Synthesis of P2P by oxidation of alpha-methylstyrene with Oxone (Potassium Peroxomonosulfate) (1kg scale)
- Thread starter WillD
- Start date
Oxone is the so called triple salt and consists of potassium peroxymonosulfate the actual oxidizer, potassium sulfate and potassium disulfate in the ratios 2 to 1 to 1 molar. So obviously there comes a lot of unwanted stuff which takes up a lot of volume as the persulfate makes up only about45% of the total weight.
This matters as you need 11 kg of Oxone per kg of methylstyrene.
Plus iodine, thats not a cheap way - you get 970 g of P2P at best.
But regarding solvent volume: It is possible to extract the persulfate from the Oxone and to use this alone what reduces solvent volume by half rather more. Ten to twenty liter should be enough. Some other approach then "sump all in" for adding reagents could reduce this even further.
The 200 liter are a joke which is caused by extrapolating numbers from millimol in articles to fictive 1kg reactions. It does not work this way.
This matters as you need 11 kg of Oxone per kg of methylstyrene.
Plus iodine, thats not a cheap way - you get 970 g of P2P at best.
But regarding solvent volume: It is possible to extract the persulfate from the Oxone and to use this alone what reduces solvent volume by half rather more. Ten to twenty liter should be enough. Some other approach then "sump all in" for adding reagents could reduce this even further.
The 200 liter are a joke which is caused by extrapolating numbers from millimol in articles to fictive 1kg reactions. It does not work this way.
You need potassium peroxymonosulfate, KHSO5, peroxysulfate is the di-sulfate and has to be converted to the monosulfate first to work. But if you use the di-sulfate sodium peroxysulfate is the better choice as it has a much higher solubility and allows to reduce solvent volume. AFAIK the üperoxy-di-sulfates are hydrolyzed to the monosulfates at temperatures >55°C.
Caros Acid aka Piranha solution made from H2O2 50% and >70% H2SO4 can also be used, thats is the correspondensing acid to peroxy monosulfate.
Caros Acid aka Piranha solution made from H2O2 50% and >70% H2SO4 can also be used, thats is the correspondensing acid to peroxy monosulfate.
- By lalalander
Do we calculate how much Caro's acid to use in relation to the oxidative power of Oxone, or are there other variables to take into account?