Guncotton

[Some Guy]

Hello all, I know you guys frown upon new members posting new threads, but I have some questions. I am looking for an explosive that is powerful, easy to make, and not too dangerous. Any suggestions? Just kidding :D, I'm not that kewl. Anyways back to the point. I am very interested in nitrocellulose and nitrostarch explosives. They are not too difficult to produce and are easy on the budget. However, lighting my nitrated cotton and watching it burn has become unamusing. I have read on numerous websites that nitrocellulose explosives become more powerful when wet, and compressed. I have yet to try this method of detonation, and am very interested. Has anyone tried this, and if so, is there any increase in VoD than if say the guncotton were merely packed dry into a container? I thank anyone who has any information on this subject. Also, I would like to know what everyone else's "recipes" are for nitrocellulose and nitrostarch explosives. Thanks again, and my appologizes for breaking the rules. Oh, and one more thing. I have heard that the amount of water one should use is anywhere from 5%weight water to 10%. Does anyone know the correct amount? Thanks.

[THErAPIST]

Well this was your first post and you made a new topic which WASN'T in the watercooler so I'm sure you'll get reamed once a mod shows up, but I'll state what I know anyway.

From what I've read wet NC doesn't burn, It has the same or near the same VoD as if detonated dry, It can be Detonated with dry NC, and it's not the easiest thing to detonate.

You would probably be better off detonating it dry or using it in mixtures with other explosives. ANNC, NCAP (AP putty), blasting gelatin (NG + NC), or NIPOLIT.

[mongo blongo]

NC will not burn when wet. Instead of packing your NC into a container you should dissolve it in acetone and let it dry. This will increase the VOD.

[zaibatsu]

I thought if you let NC dissolved in acetone and poured into a container dry it would leave voids?

[kingspaz]

Some Guy, you're aware you're breaking rules BUT this this hasn't been discussed in a long while so will remain open plus i have things to say on the matter :D

zaibatsu is right, it does leave voids.

i've not tried this but maybe NC could be made into a powder by dissolving it into hot acetone then throwing it into soapy water. this *should* result in the formation of small bits of NC. this powder would be alot easier to press to high densities.

my procedure for making NC is as follows:

1g cellulose (in reality this is about 0.5g as cellulose as more cellulose can't be submerged under the acid)
5g H2SO4
2g NH4NO3

1. add ammonium nitrate to the sulphuric acid taking care not to add it too fast.
2. add cellulose to the nitrating acid mix and using an ice bath and hot water bath maintain the mixture temperature at approximately 40*C.
3. hold at this temperature for 45 minutes.
4. pour the mixture into cold water and pull out the NC.
5. wash the NC with boiling water 3 times, then with boiling bicarb solution (bicarb will decompose due to heat forming sodium carbonate so not strictly true) then wash 3 more times with boiling water, then boiling bicarb again, then once with boiling water, once with boiling 10% urea solution then finally one more time with boiling water. (should be storage stable now!)

edit: Some Guy, its not clear from your post as to whether you've tried detonating NC with a detonator. if you haven't then you should try it. its pretty easily detonable.

[Mr Cool]

I've never had success in powdering NC by precipitation of a solution by dumping it into water. Generally the solution, which is quite thick, at least compared to water, is impossible to agitate sufficiently under the water. Therefore it forms medium-sized droplets at best, the outside of which form a layer of NC, as acetone is lost, and normally the end result is a load of squashed little irregular blobs of NC.
Maybe if you had a high-speed blender or something similar, and you didn't mind if it all got totally gummed up with a layer of NC, then you could put some water in it, turn it on to full speed, and slowly pour NC solution into the rapidly stirred water. This might break everything up well enough to at least granulate the NC. I doubt you could powder it, but it might get it fine enough to use.

"Well this was your first post and you made a new topic which WASN'T in the watercooler so I'm sure you'll get reamed once a mod shows up"

Please, can everyone just leave the warnings to the moderators?

