微波辐射法竹浆纤维素的中性TEMPO氧化及表征

doi:10.3969/j.issn.0253-2417.2015.01.016

林产化学与工业 ›› 2015, Vol. 35 ›› Issue (1): 101-106.doi: 10.3969/j.issn.0253-2417.2015.01.016

微波辐射法竹浆纤维素的中性TEMPO氧化及表征

项秀东, 万小芳, 李友明, 武书彬

华南理工大学制浆造纸工程国家重点实验室, 广东广州 510640

收稿日期:2014-03-17 出版日期:2015-02-25 发布日期:2015-03-05
通讯作者: 李友明,男,教授,博士生导师,从事生物质资源转化利用、制浆清洁生产与污染控制等方面的研究;E-mail:ymli3@scut.edu.cn。 E-mail:ymli3@scut.edu.cn
作者简介:项秀东(1988-),男,江西上饶人,硕士生,主要从事生物质资源化学与生物质转化利用研究

Neutral TEMPO Oxidation of Bamboo Cellulose Fiber under Microwave Radiation and Its Characterization

XIANG Xiu-dong, WAN Xiao-fang, LI You-ming, WU Shu-bin

State Key Laboratory of Pulp and Paper Engineering, South China University of Technology, Guangzhou 510640, China

Received:2014-03-17 Online:2015-02-25 Published:2015-03-05

摘要/Abstract

摘要： 采用微波辐射法和中性2,2,6,6-四甲基哌啶-1-氧化物(TEMPO)自由基氧化工艺来预处理竹浆纤维素,之后用超声波机械处理制备微纤化纤维素。实验结果表明,在60 ℃下,TEMPO用量为0.15 mmol/g(以绝干浆计,下同),NaClO₂用量为10 mmol/g,NaClO用量为1 mmol/g,微波氧化2 h,其羧基含量最高到达0.729 mmol/g,氧化效果最佳,超声波处理后微纤化纤维素得率高达85.7%。FT-IR分析表明纤维素氧化后引入羧基官能团;XRD结果揭示纤维素氧化反应只发生在纤维素的无定型区或结晶区表面;纤维素氧化前后的聚合度(D_p)结果表明相对于碱性氧化,微波辐射和中性TEMPO氧化对纤维的降解程度低,从而有效地保持了纤维素原本的长度。

关键词: 微波辐射, 中性TEMPO氧化, 羧基含量, 微纤化纤维素

Abstract: The bamboo fibers were pretreated by microwave radiation and neutral 2,2,6,6-tetramethylpiperidinooxy(TEMPO) oxidation, and then the microfibrillated cellulose was prepared by ultrasonic mechanical treatment. Experimental results showed that the maximal carboxyl content was 0.729 mmol/g pulp after bamboo fibers were pretreated by 0.15 mmol/g TEMPO, 10 mmol/g NaClO₂ and 1 mmol/g NaClO at 60 ℃ for 2 h. And the yield of microfibrillated cellulose was 85.7% after the ultrasonic mechanical treatment. The FT-IR spectra indicated that carboxyl groups were introduced onto cellulose. The XRD analysis indicated that the oxidation reaction was conducted only in the amorphous region or on the crystalline surface area of the cellulose. Meanwhile, the polymerization degree results of the cellulose showed that only minor cellulose fibers were degraded when they were pretreated by microwave radiation and neutral TEMPO oxidation. Therefore, the origin length of fiber was constant through this whole pretreatment process.

Key words: microwave radiation, neutral TEMPO oxidation, carboxyl content, microfibrillated cellulose

中图分类号:

TQ35
TS721

项秀东, 万小芳, 李友明, 武书彬. 微波辐射法竹浆纤维素的中性TEMPO氧化及表征[J]. 林产化学与工业, 2015, 35(1): 101-106.

XIANG Xiu-dong, WAN Xiao-fang, LI You-ming, WU Shu-bin. Neutral TEMPO Oxidation of Bamboo Cellulose Fiber under Microwave Radiation and Its Characterization[J]. Chemistry and Industry of Forest Products, 2015, 35(1): 101-106.

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微波辐射法竹浆纤维素的中性TEMPO氧化及表征

Neutral TEMPO Oxidation of Bamboo Cellulose Fiber under Microwave Radiation and Its Characterization

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