Lauric acid-grafted barley (Hordeum vulagare L.) husk for application in biocomposite films: optimization method in synthesis and characterization

  • Aanchal Mittal
  • Sangeeta GargEmail author
  • Shailendra Bajpai
Original Research


Lauric acid-grafted barley (Hordeum vulgare L.) husk (BH) samples were prepared in the presence of redox initiators. The effect of reaction time, reaction temperature, dimethyl sulphoxide content, and concentration of lauric acid on the percentage of graft yield of BH was studied through one-variable-at-a-time approach. A second-order mathematical response model was developed using response surface methodology coupled with central composite design to examine the individual and combined effect of grafting reaction parameters on the percentage of graft yield of BH. The regression model showed a good fit with the experimental data with high correlation coefficient (R2 > 0.97). Grafted BH samples were characterized using Fourier transform infrared spectroscopy, X-ray diffractometry, scanning electron microscopy, and thermal analysis techniques. Crystallinity of BH decreased from 55.5 to 30.22% after grafting with lauric acid due to destruction of crystalline structure of BH during grafting reaction. Grafted BH was more thermally stable as compared to BH. Water contact angle of grafted BH was higher than that of BH, indicating the improved hydrophobicity of BH after grafting. Swelling studies of grafted BH samples in different solvents such as water, ethanol, and dimethyl formaldehyde were performed and compared with BH.


Biopolymers Grafting IR spectra Swelling Thermal properties 

Supplementary material

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Supplementary material 1 (DOCX 12 KB)
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Supplementary material 2 (DOCX 14 KB)
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Supplementary material 3 (DOCX 13 KB)
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Supplementary material 4 (DOCX 1794 KB)


