Study On Synthesis Method Of ?-butyrolactone

The gamma butyrolactone is a kind of five yuan heterocyclic containing oxygen,it is a kind of important fine chemical raw materials,pharmaceutical intermediates,and excellent solvent.It is widely used in pharmaceutical,spices,textile,petrochemical industry and other chemical fields.Good reaction performance can make it proceed the different chemical reactions,and get kinds of fine chemicals and different heterocyclic compounds.In this thesis,the demand of the chemical market for the gamma butyrolactone in China is discussed by analyzing the technology development of GBL world widely.Firstly,we got the small-batch product by lab experiments;then we successfully enlarged the experiment to industry large scale production and obtained a good yield.First,we used furfuraldehyde and hydrogen peroxide etc.as raw material to get5H-furanone;then obtained gamma butyrolactone by catalytic hydrogenation reaction.The paper discussed the influence of ratio of the material,reaction time,temperature,and the times of catalytic we used to the reaction by orthogonal experiment and get a optimum reaction condition.(1)The optimum reaction condition for 5H-furanone: the moore ratio of furfuraldehyde to dimethylethanolamine is 3.3:1;the moore ratio of methanoic acid to dimethylethanolamine is 6.6:1.The temperature of the reaction is choosed as 40 degree centigrade and the time keep as 3h.(2)The optimum reaction condition for gamma butyrolactone: the temperature keep between 25 and 40 degree centigrade,when pass over the hydrogen with 3h and keep temperature stable about 3h,and the most important thing is that we need add30% more catalytic for the new reaction when reuse the catalytic.By operating the optimum reaction condition,we studied the scale up experiment of both reaction,and get the result as follows:(1)The reaction of 5H-furanoneYield of bench scale experiment is 49.06% while it is 48.54% of scale up experiment.(2)The reaction of gamma butyrolactoneYield of bench scale experiment is 95% while it is 93.19% of scale up experiment.In this study,we characterized the structure of final products and intermediate products by infrared spectroscopy,nuclear magnetic resonance,ultraviolet spectrum and mass spectrum analysis methods,and make sure the final product is what we want.