Technique of manufacturing trifluoro acetic anhydride
A technology of trifluoroacetic anhydride and trifluoroacetic acid, which is applied in the field of preparing trifluoroacetic anhydride and achieves the effects of reducing product loss, convenient operation and good heating effect
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Embodiment 1
[0016] Weigh 200 kilograms of phosphorus pentoxide with a content of 98.20% (mass percentage, the same below), put 189.7 kilograms of it into a clean, dry 500-liter reactor, and introduce 250 kilograms of measured trifluoroacetic acid with a content of 98.5% In the high drop tank. Check that the sealing of each interface is good, and the emptying pipeline of the top of the distillation tower and the receiving tank is unblocked. Turn on the deep well water pump to feed condensed water into the condenser to circulate, start to add phosphorus pentoxide dropwise at a rate of 0.15 liters / minute, adjust the dropping rate to 0.4 liters / minute after 10 minutes, and adjust it to 0.8 liters / minute after 10 minutes. Adjust to 1.2 liters / minute after 10 minutes, adjust to 1.8 liters / minute after 10 minutes, adjust to 2.8 liters / minute after 10 minutes, adjust to 3.8 liters / minute after 10 minutes, until the dropwise addition is completed, close the dripping pipeline valve. At this time, ...
Embodiment 2
[0028] Weigh 210 kilograms of phosphorus pentoxide with a content of 98.15% (mass percentage, the same below), put 199.38 kilograms of it into a 500-liter reactor, and introduce 250 kilograms of trifluoroacetic acid with a measured content of 98.5% into the high-level dropwise Groove, the operation of following process (1) is the same as embodiment 1, wherein in the reflux reaction, the rate of addition of phosphorus pentoxide begins to be 0.2 liters / minute, and is adjusted to 0.6 liters / minute, 1.0 liters / minute every 10 minutes afterwards , 1.6 liters / minute, 2.0 liters / minute, 3.0 liters / minute, 4.0 liters / minute, until the dropwise addition is completed; in the process of recovering the by-product phosphoric acid, add 150 kilograms of metered recovery steam condensate dropwise, and the dropping rate starts to be 0.4 L / min, adjust to 0.8 L / min after 20 minutes, adjust to 2.0 L / min after 20 minutes, until the addition is complete.
[0029] In this process (1), 143 liters of ...
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