Perfluoro(4-methylpent-2-ene) synthesis
- Product Name:Perfluoro(4-methylpent-2-ene)
- CAS Number:2070-70-4
- Molecular formula:C6F12
- Molecular Weight:300.05
116-15-4
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2070-70-4
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Yield:2070-70-4 98.43%
Reaction Conditions:
with potassium fluoride;18-crown-6 ether in acetonitrile at 130; under 11026.1 Torr; for 4 h;Flow reactor;Industrial scale;Temperature;Reagent/catalyst;Pressure;
Steps:
5 Continuing Isomerization reactionfor Synthesis of perfluoro-4-methyl-2-pentene in the following steps
Into 500L of solvent- catalyst Configuration Kettle 5 added 24.4kg of anhydrous potassium fluoride, 31.6kg of 18-crown-6 and 200kg of acetonitrile. Start the agitation and mix the system evenly. Open the solvent- catalyst Configuration Kettle 5 to discharge gate valve and adjusted solvent catalyst system into pre-cooling kettle 6 at the rate of 60kg/h. after completion of Dimerization reaction was separated out by liquid-liquid phase reactor separation, dimer into premixed kettle at the flow rate of about 30kg/h. started the stirring, the dimer with solvent - mixed catalyst system were mixed evenly, Open the premixed tank bottom valve, open the metering pump,with the flow rate of 90kg/h the reactants fed to the preheater tube 7, tube was warmed to 130°C(pressure inside the system is 1.47MPa), then for reaction reactants fed into isomerisation tubular reactor 8 , reactants in isomerisation tubular reactor 8 with a residence time of 15min, after completion of reaction reduced the pressure through pressure valve then cooling into Condenser 10. Then separation into liquid-liquid phase reactor separation 11, the lower layer Fluoride into perfluoro-4-methyl-2-pentene reservoir 12, upper layer solvent into solvent reservoir , 13.95% of the solvent pumped back to the premix tank 6 with a flow rate of 57kg/h, in Isomerization catalyst Configuration Kettle 5 of solvent - catalyst system into premixed kettle with a flow rate of the solvent into the of 3kg/h. 5% solvent recovery system to recover the solvent.result: reaction 4h total measured quantity of dimer into pre mixed kettle is 120.4 kg (content is 98.94%),obtained the quantity of perfluoro-4-methyl-2-pentene is 119.6kg, wherein, the content of perfluoro-4-methyl-2-pentene is 98.04%, Perfluoro-4-methyl-2-pentene and hexafluoropropylene residue not detected , content of polymer 0.97% and yield 98.43%.
References:
CN105837398,2016,A Location in patent:Paragraph 0026; 0027
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