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Author: Subject: Tri-Nitrocellulose
IgnorantlyIntelligent
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[*] posted on 23-10-2003 at 14:24


When nitrating cellulose with ammonium nitrate and sulfuric acid, my cellulose totaly disolves in the acid. Ive tried it 3 times and the same thing happens every time.
I know we arent allowed to post things about failed attempts at synthesis's because of some strange reason but If anyone cares to throw an answer out to what might be going wrong I'd appreciate it alot.
BTW, over 6 threads in this forum alone have been closed in the last 6 days. Its not like closing it takes up less room on the forum right? Why not just leave it open? Im not questioning the great forum admins so dont take this the wrong way...I was simply wondering.




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[*] posted on 23-10-2003 at 14:53
An explanation


The reason these threads have been closed is because they are not focused on chemistry, are not about novel procedures, and tread ground that has already been tread many times before in other forums. Discussion of these well-known topics is discouraged here as a matter of policy. Beginners are welcome here, but only beginners who are able and willing to be self-directed learners. If you haven't read the FAQ, let me remind you of good sources of information for most simple questions:

The Usenet groups alt.engr.explosives and rec.pyrotechnics, and their archives on Google Groups
The Explosives and Weapons Forum archives
books, from an actual library or in electronic form (http://bcis.pacificu.edu/~polverone/, for example)

The books are especially important, since you can't tell BS from good information until you have some basics down.
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IgnorantlyIntelligent
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[*] posted on 23-10-2003 at 21:03


Ok, I'm not questioning the way you run the forum. I like being able to use this forum and read the very informational posts and replies people write.
And at the E&W forum, they ban people left and right. The admins here do not do that which is very much appreciated. Sorry if i ofended the forum or its admins in any way...it wasnt my intent to do so.

Now for a word on NC.
Since DDT occurs very fast, and with VERY little confinment. Would NC make for good detonators ignited by a fuse?
Also, what happens to the chemical structure when NC deflagurates or detonates? (what is given off)




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\"To fight for nothing is to love nothing, to die for something is to have lived for something.\"
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[*] posted on 2-11-2003 at 05:17


NC wont detonate.I know that some smokeless powders can detonatw when initiated but those are just the ones with a high enough amount of nitroglycerin which prety much makes them gelled dynamite.
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[*] posted on 2-11-2003 at 13:45


No, nitrocellulose does detonate. IIRC, it undergoes DDT pretty easily when it's low density (freshly prepared from cotton or the like), which is one reason it took so long before it could be used to replace black powder as a propellant (it had to be tamed first).
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[*] posted on 10-11-2003 at 15:21


At what temp does the tri nitrate isomer form for Nitrocellulose? I made some about 3 days ago. I deflagrated it but it burnt slow. More like the Dinitrocellulose version. I was using an ice bath and I let the cellulose sit in the acids for 20 minutes. After nitrating I washed it in a bicarb solution and then let it sit in water. Dryed it for 2 days out in the open. What could be the problem? Or did i just need to separate the un-nitrated cotton with a solvent?
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[*] posted on 11-11-2003 at 06:50


i think that the level of nitration depends more on the concentration of used acids, than temperature.
I once made NC with 70ml H2SO4 96% and 50ml HNO3 65% for 5g of cellulose at about 15 deg.C and the NC burnt VERY rapidly.
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[*] posted on 25-9-2004 at 14:33
Burn Rate - Original vs dissolved


I recently made some nitrocellulose out of cotton. Good fast burn rate, almost no ash left behind.

So I dissolved some of this in acetone. Nearly all of it dissolved - just a small thread of cotten left behind. Upon drying in a glass dish, the product resembled scotch tape at the edges where thin (transparent plastic-like substance), and it resembled paper where thicker (white translucent substance). When ignited, it burned <i>much</i> slower than the original nitrated cotton did. Why would this be? It still left very little ash, but the burn rate was not impressive.
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[*] posted on 25-9-2004 at 15:18


The same thing has happened to me. The freshly made NC made from the cotton on top of the aspirin bottle, burned well, even with a little "fwump" sound.
After disolving in acetone and crashing into water, it still burned fast but I got no "fwump" anymore and the burn rate was noticable slower.

I believe it has something to do with in the freshly made type having large spaces for flame to propagate through very fast as oposed to the one after disolving in acetone which has fewer spaces.

