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甲基苯基碳酸酯标准品的制备及其定量分析

邢爱华1,2,张敏卿1,何志敏1,张建平1

  

  1. 1.School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China;
    2.Department of Chemical Engineering, Tsinghua University, Beijing 100084, China

  • 收稿日期:2005-06-21 修回日期:2006-03-09 出版日期:2006-05-30 发布日期:1987-03-25
  • 通讯作者: 邢爱华

Preparation and Quantitative Analysis of Methyl Phenyl Carbonate Standard Sample

XING Aihua1,2, ZHANG Minqing1, HE Zhimin1, ZHANG Jianping1

  

  1. 1.School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China;
    2.Department of Chemical Engineering, Tsinghua University, Beijing 100084, China

  • Received:2005-06-21 Revised:2006-03-09 Online:2006-05-30 Published:1987-03-25
  • Contact: Xing Aihua

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摘要：

利用甲基苯基碳酸酯(MPC)歧化反应的可逆性及逆反应在热力学上有利进行的特点,提出了以碳酸二甲酯 (DMC)和碳酸二苯酯 (DPC)为原料,在TiO2/SiO2催化下合成DMC与苯酚酯交换反应的中间产物MPC的新方法。反应产物经减压精馏、碱洗、水洗、干燥等精制处理，得到了纯度较高的MPC标准品。采用气相色谱-质谱法对所制备的MPC样品进行定性分析，结果表明其中还含有少量的苯酚和DPC杂质。卡尔·费休水分测定结果表明,MPC样品中的含水量为0.26%(质量分数)。使用常规气相色谱仪，采用OV-101毛细管色谱柱,以苯甲酸乙酯为内标物,对自制的MPC标准品中的微量苯酚和DPC进行定量分析,苯酚和DPC的含量分别为2.04%和1.59%（均为质量分数）。根据杂质分析结果可知自制的MPC标准品的纯度为96.11%。以此作为标准品,解决了对DMC与苯酚酯交换反应的中间产物MPC的准确定量问题。

关键词: 标准品, 甲基苯基碳酸酯, 气相色谱-质谱法, 制备

Abstract:

The preparation and quantitative analytical method for high-purity methyl phenyl carbonate (MPC) was developed. Dimethyl carbonate（DMC） and diphenyl carbonate (DPC) were firstly used as reactants to synthesize MPC catalyzed by TiO2/SiO2 because the disproportionation of MPC is reversible and the reverse reaction is thermodynamically favorable. The high-purity MPC standard sample was obtained by reduced pressure distillation and the removal of minor phenol with dilute sodium hydroxide solution. The qualitative analysis by gas chromatography-mass spectrometry （GC-MS） showed there were minor phenol and diphenyl carbonate in the MPC sample. The mass percent concentration of water in the MPC sample was 0.26%, which was determined by Karl Fischer titration. A gas chromatographic method with an OV-101 capillary column was established for quantifying the minor phenol and DPC in the MPC sample. The quantitative results showed the mass concentrations of phenol and DPC were 2.04% and 1.59%, respectively. The difficulty to analyze MPC, the intermediate product of the transesterification of DMC and phenol, was solved with the self-made MPC standard sample.

Key words: methyl phenyl carbonate, preparation , standard sample, gas chromatography-mass spectrometry （GC-MS）