ST2A-2-1: Chemical Pulp Production from Rice Straw by Alkaline Soaking and

Cooking with Aaded Alkaline and Oxygen

Wikhan Anapanurak1 and Sawitree Pisuthpichet2

ABSTRACT
Rice straw was studied on fiber size. The chemical analysis and chemical pulp of rice straw
from 36 conditions was produced and reported. The conditions were carried out by soaking in 1 per
cent of sodium hydroxide solution at 10:1 liquor to straw ratio and 45 Celsius for 10 minutes. The
saturated mass was squeezed and cooked with added sodium hydroxide 3 to 7 per cent of straw to
liquor of 1:4 ratio and the oxygen at a pressure of 5 kilogram per square centimeter with maximum
temperatures at 100 to 140 Celsius and cooking times upto 90 minutes. The results were summarized
that the rice straw in 8 conditions gave 45.00 to 50.59 and 0.80 to 4.45 per cent of accepted and
rejected pulp yield, respectively. The amount of pulp yield depended on cooking condition, added
sodium hydroxide, cooking temperature and time. The effects of condition to the pulp yield and
composition were discussed by monitoring the mechanical properties, the condition cooking with
added sodium hydroxide 7 per cent of straw at 4:1 liquor to straw ratio, maximum temperature at 140
Celsius and cooking time at 30 minutes was the best and obtained at 46.11 per cent of the screening
yield, and pulp with freeness at 400-200 ml. CS showed 49.78-50.78 per cent of high brightness,
breaking length of 4.00-5.20 km. burst factor of 28.33-37.75, and folding endurance of 87.87-224.44.
The condition may be used for printing, writing and cover paper.

INTRODUCTION
It is generally known that straw is the oldest papermaking material and an important sources
of raw materials. Straw is still used in some European countries, such as Bulgaria, Denmark, Greece,
Netherland, Hungary, Italy, Rumania, Spain and Yugoslavia where pulpwood supply is limited and the

1
Kasetsart Agricultural and Agro-Industrial Products Improvement Institute (KAPI), Kasetsart University,
Bangkok 10900, Thailand
2
Department of Forest Products Faculty of Forestry, Kasetsart University, Bangkok 10900, Thailand
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purchase of wood pulp from other sources is comparatively expensive to support local paper
production. Increment in the utilization of straw has also taken place in many developing countries,
particularly Algeria, Argentina, China, Egypt, India, Indonesia, Mexico, Pakistan, Sri Lanka, Syria
and Turkey. In these countries packing paper is produced from high-yield unbleached straw pulps;
bleached straw pulps are used as a major furnish for fine quality-writing, printing, and papers.
Thailand is an agricultural country and the staple of diet of her population is rice, it is necessary to
produce rice with surplus rice straw more than 60 million tons per year. The use of rice straw for other
purposes is continual to carry out but it still remains abundant and may be used for pulp and paper
production to obtain more added value goods from agricultural remmant. The soda process for rice
straw pulping was found to be the best with high pulp quality (Mira, 1987). The alkali-oxygen
bleaching method was developed and commercialized, it minimized environmental pollution. El-
Ashmawy et al. (1977) and Chen et al. (1994) reported on the alkali-oxygen pulping i. e. mixed
alkaline pulping and bleaching with oxygen. This study found suitable to a condition in part of time;
temperature and chemical substance for Thai rice straw cooking with oxygen which affected to lignin
degradation and pulp properties.

EXPERIMENTAL
Rice straw seasoned until dry and cut into small chips about 25.4 millimeter length.
1. Anatomical analysis of raw material by means of average in dimensions fiber such as
length, width, lumen diameter, and cell wall thickness.
2. Chemical analysis of raw material by means of average in correspondent to TAPPI
Standards such as organic solubility (T204-om-88), hot water solubility (T207-om-88), lignin (T222-
om-88), holocelluose by sodium chlorite method, pentosan (T223-cm-84), ash (T211-om-85).
3. Initial pulp cooking condition analysis where straw in each condition was soaked in 1 per
cent of sodium hydroxide solution at 10:1 liquor to straw ratio and 45 Celsius for 10 minutes. Then the
saturated mass was squeezed and cooked with added sodium hydroxide 3, 5, 7 per cent, respectively of
straw at 4:1 liquor to straw ratio and oxygen at a pressure of 5 kilogram per square centimeter. The
maximum temperature were 100, 120, 140 Celsius and cooking times with 0, 30, 60, 90 minutes. The

