Carbonization of α2-fraction isolated from thermosolvolysis coal pitch, analysis of the structure of carbonizates

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Abstract

The article presents the results of the study of the composition and thermal transformations of α2-fraction (quinoline-soluble, toluene-insoluble), isolated from the pitch product of thermal dissolution of coal in a binary mixture of technical solvents of coal and oil origin. Based on thermal analysis data, the dynamics of α2-fraction destruction with the release of volatile substances in the temperature range up to 1100°C was established. Carbonized products were obtained by carbonization of the α2-fraction. The features of the molecular composition and spatial structure of the starting materials and the obtained carbonizates depending on temperature were studied using chemical analysis, IR spectroscopy, CP/MAS13C NMR and X-ray diffraction. A consistent transformation of spatial structural components into packet turbostratic and graphite domains was established. It was shown that at an elevated temperature of 1100°C, extended forms of graphite domains are formed — precursors of needle coke.

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About the authors

P. N. Kuznetsov

Institute of Chemistry and Chemical Technology SB RAS, Federal Research Center “Krasnoyarsk Scientific Center SB RAS”

Author for correspondence.
Email: kuzpn@icct.ru
Russian Federation, 660036 Krasnoyarsk

B. Avid

Institute of Chemistry and Chemical Technology MAS

Email: kuzpn@icct.ru
Mongolia, Ulaanbaata

L. I. Kuznetsova

Institute of Chemistry and Chemical Technology SB RAS, Federal Research Center “Krasnoyarsk Scientific Center SB RAS”

Email: kuzpn@icct.ru
Russian Federation, 660036 Krasnoyarsk

A. M. Zhizhaev

Institute of Chemistry and Chemical Technology SB RAS, Federal Research Center “Krasnoyarsk Scientific Center SB RAS”

Email: kuzpn@icct.ru
Russian Federation, 660036 Krasnoyarsk

E. S. Kamensky

Institute of Chemistry and Chemical Technology SB RAS, Federal Research Center “Krasnoyarsk Scientific Center SB RAS”

Email: kuzpn@icct.ru
Russian Federation, 660036 Krasnoyarsk

O. Yu. Fetisova

Institute of Chemistry and Chemical Technology SB RAS, Federal Research Center “Krasnoyarsk Scientific Center SB RAS”

Email: kuzpn@icct.ru
Russian Federation, 660036 Krasnoyarsk

G. N. Bondarenko

Institute of Chemistry and Chemical Technology SB RAS, Federal Research Center “Krasnoyarsk Scientific Center SB RAS”

Email: kuzpn@icct.ru
Russian Federation, 660036 Krasnoyarsk

S. A. Novikova

Institute of Chemistry and Chemical Technology SB RAS, Federal Research Center “Krasnoyarsk Scientific Center SB RAS”

Email: kuzpn@icct.ru
Russian Federation, 660036 Krasnoyarsk

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Supplementary files

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2. Fig. 1. Scheme of pitch fractionation to obtain the α2-fraction.

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3. Fig. 2. Scheme of the unit for carbonization of the α2-fraction.

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4. Fig. 3. TG and DTG curves for the α2-fraction and carbonates obtained from it (a), (b) and the total yield of volatile substances during programmed heating to 1100°C (c).

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5. Fig. 4. FTIR spectra for the initial pitch, the α2-fraction isolated from it and carbonates obtained at different temperatures; examples of deconvolution of bands in the region of 3100–3000 cm–1 (a), (b) and 900–700 cm–1 for pitch (b), (c).

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6. Fig. 5. CP/MAS 13C NMR spectra of pitch and α2-fraction isolated from it.

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7. Fig. 6. X-ray diffraction patterns of the initial α2-fraction and carbonization products at 300, 400, 600 and 1100°C.

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8. Fig. 7. Deconvolution of the main asymmetric diffraction reflection using the sample carbonized at 400°C as an example.

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9. Fig. 8. Change in the proportion of structural components depending on the carbonization temperature of the α2-fraction: 1 – gamma 2; 2 – gamma 1; 3 – turbostratic domain; 4 – graphite domain.

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10. Fig. 9. Change in the structure of graphite-like domains depending on the carbonization temperature: 1 – turbostratic; 2 – graphite (a); 1 – Lc, turbostratic; 2 – Lc, graphite; 3 – La, graphite (b).

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