纺织学报 ›› 2026, Vol. 47 ›› Issue (05): 37-44.doi: 10.13475/j.fzxb.20250706901

• 纤维材料 • 上一篇    下一篇

麻浆粕铁离子的脱除及其Lyocell纤维性能

安钊1, 王伟1,2(), 程春祖2, 薛振军2, 王欣奇2, 杨硕2,3, 狄友波1, 曹卫东4   

  1. 1 太原理工大学 轻纺工程学院, 山西 晋中 030600
    2 中国纺织科学研究院有限公司 生物基纤维材料全国重点实验室, 北京 100025
    3 天津科技大学 轻工科学与工程学院, 天津 300457
    4 山西绿洲纺织有限责任公司, 山西 晋城 048104
  • 收稿日期:2025-07-29 修回日期:2026-03-04 出版日期:2026-05-15 发布日期:2026-07-10
  • 通讯作者: 王伟(1991—),男,讲师,博士。主要研究方向为再生纤维素纤维的制备及功能化改性。E-mail:wangwei03@tyut.edu.cn
  • 作者简介:安钊(2002—),男,硕士生。主要研究方向为功能化纤维素。
  • 基金资助:
    国家自然科学基金项目(22208247);山西省基础研究计划项目(202403021212320);天津市自然科学基金项目(24JCQNJC00330);生物基纤维材料全国重点实验室开放课题基金资助项目(SKLBFM202510)

Removal of iron ion from hemp pulp and properties of Lyocell fibers

AN Zhao1, WANG Wei1,2(), CHENG Chunzu2, XUE Zhenjun2, WANG Xinqi2, YANG Shuo2,3, DI Youbo1, CAO Weidong4   

  1. 1 College of Textile Engineering, Taiyuan University of Technology, Jinzhong, Shanxi 030600, China
    2 State Key Laboratory of Bio-based Fiber Materials, China Textile Academy, Beijing 100025, China
    3 School of Light Industry Science and Engineering, Tianjin University of Science and Technology, Tianjin 300457, China
    4 Shanxi Lvzhou Textile Co., Ltd., Jincheng, Shanxi 048104, China
  • Received:2025-07-29 Revised:2026-03-04 Published:2026-05-15 Online:2026-07-10

摘要:

为拓展Lyocell纤维纺丝用浆粕的来源,以粘胶纺丝用麻浆粕为原料,利用乙二胺四乙酸二钠(EDTA-2Na)脱铁处理,开发了符合Lyocell纺丝要求的溶解浆粕,并重点研究了脱铁工艺对麻浆粕铁离子脱除以及纤维素聚合度、结晶度及溶解性的影响;进一步利用干喷湿法的纺丝工艺,将处理后的麻浆粕与溶解木浆共混,制备了不同含量的麻浆基Lyocell纤维,探讨了麻浆粕添加量对纤维性能的影响。结果表明,麻浆粕的最佳脱铁工艺为:EDTA-2Na添加量0.3%,溶液温度50 ℃,溶液pH值8及处理时间1 h,在此条件下,麻浆粕中铁离子含量降低至6.8 mg/kg,聚合度从528略降至501,结晶度从69.8%提升至76.0%,且溶解性更好,达到了Lyocell纺丝用溶解浆的要求;纤维性能方面,随着麻浆粕添加量的增加,纤维力学性能略有下降,但仍满足行业标准(FZ/T 52019—2018)中关于Lyocell短纤维合格品的要求。

关键词: 麻浆粕, 铁离子, 溶解性, Lyocell纤维, 纤维性能, 纤维素纤维

Abstract:

Objective Lyocell fibers are recognized as the most promising cellulose-based materials in the 21st century because of their environmental profile and excellent mechanical and wear performance. However, the quality of pulp is one of the most critical factors that affect spinnability and fiber properties. In order to broaden the raw material sources for Lyocell spinning, hemp pulp intended for viscose was used as raw material, in which iron was removed using EDTA disodium salt (EDTA-2Na).

Method The influences of the EDTA-2Na mass concentration, reaction temperature, reaction time period, and solution pH value on iron ion removal rate was investigated. The changes in the microstructure, chemical structure, degree of polymerization, crystallinity, and solubility of the hemp pulp before and after the iron removal were evaluated. Finally, the influences of hemp pulp addition on the mechanical properties of Lyocell fibers was investigated through the standard Lyocell fiber spinning process.

