Removal of QI from Medium-temperature Coal Tar Pitch and Preparation of Needle Coke through Carbonization

doi:10.11901/1005.3093.2015.685

Chinese Journal of Materials Research

2016, Vol. 30

Issue (6): 448-456 DOI: 10.11901/1005.3093.2015.685

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Removal of QI from Medium-temperature Coal Tar Pitch and Preparation of Needle Coke through Carbonization

TANG Xianyi¹, WEI Xiaohui¹, XU Deping^1,^**(

), ZHANG Haiyong¹, HE Xin¹, XIONG Chu'an^1,³, TANG Hanying²

1. School of Chemistry& Environmental Engineering, China University of Mining & Technology (Beijing), Beijing 100083, China
2. Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190, China
3. Heilongjiang Institute of Science and Technology, Harbin 150022, China

Cite this article:

TANG Xianyi, WEI Xiaohui, XU Deping, ZHANG Haiyong, HE Xin, XIONG Chu'an, TANG Hanying. Removal of QI from Medium-temperature Coal Tar Pitch and Preparation of Needle Coke through Carbonization. Chinese Journal of Materials Research, 2016, 30(6): 448-456.

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Abstract

The carbonization in a tube bomb of medium-temperature coal tar pitch and the purified coal tar pitch, of which quinoline insoluble (QI) had been removed by anti-solvent method, was comparatively studied. The results show that coal tar pitch with high QI contents could not be suitable for preparation of needle coke of high quality. However, the coke which was obtained through carbonization under 0.2 MPa at 500℃ for 10 h had a relatively lower coefficient of thermal expansion (CTE). The QI could be removed effectively by anti-solvent method when kerosene and wash oil were mixed as solvents. By a precipitation process at 100℃ and precipitation time for 4 h with the ratio of wash oil to kerosene was 0.4 and stirring for 0.5 h, the QI contents of the refined coal tar pitch could be reduced to 0.0914% and 0.0695% for the ratios of solvents to coal tar pitch as 1.8 and 2 respectively. The needle coke which were prepared by such refined coal tar pitch showed lower CTE after being carbonized at 500℃, by 0.2 MPa and for 10 h.

Key words: synthesizing and processing technics medium-temperature coal tar pitch anti-solvent method QI carbonization needle coke

Received: 01 December 2015

ZTFLH:

TQ522.65

Fund: *Supported by the Joint Funds of the National Natural Science Foundation of China No.U1361124

About author: **To whom correspondence should be addressed, Tel: (010)62331048, E-mail: xdp1073@163.com

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	Xianyi TANG
	Xiaohui WEI
	Deping XU
	Haiyong ZHANG
	Xin HE
	Chu'an XIONG
	Hanying TANG

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https://www.cjmr.org/EN/10.11901/1005.3093.2015.685 OR https://www.cjmr.org/EN/Y2016/V30/I6/448

Fig.1 sketch of increase of quinolone insoluble

Fig.2 Schematic diagram of experimental apparatus of carbonization

Solvent	$d 15.6 15.6$ ¹	Initial boiling point /℃	T_V/℃	Final boiling point/℃	BMCI²
Kerosene	0.794	103	191.2	281	24
Wash oil	1.001	212	259.6	330	109

Table 1 The properties of kerosene and wash oil

Table 2 The properties of coal tar pitch

Fig.3 Polarized light micrographs of green coke lumps at different carbonization conditions (A, B, C: 460℃, 0.2, 0.4, 0.6 MPa, 16 h; D, E, F: 480℃, 0.2, 0.4, 0.6 MPa, 16 h; G, H, I: 500℃, 0.2, 0.4, 0.6 MPa, 10 h; J, K, L: 520℃, 0.2, 0.4, 0.6 MPa, 10 h)

Table 3 Properties of needle cokes

Fig.4 The change of the content of QI and the yield with the ratio of wash oil to kerosene

Fig.5 The change of the content of QI and the yield with precipitating temperature

