"MY" MDMA freebase crystallization

[btcboss2022]

Of course you can mix the freebase with solvent before adding the HCL but later you Will need more time to put the mixture at 130C due this solvent will be evaporated, with the HCL from freezer, the freebase cold too and avoiding high temperatures during the addition wont be any problem ;-)

 

[Hank Schrader]

Do you know that MDMA cannot be heated with acids to high temperatures? The product breaks down and is no longer pure MDMA.

 

[bblanco]

Look someone explaining a very interesting method l, which could change your life in so many positive ways and become instead an home living addict wanking literature chemist who can only bitch just for the bitching and hope to get imaginaire credit or such I don’t know.
Even more annoying, are all those bitchy comments fucking up the whole structure of method explaining and interesting comments so you end up getting all confused as your first I have to fill them all and remove the noise in the line.

This person is offering clean product gives you clear recipe Many people are not willing to give for free or do not even know themselves. There are people…. I know…

by the way im not talking personally to someone but in general

 

[Davidrobinson]

It should be ok because you crashed ot out in acetone. More acid just makes more impurities.
Did you get big crystals from pouring the hot acidified freebase into cold acetone?

 

[btcboss2022]

When I did It in past at 120C yes I got Big crystals now at 130C I get shiny powder

Thanks.

 

[Mr Good Cat]

It is called "crystallization of supersaturated solutions". There are 3 main parameters related with the supersaturation rate:
- crystals size
- crystals growing speed
- nucleation of crystal grains

As some point of supersaturation reached, the nucleation grows fast, and crystals simply "don't have an opportunity" to grow big. So it is a powder.

You can see the common graph, describing this relation.

 

[btcboss2022]

I have been recovering freebase from the "dirty" acetone and recovering the acetone too.
I obtained 1L of freebase from around 40L of dirty acetone is a lot of product so important to do It to increase yield.

My method for this:

Evaporate the acetone in vacuum in a rotavap until no more acetone goes down from condenser.

The resulting mixture in the ball is taken out and measured in volume.

Add the same volume of water, mix It and add the same volume of solvent and mix all together.

Add portionwise HCL 37% until pH 2.

Separate layers, the solvent layer could be discarded of keep It to recover the solvent.

Add portionwise a NaOH+water solution to the organic phase until PH 12.

Separate layers, we take out and keep bottom layer and extract with solvent the top layer.

Add this solvent layer to the bottom layer keep It before, dry It, filter It and evaporate solvent to obtain all the freebase remaining in the washing acetone.

;-)

 

[btcboss2022]

Another important point is a well known basic technique that is reducing the temp as slow as possible the theoretically best timing is 1C every 30min honestly I never did this timing and I don't think I will never do it hahah could be a nightmare ;-) In small scale could be done with a programmable hotplate.

 

[Mr Good Cat]

I read yesterday some of the theory of supersaturated solutions crystallization. I've even found a method of the slow heating from starting temperature to desirable, when temperature is gradually increased by 3C per 1 hour. This could really be a nightmare.
Have you ever tried such?

 

[Mr Good Cat]

I tried to repeat this procedure with slow temp reducing. And I'm 100% sure - hotplate doesn't work.
Look, there is a hot surface of the plate on the bottom, and cold air on the top. It means, nucleation doesn't start at the bottom - bottom is more hot, so no chance.
As the result, thin crystal layer is formed fast on the top, and it locks the water inside the solution. Water is not evaporate anymore.
You may reduce T of hotplate down to RT it will not help.. The gel inside is locked. Crystallization stopped.
Then if finally crystal layer on the top is broken, it falls down, and crystallization runs fast and immediately. This means you will not get big crystals.
I tried to cover crystallizer with a kind of cap to reduce air access and keep upper layer warmer, but it doesn't help.

I guess, to achieve big crystals, you need to manage the process of crystallization by some way, to start nucleation on the bottom. And to do this, you need a kind of drying box with adjustable T and heating source MUST BE ON THE TOP!!!

