max yield for CTAP

[Purple Fire]

I was wondering, what is the maximum yield anyone has ever got for AP? Is keeping it really cold the most important, or is it the concentration of the reagents?

Also, I have just got hold of some 50% H2O2, if I use this with conc. HCl and with 100% acetone, will I end up with a reaction thats going to be INSANELY hard to control? Would diluting something be the best option? (i was thinking probably the catylist).

The over all goal that I have in mind is producing a 100% yield of 100% CTAP, no dimeric at all. Im thinking that this is probably highly unrealistic, but how close has anyone ever got? Does everyone here usually settle for a moderately good result as opposed to spending a little extra $$$ and a little extra time etc?

<small>[ June 26, 2002, 06:44 AM: Message edited by: Purple Fire ]</small>

[andreas]

Whell as the reactants are so cheap I think it isn't worth the effort.
But I have gotten up to 55% molair yeild.
The most important is to keep the temp., both for yeild and the trimer form, down and with such concentrated stuff that's rather difficult to do.

[DBSP]

If you dilute the first half of the catalyst it shuld be controllable.

The best yield I have gotten with any conc and ratio is, 200ml of 35% H2O2 300ml of acetone and then 50ml of 30% HCl. This getts me 130g of AP. I know that there isn't as much acetone as it is supposed to be but it seemes to work the best with these ratios. I haven't done any calculations of the actual yield but I might do that soon, Has anyone got the TCAP chemicsl formula?

[ALENGOSVIG1]

Dilute your H2O2 to 30%. Ive used higher oncentrations and the yeild doesnt seem to improve much. When using 60 ml 30% h202, 48ml acetone, and 5 or 10 ml (I never measure the catalyst) of 28% HCl I get 20-25g of AP.

[kingspaz]

DBSP, i think the reason the yields go down when the acetone level is higher is because AP is soluble in acetone. maybe if you used the higher acetone amount but diluted the solution with ice cold water before filtering any AP in solution would precipitate and the yield increased.

[Purple Fire]

Just made some AP with Alengosvig's ratios. I diluted my 50% H2O2 down to 30% and diluted my conc. HCl down to 30%. Brilliant!!! The whole reaction never got above about 2 degrees C and within an hour, I have a nice thick layer of precipitate at the bottom of the jar :D Looks like it will be a higher yield than I expected, we will see when I have washed and weighed it in a few days.

<small>[ June 27, 2002, 07:34 AM: Message edited by: Purple Fire ]</small>

[Purple Fire]

WTF??? When I checked it this morning (about 7 hours in the fridge) there was no liquid!!! None, all gone. All the liquid was replaced by a fat layer of wet crystals. The container had a square of paper over the top, so I'm fairly certain that very little had evaporated. I have never had AP do this before, there should be a layer of liquid shouldn't there? Or, does this mean that the ratios were perfect and I have one hell of a yield of AP? The whole thing still reeks of Acetone, so there must be some left over...

[ALENGOSVIG1]

When i make AP, theres always a big mass of crystals and very little liquid after the reaction.

[mr.evil]

When i make AP with 30% H2O2 the crystalls rise up, and come out of the beaker!! They are also very very fine, just like powder.

[Purple Fire]

mr.evil - NICE!!! :D what are the concentrations of your other chemicals? My crystals (this time and normally) are big and fat, all stuck together in a block.

Overall I think I'm very happy with the yield for this batch, thanx for the advice people, I think I'll make this my standard "recipe" from now on :) On a similar note, I was trying to think what I will do with all this AP, I hadn't really planned anything, but a friend just got me a jar of the stuff in shotgun catriges, this is double base smokeless isnt it? I flicked through the "Makeshift Arsenal",and spotted his method for AP putty, does mixing it with DBSP really provide enough confinement for detonation with no casing at all? or will the outside burn and the inside detonate?

<small>[ June 28, 2002, 06:15 AM: Message edited by: Purple Fire ]</small>

[ALENGOSVIG1]

That has been talked about many times. Search the forum! :mad:

[Controlled Chaos]

I used ALENGOSVIG1's recipe letting it sit for 6 hours under 3 degrees Celsius. My yield was under 5 grams. How long do you let it react to obtain the 20-25g yields?

