Author Topic: Distillation of nitromethane from hobby fuel...  (Read 3186 times)

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Mercury

  • Guest
Distillation of nitromethane from hobby fuel...
« on: December 20, 2003, 07:59:00 PM »
I know that this has been discussed in the past, but after reading through all the posts I'm confused as to why you cannot simply distill nitromethane from the hobby fuel without having to add water to extract the methanol. I mean, there are many bees that say to distill out the methanol and nitromethane, leaving behind the oil lubricant, then add water to the nitro/methanol mix. The methanol will go into the aqueous layer and you can remove the nitro layer with a sep funnel.

Why do all that? If the bp of methanol is 64.55 and the bp of nitro is 101, then there is certainly enough difference between the boiling points (according to Zubrick) to perform a regular distillation. It seems like you can distill the methanol and the methanol/nitro azeotrope (which I believe boils at 65), but once the temp rises to 101 you can change receiving flasks and distill the nitro, leaving behind the oil lubricant. The bp of the lubricant is unknown, but I'm willing to bet that it boils well above 100, otherwise what good would it be acting as a lubricant anyway. So, in conclusion, I don't see any point of extracting the methanol with water, correct me if I'm wrong.

Belial

  • Guest
Try both and learn first hand
« Reply #1 on: December 20, 2003, 09:50:00 PM »
Try both and learn first hand

Mercury

  • Guest
I just read up on Dr.
« Reply #2 on: December 20, 2003, 11:16:00 PM »
I just read up on Dr. Drools Complete MDMA synthesis and he mentions that he distilled the nitro and never mentioned anything about extracting the methanol with water, so I guess it works.

Antibody2

  • Guest
here is the scoop
« Reply #3 on: December 21, 2003, 12:59:00 AM »
if you directly distill the RC fuel using simple distillation, the distillation temp will slowly rise from 65C to 102C giving you a fairly large mixed fraction. Kind of like an azeotope but not really.

So you would need to fractionally distill to avoid this problem/waste.

If you wash with water it will remove the MeOH but it will also take some MeNO2 with as well. MeNO2 is soluble to some extent in water.

so it can be done either way you want, with fractional distillation of unwashed RC fuel the best option.

btw - those cocksuckers are notorious for having much lower % of nitro than they claim on the label.


BizzyBee

  • Guest
The reductive amination requires methyl ...
« Reply #4 on: December 21, 2003, 01:07:00 AM »
The reductive amination requires methyl alcohol anyways so why go through all the trouble?

Swim used 80% nitro as is with no problem. The 10% castrol oil has no or little effect on yeilds.

Swim does not even distill until the mdma extraction.

Swim uses raw sassafras oil as is [95% safrole] in the krv wacker then extracts the mdp2p and np soluable impuritys with toluene, once the toluene evaps this mdp2p/impurity mix gets ran through through the Al/hg nitromethane with raw 80% hobby nitro fuel. Once that is finished swim sets up for fractional distillation to seporate the good and the unwanted.

Swim gets the same effect as 100mg oral from smoking 30mg.


Mercury

  • Guest
Anitbody2 Why would the temp slowly rise from...
« Reply #5 on: December 21, 2003, 03:22:00 AM »
Anitbody2
Why would the temp slowly rise from 60 to 100? It's just a regular distillation. I would think the temp would first stabilize at 65 while the methanol distills, then the temp will rise to 101 to distill the nitro. Perhaps things don't always work out that nice though  :(

BizzyBee
You smoke MDMA? Damn, never heard that before...so, what's it like?  ;)

Rhodium

  • Guest
Think "azeotrope"...
« Reply #6 on: December 21, 2003, 04:02:00 AM »
It's just a regular distillation

Think "azeotrope"...


Mercury

  • Guest
Rhode, I was thinking about it.
« Reply #7 on: December 21, 2003, 04:32:00 AM »
Rhode, I was thinking about it. Then I remembered that you mentioned the bp of the azeotrope in Dr. Drools Complete MDMA Synthesis write up...



This discrepancy is probably due to the fact that methanol and nitromethane forms an azeotrope. First a 92%/8% MeOH/MeNO2 mixture (bp 64.5°C) distills over (close to the boiling point of pure methanol, bp 64.7°C) and when all the methanol is gone, the temp shoots up to ~100°C, where pure nitromethane is collected.




I would be led to believe that the azeotrope would distill at the same time the methanol would distill. Then, once all the methanol is gone, the temps will rise to ~100C.

So I still don't understand why the temp will slowly rise between the bp of methanol and nitro producing a distilled mixture that contains both products.


BizzyBee

  • Guest
Same effect
« Reply #8 on: December 21, 2003, 05:02:00 AM »
Quicker onset and shorter duration. I find with most any
abuseable black market drug, smoking lets you regulate the
dose to fit your specific needs as opposed to an oral dose
that can be affected by many factors and can be hard to hit
that target doseage without under/over doseing.

Think what you may about swim's "shitty" way to mdma but in
his opinion distilling the sassafras oil, distilling the
mdp2p and distilling the nitro fuel is a few extra pains in
the ass that are not needed to obtain pure mdma in the end.

By the way, swim found this "shitty techneiq" at

https://www.thevespiary.org/rhodium/Rhodium/chemistry




hypo

  • Guest
tee-hee....
« Reply #9 on: December 21, 2003, 10:52:00 AM »
> I would think the temp would first stabilize at 65 while the methanol
> distills, then the temp will rise to 101 to distill the nitro.

you obviously only know distillation from paper. unfortunately this
is not how it works in reality. you know, like there's a reason
engineers use huge and hideously expensive columns with 100 plates
to distill their stuff...

see also phase-diagrams of binary mixtures and be afraid.


