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将氢溴酸放入上溴反应罐，冷却，慢慢地加入奥氏氧化物，加毕，用水浴加热，搅拌保温，取样层析，反应完全后将反应液拉到水析罐中水析，搅拌，放料离心，再用水洗涤至中性，甩干后得上溴物。 将乙醇、上溴物、冰醋酸按顺序投入反应罐中，开搅拌，水浴搅拌，通氮气保护，加入活性镍，关氮气，抽真空度，然后通氢气，再抽气，如此换气三次以上，开搅拌，通氢气，滴加缓冲液（醋酸铵、乙醇、吡啶、水配成），再继续通氢气，反应完毕，在氮气保护下，将上层清液拉到浓缩罐，将料液减压浓缩至近干，冲水，冷却，放料离心，甩干后，用冷乙醇浇洗，水洗至滤液呈中性，甩干，干燥，得脱溴粗品。 将醋酐、脱溴物、对甲苯磺酸加入反应罐，进行酰化反应，然后加入乙醇反应，再加盐酸与乙醇的混合液反应回流，冷却结晶。将结晶料液放入离心机中甩干，用碳酸钠溶液中和至中性，甩干后，放烘箱干燥，得单酯粗品。 将乙醇、粗品、冰乙酸、锌粉、活性炭加入精制罐，回流脱色，过滤，减压浓缩，冷却结晶，出料离心，甩干，入烘房烘干得单酯精品。 |
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4楼2010-08-11 11:36:58
谦恭四海
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Placed the hydrobromide on bromide reaction tank, cooling,slowly add in Ao's oxide, plus complete, with water bath,mixing heat, sampling chromatography, the reaction will complete ,analysis of the reaction solution pulled water tank water analysis,mixing, discharge centrifuge, washed with water to neutrality, drying after that thing on the bromine. To ethanol, the bromine material, glacial acetic acid into reaction tank in order, open mixing, stirring water bath, through nitrogen protection, adding active nickel,off nitrogen, vacuum degree, then pass hydrogen, then the exhaust, so ventilation for more than three times,open mixing, through hydrogen, dropping buffer (ammonium acetate, ethanol, pyridine, water, dubbed),continue through the hydrogen, the reaction is completed, under a nitrogen atmosphere, to pull the upper clear liquid concentrate cans,the feed solution evaporated to near dry, flushing, cooling, discharge centrifuge, drying after washing with cold ethanol, poured, washed with water to the filtrate was neutral, drying, drying, Detuo crude bromine. To acetic anhydride, debromination of objects by adding p-toluenesulfonic acid reaction tank, to acylation reaction, and then ethanol reaction, coupled with the mixture of reaction between hydrochloric acid and ethanol, reflux, cooling crystallization.The liquid crystal material into the centrifuges in the drying, and with sodium carbonate solution to neutral, after drying, put oven drying, then produce crude monoester. To ethanol, crude, glacial acetic acid, zinc powder, active carbon refining cans, back decolorization, filtration, vacuum concentration, cooling crystallization, discharging centrifuge, drying, into the drying chamber may monoester fine. |
2楼2010-08-11 09:01:37
noleg
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3楼2010-08-11 10:01:33
