纺织学报 ›› 2014, Vol. 35 ›› Issue (1): 25-0.

• 纤维材料 • 上一篇    下一篇

基于消晶活化预处理法的高取代度羧甲基纤维素制备

张玲玲 周乃锋 张军燚 王海龙   

  1. 浙江理工大学先进纺织材料与制备技术教育部重点实验室
  • 收稿日期:2013-01-14 修回日期:2013-05-28 出版日期:2014-01-15 发布日期:2014-01-15
  • 通讯作者: 张玲玲 E-mail:zllqx718@126.com

Preparation of carboxymethylcellulose with high substitution degree based on lowering crystallinity and activating pretreatment

  • Received:2013-01-14 Revised:2013-05-28 Online:2014-01-15 Published:2014-01-15

摘要: 采用消晶活化预处理的方法,制备出了取代度高达1.72的羧甲基纤维素(CMC)。实验研究了水用量、反应温度、反应时间、消晶活化法预处理NaOH浓度(活化碱浓度)对产品取代度的影响,并通过SEM及XRD对消晶活化反应中NaOH的浓度深入分析,测试了产品的性能。结果表明,反应适宜的用水量为8~10mL,控制反应温度在65~75℃,反应时间3h为宜;纤维素经浓NaOH溶液处理后发生溶胀,且NaOH的浓度越高,纤维素的溶胀越剧烈、结晶度越低,反应活性越高,CMC的取代度越高,最佳的NaOH浓度为500~600 g/L;3%含固量的CMC粘度在30r/min下高达35000 mPa?s;溶液粘度在pH=6~10范围内变化不大,具有良好的耐酸碱和硬水能力;所配溶液存放2周后,粘度变化不大,具有良好的贮存稳定性。

关键词: 活化, 高取代度, 羧甲基纤维素, 黏度, 溶胀

Abstract: The production of carboxymethylcellulose (CMC) with a substitution degree of up to 1.72 was achieved through a new approach of lowering crystallinity and activating pretreatment. The experiments sought to examine the effects of water amount, reaction temperature, reaction time and NaOH concentration on the degree of substitution (DS) of CMC, as well as test the performance of the product through deep analysis of the alkali concentration conducted by SEM and XRD. The results showed that the appropriate amount of water used should be 8~10mL, the proper reaction temperature should be 65~75℃, and the recommended reaction time should be 3h. The experiments also demonstrated that the cellulose would swell after the treatment of high concentration of alkali: higher concentration of NaOH would lead to more swollen cellulose, lower degree of crystallinity, more active reaction as well as higher DS. Thus, the optimal concentration of the alkali should be 500~600 g/L. Moreover, CMC with a solid content of 3% had a viscosity of as high as 35000 mPa?s when the viscosimeter was running at 30r/min. The viscosity of such CMC solution varied little when the pH was 6~10, and the solution appeared to have better stability under different pH conditions and in hard water. After this CMC solution was preserved for two weeks, its viscosity remained almost the same, which indicated its stability during storage.

Key words: activation, high degree of substitution, carboxymethylcellulose, viscosity, swelling

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