  1. 1.
    Prasad N, Agarwal VK, Sinha S (2016) Banana fiber reinforced low-density polyethylene composites: effect of chemical treatment and compatibilizer addition. Iran Polym J 25:229–241CrossRefGoogle Scholar
  2. 2.
    Baley C (2002) Analysis of the flax fibres tensile behaviour and analysis of the tensile stiffness increase. Compos Pt A Appl Sci Manuf 33:939–948CrossRefGoogle Scholar
  3. 3.
    Li X, Tabil LG, Panigrahi S (2007) Chemical treatments of fiber for use in fiber-reinforced composites: a review. J Polym Environ 15:25–33CrossRefGoogle Scholar
  4. 4.
    Oliveira FR, Zille A, Souto AP (2014) Dyeing mechanism and optimization of polyamide 6, 6 functionalized with double barrier discharge (DBD) plasma in air. Appl Surf Sci 293:177–186CrossRefGoogle Scholar
  5. 5.
    Mouhoubi S, Bourahli MEH, Osmani H, Abdeslam S (2017) Effect of alkali treatment on alfa fibers behavior. J Nat Fibers 14:239–249CrossRefGoogle Scholar
  6. 6.
    Harini K, Ramya K, Sukumar M (2018) Extraction of nano cellulose fibers from the banana peel and bract for production of acetyl and lauroyl cellulose. Carbohydr Polym 201:329–339CrossRefGoogle Scholar
  7. 7.
    Agustin MB, Nakatsubo F, Yano H (2018) Improving the thermal stability of wood-based cellulose by esterification. Carbohydr Polym 192:28–36CrossRefGoogle Scholar
  8. 8.
    Liu Y, Xie J, Wu N, Wang L, Ma Y, Tong J (2019) Influence of silane treatment on the mechanical, tribological and morphological properties of corn stalk fiber reinforced polymer composites. Tribol Int 131:398–405CrossRefGoogle Scholar
  9. 9.
    Ferreira DP, Cruz J, Fangueiro R (2019) In: Koronis G (ed), Silva A (eds) Green composites for automotive applications, 1st edn. Woodhead Publishing, SawstonGoogle Scholar
  10. 10.
    Thakur VK, Thakur MK, Gupta RK (2013) Graft copolymers from cellulose: synthesis, characterization and evaluation. Carbohydr Polym 97:18–25CrossRefGoogle Scholar
  11. 11.
    Kaith BS, Jindal R, Maiti M (2009) Induction of chemical and moisture resistance in Saccharum spontaneum L. fiber through graft copolymerization with methyl methacrylate and study of morphological changes. J Appl Polym Sci 113:1781–1791CrossRefGoogle Scholar
  12. 12.
    Totolin MI, Vasile C, Tibirna CM, Popescu MC (2008) Grafting of Spanish broom (Spartium Junceum) fibers with fatty acids under cold plasma conditions. Cellul Chem Technol 42:317–333Google Scholar
  13. 13.
    Popescu MC, Totolin M, Tibirna CM, Sdrobis A, Stevanovic T, Vasile C (2011) Grafting of softwood kraft pulps fibers with fatty acids under cold plasma conditions. Int J Biol Macromol 48:326–335CrossRefGoogle Scholar
  14. 14.
    Salem IAS, Rozyanty AR, Betar BO, Adam T, Mohammed M, Mohammed AM (2017) Study of the effect of surface treatment of kenaf fibre on mechanical properties of kenaf filled unsaturated polyester composite. J Phys Conf Ser 908, IOP Publishing, p 012002Google Scholar
  15. 15.
    Vanmarcke A, Leroy L, Stoclet G, Duchatel-Crépy L, Lefebvre JM, Joly N, Gaucher V (2017) Influence of fatty chain length and starch composition on structure and properties of fully substituted fatty acid starch esters. Carbohydr Polym 164:249–257CrossRefGoogle Scholar
  16. 16.
    Zhang Z, Jin F, Wu Z, Jin J, Li F, Wang Y, Wang Y, Wang Z, Tang S, Wu C, Wang Y (2017) O-acylation of chitosan nanofibers by short-chain and long-chain fatty acids. Carbohydr Polym 177:203–209CrossRefGoogle Scholar
  17. 17.
    Huang F, Wu X, Yu Y, Lu Y, Chen Q (2017) Acylation of cellulose nanocrystals with acids/trifluoroacetic anhydride and properties of films from esters of CNCs. Carbohydr Polym 155:525–534CrossRefGoogle Scholar
  18. 18.
    Sharma D, Singh J (2017) Synthesis and characterization of fatty acid grafted chitosan polymer and their nanomicelles for nonviral gene delivery applications. Bioconjug Chem 28:2772–2783CrossRefGoogle Scholar
  19. 19.
    Reulier M, Perrin R, Avérous LJ (2016) Biocomposites based on chemically modified cellulose fibers with renewable fatty-acid-based thermoplastic systems: effect of different fiber treatments. Appl Polym Sci 133:43878CrossRefGoogle Scholar
  20. 20.
    Kohli D, Garg S, Jana AK, Maiti M (2017) Synthesis of graft copolymers for green composite films and optimization of reaction parameters using taguchi (L16) orthogonal array. J Indian Chem Eng 59:136–158CrossRefGoogle Scholar
  21. 21.
