How to increase your AP yield...

[ikbendirk]

To some people, the yield of TriCycloAcetonePeroxide is always low. there is one reason to blame for this: the reaction is an equilibrium. the reaction only converts some amount of the recources to the material you want to create, the remainder remains un affected. [in fact, they do react, but at a certain point there will be as much H2O2 & acetone converted to AP, as the other way around, the rxn has reached an 'dynamic balance']

so the reaction would become:
H+
3 C3H6O + 3 H2O2 <=> C9H18O6 + 3 H2O

the K is defined by:
3
[C9H18O6][H2O]
K = ----------------
3 3
[C3H6O] [H2O2]

This means in normal terms:
to increase your yield; increase the concentration of precursors [H2O2;C3H6O], or decrease the concentration of your products [C9H18O6;H2O].

this finally explains why using a significantly higher percentage H2O2 increases your yield greatly; there is less water added, so the concentration of the water is lower; thus the concentration of the products is lower; thus the equilibrium moves to the right.

If you want to increase your yield even more, the thing you MUSTN'T do is add more H2O2, as you only add 30% H2O2 and add 70% H2O, moving the equilibrium to the left. this is the last thing you want to happen.

instead, there are two practical solutions to the problem:

- you add way more acetone. Not all will be used, but it helps to shift the equilibrium to the right. when you're done, you can add more H2O2 if you like, but don’t forget the concentration of water is ever increasing doing so, moving the equilibrium to the left.
-The other thing you can do is decrease the product’s concentration. The water is hard to remove, but the AP is very easily removable. Just filter it out of the solution, and whatever you do DO NOT THROW THE RESIDU AWAY!!! As the AP is removed, the rxn is trying to achieve it’s balance and the equilibrium well shoot to the right, creating more and more AP :cool:

Hope this helped to increase your yield :)

[vulture]

you add way more acetone. Not all will be used, but it helps to shift the equilibrium to the right.

This will have an adverse effect because the AP will start to redissolve in the reaction mixture.

The other thing you can do is decrease the product’s concentration. The water is hard to remove, but the AP is very easily removable. Just filter it out of the solution, and whatever you do DO NOT THROW THE RESIDU AWAY!!! As the AP is removed, the rxn is trying to achieve it’s balance and the equilibrium well shoot to the right, creating more and more AP

Won't work either. The AP already precipitated from the reaction mixture and effectively removed itself from it by doing that. Filtering won't do shit.

K = [C9H18O6][H2O]3 / [C3H6O]3[H2O2]3

One thing that'll work to shift the equilibrium to the right is proper cooling, as the formation of AP is exothermic. However, cooling reduces reaction speed, which is a whole different matter, but not to be neglected.

[matjaz]

K = [C9H18O6][H2O]3 / [C3H6O]3[H2O2]3
We were even told in the school to omit the solid from the expression in cases like this, leaving one with
K = [H2O]3 / [C3H6O]3[H2O2]3.

I'd only keep the AP in the expression to account for the tiny bit of AP dissolved in the dilute remaining acetone (?). Anyway, it supports your point, Vulture. Liquids don't matter much in a gasseous reaction, so don't solids when precipitated from solutions. Filtering doesn't remove the dissolved AP here.

BUT...! What if I add ice water before filtering, thus lowering the solubility of AP in the mix of solvents. Then filter, then... Hehe. Anyone got the nerve to boil the filtered liquor to a high conc again? ;) Shit, dimeric AP would start to form while cooking the soup... :( Unless the acetone would be all boiled off... And added again only after chilling...

Whoa. I'm out of my poor chemistry here... Help anyone?

[a_bab]

Well, when I make AP, I only use 30 % H2O2. What initially is a liquid turns into a clump of AP crystals and some liquid.

Here (http://www25.brinkster.com/uploads777/guest/ap.htm) are some pictures.

Now that's what I would call good yield.

[Anthony]

Hehe. Anyone got the nerve to boil the filtered liquor to a high conc again? ;) Shit, dimeric AP would start to form while cooking the soup... :( Unless the acetone would be all boiled off... And added again only after chilling...

