anapogeetoofar Posted November 2, 2011 Posted November 2, 2011 So, as I mentioned in a related thread, sawdust is nitrateable (<-is that a word?) to high grade nitrocellulose. Nitration of pine yields a slightly aromatic (hard to describe the smell) red/orange product that burns fast but incompletely. Dissolving in acetone and crashing in water helps. Product is insensitive to strikes of a hammer. Curiously, leaving the sawdust in the nitration bath for a few days yields a colorless (well, wood colored) product that smells faintly of nitrogen oxides, and burns very fast leaving little to no residue. Product is sensitive to a hammer blow. Size of the sawdust being nitrated made no difference on the time it took. Fine, powdery wood meal, and full on wood chips all took the same amount of time. The wood chips were fun to play with, looked like ordinary wood chips 'till ignited. Then the spun around on the ground for a few moments and then flew up into the air briefly and dissipated in flight. All I tried was pine, I imagine the assorted terpenes and other organics that pine is full of contribute to that color, and upon sitting decompose leaving pure nitrocullulose. Or not. As it turns out, cellulose has a friend: Lignin. Lignin can be nitrated. Under what conditions? Don't know. Actually, I know almost noting about nitrolignin, only that it exists, is energetic, insensitive, and isn't shelf stable. Or at least that's what Federoff says. That's pretty much my only reference, though it is mentioned in some obscure papers that I don't have access to. Why does this matter? Don't know. Is nitrolignin red? That would explain the initial color. It isn't stable, that explains the disappearance of the color. Its oxygen balance has to be terrible which explains the slow, dirty combustion until the red color goes away. What else could happen to the lignin? Does it just take forever to nitrate completely? I wish I had weighed the product in its red state, then after it lost color. That would at least tell me if the lignin hangs around or not. To further add to the mystery: I read that a UK company made a sporting powder with nitrated sawdust for a while until cordite and friends came into exisitence. The process, according to the reference, takes place in a few hours. Temperature, type of wood, conc of acids are not mentioned, not terribly useful. Maybe they left thiers red? Synthesis is simple enough: standard mixed acids, nitrate salt method works fine, just cant make as much at a time. Put in Ice bath (may not be necessary, I never noticed a temp change unless using moist wood, I er on the side of caution though.) , slowly add sawdust/wood bits, stirring well, stop if you should notice a sharp rise in temp. Continue to add until it you have a thick slurry. keep it cool, I let mine sit at 70-75 F for the few days it took to get it to clear up. Your mileage may vary. Its wood. Don't forget that. Probably the most mild mannered nitration I ever attempted. Anybody want to chip in? PS: Not intended to be HE discussion, seems nitrocellulose is tolerated in the general area, I assume this is fine too.
Arthur Posted November 2, 2011 Posted November 2, 2011 There is formal literature about this topic, you should have the real hard copy books before experimenting. Other than that I'll suggest that the moderators decide what is HE discussion.
Blackthumb Posted November 2, 2011 Posted November 2, 2011 (edited) Do a search on Prussian artillery captain Schultze for some facts on nitrating sawdust/wood chips...he was somewhat successful...don't forget that you will be dealing with 'detonation' instead of an 'explosion' with nitrated compounds....best left to someone with HE bcakground... Edited November 2, 2011 by Blackthumb
anapogeetoofar Posted November 2, 2011 Author Posted November 2, 2011 Alright, a few things need to cleared up here: 1. Nitrocellulose and its synthesis is discussed here routinely, that is what I intend this to be. 2. I have experience with HE. Done with that. Forever. A few Mg of a perchlorate ester told me I was no longer within the limits of acceptable risk. I listened. No interest In that anymore. It was fun while it lasted, and I wouldn't trade that experience for the world. Despite how it may seem, I am an extremely cautious person, I approach nothing haphazardly, and do not attempt anything that can not be controlled or made acceptably safe. 3. The whole point of this is that its another route to nitrocellulose, I thought it may be more efficient as you can get more sawdust into a nitration bath than cotton. Herr Schultz (thanks for that blackthumb) also seemed to believe that. Look, If this (or anything else I have posted) isn't appropriate for this forum, or isn't relevant, then tell me, please. I can't tell how to make your red stars redder, or what the best prime is, but I can tell you 101 different ways to make a rocket go up. Novel procedures, compositions, and contraptions are my bread and butter. If that isn't relevant here I'll stop. You have to tell me though.
Potassiumchlorate Posted November 2, 2011 Posted November 2, 2011 NC was actually invented or, better, discovered, by another German gentleman, namely Christian Friedrich Schönbein. Today the feminists would kill you for wiping up HNO3 with your wife's apron. But it's well known, and I don't think that I help any "kewl" here, because I don't give out any details, that NC is better made a bit slowly and with less concentrated acids, at least the nitric.
Arthur Posted November 2, 2011 Posted November 2, 2011 Nitrated cellulose has different properties according to the degree of nitration. At a low degree of nitration there are uses for varnish and paints at a medium degree it burns rapidly an d becomes a propellant, at the highest degree it detonates powerfully. Other properties change too especially the solubility in solvents (and the solvents themselves). ALL of the usual sources of cellulose pose problems because of their naturally porous form. -They absorb acid residues into their structure and this tends to catalyse their decomposition which (as a current thread) may go off suddenly after a random time with disastrous results.
