NCC preparation using sulfuric acid hydrolysis from cellulase pretreated fibers was optimized in order to obtain the highest possible yield with 62% and 65% wt. sulfuric acid throughout two statistical plans. At optimal conditions (10U/g odp cellulase, 25 min hydrolysis, 47 ºC and 62 % wt. H2SO4) high yields were obtained (=80%) including an increase produced by enzyme of ~9 %. Optimal conditions produced nanosized particles of around ~200 nm with a reduced surface charge and sulfur content. The performed optimization allowed reducing the hydrolysis time in a 44%, and also increasing yield in more than 10% compared to results exposed in previous works. The effects of cellulase pretreatment were noticeable even under aggressive hydrolysis conditions, emphasizing its possibilities. Zeta potential and polydispersity indexes indicated that all studied conditions leaded to good quality final products, with values among -50 mV and 0.2, respectively. TEM analysis confirmed the presence of NCC and suggested morphological differences between samples. Finally FTIR analysis provided evidence that cellulase treatment increased crystallinity of both cellulose fibers and NCC, and also increased accessibility to fibers, supporting data obtained from NCC
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机译:优化使用纤维素酶预处理纤维的硫酸水解法制备NCC的方法,以获得62%和65%wt的最高收率。整个两个统计计划中的硫酸。在最佳条件下(10U / g odp纤维素酶,25分钟水解,47ºC和62%wt。H2SO4),可获得高产率(= 80%),其中包括酶产生的〜9%的增加。最佳条件可产生约200 nm左右的纳米级颗粒,且表面电荷和硫含量降低。进行的优化使水解时间减少了44%,与以前的工作相比,收率提高了10%以上。纤维素酶预处理的效果即使在剧烈的水解条件下也很明显,强调了其可能性。 Zeta电位和多分散指数表明,所有研究条件均导致最终产品的质量良好,其值分别在-50 mV和0.2之间。 TEM分析证实了NCC的存在,并暗示了样品之间的形态差异。最后,FTIR分析提供了纤维素酶处理增加纤维素纤维和NCC的结晶度,以及增加纤维可及性的证据,支持了从NCC获得的数据。
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