Isopropyl Nitrate (IPN) and Thermobaric Fuels

[nbk2000]

I was wondering if anyone has tried making IPN yet? It's supposedly made the same way as methyl nitrate, so it couldn't be that hard to do, and has its use as a fuel in russian thermobaric warheads like the RPO-A.

[IPN]

SWIM made it once with Cipolla's method.

Take 5 ml of 50%-65% nitric acid, add about 100 mg Urea, cool and add 5 ml IPA, NOT LESS!!! [Using the stoichiometric best amount of IPA, here about 2,5 ml, may cause too much heat generating and decomposion of the mixture.] When you cool the solution you prepared after 1-2 hours a IPN-Phase on the acidic solution should have formed.

SWIM used 50ml 62% HNO3 and added 1g of urea, cooled and added 50ml IPA.
It was used to sensitize AN (making IPNAN), detonated fully with 3g HMTD.

SWIM will try mega's method when he receives the necessary equipment.


EDIT: I made quick search and found these:

http://www.kracik.com/me/w_shmel.html

http://www.janes.com/defence/land_forces/news/jidr/jidr010104_3_n.shtml

[Mr Cool]

I've made it, I can't remember the exact method I used because it was ages ago, but I remember the urea. It was probably almost the same as above.
I do remember several failed attempts, with other methods, which cause huge billowing clouds of NO2 to be formed, spraying acid everywhere. The -OH is easily oxidised...
If you fuck up and get a load of oxidation, then a low yield of TriNM (nitroform) is the result.

Good that it doesn't use sulphuric! This makes it easier on the chems. You don't even need strong nitric, as you can see.
It makes a good sensitiser because it isn't too sensitive alone. I can't remember what its volatility was like though.

IPN, what yield of IPN did you get?

[IPN]

Sorry, I didn't write down the yield.

SWIM will re-test the IPN synthesis in two weeks.. (I have to go to a camp:mad: :mad: )
Then I will take pics and record the yield.

[knowledgehungry]

You mean SWIM has to go to camp ;).

[Mr Cool]

Well I'll be getting some more acetone soon, I'll get some IPA too and give it a go.

[simply RED]

I have made large quantities with cipolla's method, the yield was 70%.
Actually, i upgraded the method.
I tried all kinds of thermobarics last year...
Very extreme explosive is made by:
40% Super Nano Al powder, 10% Nitroglycerine, 49% IPN 1% Urea. All % in mass.
This is soaked in nitrocellulose, without plastificating, just to insure the Al will not go on the bottom. Urea is just for stabilizing, if long term storage will be needed, use stabilizer for NG.
Detonated with 50grams high pressed RDX (not less).

Back on the method.

Use long (50-60 cm) glass tube (2 cm in diamater) (why not PVC with extreme colling). Add first the 59% Nitric acid, with 5-10% urea nitrate mixed in it. Cool to 0 degrees C. Then add the IPA, add the same volume IPA as was the HNO3. Slowly become heating, when the mixture reaches 5 degrees, a violent reaction will start. Very much gas will form. The temperature reaches about 10C. The mixture will bubble and will want to go off the container. After 10-20 minutes the bubbling stops and slightly yellowish layer forms on the acidic bottom. This is the IPN.
Decant the IPN(i used medicine injection to drive it off) and transfer it to other container with 2 times the IPN volume concentrated NaCl solution in water.
Decant again and again with NaCl, then use NaCl, NaHCO3, urea.
Then the last time wash with low ammount of clear water.

IPN is very volatile, so be careful, IPN + AN really makes ANNM analoge.

[Mr Cool]

So, you add the IPA all at once? Do you stir it or leave it to mix on its own? Is the temperature rise necessary for the reaction to proceed, or is it just hard to keep it cool? I have a liebig that would be perfect, after a bit of modification (it is almost exactly the dimensions that you stated), I could run ice-cold water through it to keep everything cool, unless the heat is necessary. Cooling would also be a good idea probably to condense any vapours that might escape, although if the temp only goes up to 10*C it may not be a great advantage.
Also, how much did you produce in a tube of that size? I guess you must have scaled-up Cipolla's method that IPN posted to make a tube of that size necessary.
Well, 70% is not such a bad yield, I'm not sure but I seem to remember mine being lower than that.

[simply RED]

Yes, you add all the IPA at once. Then stirr to mix the ingredients. The 10 degrees (maybe slightly different but about 10 are necessary to react the IPA and HNO3.
I've tried to make this in glass aparature with different dimentions, but only this and test tube worked.
First make attempt in test tube with cooling to see how the reaction goes. Then scale up.
For one time i was able to produce 30 ml IPN (from one cylinder) . But i used 3 such reaction cylinders. Made from glass with external cooling with water- ice mix. From 40 ml IPA you get 25-maybe 30 ml IPN.

