制备Lyocell纤维用纤维素浆粕的碱性酶处理工艺

doi:10.13475/j.fzxb.20190900108

摘要/Abstract

摘要：

为提高Lyocell纤维制备过程中纤维素的溶解效率和溶液稳定性,分别改变碱性酶处理Lyocell纤维用纤维素浆粕的时间和用量,研究其对浆粕相对分子质量和可及度的影响,并对处理工艺进行优化。结果表明:酶处理后纤维素晶型没有受到破坏,仍是典型的纤维素I型构象;当酶用量为4 000 mL/t,增加处理时间至60 min时,纤维素浆粕的聚合度降为430并趋于稳定;当处理时间为60 min,增加酶的用量至2 000 mL/t时,纤维素浆粕的聚合度由520降低至约430,相对分子质量分布变窄;经过纤维素酶处理后纤维素浆粕的可及表面积有所增加,但晶体结构未发生变化,纤维素酶主要是作用于纤维素分子的无定形区和结晶表面较差有序部分。

关键词: 纤维素酶, 纤维素浆粕, Lyocell纤维, 碱性酶, 相对分子质量分布, 晶体结构

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

中图分类号:

TQ341.5

元伟, 姚勇波, 张玉梅, 王华平. 制备Lyocell纤维用纤维素浆粕的碱性酶处理工艺[J]. 纺织学报, 2020, 41(07): 1-8.

YUAN Wei, YAO Yongbo, ZHANG Yumei, WANG Huaping. Alkaline enzyme treatment process for preparation of Lyocell cellulose pulp[J]. Journal of Textile Research, 2020, 41(07): 1-8.

图/表 13

图1

图2

图3

表1

图4

表2

图5

表3

表4

纤维素浆粕经过不同时间酶处理后的晶面间距和结晶度变化"

酶处理时间/min	晶面间距/nm						结晶度/ %
酶处理时间/min	(1 $1 ˉ$ 0)	(110)	(012)	(020)	(103)	(004)	结晶度/ %
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

表4

表5

纤维素浆粕经过不同用量的酶处理后的晶面间距和结晶度变化"

酶用量/ (mL·t^-1)	晶面间距/nm											结晶度/ %
酶用量/ (mL·t^-1)	(1 $1 ˉ$ 0)	(110)		(012)		(020)		(103)		(004)		结晶度/ %
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

表5

图6

表6

表7

参考文献 31

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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

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

酶用量/ (mL·t^-1)	占比/%
酶用量/ (mL·t^-1)	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

酶处理时间/min	占比/%
酶处理时间/min	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