摘要
以2,4-二氯苯甲醛和盐酸羟胺为原料,经醛肟化、脱水2步反应合成了2,4-二氯苯腈,通过正交实验对2步反应的影响因素进行优化分析,得出最佳合成方案。最佳工艺条件是:物料配比为n(醛)∶n(羟胺)=1.0∶1.1,反应温度为70～75℃,反应时间为30min;n(醛肟)∶n(乙酸酐)=1∶1.4,反应温度为110～120℃,反应时间为3h。2步最佳工艺条件下总收率可达90.2%。重结晶所得产品经元素分析、红外光谱分析和熔点测定,可初步确认该产品为目标化合物。
2,4-dichlorobenzonitrile is synthesized with the 2,4-dichlorobenzaldehyde and hydroxyl amine hydrochloride as raw materials,throwing oxime and dehydration.The optimum technological conditions are determined by the orthogonal experiment based on three paralleled affecting factors,which was associated with the selection of raw material ratio,reaction temperature and reaction time.The details are as follows： material molar ratio of n（2,4-dichlorobenzaldehyde）∶n（hydroxyamine hydrochloride）=1.0∶1.1;reaction temperature：70~75 ℃;reaction time： 30 min;n（formaldehyde）∶n（acetic anhydride）=1∶1.4;reaction temperature：110~120 ℃ for 3 h.Under the optimal condition,the excellent yield rate can reach 90.3% and then the product was determined through the measurement of melt point,the analysis of IR and elements.The product can be primarily affirmed to be the target product.
出处
《北京石油化工学院学报》
2012年第1期45-49,共5页
Journal of Beijing Institute of Petrochemical Technology
基金
北京市教育委员会科技发展计划项目
项目号:Z2009-07
关键词
苯腈
合成
2
4-二氯苯腈
醛肟
benzonitrile
synthesis
2
4-dilochlorobenzionitrile
oxime
