bamboo fiber was manufactured

using mild chemical pretreatment followed by

mechanical refining treatments. The process, shown in

Fig.1, is as follows: the bamboo chips were first

chemically pretreated with mild alkaline sodium sulfite

and then mechanically refined with a wide disc gap;

finally, the fiber bundle obtained after disc refining was

opened and carded. Compared with the traditional

technique for natural bamboo fiber preparation, which

usually adopts strong alkali pretreatment for an

extended period followed by mechanical rolling, the

technique in this study has the advantages of being

environmentally friendly in addition to providing a

high production efficiency, high fiber yield, and high

fiber quality.

2 Experimental

2.1 Materials

The bamboo (sinocalamusaffinis) used in this study

was three years old and was purchased from

Chongqing, China. It was cut into bamboo chips with a

length of 40~70 mm before chemical treatment.

2.2 Chemical pretreatment of bamboo chips

The chemical pretreatment of bamboo chips was

carried out in a 10-L circulating vertical cooking

vessel, loaded with 1000 g of raw material with a liquid

ratio of 1: 5. The orthogonal experimental design was

devised using an L16 (45) table, as shown in Table 1. The

cooking temperature (CT), heating time (HT), NaOH

dosage (N1), and Na2SO3 dosage (N2) were considered

as four factors, and the yield after cooking, carding,

and sulfonic acid group content were used as the

evaluation parameters. The control sample was

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Vol.5, No.2, 2020


obtained using the aforementioned treatment method

without adding chemicals.

2.3 Mechanical treatment of bamboo chips

The chemically pretreated bamboo chips were

mechanically refined on a high-consistency disc refiner

(KRK, Japan) with a refining gap of 1.5 mm. After disc

refining, the fiber bundle was dried, and then further

dispersed and refined on an opener and a carding

machine to obtain bamboo fibers.

2.4 Determination of bamboo fiber yield after chemi‐

cal pretreatment and carding

After fully soaking and washing, the pretreated bamboo

chips were air-dried and then placed in a sealed bag for

24 h to equilibrate the moisture; the moisture content

was then measured, and the yield of the bamboo chips

was calculated.

The fibers remaining on the carding machine and the

bamboo fibrils obtained by carding were collected, the

moisture content was determined, and the fiber yield

after carding was calculated based on the oven-dried

bamboo chips at the time of chemical pretreatment.

2.5 Determination of sulfonic acid group content

After chemical pretreatment, the bamboo chips were

washed and then soaked in water for 48 h; thereafter,

the bamboo chips were dried and ground. A 3-g sample

of bamboo powder, with a particle size of 40~60 mesh,

was taken to determine the sulfonic acid group content.

The 3-g sample of oven-dried bamboo powder was

soaked in 100 mL of 0.1 mol/L HCl for 45 min; this

procedure was then repeated for a further 45 min, with

the aim of converting the salt base to acid. The bamboo

powder was then washed with deionized water

(conductance <1.0 μS/cm) that did not contain any

carbon dioxide to achieve a stable conductance in the

range 1.3~1.5 μS/cm. After draining, the bamboo

powder was completely dispersed in 450 mL of

0.001 mol/L NaCl solution and then titrated with

NaOH standard solution under a nitrogen atmosphere

with electromagnetic stirring. The titration speed was

0.1 mL/min. Finally, the bamboo powder was fully

washed with deionized water and dried to a constant

weight. The titration curve was recorded by a

conductivity meter (Mettler Toledo, China). The

sulfonic acid group content was calculated according to

Equation (1) below.Sulfonic acid group content ( mmol/kg sample ) =

c2V2 - c1V1

m× 1000 (1)

where, c1 is the concentration of the HCl standard

solution, mol/L; V1 is the volume of the added HCl

standard solution, mL; c2 is the concentration of the

NaOH standard solution, mol/L; V2 is the consumed

volume of the NaOH standard solution at the first

equivalence point, mL; and m is the mass of the oven-

dried sample, g.

2.6 Determination of natural bamboo fiber proper‐

ties

Approximately 100 fibers were selected at random to

determine the properties of natural bamboo fiber. The

Fig.1 Process flow chart of natural bamboo fiber preparation

Table 1 Orthogonal experimental factors of chemicalpretreatment of bamboo chips

Levels

1

2

3

4

Value range of each factor

CT/℃100

115

130

145

HT/h

1

1.5

2

2.5

N1/%

2

3

4

5

N2/%

6

8

10

12

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Vol.5, No.2, 2020


fiber length was measured using a Verniercaliper. One

end of the fiber was placed on a flat board and secured

with double-sided tape, and the other end was

straightened to enable the measurement of length.

