化工进展

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含呋喃基双酚-双(4-羟基-3,5-二甲基苯基) 呋喃甲烷的合成与表征

凌俊利1,张军营1,程 珏1,史 翎1,张耀平1,张晓丰1,林 欣2   

  1. 1北京化工大学胶接材料与原位固化研究室,纤维及功能高分子教育部重点实验室,北京 100029;2北京化工大学常州先进材料研究院,江苏 常州213164
  • 出版日期:2011-06-05 发布日期:2011-06-05

Synthesis and characterization of bis (4-hydroxy-3,5-di-methylphenyl)- furylmethane

LING Junli1,ZHANG Junying1,CHENG Jue1,SHI Ling1,ZHANG Yaoping1,ZHANG Xiaofeng1,LIN Xin2   

  1. 1Lab of Adhesives and In-Situ Polymerization Technology,Key Laboratory of Carbon Fiber and Functional Polymers,Ministry of Education,Beijing University of Chemical Technology,Beijing 100029,China;2Changzhou Institute of Advanced Materials,Beijing University of Chemical Technology,Changzhou 213164,Jiangsu,China
  • Online:2011-06-05 Published:2011-06-05

摘要:

2,6-二甲基苯酚和糠醛为原料,氢氧化钠为催化剂,经缩合反应合成了双(4羟基-3,5-二甲基苯基)呋喃甲烷。研究了各因素对反应收率的影响规律,选择反应温度、催化剂用量和反应时间为主要影响因素进行了正交实验。实验得出优化后反应条件为:n(2,6-二甲基苯酚)n(糠醛)=2.21n(2,6-二甲基苯酚)n(氢氧化钠)= 10.11,反应温度为65?℃,反应时间为5?h。在较优条件下进行实验,所得产物收率为61.7%。采用FTIR1HNMRMS表征确定了产物结构,并测得其熔点为151.1?℃,纯度为99.52%

Abstract:

Bis4-hydroxy-3,5-di-methylphenyl-furylmethane was synthesized by the condensation reaction using 2,6-xylenol and furfural as starting materialssodium hydroxide as catalyst. The influence of various factors on this reaction was investigated. Orthogonal experiment was designed by selection of such major factorsas reaction temperaturecatalyst dosage and reaction time. The optimum reaction conditions were determined as follows2.21 of n(2,6-xylenol)/n(furfural)10.11 of n(2,6-xylenol)/n(sodium hydroxide)reaction temperature 65? and reaction time 5?h. Under the optimal conditionsthe product yield could reach 61.7%. The structure of the product with purity of 99.52% and melting point of 151.1? were confirmed by FTIR1H NMR and MS.

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