|Place of Conferral||北京|
|Keyword||壬二酸 分离纯化 固液萃取 循环利用|
壬二酸是一种重要的精细化工中间体，目前工业上主要是以油酸、亚油酸等不饱和脂肪酸为原料经过臭氧氧化制得。如何解决臭氧产物的分离问题，得到纯度更高、更具市场竞争力的壬二酸产品，成为制约壬二酸生产的重要因素。本文详细分析了臭氧氧化产物中各组分的来源和性质，对比了壬二酸和其它组分的物理化学性质，经多步分离、逐级萃取得到高品质的壬二酸。实验中考察了分离顺序、萃取溶剂、萃取温度、萃取时间和溶剂循环次数对壬二酸纯度的影响，确定了分离纯化的最优工艺为：取50g 油酸臭氧氧化，产物先于70℃旋转蒸发2h 除出醋酸溶剂；再加入2L 沸水保温萃取，冷却，结晶，得到质量分数为88.7％的壬二酸粗品； 粗品与乙酸乙酯以质量比1:7.2 的比例混合，30℃下搅拌萃取3h，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，达到电子产品要求；整个过程的收率为64.4%。在实验基础上，设计了一个完整的制备工艺流程，使所有的原料和溶剂都得到了充分地利用和回收，为工业化生产提供了可供参考的理论基础。
Azelaic acid was an important fine chemical intermediate which was made from unsaturated fatty acids such as oleic and linoleic acid and mixtures thereof by oxidization with ozone. How to separate the mixed oxidation product and obtain high purity azelaic acid with strong competitive ability, has become an important factor which restricts the production of azelaic acid. The origin and nature of various components in the intermixture were analyzed systemically and contrasted in detail in this dissertation. Then the high purity azelaic acid was made by several steps and multistage extraction. In the experiment, the effect factors of separation order, extraction solvent, extraction temperature, extraction time and solvent cycle-index were viewed. The optimum conditions were confirmed and shown as follows: 50g oleic acid was ozonized and reductive decomposition by oxygen, oxidation product was concentrated by rotatory evaporation at 70℃ for 2 hours to remove the acetic acid solvent. The residue was extracted by 2L boiling water in tap funnel, cooled and crystallization, a 88.7% crude purity was achieved. The crude azelaic acid and ethyl acetate were mixed by the weight ratio of 1:7.2, at 30℃ for 3 hours, filtered and dried in vacuum. The obtained product was detected by GC-MS, showing a purity more than 98%, which can be used in the electronic product field. The yield of the whole process was 64.4%. A flow chart of making azelaic acid was designed based on the experiment. This process recycled and reused all the solvent and rude materials. This dissertation can provide theoretical reference for industrial manufacture.
|周聪晓. 壬二酸的分离纯化工艺研究[D]. 北京. 中国科学院研究生院,2007.|
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