The fiber diameter was determined by epoxy resin

embedding. Randomly selected fibers were placed at

one end of the paper, coated with epoxy resin, and then

covered with the paper. After the epoxy resin had

completely cured, the surface was scraped off with a

blade to expose the fiber and the cross-sectional area

was measured with an optical microscope to determine

the fiber diameter [20]. Fifty fibers were used in each

group.

The fiber tensile strength was determined using an

universal tester (Instron, America) at 25℃ and a

relative humidity of 40%~50%. The fiber stretching

rate was 2 mm/min. The test was carried out in

accordance with the international standard "ASTM

D3822 Standard test method for tensile properties of

single textile fibers"; approximately 30 fibers were

used in each group.

2.7 Determination of natural bamboo fiber crystallinity

The crystallinity of natural bamboo fiber was

determined based on the X-Ray diffraction (XRD)

method on an Ultima Ⅳ spectrometer (Japan). The X-

ray generator (voltage 40 kV, current 30 mA) is

equipped with a Cu tube. Samples were scanned in the

range of 2θ=5° ~60° . A step size of 2°/min was used

during the measurements. The calculation of

crystallinity was carried out based on the following

Equation (2) according to the Segal method [21].

X-ray crystallization index =I002-Iam

I002

× 100% (2)

where, I002 is the maximum diffraction intensity of the

002 interference; Iam is the diffraction intensity of 2θ =

18 °.

2.8 Scanning electron microscopy (SEM) observation

of bamboo fibers morphology

The morphology of bamboo fibers was observed by

using a JSM-5310LV Scanning Electron Microscope

(SEM, Japan) under 15 kV acceleration voltage. The

obtained bamboo fibers were first dried and golden-

coated prior to SEM observations.

3 Results and discussion

3.1 Analysis of orthogonal experiment results

There were 16 groups of orthogonal experiments for

chemical pretreatment. The yield after chemical

pretreatment, yield after fiber carding, and sulfonic

acid group content of the bamboo chips after chemical

pretreatment were taken as the test indexes to analyze

and determine the optimized process conditions. Test

indexes and results of the orthogonal test are listed in

Table 2 and the range result analysis is presented in

Table 3 where ki (i = 1, 2, 3, 4) is the mean value of the

experimental indicators for the same factor and the

same level. Range R is the difference between the

maximum and minimum values of k1, k2, k3, and k4.

The results of the variance analysis are listed in Table 4.

The range analysis was carried out based on the

experimental results. The range R was used to

determine the influence degree of each factor on the

selected experimental indicators. The greater the range

R, the greater the influence of the influencing factor on

the experimental indicators and vice versa. According

to the range analysis in Table 3, the sequence of factors

influencing the cooking yield of bamboo chips is

cooking temperature>NaOH dosage>Na2SO3 dosage>

heating time; the sequence of factors influencing the

fiber yield after carding is cooking temperature>

heating time>NaOH dosage>Na2SO3 dosage; the main

sequence of factors influencing the sulfonic acid group

content is Na2SO3 dosage>NaOH dosage>heating time>

cooking temperature.

The relationship between different influencing

factors and testing indicators can be obtained from the

range analysis presented in Fig. 2. After the chemical

pretreatment, the yield of bamboo chips decreased with

an increase in cooking temperature, NaOH dosage,

Na2SO3 dosage, and the extension of heating time,

among which the increase in cooking temperature led

to the highest reduction in cooking yield, which

indicates that cooking temperature had the greatest

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Vol.5, No.2, 2020


influence on the cooking yield. The decline in both the

cooking and carding yields is mainly due to the partial

degradation of lignin and carbohydrates during high-

temperature alkaline sulfite treatment. Different levels

were also used to verify the varying degrees of

degradation, which have different effects on subsequent

mechanical treatment [22]. The carding yield of the

natural bamboo fiber increased with an increase in

cooking temperature and heating time. This may be due

to the increase in temperature being beneficial for the

softening of intercellular lignin and the effective

separation of fibers during the fiber carding process.

Table 2 Testing indexes and results of orthogonal test

Samples

1

2

3

4

5

6

7

8

9

10

11

12

13

14

15

16

CT/℃100

100

100

100

115

115

115

115

130

130

130

130

145

145

145

145

HT/h

1

1.5

2

2.5

1

1.5

2

2.5

1

1.5

2

2.5

1

1.5

2

2.5

N1/%

2

3

4

5

3

2

5

4

4

5

2

3

5

4

3

2

N2/%

6

8

10

12

10

12

6

8

12

10

8

6

8

6

12

10

Cooking yield/%

94.4

89.5

87.7

81.0

88.3

89.4

82.5

82.0

82.2

80.5

88.5

85.0

78.8

80.6

77.2

80.1

Carding yield/%

24.4

26.2

28.0

28.8

27.1

28.0

32.8

34.3

28.0

34.2

42.3

41.3

30.9

36.6

40.3

42.1

Sulfonic acid group content/(mmol∙kg-1)

