CAJ | 학술논문

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。
이초산위최화제、분분위액화제대매해목질소(EHL)진행액화강해，제비가이부분대체분분용우합성분철수지(PF)적EHL액화산물。채용응효삼투색보법、부립협변환홍외광보법、고효액상색보법급기상색보-질보련용의연구료액화산물적결구화분자량변화정황，병탐토료EHL여분분적물질적량지비、반응온도、반응시간、최화제용량등대액화산물분자량적영향，최후초보탐토료EHL액화산물재PF합성중적응용정황。결과표명，EHL재액화강해과정중기분자발생화학건적단렬사득분자량감소，동시생성일계렬분류급완류화합물；EHL급기액화산물여부분분분발생반응，강저료유리분분적함량；이액화산물분자량위지표，득도료초보우화적액화강해조건：EHL여분분적물질적량지비위1∶2，반응온도위135℃，반응시간위2 h，최화제적용량위분분질량적4%，차시제비적액화산물구유교소적분자량，가제공교다적반응활성점；재차우화조건하，당EHL액화산물체대량위분분질량적20%시，유기합성적PF적성능여전통열소성PF상당。
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.