Antibody2 (Commodore "Mole Bouncer")
10-10-01 21:08
No 222829
      Al/Hg How big is big?  Bookmark   

i've always heard bees pooh poohing Al/Hg because of its inability to scale effectively, what is this? fact or fiction.

case one)
Osmium's thick foil variation reported to scale to one mole rxns sucessfully in 2l glasscool

case two)
doctor??, a bee i used to know who gave me his HgBr2/Al/P2P synth. and it didn't have much detail ei the type of foil, it sounded almost as though he was using a solid chunck of Al to reduce P2P in kg+ quantities, he described a slow rxn that took days to a week, didn't seem to include stirring, think maybe he mentioned sloshing it around a couple times a day.

so anyways with renewed scruitiny of borohyrdides these days its time to reconsider BIG AL/HG. Looking ideas, precedents, modifications to existing rxns all welcome.

I'm thinking that viscosity of solvent will become an issue,possibly retarding ion exchange, neccesitating solvent addition, with Al the size and thickness of coins or maybe long rods that would extend the depth og the rxn vessel, with strong slow overhead stirring, not so much to stir the Al but to prevent suspendsion from settling. And last of all doing it in plastic garbage cans. I realize tyhat work-up will also be challenging but wtf where theres a will a way is soon in evidence.

"All those memories lost like rain..."
 
 
 
 
    Rhodium
(Chief Bee)
10-10-01 22:52
No 222863
      Re: Al/Hg How big is big?  Bookmark   

My opinion is that the Al/Hg with foil does not scale well (due to the exothermic nature of the reaction), but that reactions with Al sheet scales perfectly well.
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-10-01 23:21
No 222870
      Re: Al/Hg How big is big?  Bookmark   

Does the foil work sufficently well in 45-50g batches, or is another source desired?

PB
 
 
 
 
    Antibody2
(Commodore "Mole Bouncer")
10-11-01 00:45
No 222897
      Post deleted by Antibody2  Bookmark   

 
 
 
 
    Rhodium
(Chief Bee)
10-11-01 00:50
No 222899
      Re: Al/Hg How big is big?  Bookmark   

I believe they often use catalytic hydrogenation in those cases.
 
 
 
 
    DiethylEtherMan
(Hive Bee)
10-11-01 02:40
No 222932
      Re: Al/Hg How big is big?  Bookmark   

Dear AB:

Shit, industrial size is not my ball of wax...due to height restrictions, I cannot go too big. However, my grandmother is up to 8x (per MM) with great yields. Using 12L FBF, Sep, and a 1200 alhin condenser...addition in 55 minutes...heat on for only half an hour after reflux calms...let it go for another hour...total time including tone addition is 2.5 hours...or 3 hours, but hasn't seemed to make a difference...

 

If some of us were not so far ahead, the rest of you would not be so far behind!
 
 
 
 
    RoundBottom
(Hive Bee)
10-11-01 02:51
No 222937
      Re: Al/Hg How big is big?  Bookmark   

how about this.  why doesn't each person post their best run for different sizes of glass?  then if one looks promising, we can ask for details or a complete writeup.  i'm very interested to find out what the max a 5L setup can produce.

state glass size, method, addition time, total time (incl addition), ketone, results.

3L 3N FB, std 2x MM AlHg Nitro, 1h 10m, 4h 45m, 50g, 44.5g
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-11-01 03:17
No 222954
      Post deleted by PoohBear4Ever  Bookmark   

 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-11-01 03:29
No 222962
      Re: Al/Hg How big is big?  Bookmark   

How would you define a "good magnetic stirrer?"  SWIP just sent out for his hotplate/stirrer today, which produces 900wtt, sold for $500 new, and should have a 7x9 plate.  Sound adequate?

