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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.
Abantado
1 day
Mga Tagubilin
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.
Mga materyales para sa hakbang na ito:
Para-Xylene75 partsMga kailangang kasangkapan:
Acetic acid (glacial)
Manganese Acetate
Ammonium Bromide
Timbangang panimbang
Reactor na may presyon
Ikid ng kondensador
Salamin Laban sa Tilamsik ng Kemikal
Gwantes na Matibay sa Kemikal2
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.
Mga kailangang kasangkapan:
Reactor na may presyon
Pang-industriyang panipil ng hanginIkid ng kondensador
Termometrong Panlaboratoryo3
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).
Mga kailangang kasangkapan:
Reactor na may presyonTermometrong Panlaboratoryo
Orsat Gas Analyser4
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.
Mga kailangang kasangkapan:
Silindro ng Nitrogen
Embudong Salamin na May Tangkay
Papel na PansalaGwantes na Matibay sa Kemikal5
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.
Mga kailangang kasangkapan:
Acetic acid (glacial)Embudong Salamin na May TangkayPapel na Pansala
Hurnong pantuyoMga Materyales
1- 75 partsPlaceholder
Mga Kinakailangang Kasangkapan
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