摘要
采用三甲基氢醌(TMHQ)与乙醛在低温下合成2,4,5,7,8-五甲基-4-氢-1,3-苯并二噁英-6-醇(PBD),对其合成的影响因素进行初步探讨;并进一步将PBD与没食子酸丙酯(PG)进行对比,分析了PBD对纤维素/N-甲基吗啉氧化物(NMMO)水溶液稳定性的影响。通过傅里叶红外光谱仪、核磁共振仪以及气相-质谱联用仪等对合成产物的结构及组成的表征,发现搅拌方式以及加料顺序对PBD的合成具有很大的影响,在合适的条件下可以成功地合成出PBD;此外,紫外光谱和哈克流变仪对纤维素溶液的分析结果表明,PBD对纤维素/NMMO·H2O溶液的颜色影响较小,稳定性优于PG。
2,4,5,7,8-pentamethyl-4-hydro-1,3-benzodioxin-6-ol(PBD)was synthesized by condensation trimethylhydroquinone(TMHQ)with acetaldehyde in an acid-catalyzed reaction.The influencing factors of the synthesis were discussed.The cellulose/NMMO·H2O spinning dope adding stabilizer propionate gallate(PG)、PBD were preparedby stirring and comparative analyzed of the effects of PG and PBD on the stability of cellulose/NMMO·H2O spinning dope.The structure and composition of product were characterized by Fourier transform infrared spectrometer,nuclear magnetic resonance instrument,gas phase-mass spectrometry.It was found that the stirring method and the order of catalyst addition had a great influence on the synthesis of PBD.Under the appropriate condition,we successfully synthesized PBD.In addition,the analysis results of cellulose solution by UV spectrum and HAKKE rheometer showed that PBD had less influence on the color of cellulose/NMMO·H2O solution and had better stability than PG.
作者
杨彦菊
彭康
张慧慧
杨革生
邵惠丽
Yang Yanju;Peng Kang;Zhang Huihui;Yang Gesheng;Shao Huili(State Key Laboratory for Modification of Chemical Fibers and Polymer Materials,College of Material Science and Engineering,Donghua University,Shanghai 201600,China)
出处
《合成技术及应用》
2020年第1期1-6,共6页
Synthetic Technology & Application
基金
国家重点研发计划项目课题(2017YFB0309501)。
