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Research On Liquid-phase Catalytic Oxidation Of Arene Side Chain To Prepare Aromatic Acids

Posted on:2010-05-09Degree:MasterType:Thesis
Country:ChinaCandidate:Y LiFull Text:PDF
GTID:2121360278458074Subject:Chemical processes
Abstract/Summary:PDF Full Text Request
The synthetical route of p-tert-butyl benzoic acid (PTBA) and m-phthalic acid were studied under atmospheric pressure, which taked p-tert-butyltoluene (PTBT) and m-xylene as material, oxygen and 30% hydrogen peroxide as green oxidant respectively.In the experiment which oxidized p-tert-butyltoluene, the reaction under two kind of crafts were studied separately, which taked 30% hydrogen peroxide and oxygen as green oxidant, taked cobalt acetate and homemade catalyst as catalyst respectively. In the p-tert-butyl benzoic acid synthesis from p-tert-butyltoluene oxidated by 30% hydrogen peroxide, the optimization of the reaction conditions were determined as follows: the mass ratio of the catalyst and the material, the mass ratio of the accelerant and the material, the molar ratio of 30% hydrogen peroxide and the material, the molar ratio of acetic anhydride and the material, the molar ratio of acetic acid and the material, the temperature and time of the reaction were 0.09, 0.09, 2.5, 3.5, 9, 80℃and 7 hours respectively. Under such reaction conditions, the conversion of p-tert-butyltoluene reached 97.66% and the yield of p-tert-Butylbenzoic acid reached 87.20%. In the p-tert-butylbenzoic acid synthesis from p-tert-butyltoluene oxidated by oxygen with homemade catalyst, the molar ratio of steeping fluid was 0.17:0.17:0.49, the carrier of the catalyst was CDM-5, and the optimization of the reaction conditions were determined as follows: the choice of carrier, the mass ratio of the homemade catalyst and the material, the temperature, the time and velocity of oxygen of the reaction were 0.06, 120℃, 8 hours, 100 mL/min respectively. Under such reaction conditions, the conversion of p-tert-butyltoluene reached 80.53% and the yield of p-tert-Butylbenzoic acid reached 66.38%.In the experiment which oxidized meta-xylene, the reaction under two kinds of crafts was studied separately, which taked hydrogen peroxide and oxygen as green oxidant, taked cobalt acetate as catalyst. In the m-phthalic acid synthesis from meta-xylene oxidated by hydrogen peroxide, the optimized reaction conditions under atmospheric pressure were determined as follows: the mass ratio of the catalyst and the material, the mass ratio of the accelerant and the material, the molar ratio of 30% hydrogen peroxide and the material, the molar ratio of acetic anhydride and the material, the molar ratio of acetic acid and the material, the temperature and time of the reaction were 0.05, 0.07, 3.5, 2.8, 6.5, 90℃and 2hours respectively. Under such reaction conditions, the conversion of meta-xylene reached 95.94% and the yield of isophthalic acid reached 59.46%. In the m-phthalic acid synthesis from meta-xylene oxidated by oxygen. The optimization of the reaction conditions under atmospheric pressure were determined as follows: the mass ratio of the catalyst and the material, the mass ratio of the accelerant and the material, the molar ratio of acetic acid and the material, the temperature, the time and velocity of oxygen of the reaction were 0.12, 0.05, 87, 8 hours, 90℃and 100mL/min respectively. Under such reaction conditions, the conversion of meta-xylene reached 99.96% and the yield of isophthalic acid reached 98.36%.
Keywords/Search Tags:p-tert-Butyltoluene, p-tert-Benzoicacid, meta-Xylene, m-Phthalic acid, Liquid-phase catalytic oxidation
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