纺织学报 ›› 2019, Vol. 40 ›› Issue (12): 1-8.doi: 10.13475/j.fzxb.20181202008

• 纤维材料 •    下一篇

烟梗浆亚微米醋酸纤维的制备及其性能

吴佳骏, 覃小红()   

  1. 东华大学 纺织学院, 上海 201620
  • 收稿日期:2018-12-07 修回日期:2019-05-28 出版日期:2019-12-15 发布日期:2019-12-18
  • 通讯作者: 覃小红
  • 作者简介:吴佳骏(1990—),男,博士生。主要研究方向为亚微米功能性醋酸纤维素制备。
  • 基金资助:
    长江学者(青年学者)计划项目(51773037);国家自然科学基金项目(51373033);东华大学博士生创新基金项目(17D310123)

Preparation and characterization of cellulose acetate sub-micro fiber from burley tobacco stalk pulp

WU Jiajun, QIN Xiaohong()   

  1. College of Textiles, Donghua University, Shanghai 201620, China
  • Received:2018-12-07 Revised:2019-05-28 Online:2019-12-15 Published:2019-12-18
  • Contact: QIN Xiaohong

摘要:

为探索烟梗浆二醋酸纤维素(CDA)制备的可行性及其可纺性,以醋酸为溶剂,浓硫酸为催化剂,采用低温乙酰化法制备了烟梗木浆三醋酸纤维素(CTA)和二醋酸纤维素,将二醋酸纤维素与市售二醋酸纤维素按质量比20∶80、35∶65、50∶50共混,通过静电纺丝技术进行纺丝,并对纤维的结构和性能进行表征。结果表明:反应时间为5 h,纸浆与乙酸固液比为1∶5,在活化过程中加入硫酸后,醋酸纤维素的取代度从2.68提高到2.86,达到了三醋酸纤维素的标准;在80 ℃时水解6 h后可得到取代度约为2.5的CDA;与纯纺CDA纤维得到的亚微米混纺纤维相比,烟梗浆二醋酸纤维素与市售二醋酸纤维素混纺纤维的线密度及其不匀率降低,表明了烟梗浆CDA混纺的可行性。

关键词: 醋酸纤维素, 烟梗溶解浆, 醋化, 水解, 静电纺丝

Abstract:

In order to prepare cellulose diacetate (CDA) from burley tobacco stalk pulp (TSP) and measure its spinnability, cellulose triacetate (CTA) and CDA were prepared from burley TSP by low-temperature acetylation using acetic anhydride and sulfuric acid as catalyst. The prepared CDA was mixed with commercial CDA at a mass ratio of 20∶80, 35∶65 and 50∶50, respectively, and electrospinning was applied to spin the fibers. The structure and properties of the fibers were characterized. The result shows that with reaction time of 5 h, pulp to acetic acid sold-liquid ratio of 1∶5 and addition of sulfuric acid during activation procedure, the degree of substitution of TSP cellulose acetate increases from 2.68 to 2.86, which meets the requirements of CTA. TSP cellulose diacetate with degree of substitution about 2.5 is obtained by hydrolysis at 80 ℃ for 6 h. Compared with sub-micron blended fibers obtained from pure electrospun commercial CDA, the fiber diameter and unevenness of blended fibers of TSP cellulose diacetate and commercial CDA both reduce, proving the feasibility of blended spinning of TSP cellulose diacetate.

Key words: cellulose acetate, tobacco stalk dissolving pulp, acetylation, hydrolysis, electrospinning

中图分类号: 

  • TQ353.21

图1

不同木浆的形态"

表1

4种木浆的性能对比"

木浆名称 成分含量/% 黏度/
(mPa·s)
灰分含
量/%
水分含
量/%
白度/% 纤维长
度/mm
葡聚糖 木聚糖 木质素 甘露糖
TSP 93.7±0.5 2.4±0.1 0.4±0.0 0.0±0.0 5.9 0.15±0.01 6.81±0.53 89.0±0.4 0.43
HWP 79.5±0.1 13.6±0.1 2.2±0.2 0.0±0.0 17.6 0.33±0.06 5.03±0.32 85.7±0.2 0.70
DPA 95.7±0.6 1.7±0.2 0.3±0.0 1.4±0.1 30.4 0.21±0.02 5.97±0.22 92.3±0.4 1.37
DPB 95.4±0.1 1.6±0.2 0.3±0.0 1.0±0.2 19.1 0.27±0.02 5.48±0.14 92.1±0.4 1.43

图2

不同反应时间醋化溶液的浊度值"

图3

不同固液比处理条件下溶液的浊度值"

图4

TSP、TSP过滤物与TSP三醋酸纤维素的傅里叶红外光谱图"

图5

TSP 和TSP三醋酸纤维素与市售CTA的TG与DTG曲线"

表2

滴定法测定的CTA取代度值"

试样名称 V1 /mL V2 /mL CAV /% 水分/% X
TSP对比样 6.36±0.04 0.57±0.01 58.52±0.40 1.10±0.05 2.68±0.02
TSP 6.58±0.03 0.57±0.01 61.31±0.31 1.15±0.01 2.86±0.03
HWP 6.71±0.03 0.57±0.01 62.00±0.31 0.96±0.01 2.95±0.03
DPA 6.70±0.04 0.57±0.01 62.02±0.20 1.17±0.01 2.96±0.03
DPB 6.51±0.03 0.62±0.01 60.78±0.31 3.09±0.01 2.86±0.03
市售 CTA 6.70±0.03 0.57±0.01 61.58±0.15 0.46±0.01 2.92±0.02

图6

CTA形态及其显色机制 注:图(a)中从左至右分别为DPA、DPB、TSP、HWP 三醋酸纤维素。"

图7

市售CTA取代度值与水解时间的关系"

表3

滴定法测定的CDA取代度值"

试样
名称
V1 /mL V2 /mL CAV /% 水分/% X
TSP
对比样
6.02±0.01 0.49±0.02 57.00±0.06 3.06±0.02 2.56±0.02
HWP 6.20±0.01 0.49±0.02 59.05±0.01 3.30±0.02 2.72±0.01
DPA 6.00±0.02 0.50±0.02 56.91±0.18 3.35±0.01 2.55±0.02
DPB 5.76±0.03 0.49±0.02 55.90±0.26 5.81±0.01 2.48±0.02
市售
CDA
6.05±0.03 0.60±0.05 55.45±0.30 1.71±0.01 2.45±0.03

图8

不同木浆制备的二醋酸纤维素形态 注:样品从左至右分别为DPA、DPB、TSP、HWP二醋酸纤维素。"

图9

不同TSP二醋酸纤维素与市售CDA共混比静电纺混纺亚微米纤维的扫描电镜照片(×5 000)"

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