Also, after disolving in acetone and crashing into water the NC felt more "plastic" as opposed to the "cotton" feel of before. There also seemed to be less NC in terms of volume after disolving in acetone despite the mass being the same so I am led to believe that the density has increased a bit. I believe that a higher density would also slow down flame propagation due to decreased surface area.
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[*] posted on 26-9-2004 at 22:57


Dear IgnorantlyIntelligent
I assume you used too few Ammonium Nitrate. Sulfuric acid dissolves cellulose. If your mixed acid contains too few ammonium nitrate, your cellulose will dissolve like in pure sulfuric acid.
In theory a nitrating mix of 1g AN dissolved in ~1.5ml 98% sulfuric acid corresponds to an nitrating mix of 1g pure HNO3 with 2g H2SO4. The nitating must be cooled to minus 10 degree centigrad prior to adding the cellulose. When as much cellulose as can be drowned in the acid-AN-mix is added, continue cooling for 30 min. Then let the mix warm to room temp. an let it rest for 3 hours. Use toilett paper as cellulose, but you have to boil it in 2% NaOH solution for 30 min and wash it and let it dry prior to nitrating. This removes traces of fat in the cellulose. With unprepared cellulose the quality of the NC will be poorer which means there will be more dinitrat in the NC.
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[*] posted on 27-9-2004 at 03:50


I use cosmetic cotton wool balls, the usual drain cleaner acid (minimum 93% sulphuric) and 70% HNO3.
2:1 by volume of sulphuric:nitric.
I add as much cotton as the mixture will take (so it's all soaked in acid at least) and leave it somewhere cool and dry for at least 24 hours - usually more. Then remove and wash, neutralise with carbonate, wash some more etc until there is no acid reaction with carbonate or litmus. Then dry thoroughly.

My product always burns fast with a nice yellow flame and about 1g in a tube is good a for a firecracker. Never tried to detonate it though, nor have I tried with sulphuric and an inorganic nitrate.

Never managed to use it in a cap though - it just doesn't seem to DDT.

[Edited on 27-9-2004 by AngelEyes]
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wink.gif posted on 28-9-2004 at 21:01
Ouality of the NC


Hallo AngelEyes
Please could you report me the quality of the NC obtained by your process. Take some NC and rub it betwenn your thumb and your forefinger to get a small ball (about 4 mm in diameter). Then light it.
Is there any carbon risidue?
My NC burns without risdue when fluffy, but when I squeze the air out of it there is some porous carbon left after burning.
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[*] posted on 29-9-2004 at 00:34


" When ignited, it burned much slower than the original nitrated cotton did. Why would this be? It still left very little ash, but the burn rate was not impressive."
I think its like when you add water to BP to cake it, maybe the componds bonded together rather than be beside each other.
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[*] posted on 29-9-2004 at 03:03


There is a tiny amount of residue but it's negligible. The more I squeeze it together the slower it burns...but not that much slower. If you colloid it (with Acetone) and let it dry then the resulting plastic burns quite predictably and stably and leaves the same negligible amount of residue.

I sometimes take the neutralised NC and dunk it into an inorganic nitrate solution then dry it again. This gives a little more kick and helps to increase the Oxygen balance.

By and large I use it for firecrackers and lacquer (when mixed with Acetone to thge consistency of thin honey).

To Tokat: The reason un-nitrated burns much slower is because the nitration process implants the nitrate ion (NO3) into the cotton. The Oxygen (contained within the NO3 ion) is therefore present on a molecular level and it's this molecular combination of fuel (cotton) and oxidiser (NO3) that allows the flame to propogate waaaaaay faster than if it were to burn in atmospheric Oxygen alone. That's probably not a great explanation but I think it's accurate. I'm sure I will be corrected if it ain't...

[Edited on 29-9-2004 by AngelEyes]
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[*] posted on 29-9-2004 at 23:25


How does the plastic effect happen does NC bond with NG or does NG type of deffuse in NC.

thanks angeleyes.

[Edited on 30-9-2004 by tokat]
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[*] posted on 30-9-2004 at 03:37


When did NG get into this thread?
It matters little as I have never prepared NG so have no experience with it.

I <i>think</i> it's the NC dissolving in the NG but don't quote me on that. There are plenty of other members here who know far more about it than I.

EDIT: Ah, he means Acetone not NG....I think.
Raw cotton (normal or gun) is like a maze of tiny, tiny tubes. When nitrated it's like a big ball of quickmatch. When colloided (with Acetone) it forms a plasticky type material and all the tubes are gone. So it takes longer to burn as the flame can't flash through the whole thing.

[Edited on 30-9-2004 by AngelEyes]
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[*] posted on 31-3-2005 at 06:28
Huzzah! NC


Sorry to bring up an older thread but I thought it best not to make a new one.

When he mentions NG I think he is talking abouit the preperation of blasting gelatin.

I finnaly bought myself some more (25 kilos) of KNO3 and a bottle of analytical H2SO4 (98%). I also got some cotton face/makeup pads.

Here is my acid:
http://img.photobucket.com/albums/v466/mephistosminion/SANY0...

Here is Cotton:
http://img.photobucket.com/albums/v466/mephistosminion/SANY0...

Here is It nitrating in a bat of 90ml H2SO4 and 75g KNO3:
http://img.photobucket.com/albums/v466/mephistosminion/SANY0...

Here is the yeild:
http://img.photobucket.com/albums/v466/mephistosminion/SANY0...

