纺织学报 ›› 2023, Vol. 44 ›› Issue (09): 52-59.doi: 10.13475/j.fzxb.20230101201

• 纤维材料 • 上一篇    下一篇

醋化级芦苇溶解浆的制备及其性能

王小康1,2, 解开放1,2(), 周衡书1,2, 包新军1,2, 徐应盛3   

  1. 1.湖南工程学院 纺织服装学院, 湖南 湘潭 411104
    2.湖南工程学院 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
    3.湖南骏泰新材料科技有限责任公司, 湖南 怀化 418005
  • 收稿日期:2023-01-05 修回日期:2023-06-26 出版日期:2023-09-15 发布日期:2023-10-30
  • 通讯作者: 解开放(1988—),男,讲师,博士。主要研究方向为功能性和产业用纺织品。E-mail:20846@hnie.edu.cn。
  • 作者简介:王小康(1998—),男,硕士生。主要研究方向为纺织新材料。
  • 基金资助:
    湖南省重点研发计划项目(2022NK2042);湖南省教育厅创新平台项目(20K037);湖南省教育厅青年项目(22B0729);湘潭市科技创新双“50”项目(CG-YB20211002)

Preparation and characterization of acetate grade reed pulp

WANG Xiaokang1,2, XIE Kaifang1,2(), ZHOU Hengshu1,2, BAO Xinjun1,2, XU Yingsheng3   

  1. 1. College of Textile and Fashion, Hunan Institute of Engineering, Xiangtan, Hunan 411104, China
    2. Engineering Technology Research Center of New Fiber Fabric and Processing, Hunan Institute of Engineering, Xiangtan, Hunan 411104, China
    3. Hunan Juntai New Material Technology Co., Ltd., Huaihua, Hunan 418005, China
  • Received:2023-01-05 Revised:2023-06-26 Published:2023-09-15 Online:2023-10-30

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摘要：

为探索使用可再生的芦苇资源制备醋化级溶解浆的可行性,以湖南洞庭湖区的南荻为原料,采用水预水解-硫酸盐法蒸煮-D0EpD1(ClO2漂白脱木素段-H2O2漂白段-ClO2漂白增加白度段)3段漂白工艺制备了南荻浆粕,并对其甲种纤维素含量、白度、聚合度、多戊糖含量、灰分含量和铁含量,以及表观形貌、化学结构和晶体结构等进行测试与分析。结果表明:蒸煮后南荻的粗浆得率为46.31%,3段漂白工艺使南荻浆粕的主要性能指标得到明显改善,其甲种纤维素含量提高了1.24%达到97.70%,白度提高1倍达到91.42%,特性黏度降低38.01%,使南荻浆粕的平均聚合度达到1 413;制浆过程中高温、NaOH、Na2S、ClO2和H2O2的共同作用使南荻中的木质素、半纤维素和灰分得到有效去除。本文工艺制备的南荻浆粕的性能达到了醋化级溶解浆的基本要求,为下一步制备醋酯纤维素和醋酯纤维提供参考。

关键词: 芦苇, 南荻, 醋酯纤维, 溶解浆, 纤维素, 木质素, 半纤维素

Abstract:

Objective Based on the research on using biomass materials (such as bamboo, straw, sorghum straw, mulberry straw, hemp, bagasse, olive, tobacco stem and so on) to prepare acetate grade dissolving pulp and downstream products, this paper proposes the use of rich reed resources in Dongting Lake area to explore the feasibility of preparing acetate reed pulp, and test and analyze the performance of the prepared pulp so as to establish understanding on the preparation of cellulose acetate and acetate fiber.

