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An Efficient Method of Birch Ethanol Lignin Sulfation with a Sulfaic Acid-Urea Mixture

Описание

Тип публикации: статья из журнала

Год издания: 2022

Идентификатор DOI: 10.3390/molecules27196356

Ключевые слова: 2d nmr spectroscopy, birch ethanol lignin, ftir spectroscopy, gel permeation chromatography, sulfamic acid, sulfated product characterization, sulfation process optimization, thermal analysis, ureaalcohol, 64-17-5, lignin, 9005-53-2, sulfate, 14808-79-8, sulfur, 13981-57-2, 7704-34-9, urea, 57-13-6, ethanol, lignin, sulfates, sulfur, urea

Аннотация: For the first time, the process of birch ethanol lignin sulfation with a sulfamic acid-urea mixture in a 1,4-dioxane medium was optimized experimentally and numerically. The high yield of the sulfated ethanol lignin (more than 96%) and containing 7.1 and 7.9 wt % of sulfur was produced at process temperatures of 80 and 90 °C for 3 Показать полностьюh. The sample with the highest sulfur content (8.1 wt %) was obtained at a temperature of 100 °C for 2 h. The structure and molecular weight distribution of the sulfated birch ethanol lignin was established by FTIR, 2D 1H and 13C NMR spectroscopy, and gel permeation chromatography. The introduction of sulfate groups into the lignin structure was confirmed by FTIR by the appearance of absorption bands characteristic of the vibrations of sulfate group bonds. According to 2D NMR spectroscopy data, both the alcohol and phenolic hydroxyl groups of the ethanol lignin were subjected to sulfation. The sulfated birch ethanol lignin with a weight average molecular weight of 7.6 kDa and a polydispersity index of 1.81 was obtained under the optimum process conditions. Differences in the structure of the phenylpropane units of birch ethanol lignin (syringyl-type predominates) and abies ethanol lignin (guaiacyl-type predominates) was manifested in the fact that the sulfation of the former proceeds more completely at moderate temperatures than the latter. In contrast to sulfated abies ethanol lignin, the sulfated birch ethanol lignin had a bimodal and wider molecular weight distribution, as well as less thermal stability. The introduction of sulfate groups into ethanol lignin reduced its thermal stability. © 2022 by the authors.

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Издание

Журнал: Molecules

Выпуск журнала: Vol. 27, Is. 19

Номера страниц: 6356

ISSN журнала: 14203049

Издатель: MDPI

Персоны

  • Levdansky A.V. (Institute of Chemistry and Chemical Technology, Krasnoyarsk Science Center, Siberian Branch, Russian Academy of Sciences, Akademgorodok 50/24, Krasnoyarsk, 660036, Russian Federation)
  • Vasilyeva N.Y. (Institute of Chemistry and Chemical Technology, Krasnoyarsk Science Center, Siberian Branch, Russian Academy of Sciences, Akademgorodok 50/24, Krasnoyarsk, 660036, Russian Federation, School of Non-Ferrous Metals and Material Science, Siberian Federal University, Pr. Svobodny 79, Krasnoyarsk, 660041, Russian Federation)
  • Malyar Y.N. (Institute of Chemistry and Chemical Technology, Krasnoyarsk Science Center, Siberian Branch, Russian Academy of Sciences, Akademgorodok 50/24, Krasnoyarsk, 660036, Russian Federation, School of Non-Ferrous Metals and Material Science, Siberian Federal University, Pr. Svobodny 79, Krasnoyarsk, 660041, Russian Federation)
  • Kondrasenko A.A. (Institute of Chemistry and Chemical Technology, Krasnoyarsk Science Center, Siberian Branch, Russian Academy of Sciences, Akademgorodok 50/24, Krasnoyarsk, 660036, Russian Federation)
  • Fetisova O.Y. (Institute of Chemistry and Chemical Technology, Krasnoyarsk Science Center, Siberian Branch, Russian Academy of Sciences, Akademgorodok 50/24, Krasnoyarsk, 660036, Russian Federation)
  • Kazachenko A.S. (Institute of Chemistry and Chemical Technology, Krasnoyarsk Science Center, Siberian Branch, Russian Academy of Sciences, Akademgorodok 50/24, Krasnoyarsk, 660036, Russian Federation, School of Non-Ferrous Metals and Material Science, Siberian Federal University, Pr. Svobodny 79, Krasnoyarsk, 660041, Russian Federation)
  • Levdansky V.A. (Institute of Chemistry and Chemical Technology, Krasnoyarsk Science Center, Siberian Branch, Russian Academy of Sciences, Akademgorodok 50/24, Krasnoyarsk, 660036, Russian Federation)
  • Kuznetsov B.N. (Institute of Chemistry and Chemical Technology, Krasnoyarsk Science Center, Siberian Branch, Russian Academy of Sciences, Akademgorodok 50/24, Krasnoyarsk, 660036, Russian Federation, School of Non-Ferrous Metals and Material Science, Siberian Federal University, Pr. Svobodny 79, Krasnoyarsk, 660041, Russian Federation)

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