Author Topic: Processing 1 Mole Ketone Using Nitromethane  (Read 14677 times)

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PolytheneSam

  • Guest
How about hydrogenation of nitromethane using a ...
« Reply #20 on: November 26, 2002, 12:43:00 AM »
How about hydrogenation of nitromethane using a nickel catalyst? 

Post 53425 (missing)

(KrZ: "Raney Nickel Nitromethane Reduction", Chemistry Discourse)


http://www.geocities.com/dritte123/PSPF.html


The hardest thing to explain is the obvious

abacus

  • Guest
Solvent volume
« Reply #21 on: November 26, 2002, 02:48:00 AM »
Osmium

I found I needed that amount of solvent in the nitro reduction.  The sludge produced is a lot and I needed that much solvent and it is a lot for 1 mole ketone but I could'nt find a way around it.

Also, some water is distilled over with the methanol/methylamine solution but point taken, more water may be good.

Finally, I too have had very good results by dripping in ketone over a few hours while refluxing, and then adding even more but I didn't want to confuse anybody. 

Recycling the methanol/methylamine solution is always carried out and reused in the next reaction. 

Abacus

Osmium

  • Guest
> I found I needed that amount of solvent in ...
« Reply #22 on: November 26, 2002, 09:56:00 AM »
> I found I needed that amount of solvent in the nitro
> reduction.  The sludge produced is a lot and I needed
> that much solvent and it is a lot for 1 mole ketone but I
> could'nt find a way around it.

I see. Yes, I guess you're right. It's been a long time since I did a nitro Al/Hg.

Ever tried to neutralise the distilled MeOH/MeNH2 with HCl and removing the MeOH by distillation?

I'm not fat just horizontally disproportionate.

abacus

  • Guest
Yes Indeed
« Reply #23 on: November 26, 2002, 10:11:00 AM »
Osmium, you are right if the goal is to reduce the solvent volume, but I never bothered and use the 6% solution as it is.

The rationale was trying to process up to 200g ketone in 1 day using nitromethane in medium size glassware, which was due to serious time constraints, and eliminating the need to mess around forming the hydrochloride only to basify it once again.

The large solvent volume was the price to pay.

Abacus

BlingBling

  • Guest
>>Ever tried to neutralise the distilled ...
« Reply #24 on: November 26, 2002, 10:15:00 AM »
>>Ever tried to neutralise the distilled MeOH/MeNH2 with HCl and removing the MeOH by distillation?

Yes and all I ended up with was a yellowish oil, about 5ml's that refused to evaporate. Was expecting only a few grams of MeAm.hcl. Let the oil sit out for a few days and when I returned, it was still an oil. 



Osmium

  • Guest
Dry it in a desiccator.
« Reply #25 on: November 26, 2002, 10:22:00 AM »
Dry it in a desiccator. Or play around with different solvents (IPA should work) until it suddenly crystallizes.

I'm not fat just horizontally disproportionate.

GOD

  • Guest
Swim just went ahead and tried this at 56% scale ...
« Reply #26 on: December 01, 2002, 12:42:00 AM »
Swim just went ahead and tried this at 56% scale (in order to aminate 100G ketone)in a 3L 2n flask with foil.  Not reccomended!  He dripped in 17mls of nitro/water/meoh solution, and then started a slow drip (1/2 seconds).  Within 5 minutes, he had a runaway rxn (this is with 2 leibig condensors 200+400mm stacked on eachother, plus a vigreux with a fan on it) and a full bag of ice in the cooler- he managed to get it calmed down after stopping addition, but after resuming, he lost control again (at a slightly slower drip rate) and ended up watching the flask dry out as his MeOH solution basically hovered within the vigreux and condensors, all the while escaping through the hose he had attached on top of the vigreux.  At least no valuable precursors where lost, and the fumes where safely pointed out the window. 

Off to the store for some flashing...

Im not the bearded man upstairs, Im a bald guy with a healthy penis. So open yer pie-hole!

hCiLdOdUeDn

  • Guest
Wowa! SWIM has NEVER had a run so exothermic!
« Reply #27 on: December 01, 2002, 02:48:00 AM »
Wowa! SWIM has NEVER had a run so exothermic! How many mL of solvent were used? Swim used an 8% azeotropic mixture of nitromethane/methanol and never had a problem with runaway rxn. and he only used a 200mm Leibig condensor. He also used Reynolds Heavy Duty aluminium foil (ground up with coffee grinder).

Sink or SWIM

BlingBling

  • Guest
Your using foil, thats why!
« Reply #28 on: December 01, 2002, 03:54:00 AM »
Your using foil, thats why!  ::)

Ronald Mcdonald figures a rxn using more than 50g of foil should be done with a larger mouth'd vesel and condensor.

Invest in a 45/50 5L and a 45/50 reflux condensor if you want to use large amounts of foil

GOD

  • Guest
yessa, (snip, snip) I's went to tha 'yella' place ...
« Reply #29 on: December 01, 2002, 04:45:00 AM »
yessa, (snip, snip)
I's went to tha 'yella' place (snip...)
got me 5X7 100 pack (snip...)
aint gonna mess with dat foil no moe


Im not the bearded man upstairs, Im a bald guy with a healthy penis. So open yer pie-hole!

