09-25-03 19:22
No 461027
SWIM has a question concerning the NaOH washes in
the benzo wacker. SWIM is using two, 2 liter sep funnels
to execute the benzo wacker, (SWIM doesn't have a 4L
sep funnel) SWID did it the first time no hitches, but SWIM
doesn't rember when last time he did the first 5% NaOH
wash, he shook the sep funnel just a little and the whole
bottom laye (DCM/KETONE) was like clay brown, in the
other sep funnel SWIM didn't shake at all and no
emulsifaction, but the other funnel SWID shook has bad
emulsification, what can SWIM do to get the DCM layer to
look clean ???
-peace
10-01-03 08:35
(Rated as: off-topic)
(Hive Bee)
10-06-03 07:07
No 462887
SWIM just pulled off his first Wacker a couple days ago. Didn't really keep a lab notebook (though he probably should have) but from what SWIM recalls, there was never any real hardcore emulsion formed. In fact, after the NaOH washes, SWIM had to really look hard to see the sep in the layers. (using a 4L Sep funnel).
Curious as to where you're getting "thick" emulsion?
Though I guess I should point out one thing.. SWIM originally fucked up cuz when he first poured the Wacker rxn-mix into the 4L sep funnel (even before flooding w/HCl), half of the really thick stuff poured out into the fucking sink! SWIM forgot to close the stopcock! What a dick! lol
BUT SWIM nevertheless decided to proceed with the washes & distillations since he figured some K should still be salvagable. And in fact, yeild (after losing more then half of the organic shit) was around 55g/Ketone.
(Stranger)
10-06-03 20:21
No 463003
Hopefully this helps,
If you do the Sodium Bicarb washes as described, and REALLY shake it up, you can skip the sodium chloride washes and proceed to your 5% NaOH wash. You should once again REALLY shake the mix up in your sep, then walk away for 20-30 minutes.. upon return, you should have two very distinctive layers as the top layer will be darker, and the bottom layer will be more light brown with each wash.
If you missed some organic material when filtering, you can expect a great deal of emulsion. Filter through 2 coffee filters, and examine the amount of solids collected.
If you have barely anything collected in your coffee filter, expect an excellent yield.
A friend has also found that the addition of Hcl to the water used to flood the filtered rxn mix is pointless and did not effect yield whatsoever. If you disagree, then keep on keep on.
If you scale this Rxn 2.5x and have a 20L carboy handy with a spigot on the bottom, and a 4L sep, you will find that the 4L sep gets 95-99% filled. Unfortunatly, a 4L sep is not big enough for the flooding of the rxn contents, so a 10 - 20L carboy works great, and allows you to do get a nice little workout as you manually shake the fucker in a momentum like circular motion. You need the workout you lazy fucker. Hey, your also going to yield a nice 300-325g of ketone! You just killed 2 birds with 1 stone! Try that 20x in a week!
(Hive Bee)
10-06-03 23:14
No 463034
Swim never found out what was in his sep funnel that
wouldn't really break up (emulsion.) He just proceeded
on anyways, and got his highest MDP2P yeild of the two
wackers he's done. I guess it really didn't have a great
effect on the end product. Welp peace out.