Kinetic analysis of cellulose acetate/cellulose II hybrid fiber formation by alkaline hydrolysis

Najua Tulos, David Harbottle, Andrew Hebden, Parikshit Goswami, Richard S. Blackburn

Research output: Contribution to journalArticle

Abstract

Cellulose acetate (CA) can be converted to cellulose II through a deacetylation process using ethanolic NaOH solution. Infrared spectroscopy was used to observe the degree of acetylation by comparing the absorption intensities of C=O and C-O stretches. Attenuated total reflection-Fourier transform infrared (ATR-FTIR) analysis, which only measures a few microns into the fiber diameter, was compared with FTIR, which measures the whole fiber cross-section. Steady deacetylation of the whole fiber over 180 min was observed with FTIR to eventual complete deacetylation. In comparison, ATR-FTIR shows deacetylation occurring more rapidly to complete deacetylation after 90 min, indicating rapid deacetylation of the CA fiber periphery. Data were fitted to a pseudo-second order kinetic model, with high correlation (R 2 > 0.99), and it was observed that the deacetylation rate (k 2 ) observed with ATR-FTIR (-0.634 min -1 ) was twice as rapid as the deacetylation rate observed with FTIR (-0.315 min -1 ). IR observations were in agreement with the analysis of fiber cross-sections by confocal microscopy, where it was observed that changes in fiber morphology occurred with treatment time and progressive hydrolysis of cellulose acetate to cellulose II. A differential fiber chemical composition was created within the CA fiber cross-section; after 5 min, the outer regions of the fiber cross-section are hydrolyzed to cellulose II and this hydrolysis increases heterogeneously with time to complete hydrolysis after 180 min and conversion to cellulose II. These results indicate the potential to produce fibers with a differential periphery/core structure, which can be accurately designed according to the relative degrees of cellulose II/CA required for specific applications by varying the treatment time in application of this model.

LanguageEnglish
Pages4936-4942
Number of pages7
JournalACS Omega
Volume4
Issue number3
DOIs
Publication statusPublished - 6 Mar 2019

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Cellulose
Hydrolysis
Kinetics
Fibers
Fourier transforms
Infrared radiation
acetylcellulose
Acetylation
Confocal microscopy
Infrared spectroscopy
Chemical analysis

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Tulos, Najua ; Harbottle, David ; Hebden, Andrew ; Goswami, Parikshit ; Blackburn, Richard S. / Kinetic analysis of cellulose acetate/cellulose II hybrid fiber formation by alkaline hydrolysis. In: ACS Omega. 2019 ; Vol. 4, No. 3. pp. 4936-4942.
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abstract = "Cellulose acetate (CA) can be converted to cellulose II through a deacetylation process using ethanolic NaOH solution. Infrared spectroscopy was used to observe the degree of acetylation by comparing the absorption intensities of C=O and C-O stretches. Attenuated total reflection-Fourier transform infrared (ATR-FTIR) analysis, which only measures a few microns into the fiber diameter, was compared with FTIR, which measures the whole fiber cross-section. Steady deacetylation of the whole fiber over 180 min was observed with FTIR to eventual complete deacetylation. In comparison, ATR-FTIR shows deacetylation occurring more rapidly to complete deacetylation after 90 min, indicating rapid deacetylation of the CA fiber periphery. Data were fitted to a pseudo-second order kinetic model, with high correlation (R 2 > 0.99), and it was observed that the deacetylation rate (k 2 ) observed with ATR-FTIR (-0.634 min -1 ) was twice as rapid as the deacetylation rate observed with FTIR (-0.315 min -1 ). IR observations were in agreement with the analysis of fiber cross-sections by confocal microscopy, where it was observed that changes in fiber morphology occurred with treatment time and progressive hydrolysis of cellulose acetate to cellulose II. A differential fiber chemical composition was created within the CA fiber cross-section; after 5 min, the outer regions of the fiber cross-section are hydrolyzed to cellulose II and this hydrolysis increases heterogeneously with time to complete hydrolysis after 180 min and conversion to cellulose II. These results indicate the potential to produce fibers with a differential periphery/core structure, which can be accurately designed according to the relative degrees of cellulose II/CA required for specific applications by varying the treatment time in application of this model.",
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Kinetic analysis of cellulose acetate/cellulose II hybrid fiber formation by alkaline hydrolysis. / Tulos, Najua ; Harbottle, David ; Hebden, Andrew; Goswami, Parikshit ; Blackburn, Richard S.

