hellman (Stranger)
07-31-02 08:09
No 339262
      can steam distilled mdp2p be crystalized?  Bookmark   

If one were to steam distill the post reaction mix from either a benzo or a performic,
do you think we then could crystallise out the mdp2p, if we could meet the temperature requirements????.

Seriously folks,wink

hellman

IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity
 
 
 
 
    terbium
(Old P2P Cook)
07-31-02 08:20
No 339269
      Vapor pressure too low.  Bookmark   

The vapor pressure of MDP2P is too low to get satisfactory results with steam distillation.

What temperature do you think is the melting point of MDP2P?
 
 
 
 
    Osmium
(Stoni's sexual toy)
07-31-02 10:52
No 339320
      You can crystallize pretty much every organic ...  Bookmark   

You can crystallize pretty much every organic compound with liquid nitrogen. But I don't see what the point in doing so is.

I'm not fat just horizontally disproportionate.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
07-31-02 18:45
No 339423
      steam distillation of mdp2p  Bookmark   

Read Post 308131 (Chromic: "Problems", Novel Discourse) to understand why steam distillation of MDP2P is not a good alternative. I've done it before with small batches and don't recommend it.
 
 
 
 
    hellman
(Stranger)
08-05-02 05:39
No 341450
      excellent (mr burns style)  Bookmark   

The Day Everything changed-

chromic:
Cool, that is right  roughy 100ml of water per gram, as per the Raoult's Law , but that can be increased by super heating the steam, to a temperature avoiding decomp of mdp2p, for theorys sake let just say with steam heated to say 140c then you would probably get 1g of mdp2p per 50ml of h20,(I am guessing this, but it should't be that far off)

Osmium
Ok, If what you are saying is correct then the end of vacuum distallation is before us, if we steam distill the dirty mdp2p we will have a solution of oil that should be able to be crystalised by freezing to remove the 10-15% of the impurities,.We can do it with safrole, then hopefully we can do the same fore mdp2p,.

Terbium:
Yes I do, Do you know the boiling point of safrole?-
I will say now more except have a good look at the theory behind steam distillation, again vogels 3rd has enough to get you up to date,.

Why steam distill over vacuum distillation, well, Most of you now all the reasons but this has major implications for every body from the small scale to the large,.

- no fuck it, just dream in your little beds about this,.
And think for yourselves,.
Imagine processing a kilo of mdp2p via conventional vac distaillation, about 60-80 at the pump, the vacuum , the noise, the constant attention, the aaargghhh,.
But with steam, you just setup and then walk away, everything, and i mean everything  can be otc,
God! So yes you would have to use say 7 litres of water for say 200g mdp2p, SO FUCKING WHAT!!!!!!!!

I;ve gotta go, but i will be back,
come on let's see who can get the first mdp2p crystal


!!!!!WhhhhhhoooooooooAAAAAAHhhhhhhh
laughlaughlaughlaughlaughlaughlaughwinkwinkwinkwink

IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity
 
 
 
 
    hellman
(Newbee)
08-05-02 09:34
No 341559
      Sorry, got cut short, dang, public libraries!!!!!  Bookmark   

Sorry, got cut short, dang, public libraries!!!!!
Anyway,

Think about this, then think some more, go to sleep, get up, think some more, and look, you might as well spend the rest of week thinkning about this baby,.

I will not try this, and i will not report back tomorrow,.

-off the bat,.-following to be said with a light latin swing

understand how steam distill works
make big vessel that can boil lots and lots of water
put tube from water vessel in another vessel containing dirty ketone
boil big vessel wih water, make tube from boiling water  vessel submerge into dirty ketone vessel, make condensor, attach the whole lot,.,

I will do a formal write up but imagine the logistics of this....

No vacuum, no hot oils, no fancy lab glass 'BULLSHIT'-If that offends anyone, learn that it shouldn't(smile)

In less than a week, we WILL have MDMA.HCL without the need for any labware, or distillation.

Although i think one of the high benefits is that,
It could be a continuous project, where you could just
have this contraption permanently running, then through in dirty ketone at your request,.

crazy-------

IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity
 
 
 
 
    hellman
(Newbee)
08-07-02 07:01
No 342371
      Results
(Rated as: excellent)
 Bookmark   