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sum of replication was two 72 conditions Rice straw pulp was analyzed by averaging the mean of both
accepted and rejected yield, Kappa number (T236-cm-85), and lignin content.
4. Physical properties analysed by averaging that accepted pulp yield in each condition was
selected to obtain more than 45 per cent mean of ovendried raw material and more than 90 per cent of
residue and hand- formed sheets disintegrated 5 minutes, beating at 0, 200, 500, 1,000 revolutions and
measuring freeness (T227-om-85). The hand-sheets were tested physical according to TAPPI
Standards (T220-om-88) for thickness, basis weight, density, tensile strength, bursting strength, MIT
folding endurance and brightness.

RESULTS AND DICCUSSION

Size of fiber
Mean averages of size fiber of Thai rice straw were shown in Table 1. The length, width,
lumen diametwr, cell wall thickness of fiber were respectively 0.7018, 0.0103, 0.0034, 0.0035
millimeter, with Runkel ratio, flexibility coefficient, slenderness ratio, percentage of wall fraction
about 2.04, 0.33, 67.92, 32.90, respectively. It was estimated pulp properties with Runkel ratio more
than 1 would be harder in tension for fiber and less oriented fiber to make paper into fluffiness
(Casey,1980), with flexibility coefficient less than 0.5, the paper had medium tensile strength, burst
strength and folding endurance, with slenderness ratio no less than 75 that be the paper of medium
tearing strength but suitable beating with per cent of wall fraction less than 40 per cent would be good
paper (Rydholm, 1967) while fibers completely oriented to get higher tensile and burst strength.
However physical properties of rice straw pulp were tested to investigate an initial.
Chemical composition of raw material
The chemical composition of Thai rice straw was shown in Table 2. It contained the
solubility of alcohol-benzene , alcohol, hot water, and ash, lignin, holocellulose, pentosan about 6.26,
2.40, 10.08, 14.55, 17.50, 58.63, 20.34 per cent on ovendried weight basis. Extractive content was
determined and it was discovered the same as the US and Sri Lanka rice straw (Misra, 1987). Ask,
lignin, pentosan was the same amount as the Japanese rice straw (Chen et al., 1994). However
holocellulose content was less than 10 per cent on the ovendried weight.

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Pulp yield production

By means of soaking method the rice straw was initially soaked in 1 per cent of sodium
hydroxide solution at 10:1 liquor to straw ratio for 45 Celsius and lignin in rice straw was activated by
oxidizing the next step. This method was considered that it was convenient , to reduce chemical
substance in appropriated condition that is suitable for our climate and tradition. Besides pulp yield by
Chen et al., (1994) was high. The 36 cooking conditions were mentioned in part of added chemical
substance, maximum temperature and time above. The concoctions were cooked and analyzed for the
kappa number and lignin content. That was shown in Table 3 and in Figures 1, 2, 3, 4, and 5. It was
found that the accepted yield in the condition with temperature 120 Celsius, added sodium hydroxide 5
per cent of ovendried raw material for 60 minutes (120-5-60) was the highest about 50.59 per cen of
ovendried raw material and with 100-3-0 was the lowest about 14.53 per cent of ovendried raw
material. In this study mean average accepted and rejected pulp yield were between 14.53-50.59, 0.39-
53.12 per cent of ovendried raw material, respectively and kappa number was between 15.06-79.81.
These results showed temperature, time and chemical substance to affect directly lignin content, The
temperature 100, 120, 140, celsius with added sodium hydroxide 3, 5, 7 per cent of ovendried raw
material, yield mostly increased from 0 to 30, 60, 90 minutes, respectively. Under each level of
temperature, yield was different in low temperature more than high temperature according to
concentration of sodium hydroxide at the short time, and yields at 120 celsius degree for 30, 60, 90
minutes were the highest. These trend of curves mostly were opposite characteristic of reject yield.
The appearance of yield quantity was depended on appropriated temperature, sodium hydroxide, time
and the oxidation with the amount of the fixed oxygen supply. The kappa number in each yield was
investigated for evaluating lignin content. The delignification and the degraded lignin in pulp appeared
decreasing along low to high temperature and added sodium hydroxide rapily for short time and
slightly stably for farther time. After randomizing 19 samples from 36 conditions for finding out lignin
content, it was made the curve show relationship between kappa number and lignin and get linear
equation by mean of Y=0.1444X+1.7854 which had kappa number (X), lignin content (Y) and R2
=0.9933, so Figure 5 was the same as Figure 3. However the amount of the screening yield was as
nearly as pulp from soda process (Misra,1987) and alkali-oxygen process (Chen et al, 1994) which had

