Author Topic: Al/Hg How big is big?  (Read 6941 times)

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Dr_Sister

  • Guest
Re: Making Clear
« Reply #40 on: October 16, 2001, 09:57:00 PM »
I think you guys are missing what antibody was getting at

rxns in kg+ sizes shouldn't be done in glass, keep the temps well below reflux and you need no condenser, allowing you to use 20, 50 or 205 litre plastic pails or drums. can buy em for less than $20.00 and they will never break. and they don't look suspicious. you could stir a drum full with an electric trolling motor clamped onto the side.

as far as the methylamine hurdle, fuck it!, you don't need it. react you ketone with hydroxylamine in a quik 1.5 hour rxn >> oxime in blistering yeilds >> reduced in Al/Hg with HOAc in yields comparable to whats being posted using nitro and MeAm.

the oxime step will take less time than making MeAM so requires no extra time overall. And this will provide higher yeilds than you would be able to obtain with nitro at the kg+ scale, because low temp nitro has diminished yeilds compared to that world famous joyride of a variation posted by baalchemist.

Bonus! you get a much stronger product MDA/MDOH, makes a bigger smile on everyones face.

IMHO ;)

7.10.01

Antibody2

  • Guest
Re: How about this
« Reply #41 on: October 16, 2001, 10:18:00 PM »
LT - i like the gradual addition strategy, and have friends who have done 100g batchs that way, problem i perceive with it at kg+ scale, is that it will need babysitting conceivably for 24-48 hours (yawn).

I'm right now trying to quantify temp vs solvent volume v al surface to determine what the threshold ratio(s) is going to be, once determined back off 10-15% for comfort margin.

another thought i have is that bits and peices of foil are going to problematic, rather i like the idea of figuring out what surface area your solvent and scale will allow and then use whatever thickness of Al will give you the required mass of Al with that surface.

if these were say 2"x20"x0.0625" sheets that would stand erect in a 20litre pail, you wouldn't even require fierce stirring, you could allow all the Al dust to settle to the bottom and use mild stirring (overhead of course) just to maintain a current of the reactants flowing over the Al bars that are sticking almost to the surface, your reaction would not be impeded by the settled dust preventing ion exchange and your solvent wouldn't get really viscous slowing the rxn down.

Anyone see any flaws in this straegy? other than it might take o couple of days, but who cares because once you assured yourself the rxn was proceeding within its threshold (verfiing your math) you could go on vacation for the weekend and work it up sunday night.

LT- i would love to seee those references, if you get a chance

"All those memories lost like rain..."

LaBTop

  • Guest
Re: How about this
« Reply #42 on: October 17, 2001, 03:40:00 AM »
When I'm drunk, I always get these fabulous ideas:

Imagine a 3meter long glass aquarium you bought, standing in your garage, workshop or living room.
Glue in at 1.5 meter with silicone glue a fitting piece of 8 mm glasswall which reaches 15 cm less high than the height of the other 4 walls.
Place a submersible chemistry resistant pump (cheap, low-speed) in the back of compartment 1, on top of some little glass stand (so any alu dust settling at the bottom will not be pumped to the other compartment), with eventually a small filter attached to the intake side, and a thick silicone tubing to the outlet side, leading back to the bottom of the empty compartment 2.
Fill comp.2 with all necessairy solvents and reactants, up to the top of the dividing glass wall.

Fill comp.1 (with the pump) with your calculated amount of Alu sheeting or Alu flashings, piled up with glass rods between them in the length of the aquarium compartment, to improve fluid flow between them. (No cutting needed, use big sheetstrips to fit in that compartement).
Add just enough solvent in comp.1 to cover the Alu sheets and the pump, and add your favourite Hg salt quantity. Wait until the Alu is amalgamated (or amalgamate it separately before), and start the pump.

More sophisticated chemical engineers will add a potentiometer inbetween the powerline of the pump, to be able to regulate the pumping speed and thus the exothermic reaction temperatures, or fit any sort of electric valve halfway inbetween the pump tubing to regulate flowspeeds.
No stirring needed, pumping will take care of that.
Pumping speeds will regulate the temperatures, you can always place a cooled condenser inbetween the pump tubing, to cool a too vigorous reaction, which I do not expect, btw.

Cover the top of your ongoing spectacle with thick glassplates, place your television on top and enjoy the shows at both. Don't forget the drinks and popcorn. LT/

PS: any of you who understand the danger involved in acquiring chems these days, will start trying to perfect the Alu/Hg routes, the ultimate safe route, besides the oxime route mentioned by Dr_Sister perhaps. If you have sassafras oil, the rest is reasonable safe to acquire. LT/ still drunk.

WISDOMwillWIN

Bwiti

  • Guest
Re: How about this
« Reply #43 on: October 17, 2001, 01:51:00 PM »

  Why not use a 10-gallon fish tank? The rubbery material that holds it together is pretty weak at high temeratures, so use a razor to cut most of it out. Grind or sand the glass the used to be covered by the rubbery material and re-glue it with 'liquid metal', which you can find in the automotive section of Wal-Fart. After it drys/cures, spray it with teflon paint. As for keeping the reaction from getting way out of control, how about the use of aluminum siding? 8)

  I'm going to help all of you cleanse this diseased planet.

