Question about MCC nitration

[oldguy]

Reacting sodium nitrate + relatively pure sulfuric acid produces nitric acid.

 

If you added microcrystalline cellulose (MCC) to the mixture. Would it nitrate the MCC to some slight degree?

 

I ask because highly concentrated sulfuric acid is relatively inexpensive locally, while nitric acid is fairly expensive to buy in bulk amounts + shipping costs.

 

I am not looking to make highly nitrated microcrystalline nitrocellulose (MCNC).

Possibly just nitrated enough to make it as combustible as stearic acid or paraffin, for instance.

 

The purpose being for use as a combustible binder and/or to produce star rolling seeds that will compact into a hard durable plastic like mass under relatively low pressure.

 

　

Edited April 6, 2012 by oldguy

[oldguy]

I realize "Nitric" acid & nitration is a touchy subject.

 

If anyone has the answer to my question & don't want to post it publicly.

 

You could always PM me.

Edited April 5, 2012 by oldguy

[pdfbq]

OK Oldguy.. did not answer because of the nitration. I'm not a chemist, thats why I did not respond.

 

The answer is it will nitrate to its max!

 

It is I believe not that convenient because your nitration mixture will be very thick but it will definitely nitrate.

Edited April 5, 2012 by pdfbq

[oldguy]

GLEAMED FROM OTHER INFO: NOT SURE HOW FACTUAL IT IS: But, It seems plausible

Except I think a better wash & neutralization would be required

 

Nitration of MCC is straight forward using about any of the typical nitration methods. MCC is formed by chemical removal of the amorphous cellulose regions, usually with HCL, leaving practically pure crystalline alpha cellulose. A weak nitration mix will result in a visibly identical finished product except for the actual nitrogen content. Time to reach equilibrium depends both on the strength of the nitration mix and the particle size of the MCC. 10 to 30 micron MMC will complete in a matter of minutes. Whereas 200 micron material may take a few days.

 

If you use coarser sizes, 50+, and shorter soak times, you will have overall lower N contents. Once nitration is complete, upon standing, the MCNC will rise to the surface of spent acids in a soft mass that can be easily removed and immediatly quenched in water. This mass carries very little acid with it in contrast to cotton. Wash repeatedly with cold water, then a short boil. MCNC typically will result in higher finished N contents with a given acid mix compared to cotton.

Edited April 6, 2012 by oldguy

[pdfbq]

Maybe it works very well when MCC is a powder because it's more easy to stir in.

When finished dump everything in a big bucket of water, when washing get rid of the acid as fast as possible is the idea.

Then neutralize.

Edited April 6, 2012 by pdfbq

[FrankRizzo]

Oldguy - It will work. However, as pdfbq pointed out, the resulting mixture of sodium sulfate and nitric acid is quite thick. It will be difficult to control the temperature during the nitration. If you use ammonium nitrate, you'll get a better result.

 

If you have access to methylene chloride and a simple distillation rig, this thread might have some useful info for you: http://www.sciencemadness.org/talk/viewthread.php?tid=16589

[NightHawkInLight]

It will work fine either with sodium nitrate as you suggest, or ammonium nitrate. Ammonium nitrate is easier to use because there will be no solid byproducts in the mixture, but even with another nitrate creating a lot of solids it won't matter much with MCC. The solids make stirring cotton a pain because it gets matted and crystals solidify between the strands, but with MCC there are no strands to get tangled. Stirring should be no trouble at all, and the solids will dissolve in water leaving the MCNC behind.

 

Here's some NC using potassium nitrate in the nitration:

http://www.youtube.com/watch?v=Nbt057a8Zzc

 

And here's ammonium nitrate:

http://www.youtube.com/watch?v=J3Ot4AcO47Q

 

No difference in the final product.

 

Edit: I forgot about temperature control as Frank mentions. The key is slow addition of the cellulose. Keep the mixture in an ice bath and stir with each addition of cellulose. Once you have added it all to the mixture let it sit for a few minutes and the ice bath can be removed. With the initial heat increase from addition of cellulose dissipated there's little chance of a runaway, and the higher reaction temperature outside of the bath I've found makes for a higher quality product.

Edited April 6, 2012 by NightHawkInLight