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Study On The Synthesis Of N,N-Dimethylmorpholiniumchloride

Posted on:2007-01-08Degree:MasterType:Thesis
Country:ChinaCandidate:X Z ZhangFull Text:PDF
GTID:2121360212971769Subject:Environmental Engineering
Abstract/Summary:PDF Full Text Request
The important measures that reduce and avoid the generation of pollutants, protect and improve environments is cleaner production , application of measures for design improvement, utilization of clean energy and raw materials, the implementation of advanced processes, technologies. So the green synthetic process is necessarily exploited. N, N-dimethylmorpholinium chloride is a compound which is valuably studied and widely applied.N-methylmorpholine is a important intermediate to prepare N,N-dimethylmor pholinium chloride, the protocols of its synthesis will directly affect the production costs, industrialization of N,N-dimethylmorpholinium chloride and environmental protection. Therefore, the synthetic methods of N-methylmorpholine was firstly explored. (1) N-methylmorpholine was prepared by reaction of morpholine with sodium dihydrogen phosphite and paraformaldehyde.The optimum reaction conditions was obtained, the reaction temperature is at 115℃, the reaction time is 20 minutes, a molar ratio of morpholine to paraformaldehyde to sodium dihydrogen phosphite is 1:1.2:0.56, the yield of product is up to 95% and purity is about 98% (2) N-methylmorpholine was obtained through alkylation of morpholine with monochloromethane in sodium hydroxide solution. The influences of reaction temperature, reation time and molar ratio of reactants on the yield of the reaction were examined. The reaction conditions are as follows: reaction temperature at 35℃, time 5h, n(morpholine):n(monochloromethane) = 1:1.1, n(morpholine):n(sodium hydr- oxide) = 1:1.2 , yield of N-methylmorpholine 85%, purity 98%.Based above studying on synthetic strategiess of N-methylmorpholine.The synthesis of title compound used morpholine and monochloromethane as raw materials, water as solvent, at 40°C, in the presence of acid trap reagent was carried out , the yield was 96%, purity was 99.9%. The catalyst could recover and reuse. The manipulation is simple and convenient, without pollution, the environment was friendliness.
Keywords/Search Tags:N,N-dimethylmorpholinium chloride, Cleaner production, N-methylmorpholine, monochloromethane, Green procedure
PDF Full Text Request
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