·纤维素季铵盐·

NaOH-尿素体系中纤维素季铵盐

衍生物的均相合成与表征

王水众1张丽1吴池兴1郭延柱1,2,*周景辉1

(1.辽宁省制浆造纸工程高校重点实验室,大连工业大学轻工与化学工程学院, 辽宁大连, 116034；

2.制浆造纸科学与技术省部共建教育部重点实验室,齐鲁工业大学, 山东济南, 250353)

摘要：在NaOH-尿素体系中,以3-氯-2-羟丙基三甲基氯化铵(CHPAC)为醚化剂,纤维素本体为原料,均相合成了纤维素季铵盐衍生物(QC)。以QC中季铵盐的取代度作为考核标准,探讨了QC在合成过程中的影响因素,并优化出最佳合成条件: 反应温度25℃,纤维素浓度3%(以纤维素在NaOH-尿素中的质量分数计),醚化剂用量15∶1(以CHPAC与葡萄糖糖苷元的摩尔比计),反应时间12 h。利用傅里叶红外光谱仪(FT-IR)、氢核磁共振光谱(`1H-NMR)、热重分析仪(TGA)和X射线衍射分析仪(XRD)对QC的化学结构及物理性能进行表征。

关键词：纤维素；NaOH-尿素体系；纤维素季铵盐；均相合成

作者简介：王水众先生,本科在读；主要从事制浆造纸清洁化生产及生物质开发利用研究。

中图分类号：TS743`+.1

文献标识码：A

文章编号：0254- 508X(2015)06- 0035- 06

收稿日期：2015- 02- 06(修改稿)

基金项目：辽宁省大学生创新创业计划项目(201410152028)；大连工业大学青年基金(28000123)；制浆造纸科学与技术教育部重点实验室开放基金(08031338)。

Abstract：Quaternized cellulose derivatives (QC) was homogeneously synthesized by using cellulose as raw material and 3-chloro-2-hydroxypropyltrimethylammonium chloride as etherization agent in NaOH-urea green aqueous solutions. Using DS values of quaternary ammonium group in QC chemical structure as evaluation criterion, the synthetic conditions for QC derivatives were optimized, which were listed as the followings: reaction temperature 25℃, the concentration of cellulose in NaOH-urea solution 3%, molar ratio for etherification agent to glycosidic cellulose 15∶1, reaction time 12 h. The chemical structure of the QCs was characterized by FT-IR and `1H-NMR techniques. The results of TGA and XRD analysis showed that the crystalline structure of cellulose was destroyed in etherification process, and the thermal stability of QC was lower than that of cellulose.

*通信作者：郭延柱女士,E-mail：guoyz@dlpu.edu.cn。

Homogeneous Synthesis and Characterization of Quaternized Cellulose

Derivative in Sodium Hydroxide-urea Aqueous Solution

WANG Shui-zhong1ZHANG Li1WU Chi-xing1GUO Yan-zhu1,2,*ZHOU Jing-hui1

(1.LiaoningProvinceKeyLabofPulpandPaperEngineering,DalianPolytechnicUniversity,Dalian,LiaoningProvince,116034;

2.KeyLabofPulpandPaperScience&TechnologyofMinistryofEducation,QiluUniversityofTechnology,Ji’nan,ShandongProvince, 250353)

(*E-mail: guoyz@dlpu.edu.cn)

Key words：cellulose; sodium hydroxide-urea solution; quaternized cellulose; homogeneous synthesis

纤维素是世界上最为丰富的天然可再生生物质资源,具有价格低、易得、生物可降解等特点,备受关注[1-2]。然而,纤维素由于分子内和分子间的强氢键作用以及致密的结晶结构,在普通溶剂如水、乙醇中很难溶解[3]。……