In that case, there is a chance nucleation will start on the bottom.

I guess, a kitchen oven could be fine if temperature is adjustable precisely. But I don't have such one.

 

[Mr Good Cat]

This is intermediate part of this process. Later all watery layer on the bottom turns to a kind of "porridge". Wasting of time. Also such long exposure at high T evaporates some stuff. I lost around 20 gr of 250 gr pure powder.

I have some other ideas. Will try as I get inspiration.

 

[btcboss2022]

I will reply tomorrow with the details of what to do but the method works properlt anyway if you want to find inspiration is ok sure will be interesting to improve.
To tired today sorry.

 

[btcboss2022]

That tip is after arriving to 108C during stirring.

 

[btcboss2022]

Now I'm totally focused in MDMA production and I saw that for MDMA you get more beautiful shards when a very little portion of water is remaining during the crystallization process so the heating temp is better to leave it in 108C possibly less I will test it and update it.
Another point to update is the time of crystallization in acetone I made different tests and when acetone arrives again to -2C -5C no more crystals are generated so the waiting time could be reduced until that moment.
Thanks.

 

[Mr Good Cat]

As I got from your description, we evaporate the excess of water until we get a saturated solution of MDMA in water under the temperature 108C.
Does the speed / intensity of the heating (evaporating) make any difference?
And another question: what is approx volume of this saturated solution ready for cristallization if we are working with 100 gr of MDMA HCL?

 

[btcboss2022]

The solution for 100gr in that case is 750ML.
Intensity of heating could affect the product I recommend medium heating.
Thanks.

 

[Mr Good Cat]

Actually, I was asking about final volume.
For the beginning we have 100 gr of MDMA HCL (that is 120 ml approx) + 630 ml of water.
Then what is a final volume as we reach 108C point?

 

[mocnykutas]

This is what i get

 

[btcboss2022]

From my solution?I don't think so you don't ordered nothing from me 100%. And the stuff of that pic seems just came out from the acetone still must be recrystallized.

 

[btcboss2022]

I don't know exactly I never check the volume at this point only the temp but around 120/150ml I guess.
Temp 108-109 is ok.

 

[mocnykutas]

Crystal made your way with water 1g on 0.7 ml and heat i need only wash IT with acetone and dry and finish

 

[btcboss2022]

My method is not only heat it with water has previous important steps and the amounts are not the same you used.

 

[Mr Good Cat]

I've just finished the heating. Total volume at 108C is around 140-150 ml, that fits with Raoult's law.
Water volume - V
K = 0.52 (for the water)
dT = 8 (temperature increased)
M = 193.25 molar mass of MDMA HCL
m = 100 mass of HDMA HCL

V = m x K x 1000 / ( M x dT ) = 100 x 0.52 x 1000 / 193.25 x 8 = 33.6
then volume of MDMA HCL itself is around 110-120 ml.

For me it took around 2.5 hours to evaporate all the excess of water (from starting 750 ml of the solution) at medium heating intensity. Is it not too slow?

 

[kharpa177]

did you heat your acidified free base with distilled water and give these crystals? could you explain me better?

 

[kharpa177]

Could you tell me how you crystallized your freebase? had to warm up your freebase?

 

[mocnykutas]

Your way form water

 

[btcboss2022]

What amount of product are you using? Seems small crystals.

 

[mocnykutas]

800g

 

[Davidrobinson]

you used 1g to 0.7ml of water?
How much of you product was still dissolved in the water after the 48hrs and 30 minutes in the freezer?
And how long did it take for you to dry them crystals and how did you dry them ?

 

[tweaker2]

this method was not mentioned in this thread so i add it here because many are looking to make those big "champagne rocks" so just put your mdma hcl powder to pot and heat until it melts(140-150)and then set aside to cool and solidify and thats it break into smaller rocks if you want