Here are consectutive from a video of my NC burning:
http://img.photobucket.com/albums/v466/mephistosminion/NCfra...
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[*] posted on 31-3-2005 at 13:39


Did you add water to the mix at all? I am surprised your batch looks so 'liquid'.
If not, then the degree of nitration should be high. Adding more H2SO4 should further that purpose.




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[*] posted on 31-3-2005 at 15:18


I didnt add any water but I started with only 60ml H2SO4 and 50g KNO3. I added alot of cotton and felt it was too thick. So I mixed another 30ml H2SO4 and 25g KNO3 in a seperate beaker and added that to the reaction.
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[*] posted on 1-7-2005 at 01:42


i attempted the procedure 2 times... in the first, with powerlabs proportions, the product was not very good, lots of residue left, slow burning... the second with brainfever proportions, that are triple of that's of powerlabs (concerning acid quantity/cotton) and it worked perfectly, instant combustion, pratically no residue left, and with the no raffinated in acetone product!
powerlabs proportions are uncorrected or i could have done an error during the first procedure?

Sorry for my bad english :)
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[*] posted on 2-7-2005 at 07:15


Microcrystalline cellulose should be easily nitratable , but I have never seen it described . IIRC , cellulose flour is what is the name for it as a food additive and it is soluble like starch , but has a small number like 8 cellulose units which has a crystalline form . There are small bottles sold as a dietary supplement ,
" soluble fiber " type of material for an inflated price . But the same material is sold cheaply in bulk as a thickener additive for foods , similar to rice and potato flour .
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[*] posted on 2-7-2005 at 08:34


Roscoe,

You are correct that microcrystalline cellulose is easy to nitrate, much easier in fact since it is more dense that cotton and you can get more in the mixed acids. You can stir it more effectively and it nitrates faster since the small crystals are better exposed to the acid. After nitration is complete, leaving it to stand causes the MCNC to float to the surface of the acid in a dense layer that can be pulled out of a beaker in virtually one chunk. This brings along less spent acid and allows faster quenching thus keeping the N content as high as possible. Stabilization is a breeze as well since MCC does not have the tubular cellulose structure that cotton has therefore it traps less sulfuric acid esters. A short boil is all that's needed. The best thing about MCNC is that it retains the physical characteristics of MCC. It compresses very well in a hard and durable plastic form. Tabletted material looks very much like ivory.

I know a little bit about this since a while back, I applied for a patent on MCNC. They are slow at the USPTO it's not even in the pending list yet. My last patent took 1.5 years to show up on the website after filing.
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[*] posted on 2-7-2005 at 10:05


It makes sense that the nitrated product would likely be a superior material as a base for smokeless powder too . It would probably function especially well as a fast pistol powder or rimfire powder where a small granulation is desirable , and a highly nitrated dense cordite of very
regular and dense grain , and high loading density would be a real power boost in small caliber cartridges .

When the grain size of nitrocellulose is at about 100 mesh and smaller , it is also readily initiated when compressed as a base charge in a detonator and initiated by a primary explosive . If my guess is right , nitrated microcrystalline cellulose should have properties more similar to PETN than to the more common nitrocellulose from long fibered sources .
The stability and power and economy of manufacture is probably somewhere between the two .

If the material compresses easily to a dense grain structure , it may also have interest as a rocket propellant .

It should be a versatile high energy material , of economical manufacture .
I'd be a bit surprised if the powder manufacturers were not already onto its use , perhaps as a component in some
powder formulations having different blends of cellulosic precursors . There are such things practiced in the art and known but not published , and it wouldn't be surprising if this proved to be one of those " trade secret " sort of items .
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[*] posted on 2-7-2005 at 11:40


That's exactly what I thought when I started making MCNC some years back. But a thorough patent and chemical search revealed exactly no mention of the substance.

I came across the idea while working with nitrocellulose as high nitrogen fuel for use in indoor pyrotechnics. Regular fibrous NC is very difficult to compress to a sufficient density for my uses with out colloiding or the addition of other chemicals functioning as binders. Another problem was scrubbing in the dies upon ejection after high pressure compression. This required the addition of lubricants which further slowed the combustion. I happened to be looking at a bottle of vitamins and it mentioned MCC as an ingredient. After searching the chemical I was immediately struck with the idea, what if it could be nitrated.. would it retain it's favorable characteristics of density, compressibility and inherent lubricity. To my surprise and glee, it does! I have done no testing of MCNC as a high explosive.

The only thing that probably would limit it's usefulness in firearms and explosives would be the cost. Different grades of pure MCC in particle sizes favorable for nitration are on the order of $5.00/lb. One idea that has struck me is it could possibly be compressed into a case form such that it could accept both primer and projectile for case less firearms rounds. Upon compression the strength and machine ability of this material is almost identical to the plastic, "delrin" also known as acetal.
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[*] posted on 2-7-2005 at 11:46


Upon reading this thread from the beginning, I see that Rooster mentions MCC and it's characteristics back in
17-10-2003
He was on the right track and probably should have continued with his research.
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