【作者】 杨兰；

【导师】 陈学玺；

【作者基本信息】 青岛科技大学 ， 化学工艺， 2007， 硕士

【摘要】 本研究以工业M为原料，采用绿色氧化剂-过氧化氢，选用无毒、低毒溶剂，一步法合成了高品质的DM，所得产品无需精制即可达到药用生产的要求，工艺简单可行；利用红外光谱，对合成产物进行了结构表征；利用熔点仪、高效液相色谱，对产品进行纯度分析。同时对反应溶剂进行回收，并对整个回收流程进行模拟、实验验证，使生产过程中的溶剂可以循环使用，达到了降低成本、清洁生产的目的。通过大量实验，确定制备DM的最佳工艺条件为：以IPA为溶剂，氧化M-Na溶液得到的DM熔点可达180℃，收率80-90％；最佳工艺条件为：反应温度50℃，加料时间1h，反应时间1.5h，M-Na溶液浓度30％，物料配比2：1，碱过量程度5％，溶剂的量1.5倍（以M-Na溶液为基准的油水质量比）；以IPA为溶剂，氧化固体M得到的DM熔点可达181℃，收率90％；最佳工艺条件为：加料时间1.25h，物料配比2：1.2，溶剂与M质量比7，反应温度50℃，溶剂在H₂O₂中分配1：3（与H₂O₂混合的溶剂占溶剂总量的分数）；以THO为溶剂，氧化固体M得到的DM熔点可达184.5℃，收率96％，纯度99.6％；最佳工艺条件为：反应温度40℃，加料时间1h，反应时间3h，碳酸钠2.5％，物料配比2：1.1，有机溶剂3倍（以M质量为基准），陈化时间0h。同时发现，反应过程中加入分子筛和微量表面活性剂可提高产品收率，但对产品的熔点没有影响。用ASPAN化工模拟软件对溶剂回收环节进行模拟计算，THO萃取精馏的最佳工艺参数为：萃取塔塔板数22，进料位置19，溶剂进料位置3，溶剂温度40℃，原料温度50℃，回流比0.8，溶剂比0.65；回收塔塔板数13，进料位置6，回流比0.5。进行间歇萃取精馏实验，产物通过GC分析含量，结果表明，THO的回收率和纯度与模拟计算结果基本一致。更多还原

【Abstract】 This research takes the industrial M as the raw material, adopting the greenoxidant—hydrogen peroxide, using the nontoxic and low noxious organic reagent, theone-step method synthesized the high-quality DM. The product can immediately meetthe request in medicine production, the technology is feasible. Make use of the IRspectrum to analyze the outcome; make use of the melting point apparatus and HPLCto analyze the product’s purity. At the same time, reclaim the organic reagent,simulate and validate the whole reclaim flow. Make sure that the reagent can beused circularly; the whole process is low cost and cleanly.By a great deal of experiment, the optimum technologic condition is:Take IPA as the organic reagent, oxidizing the M- Na solution to get DM, themelting point can arrive at 180℃, Yield 80～90％; The optimum technologic conditionis: reaction temperature 50℃, addition time 1 h, reaction time 1.5 h, the concentrationof M- Na solution 30％, the ratio of materials 2:1, the excess of alkali 5％, the quantityof reagent 1.5 times;（ based on the quantity of M- Na solution）;Take IPA as the organic reagent, oxidizing the solid M to get DM, the meltingpoint can arrive at 181℃, Yield 90％; The optimum technologic condition is: additiontime 1.25 h, the ratio of material 2:1.2, reaction temperature 50℃, the ratio betweenthe quantity of reagent and M 7, the ratio of reagent in hydrogen peroxide 1 : 3 （ basedon the quantity of M）;Take THO as the organic reagent, oxidizing the solid M to get DM, the meltingpoint can arrive at 184.5℃, Yield 96％, purity 99.6％; The optimum technologiccondition is: reaction temperature 40℃, addition time 1 h, reaction time 3h, thequantity of Na₂CO₃ 2.5％（based on M）, the ratio of material is 2:1.1, the quantity of reagent 3times （based on the quantity of M）, deposited time Oh;At the same time, the addition of molecule sieve and surfactant can raise thefield, but make no difference to the melting point.Use the ASPAN software to simulate and calculate the organic reagent reclaimflow, the optimum technologic parameter of the extract distillation is: the number ofboard of extract distillation column 22, the feed plate 19, the location of solventfeed-in 3, the temperature of solvent 40℃, the temperature of raw material 50℃,reflux ratio 0.8, molecular rate of solvent and raw material 0.65; The number of boardof solvent reclaim column 13, the feed plate 6, reflux ratio 0.5. By batch extractdistillation experiment, the content of outcome is analyzed by GC; the purity isaccordant to the simulation.更多还原