催化剂预加载芬顿氧化法微纤化纤维素的制备研究
Catalyst Preloaded Fenton Oxidation of Microfibrillated Cellulose Preparation
收稿日期:2019-09-05  修订日期:2019-09-20
DOI:
关键词:  催化剂预加载  芬顿氧化  氧化效率  微纤化纤维素
Key Words:Catalyst preloaded  Fenton oxidation  Oxidation efficiency  Microfibrillated Cellulos
基金项目:国家重点基础研究发展计划(973计划)
作者单位邮编
段林娟 天津科技大学 300457
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摘要:以溶解浆为原料,采用催化剂预加载芬顿氧化协同高压均质法制备微纤化纤维素(MFC)。探讨了双氧水用量、催化剂亚铁用量、反应温度和反应时间对氧化效率的影响,并对氧化纤维的微观形貌、化学结构变化及MFC微观结构、结晶度及热稳定性进行了表征。结果表明,催化剂预加载芬顿法可显著提高氧化纤维中的羧基和醛基含量,降低聚合度和Zeta电位,增大纤维之间的静电斥力,利于后续的均质处理。在浆浓25%,溶解浆10 g,双氧水用量150 kg/t,七水硫酸亚铁用量1.5 g,pH值3,反应温度45℃,反应时间120 min条件下,氧化纤维中羧基和醛基含量分别为85.43 μmol/g和57.32 μmol/g,聚合度为154,Zeta电位为-34.72 mV。傅里叶变换红外光谱(FTIR)表明芬顿氧化纤维制备成功,扫描电子显微镜(SEM)、X射线衍射(XRD)、热重分析(TG)表明MFC尺寸分布比较均匀,直径在200 nm左右,结晶度为81.35%,热稳定性有所降低。
Abstract:Microfibrillated cellulose (MFC) was successfully prepared by catalyst preloaded Fenton oxidation with the followed homogenization. The effects of hydrogen peroxide content, catalyst ferrous content, reaction temperature and reaction time on Fenton oxidation efficiency were discussed. The microstructure, chemical structure of the oxidized fibers and the morphology, crystal properties, thermal stable properties of MFC were characterized. The results showed that the catalyst preloaded Fenton oxidation method could significantly increase the content of carboxyl and aldehyde groups in oxidized fibers, reduce the degree of polymerization and Zeta potential, which was beneficial to increase the electrostatic repulsion between the fibers and to facilitate the subsequent homogenization treatment. Under the reaction conditions of 25% pulp consistency, 10 g dissolved pulp, 150 kg/t H2O2, 1.5 g FeSO4, pH 3, 45℃and 120 min, the contents of carboxyl group and aldehyde group in the oxidized fibers were 85.43 μmol/g and 57.32 μmol/g respectively, the degree of polymerization was 154, and the Zeta potential was -34.72 mV. The Fourier transform infrared spectroscopy (FTIR) indicated that the successful preparation of Fenton oxidized fibers, and the scanning electron microscope (SEM)、X-ray diffractometer (XRD) and thermogravimetric analyzer (TG) results indicated that the obtained MFC were uniform in size and the diameter was about 200 nm, the crystallinity was 81.35%, and the thermal stability was reduced.
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