Steam distillation:
Distillation of a pair of immiscible Liquids:
When water and a immiscible substance are heated,
boiling commences when the total vapour pressure is equal to the external atmospheric pressure.
Assuming that Dalton's law of partial pressures holds,
each componenent will be contributing the pressure of vapour which it alone would be exerting at the boiling point of the mixture.
Thus is Pw and Pa are the vapour pressures of water and the immiscible liquid then at the boiling point
Pw + Pa + 760mm
and the composiion of the vapour is
Nw/Na = Pw/Pa
where Nw and Na are the numbers of moles of water and the liquid in a given volume of vapour.
But Nw = Ww/18 and Na = Wa/Ma where W is he weight of the substance in the vapour and M is the Molecular weight.
Hence Ww/Wa=18Nw/MaNa = 18Pw/MaPa
and the weights of the two liquids collecing in the distilate are directly proportional to their vapour pressures and their molecular weights.
The advantage of steam distiallation can be immediately seen in the the molecular weight of water is low compared with those of liquids which may be steam distilled
An example of steam distillation is iodobenzene.at the boiling poin of he mixture, 98.2
the vapour pressure of waer Pw is 712mm and that of iodobenzene Pa is 48mm. Subsituting these figures and
the molecular weight of iodobenzene, 204, into the equation, we have
Ww/Wa=18x712/204x48=13.1/10
Thus, for every 13.1 g of waer colleceed, 10g of iodobenzene are obtained.

Distillation with superheaed Steam
Consideration of equation above indicates that the proportion of the higher boiling point componenet in the steam distillate can be raised by increasing the vapour pressure of the component relative to water,.
This can be achieved by superheating the steam
The effect of super heated steam may be illustrated by reference to benzaldehyde, which boils at 178c at 760mm. It distills with steam at 97.9c(Pw is 703.5mm and Pa
is 56.5mm)
and the distillate contains 32.1 percent of benzaldehyde by weight.If one employs steam superheated to 133c, the vapour pressure of benzaldehyde (interpolated from the boiling point-pressure curve)
is 220mm: hence Pw is 540mm, Pa is 220mm, Ma is 106 and
Ww/Wa=540x18/220x106=41.7/100
i.e. the distillate contains 70.6 percent of benzaldehyde by weight, this compares nicely with 31.6 percent with steam at 100c and one atmosphere.
The use of superheated steam has the advantage that less condensation takes place theus obviating the use of supplimentary heat in the vessel containg the substance;
beyong this no advantage ovewr stream used underordinary
pressure will result so long as condensed water is present. If all condensation of the steam is prevented(eg surrounding the flask by a bath of liquid at the same temp as the super heated steam), the higher temp of the superheated steam will result in an increase in the proportion of he higher boiling point component of the distilate.
In practice superheated steam is genberally employed for substances with a low vapour pressure(<1mm) a 100(The mdp2p ketone!).The upper limit of temp will of course be controlled by the stability of the compound.

Notes on Purification by Crystallisation  of Organic substances.(vogels)
1) scratching the inside of the beaker
2) innoculation with a seed crystal, created by freezing a .1ml of the oil of a large surface area
3)cooling the solution
4) Adding lumps of co2
5) Or just do as i did and leave in a ice chest, freeze the fuck out of it, let it warm up for a bit untill crystals form
from the scratching method, then re freezing,.

Preface: 5/08/2002

Yes, I did it, Lil ol' hellman, I think it was prettyobvious after all these years of watching and lurking around that maybee nobody believed this could be done, or maybee ..ahh who cares here it is,.
This is for you all to enjoy,

Whether drugs are the tools to the evolution of man, or to hide our earth bound sadness,
it is for you to decide and moderate
If you can do this(moderate drugs) then you have won the battle, As what is to follow is the final piece to the puzzle,.

From Sassafras to Mdma.hcl without vacuum distillation

My journey began with chinese Sas, the clear waterwhite variety,
from this I obtained sizeable crystals through freezing,.From this I followed the benzoquinone(from hydro+h202+i2) wacker,.
Work up was standard and the post reaction mix was washed wih more care than ususal,.
I assembled a $20/20l stainless seel reaction vessel(Big Cooking Pot), loaded it with 10
litres of water,And placed it on the stove. To the small hole on the top of the airtight lid,
I attached a run of platic tube which ran to the floor, into a 5 liter pyrex bowl resting in
cool water.
Into the pot i dumped the 100 ml or so of dirty ketone,.Resealed and started the heating, until
a vigourous boil was obtained,.
Slowly, the distillation started and distillate dripped at about 3 or 4 drops per second into the
 recieving flask.(I could have increased this)
Periodically i would check the water level, and adjust as necessary to keep the pot as full as possible wih water to minimise condensation,.
My fascination quickly eluded me, retopped the water level, and continued to hang anxiously
around for the next 8 hours,.
After a total of 12 or so hours I could see what i thought was about 60 or 70 ml of clear oil
floating beautifully in the reciever bowl.
Yes chromic you are about right in your calculation, approx 1-2 oil per 100ml water,.
I am tired now, but it was breathtaking as it was a beautiful sight,.