[Trinitrotoluene]

I never had success with powdering NC. I dreamt of taking some nitrocellulose added it to acetone then it dissolved, the solution was added to 1 times the amount of water, the only thing happand was fibers formed. But no powder.

Mr Cool is it possable to scale up the amount of cellulose used? In your synthesis you it uses 10 grams of cellulose but can it double or even triple the cellulose, and the acids? And what extra precaution I must take while nitrateing a large batch?

[Mr Cool]

It can be scaled up, just do it all much more slowly, with really good stirring. Exothermic reactions get out of control a lot more easily in large batches, and also the bulky, absorbent cellulose stops convection currents, so hotspots are more likely when making NC than when making PETN, for example...

[nbk2000]

Supercritical spray evaporation is how industry powders NC to make propellant flakes. Look for a topic by me called "Spray evaporation of explosives" for more info.

[Some Guy]

Thank you all for your information, being from a secluded town there is not much info. out there. I have done further research on the subject, and found in a newer encyclopedia that the modern process is to pack nitrocellulose into blocks with a water content of 15%. Should be interesting to find out how this detonates. And kingspaz, yes I have detonated nitrocellulose with a detonator. Thanks again.

[nbk2000]

It's mentioned in COPAE that commercial NC manufacturers use blenders to shred the NC fibers into little bits so that the acid-nuetralizing wash can be more effective in remove said acid.

[blindreeper]

I have tried the powdering NC with great results. When I was purifying it in acetone like on powerlabs (I had bout 200ml of acetone that needed to go) I came back after an hour to find a slightly off grey coloured solution. I added this to 300ml of water and it precipitated as a fine white suspension. I filtered it and it seemed to clump. I then dried this in a desicator and it was rock hard. I proceded to grind it up in a motar and pestle and this resulted in a fine off white coloured powder that burns like normal NC if not faster.

Thats just my experience with NC

[Chem_of_Explos]

my nitrocellulose burns great in cotton form, but when I disolved it in acetone and let it dry to a powder, it burned patheticaly slowly. Anyone have any idea why?

[Al Koholic]

I just made an interesting discovery last night. While visiting home this weekend, I noticed a new, gallon sized jug of pool product that my parents purchased. The jug contains about a pound or so of colloid-sized 100% cellulose powder. When you open the jug, it'll just start floating out on air currents if there is any disturbance.

A company by the name of BioGuard makes it for use as a water clarifyer. Apparently it aids in the removal of ultra small particulate matter from the pool water. Anyway, this would be an interesting substrate to perform nitration on.

The experiment would have to be highly controlled (rate of addition to nitrating mix, heat, time, etc) due to the very large surface area of the cellulose involved. Anyway, it may be that you can use this stuff to make a good NC product which emerges from the nitrating mixture already in fine powder form. Filtration would probably be a bitch and managing this shit might pose a slight problem due to its incredibly small particle size and tendecny to float away but it should be interesting and might offer a speedier alternative to powdering the NC youself. Nitration time might be lower too. Acid neutralization would be very effective, perhaps with less processing.

Later this summer I should have some time to try out a nitration on it. I'll let you all know the results upon completion of the experiment.

Al

[kingspaz]

Chem_of_Explos, when it is in fluffy form it has lots of small hollow fibres. this has a very large surface area exposed to the flame so burns much faster. when it has been made into a laquer it only has the outside surface exposed to the flame so can only burn slower as only the exposed surface can burn. that help?

[Rat Bastard]

I have had some NC that I made a while back via Nitric method, that I could put to some good use. If anyone wants to see, I got a page on APPUTTY via smokeless powder (http://krimzonpyro.com/rat/he/apputty.html) . I have heard of ANNC, but I did a search and turned up with no info on ratios. Does anyone know the ratio/manufacture of ANNC?

[Trinitrotoluene]

The only info I have about ANNC is it's dynamite without nitroglycerin. I saw it on the dictionary I forgot the entire defination but it said something like a mixture of ammonium nitrate and nitrocellulose used in nitroglycerin free dynamite. Its worth a try.

