Procedure for preparing a solution of sodium azide

This procedure does not require either sodamide (NaNH2) or hydrazine, which
makes this procedure more attractive.
WARNING: Sodium azide gives off highly posionous hydrazoic acid (HN3) fumes
when mixed with water. Keeping the pH alkaline helps prevent the fumes, but
solutions should be kept in a well sealed container, and stored in an area with
plenty of ventilation. Acids should not be added to sodium azide, since this will give
off the poison gas.
Nitrourea can be made by a cold nitration with mixed concentrated nitric and
sulfuric acids on urea, similar to the procedure for nitroguanidine. The difference is
that nitrourea should be kept away from water, since it can hydrolyze and be
degraded.
Preparation of Nitrourea
9 grams of urea nitrate, was added in small portions to 32 mLof ice cold (-3 C)
concentrated sulfuric acid at such a rate that the temperature did not exceed 5 C.
Total time for addition was approximately one-half hour, after which the mixture
was poured on 75 grams of ice. The white precipitate was filtered, washed with ice
cold water, just sufficient to cover it, and air dried. Material obtained weighed 5.3
grams and melted with decomposition at 157-158 C.
20g of nitrourea, 65g of zinc dust and 10 mL pure methanol (without water) are
mixed in mortar and ground into a thick paste. A glass beaker is filled with 12 ml of
glacial acetic acid and 15 mL pure methanol, then placed into an ice water bath.
The cold nitrourea and zinc paste is added in small portions with gentle stirring. The
reaction will give off much heat, so the initial portions should be smaller, and added
over longer intervals of time, so the mixture does not overheat. The rate of addition
should be adjusted to keep the temperature from rising too much, ideally around
10 degC. Do not allow the temperature at any time to rise to 35C. If the mixture
becomes too thick or the temperature rises too rapidly, cold methanol should be
added (no more than 50g). The additions to the paste should be done over a time
of around 3 hours.
After completion, the beaker containing the reaction mixture should be allowed to
stand in ice water bath for another hour. The beaker is then removed from bath
and allowed to warm slowly to normal temperature. The final volume of the mixture
should be around 130 mL. After one hour at room temperature, the mixture is
placed on water bath, heated to 25 degC, and stirred for 30 minutes, then heated
to 32-35C, and stirred for 30 more minutes, finally being heated to 40 degC and
stirred at this temperature for another 15 minutes.
When the reduction reaction is complete, the solution is immediately filtered using
a vacuum funnel, and filtering the solid product dry. The solid is washed with 90 mL
of water, then filtered. The solids left over are discarded. The filtrates (solution that
dissolved out the semicarbazide and passed through the filter paper) are combined.
The solution will contain around 10g of dissolved semicarbazide. The yield for the
reaction of nitrourea to semicarbazide at this point is 60%)

Dilute sulfuric acid (5% solution) is added to the solution until the pH just reaches
6.5. It is important that the resulting solution not be too acidic or contain excess
acid. It may be helpful to pre-cool the acid solution.
9.2g of Sodium Nitrite is separately dissolved in 125 mL water, and this solution is
reacted with the semicarbazide sulfate solution (which contains the equivalent of
10g semicarbazide). The addition should be slowly done, over the period of roughly
ten minutes, the temperature should be kept below 20 degC, but ideally 10 degC is
good. The reaction may give off some poisonous vapors so do it outside or in a
fumehood. After this reaction, immediately proceed to the final step, which is to
gradually add a pre-chilled concentrated solution of sodium hydroxide.
The resulting solution contains dissolved sodium azide, along with byproducts of
sodium carbamate, and sodium sulfate (much of it will precipitate out as solid
crystals on the bottom below 15 degC).
Read more: http://energetic.proboards.com/thread/4#ixzz30iozr8Sw

Prepare a solution of 40g (1,0mol) NaOH in 50-60mL distilled water. Cool down and adjust the
volume to 100mL (10M conc.). Add 62g (1,0mol) 80% hydrazine hydrate and cool down to 0-5C.
Under temperature control of 0-5C (ice bath) and stirring, add dropwise 90g isopropyl nitrite
over an hour. After adding all isopropyl nitrite, stirr by 0-5C for additional 15minutes, then stop
stirring and let the mixture warm up to room temperature. After this is done, evaporate almost all
volatile parts under vacuum. You may evaporate the reaction mixture by heating it gently, but
avoid open flame or similar because of the isopropanol and traces of isopropyl nitrite boiling off
the mixture. Avoid also exposure to iPrONO, as it is toxic. After evaporating all liquids, the solid
rest is fairly pure sodium azide. Do not dry the solid substance by heat! Just put it in an desiccator
and let it dry by normal teperature. Keep in mind that it is a violent poison.

Preparation of sodium azide - Stoll way

first Preparation of amyl nitrite

200 g amyl alcohol mixed with 210 ml 34% HCl in

2000 ml conical flask so merged to a cooled solution after
adding parts cooled solution of 157 g NaNO 2 (keeps the
temperature at 0-4 C). He then let the mixture cool about 4
hours. Then add 400 ml of water and shake the bottom layer

containing the product and the top of the aqueous solution of

NaCl.

Amyl nitrite is a yellow oil, insoluble in water, soluble in

ethanol. Boils at 94-97 C, its density is 0.902 g cm -3 .
Couples amyl nitrite cause headaches.

second Preparation of sodium azide Stolleho way

33 g Hydrazine sulphate after 5 hours stirred with 62 g

of NaOH (half the stoichiometric amount) and 270 ml of water
(laboratoni temperature). Then pour 4 liters of ethanol, 200 g
of amyl nitrite, and add 62 g NaOH (second half). The entire
volume of the mixture is stirred for 40 hours. Then the basic
volume of ethanol is distilled off. Amyl alcohol is odestiluje
with water vapor and the department is recycled back into the
production of amyl nitrite. The remaining liquid contains a
mixture of sodium azide and sodium sulphate. Sodium and
sodium sulfate are separated on the basis of their different
solubilities. Yield: 60-70% of theory

Reflux 0,4 M hydrazine sulfate and 77 g NaOH and 156 ml 96% etOH 2 hours. Filtrate the cake out, and
the clear solution cold 'til 2 degree C and add fresh preparated cold (0 degree C) 47,5 g izopropyl nitrile.
(Or the same molar ethyl nitrile) Put this solution in fridge (or in ice bath) let24 hour staying, but usually
shaking. Next day filtrate out the NaN3 and wash with IPA or etOH, dry max.100 degree Celsius