23.72

30.43

35.88

45.81

38.50

53.84

28.56

42.88

47.00

42.16

55.73

27.30

28.68

23.41

62.27

62.95

Table 3 Analysis of range results

Indicators

Cooking yield/%

Carding yield/%

Sulfonic acid group content /(mmol∙kg-1)

In the column

Poor results

k1

k2

k3

k4

Range R

Primary and secondary factors

k1

k2

k3

k4

Range R


k1

k2

k3

k4

Range R


A

CT/℃0.881

0.856

0.840

0.792

0.089

ACBD

0.268

0.301

0.365

0.375

0.107

ABCD

33.958

40.946

43.049

44.326

10.368

DCBA

B

HT/h

0.859

0.850

0.840

0.820

0.039

0.276

0.313

0.353

0.366

0.090

34.474

37.462

45.609

44.734

11.135

C

N1/%

0.881

0.850

0.831

0.807

0.074

0.342

0.337

0.317

0.312

0.030

49.061

39.624

37.291

36.302

12.759

D

N2/%

0.856

0.847

0.841

0.824

0.032

0.333

0.334

0.329

0.313

0.021

25.747

39.432

44.872

52.228

26.481

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Vol.5, No.2, 2020


However, the increase in NaOH and Na2SO3 dosage led

to a slight decline in the fiber carding yield, which may

be due to the partial dissolution of the hemicellulose

and sulfonated small-molecule lignin [23]. The increase

in cooking temperature and extension of heating time

led to an increase in the content of the sulfonic acid

group, while the increase of NaOH dosage caused a

gradual decrease in the sulfonic acid group content,

indicating that the amount of alkali should not be too

high in the alkaline sulfite treatment. The content of the

sulfonic acid group in the bamboo chips increased

rapidly with the increase of Na2SO3 dosage since the

sulfonic acid groups in the bamboo chips are mainly

derived from Na2SO3.

The comprehensive analysis shows that the

increasing trends of the sulfonic acid group content and

carding yield slow down when the cooking temperature

exceeds 130℃ , while the cooking yield continues to

decrease; hence, 130℃ was considered to be the

optimal cooking temperature. Regarding the change in

the heating time, when the heating time was 2 h, the

sulfonic acid group content reached its highest, and the

carding yield also increased. The heating time

continued to increase and the cooking yield of bamboo

chips continued to decrease. The increasing trend of

fiber yield and sulfonic acid group content slowed

when the heating time exceeds 2 h. Therefore, 2 h can

be regarded as the optimal heating time. An increase in

the NaOH dosage would lead to a continuous decrease

in the yield of bamboo chips and carding yield and

sulfonic acid group content. To ensure the swelling and

softening of bamboo chips, NaOH dosage was chosen

to be 2%. When the Na2SO3 dosage increased to 10%,

the cooking yield of the bamboo chips and fiber yield

after carding did not decrease significantly; however,

when the Na2SO3 dosage increased to 12%, both yields

decreased significantly; therefore, Na2SO3 dosage was

chosen as 10%.

To evaluate the significance of the experimental

indexes selected by the orthogonal experiment, the data

were analyzed for variance, as shown in Table 4. When

P < 0.05, this factor has a significant effect and when

P < 0.01, it has an extremely significant effect.

According to the variance analysis, cooking

temperature and NaOH dosage are the main factors

influencing the cooking yield, while there is no

Table 4 Results of variance analysis

Dependent variable

Cooking yield

Carding yield

Sulfonic acid group content

Sources of variance

CT

HT

N1

N2

Error

Aggregate

CT

HT

N1

N2

Error

Aggregate

CT

HT

N1

N2

Error

Aggregate

Sum of squares

0.017

0.003

0.012

0.002

0.001

11.385

0.030

0.021

0.002

0.001

0.001

0.676

256.413

358.215

407.802

1501.741

99.293

28957.83

Degrees of freedom

3

3

3

3

3

16

3

3

3

3

3

16

3

3

3

3

3

16

Mean square error

0.006

0.001

0.004

0.001

0

0.01

0.007

0.001

0

0

85.471

119.405

135.934

500.58

33.098

F

20.277

4.013

13.892

2.512

39.24

27.72

2.674

1.921

2.582

3.608

4.107

15.124

P

< 0.05

> 0.05

< 0.05

> 0.05

< 0.01

< 0.05

> 0.05

> 0.05

> 0.05

> 0.05

> 0.05

< 0.05

*P is significance, F0.05 (3,3)=9.28, F0.01 (3,3)=29.5.

48

Vol.5, No.2, 2020


significant difference between heating time and Na2SO3

dosage. The carding yield was significantly influenced

by cooking temperature (P < 0.01) and by heating time,

while NaOH dosage and Na2SO3 dosage had no

significant difference. Na2SO3 dosage is the main

influencing factor on the sulfonic acid group content of

bamboo chips; however, there is no significant

difference in cooking temperature, heating time, and

Na2SO3 dosage. Therefore, the selected test indexes can

be used to effectively obtain the optimal process

parameters.