PB
 
 
 
 
    Rhodium
(Chief Bee)
10-11-01 03:49
No 222970
      Re: Al/Hg How big is big?  Bookmark   

Pooh: Sounds good, I hope the magnetic drive torque is strong also, and you have a  fantastic machine.
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-11-01 03:55
No 222971
      Post deleted by PoohBear4Ever  Bookmark   

 
 
 
 
    Antibody2
(Commodore "Mole Bouncer")
10-11-01 04:31
No 222987
      Allow me to rephrase  Bookmark   

I'm a goof, anyways the more i think about the issue, the dumber i feel about starting this thread.

upon reflection, this is a math problem, one need only quantify known sucessful reactions to hypothesis the question i posed.

i went into my shop and weighed a 30x0.5x0.125" piece of Al 82g with asurface of 37.5 square inches

then i weighed a 30x0.5xwho-knows piece of foil with same surface weighs 0.3g

so the 1st will react 273X slower and all that implys

but it also seems so many other variables come into play that that kind of equation is over simplistic and could use a hand constructng a better way of calculating scalability, or the physics of scaling up takingh into acount solvent ratios, temperature, surafce area of rxn vessel/cooling and of course some idea of where critical mass is in the math.

or even more B&W, how to calculate how to keep a specified amount of reactants within a temperature range by math. can someone help figure that out? that's what i am really asking,

"All those memories lost like rain..."
 
 
 
 
    spric
(Hive Addict)
10-11-01 06:26
No 223040
      Re: Allow me to rephrase  Bookmark   

It has been a while due to lack of proper facilities lately, but scaling up was not tried too much.  In a 6L flat bottom flask with a football shaped stir bar(they work much better than regular bars, eh) 100.0g of ketone processed using a #12 stopper with a 24/40 1m alihn slapped in it.  Yield would vary from 75g to 82-83g after single re-xtal, but never more than that.  That damn condensor would fill half way up with yellowish liquid unless vented, but then of course addition was under 30min..  1meter longer condensors are fucking amazing, a well spent $200.

4:20
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-11-01 06:40
No 223045
      Re: Allow me to rephrase  Bookmark   

Sounds like a experimental method might be best.  If using a set ratio of chems and Al, one could start with a very small rxn (say 10g) in a 1L flask, then double (say 20g) in a 2L flask, triple (30g) in a 3L flask, etc., and observe the amount of kJ given off from each.  Take these numbers, and find the average kJ/g, the mean kJ/g, and plot a graph to get a better idea.  How you would observe the kJ is beyond my knowledge, but for some reason "calorimeter" comes to mind...

So, say if one had a 5L flask, would he/she be able to successfully dream a batch as small as 30g, then work their way up from there?  Would the increase in exposed surface cause problems?  What size/type of condensor(s) would bee favorable if one were to dream 80g in such a vessel?

PB

* spric, I could get ya a 1200mm allihn for $140 new.
 
 
 
 
    RoundBottom
(Hive Bee)
10-11-01 10:26
No 223098
      Re: Allow me to rephrase  Bookmark   

spric, is that ground aluminum foil, aluminum wire, or aluminum sheeting/flashing?

SWIM has ~50mL (~56g) "known good" ketone and is willing to try a slower, thicker Al route, but using MeNO2, and report the results.

can SWIM have suggestions, specifically to amounts of Al, MeOH, HgCl2, MeNO2, suggested addition time, and expected reaction time.

SWIM has 1L, 2L and 3L RB flasks, with 1" and 3" egg bars (the 3" won't fit in a 24/40 neck though), a 1L mantle, the usual gear.
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-11-01 10:36
No 223101
      Re: Allow me to rephrase  Bookmark   

Read the ratios in Post 223099 (PoohBear4Ever: "Re: A Compilation of Documents", Newbee Forum).  Close fit?

PB
 
 
 
 
    RoundBottom
(Hive Bee)
10-11-01 21:24
No 223261
      Re: Allow me to rephrase  Bookmark   

well, that's a 2x MM AlHg Nitro. 

what SWIM is interested in doing is Osmium's ../rhodium/chemistry /osmium.alhg.txt but with nitromethane, like Post 221621 (abacus: "Thick Al and nitro success", Methods Discourse)

someone (rhodium?) had a post with a ratio of Al:ketone:MeNO2, but i can't find it frown

i guess i'll just watch abacus' thread play out for now.
 
 
 
 
    Rhodium
(Chief Bee)
10-11-01 22:31
No 223295
      Re: Allow me to rephrase  Bookmark   

didn't post anything about that at least. Should narrow down your search.
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-11-01 22:39
No 223299
      Re: Allow me to rephrase  Bookmark   

If one was using flashing, what would be the prefered dimensional aspects of the pieces of aluminium?  Just 1" squares, or perhaps a "U" or a "V" shape?

