Burn-off characteristics and pore structure evolution of peat-based activated carbon during steam activation
DENG Feng,XIE Qiang,YANG Minjian,WAN Chaoran,LIU Deqian,LIANG Dingcheng
孔结构调控是活性炭制备研究的核心,碳烧失伴随并决定着孔结构的演化。为研究泥炭基活性炭孔结构演化过程中碳烧失特征,将贵州毕节泥炭样品破碎、粉磨,在氮气氛围进行热重分析,并采用无黏结剂压块成型,再破碎后、炭化,在不同活化温度、时间下水蒸气活化制得活性炭,测定活性炭样品的碘值、亚甲蓝值和焦糖脱色率吸附性能指标,利用气体吸附仪、拉曼光谱和扫描电子显微镜表征其孔结构、碳结构和微观形貌,研究吸附性能、孔结构、碳结构间的关系。结果表明:泥炭基活性炭的孔结构演化随活化温度的升高分为造孔(750~800 ℃)、扩孔(800~850 ℃)、孔塌陷(850~900 ℃)和炭表面烧蚀(900~950 ℃)4个阶段,分别以无序炭(D3)及散乱石墨层结构(D1)、散乱石墨层结构(D1)及平行的石墨层间的不规则层(D2)、活性位点碳(D4)、规则的石墨微晶结构(G)的烧蚀为主;随活化时间的增加分为充分发育期(60~120 min)和过度发育期(120~150 min)2个阶段,分别以无序炭(D3)和活性位点碳(D4)的烧蚀为主。炭表面烧蚀或孔结构过度发育之前有效的调孔以全程清除无序炭、部分消耗缺陷微晶炭、少量激活活性位点碳来实现。随活化程度的加深,活性炭的碳烧失由颗粒内表面为主转为由内向外、再转为由外向内,表面孔依次呈现出生成、融并和坍塌的形貌特征。
Porosity adjustment is a core of the activated carbon preparation research,and the carbon burn-off accompanies and determines the pore structure evolution. In order to explore the relationship between the burn-off and the pore structure evolution of activated carbon from peat,the peat from Bijie,Guizhou province was sampled,crushed,ground,thermogravimetric analyzed in a nitrogen environment,and briquetted without binder,then a series of activated carbon samples were prepared by steam activation at different temperatures and times following carbonization. The adsorption indexes including iodine value,methylene blue value and caramel decolorization rate were determined,and the pore structure,carbonaceous structure and micro morphology of activated carbon samples were characterized by gas adsorption instrument,Raman spectroscopy and scanning electron microscope with the aim to study the relationship among the adsorption properties,pore structure,and carbonaceous structure. The results show that with the increase of the activation temperature,the pore structure evolution of activated carbon undergoes four stages,namely,pore forming(750-800 ℃ ),pore expanding(800-850 ℃ ),pore collapsing(850-900 ℃ ) and char surface ablating(900-950 ℃ ),respectively,and these stages are dominated correspondingly by the burn-off of amorphous carbon(D3 ) and scattered graphite layer structure(D1 ),burn-off of scattered graphite layer structure(D1 ) and irregular layers among parallel graphite layers(D2 ),burn-off of carbon in the active sites(D4 ),and burn-off of regular graphite carbon crystallite structure(G). Meanwhile,with the increase of the activation time,the pore structure evolution of activated carbon undergoes two stages,namely,pore fully development(60-120 min) and pore over development(120-150 min) respectively,are dominated correspondingly by burn-off of amorphous carbon(D3 ) and carbon in the active sites(D4 ). Thus, the pore structure of peat based activated carbon might be efficiently adjusted prior to char surface ablation or pore over development in activation process by removing disordered carbon in the whole course,consuming a portion of defective microcrystalline carbon,and activating a small amount of carbon at active sites. In other words,an elaborate control of burn-off,from internal surface mainly to inside-out and then to outside-in,and the surface pores appear to be formation,melting and collapse successively.
peat,activated carbon,carbonaceous structure,pore structure,burn-off characteristics
主办单位:煤炭科学研究总院有限公司 中国煤炭学会学术期刊工作委员会