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以油酸臭氧氧化法制备的纯度为88.37%的壬二酸粗品为原料,用固液萃取法分离提纯,得到了纯度为98.73%的壬二酸。用GC-MS气质联用仪测定了壬二酸粗品的成分,分析了常用溶剂对各个组分的溶解性能,比较了乙酸乙酯、乙醚、正庚烷和环己烷对壬二酸粗品的纯化效果,确定了以乙酸乙酯为溶剂提纯壬二酸。结果表明,100 g壬二酸粗产品加入800 mL乙酸乙酯,搅拌混合3 h,抽滤、洗涤、真空干燥,得到的壬二酸产品通过GC-MS气质联用仪分析检测,其质量分数达到98%以上。溶剂可以循环利用,并且循环3次之后均可萃取得到纯度96%的壬二酸。
The crude azelaic acid with the purity of 88.37% prepared by oleic acid ozone oxidation method was used as raw material. The pure azelaic acid was separated and purified by solid - liquid extraction, and the purity was 98.73%. The composition of crude azelaic acid was determined by GC-MS gas chromatography-mass spectrometer. The solubility of common azelaic acid for each component was analyzed. The effects of ethyl acetate, ethyl ether, n-heptane and cyclohexane on the yield of azelaic acid crude Purification effect, identified with ethyl acetate as solvent purification azelaic acid. The results showed that 100 g azelaic acid crude product was added to 800 mL ethyl acetate, stirred and mixed for 3 h, filtered, washed and dried under vacuum. The obtained azelaic acid product was detected by GC-MS GC-MS. The mass fraction More than 98%. Solvent can be recycled, and can be extracted after three times the purity of azelaic acid 96%.