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Synthesis of a novel lignin-based epoxy resin curing agent and study of cure kinetics, thermal, and mechanical properties

机译:基于木质素的环氧树脂固化剂的合成及固化动力学研究,热和力学性能研究

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In this contribution, first of all, the methoxy groups of organic solvent lignin (OSL) was converted to phenolic hydroxyl groups through demethylation reaction for the purpose of fabricating demethylated organic solvent lignin (DOSL). In addition, the resulting DOSL was utilized as a renewable material to synthesize a novel esterified lignin (EDOSL) by reacting with isobutyryl chloride for curing of epoxy resin. Finally, commercial liquid diglycidyl ether of bisphenol A was cured by EDOSL in the presence of 4-dimethylaminopyridine (DMAP) used as a catalyst based on dual-curing mechanism. Dual curing is a processing methodology based upon the alliance of two diverse and compatible polymerization reactions occurring sequentially or simultaneously. According to the FTIR spectra and H-1-NMR analyses, the demethylation of OSL, esterification of DOSL, and the curing reaction of epoxy resin with EDOSL were successfully conducted. The value of the phenolic hydrogen in the DOSL was approximately 4.89 mmol/g, which increased by 12.64% after demethylation. The thermal and mechanical performances of these cured epoxy samples were measured by DSC, DMA, TGA, and tensile testing. The epoxy system cured by 10%wt esterified lignin with 1%wt DMAP possessed the tensile strength of 71.54 +/- 7.50 MPa and the initial degradation temperature (T-5%) of 370 degrees C, which can compete fairly with commercial aromatic curing agents or other lignin-based agents studied currently for the curing of epoxy systems.
机译:本文首先通过脱甲基反应将有机溶剂木质素(OSL)的甲氧基转化为酚羟基,制备脱甲基有机溶剂木质素(DOSL)。此外,将所得DOSL用作可再生材料,通过与异丁酰氯反应合成新型酯化木质素(EDOSL),用于环氧树脂固化。最后,基于双固化机理,以4-二甲氨基吡啶(DMAP)为催化剂,采用EDOSL固化双酚A的市售液体二缩水甘油醚。双固化是一种加工方法,基于连续或同时发生的两种不同且相容的聚合反应的联盟。根据FTIR光谱和H-1-NMR分析,成功地进行了OSL的脱甲基、DOSL的酯化以及环氧树脂与EDOSL的固化反应。DOSL中的酚氢值约为4.89mmol/g,脱甲基后增加了12.64%。通过DSC、DMA、TGA和拉伸试验测定了这些固化环氧树脂样品的热性能和力学性能。用10%wt酯化木质素和1%wt DMAP固化的环氧树脂体系具有71.54+/-7.50MPa的拉伸强度和370℃的初始降解温度(T-5%),可以与商用芳香固化剂或目前研究的其他木质素基固化剂进行公平竞争。

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