纺织学报 ›› 2026, Vol. 47 ›› Issue (04): 80-87.doi: 10.13475/j.fzxb.20250802501

• 纤维材料 • 上一篇    下一篇

樟木预水解硫酸盐法溶解浆制备工艺

李园娟1, 周衡书1,2,3,4(), 徐奕1,2,3,4, 熊海鹰5   

  1. 1 湖南工程学院 纺织服装学院, 湖南 湘潭 411104
    2 短流程智能纺织湖南省工程研究中心, 湖南 湘潭 411104
    3 纺织智能加工技术湖南省高校重点实验室, 湖南 湘潭 411104
    4 湖南省新型纤维面料及加工工程技术研究中心, 湖南 湘潭 411104
    5 湖南省纤维质量监测中心, 湖南 长沙 410117
  • 收稿日期:2025-08-11 修回日期:2026-01-29 出版日期:2026-04-15 发布日期:2026-04-15
  • 通讯作者: 周衡书(1967—),男,教授,硕士。主要研究方向为新型纤维材料与智能纺织。E-mail:280434272@qq.com
  • 作者简介:李园娟(2002—),女,硕士生。主要研究方向为纺织新材料。
  • 基金资助:
    湖南工程学院研究生科研创新项目(YC202424);湖南省重点研发计划项目(2022NK2042)

Preparation of camphor wood pre-hydrolysis kraft dissolving pulp

LI Yuanjuan1, ZHOU Hengshu1,2,3,4(), XU Yi1,2,3,4, XIONG Haiying5   

  1. 1 School of Textile and Fashion, Hunan Institute of Engineering, Xiangtan, Hunan 411104, China
    2 Hunan Provincial Engineering Research Center for Short-Process Intelligent Textiles, Xiangtan, Hunan 411104, China
    3 Hunan Provincial University Key Laboratory of Intelligent Textile Processing Technology, Xiangtan, Hunan 411104, China
    4 Hunan Provincial Engineering Technology Research Center for Advanced Fiber Materials and Textile Processing, Xiangtan, Hunan 411104, China
    5 Hunan Fiber Quality Monitoring Center, Changsha, Hunan 410117, China
  • Received:2025-08-11 Revised:2026-01-29 Published:2026-04-15 Online:2026-04-15

摘要:

溶解浆是一种反应性能良好的高纯度化学浆,近年来国内对其的需求快速增长,但生产所需树种资源的短缺限制了其发展。为拓宽溶解浆原料来源,实现樟木资源的高值化利用,以废弃樟木树干与树枝为原料,采用预水解硫酸盐蒸煮工艺以及无元素氯(ECF)漂白工艺制备溶解浆,并探究预水解及蒸煮工艺对浆料性能的影响。结果表明:预水解可有效脱除半纤维素,聚戊糖和综纤维素含量随预水解温度和时间呈非单调变化;正交试验显示,蒸煮工艺因素影响顺序由大到小依次为用碱量、硫化度、保温时间、蒸煮温度,最优参数为:用碱量22%、硫化度25%、保温时间120 min、蒸煮温度160 ℃;经ClO2漂白(D1)—碱精制处理(E)—ClO2漂白(D2)—H2O2漂白(P)漂白后,所得溶解浆的聚合度(914.75)、α-纤维素含量(94.17%)和白度(78.91%)、灰分(0.42%)、铁离子含量(10.62 mg/kg)基本达到再生纤维素用纤维浆粕标准。本研究为樟木废弃资源的高值化利用提供了可行的工艺路线,所制备的溶解浆性能符合纺织纤维应用要求,具有潜在的工业化应用价值。

关键词: 樟木, 预水解, 硫酸盐, 溶解浆, 化学浆, 浆粕, 纤维素纤维

Abstract:

Objective As a popular type of urban landscaping tree, camphor trees (cinnamomum camphora) generate substantial amounts of discarded trunks and branches annually. However, China has long relied on imports to meet its demand for high-grade dissolving pulp used in textile fiber production. To achieve value-added utilization of camphor wood resources and develop novel raw material sources for producing dissolving pulp, this study investigates the preparation process of camphor wood dissolving pulp using discarded trunks and branches as feedstock.

