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Enhancing The Inserting Seletivity Of Alkyleneoxide Into Ethyl Acetate

Posted on:2012-02-05Degree:MasterType:Thesis
Country:ChinaCandidate:Z J ZhangFull Text:PDF
GTID:2131330332491494Subject:Applied Chemistry
Abstract/Summary:PDF Full Text Request
Ethylene glycol ethyl ether acetate (EGEEA) and propylene glycol ethyl ether acetate (PGEEA) are excellent solvents which have been widespread employed in modern industry for their attractive properties such as high solubility and low toxicity. They used to be synthesized in a two-step process with acetic acid as starting material. This procedure causes serious pollution and high energy consumption. It is going to be superseded by one-step production process which shows environmental friendliness and atom economy. In order to obtain the product with a narrow adduct distribution, some surface modification methods of the catalyst were well studied in the reaction of ethyl acetate and ethylene oxide. The reaction of ethyl acetate and propylene oxide was also researched, and 1-ethoxy-2-propanol acetate was the preferred product by using the alkali modified acid-base bifunction catalyst.The technique, direct inserting ethylene oxide (EO) into ethyl acetate (EA) to produce olig-EGEEA over catalyst Y, was described in detail. The products were characterized by Fourier Transferred Infrared Spectrometry (FT-IR), proton Nuclear Magnetic Resonance (1HNMR), Gas Chramatogram–Mass Spectrometry (GC-MS), GC and Elemental Analysis (EA). It was found that the alkali modified catalyst, Y3J, showed the highest production selectivity of EGEEA. It is obtained by partially poisoning the Y3 catalyst in alcoholic potash. The catalyst modification procedure was suggested as followings: the amount of KOH 0.030 g/1.000 g CAT, the volume of ethanol 20.0 mL/1.000 g CAT, reaction time 0.5 hour and drying temperature 150 oC. The selectivity of mono- or di-derivatives was 65.84% or 26.29% separately at the optimized reaction conditions.The product mixture, the reaction of ethyl acetate and propylene oxide (PO) over acid-base bifuction catalyst B, was charactered by GC-MS and GC. It was proved that the catalyst, B5JH, showed the higher region-selectivity to form 1-ethoxy -2-propanol acetate, the innoxious isomer of PGEEA. The B5JH was obtained by potassium ethoxide partially modification of B5 catalyst. The optimum modified condition was: the amount of KOH 0.030 g/1.000 g CAT, the volume of ethanol 20.0 mL/1.000 g CAT, reaction time 0.5 hour, drying temperature 150 oC and re-calcination time 5.0 hour. The highest product selectivity of innoxious PGEEA was 62.88%.
Keywords/Search Tags:green solvent, one-step process, catalyst modification, oligo-ethylene glycol ethyl ether acetate, innoxious propylene glycol ethyl ether acetate, product selectivity
PDF Full Text Request
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