核桃壳液化物合成高邻位热塑性酚醛树脂  

Synthesis of High-Ortho Novolak Resins from Liquefied Products of Walnut Shell

作　　者：卢宇晗 黄元波 杨晓琴 徐开蒙 刘灿 张全 王继大 郑志锋 LU Yuhan;HUANG Yuanbo;YANG Xiaoqin;XU Kaimeng;LIU Can;ZHANG Quan;WANG Jida;ZHENG Zhifeng(Yunnan Provincial International Joint Research Center for Bioenergy,Yunnan Provincial Engineering Laboratory for Highly- Efficient Utilization of Biomass,Yunnan Provincial University Key Laboratory for Biomass Chemical Refinery&Synthesis,School of Materials Science&Engineering,Southwest Forestry University,Kunming 650224)

机构地区：[1]云南省生物质能源国际联合研究中心,云南省生物质高效利用工程实验室,云南省高校生物质化学炼制与合成重点实验室,西南林业大学材料科学与工程学院,昆明650224

出　　处：《材料导报》2018年第18期3244-3248,共5页Materials Reports

基　　金：国家重点研发计划课题(2017YFD0601003)；云南省应用基础研究重点项目(2014FA034)。

摘　　要：以核桃壳液化物为原料、氢氧化锌为催化剂合成核桃壳生物基高邻位热塑性酚醛树脂。采用核磁共振波谱分析(NMR)、傅里叶红外光谱分析(FT-IR)、凝胶渗透色谱分析(GPC)、热重分析(TGA)和有机元素分析(OEA)对其结构和热性能进行了表征分析。结果表明:两步甲醛法可合成核桃壳生物基高邻位热塑性酚醛树脂,其长链结构由亚甲基邻-邻连接(o-o)酚环、亚甲基邻-对连接(o-p)酚环和亚甲基对-对连接(p-p)酚环组成,其中o-o和o-p酚环为主要组成结构,且邻对位结构比值(o-o/p-p)为1.22;其数均分子量为4 499g/mol,分子量分布指数为1.417;热失重过程包括两个阶段,最大失重温度为375℃、失重率为50%;由有机元素分析可推测其理论分子式为C_6H_6O_(1.2)。Walnut shell bio-based high-ortho novolak resins were synthesized by using liquefied products of walnut shell as raw material and zinc hydroxide as catalyst,their structure and thermal property were characterized by nuclear magnetic resonance spectroscopy(NMR),fourier transforming infrared spectrum(FT-IR),gel permeation chromatography(GPC),thermogravimetric analysis(TGA)and organic elements analysis(OEA).Results demonstrated that walnut shell bio-based high-ortho novolak resins can be synthesized by two-step addition of formaldehyde method,their long chain structure was consisted of phenol rings which linked with methylene by ortho-ortho connection(o-o),ortho-para connection(o-p),and para-para connection(p-p),in particular,structures of phenol rings with methylene by o-o and o-p were dominant,and the ratio of phenol rings with methylene by o-o to p-p were 1.22.Their number-average molecular weight was 4 499 g/mol,polydispersity index was 1.417.And their heat loss process included two stages which the maximum weight loss temperature was 375℃with weight loss rate of 50%.According to OEA,their theoretical formula was C 6H 6O 1.2.

关 键 词：核桃壳 液化 高邻位热塑性酚醛树脂 核磁共振谱 

分 类 号：TQ342.794[化学工程—化纤工业]