PB
 
 
 
 
    Osmium
(Stoni's sexual toy)
10-12-01 01:20
No 223372
      Re: Allow me to rephrase  Bookmark   

Doesn't matter, as long as they aren't too big to be stirred.
 
 
 
 
    Chromic
(Hive Addict)
10-12-01 02:41
No 223424
      Re: Al/Hg How big is big?  Bookmark   

Comparison:
Al/Hg a la Brightstar:
1L flask, 40g foil, 100g of MeAm.HCl, 80g of MDP2P
Al/Hg a la Methyl Man:
1L flask, 14g foil, 10mL MeNO2, 12.5g MDP2P

So Bright Star's foil reductions is 6.5 times more volumetrically efficient than Methyl Man's procedures.

Diethyl Ether Man, right now you're reacting 200g of ketone in your 12L flask, which seems pretty good... until you realize that you could be reacting about 1000g of ketone in that same flask if you were to use Osmium's method.
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-12-01 02:46
No 223427
      Re: Al/Hg How big is big?  Bookmark   

How does one fit a 3" stir bar in a 24/40 joint? 

PB
 
 
 
 
    PrimoPyro
(Hive Bee)
10-12-01 03:15
No 223434
      Re: Al/Hg How big is big?  Bookmark   

YEAH!

And how DO they get those ships into those little bottles???????
wink

                                            PrimoPyro

I collect synthetic drug precursers. Aren't you jealous? Member: C_F and pyrotek FanClubs cool
 
 
 
 
    fructose
(Stranger)
10-12-01 04:29
No 223457
      Re: Al/Hg How big is big?  Bookmark   

Would it be possible to use a reasonably thick piece of aluminium as your stirring 'propellor'  - the bit at the end of the rod that actually stirs in an overhead set up - amalgmate the Al stirrir chuck in your nitro/MeNH2.HCl blah and go? I'm assuming this is if you want to use overhead rather than stirbar. You could always put your stirbar inside a piece of activated Al tubing and just run it like that. 

anyone tried this?
 
 
 
 
    RoundBottom
(Hive Bee)
10-12-01 05:28
No 223482
      Re: Al/Hg How big is big?  Bookmark   

> Chromic: 6.5 times more volumetrically efficient

ok, i'm sold.  now to learn how to convert the hexane into MeAm.HCl.  fume hood would be nice about now.

> PB4E: How does one fit a 3" stir bar in a 24/40 joint?

you don't, not if you want to get it out again.  someone once said they shaved it down and it fit (mine barely doesn't fit), but good luck getting it out again.
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-12-01 05:34
No 223486
      Re: Al/Hg How big is big?  Bookmark   

Then how do ya stir a 50g dream?  If it would fit, is there really any reason, besides possible breakage of the flask, that one would need to take it out?

PB
 
 
 
 
    DiethylEtherMan
(Hive Bee)
10-12-01 07:39
No 223522
      Re: Al/Hg How big is big?  Bookmark   

Chromic: Yes, I do understand that I could be getting much more out of the size of the glass, however, I do not want to worry about making or aquiring MeAm HCL, or any other form of it. For me, everything I use is totally OTC...I certainly would go the Sheeting method, if I did not have to come up with MeAm.

Oh, and as for the 3in stir bar in a 24/40 joint...it fits perfectly, or at least mine does (3in octogon). It comes in and out of the joint every other day. Unless your 3in is thicker than mine...

DEM

If some of us were not so far ahead, the rest of you would not be so far behind!
 
