苯酚制苯二酚反应体系的分析方法

Analytical Method for the Reaction System of Phenol-preparing Dihydroxybenzenes

本文主要针对500吨/年苯酚制苯二酚绿色工艺中试研究项目进行相关分析。采用液相色谱法对苯酚制备苯二酚产物进行分析,以甲醇-水(30∶70,V∶V)混合溶液为流动相,经EXFORMMA Pronaos EP-C_(18) 5μm,4.6 mm×150 mm色谱柱分离,紫外检验波长为265 nm时,分析未反应完的苯酚,产物中的邻苯二酚、对苯二酚、苯醌的含量,根据分析结果可计算出苯酚的转化率,生成苯二酚的选择性以及产品的收率。分析结果表明:苯酚、邻苯二酚、对苯二酚、苯醌在各自的测定范围内均具有很好的线性关系(相关系数>0.999),峰面积测量值的相对标准偏差小于2.0%,分析精准度可达到产品工业分析要求。苯酚的转化率≥23%,苯二酚的选择性≥93%。

In this paper, 500 tons of phenol hydroxylation in green technology research projects conducted correlation analysis. Adopt the HPLC method for preparation of resorcinol phenol products were analyzed, using methanol water（30∶70, V ∶ V） mixed solution as the mobile phase, the EXFORMMA Pronaos EP-C（18） 5μm, 4.6 mm×150 mm column and UV test wavelength of 265 nm, analysis of unreacted phenol, catechol and hydroquinone in product, benzoquinone content can be calculated according to the analysis results, the conversion of phenol and hydroquinone generate selectivity and the yield of the product. The results showed that the phenol, catechol, hydroquinone, benzoquinone has a good linear relation in the determination of the scope of their respective internal（correlation coefficient 0.999）, peak area relative standard deviation of measurement value is less than 2%. The analysis precision can reach the demand of industrial analysis products. The conversion of phenol is more than 23%, more than 93% dihydroxybenzene selectivity.