Rhodium

  • Guest
that's embarrassing
« Reply #10 on: December 21, 2003, 05:09:00 PM »
By the way, swim found this "shitty techneiq" at

https://www.thevespiary.org/rhodium/Rhodium/chemistry%5B/blue

]

Where? I must clearly remove it.


BizzyBee

  • Guest
http://www.rhodium.ws/chemistry/alhg-meno2.html...
« Reply #11 on: December 21, 2003, 09:41:00 PM »

https://www.thevespiary.org/rhodium/Rhodium/chemistry/alhg-meno2.html%83



By Entropy

He says he used 60% and failed to reconize that hobby fuels
contain castrol oil. Nothing worth deleting.


Antibody2

  • Guest
mercury - you will get alot of methanol coming
« Reply #12 on: December 22, 2003, 01:52:00 AM »
mercury - you will get alot of methanol coming over at a stable 65C, its later that the temp will slowly climb to Nitromethanes BP, but that mixed MeOH/MeNO2 fraction is large.

once upon a time 1000mls 30% nitro RC fuel was simple distilled

65C - 575mls MeOH
65-102C - 150mls of mixed MeOH/MeNO2 (it was a slow steady rise in temp)
102C - 125mls of MeNO2
residue - 150mls lubricant

the 65C-102C fraction was redistilled and it came over as the same mixed fraction and it seems obvious to Ab2 that what he bought was less than the 30% nitro claimed.


Just4Fun

  • Guest
Is that a fractional distalation with or ...
« Reply #13 on: December 24, 2003, 04:17:00 AM »
Is that a fractional/regular distalation with or without a vacuum?

Chromic

  • Guest
Distilling MeNO2/MeOH/castor oils
« Reply #14 on: December 24, 2003, 07:24:00 AM »
I've done the same. Use a good column packed with stainless steel scrubbing pads (vigreux columns work too, but not quite as well). What I'd recommend is if the nitromethane is a reagent, that you don't consider precious, to just throw out the first MeNO2/MeOH fraction, then keep the MeNO2 fraction.

Alternatively, if you don't care if there's methanol in the nitromethane, then just check the density of the fractions you keep and read up on my calculations on how to figure out how much MeNO2 is in each fraction.

Just4Fun

  • Guest
So SWIM takes it that you don't use a vacuum...
« Reply #15 on: December 24, 2003, 06:55:00 PM »
So SWIM takes it that you don't use a vacuum for this one... Right?

homeslice

  • Guest
Swim just distilled nitro from fuel and didnt...
« Reply #16 on: December 24, 2003, 07:32:00 PM »
Swim just distilled nitro from fuel and didnt use vacuum. There were some liquids that came over between 64-101 at like 82 some kind of clear liquid came over? Swim just disregarded that with the meoh.

Its easy to tell when the nitro is coming over as the temp will obviously spike to about 100 and when it drips into the meoh in the receiving flask there are really obvious swirlies in the flask.
Plus pure nitro will burn with a blue flame after ignited, so test it this way.


gruns

  • Guest
Doesn't methanol also burn with a blue flame?
« Reply #17 on: December 24, 2003, 07:53:00 PM »
Doesn't methanol also burn with a blue flame?  Perhaps Nitro's blue flame is of a different character.  Could you perhaps describe it compared to methanol?


Antibody2

  • Guest
Just4fun - right, no vac.
« Reply #18 on: December 24, 2003, 09:18:00 PM »
Just4fun - right, no vac. Although you could if you wanted, my vac would boil MeNO2 at RT tho.


homeslice

  • Guest
Big difference
« Reply #19 on: December 24, 2003, 09:29:00 PM »
The MeOH burns with a dark blue/violet looking flame. It ignited pretty quick, and there was an occasional orange spark in the middle of the flame, swim assumes this was traces of water in his otc MeOH.
The nitro ignites with a little effort and also has a blue flame, but of a completely different shade. The nitro had a light blue or sky blue like color to it with no orange sparks. Im assuming that if any MeOH was in my nitro there would have been a hint of purple involved, just like the orange was in the otc MeOH indicating water. Also, by using an iodine dropper from a tincture bottle, swim dropped 2 drops of his distilled nitro into the MeOH and it created those swirlies swim mentioned earlier.


gruns

  • Guest
Now try burning the azeotrope of nitro and...
« Reply #20 on: December 24, 2003, 10:27:00 PM »
Now try burning the azeotrope of nitro and meoh :)


homeslice

  • Guest
Ok a 50/50 mix of meoh and nitro burned the...
« Reply #21 on: December 24, 2003, 10:50:00 PM »
Ok a 50/50 mix of meoh and nitro burned the same color as the nitro that swim distilled did. The only difference was an occasional orange spark and how easily it ignited as compared to the distilled nitro. Good thinking gruns swim didnt even think of that...
So... 2 hours ago swim thought he had 99% nitro b/c of the nice blue flame but now swims not too sure  :( . Suggestions anyone?


terbium

  • Guest
Density
« Reply #22 on: December 25, 2003, 01:01:00 AM »
After you distill then measure the density of the distillate to determine the ratio of nitromethane to methanol - nitromethane is much denser than methanol. The easiest way to do this is with a hydrometer - this is what the top fuel people use.


Just4Fun

  • Guest
Thanks everyone :)
« Reply #23 on: December 25, 2003, 01:40:00 AM »