Optimization of the Synthesis Process of Tri(4-hydroxyphenyl)methane

Jie GUO; Tao XIA; Jie ZHANG; Xiang-yang LIN

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Optimization of the Synthesis Process of Tri(4-hydroxyphenyl)methane

更新时间：2022-09-18

- Optimization of the Synthesis Process of Tri(4-hydroxyphenyl)methane
- Polymer Bulletin Vol. 26, Issue 12, Pages: 66-70(2013)
- 作者机构：
  
  南京理工大学化工学院，南京　210094
- 作者简介：
- 基金信息：
- DOI：
  CLC：
- Published：2013-12，
  
  Received：30 May 2013，
  
  Revised：14 August 2013，
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Jie GUO, Tao XIA, Jie ZHANG, Xiang-yang LIN. Optimization of the Synthesis Process of Tri(4-hydroxyphenyl)methane. [J]. Polymer Bulletin 26(12):66-70(2013)
DOI：

Jie GUO, Tao XIA, Jie ZHANG, Xiang-yang LIN. Optimization of the Synthesis Process of Tri(4-hydroxyphenyl)methane. [J]. Polymer Bulletin 26(12):66-70(2013) DOI：

摘要

以苯酚、对羟基苯甲醛为原料

选用对甲苯磺酸和无水氯化铝为催化剂合成三酚基甲烷

利用红外光谱、液相色谱以及核磁共振等手段对产物进行表征

考察了反应温度、催化剂用量、原料配比及反应时间等工艺参数对产率的影响

随着反应温度的升高

产率逐渐下降;随着催化剂用量的增加

产率先增加后减少;随着原料配比的增加

产率逐渐增加趋于稳定。得出优化的工艺条件为:苯酚与对羟基苯甲醛的摩尔比为10:1

对甲苯磺酸与对羟基苯甲醛质量比为1:2

无水氯化铝与对羟基苯甲醛质量比为1:6

反应时间为4h

温度为45℃

采用该工艺参数可使产率稳定在90%以上。纯化后的样品纯度高达99%以上。

Abstract

The tri(4-hydroxyphenyl)methane was synthesized by using phenol and p-hydroxy benzaldehyde as feed stock

p-toluenesulfonic acid and aluminium chloride as catalyst. The chemical structure of tri(4-hydroxyphenyl)methane was characterized by Fourier-transform infrared (FTIR) spectrometer and

H NMR spectrometer. Four factors such as usage of catalyst

reaction temperature

material ratio and reaction time was studied in experiment

with the increasing of the reaction temperature

the yield increased; with the increasing of catalyst usage

the yield showed an earlier raised and later decreased; with the increasing of material ratio

the yield increased

and then trends toward constance. The result shows that the optional process is that n(phenol)/n(p-hydroxy benzaldehyde)is 10:1

n(p-toluenesulfonic acid)/n(p-hydroxy benzaldehyde) is 1:2

n(aluminium chloride)/n(p-hydroxy benzaldehyde) is 1:6

reaction time is 4h and reaction temperature is 45℃. Under the processing parameter

the yield of product is up to 90%

the purity of the product is up to 99%.

关键词

三酚基甲烷合成工艺对羟基苯甲醛苯酚环氧树脂

Keywords

Tri(4-hydroxyphenyl)methaneSynthesis processingp-Hydroxy benzaldehydePhenolEpoxy resin

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