Antibody2

  • Guest
Re: How about this
« Reply #44 on: October 17, 2001, 04:44:00 PM »
Now we're talking!

thats a cool idea LT, it brought to mind something resembling a car radiator with cooling fins but instead reaction fins, this is the discussion i had in mind. :)

edit - actually i guess the auto part your idea most reminds me of is a disposable catalytic converter 8)



"All those memories lost like rain..."

LaBTop

  • Guest
Re: How about this
« Reply #45 on: October 17, 2001, 06:30:00 PM »
Why not use a 10-gallon fish tank? : You think too small.  :P
Actually I thought first of using a coffin with alu lining, but that seemed a bit too morbid to me.
And an aquarium is so nice to look at while the reaction is in progress, now you can buy these cute little plastic coral reef fishes, beautifull lifelike painted, and they move up and down when a mild fluid movement is present. I would for the sake of effect throw at least some 50 of them in there. (First lacquer them, so they don't dissolve by the MDP2P)
Yep, such a finned amalgamated alu cooler would be a nice addition. LT/

WISDOMwillWIN

goiterjoe

  • Guest
Re: How about this
« Reply #46 on: October 17, 2001, 06:51:00 PM »
what about using a 45 gallon aluminum trashcan inside a 55 gallon rubbermaid trashcan with a 50ft garden hose attached to the top and strung up a tree to act as a condensor? maybe fill the gap between the aluminum can and the rubbermaid can with ice to help cool down the reaction? 

Sed quis custodiet ipsos custodes?

Antibody2

  • Guest
Re: How about this
« Reply #47 on: October 17, 2001, 08:27:00 PM »
too small? nah. 10gal/40litres be just about puurferct. and the little fish would certainly relieve the boredom of watching Al reduce.

anyways i really think we are on to something, the key to keeping solvent ratios realistic, is to collect the sludge so we don't end of with a reaction with the viscosity of mud. although the sludge would have to extracted.


"All those memories lost like rain..."

Bwiti

  • Guest
Re: How about this
« Reply #48 on: October 18, 2001, 03:44:00 AM »
"i'd be  a little nervous to allow a rxn that size to get hot eneough to require a condenser"

  If anyone here is willing to let it get that hot, then use one or two of those large flourescent bulbs.

  I'm going to help all of you cleanse this diseased planet.

Grouch

  • Guest
Re: How about this
« Reply #49 on: October 18, 2001, 06:03:00 AM »
Does the container need to be perfectly round?  I thought that if it wasn't, there would be 'dead spots' that didn't mix while stirring.



Two wrongs don't make a right, but three or more might!

Antibody2

  • Guest
Re: How about this
« Reply #50 on: October 18, 2001, 03:48:00 PM »
Grouch, i wonder about that too, with a solvent current flowing over a grid of Al almost certainly you would have areas where the current was stronger, consuming the Al faster (maybe collapsing your grid).

might be an argument for vertically oriented Al sheet as opposed to horizontal, as it was consumed it would simply sink into rxn, whereas horizontal orientaion might result in contact between the plates when collapse occurs.

"All those memories lost like rain..."

Antibody2

  • Guest
btw
« Reply #51 on: December 22, 2001, 04:28:00 PM »
experiments using much thicker Al, with only mild agitation failed as AlO? crytals form all over the surface inhibiting further reaction.

LaBTop

  • Guest
Re: btw
« Reply #52 on: December 23, 2001, 07:50:00 AM »
Btw2: after sobering up, my attention fell again on that DrSister post up there.
MDOH seems QUITE interesting ... read Pihkal #114. Specificly his comments, he thinks MDA to be metabolicly altered in the body to MDOH..., so it doesn't make a big difference which one you make.
He talks btw about making the oxime with NH2OH,MDP2P in MeOH with pyridine, don't see that mentioned by DrSister.
But using the OnePot method on his #114 could be an eyeopener in yield boost... LT/

WISDOMwillWIN

LaBTop

  • Guest
Re: btw
« Reply #53 on: December 23, 2001, 08:05:00 AM »
AB2, mix counterclockwise, or do the whole shit in a vacuumed vessel or under N2. Air mixed in seems to form your alu oxides. ( a bit drunk, don't take me too serious now) LT/ ;)  
I don't like Glenfiddich, too sharp, give me Famous Grouse, or better Dimple. Pfuhhf, Black Label also good? Love those softonthetongue Malts.

WISDOMwillWIN

Antibody2

  • Guest
Re: btw
« Reply #54 on: December 24, 2001, 05:57:00 PM »
LT, one word, Lagavulin. Makes the hair on your chest grow faster ;) .

Antibody2

  • Guest
Re: Al/Hg How big is big?
« Reply #55 on: January 01, 2002, 07:49:00 AM »
toluene is cheap, freebase isn't, err o the side of xcess

Chromic

  • Guest
Sweet. :)
« Reply #56 on: April 21, 2002, 07:37:00 PM »
Good going... but do realize that you could squeeze in a lot more ketone if you went with the MeAm Al/Hg, plus you wouldn't have to worry about it generating too much heat and it erupting into a volcano.... just some food for thought.