[Chem_of_Explos]

Thanks for the info Kingspaz.

[Sparky]

kingspaz, I just want to say that my friend had a failure when he tried using your method to make nitrocellulose. I'm not blaming the method, rather I guess that his sulfuric acid was too dilute (Drain cleaner, concentration unknown - Pretty sure it is above 90%). The failure mode was the same as the other times he tried making nitrocellulose - the cellulose began to fall apart and turn to mush as it was supposed to be nitrating. The end product was very slightly nitrated. BTW he found that he could effectively use the top of the oven (which was by chance drying things inside) as a hotplate to keep the mix at 40C quite well.

Then when he tried to concentrate his sulfuric acid on a gas stove (outdoors!) (using boiling chips and everything) the pyrex measuring cup - used because it is much thicker than a beaker - shattered upon cooling. Using a sandbath probably would have prevented this. Fortunately there was only about 50 or 100 mls of acid in there but it sure made his heart beat faster for a while!

Lesson learned: use sandbath when boiling sulfuric acid. Know thy reagents.

[kingspaz]

Sparky, i used drain opener H2SO4 aswell. i can't think what the problem could be. what form of cellulose did you use? i used cotton wool pads.
i've found the cellulose to turn to mush before. but not with this method! only upon me trying to neutralise some cellulose nitrate with ammonia (silly me). ended up hydrolysing it and it turned to mush then.

edit: forgot to say if the acid wasn't concentrated enough then the cellulose would be hydrolised adn turn to mush as you described. was your AN dry? this may have introduced additional water into the mix.

[ALENGOSVIG1]

I've never needed a sandbath. I just use a 1 L pyrex beaker and heat it on a hotplate turned to max heat. I cant even count how many liters of sulphuric acid i've concentrated and i've never had an incident.

Except ofcourse when I attempted to pour a litre of quite warm sulphuric acid into a glass storage container which shattered, and started slowly leaking acid all over the place. The the whole conatiner was shattered, but it was holding it together with my hands. I managed to pour out mabe 300 ml of acid when the whole container fell apart. Ruined a nice pair of gloves that day.

[fowkes.l]

I have recently been trying to make NC using 68% nitric acid and 93% sulphuric acid. Nitric acid is two weeks old but sulpuric is about 5 years old. I used powerlabs method.
I added small amount of cotton to a mix of 35% nitric acid and 65% sulphuric. I left this medium/cold mix for 5 minutes, strained and then washed twice with water and once with sodium bicarbonate solution. Once it was dried (in the sun) I tested. I lit it with a match- it slowly burnt, i could almost blow it out.

I then tried other mixes 50/50 mixes of acids, same result- im using pure cotton balls.
I was wondering if it was the sulphuric acid? or is that how fast NC burns. Should it make a small fireball or burn furiously?? Has anyone had a successful result??

[vulture]

Ehm 35% nitric and 65% sulfuric? You can't nitrate with water....

No seriously, there's waaaaaaaaaaaaaay too much water in your mix. Try concentrating your acids or use a shitload of 90%+ sulfuric acid.

[Microtek]

To those interested in powdered NC: I made a post a few months ago explaining how this can be done by first preparing powdered cellulose from wood and then nitrating this as usual. The product is much easier to work with and is fully dissolved by acetone. I never use NC on its own, only as energetic binder so I don't know how good the nitrogen content is, but when making any kind of nipolit or similar, it is way superior to guncotton. It is possible to use very little acetone or nitromethane if the NC and RDX is mixed beforehand, so no voids are left when the solvent evaporates. This gives higher density --> higher VOD , even though the NC may be less nitrated.

[Mr Cool]

Vulture, he's using 68% nitric and 93% sulphuric, in a 35:65 ratio (vol. I assume).