Fig.6 The change of the content of QI and the yield with precipitating time

Fig.7 The change of the content of QI and the yield with the ratio of solvents to coal tar pitch

Fig.8 Polarized light micrographs of Green coke carbonization by purified coal tar pitch

Fig.9 Lump cokes’ photographs of CTP3 and CTP4\

Fig.10 XRD pattern of needle coke

Fig.11 Characteristic peaks of XRD of needle coke

Table 4 Microstructural parameters of XRD of needle cokes

Fig.12 SEM images of needle coke

1	XIAO Ruihua, Coal Tar Chemical Engineering (Beijing, Metallurgical Industry Press, 2009) p.262
	(肖瑞华, 煤焦油化工学(北京, 冶金工业出版社, 2009) p.262)
2	WU Su, WANG Lei, WANG Xiaobing, CAI Chuang, Effect of pretreatment methods of raw material on coking of needle coke from coal tar pitch by delayed coking, Carbon Techniques, 31(003), 5(2012)
	(吴甦, 王磊, 王小冰, 菜闯, 原料预处理方法对延迟焦化成焦的影响, 炭素技术, 31(003), 5(2012)) doi: 10.3969/j.issn.1001-3741.2012.03.010
3	A. Figueiras, M. Granda, E. Casal, J. Bermejo, J. Bonhomme, R. Menéndez, Influence of primary QI and on pitch pyrolysis with reference to unidirectional C/C composites, Carbon, 36(7-8), 883(1998)
4	C. Panaitescu, G. Predeanu, Microstructure characteristics of toluene and quinoline insolubles from coal-tar pitch and their cokes, International Journal of Coal Geology, 71(4), 448(2007) doi: 10.1016/j.coal.2006.11.003
5	Moriyama R, Hayashi J, Chiba T, Effects of quinoline-insoluble particles on the elemental processed of mesophase sphere formation, Carbon, 42(12-13), 2443(2004) doi: 10.1016/j.carbon.2004.04.044
6	H. Marsh, C. S. Latham, E. M. Gray, The structure and behavior of QI material in pitch, Carbon, 23(5), 555(1985) doi: 10.1017/S0260210500118054
7	SHUI Henfu, FENG Yingtong, YUAN Xiaoming, Structural characteristics of quinolone Insoluble fraction and their Influence on mesophase transformation, Journal of Fuel Chemistry and Technology, 23(1), 62(1995)
	(水恒福, 冯映桐, 哀晓敏, 不同喹啉不溶物的特性及对中间相转化过程的影响, 燃料化学学报, 23(1), 62(1995))
8	Isao Mochida, Takashi Ando, Keiko Maeda, Hiroshi Fujitsu, Kenjiro Takeshita, Catalytic Carbonization of aromatic hydrocarbons-Ⅸ: carbonization mechanism of heterocyclic sulfur compounds leading to the anisotropic coke, Carbon, 18(2), 131(1980)
9	GUO Shaoqing, ZHANG Wei, WANG Guiyun, ZHAO Liangfu, Progress of pretreatment methods of raw material for needle coke from coal tar, Carbon Technique, 30(3), 40(2011)
	(郭少青, 张伟, 王桂云, 赵亮富, 煤系针状焦原料预处理技术进展, 炭素技术, 30(3), 40(2011)) doi: 10.3969/j.issn.1001-3741.2011.03.011
10	H. S. Kitakyushu, W. M. Kawasaki, Process for preparing needle coke, United States Patent US 4116815(Sep.26, 1978)
11	W. M. Kawasaki, H. S. Kitakyushu, Y. O. Kitalyushus, Process for preparing a raw material for the manufacture of needle coke, United States Patent US 4127472(Nov.28, 1978)
