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研究了以油酸甲酯为原料,乙酸和正己烷的混合物做溶剂,臭氧氧化法制备壬二酸单甲酯的方法。考察了物料比、臭氧化温度、氧化裂解温度和氧化裂解时间对反应结果的影响。结果表明,合成壬二酸单甲酯的最佳条件为:V(油酸甲酯):V(混合溶剂)=1:4,臭氧化反应温度为10~13℃,氧化裂解温度为90~95℃,氧化裂解时间为2.5 h,反应粗产物用分子蒸馏技术进行分离纯化。在此条件下,壬二酸单甲酯的收率≥78%,纯度≥96%。其结构经过IR,~1H NMR,GC-MS确证。
A method for preparing monomethyl azelate by using methyl oleate as a raw material and a mixture of acetic acid and n-hexane as a solvent and ozone oxidation was studied. The effects of material ratio, ozonation temperature, oxidative pyrolysis temperature and oxidative pyrolysis time on the reaction results were investigated. The results showed that the optimal conditions for the synthesis of monomethyl azelate were: V (methyl oleate): V (mixed solvent) = 1: 4, the ozonization temperature was 10 ~ 13 ℃ and the oxidation cracking temperature was 90 ~ 95 ℃, the oxidative cleavage time was 2.5 h, the crude reaction products were separated and purified by molecular distillation. Under these conditions, the yield of monomethyl azelate is ≥78% and the purity is ≥96%. Its structure was confirmed by IR, 1H NMR and GC-MS.