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8 conditions for physical testing. That was 120-5-30,120-5-60, 120-5-90, 120-7-30, 120-7-60, 140-5-
30, 140-5-60, 140-7-30 and the screening yield about 48.30, 50.59, 48.75, 45.00, 46.98, 45.79, 45.02,
46.11 per cent of ovendried raw material, respectively.
Physical properties of pulp
The pulps were beaten and measured freeness. It was shown in Table 4 and 5. Hand sheet
was formed from 8 conditions, compared with breaking length at different freeness by the different of
120-5, 120-7, 140-5, and 140-7 and the best of each condition group, and shown in Figure 6, 7, 8 and
9, respectively. It was found that the breaking length of 120-7-30, 140-5-30 and 140-7-30 at different
freeness was not different. For burst factor was shown in Figure 10, 11, 12, 13. folding endurance
shown in Figure 14, 15, 16, 17., brightness shown in Figure 18, 19, 20, 21. The comparasion
procedure of burst factor, folding endurance and brightness were the same as breaking length. The
results of burst factor with 140-7-30, 140-5-60, 120-7-30., folding endurance with 140-7-30, 140-5-30,
120-7-30.,brightness with 140-7-30, 120-7-60 were not different. It was concluded that the best
condition was 140-7-30 and saved time and temperature to compare with soda process, time and
chemical substance to compare with alkali-oxygen process (Chen et al., 1994).

CONCLUSION
The Thai rice straw had size of fiber and chemical composition of raw material had been
studied already. When it was soaked and cooked with sodium hydroxide and oxygen, its yield was best
the paper had 49.78-50.78 per cent of brightness, breaking length of 4.00-5.20 kilometers, burst factor
of 28.33-37.75 and folding endurance of 87.87-224.44 at the accepted pulp yield of 46.11 per cent of
ovendried raw material and 400-200 ml .CS of freeness. As Thai Industrial Standards this condition
may be used for printing paper, writing paper and cover paper.

REFERENCES
Anonymous. Thai Industrial Standard for Printing and Writing Paper. TIS. 287-1990. Industrial
Standard Institute, Ministry of Industry, Bangkok, Thailand. 13, 1990.

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Casey, J. P. Pulp and Paper Chemistry Technology. Vol. I. 3rd ed., John Wiley & Sons, New York,
1980.
Chen, K.; Tosaka, K.; and Hayashi, J. Alkali-oxygen pulping of rice straw: two-stage pulping by alkali
soaking and oxygen cooking. Tappi Journal, 77(7), 1994.
El-Ashmawy, A. E., Fadl, M. H., Saleh, T. M., et al. ????? TAPPI J. 60(6): 109, 1977.
Misra, D. K. Cereal secondary fibers and non-wood pulping. ????? Canada. 82-93, 1987.
Rydholm, S. A. Pulping Processes. John Wiley & Sons, New York. 1167, 1967.

Table 1. Fiber dimension of Rice Straw

Fiber dimension Average
Length, mm. 0.7018
Width, mm. 0.0103
Lumen width, mm. 0.0034
Cell wall thickness, mm. 0.0035
Runkel ratio 2.0400
Flexibility coefficient 0.3300
Slenderness ratio 67.9100
Wall fraction, % 32.9000

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Table 2. Chemical composition of Rice Straw

Chemical composition Percentage base on ovendry weight
Alcohol-benzene solubility 6.26
Alcohol solubility 2.40
Hot water solubility 10.08
Total extractives 18.74
Ash 14.55
Lignin 17.50
Holocellulose 58.63
Pentosan 20.34

