摘要
以固体光气和邻苯二甲酸为原料,1,2-二氯乙烷作溶剂,DMF为催化剂合成了邻苯二甲酰氯。考察了原料配比、反应温度、溶剂用量、催化剂用量和反应时间对收率的影响。结果表明,当固体光气与邻苯二甲酸摩尔比为1.5∶1,催化剂DMF用量3 mL,反应温度60℃,溶剂1,2-二氯乙烷用量为100 mL,反应时间3.5 h时,合成邻苯二甲酰氯的收率达71.3%,产物纯度为92.4%。利用邻苯二甲酰氯与甲醇的衍生化反应,建立了邻苯二甲酰氯的气相色谱分析方法,并采用外标法对邻苯二甲酰氯进行定量分析,含量为92.4%。
Phthaloyl dichloride was prepared by triphosgene and o-phthalic acid as raw material,using N,N-dimethylformamide as catalysts,and 1,2-dichloroethane as solvent.The effects of the ratio of material,reaction temperature,solvent volume,the catalyst amount and reaction time on yield was studied by experiments.The yield of phthaloyl dichloride obtained 71.3% when the ratio of triphosgene to o-phthalic was 1.5 ∶1 in the presence of DMF 3 mL at 60 ℃ in 1,2-dichloroethane for 3.5 h.The purity of products was 92.4%,in this foundation,meteorological chromatographic analysis was used after the derivative way of phthaloyl dichloride and methanol,then a quantitative analysis used external standard method was did.Its purity reached 92.4%.
出处
《应用化工》
CAS
CSCD
2010年第5期716-719,共4页
Applied Chemical Industry
