三步共聚法制备木质素基酚醛树脂胶粘剂  

Preparation of lignin-based phenolic resin adhesive by three-step copolymerization

作　　者：王凯[1] 刘凤霞[1] 魏炜[1] 王晓娟[1] 刘志军[1] WANG Kai;LIU Feng-xia;WEI Wei;WANG Xiao-juan;LIU Zhi-jun(Research and Design Institute of Fluid and Powder Engineering,Dalian University of Technology,Dalian 116023,China)

机构地区：[1]大连理工大学大学流体与粉体工程研究设计所,辽宁大连116023

出　　处：《热固性树脂》2020年第2期12-17,共6页Thermosetting Resin

基　　金：国家自然科学基金资助项目(21706026);省博士启动基金(201601045)。

摘　　要：利用木质素部分替代苯酚,三步共聚制备了木质素基酚醛树脂胶粘剂(LPF),研究了碱浓度、醛酚比、木质素添加量对LPF的粘度、固含量、游离甲醛含量、游离苯酚含量和胶合强度的影响,并采用FT-IR、13C-NMR和TG对LPF官能团结构和热固化特性进行了表征。结果表明:采用三步共聚法分步加入甲醛溶液,更有利于羟甲基化反应和后续的缩聚反应,并且可操作性好。胶粘剂的最优制备工艺为:碱的质量分数15%(以木质素和苯酚总质量为基准);醛、酚物质的量比2.0∶1;木质素添加量为苯酚物质的量分数30%。制得的LPF胶粘剂的粘度为183.2 mPa·s,固体质量分数45.05%,游离甲酵质量分数0.22%,胶合强度0.85 MPa,均达到GB/T 14732-2006要求。木质素的添加还改善了酚醛树脂的热固化特性。The lignin-based phenolic resin adhesive(LPF)was prepared by three-step copolymerization using partial replacement of phenol with lignin. The effects of alkali concentration,aldehyde-phenol ratio and lignin amount on the viscosity,solid content,free formaldehyde content,free phenol content and bonding strength of the LPF were investigated. The functional group structure and thermal curing characteristics of LPF were characterized by FT-IR,13C-NMR and TG. The results showed that the stepwise addition of the formaldehyde solution by the three-step copolymerization method was more conducive to the methylolation reaction and the subsequent polycondensation reaction,and had good operability. The optimal preparation process of the adhesive was as followed : mass fraction of alkali 15 %(based on the total mass of lignin and phenol),ratio of aldehyde to phenol 2. 0:1 and lignin amount 30 % of the molar of phenol. The viscosity,solid mass fraction,free formaldehyde mass fraction and bonding strength of the prepared LPF adhesive were 183. 2 mPa·s,45. 05 %,0. 22 %,and 0. 85 MPa,respectively and all met the requirements of GB/T 14732 - 2006. The addition of lignin also improved the thermal curing properties of phenolic resins.

关 键 词：木质素 生物质 三步共聚法 酚醛树脂 胶粘剂 

分 类 号：TQ323.1[化学工程—合成树脂塑料工业]