-In hindsight I believe that there was no need to crystalize the mdp2p, I believe its purity was sufficient,.
But i had to try it, next time I wont bother,.
I created a cooling chest by slowly heating a drinking glass 500ml in the oven to about 300c(this can be done, the trick is o do it slowly)
With this heated glass I submerged it ino a 20cm CUBED BLOCK of polystyrene(I was going to ozonate this styrene, but I will leave that to another day)
Into the glass which had cooled-(smile), I poured my Co2/acetone/salt/ slurry, and ino that i placed
my testube containing roughly 50ml clear as water Mdp2p,.
Being not a professional in crystallizing, It took me a while to get a seed crystal to start,.
I furiuosly went through vogels, and realized that letting the substance warm just a little, then scratching it with a glass rod produced the seed that i was after,.
Back into the ice chest it went, and back into the freezer,.
And with 2 hours after that the whole testube was a crystalline solid, WOW,.(or for you american dudes-Neat-)
I let it warm jst a bit drained the oil and refroze,.
So, Yes you can crystalize Mdp2p, but after steam distillation, I don't believe that it really makes that much difference.

I aminated the crystal and got 9g from 10g-It was the same yield as when Vacuum is used
I aminated the steam distilled oil,. I got 8.2g from 10g oil.
But I think the point here is that I have crap technique,.
The yield here is not what is the interesting bit,.
-it is thae fact that this operation was not babysitted,.
-It could be ran unnatended in a remote location, done in multiple reaction vessels, I am am talking like 50 small vessels, all fed by one steam generator,.
Then you are talking big scale,.
think abou that, really think about it,.
In hindsight i could have used superheated steam,to further increase the ratio of ketone to water,.
I honestly believe that you could process say 1 litre of mdp2p remotely
with multiple vessels, in say a week or maybee less, I haven't done the math, but I am sure one of
you guys can,.
Use superheated steam,-
you see I modified the reaction vession by making the whole thing kinda of in situ,.
Normally you would pump steam into the reaction vessel, I created the steam in-situ,.
But Your reacion vessels could be like 100 testubes bound together in a matrix, all with 2 holed pluro
stoppers with say one litre of dirty ketone spread amongst each one, all fed by the one steam generator
With the run off all going into a centralized recieving flask,.

Hellman's Matrix, 0 Yeah I like that,.
And you know what, it will work,.
Imagination, fuck i can really feel it,.
Good luck everyone,.
-you see ladies and gentlebees, fear really can be over run by logic, which really is just a little bit of wisdom seeded byimagination.
Now you should never get caught right?
-imagine having your apparatus in the forest, or in the country,
Just like cooking damper, you could come back after a week to find 1 litre of the cleanest mdp2p sitting in the recieving flask, buried below
the ground,

I would like to thank Placebo for the Hydroquinone Source
Osmium for his Logic behind muliple batches vs increased size labware
Methyl Man, An old Friend, And Kapten, Baalchemist, chromic who have powered the dreams to push the envelope and stand on the shoulders and see further into the dark.
And a special respectful hello to rhodium for archiving the ingredients to this ordered madness.

Caveat Emptor

The end.







wink

IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity
 
 
 
 
    hCiLdOdUeDn
(Hive Bee)
08-07-02 07:20
No 342378
      uhh!! aminated not animated! oh well...  Bookmark   

uhh!! aminated not animated! oh well...

hmmm very nice results. Interesting that you got purified mdp2p via steam distillation...what did it take 12hours?? I can distill that same volume in less than an hour via vacuum distillation.

Interesting and new concept though, more than one way to skin a cat, eh?

Thanks for your contribute...every little bee counts!

hidden cloud

hcildoduedn
 
 
 
 
    hellman
(Newbee)
08-07-02 07:24
No 342379
      Takes roughly 8 hours, because you are only ...  Bookmark   

Takes roughly 8 hours, because you are only getting 1ml of ketone per 100ml of water distilled,.
I also had a lot of condensation happening, which i think slows it down some,.

Cheers though,


IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity
 
 
 
 
    TheBlindGenius
(Hive Bee)
08-07-02 11:46
No 342416
      looking for the answer  Bookmark   

OK, yeah cool.  but, wouldn't it be cooler if ketone from a wacker, which is already about 70% pure, could be purified just like safrole, in a freezer?  Why does the concept pop up so much but no one actually mentions what exact temp it freezes at?  swim could not find the freezing point of MDP2P after searching for 3 hours here, on the net and in some reference books.   Nothing... MDP2P isn't even mentioned.  even when swim looked up by CAS no., in case maybe they used a synonym or something! they like fucking censored it or something. it just ain't there.  Sig-Ald don't even sell it, but they sell MDMA and every other fucking drug!! So does anyone actually know what exactly is the temp the shit freezes at?  If it's higher than -86C, then it can be done without liquid nitrogen or dry ice, ever heard of deep freezers? a little expensive, but maybe worth it?
 
