纺织学报 ›› 2020, Vol. 41 ›› Issue (08): 1-8.doi: 10.13475/j.fzxb.20191205408

• 纤维材料 •    下一篇

高邻位酚醛基纳米活性碳纤维制备及其吸附性能

杨凯1, 张啸梅1, 焦明立2(), 贾万顺1, 刁泉2, 李咏1, 张彩云2, 曹健2   

  1. 1.中原工学院 服装学院, 河南 郑州 450007
    2.中原工学院 材料与化工学院, 河南 郑州 450007
  • 收稿日期:2019-12-24 修回日期:2020-05-11 出版日期:2020-08-15 发布日期:2020-08-21
  • 通讯作者: 焦明立
  • 作者简介:杨凯(1982—),女,副教授,博士。主要研究方向为功能性材料。
  • 基金资助:
    国家自然科学基金项目(51973246);国家自然科学基金项目(51803245);河南省高校科技创新人才支持计划项目(19HASTIT024);河南省重点科技攻关计划项目(182102210129);河南省高等学校青年骨干教师培养计划项目(2019GGJS145);中原工学院交叉学科团队支持计划项目(2018003)

Preparation and adsorption performance of high-ortho phenolic resin based activated carbon nanofibers

YANG Kai1, ZHANG Xiaomei1, JIAO Mingli2(), JIA Wanshun1, DIAO Quan2, LI Yong1, ZHANG Caiyun2, CAO Jian2   

  1. 1. School of Fashion, Zhongyuan University of Technology, Zhengzhou, Henan 450007, China
    2. School of Materials and Chemical Engineering, Zhongyuan University of Technology, Zhengzhou, Henan 450007, China
  • Received:2019-12-24 Revised:2020-05-11 Online:2020-08-15 Published:2020-08-21
  • Contact: JIAO Mingli

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摘要：

为提高酚醛基纳米活性碳纤维的吸附性能,首先采用乙酸锌、硫酸双催化合成高邻位酚醛树脂,然后配制酚醛/聚乙烯醇缩丁醛(PVB)混合溶液,采用静电纺丝、固化、炭化和活化工艺制备得到柔性高邻位酚醛基纳米活性碳纤维,借助傅里叶变换红外光谱仪、扫描电子显微镜、热重分析仪、比表面积及孔径分析仪对其结构和性能进行测试与分析。结果表明:静电纺丝制备的酚醛初生纤维在溶液固化后,酚环对位取代增加,纤维内发生了分子间交联,但PVB有一定的醇解,使酚醛纤维在炭化过程中低温稳定性下降,而高温残碳率升高,炭化后制备得到多孔碳纤维;活化后得到的高邻位酚醛基纳米活性碳纤维比表面积为1 409 m2/g,其对亚甲基蓝及碘的吸附量分别达到837和2 641 mg/g。

关键词: 高邻位酚醛树脂, 纳米活性碳纤维, 静电纺丝, 吸附性能, 微孔结构

Abstract:

In order to improve the adsorption performance of phenolic resin based activated carbon fibers, the high-ortho phenolic resin was catalyzed by zinc acetate and sulphuric acid, and then mixed with polyvinyl butyral(PVB)as raw material, the flexible high-ortho phenolic resin based activated carbon nanofibers were prepared by a sequence of processes, including electrospinning, consolidation, carbonization and activation, and then the structure and performance were tested and analyzed by Fourier infrared spectrum, scanning electron microscopy, thermogravimetric analysis and specific surface area and pore size distribution analyzer. The results show that the crosslinking structures of the phenolic fibers are formed with the increase of the char yield, and the thermal stability at low temperature decreases with the alcoholysis of PVB. The adsorbing evaluation demonstrates that the high specific surface area of the high-ortho phenolic resin based activated carbon nanofiber reaches 1 409 m2/g, and its adsorption capacity for methylene blue and iodine appears as high as 837 and 2 641 mg/g, respectively.

Key words: high-ortho phenolic resin, activated carbon nanofiber, electrospinning, adsorption performance, microporous structure

中图分类号: 

  • TQ342.86

表1

纺丝原液中PR和PVB的配比"

样品编号 PR质量分数 PVB质量分数
1# 1.1 4.00
2# 2.2 3.75
3# 3.3 3.50
5# 5.5 3.00
7# 7.7 2.50
9# 9.9 2.00

图1

不同制备阶段酚醛试样的红外光谱图"

图2

不同PR和PVB配比的PACF纤维的扫描电镜照片"

图3

不同制备阶段酚醛试样的TG曲线"

图4

不同PR和PVB配比的PCF及 PACF纤维的氮气吸附/脱附等温线和孔径分布 注:图(c)和(d)纵坐标中V为孔容,cm3/g;D为平均孔径,nm。"

表2

不同PR和PVB配比的PCF 和 PACF纤维的孔结构参数"

试样编号 比表面积/
(m2·g-1)		 微孔比表面积/
(m2·g-1)		 孔容/
(m3·g-1)		 微孔孔容/
(m3·g-1)		 平均孔
径/nm		 介孔比
例/%
PCF-1# 375 313 0.207 0.147 2.22 28.8
PCF-2# 507 422 0.273 0.196 2.16 28.3
PCF-3# 712 648 0.344 0.278 1.94 19.2
PCF-5# 648 594 0.299 0.248 1.85 17.1
PACF-2# 1 302 1 133 0.668 0.523 2.05 27.7
PACF-3# 1 409 1 198 0.771 0.568 2.19 26.4
PACF-5# 773 599 0.434 0.302 2.25 30.5

图5

不同PR和PVB配比的PCF和PACF纤维的碘及亚甲基蓝吸附量"

图6

吸附时间对PACF-3#纤维亚甲基蓝、碘吸附量的影响"

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