Author Topic: Baal,Al/Hg/Nitro, & a 55gal drum.....  (Read 5407 times)

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baalchemist

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Baal,Al/Hg/Nitro, & a 55gal drum.....
« on: January 21, 2002, 01:49:00 PM »
Baal came across a man on the roadside the other day, selling all different kinds of containers. After careful consideration, Baal left with a food-grade,55gal drum, w/a locking lid device, & lined with a chem-resistant coating for a mere $7.00. First a hole was drilled in the lid and a 3/8"brass fitting was installed and hooked up to an air compressor and filled with air to 200psi to test pressure capability. Brass fitting was then topped off with a 175psi poppet valve. Into the drum went 20L>MeOH,400g>Al foil chunks & 200g>thin Al flashing cut into 1/4" strips, 600mg>HgCl2, this was stirred with a cordless electric drill fitted with a home-made stirrod & paddle for about 5 mins. Then another solution consisting of 500g>Ketone, 400g>Nitromethane, & 500ml>MeOH was prepared and ~150mls of this was added to the drum and stirred for ~2 mins. Now the MeOH was becoming more gray & amalgamation was present, this was periodically stirred for a period of just a few short mins. The bubbling pace was picking up, and now at about the 15 min. point, the rest of the Ketone solution was quickly dumped in. The lid was then quickly affixed to the drum, it was then sealed with the locking device and a nylon safety strap was wrapped around the drum lid for extra safety(in hindsight it wasnt necessary). A garden hose provided cold water flow across the top & the drum was then periodically "rocked" over the next hour to help with the mixing. During this time, the 'poppet valve' only went off twice for a second or so. The drum was then set atop 2
hotplates set on medium and it was periodically 'rocked' over another period of 2.5 hours, at which time the hotplates were removed and the drum was allowed to cool for a bit before the lid was removed. A 15L>35%NaOH solution was quickly prepared using bags of ice in order to keep the heat down, and 15L>Toluene was added to the drum and then stirred overhead on high. The NaOH was then added slowly and this whole shebang was stirred for 1 hr. at which time it was allowed to settle into its 2-layers. The top Toluene layer was siphoned off into a small plastic garbage can containg 7L of brine, this was stirred for 10 mins then allowed to separate. The top Toluene layer was siphoned off into another garbage can containing 7L>H2O, stirred for 10 mins, Toluene layer was siphoned off into garbage can once again. Then ~1/2kg>Dried MgSo4 was added to the Toluene and stirred for 5 mins, this was then allowed 20 mins to settle. Baal then went to prepare his 'Battle gasser', which is a modified 2-gal. plant sprayer. Then to the dismay of Baal, he discovers that he needs more Hcl than whats on hand. H-store opens in 4 hours, time for a quick nap.
More to come soon...... 

GODISNOWHERE

baalchemist

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #1 on: January 21, 2002, 08:46:00 PM »
Well Baal, now being equipped with a fresh gal>Hcl, pours it into the gassing apparatus. The dried Toluene layer was siphoned off into a 5gal bucket, and a wad of Al foil(~50g's) was tossed into the Hcl in the gassing rig and the lid was quickly replaced. Within ~1 min gas was beginning to evolve, and the Toluene was briskly stirred with the glass gassing wand. The gasser was charged with a couple more wads of Al foil to finish off. The bucket contents were now resembling a VERY large coconut slurpee, and Baal promptly stuck the probe from his immersion cooler into the slush. Within 1 hour, the precipitation stopped, this was then filtered on a giant Buchner. The Toluene was gassed once again, chilled, filtered and added to the first gassings' yields. After drying, the grand total in yield
came out to 467g>MDMA Hcl. Baal thinks that an epic 1000++g'er could happen with this setup, we'll soon find out I'm sure.  8)

GODISNOWHERE

RoundBottom

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Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #2 on: January 21, 2002, 09:20:00 PM »
wow.  is there an icon for bowing down?  congrats.

have you had a chance to look at the inside of the drum to see if there is any damage to the lining?  any idea what the drum used for before this?

i learned a thing or two from charlie dontcha know.

yellowjacket

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Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #3 on: January 21, 2002, 09:22:00 PM »
holy shit...

marijuana is the flame, heroin is the fuse, LSD is the bomb!

noj

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #4 on: January 21, 2002, 09:25:00 PM »
Very well done! I really liked that!

crucify the ego before it's far too late
and you will come to find that we are all one mind

Dr_Sister

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Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #5 on: January 21, 2002, 10:34:00 PM »
You da man, Baal! Fuck wow!

couple questions, curious why you choose to run the rxn under pressure, could it not have been run with lid off? or were you trying to increase the MeOH BP? Do you think it boosted yeilds?

How viscous was the rxn before the toluene addition, i'm wondering if the solvent volume could be reduced?