By the way, another thermobaric mix peaked my interest last year:
40% Al, 35%NG, 15% acetone, 10% Nitrocellulose
This is gelled mix. Made by first mixing the NC and acetone, then mix with the NG and last mix with the Al slowly. Has the same propperties as the first, but more heat sensitive.

[nbk2000]

The purpose of the IPN in the TB fuel is to act as an oxidizer to increase the combustion rate of the metal fuels. That, and it also helps improve dispersal. Collodial silica gel as a thixotropic gelant is much improved, since you need only 1.5% to gel the fuel, rather than the 10% NC, which adds to the combustion, but not to the same level as the Al/IPN.

I wonder if the nitrate/acid mix could be used instead of neat nitric. Perhaps after diluting the acid prior to adding the nitrate, so it's not too concentrated? Did you guys use anhydrous IPA, or the ~70% drugstore variety? I've got a fifth of everclear (95% ethanol) that I'm wondering could be used to make Ethyl nitrate by this process, or would that require the more vigorous mixed acids?

And why IPN instead of MN or EN? Less volatile? Less shock senstive? Or just easier for poor third-world contries to make?

The TB formulation I got from one of the "Big Boys" that I'm in contact with has more than 70% metallic fuels, with the balance being IPN with the thixotropic silica gellant. It burns at 1,200&degC with a heat flux of ~130 cal/sq cm-sec.

It takes less than 15 cal/sq. cm to ignite denim (the most heat resistant fabric listed), and only 5 cal/sq. cm for second degree burns, so you can imagine what 25x that would do to someones skin! :) (Thermal energies taken from "The Effects of Nuclear Weapons", Wash. DC. '62)

Modern protective equipment is designed chiefly to protect soldiers/police from bullets and fragments, and not blast effects. Consequently, helmets and ballistic armor would provide relatively little protection from a TB explosion, especially when you consider the thermal effects to their clothing (FwoOOSSH!). :D

The best fuel to use for a thermobaric, for both calories/cc and calories/gm, is elemental boron. It has a heat output a third again more powerful then that of the next best TB fuel (aluminum), both for weight and volume. :D

Boron is rather easy to make oneself, if you have plenty of magnesium around, to form it by thermite reduction of boric acid (OTC eye wash solution), which itself is makeable from borax which is as OTC as dirt. :)

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CRYSTALLINE B2O3

Fused boric acid is heated in a loosely stoppered Pyrex flask to 225-250°C; after this treatment the melt retains 8-15% water. Crystallization requires a few days. If a small amount of crystalline B2O3 seed is added to the melt, which contains some water, crystallization occurs very rapidly and the water separates out. Alternatively, fused boric acid is heated to 175°C, at which point crystalline HBO2 separates. The material is then transferred to a closed tube and the temperature is raised to about 236°C, i.e., just below the m.p. of HBO2. As a result the latter evolves water and transforms to crystalline B2O3.

PROPERTIES:
M.p. 450°C; d 2.42-2.46. Hexagonal crystals.
REFERENCES:
I. McCulloch. J. Amer. Chem. Soc. 59, 2650 (1937).

BORON

According to Moissan, very impure amorphous boron, containing about 80-90% B (good enough for TB use. NBK), is obtained by the reaction of B2O3 with magnesium. According to Kroll the optimum yields are obtained as follows:

A fireclay crucible, approximately 20 cm. high and 16 cm. in diameter, is painted with a paste of ignited MgO and sintered MgCl2 and dried in a low-temperature oven. A mixture of 110 g. of B2O3, 115 g. of Mg shavings (the use of Mg powder frequently leads to explosive reactions) and 94 g. of powdered S is placed in the crucible. The reaction is started with an ignition pellet, after which it proceeds vigorously. After the mixture has cooled, it is extracted in water and then in dilute HCl for a week. The residue is treated several times by heating with HF and HCl, washed with water and dried in vacuum at 100°C. The yields are variable, with a maximum of 46%.

PROPERTIES:
Atomic weight 10.82. Gray-brown to yellow-brown powder. M.p. 2300°C; d 2.3. Ignites in air at 700°C. Reacts violently with concentrated HNO3.
REFERENCES:
H. Moissan. Compt. Rend. Hebd. Seances Acad. Sci. 114, 392 (1892); W. Kroll. Z. anorg. allg. Chem. 102, 1 (1918).

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