In: ACS Omega, Vol. 4, No. 3, 06.03.2019, p. 4936-4942.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Kinetic analysis of cellulose acetate/cellulose II hybrid fiber formation by alkaline hydrolysis

AU - Tulos, Najua

AU - Harbottle, David

AU - Hebden, Andrew

AU - Goswami, Parikshit

AU - Blackburn, Richard S.

PY - 2019/3/6

Y1 - 2019/3/6

N2 - Cellulose acetate (CA) can be converted to cellulose II through a deacetylation process using ethanolic NaOH solution. Infrared spectroscopy was used to observe the degree of acetylation by comparing the absorption intensities of C=O and C-O stretches. Attenuated total reflection-Fourier transform infrared (ATR-FTIR) analysis, which only measures a few microns into the fiber diameter, was compared with FTIR, which measures the whole fiber cross-section. Steady deacetylation of the whole fiber over 180 min was observed with FTIR to eventual complete deacetylation. In comparison, ATR-FTIR shows deacetylation occurring more rapidly to complete deacetylation after 90 min, indicating rapid deacetylation of the CA fiber periphery. Data were fitted to a pseudo-second order kinetic model, with high correlation (R 2 > 0.99), and it was observed that the deacetylation rate (k 2 ) observed with ATR-FTIR (-0.634 min -1 ) was twice as rapid as the deacetylation rate observed with FTIR (-0.315 min -1 ). IR observations were in agreement with the analysis of fiber cross-sections by confocal microscopy, where it was observed that changes in fiber morphology occurred with treatment time and progressive hydrolysis of cellulose acetate to cellulose II. A differential fiber chemical composition was created within the CA fiber cross-section; after 5 min, the outer regions of the fiber cross-section are hydrolyzed to cellulose II and this hydrolysis increases heterogeneously with time to complete hydrolysis after 180 min and conversion to cellulose II. These results indicate the potential to produce fibers with a differential periphery/core structure, which can be accurately designed according to the relative degrees of cellulose II/CA required for specific applications by varying the treatment time in application of this model.

AB - Cellulose acetate (CA) can be converted to cellulose II through a deacetylation process using ethanolic NaOH solution. Infrared spectroscopy was used to observe the degree of acetylation by comparing the absorption intensities of C=O and C-O stretches. Attenuated total reflection-Fourier transform infrared (ATR-FTIR) analysis, which only measures a few microns into the fiber diameter, was compared with FTIR, which measures the whole fiber cross-section. Steady deacetylation of the whole fiber over 180 min was observed with FTIR to eventual complete deacetylation. In comparison, ATR-FTIR shows deacetylation occurring more rapidly to complete deacetylation after 90 min, indicating rapid deacetylation of the CA fiber periphery. Data were fitted to a pseudo-second order kinetic model, with high correlation (R 2 > 0.99), and it was observed that the deacetylation rate (k 2 ) observed with ATR-FTIR (-0.634 min -1 ) was twice as rapid as the deacetylation rate observed with FTIR (-0.315 min -1 ). IR observations were in agreement with the analysis of fiber cross-sections by confocal microscopy, where it was observed that changes in fiber morphology occurred with treatment time and progressive hydrolysis of cellulose acetate to cellulose II. A differential fiber chemical composition was created within the CA fiber cross-section; after 5 min, the outer regions of the fiber cross-section are hydrolyzed to cellulose II and this hydrolysis increases heterogeneously with time to complete hydrolysis after 180 min and conversion to cellulose II. These results indicate the potential to produce fibers with a differential periphery/core structure, which can be accurately designed according to the relative degrees of cellulose II/CA required for specific applications by varying the treatment time in application of this model.

KW - Textiles

KW - Sodium hydroxide

KW - Deacetylation

KW - Differential fiber

KW - Periphery/core

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DO - 10.1021/acsomega.9b00159

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VL - 4

SP - 4936

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T2 - ACS Omega

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