摘要
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。
Phenoxy acetic acid was prepared by catalytic oxidation reaction, using phenoxyethanol and oxygen as raw materials. HPLC （liquid chromatograph） was used for quantitative analysis, and FrIR （infrared absorption spectrum）, NMR（ nuclear magnetic resonance） and GC -MS（ gas chromatography mass spectrometry） were used for qualitative analysis. The effects of catalysts, solvents, and reaction conditions on reaction results were investigated. The results show that N-hydroxy phthalimide（NHPI） is an efficient catalyst, and dimethylglyoxime and cobaltous acetate are suitable cocatalysts, and acetonitrile is a suitable solvent. The yield of phenoxy acetic acid could reach 68.6% when phenoxyethanol was 0. 1 mol, the amount of NHPI was 8% of molar weight of phenoxyethanol, the suitable molar ratio of NHPI： dimethylglyoxime：cobaltous acetate = 8：7.5：1 and the reaction took place at 80 ℃, 0. 8 MPa O2 for 6 h. The plausible reaction pathway was proposed based on GC - MS analysis.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2013年第6期716-720,共5页
Fine Chemicals
关键词
苯氧乙酸
氧化
催化剂
苯氧乙醇
氧气
精细化工中间体
phenoxy acetic acid
oxidation
catalyst
phenoxyethanol
oxygen
fine chemicalintermediates
