AP Experiment

[flashpoint]

Well this experiment is for people that really don't want to post in AP Beginners Guide :) Like myself...I'm experimenting with CTAP and well I've found some stuff to be VERY interesting. Well I did the following synthesis from blindreepers website.

75ml of 25% H2O2
45ml of 100% Acetone
20ml of 30% HCl

Make a salted ice bath, by adding salt to ice so the temperature is lowerd to 5 *C. Place the beaker into the ice bath and add 75ml of 25% H2O2 to the beaker aswell as 45ml of 100% acetone. Wait until the temperature of this has dropped to5 *C. Dropwise, add the HCl keeping one eye on the thermometer to make sure the temperature doesn't rise above 10 *C. If it does stop adding acid and wait till it cools back down. Now I prefer to leave the beaker int he ice bath for an hour then then into the freezer for a day or 2. After this the beaker will be filled with AP. Now i add soem distilled water to break up the AP and pour it into the large container. Then add 250ml of distilled water and stirr around. Then add your base to the solution. It will fizz a lot thats why it's in a big container ;) Once the solution fizzes no more when your base is added it is ready to filter. Filter the solution and keep the residue (white crystals of AP in the filter) You may discard the filtrate. Lay the crystals out onto a plate and leave to dry over night. DO NOT dry in an oven unless you don't want the oven any more!!!

Anyway...I used rocksalt and ice, and rocksalt and ice, like that in layers till my icebath was full of salt and ice, and had the beaker with the H202 and Acetone inside, and I finally got the two down to about 5 *C, and I added a few drops of HCl and I noticed the temperature started to rise since it was speeding the reaction. So after added 1-2ml of HCl, I went inside and forgot about it. I returned 20 min later after forgetting about it...and noticed it was -7 *C, I was estonished that an icebath good get it that cold...I've never let it keep going to see before though...anyway...I started adding it by ml by then, since it was so far from 10*C, and I ended up pouring 20 ml in, in the end I added 30ml of HCl instead of 20 because the reaction hadn't started. I figured it was too cold...so I added another 10ml and well I went inside and returned not 5 minutes later to see the reaction had turned snow white...it was the thickest I've EVER had AP be...so I'm guessing if you let the temperature drop as far as you can...you can possibly still have a Trimeric version of AP and have the highest possible yield....any explanations for this high yield? I've haven't had time to weigh it...I'm about to go wash and strain in after dinner.

[blindreeper]

I am so honoured that someone used my synthesis :) Never expected it.
Maybe my procedure is just awsome thats why so much AP formed ;) Seriously now, I think that if you have never used high conc. H2O2 before and only used 6% or what not you will be amazed at the yeilds. I know I was. I find when I add the acid I pour in 10ml at a time and nothing happens except a few degrees rise in temperature and then keep adding acid. I can do it in about 2 minutes if I am in a hurry. Not the wisest thing to do :rolleyes:
I find I add 30ml acid to that AP mix anyways so it was good you used 30ml. If you leave it in a fridge for a day the reaction mixture will be like a frozen coke type mix = lots more AP.

[flashpoint]

I checked on it again, I left the damn thermometer in it, the acid was eating away at it (because I use a metal probed digital one, I'm going to now use an infra-red thermometer). Usually when I make AP, it isn't as milky as this, its like straight milk, I'm going to let it go at it some more for about 30 minutes, until then I'll add 250ml of 10% bicarb solution and see what' the wet yield is, until it drys.

[blindreeper]

If you can leave it for a day or so before filtering it, the yeild will be larger.

[flashpoint]

I dumped all the acid in at once though, I've never done that before...and the whole time in making it, I've added drop by drop, the temperature didn't move though when I added all of it, and I've always used Baquacil Shock and Oxidizer....don't use just plain Baquacil, it doesn't have enough H202. Anyway, once it got to the -6*C, I dumped alll of it in...this was the second batch I just made...its already got a frozen coke look to it on top...its been a total of 15 mintues, the whole procedure! I can't believe this...unbelievable.

[flashpoint]

I am so honoured that someone used my synthesis

The reason I used your synth, by the way, was the first one I came to that used HCl instead of Sulphuric acid :)

[Blackhawk]

Although the acid actually makes no differance, and seeing as it is not involved in the reaction the type isn't particularly important, what you have to whatch for is that most synths with H2SO4 use ~98% pure while you will only ever get around 30% HCl

[flashpoint]

See that's the thing, I have total access to H2S04, 98%, 75%....my dad owns a pool store...I'm straight with chemicals :)

[Zeitgeist]

Interesting....... I didn't know H2SO4 was used with pools, only HCl for dropping the pH

[flashpoint]

H2S04, we use it on decks as well as Muratic (HCl). We use it to acid etch metals, clean decks...we carry it at the store for various reasons. Don't sell too much of it, just use it mainly.

[Zeitgeist]

I've heard that it's unwise to use 50% H2O2 straight for most reactions, instead diluting it to 25-30% first instead to reduce the heating when it's added to the reactants. That's correct isn't it?

[blindreeper]

Yes that is correct

[flashpoint]

Why is it "unwise" to use 50% H202? I use 27%, so I say its 30%.

[blindreeper]

Because the reaction gets more violent as the concentrations get higher.

[flashpoint]

I see, well are the yields higher, if they are, is it worth taking the risk. That's the real question that I wanted to know :D

[vulture]

It's not true that yields will be higher with higher concentration, the reaction speed will be higher. But, as the temperature goes up, your yield will decrease because the formation of AP is an exothermic reaction.

[flashpoint]

I understand what you mean...thanks :)

[flashpoint]

After straining off the second batch I made...that I allowed to stay over night in the freezer. It almost froze completely, so I added 250ML water, and a few spoonfuls of baking soda, until the neutralizing was done. Then strained it as I said, added some acetone to the pile while it was still wet to aid in the drying process. I forgot about the filtrate and left it in my pyrex on the ground in the garage. I came back notice, the filtrate had more AP in it, which I think came into solution after I filtered the other one...possibly some that went thru the coffee filter, who knows but I took some out with a dowel and lit it while it was wet, it was stronger wet, than my normally dry powder. I'm going to do some tests soon to see.