Method The camphor wood dissolving pulp was prepared by the pre-hydrolysis kraft process. First, camphor wood chips were subjected to hot water pre-hydrolysis to remove most hemicellulose, with single factor experiments to investigate how different process conditions would affect the pre-hydrolysis. Subsequently, the pre-hydrolyzed wood chips underwent kraft cooking using NaOH and Na2S to eliminate lignin, and orthogonal experiments was employed to determine optimal cooking parameters. Finally, the obtained pulp was bleached through a four-stage elemental chlorine-free (ECF) bleaching sequence, whick are ClO2 bleaching (D1), alkali refining treatment (E), ClO2 bleaching (D2), and H2O2 bleaching (P), to improve pulp quality. The prepared dissolving pulp was then tested for degree of polymerization, α-cellulose content, and brightness, while its surface morphology was examined by scanning electron microscopy.

Results The hot water pre-hydrolysis process was found effective in removing a substantial portion of hemicellulose from camphor wood. The single-factor variable study revealed that the contents of pentosan and holocellulose exhibited non-monotonic trends with increasing pre-hydrolysis temperature or prolonged holding time, while variations in the solid-to-liquid ratio showed no significant effect on their contents. For the kraft cooking process, given the stringent requirements for dissolving pulp regarding degree of polymerization, α-cellulose content, and brightness, a comprehensive evaluation through orthogonal experimental analysis indicated the following order of parameter influence: alkali charge > sulfidity > holding time > cooking temperature. The optimal conditions were determined as 22% alkali charge, 25% sulfidity, and a holding time of 120 min at 160 ℃. Under these conditions, the resulting camphor wood pulp exhibited a polymerization degree of 1 035.85, an α-cellulose content of 90.63%, and a brightness of 21.35%. During ECF bleaching, the stepwise removal of lignin through the four-stage D1ED2P sequence increased the pulp brightness to 78.91%, while simultaneously elevating the α-cellulose content and reducing the polymerization degree. SEM observations indicated that the original camphor wood surface contained abundant tubular pores, facilitating the penetration of pre-hydrolysis and cooking liquors. After the pre-hydrolysis kraft treatment, complete fiber separation was achieved due to the extensive removal of lignin and hemicellulose. The liberated fibers displayed a flattened morphology with surface wrinkles and grooves.

Conclusion Pre-hydrolysis effectively removes hemicellulose, with the contents of pentosan and holocellulose showing non-monotonic variations depending on pre-hydrolysis temperature and duration. Orthogonal experiments revealed that the influencing order of kraft cooking parameters was alkali charge > sulfidity > holding time > cooking temperature. The optimal conditions were determined as: 22% alkali charge, 25% sulfidity, 120 min holding time, and 160 ℃ cooking temperature. After four-stage ECF bleaching (D1ED2P sequence), the resulting dissolving pulp exhibited satisfactory properties, with 914.75 of polymerization degree, 94.17% α-cellulose content, 78.91% brightness, 0.42% ash content, and 10.62 mg/kg iron content, meeting essentially the requirements for regenerated cellulose fiber pulp. This indicates that camphor wood can serve as a high-quality raw material for producing dissolving pulp for spinning. However, further process optimization is necessary to enhance pulp brightness and reduce ash content. This study demonstrates a viable approach for the value-added utilization of camphor wood waste resources, with the prepared dissolving pulp satisfying the requirements for textile fiber applications and showing promising potential for industrial-scale implementation.

