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以苯氧乙醇和氧气为原料,经催化氧化合成苯氧乙酸。用高效液相色谱仪(HPLC)进行定量分析,红外吸收光谱仪(FTIR)、核磁共振波谱仪(1HNMR、13CNMR)、气质联用仪(GC-MS)对产品进行了定性分析。考察了催化剂、溶剂对反应的影响,并对反应的单因素进行了考察。结果表明,N-羟基邻苯二甲酰亚胺(NHPI)为主催化剂,丁二酮肟和乙酸钴为助催化剂,乙腈为溶剂;固定苯氧乙醇为0.1 mol,NHPI用量为苯氧乙醇物质的量的8%,催化剂配比是n(NHPI)∶n(丁二酮肟)∶n(乙酸钴)=8∶7.5∶1,0.8 MPa氧压力,于80℃反应6 h,苯氧乙酸收率达68.6%。并根据GC-MS分析结果提出了可能的反应途径。
Using phenoxyethanol and oxygen as raw materials, phenoxyacetic acid was synthesized by catalytic oxidation. The products were qualitatively analyzed by high performance liquid chromatography (HPLC), infrared absorption spectrometer (FTIR), nuclear magnetic resonance spectroscopy (1HNMR, 13CNMR) and gas chromatography-mass spectrometry (GC-MS) The effects of catalyst and solvent on the reaction were investigated, and the single factor of the reaction was investigated. The results showed that N-hydroxyphthalimide (NHPI) was the main catalyst, dimethylglyoxime and cobalt acetate as cocatalyst and acetonitrile as solvent. The amount of phenoxyethanol was 0.1 mol and the amount of NHPI was phenoxyethanol (NHPI): n (dimethylglyoxime): n (cobalt acetate) = 8: 7.5: 1, 0.8 MPa oxygen pressure, reaction at 80 ℃ for 6 h, phenoxyacetic acid The yield was 68.6%. According to the results of GC-MS analysis, the possible reaction routes were proposed.