Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
Author: Subject: NAN3 synth
prometheus1970
Hazard to Others
***




Posts: 138
Registered: 14-4-2010
Location: San Antonio, tx.
Member Is Offline

Mood: happy/ inquisitively eager

[*] posted on 31-1-2011 at 09:28
NAN3 synth


somewhere online I saw a synthesis for sodium azide (which is about as easy to obtain[buy] as tnt). It was very vague with no references to quantities, temperatures, concentrations, etc. Here's essentially what it said:

"Melt NANO3 and urea together, mix with pure lead acetate, lead nitrate and recrystallize with H2O. Is this a feasible route to NAN3? Doest anybody know the specifics?




Just because you're paranoid doesn't mean everybody isn't out to get you.
View user's profile View All Posts By User
bbartlog
International Hazard
*****




Posts: 1139
Registered: 27-8-2009
Location: Unmoored in time
Member Is Offline

Mood: No Mood

[*] posted on 31-1-2011 at 10:44


Sounds like a mangled echo of a post in this thread: http://www.sciencemadness.org/talk/viewthread.php?tid=7553

Seems dubious. Anyway one of the links shows more details (still no stoichiometry!) which suggests that one of the steps involves distillation of hydrazoic acid. I would suggest merging this thread with that one, there are at least a bunch of references there, though almost all of them are for other urea/NaNO3 products.
View user's profile View All Posts By User
prometheus1970
Hazard to Others
***




Posts: 138
Registered: 14-4-2010
Location: San Antonio, tx.
Member Is Offline

Mood: happy/ inquisitively eager

[*] posted on 31-1-2011 at 16:05


I looked up that thread and... I need to go lie down now.



Just because you're paranoid doesn't mean everybody isn't out to get you.
View user's profile View All Posts By User
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
*****




Posts: 1986
Registered: 2-3-2011
Member Is Offline

Mood: No Mood

[*] posted on 20-9-2011 at 12:41


Hopefully this helps:

Information about Hydrazoic Acid, HN3

Anhydrous hydrazoic acid (formula HN3 ) boils at 35.7degC, and has a freezing point of (minus) -80degC. This liquid gives of extremely poisonous fumes with a sharp corrossive unbearable smell, somewhat comparable to that of NO2. However, concentrations of fumes below the odor threshold are easily sufficient to cause poisoning. The liquid gives off vapors which can initiate explosion of the liquid if there is any nearby flame.

The actual creation of azides is difficult in the laboratory, but it can be carried out. Azides are as poisonous as cyanide, even sodium azide can give of some HN3 fumes when dissolved in water. Acids should not be added to basic azides, highly poisonous HN3 gas will result, and this gas has the potential for explosion. There are basically two routes, from sodium amide, or from hydrazine. The chain of reactions either way is long and complex.

Hydrazoic acid can act as either an oxidizing agent or reducing agent. For example, it reacts with copper according to the following equation:
(3)HN3 + Cu --> Cu(N3)2 + NH3 + N2


Preparation of Metallic Sodium

Elemental Sodium can be made in a thermite reaction between NaOH and Aluminum, there are several other threads dealing with this type of reaction on this forum.
http://www.sciencemadness.org/talk/viewthread.php?tid=14970
http://www.sciencemadness.org/talk/viewthread.php?tid=2105&a...

It is, in fact, quite surprising that an element as reactive as sodium can prepared by a chemical reaction, even many professional chemists are unaware that such a reaction can procede.


Preparation of Sodium Amide

Sodium and dry ammonia, when heated to 320-350degC, react to form sodium amide and hydrogen.

Metallic sodium dissolves in cold anhydrous liquid ammonia to form a deep blue colored solution. If Sodium Ferrate (which acts as a catalyst) is added to a blue solution of sodium dissolved in ammonia, the solution will slowly turn to a bronze color as all the sodium reacts.

Sodium and anhydrous liquid ammonia react, rather than simply dissolve into the typical blue solution, with the use of a black catalyst prepared originally by the reaction of a ferric salt with oxides of sodium in liquid ammonia. Liquid ammonia (500ml) was stirred at -32C and treated with 0.3g Fe(NO3)3 hexahydrate and then with 1g of metallic sodium. Air was bubbled through the mixture to discharge the initial blue color and produce a black precipitate of catalyst. Additional sodium 24g, added portionwise was then consumed in about 20 minutes with dissappearance the blue colour and formation of a grey suspension of sodium amide. The solubility of sodium amide thus prepared is very low (about 1mol per liter of liquid ammonia).


Azide from Sodamide

Sodium azide has been prepared by passing nitrous oxide over sodamide heated to 230degC.

