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A two-stage C5 selective hydrolysis on soybean hulls for xylose separation and value-added cellulose applications

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Abstract

Soy hulls from dehulling of soybeans are typically disposed of with soymeal or cattle feed. The hulls contain about 38.8% cellulose and 23.8% hemicelluloses and less than 4% lignin. The low lignin content, large volume availability, and being a “captive” feedstock make soy hulls an affordable raw material to produce C5 sugars such as arabinose and xylose from hemicelluloses. In this work, dilute acid hydrolysis of soy hulls using acid concentrations less than 1% (w/w) in solution and at different temperatures (125 °C, 140 °C, and 155 °C) was investigated to generate the kinetics data for sugar and degradation product release and study selectivity towards arabinose and xylose. The primary goal was to produce a hydrolysate rich in C5 sugars with minimal glucose and degradation products. Lower acid concentration (0.4% w/w) at 140 °C and lesser reaction time favoured selectivity towards arabinose release, while xylose release needed higher acid (0.6 to 0.8%) and longer time at the same temperature. From the kinetics data, a two-stage process was devised to achieve two separate hydrolysate streams rich in arabinose (5.00 ± 0.15 g dm−3, 78.1% of total C5 sugars) and xylose (17.20 ± 0.71 g dm−3, 87.7% of total C5 sugars). The xylose-rich stream was used to isolate xylose (powder form) under ambient process conditions using our patented process. The residual soy hulls, post the two-stage hydrolysis, showed high crystallinity with morphology analogous to microcrystalline cellulose, thus making them an effective starting material for high-value cellulose applications such as microcrystalline cellulose and polymer composites.

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References

  1. Mielenz JR, Bardsley JS, Wyman CE (2009) Fermentation of soybean hulls to ethanol while preserving protein value. Bioresour Technol 100:3532–3539. https://doi.org/10.1016/j.biortech.2009.02.044

    Article  Google Scholar 

  2. Schirmer-Michel ÂC, Flôres SH, Hertz PF, Matos GS, Ayub MAZ (2008) Production of ethanol from soybean hull hydrolysate by osmotolerant Candida guilliermondii NRRL Y-2075. Bioresour Technol 99:2898–2904. https://doi.org/10.1016/j.biortech.2007.06.042

    Article  Google Scholar 

  3. Fonseca DA, Lupitskyy R, Timmons D, Gupta M, Satyavolu J (2014) Towards integrated biorefinery from dried distillers grains: selective extraction of pentoses using dilute acid hydrolysis. Biomass Bioenergy 71:178–186. https://doi.org/10.1016/j.biombioe.2014.10.008

    Article  Google Scholar 

  4. Kalapathy U, Proctor A (2001) Effect of acid extraction and alcohol precipitation conditions on the yield and purity of soy hull pectin. Food Chem 73:393–396. https://doi.org/10.1016/S0308-8146(00)00307-1

    Article  Google Scholar 

  5. Zhang T, Yu S, Meng H, Zhu S, Guo X (2015) Purifying sugar beet pectins from non-pectic components by means of metal precipitation. Food Hydrocoll 51:69–75. https://doi.org/10.1016/j.foodhyd.2015.05.009

    Article  Google Scholar 

  6. Müller-Maatsch J, Bencivenni M, Caligiani A, Tedeschi T, Bruggeman G, Bosch M, Petrusan J, Van Droogenbroeck B, Elst K, Sforza S (2016) Pectin content and composition from different food waste streams in memory of Anna Surribas, scientist and friend. Food Chem 201:37–45. https://doi.org/10.1016/j.foodchem.2016.01.012

    Article  Google Scholar 

  7. Brinchi L, Cotana F, Fortunati E, Kenny JM (2013) Production of nanocrystalline cellulose from lignocellulosic biomass: technology and applications. Carbohydr Polym 94:154–169. https://doi.org/10.1016/j.carbpol.2013.01.033

    Article  Google Scholar 

  8. Alemdar A, Sain M (2008) Isolation and characterization of nanofibers from agricultural residues - wheat straw and soy hulls. Bioresour Technol 99:1664–1671. https://doi.org/10.1016/j.biortech.2007.04.029

    Article  Google Scholar 

  9. Wei L, Agarwal UP, Matuana L, Sabo RC, Stark NM (2018) Performance of high lignin content cellulose nanocrystals in poly(lactic acid). Polymer 135:305–313. https://doi.org/10.1016/j.polymer.2017.12.039

    Article  Google Scholar 

  10. https://www.nass.usda.gov/Newsroom/2019/02-08-2019.php accessed June 4, 2019, (n.d.)