 
 
 
    hellman
(Newbee)
08-07-02 12:47
No 342430
      nobody knows yet!  Bookmark   

I wish i could of measured the temp, but i don't have a -C thermometer,.
On the purification of the O2 wacker, well I think that 75% is too impure to crystallize, there are many methods that could make it work, but I think and i say i think because i do not know that there are many organic Pd complexes that interefere with the crystallisation,.
But yes I do believe it is possible, There are many dual solvent systems, that could make it work, making the pd complex's sparingly soluable in one, and not so in the other, we can only do experimentation with the mdp2p species to find what is suited best,.
I would like to see it done, And I hope that someone with more knowledge than me can do this,.

Anyway untill that time, this is pretty good,.

hellskiwink

IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity
 
 
 
 
    hellman
(Newbee)
08-08-02 05:34
No 342818
      results 2  Bookmark   

results II
Sperheated steam in high volume:
Theory:
So the amount of steam that can be pushed into this reaction vessel
will result in the higher volume of ratio'd distillate that reaches the reciver bowl
If I can multiply the volume of ingoing steam massivly by increasing the surface area
of the water being boiled thus increasing the water in the recieving flash i will win.
Running a borosilicate thick walled tube 30cm into the reaction vessel, i can also
increase the steams temp to 150c., thus increasing the oil/water ratio 2 or 3 fold,.
4x10litre pots were assembled, each mounted on a 200 hole propane burner all hooked up
and fed from a large 20kg LPG gas cylinder, the outlet from the top of each
sealed steam generator was fed into a junction point which ran into the 30cm piece of
glass tubing the bent at the end and entered into the reaction vessel, into which sat 100
ml of dirty ketone,.
The system was turned on, and the steam temp at the entry into reaction vessel measured
~145. Cool,.
There was a lot of steam,.
The reaction vessel sat in canola oil bath heated to exactly 145c, a small make shift splash head
was implemented and the games begun,.
The distillate drove madly down into the recieving flash at a rate where there was no drips
but a gently stream of mosly water and ketone,.
I collected 90mls of oil in 1.5 hour, i measured the water 7 litres of water,.
A very aminated experience,.

thankyou,.


IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity
 
 
 
 
    hCiLdOdUeDn
(Hive Bee)
08-08-02 05:40
No 342821
      again, nice results...how clean was this ketone?  Bookmark   

again, nice results...how clean was this ketone? Did you try the bisulfite adduct? seems like an awful lot of water for just 90mL ketone---damn thats like 2 gallons!

hcildoduedn
 
 
 
 
    hellman
(Newbee)
08-08-02 05:50
No 342824
      Really, really clean, a tinge of amber,.  Bookmark   

Really, really clean, a tinge of amber,.
Yeh, water 2 gallons, but this is it,.
No vacuum,no column,no stir bar, your mother could run this one,.(no offence to your mother either)
My reasoning is quite simple in why I am doing this,.
If you are going to make a large amount of ketone,
This is the safest way to do it,
And it dead simple, you could run this in a share house,
and nobody would know, gotta go back soon

wink

IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity
 
 
 
 
    foxy2
(Distinctive Doe)
08-09-02 07:44
No 343389
      Clapping  Bookmark   

From one bee who has no vacuum pump.

THANK YOU!!!

Those who give up essential liberties for temporary safety deserve neither liberty nor safety
 
 
 
 
    hellman
(Newbee)
08-09-02 12:59
No 343432
      Diffilculties encountered in Crystallisation  Bookmark   

Reheat the mixture untill it is mobile again,
then cool slowly until first crystals appear.
If they don't appear scratch, or disturb the solution just before it hard freezes,.
When you get the crust of crystals appearing,stir, really hard, freeze, and the crytals should seperate out,,
Ironically the adddtion of a small impurity may catalyse
the initial crystal,.
If not scrath hard, blow, or take a hard frozen sample,
and then add the mobile oil, and freeze,.

Try letting it get mobile, then drop a wee piece of co2
into it,
If all that fails  then a sparingly soluble or insoluable solvent can be used(I have not tried this)

It will happen.
Practice on safrole to get the hang, if you have't already,
Hmmm.

hope this helps,.

hm


IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity
 
 
 
 
    Osmium
(Stoni's sexual toy)
08-09-02 15:43
No 343479
      Doesn't work with stuff freezing very much below ...  Bookmark   

Doesn't work with stuff freezing very much below 0C. Seed crystal generation is fastest much below the melting point (usually 70C or so) and very slow around the freezing point, and crystal growth is slowed down just like any other chemical reaction by lower temps. You won't be able to see big solid ketone crystals growing in liquid ketone, it will always be in some glassy state.
You might be able to measure the MP by slowly letting frozen ketone heat up though.

I'm not fat just horizontally disproportionate.