2 NaNH2 + N2O → NaN3 + NaOH + NH3

Nitrous oxide can be generated by the gentle heating of small ammounts of ammonium nitrate until decomposition, traces of nitric oxide and nitrogen dioxide are also produced, these can be eliminated by bubbling the gases into a solution of sodium carbonate, leaving only nitrogen and nitrous oxide. Sodium nitrite will be produced in the solution. Depending on the ratio of NO2 to NO in the decomposition products, sodium nitrate may be the main byproduct forming, or some of the nitric oxide may not be absorbed by the basic solution, where it will either react with air to form nitrogen dioxide, or in the absence of air the unstable gas will decompose into nitrous oxide and nitrogen gas within several minutes.

Sodium nitrate can also be reacted with sodamide, both dissolved in anhydrous liquid ammonia under pressure at a temperature of 100degC to produce the dissolved azide. This is dangerous since the pressurized container is likely to burst since anhydrous ammonia has a boiling point of only (minus) -33degC. The reaction can take place at 80degC, while heating to 135degC allows a shorter reaction time and gives higher yields. First the two reactants react to form nitrous oxide, and then the intermediate nitrous oxide reacts with more amide.

KNO3 + 3KNH2 → KN3 + 3KOH + NH3


Another method is to react a dispersion of sodium amide in a hydrocarbon solvent with isopropyl nitrite dissolved in a hydrocarbon solvent. Excess amide should be used, and the solution of nitrite should be gradually added to the amide dispersion, with rapid stirring.

The below might be a possible reaction:

(13)NaNH2 + (6)PrNO2 → (2)NaNO2 + (3)NaN3 + (6)NaOPr + (2)NaOH + (8)NH3

where NaNH2 is sodamide, and PrNO2 is the nitrite ester of isopropanol. NaN3 is sodium azide and
NaOPr is sodium isopropoxide, which is analogous to sodium methoxide.

Ispropyl Nitrite can easily be made by adding concentrated HCl solution cooled to 0degC to a cold solution of sodium nitrite and isopropyl alcohol.


Azide from Hydrazine

Hydrazine hydrate can be converted to anhydrous hydrazoic acid by reaction with a nitrous acid ester in ether at 0°C with some sodium ethoxide present. This pure hydrazoic acid may be useful for the synthesis of Diaminotetrazole.

Hydrazoic acid HN3 can also be obtained by the action of nitrous acid on hydrazine sulphate.
(W. Wislicenus, Berichte, 1892, 25, p. 2084)

Hydrazine sulfate reacts with a solution of hydrogen peroxide and sulfuric acid to produce hydrogen azide gas in up to a 28% yield. It is important that the reactants be free from any traces of dissolved copper ions.

Possible Unusual Method
Supposedly, by heating finely powdered sodium nitrite in a fusion of excess urea at 160degC, low yields of sodium azide can be obtained, but I cannot confirm this with any certainty.

[Edited on 20-9-2011 by AndersHoveland]
View user's profile Visit user's homepage View All Posts By User
Phantom
Harmless
*




Posts: 43
Registered: 26-4-2011
Member Is Offline

Mood: AUDENDUM EST,FORTES AUDIUVAT IPSE DEUS

[*] posted on 28-9-2011 at 08:43


Here is a synthesis but in your place I wouldn't try to make it.

SODIUM AZIDE

This not actual a primary explosive, but it is used in the manufacture of lead azide.
Its preparation is extremely dangerous, because of the use of hydrazine.

PREPARATION:

Chemicals:

hydrazine hydrate (85 %) (TOXIC !)
butyl or isopropyl nitrite
ethyl alcohol
water
sodium hydroxide
Materials:
glass distilling flask
heating source
water bath
glass stirrer

MANUFACTURE:

1. Dissolve 5 grams of sodium hydroxide in 50 ml ethanol.
2. This mixture is poured down in a 100 ml distilling flask containing 6 ml hydrazine
hydrate.
3. Carefully add 10 ml of butyl or isopropyl nitrite, heat the mixture on a water bath.20
4. Add 12 ml more of the nitrite, slowly, so that the mixture refluxed slowly. This will
take about one hour.
5. After heating additional 15 minutes, the mixture is cooled to room temperature and
the white crystalline powder is collected and washed with alcohol.
This should be sodium azide.
View user's profile View All Posts By User
quicksilver
International Hazard
*****




Posts: 1820
Registered: 7-9-2005
Location: Inches from the keyboard....
Member Is Offline