Key words: camphor wood, pre-hydrolysis, kraft, dissolving pulp, chemical pulp, pulp, cellulose fiber

中图分类号: 

  • TS102.2

图1

樟木溶解浆制备工艺"

表1

正交试验因素水平表 "

水平 A
用碱量/%
B
硫化度/%
C
蒸煮温度/℃
D
保温时间/min
1 18 15 160 60
2 20 20 165 90
3 22 25 170 120

表2

漂白工艺参数 "

漂段 漂白剂
名称
漂白剂
质量分
数/%
浆粕质
量分
数/%
温度/
反应时
间/min
pH值
D1 ClO2 3.6 10 70 90 3~4
E NaOH 2.0 10 75 60
D2 ClO2 0.9 10 70 90 3~4
P NaOH
H2O2
2.5
2.5
10 70 90

表3

樟木、桉木和杨木主要化学成分含量"

材种 不同化学成分含量/%
综纤维素 聚戊糖 总木质素 热水抽出物 1%NaOH抽出物 苯-醇抽出物 灰分
樟木 84.87 22.27 20.88 4.23 14.90 4.05 0.93
桉木[17] 77.90 21.37 25.43 1.50 11.40 1.10
杨木[17] 81.36 22.65 24.40 1.20 16.10 1.80

表4

温度对预水解工艺的影响"

温度/℃ 得率/% 综纤维素含量/% 聚戊糖含量/%
150 84.85 68.00 7.13
160 76.90 60.54 7.65
165 76.17 57.95 10.55
170 73.35 59.80 7.99

表5

保温时间对预水解工艺的影响"

保温时间/min 得率/% 综纤维素含量/% 聚戊糖含量/%
60 78.59 60.19 11.67
90 76.17 57.95 10.55
120 75.69 58.78 9.83
180 74.68 58.34 7.65

表6

固液比对预水解工艺的影响"

固液比 得率/% 综纤维素含量/% 聚戊糖含量/%
1∶4 76.20 59.53 9.97
1∶5 76.17 57.95 10.55
1∶6 76.10 59.77 8.67
1∶7 75.35 60.66 9.98

表7

硫酸盐法蒸煮工艺正交试验结果与分析"

试验号 A
用碱量
B
硫化度
C
蒸煮温度
D
保温时间
聚合度 α-纤维素含
量/%
白度/%
1 1 1 1 1 926.19 90.59 16.06
2 1 2 2 2 811.80 90.95 21.50
3 1 3 3 3 1 519.11 89.66 21.65
4 2 1 2 3 1 157.68 87.71 21.90
5 2 2 3 1 948.60 92.55 16.79
6 2 3 1 2 963.82 90.97 18.73
7 3 1 3 2 896.74 91.18 24.19
8 3 2 1 3 1 005.21 93.22 23.34
9 3 3 2 1 842.67 94.17 24.23
聚合度 K1 3 257.10 2 980.61 2 895.22 2 717.46 因素主→次DBCA
最优方案D3B3C3A1
K2 3 070.10 2 765.61 2 812.15 2 672.36
K3 2 744.62 3 325.60 3 364.45 3 682.00
极差R 170.83 186.66 184.10 336.55
α-纤维
素含量
K1 271.20 269.48 274.78 277.31 因素主→次ABDC
最优方案A3B2D1C1
K2 271.23 276.72 272.83 273.10
K3 278.57 274.80 273.39 270.59
极差R 2.46 2.41 0.65 1.40
白度 K1 59.21 62.15 58.13 57.08 因素主→次ADCB
最优方案A3D3C2B3
K2 57.42 61.63 67.63 64.42
K3 71.76 64.61 62.63 66.89
极差R 4.78 0.99 3.17 3.27

表8

漂白前后樟木溶解浆的性能"

漂白
前后
聚合
α-纤维
素含量/
%
白度/
%
灰分含
量/%
铁离子
含量/
(mg·kg-1)
漂白前 1 035.85 90.63 21.35
漂白后 914.75 94.17 78.91 0.42 10.62

图2

樟木片及浆粕的表观形貌照片"

图3

樟木及樟木溶解浆的红外光谱图"

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