    Mittal A, Garg S, Kohli D, Maiti M, Jana AK, Bajpai S (2016) Effect of cross linking of PVA/starch and reinforcement of modified barley husk on the properties of composite films. Carbohydr Polym 151:926–938CrossRefGoogle Scholar
  22. 22.
    Carley MK, Kamneva NY, Reminga J (2004) Response surface methodology: CASOS Technical Report CMU-ISRI-04-136. Carnegie Mellon University, PittsburghCrossRefGoogle Scholar
  23. 23.
    Giovanni M (1983) Response surface methodology and product optimization. Food Technol 37:96–105Google Scholar
  24. 24.
    Garg S, Jana AK (2007) Studies on the properties and characteristics of starch-LDPE blend films using cross-linked, glycerol modified, cross-linked and glycerol modified starch. Eur Polym J 43:3976–3987CrossRefGoogle Scholar
  25. 25.
    Singha AS, Thakur VK (2008) Fabrication and study of lignocellulosic Hibiscus sabdariffa fiber reinforced polymer composites. Bioresources 3:1173–1186Google Scholar
  26. 26.
    Catalan J, Diaz C, Garcia-Blanco F (2001) Characterization of binary solvent mixtures of DMSO with water and other cosolvents. J Org Chem 66:5846–5852CrossRefGoogle Scholar
  27. 27.
    Zare A, Morshed M, Bagheri R, Karimi (2013) Effect of various parameters on the chemical grafting of amide monomers to poly (lactic acid). Fiber Polym 14:1783–1793CrossRefGoogle Scholar
  28. 28.
    Bajpai S, Gupta SK, Dey A, Jha MK, Bajpai V, Joshi S, Gupta A (2012) Application of central composite design approach for removal of chromium(VI) from aqueous solution using weakly anionic resin: modeling, optimization, and study of interactive variables. J Hazard Mater 227:436–444CrossRefGoogle Scholar
  29. 29.
    Pushpamalar V, Langford SJ, Ahmad M, Lim YY (2006) Optimization of reaction conditions for preparing carboxymethyl cellulose from sago waste. Carbohydr Polym 64:312–318CrossRefGoogle Scholar
  30. 30.
    Sobhana SSL, Zhang X, Kesavan L, Liias P, Fardim P (2017) Layered double hydroxide interfaced stearic acid-cellulose fibres: a new class of super-hydrophobic hybrid materials. Colloids Surf A 522:416–424CrossRefGoogle Scholar
  31. 31.
    Sdrobiş A, Cazacu G, Totolin M, Vasile C (2011) Alkaline solution swelling of fatty acids-modified softwood kraft pulp fibers under cold plasma conditions. Cellul Chem Technol 45:329–338Google Scholar
  32. 32.
    Arfaoui MA, Dolez PI, Dubé M, David É (2017) Development and characterization of a hydrophobic treatment for jute fibres based on zinc oxide nanoparticles and a fatty acid. Appl Surf Sci 397:19–29CrossRefGoogle Scholar
  33. 33.
    Hassan MS (2015) Removal of reactive dyes from textile wastewater by immobilized chitosan upon grafted Jute fibers with acrylic acid by gamma irradiation. Radiat Phys Chem 115:5–61CrossRefGoogle Scholar
  34. 34.
    Rehman M, Madni A, Ihsan A, Khan WS, Khan MI, Mahmood MA, Ashfaq M, Bajwa SZ, Shakir I (2015) Solid and liquid lipid-based binary solid lipid nanoparticles of diacerein: in vitro evaluation of sustained release, simultaneous loading of gold nanoparticles, and potential thermos responsive behavior. Int J Nanomed 10:2805–2814CrossRefGoogle Scholar
  35. 35.
    Maiti M, Jindal R, Kaith BS, Jana AK (2012) Induction of physico-chemical and thermal resistance on Saccharumspontaneum L by grafting under microwave irradiation. Int J Polym Mater 61:1–16CrossRefGoogle Scholar
  36. 36.
    Mittal V, Sinha S (2015) Effect of chemical treatment on the mechanical and water absorption properties of bagasse fiber-reinforced epoxy composites. J Polym Eng 35:545–550CrossRefGoogle Scholar
  37. 37.
    Mansaray KG, Ghaly AE (1998) Thermal degradation of rice husks in nitrogen atmosphere. Bioresour Technol 65:13–20CrossRefGoogle Scholar
  38. 38.
    Milosavljevic I, Oja V, Suuberg EM (1996) Thermal effects in cellulose pyrolysis: relationship to char formation processes. Ind Eng Chem Res 35:653–662CrossRefGoogle Scholar
  39. 39.
    Liu R, Dong A, Fan X, Yu Y, Yuan J, Wang P, Wang Q, Cavaco-Paulo A (2016) Enzymatic hydrophobic modification of jute fibers via grafting to reinforce composites. Appl Biochem Biotechnol 178:1612–1629CrossRefGoogle Scholar

Copyright information

© Iran Polymer and Petrochemical Institute 2019

Authors and Affiliations

  1. 1.Department of Chemical EngineeringDr B R Ambedkar National Institute of TechnologyJalandharIndia

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