木质素纳米颗粒/天然纤维基活性碳纤维材料的制备及其电化学性能

doi:10.16085/j.issn.1000-6613.2021-1797

化工进展 ›› 2022, Vol. 41 ›› Issue (7): 3770-3783.DOI: 10.16085/j.issn.1000-6613.2021-1797

木质素纳米颗粒/天然纤维基活性碳纤维材料的制备及其电化学性能

张伟¹(), 安兴业¹(), 刘利琴¹, 龙垠荧¹, 张昊¹, 程正柏², 曹海兵², 刘洪斌¹()

^1.天津科技大学轻工科学与工程学院，天津市制浆造纸重点实验室，天津 300457
^2.浙江景兴纸业股份有限公司，浙江平湖 314214

收稿日期:2021-08-22 修回日期:2021-11-22 出版日期:2022-07-25 发布日期:2022-07-23
通讯作者: 安兴业,刘洪斌
作者简介:张伟（1996—），男，硕士研究生，研究方向为先进纤维与纸基功能材料。E-mail：1435048976@qq.com。
基金资助:
国家重点研发计划(2019YFC1905904);国家自然科学基金(3210140637);浙江景兴纸业股份有限公司校企合作项目;中国博士后科学基金(2021M692401);天津市自然科学基金(19JCQNJC05400)

Preparation and electrochemical performance of lignin nanoparticles/natural fiber based activated carbon fiber materials

ZHANG Wei¹(), AN Xingye¹(), LIU Liqin¹, LONG Yinying¹, ZHANG Hao¹, CHENG Zhengbai², CAO Haibing², LIU Hongbin¹()

^1.Tianjin Key Laboratory of Pulp and Paper, College of Light Industry Science and Engineering, Tianjin University of Science and Technology, Tianjin 300457, China
^2.Zhejiang Jingxing Paper Joint Stock Company Limited, Pinghu 314214, Zhejiang, China

Received:2021-08-22 Revised:2021-11-22 Online:2022-07-25 Published:2022-07-23
Contact: AN Xingye,LIU Hongbin

摘要/Abstract

摘要：

以木质素纳米颗粒（LNPs）负载的天然纤维复合材料为研究对象，利用KOH活化的方法对其进行处理制备生物质基复合多孔活性碳纤维电极材料。随后在三电极体系中对合成的复合多孔活性碳纤维电极材料进行了电化学性能测试。研究表明，在0.5A/g的电流密度下，KOH活化的复合碳纤维电极材料的比电容为351.13F/g，远高于相同条件下未活化的复合碳纤维电极材料的比电容（7.88F/g）和未负载LNPs的天然纤维基活性碳纤维材料（306.50F/g）。而且在活化过程中，负载在纤维表面的LNPs会形成多孔的活性碳层结构，这会进一步提高复合活性碳纤维材料的循环稳定性，同时LNPs中丰富的羟基赋予复合材料额外的赝电容。在10A/g的电流密度下经过10000次循环后，复合活性碳纤维电极材料的电容保持率仍然为95%，高于未负载LNPs的活性碳纤维电极材料的电容保持率87%。结果表明，木质素纳米颗粒/天然纤维基活性碳纤维材料是一种理想的电极材料，本研究也为LNPs在生物质碳纤维作为储能电极材料的高值化应用提供了一条新途径。

关键词: 活化, 氢氧化钾, 木质素纳米颗粒, 生物质, 超级电容器, 电化学

Abstract:

This study was focused on the composite lignin nanoparticles (LNPs) loaded natural fibers, which was by KOH activation to prepare composite porous activated carbon fiber electrode materials. Then the as-prepared activated carbon fiber electrode was tested to evaluate the electrochemical performance in a three-electrode system. The results showed that the specific capacitance of KOH activated carbon fiber electrode material was 351.13F/g at the current density of 0.5A/g, which was much higher than that of non-activated carbon fiber electrode material (7.88F/g) and natural fiber activated carbon fiber material without LNPs (306.50F/g) under the same conditions. In addition, fiber surface loaded with LNPs formed porous activated carbon layer structure during the activation process, which further improved the cyclic stability of the composite activated carbon fiber material. Meanwhile, the abundant hydroxyl of LNPs endowed the composite material with additional pseudocapacitance. After 10000 cycles at a current density of 10A/g, the capacitive retention of the composite activated carbon fiber electrode was still at 95%, which was higher than that of the activated carbon fiber electrode of 87% without LNPs loading. The results indicated that lignin nanoparticles/ natural fiber based activated carbon fiber was an ideal electrode material for supercapacitors. This study also provided a new way for the high-value application of LNPs in biomass carbon fiber as energy storage electrode material.

Key words: activation, potassium hydroxide (KOH), lignin nanoparticles (LNPs), biomass, supercapacitor, electrochemistry

中图分类号:

TM53

张伟, 安兴业, 刘利琴, 龙垠荧, 张昊, 程正柏, 曹海兵, 刘洪斌. 木质素纳米颗粒/天然纤维基活性碳纤维材料的制备及其电化学性能[J]. 化工进展, 2022, 41(7): 3770-3783.

ZHANG Wei, AN Xingye, LIU Liqin, LONG Yinying, ZHANG Hao, CHENG Zhengbai, CAO Haibing, LIU Hongbin. Preparation and electrochemical performance of lignin nanoparticles/natural fiber based activated carbon fiber materials[J]. Chemical Industry and Engineering Progress, 2022, 41(7): 3770-3783.