 
 
 
    RoundBottom
(Hive Bee)
10-12-01 08:33
No 223533
      Re: Al/Hg How big is big?  Bookmark   

well, i don't know if it's thicker, but it's not three inches.  ba-doom-boom.

sorry, i was refering to a 3" egg bar.  my 3" octagonal fits 24/40 no problems.

i thought MeAm could be made OTC from hexamine?  i bought 2 boxes of about 250g each for about $5USD at the surplus store.  hell, that's so OTC it makes my paint thinner purchases look like a freakin' drug deal.  wink
 
 
 
 
    RoundBottom
(Hive Bee)
10-12-01 08:38
No 223538
      Re: Al/Hg How big is big?  Bookmark   

stirring was a real bitch to get going in a 2x MM.  took a while to get it going, but once the amalgamation really started in ernest, it got going and kept going, quite strong.  this is with a crappy thermolyne 1000, and a kick ass 3" octagonal (my 3" round really bites, stick to the octagonal). 

the trick is to find the sweet spot on the flask bottom where the bar spins the freest.  experiment a bit by moving the flask around, you'll find it.
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-12-01 08:44
No 223542
      Re: Al/Hg How big is big?  Bookmark   

We tawking FB or RB flasks?

PB
 
 
 
 
    RoundBottom
(Hive Bee)
10-12-01 09:26
No 223556
      Re: Al/Hg How big is big?  Bookmark   

FB for SWIMs 3L 2x MM.
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
10-12-01 09:47
No 223563
      Re: Al/Hg How big is big?  Bookmark   

Well, guess this bee will follow in your footsteps on this issue.  A 3" octagon stir-bar you say...

Off I go changing my order sheet again, 

PB

* Thanks
 
 
 
 
    pimpmaster
(Stranger)
10-12-01 14:45
No 223632
      Re: Allow me to rephrase  Bookmark   

hey rb  read the procedure written by osmium on rhodium's site better you might find this "Ketone:amine
molar ratio was usually about 1: 2.5-3.5 " and also that he uses 50-60 grams Al :mole ketone.shocked
 
 
 
 
    Goodtimes
(Hive Bee)
10-12-01 18:24
No 223668
      Re: Al/Hg How big is big?  Bookmark   

Sorry Pooh, I misinformed you, looked like the 2.5" egg would have fit into the 24/40, but very wrong, almost didn't get the fucker out...  at least what Swim said...

Lessons learned... very frustrating projects. frown

"I have not failed. I've just found 10,000 ways that won't work." - Thomas Alva Edison (1847-1931)
 
 
 
 
    DiethylEtherMan
(Hive Bee)
10-15-01 08:55
No 224666
      Making Clear  Bookmark   

OK. Today I began a venture to try and use OS Al sheeting method with nitro. Unfortunately for me, the only thing I lacked was the overhead. Which didn't prove to be that much of a nusance, but called for more meoh in the reaction.

I will give the fine details when I am finished but before that I will give some broad details. Suggested by a well known bee here... basically this is how it has gone so far. The ingredients:

86g ketone
61g Nitro
75g al sheeting
1+ml Meoh

First, added the al to a 3L FBF and covered with approx 1L meoh. Added 1.2g HgCl2 and let go for 30 min. Solution turned med grey. After the 30min period, I added 30.5g of the nitro to an addition funnel and set up for reflux on the 3L, and with the addition funnel. I droped, one drop per second or second and a half, the nitro into the meoh/al/hgcl2. This took less than an hour, but I let the reaction run 2 hours...during which time the mixture got exothermic and refluxed fairly hard. After two hours, the reaction cool quite a bit, but still at a slight reflux. Then, into the addition funnel I added the remaining nitro (30.5g) 86g of mdp2p, and approx 20ml meoh. Started this at a very slight drip. The drip was finished in approx 2-2.5 hours. While the reaction only refluxed slightly, as I had to add heat as well. This was all done with a mag stirrer which gave many problems to keeping the mixture stirring. There was much shaking and swirling to try and catch the stirr bar....eventually I found myself adding approx 1.5L to 2L meoh, just to keep the thing stirring for more than a few minutes...At this point the reaction will continue, I'm sure, for an unsepcified time...which at the end, I will give the details. I am under the impression that the reason for the intitial nitro drip is to make availible for the next step, our precious MeAm...which, btw, during my swirling trials, the condenser came loose, and there was an immense smell of MeAm, for sure. The reaction, looks good and sure seems to be doing its thing. 4 hours into the reaction and there are still large al pieces however, it seems as though the majority of it has turned into your typical al sludge, slightly bluish grey.

SO, anyway...I wanted to discuss some further liknesses with this reaction and the typical MM reaction. First, I would like to clarify that the only reason a 12L FBF is used for 200g reactions, is because granny likes to save all that head room, so that basifying can be done in the same flask, therefore leaving begind her the work of trying to get the sludge out of one flask and into another. or into a sep.

