Simple steam distillation of P2P

OrgUnikum

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Adding Potassium Carbonate solution to the flask with the dirty P2P is a very bad idea and makes absolutely no sense except one intends to kill a lot of P2P on purpose. P2P is highly succeptible to base catalyzed autocondensation, say the P2P condenses with itself forming a polymere, in the extrem it turns completely to the infamous "red tar" otherwise the red goo is well known, or pink to dark red discolorations.
P2P is much more stable towards acids.
If you want to raise the boiling point of the water in the flask use table salt.
Also tilting the flask with the P2P by up 45 degrees or even more if you use a long-necked flask (recommended) helps to prevent water splashing into the condenser in case of hard "bumping" or too much steam. The bumping can be completely omitted when the P2P flask is heated not from below but only from the sides (bottom third of flask unheated). Many heating mantles have double heating exactly for this, one heating for upper part, one for lower part, you use both for quick heating up and only the upper part in distillation which avoids the bumping. Mostly. Don't tell me you knew this. Nobody knows this anymore. So much got lost in time since the hey-days of chemistry....
 

hacke8

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Hi, sir, if you use acid to purify p2p, which acid is the highest? Sulfuric acid 98%, hydrochloric acid 37%, oxalic acid solid, phosphoric acid 85%) This is the reagent I have. 2L steam generator flask, 1L P2P flask, how many dirty P2P can be added in such a combination? Water vapor distillation is really a painful thing.
 

hacke8

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Dear chemist, I don't have potassium carbonate. Can I use sodium hydroxide solution instead? Is the proportion the same as using potassium carbonate?
 

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You cannot find potash? Did you consider switching to binge watching porn instead of making drugs as hobby? And have you tried to switch it off and on again? Da brain?

But yes you can use NaOH. Any hot base will polymerize a good part of the P2P, makes no difference actually.
 

Manisj@1290

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Dear sir,
I am confused for this distinction process Do the P2P and potassium carbonate solution also have to be heated, or does distillation start with water steam only?
If heat the solution of P2P and pottasium carbonate solution than what's is the temperature of this
 

G.Patton

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Hello. You need to boil both solutions.
Heat until the boiling point is reached.
 

Manisj@1290

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Hello sir G.Patton
Can I make methamphetamine without purifying P2P?
 

hacke8

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Of course, but it will affect the output. When there are more impurities, the reaction temperature will rise.
 

TheNut22

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Can someone help me with this problem: I have purified my P2P with acid/base purification, and now it is clear, honey smelling and golden yellow oily liquid. So now I have pretty pure, but impure P2P, because I haven't distill the half of it. The other half (~ 28 g) is now in steam distilling. I have a problem, that when I put my undistilled P2P in the fridge, it sill will precipitate some thick oily-like pieces. Are those particles impurities? When I heat that impure P2P, those particles will dissolve in my P2P. So, can I just put my impure P2P in my fridge. Let it be in the fridge for some hours, and filter those oily particles out, or are those part of my P2P? In the beginning of washing my P2P, when I put base solution in, almost the whole P2P went into a thick, doughy mess. I washed it a total of six times with about 12% hydrochloric acid solution, resulting in a clear golden yellow P2P, from which I removed the xylenes.
So, what can I do about those "particles", because I want to try Leuckart with just a little bit of my undistilled P2P to see if it works this time, because my P2P is P2P now, and it is pretty pure without distilling. It is totally clear in room temperature.
 

G.Patton

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Hi. AB extraction is useless procedure in case you want to carry out steam distillation.
 

TheNut22

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I just want to do everything as good as possible. Following Festers book; First do purification, then distillation.
 

TheNut22

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I noticed that when I cleaned the P2P properly to get bright yellow oily liquid from it. Now that I've already distilled some water/P2P vapors, the dropped P2P is absolutely water clear, and it floats on top of the water I think, because both phases are water clear. Is this normal, or am I doing something wrong here. I put 10 grams of sodium carbonate, 28 grams of P2P and about 120 ml:s of pure water in the rbf.
 

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It's strange, cuz P2P has 1.01g/ml density and has to be on the bottom layer.
 

TheNut22

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Well, I think my P2P is in the bottom layer, because the upper layer looks more like water, when a shake the jar a little bit.
The smell is so good! I'm satified. There is a good day or two of work with this half, but this is looking nice!
 

TheNut22

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There where just little bit of xylene, and I removed it and now the distillate is cloudy, like it's supposed to be, peace!
 

TheNut22

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This is important to me. Can someone help me with this, please?
Can I use potassium metabisulfite to make P2P bisulfite adduct, and then purifyi it with IPA.
Then use potassium carbonate to free the purified P2P in solution, or is the metabisulfite different kind of game?
OR, is it better to use my sodium tiosulfate (sodium disulfite), and then use sodium carbonate, when it's purified?
 
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