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Synthesis And Design Of200t/a Process Flow For DMAP And The Study On Chlorination Technology Of3-methylpyridine

Posted on:2015-01-03Degree:MasterType:Thesis
Country:ChinaCandidate:W C WangFull Text:PDF
GTID:2251330428974556Subject:Pharmaceutical engineering
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This thesis consists of two parts:The first part4-dimethylaminopyridine (abbreviation DMAP) is a widely used catalyst, and iswidely used in a variety of organic reactions, so it is called super-catalyst. In thisarticle, based on the needs of the market, we researched and summarized thesynthesis method from literature. We designed a more rational synthesis route.In this article, we used4-cyanopyridine and styrene as raw materials to prepareDMAP. The best reaction condition was mol (4-cyanopyridine): mol (styrene)1:1.2,complexation reaction temperature was60℃, the reaction time was10h; substitutionreaction temperature was40℃, the reaction time was4h; the hydrolysis reaction timewas2h, the reaction temperature was95℃. The product structure was confirmed byNMR and melting point apparatus. Finally the total yield was73.8%.Combining technology research laboratory test, The issue started with anannual output200tons DMAP process design project. According to the factors fromthe laboratory test which included material properties of the resulting reactionprocesses, reaction process and product requirements, experimental conditions, thedesign process included craft demonstration, material balance, equipment selection,drawing of chemical process flow diagram.The second partA new generation of pesticides related to pyridine and pyridine derivativeswhich have low toxicity, high efficiency, environmental protection and other featureshas become a new hot spot of pesticides.2.chlorol-5-methyl pyridine is an important intermediate for preparing the newpesticide. In this article, Based onmarket demand, a more reasonable synthesis routehas been designed.3-methyl pyridine as raw material, chlorine as chlorine source, carbontetrachloride as a solvent, to achieve3-methyl pyridine positioning chloride bycatalytic composite metal catalysts, and get the product2-chlorol-5-methyl pyridineby post-processing-related.Through process optimization, Finally the total yield was30%.
Keywords/Search Tags:synthesis of DMAP, Process Improvement, Design of production process, synthesis of2-chloro-5-methyl pyridine
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