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Author: Subject: Nitromethane extraction
plasma
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[*] posted on 21-5-2002 at 11:49
Nitromethane extraction


I have one gallon of fuel for r/c cars witch
contains 15 % nitromethane, 18 % oil and the rest is methanol. How can I extract the nitromethane. When mixed with water I can remove the oil with a eye-dropper, but is it possible to remove the methanol ?
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[*] posted on 21-5-2002 at 11:50


It will be hard to get pure nitromethane from your fuel. Methanol evaporates considerably faster than nitromethane, so I'd first just expose it to the air and see when the volume of the liquid had dropped about the right amount. At that point, I don't know exactly how well the oil, nitromethane, and remaining methanol will separate. Water will dissolve up to 10% nitromethane, so you may have considerable losses if you need to add water to separate the oil. Water and nitromethane have close to the same boiling point (not that I'd boil nitromethane) and evaporation rates. So you may only be able to get oily nitromethane.
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plasma
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[*] posted on 21-5-2002 at 11:50


Thanks for your replies. I will try your first suggestion, and let it evaporate, I think it will work. But when it has evaporated down to 33% of the original volume, it is more oil than Nitromethane.
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[*] posted on 21-5-2002 at 11:51


So your racing fuel contains:
15% NM (CH3-NO2)
18% Oil (X-YZ)
67% Methanol (CH3-OH)
You first need to know properties off the components to be able to separate them:
1)All are soluble in each other
2)NM:BP= 101°C; MP= -29°C
Methanol:BP= 65°C; MP= -98°C
Oil BP>200°C; MP=? usually not far from ambiant T or close to freezing Temp!

With this you can conclude that distillation can be the way to go Methanol will leave the system; then the NM and finally the Oil will remain! You can also conclude that Freezing is a good way to get the oil out, and then the NM...(it is a special kind of cristallisation separation); Carbo-ice allows you to go as low in T as -80°C when in methanol or aceton (methanol will remain liquid!).I would first try deep freezer at -20°C to see if you can get hold of the Oil!

3)Oil water solubility is low; so does NM solubility; methanol is 100% miscible with water.
So water could be a way to go; but NM is a little soluble in water and very soluble in methanol (so its solubility can be good in a methanol/water mix!)
Assuming you have 1 liter of fuel:
180ml of oil
150ml of NM
670 ml of MeOH
By adding 6,7 Liter of water, you will decantate a lot of oil as an upper layer (probabily 90% of it), but also a part of your NM (maybe 50% of it) stil 50% will remain in solution; this is a poor choice!
You can add a little acid strong acid to diminish solubility of NM but still it wont help a lot!

4)
Oils are rather inert towards acids, but may react with bases to make soaps (depend on the oil of course; parafin oil is inert).
R-CO2H + NaOH --> R-CO2Na + H2O
Soaps are much more soluble in water than the original oil!
Original oil (if soaponifiable) can be regenerated by strong mineral acids!
R-CO2Na + HCl --> R-CO2H + NaCl

NM forms "explosive salts" with NaOH or with KOH and NH4OH; those salts are brown/orange and form slowly when biphasic (but it can increase speed with heat (runaway) and be quite fast when both base and NM are in the same phase what can be the case here since methanol is amphiphile solvant....reaction is quite exothermic as all acid-base neutralisation! Salts are usually unsoluble in methanol (most of them) and weakly soluble in methanol/water (I found recently that methanenitronate salts are weakly soluble in methanol and can be easily separated.
Nitromethane is inert towards acid exposure (except long boiling exposure to H2SO4)

Methanol is inert towards bases but forms esters with acids!

From this you see:
That treating your batch with acid will give esterification of methanol and leave NM and oil unattacked:
Amongst interesting esters are:
-Nitrous ester CH3-ONO is gaseous at ambiant T and forms spontaneously when 30%HCl and NaNO2 are dropped in methanol (Flamable and liable to make gas explosion) it will bubble a lot!
CH3-OH + HCl + NaNO2 --> CH3-ONO + NaCl + H2O
This process is interesting but toxic due to NOx (HNO2 free some of it)and might be expensive if you don't have cheap sources of NaNO2/HCl.
Oil remains unafected and NM too; as a conclusion, water is formed, NaCl also and methanol leaves the batch- keep the batch T arround 10°C!
-Methyl chloride (it is also gaseous) but formation is quite slow and needs HCl conc and ZnCl2 as a catalyst + heating arround 60°C
CH3OH + HCl + ZnCl2 --> CH3Cl(g) + H2O + ZnCl2
Here you have a catalytical qtity of ZnCl and H2O; oil and NM remain unaffected!

