Skip to main content
Log in

The residual amide content of cellulose sequentially solvent-exchanged and then vacuum-dried

  • Published:
Cellulose Aims and scope Submit manuscript

Abstract

Most celluloses are soluble in 8 mass % lithium chloride/N,N-dimethylacetamide (LiCl/DMAc) and/or 8 mass % LiCl/1,3-dimethyl-2-imidazolidinone (LiCl/DMI) with solvent-exchange treatment from water to DMAc or DMI through acetone. In this study, the residual DMAc or DMI adsorbed on celluloses after the solvent-exchange and then vacuum-drying at 60 °C for 48 h was determined by UV spectroscopy and elementary analysis. Significant amounts of DMI or DMAc remain in the solvent-exchanged celluloses even after vacuum drying: about 1.2 mmol/g and 1.0 mmol/g for DMI and DMAc, respectively. Thus, corrections of molecular-mass parameters of celluloses, which were reported in previous literatures based on the assumption that no residual amides are present in the solvent-exchanged and then vacuum-dried celluloses, are needed.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Scheme 1
Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

References

  • Ishii D, Tatsumi D, Matsumoto T (2003) Effect of solvent exchange on the solid structure and dissolution behavior of cellulose. Biomacromolecules 4:1238–1243

    Article  CAS  Google Scholar 

  • Ishii D, Kanazawa Y, Tatsumi D, Matsumoto T (2007) Effect of solvent exchange on the pore structure and dissolution behavior of cellulose. J Appl Polym Sci 103:3976–3984

    Article  CAS  Google Scholar 

  • Ishii D, Tatsumi D, Matsumoto T (2008) Effect of solvent exchange on the supramolecular structure, the molecular mobility and the dissolution behavior of cellulose in LiCl/DMAc. Carbohydr Res (in press) doi: 10.1016/j.carres.2008.01.035

  • Isogai A, Atalla RH (1998) Dissolution of cellulose in aqueous NaOH solutions. Cellulose 5:309–319

    Article  CAS  Google Scholar 

  • Heinze T, Liebert T (2001) Unconventional methods in cellulose functionalization. Prog Polym Sci 26:1689–1762

    Article  CAS  Google Scholar 

  • Matsumoto T, Tatsumi D, Tamai N, Takaki T (2002) Solution properties of celluloses from different biological origins in LiCl·DMAc. Cellulose 8:275–282

    Article  Google Scholar 

  • McCormick CL, Callais PA, Hutchinson BH Jr (1985) Solution studies of cellulose in lithium chloride and N,N-dimethylacetamide. Macromolecules 18:2394–2401

    Article  CAS  Google Scholar 

  • Potthast A, Rosenau T, Sixta H, Kosma P (2002) Degradation of cellulosic materials by heating in DMAc/LiCl. Tetrahedron Lett 43:7757–7759

    Article  CAS  Google Scholar 

  • Sjöholm E, Gustafsson K, Berthold F, Colmsjö A (2000) Influence of the carbohydrate composition on the molecular weight distribution of kraft pulps. Carbohydr Polym 41:1–7

    Article  Google Scholar 

  • Tamai N, Tatsumi D, Matsumoto T (2004) Rheological properties and molecular structure of tunicate cellulose in LiCl/1,3-dimethyl-2-imidazolidinone. Biomacromolecules 5:422–432

    Article  CAS  Google Scholar 

  • Turbak A (1984) Recent developments in cellulose solvent systems. Tappi J 67:94–96

    CAS  Google Scholar 

  • Yanagisawa M, Shibata I, Isogai A (2004) SEC-MALLS analysis of cellulose using LiCl/1,3-dimethyl-2-imidazolidinone as an eluent. Cellulose 11:169–176

    Article  CAS  Google Scholar 

  • Yanagisawa M, Shibata I, Isogai A (2005a) SEC-MALLS analysis of softwood kraft pulp using LiCl/1,3-dimethyl-2-imidazolidinone as an eluent. Cellulose 12:151–158

    Article  CAS  Google Scholar 

  • Yanagisawa M, Isogai A (2005b) SEC-MALS-QELS study on the molecular conformation of cellulose in LiCl/amide solutions. Biomacromolecules 6:1258–1265

    Article  CAS  Google Scholar 

  • Zhang L, Ruan D, Zhou J (2001) Structure and properties of regenerated cellulose films prepared from cotton linters in NaOH/urea aqueous solution. Ind Eng Chem Res 40:5923–5928

    Article  CAS  Google Scholar 

  • Zhang L, Ruan D, Gao S (2002) Dissolution and regeneration of cellulose in NaOH/thiourea aqueous solution. J Polym Sci Polym Phys 40:1521–1529

    Article  CAS  Google Scholar 

Download references

Acknowledgments

This research was supported by a Grant-in-Aid for Young Scientists (Grant number 19-4140) from the Japan Society for the Promotion of Science (JSPS). The authors thank Mr. Takehiko Uematsu of our laboratory, who is a visiting researcher from Kao Corporation, Japan, for his help in determining nitrogen contents of celluloses.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Daisuke Ishii.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Ishii, D., Isogai, A. The residual amide content of cellulose sequentially solvent-exchanged and then vacuum-dried. Cellulose 15, 547–553 (2008). https://doi.org/10.1007/s10570-008-9211-y

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10570-008-9211-y

Keywords

Navigation