Interpretation of Carboxymethylation in Cellulose Pretreatment by 1H-NMR Spectroscopy

Woo-Young Song; Audrey Zahra; Soo-Jeong Shin

doi:10.7584/JKTAPPI.2024.2.56.1.11

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2024 Vol.56, Issue 1 Preview Page Next Page

Research Article

Interpretation of Carboxymethylation in Cellulose Pretreatment by ¹H-NMR Spectroscopy

28 February 2024. pp. 11-21

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Abstract

Carboxymethylation reaction in cellulose was investigated with sodium hydroxide concentration, monochloroacetic acid concentration, temperature, and reaction time as main variables. The degree of carboxymethylation in cellulose was analyzed by phenolphthalein titration, IR spectroscopy, and ¹H-NMR spectroscopy methods. The NMR spectroscopic method showed more accurate DS (degree of substitution) values than other IR spectroscopy or titration methods. IR method had the advantage of quick measurement but was difficult in baseline correction. The titration method needed longer data acquisition time and higher deviation to less accuracy. Carboxymethylation in cellulose was run in S_N2 reaction by sodium hydroxide and monochloroacetic acid concentration with main variables. Substitution position was analyzed by ¹H-NMR spectroscopic with acid hydrolysates of carboxymethylated cellulose. Carboxymethylation in lower reaction temperatures led to more C6-hydorxyl substitution reactions in cellulose, but the C6- and C2-hydroxyl group position competed with increasing reaction temperature.

Keywords

Carboxymethylation

NMR

FT-IR

titration

cellulose

cellulose nanofibril

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Information

Publisher :Korea Technical Association of The Pulp and Paper Industry
Publisher(Ko) :한국펄프종이공학회
Journal Title :Journal of Korea TAPPI
Journal Title(Ko) :펄프종이기술
Volume : 56
No :1
Pages :11-21
Received Date : 2024-01-08
Revised Date : 2024-02-13
Accepted Date : 2024-02-16
DOI :https://doi.org/10.7584/JKTAPPI.2024.2.56.1.11

Journal of Korea TAPPI 펄프종이기술 ISSN:0253-3200(Print)

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