Table 3. Pulping yield and Kappa number of Rice Straw pulps from alkali-oxygen cooks
Treatment Pulping Reject Kappa
(Temp.-NaOH-time) yield, % % no.
R-100-3-0 14.53 53.12 78.77
R-100-3-30 22.63 40.27 70.00
R-100-3-60 25.75 40.19 57.23
R-100-3-90 30.99 29.22 56.89
R-100-5-0 22.87 39.61 78.63
R-100-5-30 39.17 13.76 59.93
R-100-5-60 43.49 11.15 57.79
R-100-5-90 45.72 7.64 51.00
R-100-7-0 26.06 33.83 80.16
R-100-7-30 45.46 6.73 60.35
R-100-7-60 44.00 6.42 51.42
R-100-7-90 44.65 3.65 46.08
R-120-3-0 17.32 51.07 78.77

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Table 3. Pulping yield and Kappa number of Rice Straw pulps from alkali-oxygen cooks
Treatment Pulping Reject Kappa
(Temp.-NaOH-time) yield, % % no.
R-120-3-30 43.98 14.68 52.08
R-120-3-60 47.02 5.94 45.62
R-120-3-90 43.58 4.24 39.30
R-120-5-0 33.22 24.37 57.44
R-120-5-30 48.30 4.45 47.82
R-120-5-60 50.59 2.60 37.98
R-120-5-90 48.45 2.60 36.18
R-120-7-0 40.74 10.24 59.93
R-120-7-30 45.00 2.86 39.23
R-120-7-60 46.98 1.31 27.80
R-120-7-90 43.86 1.31 22.47
R-140-3-0 17.87 43.00 66.44
R-140-3-30 45.37 5.60 41.65
R-140-3-60 43.35 3.04 27.87
R-140-3-90 41.43 3.58 28.01
R-140-5-0 39.01 18.77 56.96
R-140-5-30 45.79 1.38 29.95
R-140-5-60 45.02 1.30 22.89
R-140-5-90 43.68 1.80 23.79
R-140-7-0 39.44 19.88 63.95
R-140-7-30 46.11 0.80 22.05
R-140-7-60 41.60 0.48 17.62
R-140-7-90 41.26 0.39 15.06

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Table 4. Freeness of rice straw pulp from alkali-oxygen cooks refined by PFI mill at different
revolution
Pulp freeness refined at revolution
Treatment 0 200 500 1,000
R-120-5-30 490 190 180 150
R-120-5-60 520 270 200 180
R-120-5-90 480 210 200 190
R-120-7-30 480 170 160 140
R-120-7-60 510 220 140 120
R-140-5-30 540 270 200 160
R-140-5-60 610 300 180 170
R-140-7-30 570 250 170 160

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Table 5. Physical properties of unrefined and refined pulp at freeness of 200, 300 and 400 ml CS from alkali-oxygen cooks of rice straw
Treatment
Items
R-120-5-30 R-120-5-60 R-120-5-90 R-120-7-30 R-120-7-60 R-140-5-30 R-140-5-60 R-140-7-30
Thickness, mm
Unrefined pulp 0.105 0.113 0.113 0.100 0.108 0.097 0.112 0.122
400 ml 0.104 0.105 0.107 0.096 0.103 0.095 0.099 0.108
300 ml 0.104 0.099 0.101 0.093 0.100 0.093 0.093 0.099
200 ml 0.104 0.094 0.098 0.090 0.096 0.086 0.093 0.088
Basis weight, g/m2
Unrefined pulp 56.84 52.91 61.09 53.36 53.25 51.95 52.77 55.95
400 ml 57.63 53.01 60.75 52.96 53.48 55.09 55.64 54.53
300 ml 58.53 53.01 60.27 52.34 53.56 57.43 57.04 53.45
200 ml 59.47 53.99 60.40 51.88 54.12 56.61 56.32 53.45

