Journal of Textile Research ›› 2020, Vol. 41 ›› Issue (07): 1-8.doi: 10.13475/j.fzxb.20190900108

• Fiber Materials •     Next Articles

Alkaline enzyme treatment process for preparation of Lyocell cellulose pulp

YUAN Wei1, YAO Yongbo2, ZHANG Yumei1(), WANG Huaping1   

  1. 1. College of Materials Science and Engineering, Donghua University, Shanghai 201620, China
    2. College of Material and Textile Engineering, Jiaxing University, Jiaxing, Zhejiang 314001, China
  • Received:2019-09-02 Revised:2020-03-04 Online:2020-07-15 Published:2020-07-23
  • Contact: ZHANG Yumei E-mail:zhangym@dhu.edu.cn

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Abstract:

In order to improve the dissolving efficiency and solution stability of cellulose during the preparation of Lyocell fiber, the alkaline enzyme treatment time and dosage with cellulose pulp were experimented on, and the changes of relative molecular weight and accessible properties of the pulp were studied. The results show that after enzyme treatment, the crystalline form of cellulose is not destroyed, remaining to be a typical cellulose I-type conformation. When the enzyme dosage is set to 4 000 mL/t and the enzyme treatment time increases, the polymerization degree decreases to 430 and tends to be stable, as the enzyme treatment time is more than 60 min. When the enzyme treatment time is set to 60 min and the enzyme dosage increased to 2 000 mL/t, the polymerization degree of cellulose pulp reduces from 520 to about 430, and the relative molecular weight distribution reduces. It is found that the accessible surface area of cellulase pulp treated by cellulose increases, but the crystal structure remains the same. Cellulose mainly acts on the amorphous area in cellulose molecules and the poorly ordered part of crystalline surface.

Key words: cellulase enzyme, cellulose pulp, Lyocell fiber, alkaline enzyme, relative molecular weight distribution, crystal structure

CLC Number: 

  • TQ341.5

Fig.1

Effect of enzyme treatment time(a)and dosage(b)on moisture regain of cellulose pulp"

Fig.2

Effect of enzyme treatment time(a) and dosage(b)on water content of cellulose pulp"

Fig.3

FT-IR spectra of cellulose pulp treated with enzymes at different time(a)and dosage(b)"

Tab.1

Effect of enzyme treatment time on dehydration enthalpy of pulp"

酶处理时间/min 热焓值/ (J·g-1)
0 123.0
15 128.1
30 132.3
45 132.4
60 133.4
90 133.6
120 133.7

Fig.4

Effect of with enzyme dosage (a) and treatment time (b) on polymerization degree of cellulose pulp"

Tab.2

Effect of enzyme treatment time on reducing sugar content of cellulose pulp"

酶处理时间/min 还原糖质量分数/%
15 0.39
30 0.50
45 0.60
60 0.62
90 0.61
120 0.62

Fig.5

Effect of enzyme dosage on molecular weight distribution of pulp"

Tab.3

Effect of enzymes with different dosage on molecular weight of cellulose pulp"

酶用量/
(mL·t-1)		 平均数均
分子量/104		 平均重均
分子量/105		 PDI
0 3.30 1.47 4.47
500 3.28 1.16 3.52
1 000 3.24 1.13 3.49
2 000 3.17 1.06 3.36
4 000 3.38 1.07 3.18

Tab.4

Changes of crystalline spacing and crystallinity of cellulose pulp after enzymatic treatment at different time"

酶处理
时间/min		 晶面间距/nm 结晶度/
%
(11ˉ0) (110) (012) (020) (103) (004)
0 0.588 0.537 0.433 0.393 0.318 0.260 81
15 0.589 0.538 0.432 0.393 0.318 0.260 79
30 0.591 0.536 0.433 0.393 0.318 0.260 80
45 0.587 0.537 0.432 0.393 0.318 0.260 80
60 0.589 0.535 0.433 0.393 0.319 0.260 79
90 0.589 0.537 0.432 0.394 0.319 0.260 81
120 0.587 0.538 0.431 0.393 0.319 0.260 81

Tab.5

Changes of crystal plane spacing and crystallinity of cellulose pulp after enzymatic action at different dosage"

酶用量/
(mL·t-1)		 晶面间距/nm 结晶度/
%
(11ˉ0) (110) (012) (020) (103) (004)
0 0.588 0.537 0.433 0.393 0.318 0.260 81
500 0.588 0.537 0.433 0.393 0.319 0.260 79
1 000 0.587 0.537 0.433 0.393 0.318 0.260 80
2 000 0.586 0.536 0.433 0.393 0.318 0.260 80
4 000 0.589 0.537 0.432 0.393 0.319 0.260 79

Fig.6

Solid state NMR of cellulose pulp treated with enzyme at different dosage(a)and time(b)"

Tab.6

Effect of proporation of crystalline regions in cellulose pulp at different enzyme dosage"

酶用量/
(mL·t-1)		 占比/%
结晶表面较好
有序结构		 表面较差有序
以及无序结构		 结晶内部有序
结构
0 9.6 26.0 64.4
500 10.1 25.3 64.6
1 000 10.2 23.6 66.2
2 000 10.5 22.7 66.8
4 000 11.4 22.0 66.6

Tab.7

Effect of proporation of crystalline regions in cellulose pulp at different enzyme treatment time"

酶处理
时间/min		 占比/%
结晶表面较好
有序结构		 表面较差有序
以及无序结构		 结晶内部
有序结构
0 9.6 26.0 64.4
15 9.8 24.9 65.3
30 10.4 24.0 65.6
45 10.7 23.0 66.3
60 11.7 21.9 66.4
90 12.0 21.7 66.3
120 11.8 21.8 66.4
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