Secondly, I would like to take a look at the ratios here for each reaction.

with 150g of al sheeting you can use more or less 180g of tone.

with 150g of al foil you can use more or less (according to MM write-ups) approx 130g of tone...although, I am sure as you upscale, you can use less al as in the sheeting method...only with this bees experience, he has always just added equally to the ratio's when upscaling...never thinking that it is a good possiblilty that when you upscale this rection, that it will probably not need as much al as does the smaller 1x al/hg per MM.

The only real difference between these two, and upgrading each, is the overhead stirrer. I learned that today when trying to stir the sheeting with my magnetic, and realizing that it wouldn't.. I had to add another 1.5-2L of meoh. So, for this 86g reaction, I still needed approx 3L meoh....and in a past 130g reaction FOIL style, I had to use 4L to keep the thing stirring....so the difference is still quite the same....if I had an overhead and wanted to do the foil method, I could definately use less meoh...and I probably wouldn't have to use as much al when I upscale...I imagine, with 150g of al, I could get very close to using 150g of tone using the foil method...therefore allowing me to have a much bigger reaction in a smaller flask...

In my 200g reaction I use 225g of foil, 6.5L meoh...although, the foil could for sure be cut down, just never tried it, and if an overhead was in place, you for sure wouldn't need as much meoh, therefore allowing you very close to the same amounts and volumes as the sheeting method.

Now, I am not trying to pick a fight and shit, I have just now see both done, and both a very much alike, no matter which way you look at it. At this point, I would not be able to agree which is better without getting an overhead stirrer to test my own theories out.

Shit, I got to get me one of those overheads.

DEM

Got another one coming!

If some of us were not so far ahead, the rest of you would not be so far behind!
 
 
 
 
    LaBTop
(Daddy)
10-15-01 10:22
No 224697
      Re: Making Clear  Bookmark   

Why did nobody ever thought of adding the cut amalgamated Alu foil or pieces of Alu sheet/flashing  slowly through a special device to the total reaction mix? That way you can regulate the exothermic reaction with the rate of amalgamated Alu.
"Dripping" in Alu. tongue
It will need some finetuning, to obtain the highest reaction rate per timeframe and amount of Alu.
Eventually you could even try DRIED amalgamated Alu powder "dripping" in.
This seems to me the only way to controll the exotermic attitude of all Al/Hg reactions. LT/

PS: Antibody2, I have scale-ups with Al/Hg in my files which were MUCH bigger than anybody talks about here, MDP2P wise, I will look through them to give yields, if I remember correct it was somewhere near 75% yields with 5 and 20 kg MDP2P batches.

WISDOMwillWIN
 
 
 
 
    sYnThOmAtIc
(Hive Bee)
10-15-01 21:18
No 224861
      Re: Making Clear  Bookmark   

Yea labtop has a point.  Oh and labtop where do you have your industrial scale writeups(other thann the few here)? I have a friend who is movin on to bigger things and would like to test some of your writeups.

I have heard of cooks that used stainless keigs (spelling) with an open top with 10kg+ mdp2p/nitro mix slowly being added while they drink beer and toss in the aluminum at a certain time in the reaction.

Diethyletherdude, why did you use so much hgcl2? That much is not needed. Although if you like to prepare hgcl2 every other week or raise suspicion buying an ounce every month then so be it.
 
 
 
 
    DiethylEtherMan
(Hive Bee)
10-16-01 01:36
No 224960
      Re: Making Clear  Bookmark   

LT, that certainly is a good point. Maybe someone could give it a try here...although, the hard refluxing doesn't much bother me, being that I am using a 1200 condenser..

For me anyway, the reaction still needs an overhead to be able to stir the reaction...this is the only thing that has really held me back from upscaling into the kg range...that and a little larger glassware...I am sure that you could be doing 1-1.5kg kg in 22L FBF with overhead stirring.

Snyth: I am aware that that is an excessive amount...for sure....but it surely seems to help the process progress a little quicker...

Not that I am trying to brag here either...but my grandmother is always getting 100% (not molar) yields...or better. Every single time...

Still havent complete the above reac, but will soon.

