顏丙峰等:煤瀝青與煤直接液化殘渣共炭化製備中間相炭微球機理及...

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原文連結：https://link.springer.com/article/10.1007/s40789-019-00271-6

文章創新點

通過煤液化殘渣精製瀝青(DCLR-P)與煤瀝青（CTP）共炭化製備中間相炭微球，彌補了單一原料（CTP）的缺陷，改進了原料炭化的反應性，調整了炭化速度及中間相的結構，提高了產品收率，改善了粒徑分布，產品可以用作鋰電池負極材料。

摘要：本文對煤直接煤液化殘渣(DCLR)進行脫灰得到了煤液化殘渣精製瀝青(DCLR-P)。通過煤焦油瀝青(CTP)與煤液化殘渣精製瀝青(DCLR-P)共炭化製備了中間相炭微球(MCMBs)。隨著DCLR-P加入量的提高，MCMBs的產率由47.8%提高到56.8%。同時，MCMBs的粒徑分布變窄，其粒徑D90/D10的比值由154.88降至6.53。結果表明，DCLR-P的加入有利於MCMBs的生成。採用1H-NMR、FTIR、SEM、XRD等手段分析了CTP與DCLR-P共炭化製備MCMBs的機理及其產品特性。結果表明，DCLR-P的供氫指數(PDQI)為13.32，明顯高於CTP(0.83)。這表明，與CTP相比，DCLR-P含有更多的環烷結構，在縮聚反應中會發生氫轉移。DCLR-P的脂肪結構可以提高瀝青的溶解度和流動性，使MCMBs結構更加有序。石墨化後的MCMBs微觀結構為層狀結構，這對其電學性能是有利的。對石墨化後的MCMBs用作鋰離子電池負極材料進行了測試，石墨化後的MCMBs粒度、堆密度、比表面積和初始充放電效率均達到了國家標準GB/T-24533-2009中CMB-I（中間相炭微球類鋰電負極材料一級產品）的要求。然而，由於石墨化程度不高，導致其初始放電容量僅為296.3 mAh·g1。

關鍵詞：中間相炭微球，煤直接液化殘渣，機理，特性

Mechanisms and characteristics of mesocarbon microbeads prepared by co-carbonization of coal tar pitch and direct coal liquefaction residue

Abstract:DCLR-P was prepared by direct coal liquefaction residue (DCLR) with ash removal. In the present experiments, mesocarbon microbeads (MCMBs) were prepared by co-carbonization of coal tar pitch (CTP) and DCLR-P. With the increase of DCLR-P content, the yield of MCMBs increased from 47.8% to 56.8%. At the same time, the particle sizes distribution of MCMBs was narrowed, resulting in the decrease ofD90/D10ratio from 154.88 to 6.53. The results showed that DCLR-P had a positive effect on the preparation of MCMBs. 1H-NMR, FTIR, SEM and XRD were used to analyze the mechanisms and characteristics of MCMBs prepared by co-carbonization of CTP and DCLR-P. The results showed that the Proton Donor Quality Index (PDQI) of DCLR-P was 13.32, significantly higher than that of CTP (0.83). This indicated that DCLR-P had more naphthenic structure than CTP, which leads to hydrogen transferring in polycondensation reaction. The aliphatic structure of DCLR-P can improve the solubility and fusibility of mesophase, thereby making the structure of MCMBs more structured. The microstructure of the graphitized MCMBs had a substantially parallel carbon layer useful for its electrical performance. The performance of graphitized MCMBs as a negative electrode material for Li-ion batteries was tested. The particle sizes, tap density, specific surface area and initial charge–discharge efficiency of graphitized MCMBs met the requirements of CMB-I in GB/T-24533-2009. However, the initial discharge capacity of graphitized MCMB was only 296.3 mAh·g1 due to the low degree of graphitization of MCMBs.

Keywords: Mesocarbon microbeads, Direct coal liquefaction residue, Mechanisms, Characteristics

文中插圖：

Fig. 1Yields of MCMBs with different contents of DCLR-P

Fig. 2Particle sizes distribution of MCMBs

Fig. 3Variation of terminal pressure with different ratios of DCLR-P

Fig. 4The ratios of C/H of MP and MCMBs with DCLR-P added

Fig. 5FTIR spectra of CTP, DCLR-P and MP

Fig. 6XRD patterns of MCMBs with DCLR-P added

Fig. 7Polarized micrographes of MP (×500) a 0%, b 10%, c 20%, d 30%

Fig. 8SEM micrographs of MCMBs10 and graphitized MCMBs10 a MCMBs10. b, c graphitized MCMBs10

Fig. 9XRD patterns of graphitized MCMBs0 and MCMBs10

Fig. 10Raman Spectra of graphitized MCMBs0 and MCMBs10

引用格式：

Yan Bingfeng, Wang Guangyao. Mechanisms and characteristics of mesocarbon microbeads prepared by co-carbonization of coal tar pitch and direct coal liquefaction residue. International Journal of Coal Science and Technology, 2019,6(4): 633-642.

來源：JCST國際煤炭科學技術學報

徵稿郵箱：[e-mail]

信息提供：常明然編輯整理：劉暘

審核：畢永華

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