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Table 5. Physical properties of unrefined and refined pulp at freeness of 200, 300 and 400 ml CS from alkali-oxygen cooks of rice straw
Treatment
Items
R-120-5-30 R-120-5-60 R-120-5-90 R-120-7-30 R-120-7-60 R-140-5-30 R-140-5-60 R-140-7-30
Density, g/cc
Unrefined pulp 0.54 0.47 0.54 0.53 0.49 0.54 0.47 0.46
400 ml 0.54 0.50 0.56 0.54 0.51 0.59 0.56 0.51
300 ml 0.55 0.54 0.59 0.57 0.53 0.61 0.61 0.55
200 ml 0.57 0.57 0.62 0.58 0.56 0.66 0.62 0.61
Breaking length, km
Unrefined pulp 2.81 2.49 2.43 3.36 2.64 2.98 2.64 2.41
400 ml 3.30 3.40 2.90 3.85 3.50 4.15 4.10 4.00
300 ml 3.60 3.90 3.50 4.50 4.15 4.70 4.55 4.85
200 ml 3.90 4.06 4.46 5.10 4.85 5.59 4.35 5.20
Burst factor
Unrefined pulp 19.00 15.88 16.53 23.99 18.78 20.98 17.24 16.62
400 ml 22.36 22.14 21.43 28.33 24.17 27.17 27.58 28.33
300 ml 26.29 27.50 28.57 32.33 27.92 31.66 32.33 35.00
200 ml 30.00 29.08 36.42 38.42 35.67 36.75 38.58 37.75

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Table 5. Physical properties of unrefined and refined pulp at freeness of 200, 300 and 400 ml CS from alkali-oxygen cooks of rice straw
Treatment
Items
R-120-5-30 R-120-5-60 R-120-5-90 R-120-7-30 R-120-7-60 R-140-5-30 R-140-5-60 R-140-7-30
Folding endurance
Unrefined pulp 9.83 5.90 6.81 14.62 7.08 13.01 5.91 6.04
400 ml 34.55 16.81 23.64 68.75 37.50 73.33 73.33 87.87
300 ml 67.27 27.72 53.64 140.63 61.88 124.44 108.26 134.44
200 ml 95.45 60.92 142.05 213.13 87.50 263.17 192.22 222.44
Brightness, %
Unrefined pulp 43.04 43.47 36.45 50.76 51.60 35.14 46.86 52.72
400 ml 39.01 41.82 36.91 49.31 50.69 32.22 43.89 50.78
300 ml 34.82 41.36 39.18 47.46 49.77 31.11 42.04 49.78
200 ml 31.00 40.36 40.49 45.60 48.83 31.87 42.22 50.00

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Figure 2- Relationship between time cooking and reject yield at

different temperature and percentage of sodium hydroxide

60.00
Reject yield (% based on raw material.)

50.00 100-3

40.00 100-5
100-7
30.00
120-3
20.00 120-5
10.00 120-7
140-3
-
140-5
0 30 60 90
140-7
Time at maximum temperature (min.)

Figure 3- Effect of cooking time to Kappa number on rice straw pulp

from alkali-oxygen cooks

100.00
100-3
80.00 100-5
Kappa number

60.00 100-7

40.00 120-3
120-5
20.00
120-7
-
140-3
0 30 60 90
140-5
Time at maximum temperature (min) 140-7

Figure 4- Relationship between Kappa number and lign

Lignin (% based on ovendry pulp)

15
y = 0.1444x + 1.7854
10 R2 = 0.9933

0
0 10 20 30 40 50 60 70

Kappa number

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Figure 5- Lignin in pulp from alkali -oxygen cooks of rice straw at

different cooking time

16.00
100 -3
14.00
100 -5
12.00
Lignin in pulp (% )

100 -7
10.00 120 -3
8.00 120 -5

6.00 120 -7

4.00 140 -3
140 -5
2.00
140 -7
-
0 30 60 90

Cooking time (min.)

Figure 6- Rice straw pulp conditions were 120-5-30, 120-5-60, 120-5-90

and compared with their breaking length at different freenesses

5.00
4.50
4.00
3.50
Breaking length (km)

3.00 120-5-30
2.50 120-5-60
2.00
120-5-90
1.50
1.00
0.50
-
200 300 400 500

Freeness (ml)

Figure 7- Rice straw pulp conditions were120-7-30, 120-7-60 and compared

with breaking length at different freenesses

฿6

฿5

฿4
Breaking length (km)

120-7-30
฿3
120-7-60

฿2

฿1

฿0
200 300 400 500

Freeness (ml)