[Cobalt.45]

The reaction progresses very slowly, the closer to 0C you get.

You might need to wait 48 hours or more at those temps.

[Controlled Chaos]

Thanks Cobalt, I thought that may be the case.

That is just how cold my ice bath achieved. I guess there is no need to keep it that low. The refrigerator should work and form the trimer at a much faster rate.

[Raffikki]

I make AP with HCl and use my own percentages and with in about 5mins the whole mixture turns into hard AP there is about n drop of liquid left in the jar and also rises a bit like Mr.evil said.When I use HCl the AP is like a fine powder and with Sulfuric Acid it becomes Crystals and takes much longer for it to form.

[Controlled Chaos]

Amazing Raffikki. What are the magic numbers?

Also, at those fast rates you may be producing a dimer form. Do you allow your solution to stay cool, or do you keep it warm?

[Cindor]

0162017402290215 you are right, Raffikki is getting the dimer form of AP.

Raffikki, you are probalby using to much acid, what is the temp. that reach you synthesis ?

[Raffikki]

Cindor you are right I use more acid.I still keep it cool.I made a large batch once and couldnt keep the temp low and there was about 1/4 left that wasnt AP.

The AP sounds, looks and feels the same as the original AP method from the Forum.Actually when I started using stronger Hydrogen Peroxide the more AP I got.Ill chek my numbers and put on.O and just so btw 500grams of AP costs me about 1.65$

Why is the reaction so much faster when I use HCl instead of Sulfuric Acid??

[Flamethrowa]

Just drew it out so I could picture it. The chemical formula of the trimer will be C9H18O6.

I've found (as might be expected) that using more acid than might be necessary gives smaller crystals as they form faster. My latest batch seemed less sensitive, perhaps because of this. The temperature was kept around 5 C (my fridge).

In the past, I have achieved a yield of about 20g with 25mL 30% HOOH, 20ml Acetone, and about 7mL 30% HCl. This was left for about 36hrs at 5 C.

[Rbick]

I just made a batch of AP, except a little differently than usual. The yield was pretty amazing, and it only reacted for 10 hours. For the method I used 106ml of 50% H2O2, 200ml acetone and 30ml of 30% HCL. I mixed these using the usual method, except I just quadrupled the H2O2 and the acetone. Only about 20ml of liquid remained after the reaction.

I think the reason as to the speed could be that I used a large amound of catalyst, causing the reaction to happened in half the time. Normally I have to wait about 24-30 hours to get a full yield. The 50% H2O2 can be found at the Hach chemical supplier site for 25 USD. If you only have 35%, just use 120ml instead of 106. The only difficulty I had with using 50% was controlling the reaction and keeping the temp. low.
AP Pics
#1 (http://i164.photobucket.com/albums/u6/pudgedog69/PA010005.jpg)
#2 (http://i164.photobucket.com/albums/u6/pudgedog69/PA010006.jpg)
#3 (http://i164.photobucket.com/albums/u6/pudgedog69/PA010007.jpg)

[nbk2000]

We used to have a member named Phone, and he liked making large amounts of AP.

He's no longer alive, having exploded himself with a kilo of AP while showing off to his friends.

No doubt his last words were 'Hey guys, check this shit out!'.

[DONMAN]

THAT IS ALOT OF AP!!! I would never attempt that much. I never make more than what can react in a film capsule. If what you said was true I doubt your getting the dimer form. Especially if you didn't keep it really cold. What you have is like 300g of really sensitive ap!

[Rbick]

Yeah you guys are right. I wasn't expecting such a large yield, and I definatley don't plan on making this much ever again. Considering I only use AP in my caps (having just recieved some NM), this is way too much. I'm gonna get rid of it today, maybe make a few 500g charges of APAN :eek: I'll post the videos of that later.

[Shalashaska]

Didn't phone die when he went to check it after it went out?
That would make his last words, and I quote;

"FUCK! Hang on a sec, guys." =D