3.2 Fiber properties under optimum chemical pretreat‐

ment conditions

The optimum process parameters obtained by the

orthogonal test for cooking temperature, heating time,

NaOH dosage, and Na2SO3 dosage were 130℃ , 2 h,

2%, and 10%, respectively. The properties of the

natural bamboo fiber obtained under the above

conditions are presented in Table 5. As the length of the

bamboo chips is 40~70 mm and the average length of

the obtained natural bamboo fiber is 36.71 mm, this

indicates that excessive cutting of the fiber does not

occur during the subsequent mechanical treatments.

This is mainly due to the fiber softening caused by the

alkaline sodium sulfite treatment. Compared with

natural bamboo fiber prepared by other methods, in this

study, the fiber yield after carding is higher, the fiber

length is longer, and the fiber strength is close to that

obtained using other methods [14, 24-25]. It can be deduced

that continuous production can be realized by disc

refining and thus the production efficiency will be

increased.

Fig.2 Effect of chemical pretreatment on cooking yield of bamboo chips, carding yield of bamboo fiber, and sulfonic acid

group content of bamboo fiber

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Vol.5, No.2, 2020


3.3 XRD analysis

The XRD pattern of the original bamboo fiber obtained

without chemical treatment, and the natural bamboo

fiber which was extracted under optimum chemical

treatment conditions is shown in Fig. 3. The figure

shows that the characteristic peak position of the

natural bamboo fiber is basically consistent with the

characteristic peak position of the original bamboo

fiber, indicating that the extraction process does not

change the crystal structure of the natural bamboo

fiber. The relative crystallinity of the original bamboo

fiber is 50.18% and that of the natural bamboo fiber is

59.31%. This may be attributed to the fact that the

chemical treatment in the extraction process removes

some of the amorphous hemicellulose and a small

amount of non-crystalline cellulose from the bamboo,

which increases the relative crystallinity of the natural

bamboo fiber [26-28].

3.4 SEM observation of fiber morphology

Fig. 4 shows a real photographic image of the natural

bamboo fiber obtained under the optimized process

conditions and SEM images of the natural bamboo

fiber obtained at different chemical pretreatment

temperatures. Fig. 4(a) shows that the alkali treatment

can partially remove lignin and colloids and the

obtained natural bamboo fibers are bright in color.

Table 5 also shows that the fiber length and fiber

diameter are 36.71 mm and 0.285 mm, respectively,

which are apparently longer and larger than those of the

pulp fiber used in papermaking. Fig. 4(b) and Fig. 4(c)

show that the surface of natural bamboo fiber obtained

after chemical pretreatment at 130℃ is smooth and the

structure is relatively dense compared with natural

bamboo fiber obtained at 145℃ . After chemical

pretreatment at 145℃ , the natural bamboo fiber was

brittle, indicating that the process temperature should

not be too high and should be lower than 145℃.

Fig.4 Photographic image of bamboo fiber and SEM images

Table 5 Properties of natural bamboo fiber obtained under optimum chemical pretreatment conditions

Cooking yield

/%

89.5

Carding yield

/%

43.0

Fiber length

/mm

36.71

Fiber diameter

/mm

0.285

Fiber tensile strength

/MPa

407

Fiber elasticity modulus

/GPa

27.7

Fig.3 XRD diagram of the original bamboo fiber

and natural bamboo fiber

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Vol.5, No.2, 2020


4 Conclusions

Natural bamboo fiber was prepared by chemical

pretreatment combined with disc refining, opening, and

carding treatments. The effects of different

technological parameters on the cooking yield of

bamboo chips, sulfonic acid group content of bamboo

chips, and carding yield of natural bamboo fiber were

determined by the orthogonal test. The optimum

parameters of the chemical pretreatment process for

cooking temperature, heating time, NaOH dosage, and

Na2SO3 dosage are 130℃ , 2 h, 2%, and 10%,

respectively. Under the optimum conditions, the

cooking yield of bamboo chips and carding yield of

natural bamboo fiber were 89.5% and 43.0%,

respectively. The natural bamboo fiber length,

diameter, tensile strength, and modulus of elasticity

were 36.71 mm, 0.285 mm, 407 MPa, and 27.7 GPa,

respectively. X-ray diffraction (XRD) and Scanning

electron microscopy (SEM) morphology analyses show

that the natural bamboo fiber obtained by the optimized

pretreatment process is bright in color, shiny, and has a

dense structure and high crystallinity of cellulose.

AcknowledgmentsThis work was financially supported by the National

Key R&D Program of China (2017YFD0600802).

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