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Figure 8- Rice straw pulp conditions were 140-5-30, 140-5-60, 140-7-30

and compared with their breaking length at different freenesses

฿6

฿5

฿4
Breaking length (km)

140-5-30
฿3 140-5-60
140-7-30
฿2

฿1

฿0
200 300 400 500 600

Freeness (ml)

Figure 10- Rice straw pulp conditions were 120-5-30, 120-5-60, 120-5-90
and compared with burst factor at different freenesses

฿40
฿35
฿30
฿25 120-5-30
Burst factor

฿20 120-5-60
฿15 120-5-90
฿10
฿5
฿0
200 300 400 500

Freeness (ml)

Figure 9- Rice straw pulp of the best of each condition groups were compared
with breaking length at different freenesses

฿6

฿5

฿4 120-5-60
Breaking length (km)

120-7-30
฿3
140-5-30
฿2
140-7-30
฿1

฿0
200 300 400 500

Freeness (ml)

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Figure 11- Rice straw pulp conditions were 120-7-30, 120-7-60 and compared
with burst factor at different freenesses

45

40

35

30

25
Burst factor

120-7-30

20 120-7-60

15

10

0
200 300 400 500

Freeness (ml)

Figure 12- Rice straw pulp conditions were 140-5-30, 140-5-60, 140-7-30
and compared with burst factor at different freenesses

45

40

35

30
140-5-30
25
Burst factor

140-5-60
20
140-7-30
15

10

0
200 300 400 500 600

Freeness (ml)

Figure 13- Rice straw pulp of the best of each condition goups were compared
with burst factor at different freenesses

฿45
฿40
฿35
฿30 120-5-90
Burst factor

฿25 120-7-30
฿20 140-5-60
฿15
140-7-30
฿10
฿5
฿0
200 300 400 500 600

Freeness (ml)

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Figure 14- Rice straw pulp conditions were120-5-30, 120-5-60, 120-5-90

and compared with folding endurance at different freenesss

฿160
฿140
฿120
Folding endurance

฿100 120-5-30
฿80 120-5-60
฿60 120-5-90
฿40
฿20
฿0
200 300 400 500

Freeness (ml)

Figure 15- Rice straw pulp conditions were 120-7-30, 120-7-60 and compared
with folding endurance at different freenesses

250

200
Folding endurance

150
120-7-30

100 120-7-60

50

0
200 300 400 500

Freeness (ml)

Figure 16- Rice straw pulp conditions were 140-5-30, 140-5-60, 140-7-30
and compared with folding endurance at different freenesses

300

250

200
Folding endurance

140-5-30
150 140-5-60

100 140-7-30

50

0
200 300 400 500 600

Freeness (ml)

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Figure 17- Rice straw pulp of the best of each condition groups were compared
with folding endurance at different freenesses

300

250

200 120-5-30
Folding endurance

120-7-30
150
140-5-30
100
140-7-30
50

0
200 300 400 500

Freeness (ml)

Figure 18- Rice straw paper sheet conditions were 120-5-30, 120-5-60, 120-5-90
and compared with brightness at different freenesses

฿50

฿45

฿40

฿35

฿30 120-5-30
Brightness (%)

฿25 120-5-60
฿20 120-5-90

฿15

฿10

฿5

฿0
200 300 400 500

Freeness (ml)

Figure 19- Rice straw paper sheet conditions were 120-7-30, 120-7-60 and
compared with brightness at different freenesses

฿52

฿51

฿50

฿49

฿48
Brightness (%)

120-7-30
฿47
120-7-60
฿46

฿45

฿44

฿43

฿42
200 300 400 500

Freeness (ml)

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Figure 20- Rice straw paper sheet conditions were 140-5-30, 140-5-60,
140-7-30 and compared with brightness at different freenesses

฿60

฿50

฿40
140-5-30
Brightness (%)

฿30 140-5-60
140-7-30
฿20

฿10

฿0
200 300 400 500 600

Freeness (ml)

Figure 21- Rice straw paper sheet of the best of each condition groups
were compared with brightness at different freenesses

60

50

40
120-5-60
Brightness (%)

120-7-60
30
140-5-60
140-7-30
20

10

0
200 300 400 500 600

Freeness (ml)

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