Quantification of cellulose nanowhiskers sulfate esterification levels

Jin Gu, Jeffrey M. Catchmark, Edward Q. Kaiser, Douglas D. Archibald

Research output: Contribution to journalArticle

52 Citations (Scopus)

Abstract

Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, combustion gas analysis and N2 adsorption were used to quantify the degree of desulfation of cellulose nanowhiskers (CNWs). CNWs were produced by hydrolyzing cotton cellulose with sulfuric acid or hydrochloric acid. Hydrochloric acid treatment did not result in any cellulose chemical modification. Hydrolysis using H2SO4 introduced sulfate groups onto the cellulose surface. Our results indicate that commercial cotton cellulose as received contained sulfur. The sulfur content of H 2SO4-prepared CNWs was higher than that exhibited by the original cellulose due to the esterification process. Two desulfation methods, acid-catalyzed and solvolytic desulfation, have been explored to remove the sulfate groups. Neither desulfation method examined removed the sulfate groups from H2SO4-prepared CNWs completely. An estimation of surface sulfate esterification levels was made based on a model of the cellulose structure and available surface area of CNWs. According to these models, more than one third of hydroxyl groups on the surface were substituted by sulfate.

Original languageEnglish (US)
Pages (from-to)1809-1816
Number of pages8
JournalCarbohydrate Polymers
Volume92
Issue number2
DOIs
StatePublished - Feb 15 2013

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Nanowhiskers
Esterification
Cellulose
Sulfates
Hydrochloric Acid
Hydrochloric acid
Sulfur
Cotton
cellulose sulfate
Gas fuel analysis
Chemical modification
Sulfuric acid
Hydroxyl Radical
Fourier transform infrared spectroscopy
Hydrolysis

All Science Journal Classification (ASJC) codes

  • Organic Chemistry
  • Polymers and Plastics
  • Materials Chemistry

Cite this

Gu, Jin ; Catchmark, Jeffrey M. ; Kaiser, Edward Q. ; Archibald, Douglas D. / Quantification of cellulose nanowhiskers sulfate esterification levels. In: Carbohydrate Polymers. 2013 ; Vol. 92, No. 2. pp. 1809-1816.
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Quantification of cellulose nanowhiskers sulfate esterification levels. / Gu, Jin; Catchmark, Jeffrey M.; Kaiser, Edward Q.; Archibald, Douglas D.

In: Carbohydrate Polymers, Vol. 92, No. 2, 15.02.2013, p. 1809-1816.

Research output: Contribution to journalArticle

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AU - Gu, Jin

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AU - Archibald, Douglas D.

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AB - Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, combustion gas analysis and N2 adsorption were used to quantify the degree of desulfation of cellulose nanowhiskers (CNWs). CNWs were produced by hydrolyzing cotton cellulose with sulfuric acid or hydrochloric acid. Hydrochloric acid treatment did not result in any cellulose chemical modification. Hydrolysis using H2SO4 introduced sulfate groups onto the cellulose surface. Our results indicate that commercial cotton cellulose as received contained sulfur. The sulfur content of H 2SO4-prepared CNWs was higher than that exhibited by the original cellulose due to the esterification process. Two desulfation methods, acid-catalyzed and solvolytic desulfation, have been explored to remove the sulfate groups. Neither desulfation method examined removed the sulfate groups from H2SO4-prepared CNWs completely. An estimation of surface sulfate esterification levels was made based on a model of the cellulose structure and available surface area of CNWs. According to these models, more than one third of hydroxyl groups on the surface were substituted by sulfate.

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