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酶解木质素液化降解制备酚醛树脂用酚类化合物的研究     被引量:4

Liquefi ed Degradation of Enzymatic Hydrolysis Lignin for Preparing Phenolic Compound used to Synthesize Phenolic Resin

文献类型:期刊文献

中文题名:酶解木质素液化降解制备酚醛树脂用酚类化合物的研究

英文题名:Liquefi ed Degradation of Enzymatic Hydrolysis Lignin for Preparing Phenolic Compound used to Synthesize Phenolic Resin

作者:周静[1,2,3,4] 胡立红[1,2,3,4,5] 周永红[1,2,3,4] 薄采颖[1,2,3,4] 梁兵川[1,2,3,4]

第一作者:周静

机构:[1]中国林业科学研究院林产化学工业研究所;[2]生物质化学利用国家工程实验室;[3]国家林业局林产化学工程重点开放性实验室;[4]江苏省生物质能源与材料重点实验室;[5]中国林业科学研究院林业新技术研究所

年份:2014

卷号:42

期号:2

起止页码:101-106

中文期刊名:工程塑料应用

外文期刊名:Engineering Plastics Application

收录:CSTPCD;;北大核心:【北大核心2011】;CSCD:【CSCD2013_2014】;

基金:国家863计划项目(2013AA050703)

语种:中文

中文关键词:酶解木质素;催化;液化;降解;热塑性酚醛树脂

外文关键词:EHL;catalytic;liquefaction;degradation;thermoplastic phenolic resin

分类号:TQ321.5

摘要:以草酸为催化剂、苯酚为液化剂对酶解木质素(EHL)进行液化降解,制备可以部分代替苯酚用于合成酚醛树脂(PF)的EHL液化产物。采用凝胶渗透色谱法、傅立叶变换红外光谱法、高效液相色谱法及气相色谱–质谱联用仪研究了液化产物的结构和分子量变化情况,并探讨了EHL与苯酚的物质的量之比、反应温度、反应时间、催化剂用量等对液化产物分子量的影响,最后初步探讨了EHL液化产物在PF合成中的应用情况。结果表明,EHL在液化降解过程中其分子发生化学键的断裂使得分子量减小,同时生成一系列酚类及烷类化合物;EHL及其液化产物与部分苯酚发生反应,降低了游离苯酚的含量;以液化产物分子量为指标,得到了初步优化的液化降解条件:EHL与苯酚的物质的量之比为1∶2,反应温度为135℃,反应时间为2 h,催化剂的用量为苯酚质量的4%,此时制备的液化产物具有较小的分子量,可提供较多的反应活性点;在此优化条件下,当EHL液化产物替代量为苯酚质量的20%时,由其合成的PF的性能与传统热塑性PF相当。
The liquefied degradation of enzymatic hydrolysis lignin (EHL) was done by using oxalic acid as catalyst and phenol as liquefaction agent,then the EHL liquefaction products used for replacing phenol partially to synthesize thermoplastic phenolic resin (PF) were prepared. The change conditions of the structure and molecular weight of the liquefaction products were studied through GPC,FTIR,HPLC and GC-MS and the effects of molar ratio of EHL and phenol,reaction temperature,reaction time and the catalyst content on the molecular weight of the liquefaction products were studied,at last,the application of the liquefaction products on the synthesis of PF was investigated preliminarily. The results show that the chemical bond fracture in EHL molecules occurs and the molecular weight decreases in the process of liquefied degradation,meanwhile,a series of phenolic compounds and alkyl compounds were generated. The content of free phenol decreases due to EHL and it’s liquefaction products reacting with phenol. The optimization process conditions of liquefied degradation are as follows:the molar ratio of EHL and phenol is 1∶2, the reaction temperature is 135℃,the reaction time is 2 h and the catalyst content is 4%of phenol mass. Under the optimization process conditions,the liquefaction products have minor molecular weight and can provide more reactivity,meanwhile,when the replacement content of the liquefaction products is 20%of phenol mass,the performances of PF synthesized by the liquefaction products are equal with traditional thermoplastic PF.

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