When the releif valve went was there a spray of reactants?

featly done amigo 8)

7.10.01

yellowjacket

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #6 on: January 21, 2002, 11:54:00 PM »
I don't mean to sound like grandma, but be careful! That is a lot of drugs. My friend was recently sent up (3 yrs) for cultivation. He had been growing a pound here and a pound there for years no problem, and then he scaled up pretty drastically, got cocky. The money got bigger, more people got involved and someone dropped the dime. I have found your posts invaluable so far, so stay free!

marijuana is the flame, heroin is the fuse, LSD is the bomb!

Vibrating_Lights

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #7 on: January 22, 2002, 01:47:00 AM »
Pressure reactions are great they keep your MeAm in the solvent where it needs to be.  i bet the ammount of nitro used could be cut down in such a reaction.
VL_

hest

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #8 on: January 22, 2002, 05:13:00 PM »
-----------------------------------
and a wad of Al foil(~50g's) was tossed into the Hcl in the gassing rig and the lid was quickly replaced. Within ~1 min gas was beginning to evolve, and the Toluene was briskly stirred with the glass gassing wand.
------------------------------------------
Why are you making H2 instead off HCl?? or is it just my reading and understanding there is bad ??

Goodtimes

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #9 on: January 22, 2002, 08:29:00 PM »
Interesting read Baal........

Stay safe......

;)

One more thing... what color was your tolly before gassing???

"The gods are too fond of a joke."  (Aristotle)


LaBTop

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #10 on: January 23, 2002, 03:14:00 AM »
Next step: for real men, the biker method.  :P

Take 10 beer barrells, the alu alloy type one.
Roll your alu flashing in neat little rolls, so they fit in the fill opening.
Dump the whole shebang in ( btw, a WHOLE LOT less solvent, and a LOT more alu/ketone/nitro, a pinch more of Hgsalt, and screw the original lids back on.
Dump barrells in oil bath, 55°C.
When outer hull is same temp as oilbath, take out and rig up to 5 shaker motors.
Shake the hell out of them for a few hours.
If you really wanna know a bit more, rig a pressure meter in the fill openings.
Then stop shaking (you?), and proceed as usual. LT/  8)

WISDOMwillWIN

Vibrating_Lights

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #11 on: January 23, 2002, 04:26:00 AM »
Again why the h2 instead of the hcl agreed that H is the definition of acidity but will it make crystals.  does it form the hydronium salt instead if so is it prefered.

Sektor7G

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #12 on: January 23, 2002, 04:37:00 AM »
Well i think you can officaly call that large scale!

LaBTop

  • Guest

baalchemist

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #14 on: January 23, 2002, 10:04:00 AM »
Thats uncanny you mentioned that LabTop, that was my whole inspiration in a nutshell. The ol' biker speed cook story, with the barrels dumped into a creek for cooling, ah yes...

The Toluene was clear prior to gassing, as always. Gassing those 'colored' toluene solutions are a no-no, too dirty to risk it.

GODISNOWHERE

zooligan

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #15 on: January 23, 2002, 04:54:00 PM »

Gassing those 'colored' toluene solutions are a no-no, too dirty to risk it.




Agreed.  Wash that tol w/sat bicarb (if necessary) until it cleans up, then gas.  Or A/B it again.


"No one can build his security upon the nobleness of another person." -- Willa Cather

Rhodium

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #16 on: January 23, 2002, 05:09:00 PM »
Why cannot anyone vacuum distill their freebase? Even if the amine solution is clear, there is still dimers and other impurities left.

zooligan

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #17 on: January 23, 2002, 08:51:00 PM »
At that quantity, it would certainly be feasible to vac distill.  I believe the reason most bees don't is because the mechanical losses in the glassware would make a significant %'age of their yield go away.  Also, most folks are led to believe (I think) that freebase is delicate and any additional operations will decrease yield and produce additional dimers and such by degredation of the amine.

Just guessing...

z


"No one can build his security upon the nobleness of another person." -- Willa Cather

Rhodium

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #18 on: January 23, 2002, 09:06:00 PM »
It doesn't make sense to not distill, as the "mechanical losses" (as in you losing product weight) is mostly just the removal of impurities.

Osmium

  • Guest
Re: Baal,Al/Hg/Nitro, & a 55gal drum.....
« Reply #19 on: January 24, 2002, 12:07:00 AM »
I personally distilled freebase from an Al/Hg reaction, after cleaning it up by an A/B, at the 40g scale with standard non-microscale glassware. Losses were less than 3%. When doing this with more than 100g the losses will probably still be the same weight-wise, so you lose less than 2% in that step. But most bees consider that loss to be similar to $$$ thrown out of the window, which is sad and makes them cheap asses.

Live long and Prosper.