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REVERSE ENGINEERING
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ÌMỌ̀-Ẹ̀RỌ
ÀWỌN OHUN WÍWỌ̀
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.
Ilọsíwájú
1 day
Ìlànà
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.
Àwọn ohun èlò fún ìgbésẹ̀ yìí:
Para-sílẹ́ìnì75 partsÀwọn irinṣẹ́ tí a nílò:
Acid acetic (glacial)
Mangánísì Asítétì
Amóníọ́mù Bírómídì
Òǹwọ̀n ìdọ́gba
Ìkòkò ìṣesí ìfúnpá
Ìyípo ẹ̀rọ ìtutù
Gílásì Ààbò Fún Ìfọ́n Kẹ́míkà
Ìbọ̀wọ́ Tí Ń Kojú Kẹ́míkà2
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.
Àwọn irinṣẹ́ tí a nílò:
Ìkòkò ìṣesí ìfúnpá
Ohun ìtẹ̀ afẹ́fẹ́ ti iléeṣẹ́Ìyípo ẹ̀rọ ìtutù
Ẹ̀rọ Ìwọ̀n Ooru Yàrá Ìwádìí3
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).
Àwọn irinṣẹ́ tí a nílò:
Ìkòkò ìṣesí ìfúnpáẸ̀rọ Ìwọ̀n Ooru Yàrá Ìwádìí
Ẹ̀rọ Ìtúpalẹ̀ Gáàsì 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.
Àwọn irinṣẹ́ tí a nílò:
Sílíńdà Gáàsì Nàìtírójìn
Kọ́nfù Gílásì Onípọ̀n
Bébà Ìsẹ́Ìbọ̀wọ́ Tí Ń Kojú Kẹ́míkà5
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.
Àwọn irinṣẹ́ tí a nílò:
Acid acetic (glacial)Kọ́nfù Gílásì Onípọ̀nBébà Ìsẹ́
Ààrò ìgbẹ̀Àwọn ohun-èlò
1- 75 partsÀyè
Àwọn irinṣẹ́ tó nílò
15- Àyè
- Àyè
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