BlingBling

  • Guest
WhoooPSHhhh
« Reply #30 on: December 01, 2002, 04:56:00 AM »

hCiLdOdUeDn

  • Guest
Since the MeOH/MeNH2 mixture is distilled you can ...
« Reply #31 on: December 01, 2002, 07:27:00 PM »
[r]Since the MeOH/MeNH2 mixture is distilled you can use RC fuel bought OTC without cleaning it up! A great simplification for many of the bees![/r]

Osmium, Does this mean that swim can use the RC fuel with all the oils in it and it should still work? Does the oil react in the al/hg at all? swim just wants to recover the 6% methylamine methanolic solution.

If he can use RC fuels with oils in it then it just saved him a day of distilling fuel!  :)

WOW, thanks abacus! You saved me alot of time trying to make methylamine.hcl from paraformaldehyde/ammonium chloride because it took me a full day just to get a mere 40g  ::)

AWESOME I LOVE IT!!!

Sink or SWIM

BlingBling

  • Guest
I doubt it..
« Reply #32 on: December 01, 2002, 10:36:00 PM »
>>Does this mean that swim can use the RC fuel with all the
>>oils in it and it should still work?

I doubt it will interfere with anything, for the oil is just castor, but why not turn the lightbulb on and go buy a gallon of pure nitro for a whopping 20 bucks! It's not watched AT ALL! THERE IS NO EXCUSE!  :P  :)  :P  Your wasting more money on RC fuel!

Bubbleplate

  • Guest
Questions For God
« Reply #33 on: December 02, 2002, 02:48:00 AM »
What temperature was your Methanol when you started drip?
Also, how much Hg Chloride did you use?

GOD

  • Guest
Sorry, didnt take any temps- everything was ...
« Reply #34 on: December 02, 2002, 09:53:00 AM »
Sorry, didnt take any temps- everything was started at room temp, and a little under 300mgs of HgCl2 were used. (remember, everything was at 56%)

Im not the bearded man upstairs, Im a bald guy with a healthy penis. So open yer pie-hole!

Osmium

  • Guest
> why not turn the lightbulb on and go buy a ...
« Reply #35 on: December 02, 2002, 12:05:00 PM »
> why not turn the lightbulb on and go buy a gallon of pure
> nitro for a whopping 20 bucks! It's not watched AT ALL!
> THERE IS NO EXCUSE!  Your wasting more money on RC fuel!

Not everyone is able to get pure NM.


I'm not fat just horizontally disproportionate.

BlingBling

  • Guest
??
« Reply #36 on: December 02, 2002, 07:56:00 PM »
>>Not everyone is able to get pure NM.

It's not available in every country? I just assumed it would be being that most countrys enjoy race cars and experiment with rocket scientry. Although, I can see how 3rd world countries wouldn't have any available.

Rhodium

  • Guest
Not having access to *pure* nitromethane does not ...
« Reply #37 on: December 02, 2002, 08:14:00 PM »
Not having access to *pure* nitromethane does not equal a complete lack of RC hobbyists. Why do you americans always go from one extreme to another? There is always a middle road, even if that is not as fantastic as either or.

I have a neighboring country where 99% NM is nowhere at all to be found, as it is not legal to sell anything containing over 50% nitro OTC. Hence they only have brands containing a lot of methanol, some nitromethane and a dab of oils.

Osmium

  • Guest
> It's not available in every country?
« Reply #38 on: December 02, 2002, 08:33:00 PM »
> It's not available in every country?

Obviously not. Since there are an estimated 200 nations on this planet you can bet your right thumb that some will have outlawed NM for obvious reasons.

> I just assumed it would be being that most countrys enjoy
> race cars and experiment with rocket scientry.

Nitro cars aren't that common outside the US. And even if they were, not everyone is willing to acquire a race license to be able to buy it. Or not everyone is willing to go through all the hassle of obtaining pure NM when the widely available RC fuel will do just fine.

Which hobby rockets use nitromethane? I am not aware of any.
Besides, rocketry is illegal in many countries too, and would be a pretty stupid excuse to acquire NM because it simply raises too much questions and eyebrows.

> Although, I can see how 3rd world countries wouldn't have
> any available. 

Not too long ago all the NM dealers in the not quite third world country of the US were questioned by gov officials about their customers, because someone had blown up a federal building somewhere in Oklahoma. Remember?
Different countries, different laws. You can get a lot of interesting shit in thirld world countries that we all are  uncontrollably drooling for. Money can buy you everything you want in thirld world countries. It's the first world countries where stuff is unavailable.

I'm not fat just horizontally disproportionate.

placebo

  • Guest
Re: WOW, thanks abacus!
« Reply #39 on: December 03, 2002, 12:00:00 AM »

WOW, thanks abacus! You saved me alot of time trying to make methylamine.hcl from paraformaldehyde/ammonium chloride because it took me a full day just to get a mere 40g



Any moron who can follow simple directions should be able to make methylamine from paraformaldehyde & ammonium chloride by the kilo in half a day.


Intelligence is not the recall of knowledge, but the ability to use it. (Rainman was a retard)