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Study Of Preparation, Characterization And Evaluation Of Catalyst For Synthesis Of ε-caprolactone

Posted on:2015-08-01Degree:MasterType:Thesis
Country:ChinaCandidate:H B ZhangFull Text:PDF
GTID:2181330452950159Subject:Chemical Engineering
Abstract/Summary:PDF Full Text Request
ε-caprolactone monomer is a useful chemical intermediates and solute,as a rawmaterial for synthetic products provide many excellent chemical properties,such as:biocompatibility, of biodegradable,of thermoplastic, permeability.It mainly used insynthesis of environmental protection materials and medical materials. Metalcomposite oxides have been widely used in chemical industry as catalysts. For thestatus quo of ε-caprolactone low yield and selectivity, in this paper, we preparatedmetal composite oxides as an efficient catalyst for synthesis of ε-caprolactone usingindirect method for oxidation of cyclohexanone with H2O2and acetic acid. And thepreparation conditions of the catalysts are optimized to determine the mosttechnological conditions. What of catalyst were carried out to explore weredeactivation, regeneration and pilot production. The preparation of a series ofcatalysts was evaluated and characterization analysis.1) W/Sn/Mg composite metal oxide catalysts were prepared byprecipitation,using magnesium chloride, tin chloride and tungsten acid as rawmaterials. ε-caprolactone yield was82.91%, the selectivity was92.12%, W/Sn/Mgcomposite metal oxide catalyst is highly active in the reaction.2) With the reaction conversion, yield and selectivity for evaluation standard,catalyst preparation process is optimized through the single factor experiment. Theresults showed that catalysts is the highest activity when the ammonia as precipitant,pH=10, tungsten acid dosage is9.5g, calcination temperature is600℃, roastingtime is3h. Cyclohexanone conversion, ε-caprolactone yield and selectivityrespectively were92.29%,89.84%and97.35%.3) Through the research of catalyst use times and regeneration of catalyst afterdeactivation, results showed that the new catalyst could be used for5times, catalystregeneration conditions: regeneration of roasting temperature is450℃, regenerationof roasting time is3h after the deactivation. Cyclohexanone conversion,ε-caprolactone yield and selectivity respectively were90.55%,80.86%and89.29%.4) The catalyst were prepared through pilot production device makes ananalysis under laboratory conditions, preparation of catalyst is more successful withgood repeatability from lab to pilot amplification. Cyclohexanone conversion,ε-caprolactone yield and selectivity respectively were92.20%,89.59%and96.69%.
Keywords/Search Tags:ε-caprolactone, metal composite oxides catalyst, deactivation, regeneration, pilot amplification
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