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Author: Subject: MEKP from butanone-containing solvent
TacosNitrate
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[*] posted on 9-9-2016 at 10:34
MEKP from butanone-containing solvent


Hi everyone!

So:

I have about 2 liters of mixed butanone-isopropanol-ethanol solvent and i need to remove the methyl ethyl ketone (butanone).

I was thinking if it was possible to remove it by converting it into MEKP using an excess of Hydrogen peroxide and acid catalyst so that all of the MEK would be converted (and obivously recovering it to blow something up >:D ) so that it would form and insoluble layer that can be removed...

I really dont have a use for butanone at the moment, and i think that the MEKP would be somewhat more useful, since i love explosions.

The only problem that i encountered and that i quickly solved was the catalyst, since i could probably use HCl instead of H2SO4, because that would form a concentrated solution of peroxymonosulfuric acid that would probably destroy the alcohols....

Do you think that it it could be possible?
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Metacelsus
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[*] posted on 9-9-2016 at 16:37


1) MEKP would dissolve in the other solvents and not form a separate layer.
2) Peroxide will probably react with the other compounds present.

You could form the bisulfite adduct if you want to remove the ketone.




As below, so above.
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gdflp
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[*] posted on 9-9-2016 at 17:35


Quote: Originally posted by Metacelsus  
1) MEKP would dissolve in the other solvents and not form a separate layer.
2) Peroxide will probably react with the other compounds present.

You could form the bisulfite adduct if you want to remove the ketone.

He's already gotten that advice. http://www.sciencemadness.org/talk/viewthread.php?tid=68973#...

Wholeheartedly agree with both of your points.




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PHILOU Zrealone
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[*] posted on 10-9-2016 at 00:57


You could add hydrazine to make a hydrazone and then an azine... then recover the hydrazine and MEK (butanone) by hydrolysis in acidic media.
H2N-NH2 + CH3-CH2-CO-CH3 --> CH3-CH2-C(-N-NH2)-CH3 + H2O
CH3-CH2-CO-CH3 + CH3-CH2-C(-N-NH2)-CH3 --> CH3-CH2-CO-CH3 --> (CH3-CH2-)(CH3-)C-N-N-C(-CH3)(-CH2-CH3) + H2O
(CH3-CH2-)(CH3-)C-N-N-C(-CH3)(-CH2-CH3) --H(+)/H2O--> H2N-NH3(+) + 2 CH3-CH2-CO-CH3

Excess hydrazine could be catched by complexation from Ni(NO3)2, Zn(NO3)2 or Co(NO3)2 (forms an unsoluble precipitate). Then filtration.
Excès complexing nitrate will be left over by distillation of the MEK.

Isopropanol and ethanol are inert towards hydrazine...so a first distillation step will take the ethanol and isopropanol away from the azine...eventually with some excès hydrazine.
Isopropanol and ethanol are inert towards the complexing nitrates and will even favor the precipitation of the complexes.

Beware of the complexes they are energetic so filtrate before submitting to distillation to avoid heating them...
Pink Ni(N2H4)3(NO3)2, white Zn(N2H4)3(NO3)2 or peach Co(N2H4)(NO3)2 may go bang with loud report if heated dry and confined.

[Edited on 10-9-2016 by PHILOU Zrealone]




PH Z (PHILOU Zrealone)

"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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