  11. Boyles S (2017) Effects of soy hulls in finishing diets with DDGs on performance and carcass, 2. https://u.osu.edu/beef/2017/02/01/effects-of-soy-hulls-in-finishing-diets-with-ddgs-on-performance-and-carcass/

  12. Liu H-M, Li H-Y (2017) Application and conversion of soybean hulls, in: Soybean - basis yield, biomass product, pp. 110–132. https://doi.org/10.5772/66744

  13. Flauzino Neto WP, Silvério HA, Dantas NO, Pasquini D (2013) Extraction and characterization of cellulose nanocrystals from agro-industrial residue - soy hulls. Ind Crop Prod 42:480–488. https://doi.org/10.1016/j.indcrop.2012.06.041

    Article  Google Scholar 

  14. Corredor DY, Sun XS, Salazar JM, Hohn KL, Wang D (2008) Enzymatic hydrolysis of soybean hulls using dilute acid and modified steam-explosion pretreatments. J Biobased Mater Bioenergy 2:43–50. https://doi.org/10.1166/jbmb.2008.201

    Article  Google Scholar 

  15. Cassales A, de Souza-Cruz PB, Rech R, Záchia Ayub MA (2011) Optimization of soybean hull acid hydrolysis and its characterization as a potential substrate for bioprocessing. Biomass Bioenergy 35:4675–4683. https://doi.org/10.1016/j.biombioe.2011.09.021

    Article  Google Scholar 

  16. Davidson D (2019) New uses for soy hulls. ILSOYADVISOR POST. https://www.ilsoyadvisor.com/on-farm/ilsoyadvisor/new-uses-soy-hulls

  17. Merci A, Urbano A, Grossmann MVE, Tischer CA, Mali S (2015) Properties of microcrystalline cellulose extracted from soybean hulls by reactive extrusion. Food Res Int 73:38–43. https://doi.org/10.1016/j.foodres.2015.03.020

    Article  Google Scholar 

  18. Gnanasambandam R, Proctor A (1999) Preparation of soy hull pectin. Food Chem 65:461–467. https://doi.org/10.1016/S0308-8146(98)00197-6

    Article  Google Scholar 

  19. Kim HW, Lee YJ, Kim YHB (2015) Efficacy of pectin and insoluble fiber extracted from soy hulls as a functional non-meat ingredient. LWT Food Sci Technol 64:1071–1077. https://doi.org/10.1016/j.lwt.2015.07.030

    Article  Google Scholar 

  20. Rojas MJ, Siqueira PF, Miranda LC, Tardioli PW, Giordano RLC (2014) Sequential proteolysis and cellulolytic hydrolysis of soybean hulls for oligopeptides and ethanol production. Ind Crop Prod 61:202–210. https://doi.org/10.1016/j.indcrop.2014.07.002

    Article  Google Scholar 

  21. Porfiri MC, Wagner JR (2018) Extraction and characterization of soy hull polysaccharide-protein fractions. Analysis of aggregation and surface rheology. Food Hydrocoll 79:40–47. https://doi.org/10.1016/j.foodhyd.2017.11.050

    Article  Google Scholar 

  22. R. Gnanasambandam, M. Mathias, A. Proctor, Structure and performance of soy hull carbon adsorbents as affected by pyrolysis temperature, JAOCS, J Am Oil Chem Soc 75 (1998) 615–621. https://doi.org/10.1007/s11746-998-0074-z

  23. Hong Y, Proctor A, Shultz J (2000) Acid-treated soy hull carbon structure, 785–790

  24. Marshall WE, Wartelle LH (2004) An anion exchange resin from soybean hulls. J Chem Technol Biotechnol 79:1286–1292. https://doi.org/10.1002/jctb.1126

    Article  Google Scholar 

  25. Gori SS, Raju MVR, Fonseca DA, Satyavolu J, Burns CT, Nantz MH (2015) Isolation of C5-sugars from the hemicellulose-rich hydrolyzate of distillers dried grains. ACS Sustain Chem Eng 3:2452–2457. https://doi.org/10.1021/acssuschemeng.5b00490

    Article  Google Scholar 

  26. Satyavolu J, Gori SS, Nantz MH, Raju MVR, Burns CT (2019) Process for isolating C5 sugars from biomass hydrolyzate, US Patent # 10,407,453. https://patents.google.com/patent/US10407453B2/en

  27. Kim ES, Herde ZD, Thilakaratne R, Burns CT, Satyavolu J (2018) Evaluation and utilization of dicarboxylic acids (DCA) as an alternative to strong mineral acids for selective extraction of C5-sugars in an integrated biorefinery. Adv Ind Biotechnol 1:1–8. https://doi.org/10.24966/aib-5665/100001

    Article  Google Scholar 

  28. Kauss H, Hassid WZ (1967) Biosynthesis of the glucuronic acid unit of hemicellulose B from UDP-glucuronic acid. J Biol Chem 242:1680–1684. https://doi.org/10.1016/0304-4165(67)90161-4

    Article  Google Scholar 

  29. Wang F-Y, Li H-Y, Liu H-M, Liu Y-L (2015) Fractional isolation and structural characterization of hemicelluloses from soybean hull. BioResources. 10:5256–5266. https://doi.org/10.15376/biores.10.3.5256-5266