DEM

If some of us were not so far ahead, the rest of you would not be so far behind!
 
 
 
 
    sYnThOmAtIc
(Hive Bee)
10-16-01 03:51
No 225032
      Re: Making Clear  Bookmark   

Once you break the 1kg barrier glassware should be replaced. It is expensive, suspicous for 22l flasks and larger. The idea when doing large reactions (5-10kg and up)is disposable inexpensive equipment and speed. You want to get your shit, containers, and stuff. Then cook, crystalize, and destroy everything and all leftovers. And if for soem reason you must abandon it  that you can take your goods out and leave in a hurry without worrying about any of it being traced back to a name. Finding a sale and name for a glass kit is easier than finding out who bought a bottle of water at a grocery store. Like those glass 5gal water juggs at the organic foods market for those who don't trust plastics make great reaction vesselsat about 3 bucks each. Equiped with a powerdrill/overhead mixer with a stainless/copper encased glass tube for condenser ou could bail your reaction if needed or not worry bout your equipment.

100% yields??? Care to elaborate?
 
 
 
 
    DiethylEtherMan
(Hive Bee)
10-16-01 04:49
No 225067
      Re: Making Clear  Bookmark   

How would you like me to elaborate? Send you a video.

For example, my mother just gassed two (8x per MM) reactions. That is, 200g tone used in each. She ended up with 408g xtal. Thats the best I can do.

Also, the honey used is very good, clean stuff.

DEM

PS> didn't mean any wise assedness...its just that I can feel the non-believers whipsering away.

If some of us were not so far ahead, the rest of you would not be so far behind!
 
 
 
 
    Dr_Sister
(Hive Bee)
10-16-01 21:57
No 225377
      Re: Making Clear  Bookmark   

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.

IMHOwink

7.10.01
 
 
 
 
    Antibody2
(Commodore "Mole Bouncer")
10-16-01 22:18
No 225387
      Re: How about this  Bookmark   

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
(Daddy)
10-17-01 03:40
No 225495
      Re: How about this  Bookmark   

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
(Hive Addict)
10-17-01 13:51
No 225756
      Re: How about this  Bookmark   


  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?cool

  I'm going to help all of you cleanse this diseased planet.
 
 
 
 
    Antibody2
(Commodore "Mole Bouncer")
10-17-01 16:44
No 225791
      Re: How about this  Bookmark   

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.smile

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



"All those memories lost like rain..."
 
 
 
 
    LaBTop
(Daddy)
10-17-01 18:30
No 225829
      Re: How about this  Bookmark   

Why not use a 10-gallon fish tank? : You think too small. tongue
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
(Hive Addict)
10-17-01 18:51
No 225837
      Re: How about this  Bookmark   

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
(Commodore "Mole Bouncer")
10-17-01 20:27
No 225860
      Re: How about this  Bookmark   

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
(Hive Addict)
10-18-01 03:44
No 226030
      Re: How about this  Bookmark   

"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
(Hive Bee)
10-18-01 06:03
No 226067
      Re: How about this  Bookmark   

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
(Commodore "Mole Bouncer")
10-18-01 15:48
No 226242
      Re: How about this  Bookmark   

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
(Commodore "Mole Bouncer")
12-22-01 16:28
No 249807
      btw  Bookmark   

experiments using much thicker Al, with only mild agitation failed as AlO? crytals form all over the surface inhibiting further reaction.
 
 
 
 
    LaBTop
(Daddy)
12-23-01 07:50
No 249983
      Re: btw  Bookmark   

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
(Daddy)
12-23-01 08:05
No 249989
      Re: btw  Bookmark   

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/wink
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
(Commodore "Mole Bouncer")
12-24-01 17:57
No 250260
      Re: btw  Bookmark   

LT, one word, Lagavulin. Makes the hair on your chest grow fasterwink.
 
 
 
 
    Antibody2
(Commodore "Mole Bouncer")
01-01-02 07:49
No 251699
      Re: Al/Hg How big is big?  Bookmark   

toluene is cheap, freebase isn't, err o the side of xcess
 
 
 
 
    Chromic
(Hive Addict)
04-21-02 19:37
No 299840
      Sweet. :)  Bookmark   

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.