石油炼制与化工 ›› 2012, Vol. 43 ›› Issue (6): 16-19.

• 基础研究 • 上一篇    下一篇

FCC油浆研制中间相沥青泡沫炭

杨小军,査庆芳,郭燕生,张玉贞   

  1. 中国石油大学(华东)重质油国家重点实验室
  • 收稿日期:2011-09-21 修回日期:2011-11-28 出版日期:2012-06-12 发布日期:2012-05-31
  • 通讯作者: 査庆芳 E-mail:cqf@sdkj.hdpu.edu.cn

PREPARATION OF MESOPHASE PITCH CARBON FOAM FROM FCC SLURRY OIL

  • Received:2011-09-21 Revised:2011-11-28 Online:2012-06-12 Published:2012-05-31

摘要: 以FCC油浆富芳油制备中间相沥青基泡沫炭,在箱式电阻炉内800~1 400 ℃范围、通入1 L/min氮气稀释空气的条件下,考察了中间相沥青泡沫在炭化前后的SEM微观形态、表面官能团和XRD衍射图的变化情况,尤其是炭化温度的影响。SEM照片表明:随炭化温度升高,泡沫炭孔壁逐渐被破坏。XRD分析结果表明:随炭化温度升高,泡沫炭的晶格规整性得到改善。红外分析结果表明:中间相沥青泡沫固化后,表面存在大量的C-H、C=O和COO-基团,经过炭化后,COO-和C-H含量减少,O-H含量增加,在1 100 ℃以上继续炭化,泡沫炭表面的C-H,C=O,O-H和COO-基团含量变化较小。综合考虑泡沫炭的表面官能团、晶格参数和形态,适宜的炭化温度为1 100 ℃,在此温度下可以得到形貌较好、孔径为150~300μm的泡沫炭样品,其晶体结构参数La,Lc,N,d002分别为2.5 nm,2.31 nm,10,0.347 6 nm。

Abstract: Mesophase pitch-based carbon foams were prepared from aromatics rich FCC slurry oil. The effect of carbonization temperature (800—1 400 ℃) on the microstructure, surface properties, microcrystal structure and shape of the prepared carbon foams was studied using a box resistance furnace under air diluted with 1 L/min nitrogen conditions. Carbon foam samples prior and post to carbonization were characterized by SEM, FT-IR and XRD techniques. Results showed that there were large amount of functional groups on the surface of the mesophase pitch carbon foam, such as C-H, C=O and COO- groups. After carbonization, the content of COO- and C-H groups reduced greatly, meanwhile, the content of O-H group increased. However, when carbonization temperature exceeded 1 100 ℃, the content of such functional groups on the surface of carbon foam was basically unchanged. With the increase of carbonization temperature, the shape and microcrystal structure of the carbon foams were improved, and the interlayer spacing of the microcrystal became regularly, which was helpful to form graphite microcrystal structure. On the whole, the optimum carbonization temperature was selected as 1 100 ℃,carbonizing under such temperature, good shape of carbon foam sample with pore size in the range of 150—300 μm could be obtained and its microcrystal structure parameters were as follows: La=2.5 nm, Lc=2.31 nm, N=10 and d002=0.347 6 nm.