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Terephthalic Acid: Para-Xylene Oxidised by Air with Manganese and Bromide
Terephthalic acid is the acid half of PET. Both methyl groups of para-xylene are burnt to acid groups by air under pressure in hot acetic acid, with a little manganese salt and bromide as catalyst: the Mid-Century process of Saffer and Barker (US 2,833,816, 1958). The acid does not dissolve, so it is simply filtered off. Example 24 of the patent, all parts by weight.
The picture: our diagram of the reactor.
高级
1 day
说明
1
1
Charge the reactor
Charge the reactor
Into a corrosion-resistant pressure reactor with a water-cooled condenser on top, put 75 parts para-xylene, 150 parts acetic acid, 1 part manganese acetate (tetrahydrate) and 0.75 part ammonium bromide.
此步骤所需材料：
对二甲苯75 parts所需工具：
乙酸（冰醋酸）
乙酸锰
溴化铵
等臂天平
压力反应器
冷凝器盘管
化学防溅护目镜
耐化学品手套2
2
Pressurise with air and heat to 385 °F
Pressurise with air and heat to 385 °F
Raise the pressure to 400 psig with air, blown in near the bottom. Set the vent so gas leaves at 3,000 volumes per hour per volume of liquid. Heat to 385 °F (196 °C), then switch the heat off: the reaction heats itself.
所需工具：
压力反应器
工业空气压缩机冷凝器盘管
实验室温度计3
3
Hold at 385–400 °F
Hold at 385–400 °F
Once the first rush is over, heat as needed to hold 385–400 °F (196–204 °C), 1.5 hours in all. It is finished when the exit gas is back to 20–21 % oxygen (Orsat analysis).
所需工具：
压力反应器实验室温度计
奥氏气体分析仪4
4
Cool, empty and filter
Cool, empty and filter
Cool to 185 °F (85 °C) and let the pressure off. Push the liquid out at 150–200 °F with nitrogen pressure, scrape out the solid, and filter everything together.
所需工具：
氮气瓶
带颈玻璃漏斗
滤纸耐化学品手套5
5
Wash and dry
Wash and dry
Wash the terephthalic acid twice with hot acetic acid (75 ml each in the example) and dry it. The patent got 115 parts by weight from 100 of para-xylene.
所需工具：
乙酸（冰醋酸）带颈玻璃漏斗滤纸
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