图/表 13

表1 实验所用材料

材料名称	材料纯度	生产厂家
天然针叶木浆纤维	—	浙江景兴纸业股份有限公司
木质素	—	实验室碱法蒸煮制浆过程中自提
氢氧化钾（KOH）	分析纯	福晨（天津）化学试剂有限公司
无水乙醇	分析纯	天津市东天正精细化学试剂厂
硫酸（H₂SO₄）	分析纯	天津市风船化学试剂科技有限公司
盐酸（HCl）	分析纯	天津市风船化学试剂科技有限公司
不锈钢网	—	天津安诺合新能源科技有限公司
聚四氟乙烯乳液（质量分数60%）	—	上海麦克林生化科技有限公司
乙炔炭黑	—	上海麦克林生化科技有限公司
氮气	高纯（>99.9%）	天津市军粮城常福气体有限公司

表2 实验所用仪器

仪器名称	型号	生产厂家
电子分析天平	EL204	梅特勒（上海）有限公司
管式炉	OTF-1200X	合肥科晶仪器有限公司
扫描电子显微镜	JSM-IT300LV	日本电子公司
比表面积和孔径分析仪	BELSORP-max	日本麦奇克拜尔有限公司
同步热分析仪	SDT650	美国TA仪器公司
X射线衍射仪	D8	德国布鲁克公司
X射线光电子能谱仪	Escalab 250Xi+	Thermo Scientific科技公司
手动压片机	769YP-15A	天津市科器高新技术公司
电化学工作站	CHI660	上海辰华有限公司

表3 各生物质碳纤维样品的制备条件

样品名	材料	活化条件（前体与KOH的比例，m/m）
LF₀	LNPs/天然纤维复合材料	未活化
LFC	LNPs/天然纤维基复合碳纤维材料	未活化
LFC_1∶2	复合多孔生物质活性碳纤维材料	1∶2
LFC_1∶4	复合多孔生物质活性碳纤维材料	1∶4
LFC_1∶6	复合多孔生物质活性碳纤维材料	1∶6
LFC_1∶8	复合多孔生物质活性碳纤维材料	1∶8
LFC_1∶10	复合多孔生物质活性碳纤维材料	1∶10
FC_1∶2	天然纤维基活性碳纤维材料	1∶2
FC_1∶4	天然纤维基活性碳纤维材料	1∶4
FC_1∶6	天然纤维基活性碳纤维材料	1∶6
FC_1∶8	天然纤维基活性碳纤维材料	1∶8
FC_1∶10	天然纤维基活性碳纤维材料	1∶10

图1 复合多孔生物质活性碳纤维材料的制备机理图

图2 LF0和LFC的SEM图

图3 不同KOH用量的复合多孔生物质活性碳纤维材料的SEM图

图4 LFC（未活化）、LFC1∶8（前体∶KOH=1∶8）、FC1∶8（前体∶KOH=1∶8）样品的N2吸附-脱附等温线和孔径分布曲线

表4 LFC、LFC1∶8、FC1∶8样品的孔特性

样品名	总比表面积/m²?g^-1	微孔比表面积/m²?g^-1	介孔比表面积/m²?g^-1	总孔容/cm³?g^-1	微孔孔容/cm³?g^-1	介孔孔容/cm³?g^-1
LFC	312.97	134.10	178.87	0.2658	0.0611	0.2047
LFC_1∶8	2187.10	1820.14	366.96	1.1798	0.7604	0.4194
FC_1∶8	3274.0	2196.2	1077.8	1.6719	0.9075	0.7644

图5 LFC（未活化）、LFC1∶8（前体∶KOH=1∶8）、FC1∶8（前体∶KOH=1∶8）样品的XRD谱图和XPS谱图

表5 LFC、LFC1∶8和FC1∶8样品的C 1s与O 1s含量分析（质量分数）

样品	C 1s/%			O 1s/%
样品	C―C	C―O	C $? ????$ O	C $? ????$ O	O $? ????$ C―O―C $? ????$ O
LFC	65.0	29.5	5.5	53.8	46.2
LFC_1∶8	47.2	24.5	28.3	52.8	47.2
FC_1∶8	48.9	23.0	28.1	50.2	49.8

表5 LFC、LFC1∶8和FC1∶8样品的C 1s与O 1s含量分析（质量分数）

样品	C 1s/%			O 1s/%
样品	C―C	C―O	C $? ????$ O	C $? ????$ O	O $? ????$ C―O―C $? ????$ O
LFC	65.0	29.5	5.5	53.8	46.2
LFC_1∶8	47.2	24.5	28.3	52.8	47.2
FC_1∶8	48.9	23.0	28.1	50.2	49.8

表6 LFC、LFC1∶8和FC1∶8样品的元素组成（质量分数） (%)

样品	C	O	N	P	S
LFC	88.92	7.66	3.03	0.17	0.22
LFC_1∶8	91.71	6.52	0.95	0.27	0.55
FC_1∶8	87.56	10.42	1.30	0.40	0.31

图6 各负载LNPs的活性炭材料（LFC）与未负载LNPs的活性炭材料（FC）的GCD曲线与CV曲线

图7 复合多孔生物质活性碳纤维材料的倍率性能、交流阻抗以及循环稳定性

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木质素纳米颗粒/天然纤维基活性碳纤维材料的制备及其电化学性能

Preparation and electrochemical performance of lignin nanoparticles/natural fiber based activated carbon fiber materials

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