Microtek, if you were interested you could easily work out nitrogen content. Since cellulose and all nitrated celluloses are totally insoluble in water, you know that nothing is washed away in washings etc. So you always have an almost 100% yield. Therefore it's easy to work out the % N from the % increase in mass. Well, that's what I've been doing anyway.

fowkes, you say you washed twice with water and then once with bicarb - did you give it a final thorough rinse with water? If not, then that is probably where you are going wrong. Also, dry it well. It can still contain a surprising amount of moisture even if it feels dry.

[Sparky]

Kingspaz, my friend also used 100% cotton absorbent pads. When looking at his notes I notice no mention of drying the ammonium nitrate but I don't believe he could be stupid enough to not dry it. After all, it would not only add water but also alter the amount of ammonium nitrate added since some of the measured stuff is water.

If anyone out there has or knows where to find a density/concentration curve or table which he can use to try and find the concentration of his sulfuric acid, that would be very useful. Otherwise my friend may have to find some way of performing a titration with improvised equipment. Kingspaz, you wouldn't happen to know the density or concentration of your sulfuric acid would you?

Alen, I would guess that the uneven and relatively intense temperature of the gasoline Coleman stove is a big factor in shattering of the Pyrex container. A hot plate is a much better idea ;).

"Should it make a small fireball or burn furiously??"
It should burn quite quickly if it has a high nitrogen content, which is the goal. Slow, low nitrogen nitrocellulose is useful and more commonly used than high nitrogen nitrocellulose as a binder. I'm sure we can all agree faster burning is more fun though. You can find videos of nitrocellulose of varying nitrogen content burning on the internet (pretty vaque I know... :)).

[nbk2000]

Try using some dry sand in a shallow pan next time, so the glass doesn't shatter, eh? ;)

[nbk2000]

Here's a table for determining H2SO4 concentration from volumetric density.

[Microtek]

Titration would be the most accurate way to determine concentration, and can be applied to your distilled nitric acid as well. The problem of finding a reliable primary standard for calibrating your titrant can be solved by using benzoic acid precipitated from an acidified sodium benzoate solution. The low solubility and hygroscopicity of benzoic acid means that it is easy to purify and dry it, and ethanol can be used to dissolve it prior to titration. The sodium benzoate availible commercially should be quite pure as it is intended for use in food.

[Snipie]

Merck has some pretty good density/concentration tables, along with some other interesting data:
http://chemdat.merck.de/cdrl/services/labtools/en/index.html

You can also order the ChemDat CD-rom for free. They send the CD pretty quick :D

http://chemdat.merck.de/cdrl/services/chemdat/en/cd.html

[Sparky]

Thanks Microtek but finding the density is so much more convenient, so I used that instead. Thanks NBK and Snipie. Using your tables I have found my sulfuric acid to be 92%. I used a graduated cylinder to measure 500 ml of acid, then found the sulfuric to be 912 grams -+1gram. So it should be pretty accurate. My next step is to steal some sand from little kids the playground...

[tri-x]

Snipie, I checked out the Merck links above. The ChemDat CD looks like a very
useful reference, but they don't distribute it to the US. Do you have facilities to
host a Cd image?

[blindreeper]

I got the CD to Australia in about 5 days so I think they are very good. It basicly has thousands and thousands (litterally) of chemicals listed. They come with saftey and storage sheets, properties (boiling point, melting point ect) and lots of other neat stuff. Most of them have a 2D structure of the molecule to go with them.

I will have a fiddle around and try and get the CD onto the net for download.

Some good news guys but some bad. I put the CD on my harddrive and it takes up 371MB :eek:
I don't think anyonme wants to download that...
But I think I'll go through and try and delete the other languages except english (sorry but it will be for english only but I may consider making the other languages into different files)

I'll try and move em out and get rid of the other crap.
But if I don't do anything to it and you burn it onto a CD will it function as the original?

All the MSDS things are tiny 10-20kb PDF's

[simply RED]

kingspaz, what kind of nitrocellulose do you get with the process above (1g C, 2gAN, 5g H2SO4)
Pyroxilin, coloxilin or coloidin. Does it left some residue after combustion?

