摘要
以熔融纺丝制备的Kraft硬木木质素纤维(HKL)为原料,经炭化得到木质素基炭纤维(HKL-CF),再采用水蒸气活化法制备了活性炭纤维(HKL-ACF),通过红外光谱仪和扫描电镜研究了水蒸气活化对活性炭纤维化学结构和表面形貌的影响,采用全自动物理吸附仪、X射线衍射仪和拉曼光谱仪等研究了活化时间、活化温度和活化水蒸气流量对所制备活性炭纤维的比表面积、孔结构和微晶结构的影响规律。研究表明,水蒸气活化处理提高了活性炭纤维中的C—O和■结构含量;随着活化时间的延长,活性炭纤维的比表面积增大,且随活化温度和水蒸气流量的提高呈现出先增大后减小的趋势;晶粒尺寸随着活化时间和温度的提高,逐渐变小,纤维表面的石墨化程度随活化时间的增加,逐渐变大;活化温度800℃,活化时间4 h,水蒸气流量1 mL/min下制备的活性炭纤维的BET比表面积最高可达2 081.34 m~2/g,总孔容最大为1.60 cm~3/g。
Kraft hardwood lignin activated carbon fiber(HKL-ACF)was prepared from carbon fiber(HKL-CF)by water vapor activation using melt-spun kraft hardwood lignin(HKL)fiber as raw material.On this basis,the effects of water vapor activation on the chemical structure and morphology of activated carbon fibers were investigated by infrared spectrometer and scanning electron microscopy.And the effects of different activation time,activation temperature and water vapor flow rate on specific surface area,pore structure and microcrystalline structure of the carbon fiber were studied by automatic physical adsorption instrument,X-ray diffractometer and Raman spectrometer.The results showed that the chemical structure of carbon fiber was changed greatly after water vapor activation,and the contents of C—O and ■ were increased.At the same time,the specific surface area increased with the increase of activation time,and increased firstly and then decreased with the increase of activation temperature and water vapor flow rate.With the increase of activation time and temperature,the grain size became smaller.The degree of graphitization of the fiber surface became larger with the increase of activation time.The maximum BET specific surface area of activated carbon fiber was 2 081.34 m~2/g and the maximum pore volume was 1.60 cm~3/g under the activation temperature of 800℃,activation time of 4 h,and water vapor flow rate of 1 m L/min.
引文
[1]RAGAUSKAS A J,BECKHAM G T,BIDDY M J,et al.Lignin valorization:Improving lignin processing in the biorefinery[J].Science,2014,344(6185):1246843.
[2]UPTON B M,KASKO A M.Strategies for the conversion of lignin to high-value polymeric materials:Review and perspective[J].Chemical Reviews,2015,116(4):2275-2306.
[3]SAHA D,LI Y,BI Z,et al.Studies on supercapacitor electrode material from activated lignin-derived mesoporous carbon[J].Langmuir,2014,30(3):900-910.
[4]ZHU H,LUO W,CIESIELSKI P N,et al.Wood-derived materials for green electronics,biological devices,and energy applications[J].Chemical Reviews,2016,116(16):9305-9374.
[5]WANG S,LI Y,XIANG H,et al.Low cost carbon fibers from bio-renewable lignin/poly(lactic acid)(PLA) blends[J].Composites Science and Technology,2015,119:20-25.
[6]金枝.水蒸气活化木材液化物炭纤维的孔结构与性能[D].北京:北京林业大学,2015.
[7]LIU W,WANG X,ZHANG M.Preparation of highly mesoporous wood-derived activated carbon fiber and the mechanism of its porosity development[J].Holzforschung,2017,71(5):363-371.
[8]LIN J,ZHAO G.Preparation and characterization of high surface area activated carbon fibers from lignin[J].Polymers,2016,8(10):369.
[9]WANG S,ZHOU Z,XIANG H,et al.Reinforcement of lignin-based carbon fibers with functionalized carbon nanotubes[J].Composites Science and Technology,2016,128:116-122.
[10]金彦任,黄振兴.吸附与孔径分布[M].北京:国防工业出版社,2015.
[11]LI Z Q,LU C J,XIA Z P,et al.X-ray diffraction patterns of graphite and turbostratic carbon[J].Carbon,2007,45(8):1686-1695.
[12]程朝歌,石彦平,陈师,等.不同活化温度下粘胶基炭纤维的拉曼光谱研究[J].炭素技术,2016,35(1):1-14.
[13]吕永根.高性能炭纤维[M].北京:化学工业出版社,2016.