Method The typical sulfate method was adopted to prepare the Triarrhena lutarioriparia dissolving pulp. Firstly, the water pre-hydrolysis of Triarrhena lutarioriparia slices was carried out in an electrothermal high-pressure boiling pot (Fig. 2) with a liquor ratio of 1∶4. Then, the equipment was used for sulfate boiling (Fig. 3), where the main components of the boiling solution were NaOH and Na2S. Crude pulp was cleaned with a 45 μm polyester mesh bag and sieved with a sieve machine with a sieve gap of 0.25 mm. Finally, the D0EpD1 three-stage bleaching process (Tab. 2) was used for bleaching, and the bleaching agents were ClO2 and H2O2. The cellulose I content, whiteness, polymerization degree, pentosan content, ash content and iron content of the prepared triarrhena lutarioriparia dissolving pulp were tested, and the apparent morphology, infrared spectroscopy, Raman spectroscopy and X-ray diffraction were employed for analysis.

Results The yield of crude pulp after boiling was 46.31%. The three-stage bleaching process significantly improved the main performance indexes of Triarrhena lutarioriparia pulp. The content of cellulose I increased by 1.24% to 97.70%, the whiteness doubled to 91.42%, and the intrinsic viscosity decreased by 38.01%, which made the average degree of polymerization of pulp reach 1 413. In addition, the pentosan content, ash content and iron content of the pulp after bleaching were 5.76%, 0.004% and 0.000 562%, respectively. The cellulose fibers prepared from Triarrhena lutarioriparia dissolving pulp were long cylindrical with rough surface showing a large number of grooves, cracks, pores and filaments. In the infrared spectra (Fig. 5), the Triarrhena lutarioriparia dissolving pulp showed a typical cellulose characteristic peak, and the intensity of the absorption peak was enhanced compared with that of Triarrhena lutarioriparia. The characteristic peaks of lignin at 1 254 cm-1 and 1 511 cm-1 and the characteristic peaks of hemicellulose at 1 726 cm-1 disappeared, indicating that the pulping process removed the lignin and hemicellulose in Triarrhena lutarioriparia. The characteristic peaks at 1 169 cm-1 and 1 607 cm-1 relating to lignin disappeared, and the intensity of the characteristic peak at 2 896 cm-1 decreased indicating that non-cellulose substances such as lignin in Triarrhena lutarioriparia were removed during pulping (Fig. 6). The Triarrhena lutarioriparia dissolving pulp showed a typical diffraction curve of cellulose I. The small peak at 26.4°disappeared and no peak appeared at 29.4°(Fig. 7), suggesting that the inorganic components such as SiO2 in Triarrhena lutarioriparia were effectively removed after the pulping process.

Conclusion The acetate grade Triarrhena lutarioriparia dissolving pulp was prepared by water pre-hydrolysis-sulfate cooking-D0EpD1 three-stage bleaching process. The combined action of high temperature and chemical agents during the pulping process effectively removed the lignin, hemicellulose and ash in Triarrhena lutarioriparia, formed irregular microfibril structure on the surface of cellulose fiber, and presented a rough surface full of grooves. The successful preparation of acetate grade Triarrhena lutarioriparia dissolving pulp not only lays a foundation for the preparation of cellulose acetate and acetate fiber, but also helps open up a new way for high-value and efficient utilization of reed resources.

Key words: reed, Triarrhena lutarioriparia, acetate fiber, dissolving pulp, cellulose, lignin, hemicellulose

中图分类号: 

  • TS151

图1

南荻纵横向形态及溶解浆的制备工艺"

图2

南荻预水解工艺"

图3

南荻硫酸盐法蒸煮工艺"

表1

南荻浆粕漂白工艺参数"

漂白
工艺		 漂白剂
种类		 漂白剂用量/
(kg·t-1)		 漂白
温度/℃		 漂白
时间/min
D0 ClO2 15 70 25
EP H2O2 8 90 90
D1 ClO2 5 70 120

图4

南荻内外表面、纵横向截面和溶解浆的表观形貌"

图5

南荻和南荻溶解浆红外光谱图"

图6

南荻和南荻溶解浆的拉曼光谱图"

图7

南荻和南荻溶解浆的X射线衍射曲线"

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