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Study On The Clean Catalytic Oxidation To Adipic Acid

Posted on:2011-05-28Degree:MasterType:Thesis
Country:ChinaCandidate:L ZhangFull Text:PDF
GTID:2121360305978080Subject:Chemical Engineering
Abstract/Summary:PDF Full Text Request
Adipic acid (AA) is an important organic intermediates and organic raw materials, which is mainly used in the production of nylon-66, in addition to the synthesis of Lubricants, plasticizers, food additives, plastic foam, dyes and so on. At present, There are many ways of producing adipic acid industry, but most of them have the shortcomings of environmental pollution, serious equipment corrosion and so on. These ways don't meet the requirements of environmental protection. Herein we deseribe the functional ionic liquids, which can replace traditional acid eatalyst. In this paper, the choice of phosphotungstic acid and ionic liquids, ([MIm(CH2)4SO3H][HSO4]) phosphotungstic acid in Supported Ionic Liquid respectively as a catalyst, use 30% hydrogen peroxide catalytic oxidation cyclohexanone synthesis of adipic acid. A more systematic study of the reaction temperature,reaction time, the amount of hydrogen peroxide, the amount of catalyst, catalysts of different loading and catalyst reusability impact on production yield.Four functional ionic liquids was prepared by using one step method or two step method, such as [Bmim][HS04], [MIm(CH2)4SO3H][HSO4], [MIm(CH2)4SO3H][pTSO], and [Hmim][HSO4], and were screening and FT-IR for their, results show that [MIm(CH2)4SO3H][HSO4] has the highest activity.Through the orthogonal experiment, Identified the factors synthesis of MIm(CH2)4SO3 (butyl inner salt), From strong to weak were the order is ratio of raw materials, reaction temperature and dropping the time. The optimum conditions are reaction temperature 80℃, ratio of raw materials 1:1.5, dropping the time 0.5h.Ionic liquids and phosphotungstic acid as catalyst, at appropriate reaction conditions n(H3PW12O40):n(ionic liquids):n(C6H10O):n(H2O2)=1:2:300:1200, reaction temperature 90℃, response time 8h, the yield of adipic acid can be achieved 77.41%.[MIm(CH2)4S03H]3PW12O40 as catalyst, at appropriate reaction conditions:reaction temperature 90℃, response time 8h, n(H2O2):n(C6H10O):n(catalyst)=1350:300:1, the yield of adipic acid can be achieved 82.64%.[MIm(CH2)4SO3H]3PW12O40 as catalyst, at appropriate reaction conditions:reaction temperature 90℃, response time 8h, n(H202):n(C6H10O):n(catalyst)=800:200:1, the yield of adipic acid can be achieved 86.27%.The recovery catalyst was used in the oxidation of cyclohexanone to adipic acid oxidized by H2O2. Atfer catalysis cycle was quintic, catalysis activity dind't reduce. The new caatlyst and the used caatlyst were analysed by FT-IR, and found FT-IR spectra of recovery catlyst in accord with FT-IR spectra of the Keggin structure of [PW12O40]3-...
Keywords/Search Tags:adipic acid, Cyclohexanone, hydrogen peroxide, ionic liquids, Heteropoly acid
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