I've tried only the standard process with mixed acids, it yield pure pyroxilin when you put 1 gram cellulose to 10ml mixed acids (20ml HNO3, 30ml H2SO4) with 80-85% HNO3. Nitration at 12 degrees. Using more than 90% HNO3 for NC gives very colided product, the cellulose desintegrates in the mix.
With 95-98% sulphuric and 59% nitric it was imposiible to get anything, absolutely no nitration of the cellulose. With 65% coloidin with 75 coloxilin, with 85 pyroxilin. (1 gram Cell, to 10ml mixed acids).
(data from my own experiments)

[kingspaz]

simply RED, i'm not sure of the exact differences between the types of nitrocellulose that you have mentioned but my nitrocellulose is soluble in acetone, burns in a flash (in 'natural' form) and leaves little residue if any.

[simply RED]

It must be pyroxilin (trinitro cellulose) or mixture of coloxilin and pyroxilin.
The three types of nitrocellulose differ from the percentage of nitrogen in them. Pyroxilin is the most nitrated form. (fully nitrated)

[Snipie]

Unfortunately my internet connection is ISDN :(

But I could upload it somewhere from my work (I can’t host it at my work)
I had access to the FTP from Ctrl_C. But it’s gone, and a quick look at the Forum FTP topic shows no alternate FTP that works.

So if you can give me a location to upload it to…..

Btw. the nero image is 423 MB, and compressed (RAR) it’s 233 MB.

[tri-x]

Snipie, you could try HNIW's FTP in Poland. It's in the Forum FTP thread in Forum matters.
I don't want to post the login info here as this section is viewable by non-forum members,
so here (http://www.roguesci.org/theforum/search.php?s=&action=showresults&searchid=20962&sortby=lastpost&sortorder=descending) is a link to the post with the login id and password. The IP has been updated and is here (http://www.roguesci.org/theforum/search.php?s=&action=showresults&searchid=20964&sortby=lastpost&sortorder=descending)

EDIT: Mods, sorry about getting off topic here.

Snipie, we should either be in links & literature or take this to e-mail... Tri-x

[simply RED]

I made lots of pyroxilin with 95% HNO3 and 95%H2SO4. If you don't put too much H2SO4 the product does not colide.
The acids were 1:1 in volume. Nitration at 12 degrees (12 degrees seems the optimal temperature for getiing nitro esters). 1 - 1,2 grams cellulose to 10 ml mixed acids. Nitration time 8-10 minutes.

[Axt]

Anyone have drop test figures for guncotton? I remember it being suprisingly sensitive.

Ive uploaded a guncotton movie <a href="http://www.geocities.com/roguemovies2/index.html">here</a>

[Microtek]

When I make NC I use 62 % HNO3, 96 % H2SO4 1:2 volumetric ratio. Nitration is carried out at room temp ( 22-24 C ) for ca. 45 minutes.
The product, after thorough neutralization and washing, burns smokelessly with a flash leaving no residues.

[KABOOOM [pyrojustforfun]]

simply RED u can't make NC with higher N percentage than 13.4-13.5 when using H2SO4-HNO3. fully nitrated cellulose has 14.15% nitrogen content. for higher N% NC, H3PO4-HNO3 is used.
I think the problem of powdering via precipitation is because of low N content NC. as nitration degree increases its crystalline properties increases as well.

[Von Moltke]

Before nitration it is advisable to dry the cotton at around 100C for quite a long time (e.g. 2 hours) - people often neglect this step, but I find it means there is very little temperature rise on addition e.g on adding 30g of v. absorbant cotton to 800c.c of mixed acid (65%-35% by vol. H2SO4-HNO3) there is a temp. rise of only 5-10C: this isn't a problem obviously.

