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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.
Lanjutan
1 day
Instruksi
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.
Material untuk langkah ini:
Para-xilena75 partsAlat yang dibutuhkan:
Asam asetat (glasial)
Mangan Asetat
Amonium Bromida
Neraca lengan
Reaktor bertekanan
Kumparan kondensor
Kacamata Pelindung Cipratan Kimia
Sarung Tangan Tahan Bahan Kimia2
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.
Alat yang dibutuhkan:
Reaktor bertekanan
Kompresor udara industri
Kumparan kondensor
Termometer Laboratorium3
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).
Alat yang dibutuhkan:
Reaktor bertekanan
Termometer Laboratorium
Penganalisis Gas Orsat4
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.
Alat yang dibutuhkan:
Tabung Gas Nitrogen
Corong Kaca Bertangkai
Kertas Saring
Sarung Tangan Tahan Bahan Kimia5
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.
Alat yang dibutuhkan:
Asam asetat (glasial)
Corong Kaca Bertangkai
Kertas Saring
Oven pengeringanBahan
1- 75 partsPlaceholder
Alat yang Diperlukan
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