【摘要】 目的建立了气相色谱法中外标法测定Friedel-Crafts烷基化反应中的氯化苄和二苯甲烷含量的方法。方法实验采用PEG-20M填充柱(3m×3mm),FID检测器,以氮气为载气,氮气、空气和氢气的压力比为8∶8∶5,不分流进样,进样口、柱温和检测器的温度分别为260℃,180℃和250℃。结果在此条件下,反应体系中的苯、氯化苄和二苯甲烷分离良好。氯化苄和二苯甲烷的最大体积分数分别小于9.09%和12.5%时,外标法所测得的二者的峰面积与体积分数线性关系良好,线性相关系数均为0.999,两种组分低、中、高3个浓度水平的回收率分别在94.59%～104.61%和98.85%～107.30%范围内,相对标准偏差均小于2.20%。依据建立的外标测定方法,对烷基化反应工艺条件中反应温度、时间和催化剂用量进行了优化,由该法所得出的优化结论与理论研究结果一致。结论所建立的方法是测定Friedel-Crafts烷基化反应中氯化苄和二苯甲烷含量的一种快速、准确和实用的方法。更多还原

【Abstract】 Aim An external standard method in gas chromatography was established for the determination of benzyl chloride and diphenylmethane in Friedel-Crafts alkylation.Methods PEG-20M packed column(3m×3mm) with FID detector was adopted.The pressure ratio of nitrogen(carrier gas),air and hydrogen was 8:8:5.Splitless injection was chosen.The inlet,column and detector temperatures were 260℃,180℃ and 250℃,respectively.Results The good separation of the benzene,benzyl chloride and diphenylmethane was obtained under optimal chromatographic conditions.When the maximum volume fractions of the benzyl chloride and diphenylmethane were less than 9.09% and 12.5%,the volume fractions and their peak areas were well linear relationship and the linear correlation coefficients were all 0.999.The recovery rates of these two components at low,medium and high concentration levels were 94.59% ～ 104.61% and 98.85% ～ 107.30%.The relative standard deviations were all less than 2.20%.Based on the established external standard method,the reaction temperature,time,and the quantity of the catalyst were optimized.Conclusion The optimization results obtained by this method were consistent with theoretical conclusions.The results show that the proposed method is a fast,accurate and practical method for determining the contents of benzyl chloride and diphenylmethane in the Friedel-Crafts alkylation reaction.更多还原