You see also that another alternative is to treat the batch with saturated NaOH, KOH or NH4OH solution (drop by drop);(oil may soaponifiate but will remain in methanol/water solution) under stirring and cooling (30°C max)! When base addition is finished and the T starts to drop,allow the batch to cool down on its own, cristalls of Na,K or NH4 Nitronate should form and precipitate.If they don't form, allow to cool further with the help of ice cold bath!(Normally it should precipitate if you have a saturated solution of base I have done it many times).
Those cristalls are no pure nitronate but complexes of NM with it so don't be alarmed they don't explode unless very dry and hot in contact with a flame or a strong shock!
Filter them.And drop them fast (to avoid any drying) in 10 times the amount of water (or more) until fully dissolved.Then add dropwise under stirring and strong cooling medium conc strong acid (H2SO4 40%, HCl 33%, AcH 100%) (max 30°C)It is a neutralisation reaction between a strong acid and a strong base, so it heats a lot!A yellow layer of NM will form on top of the the beacker, add acid until the water that was initially black brown turns orange, then yellow test for acidity with lithmus; if positive allow to stand with a cover on top until transparent!
CH3-NO2 + NaOH <-=> CH2=NO-ONa(blackbrown)+H2O
CH2=NO-ONa + HCl --> CH2=NO-OH(yellow) + NaCl
CH2=NO-OH <-=> CH3-NO2
nitronic form of NM is soluble in water while its non nitronic form (the most stable) is nearly unsoluble.
You should then have two layers; test them for flamability; only the NM will burn (a bit like ethanol or nitroglycerin flame)!

With all this you can make a separation tree following your abilities!

PH Z




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[*] posted on 21-5-2002 at 11:52


I'm a bit confused, have I done it right ?
When saturated NaOH is dropped in the fuel when cooling and stirring, the solution gets pink and a large amount of very small cristalls appear. When they are filtered and dumped in water and fully desolved, the solution turns yellow. When adding 30% HCl to the solution under stirring and cooling, the solution turns dark red. Oily droplets form slowly on the surface. (They don't burn)
BTW the oil is none-petroleum

Thanks
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[*] posted on 21-5-2002 at 11:52


Is destillation of NM safe ? It seems crazy to destill a high explosive.
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smile.gif posted on 21-5-2002 at 11:53


I would think that would be dangerously risky.



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sad.gif posted on 29-5-2002 at 14:06


If destillation is so dangerous why would PH Z say this :
"With this you can conclude that distillation can be the way to go Methanol will leave the system; then the NM and finally the Oil will remain"
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[*] posted on 29-5-2002 at 15:47


When I heard "distillation" from you, I was thinking of you heating nitromethane with a propane burner. :)



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smile.gif posted on 30-5-2002 at 09:16


Please don't think like that.
I have ordered some real equipment (condenser, hotplate, flasks, beakers etc.). I think I will get the pack over the weekend. Then I will start with all the "complex" sythesis. (like NM dest.)

"Professional" destillation of NM will be all right, right ? :)




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[*] posted on 30-5-2002 at 11:55


Possibly. It may still be risky. Go to groups.google.com and search sci.chem for nitromethane distillation. There was a fairly long thread about this a while ago - Philou was one of the primary contributors.

It sounds like you are really making progress in chemistry, by the way! Only a couple of months ago you had virtually no chemical knowledge and were trying to improvise things from toilet bowl cleaner. Now you seem to have been doing some reading and you're getting some real equipment. Way to go! I hope you remain safe as you continue to expand your horizons of knowledge.
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thumbup.gif posted on 8-6-2002 at 08:58


I don't think that the distillation of NM is more dangerous than distilling sth highly flammable like gasoline or so. Otherwise they wouldn't sell it pure (think of a building with 100l drums inside on fire). The stuff won't detonate unless it is sensitized or a big booster is used.
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[*] posted on 8-6-2002 at 09:26


i have a video of some pure NM being detonated with a booster of tetrly. u can also detonate it easier if you mix it with H2O2 or something like flour to give it a lower densitity
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smile.gif posted on 15-7-2002 at 06:22
distilling nitromethane


Use vacuum distillation if you really want to be safe. You only need to warm it around 50deg. with the average fridge pump or aspirator, so a warmwaterbath will be fine. Be sure to throw in some boiling rocks.

Vac. distilling is not that more difficult if you already know how to perform it at atm.pressure, but you should read up on it fiorst.





