Author Topic: save that HI!  (Read 2339 times)

0 Members and 1 Guest are viewing this topic.

elfspice

  • Guest
save that HI!
« on: March 25, 2004, 07:46:00 PM »
I've been delving into the subject of the mechanism of generating HI, and it seems to me that one should make a lot of effort to recover it with a minimum of steps (steps being sites of mechanical losses and operator error).

When the e/rp/i reaction is done, a lot of HI is generated, and one of the classic signs of a good reaction is that at the end the HI solution is still concentrated HI, almost clear maybe a faint tint of yellow. It seems crazy to me to go and bind up that HI with a base (NaOH presumably) meaning you have to unhook it again later on if you want to re-use it.

So, in our post reaction solution we have a lot of phosphoric acid, hydriodic acid and methamphetamine, which is likely going to be bound up with a proportion of HI and H3O4P as is found in the solution. we would have also some water in the solution. The water and HI would distill straight out of the reaction mixture, so long as the temperature was controlled so as to prevent phosphoric acid from vapourising and coming across as well (below 150 degrees) though obviously, this is an inert element in the reaction, it would be nicer to leave it out, feed it to your flowers ;) the meth obviously can't boil out below the temperature of the dissociation of its salts with HI and phosphoric acid... a lot of people say to boil your post reaction liquid, i say, distill it. Thinking about what would be needed to do this, it's not much either, a metre of vinyl hosing attached to the top of a small flask (the rxn flask probably) with a thermometer to monitor the temperature that is distilling across, and the end dripping into a receiving container (preferably the storage container) - oh and probably good to either blow air over the tube or make it coil through a bunch of water or something similar. Vinyl tubing of about 1m length with fairly high boiling liquids condense vapour effectively enough to be practical. People use vinyl hose all the time with push-pull setups so it must be safe enough to use with boiling HI and water going through it (i was rather surprised to find that i was able to distill a light fatty acid in a vinyl tube... the only things which damage vinyl seem to be boiling aromatics, and probably ketones, aliphatics are fairly benign at below about 80 degrees.)

Then once the temperature in the boiling flask with rxn mixture starts to rise above 127 degrees or not distilling anything anymore or looks almost fully dry, the majority of the HI will be recovered. A pinch of the rp recovered could be added to the container the HI is stored in to keep it as 57% HI until next time :D and subsequent reactions done as HI/rP reactions rather than I2/rP reactions. Saves all that work turning the iodides back into iodine.

HI reactions are much safer to start than I2/rP based reactions because the reaction starts immediately that the ephedrine is added and flask fires are much easier to avoid because the reaction takes place immediately and doesn't need to be prompted with heating. The rP only reacts in a HI/rP reaction when the HI reacts and decomposes into I2 again, so one doesn't need to risk raising the temperature high, as once the ephedrine reduction starts taking place (which just requires enough joules of heat energy to kick off) in an already formed solution of HI, the temperature is already high enough for the rP to continue turning the I2 into HI.

If one had nice little pieces of ground glass thingies, still heads and whatnot, one would take the condenser off the top of the flask and replace it with a still head and attach the condenser to that.. and voila. Then the meth phosphate and red phosphorous solids remaining would be dissolved, gently boiled to clarify and rP filtered and the meth acid/base extracted into the HCl salt.

Obviously it is most important not to let the temperature get high enough to start the remaining phosphorous burning, this should be fine, i think this requires fully dry rp and over 130 degrees to occur so it's probably wise to stop distilling the HI off at the point there is almost no liquid left in the reaction mixture, just shy of fully distilling it as that red phosphorous is nasty, and the whole point of distilling the HI without first diluting it is so that it remains concentrated enough to react later on.

