Research On Synthesis Of P-tert-Butylb Enzoic Acid By Liquid-phase Oxidation Of P-tert-butyltoluene

In this text,the craft route of p-tert-butylbenzoic acid(PTBA) synthesis is studied under atmospheric pressure,which taked p-tert-butyltoluene(PTBT) as material,oxygen and 30% hydrogen peroxide as green oxidant respectively.In the experiment with no solvent,the reaction under two kind of crafts were studied conditions separately,which taked Co(COOH)₂ and MnSO₄ as catalyst respectively to synthesize PTBA from PTBT.The influence of a series factors such as species and dosage of the promoter,the dosage of the catalyst,the time and temperature of the reaction as well as the velocity of oxygen on the reaction were investigated in the experiment taking oxygen as oxidant and Co(COOH)2 as catalyst under atmospheric pressure without solvent,and the proper reaction conditions were determined under atmospheric pressure as follows:the mass ratio of the catalyst and the material,dosage of the promoter,time and temperature of the reaction and the velocity of oxygen were 0.027,0.3mL, 8hours,130℃and 100mL/min respectively.Under such reaction conditions,the yield of p-tert-butylbenzoic acid reached 68.09%. The influence of a series factors such as species and dosage of the promoter,the dosage of the catalyst,the time and temperature of the reaction as well as the velocity of oxygen on the reaction were investigated in the experiment using oxygen as oxidant and MnSO4 as catalyst under atmospheric pressure without solvent,and the proper reaction conditions were determined under atmospheric pressure as follows:the mass ratio of thecatalyst and the material,dosage of the promoter,time and temperature of the reaction and the velocity of oxygen were 0.027, 0.5g, 8hours,130℃and 100mL/min respectively.Under such reaction conditions,the yield of p-tert-butylbenzoic acid reached66.94%.In the experiment taking H₂O₂ as oxidant, we discovered that the H₂O₂-NaBr was a very good catalyzed system,and the influence of a series factors on the reaction such as the dosage of hydrogen peroxide,the dosage of acetic anhydride,the dosage of bromide natrium,the time and temperature of the reaction and the dosage ofhydrochloric acid were investigated.Under optimal reaction conditions: the dosage ofPTBT was 4 mL,the dosage of acetic anhydride was 6 mL,the mass ratio of the NaBr and the material was 0.029,the dosage of hydrochloric acid was 0.06mL,the mo l ratio of the H₂O₂ and the material was 2.653,the temperature and time of reactionwas 80℃and 8h respectively, the yield of p-tert-butylbenzoic acid reached 47.76%.The craft route of synthesis of PTBA by Liquid-phase oxidation of PTBT that was studied in this text has many advantages such as environment-friendly,conditions moderately and lowest costing etc. This work opened up a new way that can be followed by green synthesis of other organic compounds and has a certain referencevalue.