Results The iron removal performance of EDTA-2Na under different reaction conditions was assessed by measuring the iron content in the pulp. The iron content in the pulp first decreased and then increased with the increase of reaction temperature, with the minimum at 50 ℃. As the mass concentration of EDTA-2Na increased, the iron content first decreased, but when the mass concentration was beyond 0.3%, iron in the pulp was almost completely chelated and the content became stabilized. With increasing solution pH value, the iron content decreased and then increased, reaching a minimum at pH value of 8. During the reaction, the iron content in the pulp first decreased, but increased when the reaction time period exceeded 1 h. Under the optimal conditions, the iron content in hemp pulp was reduced to 6.8 mg/kg. Comparison of hemp pulp before and after iron removal treatment revealed almost no changes occurred in its microstructure and chemical structure. The degree of polymerization decreased from 528 to 501, but remained above 500, meeting the requirement for Lyocell spinning. Crystallinity increased from 69.8% to 76.0%. Orientation improved and offset the potential impact of the lower degree of polymerization. After the iron removal treatment, the solubility of hemp pulp in NMMO solvent was improved. The mixing ratio of hemp pulp to wood pulp was adjusted and fibers were spun. Compared with Lyocell fibers prepared from pure wood pulp, fibers perpared from pure hemp pulp exhibited a decrease in crystallinity from 79.28% to 76.67%. The dry breaking strength decreased from 3.8 cN/dtex to 3.29 cN/dtex, and the wet breaking strength decreased from 3.58 cN/dtex to 3.31 cN/dtex. The mechanical properties declined slightly, but still met the requirements the industry standard FZ/T 52019—2018 Lyocell staple fiber.

Conclusion This study confirms the feasibility of using hemp pulp as a raw material for Lyocell fiber production. It also clarified the influence of EDTA-2Na iron removal treatment conditions on pulp properties and spinning quality. The optimal reaction conditions were established, where reaction temperature 50 ℃, EDTA-2Na mass concentration 0.3%, solution pH value 8, and reaction time period 1 h. These conditions reduced the iron content in hemp pulp to 6.8 mg/kg. Compared with the untreated hemp pulp, the de-ironed pulp shows almost no change in chemical structure. However, its degree of polymerization decreases from 528 to 501, and its crystallinity increases from 69.8% to 76%. Solubility also improves. These properties meet the requirements for Lyocell spinning. As the proportion of hemp pulp increases from 0% to 100%, the crystallinity of the spun Lyocell fibers decreases from 79.28% to 76.67%. The dry and wet breaking strengths decrease from 3.8 cN/dtex and 3.58 cN/dtex to 3.29 cN/dtex and 3.31 cN/dtex, respectively. The properties of the prepared Lyocell fibers decrease slightly but remain within the acceptable range.

Key words: hemp pulp, iron ion, dissolvability, Lyocell fiber, fiber property, cellulose fiber

中图分类号: 

  • TS151

表1

脱铁处理工艺参数"

试样
编号
EDTA-2Na
质量分数/%
温度/℃ pH值 处理
时间/h
0#
1# 0.5 30 7 2
2# 0.5 40 7 2
3# 0.5 50 7 2
4# 0.5 60 7 2
5# 0.5 70 7 2
6# 0.1 50 7 2
7# 0.2 50 7 2
8# 0.3 50 7 2
9# 0.4 50 7 2
10# 0.5 50 7 2
11# 0.3 50 6 2
12# 0.3 50 7 2
13# 0.3 50 8 2
14# 0.3 50 9 2
15# 0.3 50 10 2
16# 0.3 50 8 0.5
17# 0.3 50 8 1
18# 0.3 50 8 1.5
19# 0.3 50 8 2
20# 0.3 50 8 2.5

图1

不同反应条件下麻浆粕的铁离子含量"

图2

脱铁前后麻浆粕的光学与扫描电镜照片"

图3

脱铁前后麻浆粕的FT-IR图"

图4

脱铁前后麻浆粕的XRD图"

图5

脱铁前后麻浆粕的溶解动态情况(×100)"

图6

不同Lyocell纤维的SEM照片(×1 000)"

图7

不同Lyocell纤维的FT-IR图"

图8

不同Lyocell纤维的XRD图"

表2

不同Lyocell纤维的力学性能"

试样
编号
断裂强度/(cN·dtex-1) 断裂伸长率/% 初始模量(5%)/(cN·dtex-1)
干态 湿态 干态 湿态 干态 湿态
S-1 3.80 3.58 7.72 10.05 10.06 7.29
S-2 3.61 3.29 7.44 8.60 8.88 7.40
S-3 3.29 3.31 7.60 9.51 6.81 7.00
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