NightHawkInLight Posted November 2, 2011 Posted November 2, 2011 Nitrated cellulose has different properties according to the degree of nitration. At a low degree of nitration there are uses for varnish and paints at a medium degree it burns rapidly an d becomes a propellant, at the highest degree it detonates powerfully. Other properties change too especially the solubility in solvents (and the solvents themselves). ALL of the usual sources of cellulose pose problems because of their naturally porous form. -They absorb acid residues into their structure and this tends to catalyse their decomposition which (as a current thread) may go off suddenly after a random time with disastrous results. This is going too far. NC is not AP. A spontaneous detonation of anything less than an industrial quantity is about as likely as getting struck by a flying rodeo clown. Without a blasting cap the worst a hobbyist quantity will do is catch fire. Even that is far from likely if it is properly processed and used up within a quarter of a decade. In the same respect as ammunition containing nitrocellulose based powders, if kept cool and out of the elements it will last ages if need be. There are far more dangerous things we use building fireworks than NC, and if treated like any pyro composition there is nothing additional to worry about.
dagabu Posted November 2, 2011 Posted November 2, 2011 ... is about as likely as getting struck by a flying rodeo clown. LOL! Nice color commentary NHIL. -dag
Blackthumb Posted November 3, 2011 Posted November 3, 2011 "... is about as likely as getting struck by a flying rodeo clown. " That's precisely why I sit high in the stands!! Good one Hawk...
dan999ification Posted November 3, 2011 Posted November 3, 2011 i'll have to find the vid on the tube but ive seen nc/guncotton detonate confined lit with only bickford fuse in a side by side test with bp to demonstrate the power difference between the two when rock blasting they used 10 times [or something along them lines] more bp than nc and the damage by the nc was far superior to the bp damage, i tried to find it for the other thread but no luck bare with me.that said i agree it is not the most dangerous pyro comp used prepared correctly. dan.
psyco_1322 Posted November 3, 2011 Posted November 3, 2011 Being that NC is a secondary, its rather impossible for it to go high order with a piece of fuse. That must be some "modified" stuff that was in the video. All the times I've made NC, using a H2SO4/Nitrate bath, and washed very well, it has never started any decomposition in storage. I've kept some around for probably the better part of 2 years I'd say, it still looks like cotton. But I don't whack mine with a hammer, I just dissolve it into acetone for lacquer.
NightHawkInLight Posted November 3, 2011 Posted November 3, 2011 i'll have to find the vid on the tube but ive seen nc/guncotton detonate confined lit with only bickford fuse in a side by side test with bp to demonstrate the power difference between the two when rock blasting they used 10 times [or something along them lines] more bp than nc and the damage by the nc was far superior to the bp damage, i tried to find it for the other thread but no luck bare with me.that said i agree it is not the most dangerous pyro comp used prepared correctly. dan. I can see this being true, at least in effect. Whether or not it detonated NC is capable of much higher pressures than BP when confined and ignited. If confined in a tapped stone with a meter of packed sand above it all the energy that is contained in the NC is going to shatter that stone. I do not think it would need to detonate to do so. We know NC in particular has a powerful deflagration as evidenced by the near 3000fps muzzle velocity of some NC propelled rifle rounds. On the other hand, under the confinement of quarry blasting I can also see NC being able to potentially go high order without a blasting cap when the first segment burns and exerts extreme pressures on the rest. In any case, that is not a situation many of us will have to consider when using NC for fireworks purposes.
Potassiumchlorate Posted November 3, 2011 Posted November 3, 2011 NC was actually used in all military devices before TNT and the likes were invented, but you need a blasting cap for it to go HE. Though the deflagration of it is also violent.
dan999ification Posted November 3, 2011 Posted November 3, 2011 NC was actually used in all military devices before TNT and the likes were invented, but you need a blasting cap for it to go HE. Though the deflagration of it is also violent. i only said because it suprised me not to argue, it was a segment on detonation by a bbc program,guncotton is prone to detonation when heavily confined/tamped which is the reason it was phased out as a propellant and smokeless powder was invented and favoured. dan.
Potassiumchlorate Posted November 3, 2011 Posted November 3, 2011 It is possible to detonate it without a blasting cap, yes, but it needs pretty extreme circumstances. I first got obsessed with NC as a boy, reading From the Earth to the Moon Those guys use 200 tons of NC to fire a hollow projectile with astronauts to the Moon. As a boy in a country with hard regulations on chemicals I could only "borrow" a couple of grandpa's shotgun cartridges to get hold of NC just to see what it was like. It would take me about 20 years more before I could synthezise it myself, in quantities of a few grams. It is worthy of respect.
Mumbles Posted November 3, 2011 Posted November 3, 2011 This has ventured slightly beyond my comfort level for an openly discussed topic. For what it's worth, I don't know if I've ever knowingly or really intentionally allowed the synthesis of NC to be talked about in the open part of the forum. I guess it sort of depends on application. There was some discussion recently related to stabilization and such in another thread, but that is about as far as I'd be willing to let it go. NC is kind of a grey area topic, as it is quite useful for certain pyro applications, but the homemade variety tends not to be the same sort of nitration level that one typically uses for these applications. It is also one of those reactions that does not scale up particularly well. There are different procedures, safety requirements, etc. when doing large batches. These sorts of things are not particularly trivial either, so it's really almost required to be shown how. I've been told that there are really only a few dozen people in the world who can do this processes on an even relatively moderate scale (1-2lbs at a time). I've been shown how, and even I'd have reservations about giving it a shot.
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