Journal of Korea Technical Association of The Pulp and Paper Industry (펄프종이기술)

Korea Technical Association of the Pulp and Paper Industry (한국펄프종이공학회)
권호 표지
DOI QR코드

DOI QR Code

Analysis of secondary reactions in concentrated sulfuric acid hydrolysis of hollocellulose by 1H-NMR spectroscopy

1H-NMR 분광분석을 통한 진한 산 가수분해 반응 2차 반응 조건 분석

  • Lee, Jai-Sung (Department of Wood and Paper Science, Chungbuk National University) ;
  • Shin, Soo-Jeong (Department of Wood and Paper Science, Chungbuk National University)
  • 이재성 (충북대학교 목재종이과학과) ;
  • 신수정 (충북대학교 목재종이과학과)
  • Received : 2014.05.20
  • Accepted : 2014.06.11
  • Published : 2014.06.30
Download PDF
⟨ Previous Next ⟩

Abstract

Kinetics of holocellulose hydrolysis in concentrated sulfuric acid was analyzed using $^1H$-NMR spectroscopy with different reaction time, temperature and acid concentration in secondary hydrolysis. In this work, reaction condition of secondary hydrolysis was similar to concentrated sulfuric acid process with electrodialysis or simulated moving bed chromatography process for sulfuric acid recycling. By $^1H$-NMR spectroscopy, acid hydrolyzates from higher secondary acid hydrolysis (25-35% acid concentration) was successfully analyzed without any difficulties in neutralization or adsorption of acid hydrolyzate to solid salt. Higher acid concentration, higher temperature and longer reaction time led to more cellulose for glucose conversion but accompanied with glucose to galactose isomerization, glucose to unknown compounds and degradation of glucose to organic acid via furans.

Keywords

References

  1. Kim, H.Y., Lee, E.S., Kim, W., Suh, D.J.,and Ahn, B.S., Material and heat balances of bioethanol production process by concentrated acid saccharification process from lignocellulosic biomass, Clean Technol., 17(2):156-165 (2011).
  2. Batsy, D.R., Solvason, C.C., Sammons, N.E., Chambost, V., Bilhartz, D.L., Eden, M.R., El-halwagi, M.M., and Stuart, P.R., Product portfolio selection and process design for the forest biorefinery, In Integrated biorefineries : design, analysis, and optimization, Stuart, P.R., El-Halwagi, M.M. (eds.), CRC press, Boca Raton, Florida, pp.837-845 (2013).
  3. Xie, Y., Phelps, D., Lee, C.H., Sedlak, M., Ho, N., and Wang, N.H.L., Comparison of two adsorbents for sugar recovery from biomass hydrolyzate, Ind. Eng. Chem. Res., 44:6816-6823 (2005). https://doi.org/10.1021/ie049079x
  4. Shin, S.J., Kim, Y.H., Cho, D.H., Sung, Y.J., Kim, B.R., and Cho, N.S., Kinetics study of 2nd hydrolysis in concentrated sulfuric acid hydrolysis process by 1H-NMR spectroscopy, Proceeding of spring conference of the Korea TAPPI 2011, 93-99
  5. Jupke, A., Epping, A., and Schnidt-Traub, Optimal design of batch and simulated moving bed chromatographic separation processes, J. Chromatogr. A, 944(1-2):93-117 (2002). https://doi.org/10.1016/S0021-9673(01)01311-5
  6. Shin, S.J., Park, J.M., Cho, D.H., Kim, Y.H., and Cho, N.S., Acid hydrolysis Characteristics of yellow poplar for high concentration of monosaccharides production, Mokchae Konghak 37(6):578-584 (2009).
  7. Shin, S.J., and Cho, N.S., Conversion factors for carbohydrate analysis by hydrolysis and 1H-NMR spectroscopy, Cellulose 15(2):255-260 (2008). https://doi.org/10.1007/s10570-007-9156-6
  8. Sim, J. and Shin, S.J., Quantitative analysis of 5-HMF produced from fructose, J. Korea TAPPI 45(1):27-34 (2013). https://doi.org/10.7584/ktappi.2013.45.1.027
  9. Yoon, S.Y., Han, S.H., and Shin, S.J., The effect of hemicelluloses and lignin on acid hydrolysis of cellulose, Energy, http://dx.doi.org/10.1016/j.energy.2014.01.104 (2014).
  10. Cho, D.H., Kim, Y.H., Kim, B.R., Park, J.M., Sung, Y.J., and Shin, S.-J., Kinetic study of xylan hydrolysis and decomposition in concentrated sulfuric acid hydrolysis process by 1H-NMR spectroscopy, J. Korea TAPPI, 43(3):52-58 (2011).
  11. Ryu, J.H., and Youn, H.J., Effect of sulfuric acid hydrolysis condition on yield, particle size and surface charge of cellulose nanocrystals, J. Korea TAPPI, 45(4):67-75 (2011).
  12. Roman-Leschkov, Y., Moliner, M., Labinger, J.A., and Davis, M.E., Mechanism of glucose isomerization using a solid lewis acid catalyst in water, Angew. Chem. Int. Edit. 49(47) 8954-8957 (2010). https://doi.org/10.1002/anie.201004689