Mood: ~-=SWINGS=-~

[*] posted on 28-9-2011 at 09:02


Please - let's site source when we offer any synthesis. If it's from personal notes, please say so, if it's from a textbook or patent - same thing.
Generally notes should only be offered if you have worked through the lab and are familiar with it and the original material was documentable. If it is a guess based on certain logical premises: please say so. There ARE some "recipes" floating around the internet that are problematic. When the E&W Forum was running back some years ago, the admin (Mega) was not pleased with many of the energetic synthesis in the info section and had often said he wanted to edit many of them. Some of those very same synthesis have been quoted on occasion and every effort should be made to explain that it was from that site - .Not that there is a definitive problem with all of them but that some of them were extrapolations from sources or patents that the site admin himself felt should be edited.

Patent material is a tough call becasue later period patents allow a material to come under legal protect yet certain facts not spelled out as the owner or company is allowed aspects of commercial production to remain secret. Occasionally the patent may be quoted incorrectly or written by someone other than the inventor.

Letting people know where the material is from is vitally important.




View user's profile View All Posts By User
Phantom
Harmless
*




Posts: 43
Registered: 26-4-2011
Member Is Offline

Mood: AUDENDUM EST,FORTES AUDIUVAT IPSE DEUS

[*] posted on 28-9-2011 at 09:20


Yes, you're right sorry.

Here is my source: http://nowa.pirotechnika.one.pl/www2/ipe.PDF
View user's profile View All Posts By User
plastics
Hazard to Others
***




Posts: 141
Registered: 6-11-2009
Member Is Offline

Mood: No Mood

[*] posted on 28-9-2011 at 23:44


Our very own len1 gives a very comprehensive description of the synthesis of sodium and potassium azide in his book "Small-scale synthesis of laboratory reagents" chapter 12 (ISBN 978-1-4398-1312-6). His write up also uses isopropyl nitrite and hydrazine hydrate. He also details the synthesis of isopropyl nitrite and hydrazine hydrate from simpler precursors
View user's profile View All Posts By User
Bhaskar
Hazard to Self
**




Posts: 64
Registered: 6-10-2011
Location: India
Member Is Offline

Mood: Like nitro runaway!

[*] posted on 8-5-2012 at 02:24


I read on wiki that the reaction of sodium nitrite and hydrazine may result in the formation of sodium azide...can this reaction be true?
View user's profile View All Posts By User
woelen
Super Administrator
*********




Posts: 7608
Registered: 20-8-2005
Location: Netherlands
Member Is Online

Mood: interested

[*] posted on 8-5-2012 at 02:39


Yes, nitrite and hydrazine can react with each other, giving azide. You need the right conditions for the reaction, otherwise you just get N2-gas. I do not know the details, but if you do a search on sciencemadness, then I'm sure you find more details about this reaction. It is a possible route for making azides.



The art of wondering makes life worth living...
Want to wonder? Look at https://woelen.homescience.net
View user's profile Visit user's homepage View All Posts By User
hissingnoise
International Hazard
*****




Posts: 3939
Registered: 26-12-2002
Member Is Offline

Mood: Pulverulescent!

[*] posted on 8-5-2012 at 04:17


Quote:
You need the right conditions for the reaction, otherwise you just get N2-gas.

Hydrazoic acid is decomposed by nitrous acid ─ a high pH is needed for best yields . . .

View user's profile View All Posts By User
Hennig Brand
International Hazard
*****




Posts: 1284
Registered: 7-6-2009
Member Is Offline

Mood: No Mood

[*] posted on 8-5-2012 at 09:13



I think this is what you are looking for.

N2H4 + CH3CH(NO2)CH3 + NaOH → NaN3 + CH3CH(OH)CH3 + 2H2O

Other alkyl nitrites can be used, but isopropyl nitrite has several advantages over most of the common alternatives.

If you are going to attempt the synthesis, know what you are doing beforehand and, watch out for gaseous hydrazine (especially during freebasing). I gassed myself a little with it a year or so ago. I doubt it increased my life expectancy any.

Also watch out for hydrazoic acid, it is very important to keep all reactions involving azides at least slightly basic for this reason. Hydrazoic acid is also very toxic and volatile.

Like woelen says, do a search, there are threads that go into this in quite a bit of detail.

[Edited on 8-5-2012 by Hennig Brand]




"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
View user's profile View All Posts By User
Bhaskar
Hazard to Self
**




Posts: 64
Registered: 6-10-2011
Location: India
Member Is Offline

Mood: Like nitro runaway!