Why would you add more acetone after boiling?

Anyway, excluding AN based explosives (and similar), AP has got to be one of the cheapest and most easily prepared explosives going. So why worry about that last 1-2% dissolved in the reactants?

Squeezing out the last few drops efficiency wise is worthwhile when something is either very expensive, or you're producing it in large quantities.

You only need a few grams to make blasting caps...

[Ibanez_90]

Is it safe to filter AP more than once? I mean, everybody seems to throw a way the liquid part, what haven´t form to solid AP...

[NitroKaBooM]

Well.. Some years ago I made many pounds of AP and with great results! My advices are:
1- Use 30% H2O2 (3% still works but with very low yelds)

And, despite many other people, I've found that:
2- Pure H2SO4 gives higher yelds then HCL, but I suggest you to keep your mixture *cold* while adding the acid!
Hope this can help

[knowledgehungry]

Well.. Some years ago I made many pounds of AP and with great results! My advices are:
1- Use 30% H2O2 (3% still works but with very low yelds)

And, despite many other people, I've found that:
2- Pure H2SO4 gives higher yelds then HCL, but I suggest you to keep your mixture *cold* while adding the acid!
Hope this can help

I hope that you didn't make these "many pounds of AP" at one time. If you did you truely have no idea how lucky you are to be in the land of the living.

I should just put this as my sig because of how many times I have been forced to say it:mad: , if you make large amounts of AP it is only a matter of time until you have an accident and you die.

[Cobalt.45]

I cringe every time I read the same things in re "AP". Yes, 30% H2O2 is better than 3%. Yes, H2SO4 and HCL will both get the job done. Yes, keep the solution cold. Yes, it's sensitive. Etc., etc., etc...

The subject should be locked unless there's something new or constructive to be added, IMHO.

Last time I dreamt of making it, I added a drop of red food coloring. Turned it pink.

Pitiful that this is the only "new" thing having to do with the stuff that I know of. I promptly used it, so I have no idea if the food coloring effects the compound after about three hours, so don't do it unless you're into pain (possibly).

[nbk2000]

The problem is with people who can't be bothered to UTFSE and expect a spoonfeeding, not with the thread.

The thread will remain open as there is always the off-chance someone will come up with something new.

[SafetyLast]

I don't even know why I'm bothering to post to this mundane and repetitive topic, but once upon a time when I ran out of my usual 31% pool HCl I used about twice as much of a toilet bowl cleaner called "The Works" which is about 15% HCl. The result was my AP was light blue when it was filtered. Now mind you this was years ago when I was KeWl and didn't care much as to what other chemicals could have been in it that might have reacted and contaminated my batch. "cringe"

When the filtrate was washed with a bicarb solution the blue coloring disappeared.

Maybe a few an acid indicator such as Methyl Red could be added to the soln. to indicate the presence of the acid, when it is neutralized with bicarb the color would disappear.

[knowledgehungry]

The biggest myth about AP is that you need to neutralize all the acid, organic peroxides are more stable in an acidic enviroment than a basic one. The best thing is to rinse the AP with water several times, andmaybe a small amount of sodium carbonate to netralize some of the acid(so your AP is not Hydroscopic or corrosive). You do not want it to be basic.

[sparkchaser]

The last time I dreamt of making AP, HCl acid would have been used. After a good filtration I was thinking of adding a little bicarbonate to the filtrate. I was thinking that neutralizing the acid (slowly to prevent overheating in an ice bath) would precipitate a little more.

In my mind's eye, I saw a sudden increase in suspended particles that didn't float on water after final filtration the way that TATP would. These particles were exceedingly fine, and much less sensitive to heat and shock than TATP. Upon ignition, however, the deflagration was still very violent. With containment, detonation occured.

Any ideas on this mystery particulate? Could it just be TATP that's less sensitive because of the fine particle size?

[knowledgehungry]

Smaller particle size definitely will reduce the sensitivity of AP, but it could be DPPP ;) :p