Here is some goods from the anonymous contributor

A nitroethane synth, made OTC

Preparation of Nitroethane by Gerard Desseigne & Henri Giral
The reaction flask is charged with:26.5 g (0.0625 * 3moles) of tech grade K2CO3 dissolved in 137 g of water320 g of 97% tech sodium nitrite
6 ml of cetyl-oleic alcohol or oleic alcoholm(antifoaming agent)Vol of the mixture is about 420 mls. The mixture is heated on a bath at 130C with stirring.
The addition funnel is charged with 750 ml of an aqueous solution of 444 g (3moles) sodium ethylsulfate.
 The solution is added to the reaction mixture during 50-60 mins at asuitable rate to keep the reaction mixture at 125-130C, with vigorous stirring.The distillation of the nitroethane begins when the addition is started. When addition of NaEtSO4 is complete 100 mls of water is added during 10 mins.
The distillate separates into 2 layers. Can be distilled at 760mmHg with a distillation column. Distillation starts at 30C. All below 74C is discarded.
Temp should settle at 87C & distillation is stopped at 99.8C.
Yield of nitroethane:96 g (1.28 moles), 42.6% based on NaEtSO4

and this was posted by Evil_Lurker:
Nitroethane, that substance which is so cheap at any chem supply house, but so damn hard to get. Making the stuff ain't very much easier than buying it from the recipes on the net.The two OTC easiest ways, using sodium ethyl sulfate and diethyl sulfate as reagents are very hard and dangerous to manufacture. The problem lies in the water molecule the ETOH creates when it forms the ester. The apparatus looks plain scary to operate, and creates diethyl ether as a side product and the yields suck ass!But now that problem has been fixed. Sodium ethyl sulfate can be easily prepared in the home laboratory from common sodium bisulfate found in pool pH down and 95% pure grain alcohol, and baking soda or sodium carbonate found in pH up.113 parts by weight of sodium bisulfate and 20 parts by weight of pure grain alcohol are combined in a flask and brought to boiling upon which time the sodium bisulfate crystals disappear and sodium sulfate forms.When the reaction has been completed, the flask was is immersed in an ice bath and vigorously stirred until the tempurature rapidly goes below 32.3C.The formed sodium sulfate is thus filtered out leaving an anhydrous ethyl hydrogen sulfate/ethanol mix.The excess ethanol is distilled off, and the ethyl hydrogen sulfate is neutralized with an appropriate quantity of sodium carbonate leaving sodium ethyl sulfate.Simple... thats all there is to it! The secret to how it works is the excess

Source: http://www.scribd.com/doc/10270006/Otc-Nitroethane-Synthesis


[Edited to include the source and keep the forum in one piece]

Potassium persulfate can be prepared by electrolysis of a mixture between potassium sulfate and hydrogen sulfate at a high current density.

    2 KHSO4 ? K2S2O8 + H2

It seems like you'd actually want to use sodium bisulfate in the electrolysis wouldn't you?


Hex, very nice find!
That looks like something I might be attempting to make soon as well!


EDIT: *Sigh* How do you guys get Nitrites?

Very over the counter the means thru which I get my sodium nitrite. I get ammonia nitrate out of hand warmers and convert it to sodium nitrate with Sodium bicarbonate or sodium hydroxide and then reduce the nitrate with Lead to the nitrite. This can be done albeit what appears to be lower yeilds using lead shot in a ball mill but I got way better results just melting the damn lead and slowly stirring NaNO3 into the mixure.

The NaNO3 will go into the melt with stirring and then rise to the surface as a mixture of Litharge and NaNO2. After everything is allowed to react for sometime and cooled down the remains which are normaly just litharge with now lead shot in it and NaNO2 is allows to leach into water and filtered twice to remove the litharge. Slowly evaporate the water as to not oxidise the NaNO2 back to the nitrate and what you have will be the nitrite.

It sounds like alot of work but its really not. If every step is done at its own pace its really no probem. I make a decent amount of NaNO3 when Im feeling up to it and then reduce the nitrate also when Im feeling up to it.

Im kind of feeling up to it also since I need some nitrite and only have a few grams left so maybe...If im feeling up to it .... Ill post some pictures.

PS: The nitrite curing salt from the butchers is a mixture of a bunch of crap don' t want like chlorides and carbonates.

Let us know how Ball milling the nitrate + Carbon works out.
You should make a small amount or nitrite using melted Pb just to use as a standard for other methods. Im interested in Polverons calcium oxide + sulfamic method to reduce the nitrate because it seems like it could be one of the most food safe methods. I have ran melts with carbon a few times and I find it to be less then satisfactory compaired to lead.

I just add excess of carbon to some nitrate and a small amount of H2O and grind the shit out of it in a morter. This drys before it starts the melt but I have had a couple of times where ignition has occured so be careful because this is not a much different compound then gun powder at this stage. I have never done it but a melt of NaNO3 with a very slow addition of carbon may just be a better way to go.

The way I see it though Pb is known to work very very nicely(and it does). You get two materials for the price of one, litharge and NaNO2 so its worth is as a control at the very least.

Within the next week I'll hopefully(if I'm not too busy) post a write up of the mentioned EtNO2 synth involving NaHSO4.

I've uploaded the patent mentioned in the linked article in case anyone wants it.

Thank you.

I would think this method would work just as well for Sodium Methyl Sulfate?

Oh boy, I honestly don't know. I'd presume it would work. MeOH and EtOH are so similar I'd imagine the chances of it working are MUCH greater than it not working.

Has anyone out there tried the synth in the first post?

I've tried the first half, making sodium ethyl sulfate and sodium methyl sulfate.

The problems for me come at the end, when trying to filter out the liquid from the sodium sulfate; it seems to have absorbed everything, and when I put this in my buchner, no liquid comes through.

What about ethylating KNO2 with a different ethylating agent? Maybe DES, or something. There was a recent post at SM that mentioned other agents that can methylate KNO2.

What about ethylating KNO2 with a different ethylating agent? Maybe DES, or something. There was a recent post at SM that mentioned other agents that can methylate KNO2.

 

under what topic Enkidu?

2b