DETERMINATION OF THE STRUCTURE OF CELLULOSE ETHERS BY 13C NMR SPECTROSCOPY OF PRODUCTS OF ACID-CATALYZED HYDROLYSIS

  • Сергей (Sergey) Валерьевич (Valer'evich) Арасланкин (Araslankin) National Research Mordovia State University Email: araslankin@bk.ru
  • Валентин (Valintin) Александрович (Aleksandrovich) Калязин (Kalyazin) National Research Mordovia State University Email: valentin1k@rambler.ru
  • Сергей (Sergey) Геннадьевич (Gennad'evich) Кострюков (Kostryukov) National Research Mordovia State University http://orcid.org/0000-0002-1774-0836 Email: kostryukov_sg@mail.ru
  • Павел (Pavel) Сергеевич (Sergeevich) Петров (Petrov) National Research Mordovia State University Email: petrovps83@gmail.com
DOI_disc_logo https://doi.org/10.14258/jcprm.2019014127
Keywords: hydroxypropyl methylcellulose (HPMC), hydroxyethyl cellulose (HEC), hydroxyethyl methylcellulose (HEMC), glucopyranose, acid-catalyzed hydrolysis, degree of substitution (DS), molar substitution (MS), 13C NMR spectroscopy, integral intensity

Abstract

Cellulose ethers (CE) are widely used in the pharmaceutical, food and construction industries to impart the necessary rheological, thixotropic and water-retention properties to water dispersion systems. In this paper, we compare the substitution parameters of hydroxypropyl methylcellulose (HPMC), hydroxyethyl cellulose (HEC) and hydroxyethyl methylcellulose (HEMC), which are obtained from 13C NMR spectroscopy of products of acid-catalyzed hydrolysis and cellulose ethers. Accurate data on the degree of substitution at the 2, 3 and 6 positions (DSC-2, DSC-3 and DSC-6) were obtained from 13С NMR spectra of products of acid-catalyzed hydrolysis. The total degree of substitution (DStotal) and molar substitution (MS) for the hydroxyethyl and hydroxypropyl substituents were determined. The distribution of substituents at different positions of the glucopyranose link indicates that the most reactive are the C-2 and C-6 positions, as well as the hydroxyl of the hydroxyethyl fragment. Within the proposed method, the degree of substitution and molar substitution are determined: DSHPMC = 1.79 and MSHPMC = 0.38; DSHEC = 1.02 and MSHEC = 2.03; DSHEMC = 1.93 and MSHEMC = 1.82. It is shown that the results are consistent with the data obtained from 13C NMR (СРMAS) spectra of the same cellulose ethers. The proposed method of analysis is characterized by the simplicity of the experiment, the accuracy and informative of the results obtained.

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Author Biographies

Сергей (Sergey) Валерьевич (Valer'evich) Арасланкин (Araslankin), National Research Mordovia State University

преподаватель кафедры физической химии

Валентин (Valintin) Александрович (Aleksandrovich) Калязин (Kalyazin), National Research Mordovia State University

инженер лаборатории ядерного магнитного резонанса

Сергей (Sergey) Геннадьевич (Gennad'evich) Кострюков (Kostryukov), National Research Mordovia State University

доцент кафедры органической химии, кандидат химических наук

Павел (Pavel) Сергеевич (Sergeevich) Петров (Petrov), National Research Mordovia State University

заведующий лабораторией ядерного магнитного резонанса, кандидат химических наук

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Фрагменты спектров ЯМР 13С
Published
2019-03-06
How to Cite
1. Арасланкин (Araslankin)С. (Sergey) В. (Valer’evich), Калязин (Kalyazin)В. (Valintin) А. (Aleksandrovich), Кострюков (Kostryukov)С. (Sergey) Г. (Gennad’evich), Петров (Petrov)П. (Pavel) С. (Sergeevich) DETERMINATION OF THE STRUCTURE OF CELLULOSE ETHERS BY 13C NMR SPECTROSCOPY OF PRODUCTS OF ACID-CATALYZED HYDROLYSIS // Chemistry of plant raw material, 2019. № 1. P. 51-62. URL: https://journal.asu.ru/cw/article/view/4127.
Issue
No 1 (2019)
Section
Biopolymers of plants

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