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[*] posted on 15-8-2002 at 13:17


NM boils at 101°C; unless you boil it without condenser/cooler or boil it over ammonium nitrate or over a sensitive primary or over an amine or strong base like NaOH/KOH/LiOH/...
there is no risk of fire/explosion/detonation.
There is less risk in distillating NM than in distillating ethanol or methanol.
You can set it on fire, it simply burns like ethanol.Since it is flamable liquid, its vapour with air form explosive mixture (like many organic solvants).

Enjoy!
Plasma, did you tried freezing the mix to take the oil away?
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[*] posted on 24-8-2002 at 12:57


I did try freezing, but it didn't work very well.

BTW, the equipment I ordered 2 months ago arrived today. :D
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biggrin.gif posted on 8-9-2002 at 09:59


Great!:)
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thumbup.gif posted on 27-10-2002 at 10:27


Nitromethane is easily and safely disstilled at atm.It does however form a azetrope with methanol,the MeOH/nitro azetrope will come over first and then pure nitro will come over resulting in quite a loss of product to the azetrope.Guess it depends on the purity you require.btw the azetrope will be about 8%nitro and the rest MeOH.Peace,Chambered.
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[*] posted on 27-12-2002 at 23:23
re


When you said NM the first thing that came to mind is ANNM. If this is what you want, wouldn't it be good enough to evaporate off the methanol and add the oil/NM solution to the AN? ANFO and ANNM are both secondaries, so wouldn't a combination of the two just make it a bit more sensitive, yet serve the purpose you intended? Oh well, that is only assuming that you were working for ANNM. I hope my reply is not out of line for the reagent section.
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wink.gif posted on 10-11-2003 at 08:32


Nitromethane is in fact very hard to ignite with a match, and if it does burn, it does so with a lazy blue flame. It does detonate on shock though.
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[*] posted on 26-11-2003 at 22:13
Nitro distillation


Well if you take that oil formed from re acidification of your sodium/ nitro salt and distill it you will get pure nitro.

The sodium salt is quite sensitive so I don't reccomend doing this method.

However it is not the distillation that is dangerous, the distillation is safe and easy under atmospheric conditions. This is not a sensitive high explosive! Man up.

You need to find 50% or better nitro fuel, then distill this, your forerun is an azeotrope of nitro and methanol, something like 8/92, then over comes pure nitro, and you leave the oil in the flask.

Simple, not dangerous in the least, the explosive nature of nitromethane is overstated.

I just noticed that I was beat to the punch, but hell I've done it, so go for it!

[Edited on 27-11-2003 by tryptamine]
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smile.gif posted on 28-11-2003 at 14:19
NITROMETHANE FRACTIONAL DIST. IS SAFE!!


relatively safe anyway!!!

From racing, I can safely say that nitromethane is VERY safe, It has a very high flashpoint, so vapours in air are quite difficult to ignite, and it is not a very energetic compound, (far less than gasoline)

as for detonation, try not to dip strings of blasting caps into it and you should be OK!;)

the reason it is used in racing is to allow the addition of vast amounts of raw fuel without "drowning" the spark plug.

I think it had something to do with increasing the amount of available oxygen in the cylinder, and that it led to its use as a component of liquid explosive, not because of its inherent instability!!!
:)




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[*] posted on 28-11-2003 at 14:20


not because of its inherent instability!!!

correction....because of ANY inherent instability (its pretty damn stable)




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[*] posted on 12-2-2004 at 01:37


Theoretic, How strong of a shock wave does it take to detonate 100% pure nitromethane?



N/A
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[*] posted on 12-2-2004 at 02:27


Nitrometane distilation from racing fuel is very straighfoward. It works fairly as a classic simple distillation but to get good results you should try to fraction it as much as possible (long column, packing...). You have to use a decent distillation setup with a thermometer. And no open flames! Eletric heating!

First the temperature remains stable at the bp of methanol. You have only methanol coming. This is by far the largest fraction.

Then temperature start rising. You are now collecting a mix of methanol and Nitromethane. This is a large fraction, don't discart it, redistill.

Than temperature stays at the bp of nitromethane. You are now collecting nitromethane.

Then you stop getting condensates and your oil begin to smoke a bit. Turn the heat off.

I don't care what theory says. This is what happens in the real world.

If you didn't fraction your distilation enough, a second distilattion will give you almost pure nitrometane.

I got 150ml of rather pure nitromethane out of a gallon of 10% nitro fuel.

Extractions are messy and useless.

Good luck.
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