To produce guncotton I leave a batch as above in the acid for six hours; which is what they use in undustry, and the resulting guncotton deflagrated extremely rapidly (as one) with a dull thud. I find leaving for 10-30mins will only yeild pyroxylins and collodions, which are rather tame. (there is of course no defined formula,only; Nitrocellulose = C6H7O2(OH)x(ONO2)y where x + y = 3)

The highest nitrogen content you can get in practise with normal acids is 13.5% nitrogen, while the theoretical possible is 14.4%. [splitting hairs, I know]

[Boomer]

While we are at it (the hairs), Davis etc say 14.14% with 100% HNO3 + P4O10.

The reason for drying before nitration is that cotton absorbs approx. (15% moisture minus N-content) from the air. I.e. at 13% N it still takes up 2% water. This pre-drying is even more important for nitrostarch, as much more is used for a given amount of acid, therefore not only warming it more, but also diluting it.

BTW I tried NC using SA/AN with surprisingly good results:

60ml pre-chilled SA (96+%) and 40g AN (120C dried) were mixed at RT. It heats up to about 40-50C, dissolving in 2 minutes. After cooling back to RT under running water, 3.0g pre-dried cotton were added. The mix was left at RT for 4 hours, then gradually heated to 50C (within 1h) and held there for another hour with occasional stirring. After naturally cooling back to 30C, the acid was squeezed out with a glove and saved, the NC washed, neutralised and dried as usual. 2 things were observed:

1. The yield was very good (5.1g) and the product was much higher nitrated than with 2:1 SA/NA (65%). It burned not only with a flash but with a distinct "popp" on the hand.

2. The synth used up only 4g AN, while adding 1g water to the acid. This means the acid can be re-used several times!

BTW I only use weak ammonia water for the last neutralisation step. After the usual soda and water washings I boil in dH2O, which gets some more acid out (ph goes from 7 to 5.5 again). NH3 is added to ph=8.5, after an hour the product is then pressed out and dried. I read that the ammonia replaces any hidden acid traces, and what is too much gets lost on drying.

[Von Moltke]

You are correct to say 14.14% - I think it was a typo when I wrote that, but there we are...

I have some data for dry guncotton (13.4%N) below: (You can find this in J. Akhavan's 'Chemistry of Explosives' - RSC Paperbacks 2004)

Friction sensetivity / N
>353 (Where Picric acid = >353 and Mercury fulminate = 3-5 and TNT = >353)

Impact sensetivity / Nm
3 (Where Picric acid = 7.4 and Mercury fulminate = 1-2 and TNT = 15)

Figure of insensitiveness
23 (Where Picric acid = 120 and Mercury fulminate = 10 and TNT = 152)

Hope this is of use.
P.S. I have found it difficult to detonate small quantities of guncotton with fulminate, but with a booster of picric acid it is reliable.

[The_Rsert]

I have about 100g powdered NC with about 11% N. Is it possible to improve the nitrogen content?

[Mumble]

Yes, you can in a sense renitrate to add more nitrate ester groups and improve %N. You may want to just keep using the excess nitrating mix for the next batch as you wont need a full nitration mix, and the mix would be too full if you put in the amount of cotton you would need to make use of the nitration materials. Hell, my mix for NC from cotton is basically solid, I would not think you could fit 4 times as much cotton in it.

[pdb]

After naturally cooling back to 30C, the acid was squeezed out with a glove and saved

What are your gloves covered with to resist to conc H2SO4 & HNO3 ? Neoprene ? Nitrile ? PVC ?

[Boomer]

They are just cheap throw-away AIDS gloves, vinyl type. Nearly every type will resist long enough, pressing takes a few seconds only. Actually the vinyl gloves take quite long to dissolve, I use them a lot and never had yellow fingers after a conc nitric job. :)

[V2A]

i also use these AIDS gloves.
they are imo the best ones, cause u have nearly the same sure instinct as without gloves nevertheless protection against acids is pretty good.

[bonusiletisim]

Can it be dangerous to press nitrocellulose for a good confinement? I followed the procedure in Powerlabs and I have 25 grams of nitrocellulose now. I'm just thinking of a mechanism like a huge syringe with a hole for the detonator.