Relux

  • Guest
No heat distill, evaporate instead
« Reply #1 on: March 25, 2004, 11:08:00 PM »
This sounds like an interesting idea. I think if I were to try it I would instead go the route of evaporating under low heat with a vacuum with a cold cold condenser and collection flask. The problem with merely distilling is that the distilling vapor would be mostly water and HCl (from the pseudo salt added) until the solution was at the constant boiling temperature of HI which is above 100C. In other words, it sounds like in either situation you would have to go until dryness and throw away everything distilled up until a certain temperature of vapor started to come over which would tell you you were getting the constant boiling HI (and I wouldn't dry it if not in vacuum). Remaining residue could be freed with basic water and then steam distilled like usual. There has got to be and easier way though...

elfspice

  • Guest
there's an argument for fb rxns
« Reply #2 on: March 26, 2004, 12:22:00 AM »
i have been thinking in terms of ephedrine freebase reactions for some reason, i forgot about that thing about HCl... as far as i am concerned, the HCl ions, although they will not hurt, here is an example of the advantage of the fb rxn - there's no HCl floating around to mess with distilling the HI out of the reaction fluid. freebase makes a lot more sense in terms of the use of a pre-made HI solution which doesn't need so much heat to start reacting (risking damaging our precioussss).

When water with HCl in it distills across you will find the HI is coming across too, remember we are talking about 57% HI solution (if you did the rxn properly) it *fumes* at this concentration (that's why it's so smelly)

oh, and as for the HCl coming across... don't you remember that HCl only goes into the atmosphere when it reaches maximum concentration - and you can see because it fumes. every gram of pseudoephedrine HCl contains 22% (by weight) HCl, so in fact the HCl won't start fuming until probably half the water is gone. Remember also the base (in this case our precious and hopefully transformed aklaloids) takes up some of the acids in the mixture, which will retain one or other of the acids, one would suspect the more soluble salt would be the one that would hold the acid in solution, and in this case i think that would be meth/pseudo.HCl not the phosphate (phosphoric acid is formed out of the phosphorous during the reaction) and not the hydriodide... I suspect the hydriodide salt probably decomposes into it's components more readily than the HCl but i have no proof of that.

Okay, so bearing all this in mind, i think the way to do it is gently bring the boiling temperature up in the distillation, first you will get water and then as the water disappears the HI will vapourise simply for that reason. then once the temperature of the distillation climbs over 130 the water and HI will be distilled and what's left in the boiling flask will be meth/pseudo plus phosphate and HCl ions. The HCl won't distill out with the water until it is concentrated enough, and by then most of the HI is gone, so that's not competing with the HCl anywhere near as much to conjugate with the ephedrine, and also, one should also bear in mind, the amount of water in a reaction is not that much, specifically so that the HI concentrations don't get too low... The material resulting after boiling off all that HI/water solution will be alkaloid HCl salts and remnant phosphoric acid and phosphorous. The mixture will not appear to fully dry, as phosphoric acid is a hygroscopic acid, but you can certainly say there's no water left, it will cease to bubble, though it may look still hydrated. that last remaining water doesn't matter, it's just being held up by the phosphoric acid.

Organikum

  • Guest
The recovery of HI is for sure a good idea,...
« Reply #3 on: March 26, 2004, 08:39:00 AM »
The recovery of HI is for sure a good idea, not at least because I suggested this some time ago already  ;) ....
Some points:
- add some more H3PO4 and boiling stones to avoid getting the meth burned, otherwise you will have to stirr the shit (what might be the best solution anyways).
- whats the fuss about HCl? Some HCl wont hurt in no way so forget about it.
- if you have phosphoric acid it might be worth to consider to let this go and to meke fresh HI by NaI and phosphoric acid - the NaI is left in the flask after basifying so there is no problem in recovering this.


elfspice

  • Guest
phosphoric is a product of the rxn isn't it?
« Reply #4 on: March 26, 2004, 02:17:00 PM »
so what you are saying is if you have NaI and phosphoric acid in a solution, when you boil it down the iodine ions will be released in preference to the phosphorous ones due to the higher temperature of dissociation of phosphoric acid (158), therefore at 127 degrees, the phosphate ions remain in the water but the iodine ions don't.

that makes more sense than risking burning the honey...

don't forget to add a little formic acid to the HI distilled across to prevent it decomposing  ;)

Organikum

  • Guest
No. Thats not what I am saying.
« Reply #5 on: March 26, 2004, 02:58:00 PM »
No.
Thats not what I am saying.


cublium

  • Guest
I personally can't see how using ephedrine...
« Reply #6 on: March 27, 2004, 02:15:00 AM »
I personally can't see how using ephedrine freebase in rx would be better than HCl salt as freebase immediatly turns to HI salt in rx.