Sciencemadness Discussion Board

Manufacture of sodium azide via hydrazine

Picric-A - 20-7-2008 at 13:53

After a bit of research i found that sodium azide could be made by reacting Sodium Nitrite with Hydrazine. Has anyone done this? if so what are the reaction conditions?
NaNO2 + N2H4 --> NaN3 + 2H2O

Also, i have found text that Hydrazine can be made by reacting soidum hypochlorite (probably swimming pool strength ( 14-15%)) with urea:
(H2N)2C=O + NaOCl + 2 NaOH → N2H4 + H2O + NaCl + Na2CO3

Both reactions involving hydrazine should be carried out under a fume hood as i hear hydrazine is nast stuff :P

thanks for any help
Picric-A

cobrasniper555 - 21-7-2008 at 17:04

I haven't heard of creating sodium azide that way. Just a question as I don't use sodium nitrite, where's a source of it? I've been meaning to conduct some little experiments with it. As for the hydrazine, wouldn't a greater percentage of sodium hypochlorite create better yields or would it become too dangerous to handle?

Picric-A: Nice post. I've been waiting for something similiar to appear.

The_Davster - 21-7-2008 at 21:25

You mean like http://www.sciencemadness.org/talk/viewthread.php?tid=470&am...
(post by Polverone 24-2-2003)

followed by the synthesis of sodium azide, which has been posted on the forum before, but I have been unable to find it this morning.

Picric-A - 22-7-2008 at 03:43

yes i have made Hydrazine in the past using NaClO 14%.
here is a site describing th manufacture of Hydrazine and ultimatly Hyadrazine sulphate:
http://designer-drugs.com/pte/12.162.180.114/dcd/chemistry/h...
as long as the reation is carried out in a good fume hood i guess it shouldt be too dangerous.
I think i will try it small scale to start off with. :P

cobrasniper555 - 22-7-2008 at 09:12

Picric-A: That site's document was written by a friend I know over at A0tu (Douchermann). He has another forum post of a much more OTC-like approach. I was reading up on the post and maybe you'll be interested:

http://www.a0tu.com/bbs/showthread.php?t=1676

As for the sodium azide, I'll help research but I can't quarantee anything.

Rosco Bodine - 31-7-2008 at 07:43

The Hodgkinson patents GB128014 and GB129152 are what that simplified reaction for producing azide describe,
and many experiments were done by me trying unsuccessfully to reproduce those patents reported results.

What works out nicely as equations on paper may not square with the real world result that is gotten in actual experiments.

More than a bit of research and actual experiments will need to be provided as *proof* to show that this reported simpler route to azides has any veracity.

UnintentionalChaos - 31-7-2008 at 08:42

There is an ENORMOUS thread on both these topics. You have to dig a little to find the useful material, but it's there.

I would scrap the hydrazine disussion here as it has been thoroughly covered, however, the azide discussion is still up for grabs AFAIK.

[Edited on 7-31-08 by UnintentionalChaos]

S.C. Wack - 31-7-2008 at 15:25

The preparation using alkyl nitrite is found in 3 of my scans (Schlesinger, Brauer, Inorg Syn), and I have given patent numbers for this in the azide thread. People would probably not bother with alkyl nitrite if they could use sodium nitrite just as well.

-=HeX=- - 1-8-2008 at 08:16

My soon to be released .pdf on Azides has the alkyl nitrite method simply because it always works! i have had nothing but failures with the simplified processes in the past, so I just actually bought some azide from a chem supplier. Primary Azides like silver azide is good stuff.

Formatik - 1-8-2008 at 22:44

Azides can be formed several different ways, nitrites is one way. HN3 forms from hydrazonium hydrosulfate and KNO2 in solution under strong cooling, and then distill off (deadly if you don't know what you are doing) but the yield is low at 20%, with the alkyl nitrites yield is in area of 70%. The yield is low due to oxygen in the gases released (N2, O2, N2O) which partly oxidizes the HN3.

kclo4 - 2-8-2008 at 21:05

Quote:
Originally posted by cobrasniper555
Picric-A: That site's document was written by a friend I know over at A0tu (Douchermann). He has another forum post of a much more OTC-like approach. I was reading up on the post and maybe you'll be interested:

http://www.a0tu.com/bbs/showthread.php?t=1676

As for the sodium azide, I'll help research but I can't quarantee anything.


Although Doucherman is a great chemist, I'm pretty sure he didn't write anything in the rhodium and hive archives. :P
The link you gave doesn't work, but I'm pretty sure he just used the syntheses, or posted it while they were on the topic of making hydrazine.

[Edited on 2-8-2008 by kclo4]

cobrasniper555 - 2-8-2008 at 22:40

He did. I've had some pretty interesting conversations with him before with hydrazine and the likes so I'm pretty sure that if anyone asked for a detailed explanation, he would provide it (so far, everyone just wants to deal with synthesis over there, so he gave one the majority requested). But you are right, I won't argue with that.

kclo4 - 2-8-2008 at 23:18

Yeah he would, his site is pretty much like that I think.. detailed synthesis and a bunch of notes on it.

cobrasniper555 - 3-8-2008 at 10:10

Yeah! It was helpful until it got shut down.