[*] posted on 9-5-2012 at 01:23


Thank you, I will do a search on it... :cool:
View user's profile View All Posts By User
SM2
National Hazard
****




Posts: 359
Registered: 8-5-2012
Location: the Irish Springs
Member Is Offline

Mood: Affect

[*] posted on 30-7-2012 at 10:18


Why not start with hydrazonium sulphate. Seems much more sane.

Oh and of course there's the air bag method of harvesting it, mua ha ha ha. I'm WAY too frightened of explosives to get near them. When I was 18, yes, but now that I'm older, it's like I have shell shock, just seeing 4'th july fireworks.

A huge blockbuster and everyone is impressed with the big, jammy noise. A little bang from a HV, and people are freaked out to see the insane damage wrought there.

[Edited on 30-7-2012 by Fennel Ass Ih Tone]
View user's profile View All Posts By User
Hennig Brand
International Hazard
*****




Posts: 1284
Registered: 7-6-2009
Member Is Offline

Mood: No Mood

[*] posted on 30-8-2012 at 05:42


In my last post I discussed safety a bit. The bit about being careful during freebasing was in reference to freebasing hydrazine from an acid salt of hydrazine. Hydrazine sulfate is what I have been using, even though it wasn't stated explicitly in the last post.



"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
View user's profile View All Posts By User
detonator
Harmless
*




Posts: 29
Registered: 12-4-2011
Location: Maoming City, Guangdong Province, China.
Member Is Offline

Mood: No Mood

[*] posted on 31-8-2012 at 03:41


Preparation System chlorine test apparatus A, an ice tank (with a small amount of water), the raw material: hydrazine hydrate (preferably 85%), nitric acid, copper (a simple substance), sodium carbonate (sodium hydroxide may also be, and preferablywith sodium carbonate). A large number of the copper material into a conical flask device seal to ensure there outtake bottle inserted a burette formulated 600ML: 10% ~ 25% dilute nitric acid was charged burette, in another conical flask loaded 300ML hydrazine hydrate, ensure that installed hydrazine bottle has a vent and installed hydrazine bottles into ice slot. Ensure that equipment containing copper bottle the vent pipe into the bottom of the bottle loaded hydrazine seal (key to the reaction of the success or failure), start reaction burette faster injection of dilute nitric acid containing copper bottle reaction control in about 2h completion of the reaction, to ensure that the ice tank leaving a lot of ice (bottle temperature to the critical point of 37 degrees, to exceed this temperature, scrap) at low temperatures, will be about 50 to about 72 grams of sodium carbonate was slowly added loaded hydrazine bottle, added when you want to be careful, must bring gas masks, gloves. Completion of addition the reaction mixture was put in the refrigerator freezer, about 4 hours to crystallize with a clean filter cloth filter bottling water was added to a solution of the spare (50 g of sodium azide is about dissolved in 100 grams of water), this product is highly toxic ! Good stability in solution, do not worry, fried. Sodium azide in industrial (explosives) used for synthesis of lead azide, here to tell a system azide (more stable) lead the prepared sodium azide added a certain amount of dextrin or carboxymethyl cellulose plus crystallized, such as lead nitrate or lead acetate, plus dextrin obtained crystals should be short columnar, of carboxymethyl cellulose, the crystallization should be spherical polycrystalline, also known as α-crystalline form, and stability of such crystallization. β-crystal form should be directly with stack sodium azide with lead salts reaction, needle-like crystals, sensitive, unstable, explosive. Well, know that Dora, write poetry and go, we have doubts or discovered the error must be pointed out that, thanks! ! Bold research under the premise of not jeopardizing public safety.

HNO3 (dilute solution) + Cu → NO ↑

HNO3 +2 NO +3 N2H4 = 3HN3 +5 H2O

This idea is derived from: http://bbs.kechuang.org

[Edited on 31-8-2012 by detonator]
View user's profile Visit user's homepage View All Posts By User
Phantom
Harmless
*




Posts: 43
Registered: 26-4-2011
Member Is Offline

Mood: AUDENDUM EST,FORTES AUDIUVAT IPSE DEUS

[*] posted on 1-9-2012 at 03:44


The common synthesis method is the "Wislicenus process," which proceeds in two steps from ammonia. In the first step, ammonia is converted to sodium amide:
2 Na + 2 NH3 → 2 NaNH2 + H2
The sodium amide is subsequently combined with nitrous oxide:
2 NaNH2 + N2O → NaN3 + NaOH + NH3
Alternatively the salt can be obtained by the reaction of sodium nitrate with sodium amide.

[Edited on 1-9-2012 by Phantom]




Adrenaline filled experimentalism.
View user's profile View All Posts By User

  Go To Top