    Article  Google Scholar 

  30. Izydorczyk MS (2009) 23-Arabinoxylans, in: G.O. Phillips, P.A. Williams (Eds.), Woodhead Publ. Ser. Food Sci. Technol. Nutr. Handb. Hydrocoll., 2nd ed., Woodhead Publishing, pp. 653–692. https://doi.org/10.1533/9781845695873.653

  31. Dussan K, Girisuta B, Lopes M, Leahy JJ, Hayes MHB (2015) Conversion of hemicellulose sugars catalyzed by formic acid: kinetics of the dehydration of D-xylose, L-arabinose, and D-glucose. ChemSusChem. 8:1411–1428. https://doi.org/10.1002/cssc.201403328

    Article  Google Scholar 

  32. Rodrigues J, Faix O, Pereira H (1998) Determination of lignin content of Eucalyptus globulus wood using FTIR spectroscopy. Holzforschung. 52:46–50. https://doi.org/10.1515/hfsg.1998.52.1.46

    Article  Google Scholar 

  33. Mwaikambo LY, Ansell MP (2002) Chemical modification of hemp, sisal, jute, and kapok fibers by alkalization. J Appl Polym Sci 84:2222–2234. https://doi.org/10.1002/app.10460

    Article  Google Scholar 

  34. Derkacheva O, Sukhov D (2008) Investigation of lignins by FTIR spectroscopy. Macromol Symp 265:61–68. https://doi.org/10.1002/masy.200850507

    Article  Google Scholar 

  35. Xu F, Yu J, Tesso T, Dowell F, Wang D (2013) Qualitative and quantitative analysis of lignocellulosic biomass using infrared techniques: a mini-review. Appl Energy 104:801–809. https://doi.org/10.1016/j.apenergy.2012.12.019

    Article  Google Scholar 

  36. Sgriccia N, Hawley MC, Misra M (2008) Characterization of natural fiber surfaces and natural fiber composites. Compos A: Appl Sci Manuf 39:1632–1637. https://doi.org/10.1016/j.compositesa.2008.07.007

    Article  Google Scholar 

  37. Chen YW, Tan TH, Lee HV, Hamid SBA (2017) Easy fabrication of highly thermal-stable cellulose nanocrystals using Cr(NO3)3 catalytic hydrolysis system: a feasibility study from macroto nano-dimensions. Materials (Basel) 10:42. https://doi.org/10.3390/ma10010042

    Article  Google Scholar 

  38. Balla VK, Kate KH, Satyavolu J, Singh P, Tadimeti JGD (2019) Additive manufacturing of natural fiber reinforced polymer composites : processing and prospects. Compos Part B 174:106956. https://doi.org/10.1016/j.compositesb.2019.106956

    Article  Google Scholar 

  39. Park S, Baker JO, Himmel ME, Parilla PA, Johnson DK (2010) Cellulose crystallinity index: measurement techniques and their impact on interpreting cellulase performance. Biotechnol Biofuels 3:1–10

    Article  Google Scholar 

  40. Balla VK, Tadimeti JGD, Satyavolu J, Kate KH (2020) First report on fabrication and characterization of soybean hull fiber: polymer composite filaments for fused filament fabrication. Prog Addit Manuf. https://doi.org/10.1007/s40964-020-00138-2

  41. Balla VK, Tadimeti JGD, Kate KH, Satyavolu J, (2020) 3D printing of modified soybean hull fiber/polymer composites. Mater Chem Phys 254:123452. https://doi.org/10.1016/j.matchemphys.2020.123452

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Acknowledgments

The authors thank Owensboro Grain Company, Owensboro, KY, USA, for their material support during this project.

Funding

The authors received financial support from the United Soybean Board, MO, USA (Contract No. USB#1940-362-0703-E).

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Authors and Affiliations

  1. Conn Center for Renewable Energy Research, University of Louisville, Louisville, KY, 40208, USA

    Jogi Ganesh Dattatreya Tadimeti & Jagannadh Satyavolu

  2. BioProducts, LLC, Louisville, KY, USA

    Rajeeva Thilakaratne

  3. Bioceramics and Coating Division, CSIR-Central Glass & Ceramic Research Institute, 196 Raja S.C. Mullick Road, Kolkata, West Bengal, 700 032, India

    Vamsi Krishna Balla

  4. Materials Innovation Guild, Department of Mechanical Engineering, University of Louisville, Louisville, KY, 40208, USA

    Kunal H. Kate

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  1. Jogi Ganesh Dattatreya Tadimeti
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Correspondence to Jagannadh Satyavolu.

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Tadimeti, J.G.D., Thilakaratne, R., Balla, V.K. et al. A two-stage C5 selective hydrolysis on soybean hulls for xylose separation and value-added cellulose applications. Biomass Conv. Bioref. 12, 3289–3301 (2022). https://doi.org/10.1007/s13399-020-00860-5

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  • DOI: https://doi.org/10.1007/s13399-020-00860-5

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