12	SUN Zhenxing, XIONG Jieming, GE Minglan, CHI Yaoling, YI Yufeng, WANG Kuiguang, LI Tianxiang, Removal quinolone-insolubles from medium coal tar pitch, Carbon Technique, 28(3), 10(2009)
	(孙振兴, 熊杰明, 葛明兰, 迟姚玲, 易玉峰, 王奎光, 李天祥, 中温沥青的喹啉不溶物脱除, 炭素技术, 28(3), 10(2009))
13	SUN Yanrui, XIONG Jieming, FANG Yi, SUN Guojuan, Removal of quinoline-insolubles in soft coal tar pitch by mixed solvent method, Journal of Beijing Institute of Petro-chemical Technology, 18(3), 32(2010)
	(孙艳悦, 熊杰明, 方懿, 孙国娟, 混合溶剂法脱除软沥青的喹啉不溶物, 北京石油化工学院学报, 18(3), 32(2010)) doi: 10.3969/j.issn.1008-2565.2010.03.007
14	J. D. Books, G. H. Taylor, The formation of graphitizing carbons from the liquid phase, Carbon, 3(2), 185(1965)
15	Yoon Seong-Ho, Korai Yozo, Mochia Isao, Axial nano-scale microstructures in graphitized fibers inherited from liquid crystal mesophase pitch, Carbon, 34(1), 83(1996) doi: 10.1016/0008-6223(95)00138-7
16	ZHA Qingfang, GUO Yansheng, WU Mingbo, WANG Hui, ZHANG Yuzhen, Composition changes in The co-caboniazation of FCC slurry and VR, New carbon materials, 17(2), 4(2002)
	(查庆芳, 郭燕生, 吴明铂, 王辉, 张玉贞, 减压渣油与 FCC油浆共炭化的化学组成变化, 新型炭材料, 17(2), 4(2002)) doi: 10.3321/j.issn:1007-8827.2002.02.002
17	LIU Yihong, LUO Yunhua, CHENG Jian, Needle coke from petroleum residue—a study of the thermal behavior of the middle fraction of the residue, New carbon materials, 18(2), 128(2003)
	(刘以红, 罗运华, 程健, 石油渣油制备针状焦研究-中间馏分热反应研究, 新型炭材料, 18(2), 128(2003)) doi: 10.3321/j.issn:1007-8827.2003.02.009
18	SUN Quan, WANG Baocheng, ZHANG Huaiping, LI Xianglan, BAI Yingbin, The influence of a magnetic field during carbonization on the microstructure and electrical conductivity of needle cokes, New carbon materials, 26(6), 429(2011)
	(孙权, 王保成, 张怀平, 李香兰, 白英彬, 炭化过程中的磁场作用对针状焦结构及导电性能的影响, 新型炭材料, 26(6), 429(2011))
19	GAO Lijuan, ZHAO Xuefei, LAI Shiquan, CHENG Junxia, LU Yiqiang, Compositions and structure characterizations of coal tar refined soft pitch, Spectroscopy and Spectral Analysis, 29(8), 2152(2009)
	(高丽娟, 赵雪飞, 赖仕全, 程俊霞, 鲁毅强, 煤焦油精制软沥青组成及结构的表征, 光谱学与光谱析, 29(8), 2152(2009)) doi: 10.3964/j.issn.1000-0593(2009)08-2152-05
20	Isao Mochida, You Qing Fei, Kinya Sakanishi, Yozo Korai, Hidehiko Usuba, Kunio Miura, Carbonization of coal tar pitch denitrogenated by metal sulfates, Carbon, 30(2), 241(1992) doi: 10.1016/0008-6223(92)90085-B
21	QIAN Shuan, The Basic theory on formation process of shape structure of needle coke, Petroleum processing and petrochemicals, 1(1), 14(1980)
	(钱树安, 针状焦形态结构形成过程基本原理, 石油炼制与化工, 1(1), 14(1980))
22	Isao Mochida, You Qing Fei, Yozo Korai, Carbonization in the tube bomb leading to needle coke: III. Carbonization properties of several coal tar pitch, Carbon, 27(3), 375(1989) doi: 10.1016/0008-6223(89)90069-9

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