Cellulose Hexanitrate

[Demolition]

Taken from Mr Cools website.

30mL of 70% nitric acid,
70mL of 98% sulphuric acid,
10g of cellulose (cotton wool),
5g of sodium bicarbonate,
5g Urea,
Distilled water,
Two 150 beakers,
A thermometer,
An ice bath,
A hot water bath.

1) Mix the two acids in a 150mL beaker.
2) Cool them to 10*C, and add the cellulose.
3) Stir it with the thermometer, and keep it between 10*C and 30*C, for 45 minutes.
4) Using the thermometer, fish the nitrated cellulose out of the acid, and sqeeze out excess acid back into the beaker. This can be recycled.
5) Put the Cellulose Hexanitrate into the other 150mL beaker, add 100mL of distilled water.
6) Stir it around, and drain off the water.
7) Repeat steps 5) and 6).
8) Pour 100mL of water into the 150mL beaker with the Cellulose Hexanitrate, and add the sodium bicarbonate. Stir it for 10 minutes, heating it at around 60*C using the hot water bath.
9) Repeat step 8), with urea instead of sodium bicarbonate.
10) Let the Cellulose Hexanitrate dry in a warm place.

Does 10 grams of cellulose seem like a bit too much?It only just fitted all in,and then when It did I could hardly stir it,I could only push the cotton down and around (in one whole large piece) with the end of the thermometer.I dont think the cotton would get fully nitrated or would it?I ended up just dumping it into a bucket of water :( (other commitments) <img border="0" title="" alt="[Wink]" src="wink.gif" />
Maybe next time I'll try 7 grams instead of 10,or is 10 grams ok as long as I leave it for 45 minutes so the acid mix can pass through all the layers of cotton to fully nitrate it?
Thanks in advance :) I'll post my results.

[kingspaz]

hey, it just so happens i've just started some off aswell.
my last attempts have failed :(....due to use of paper as a cellulose source, not fully dried AN, and not leaving it to react for long enough.
i have tried again this morning using calculations i made from the powerlabs recipe (which is linked to on mr cools page).
i used:
20g of H2SO4
5g of NH4NO3
2g of cellulose (i used cotton face care pads this time - i calculated it to be 4g bu that was way too much last time...no enough acid to soak into it!)
but this time i think its just enough, each piece has soaked up the acid and i'm going to leave it until tomorrow afteroon to nitrate.
my last batch which was performed similarly but with 4g of cellulose was left for only 30minutes to nitrate, i achieved a VERY partial nitration as the edges of the pads where plastic to touch.
i'll report back in the net couple of days, hopefully with good results...it may be longer since i have to make this stuff VERY stable for use in castable primaries.

[vulture]

I've made this once, but it yielded different sorts of celluloids, i had plastic foil and a rock hard mass of celluloid. Neat for chemistry class, but not for explosives... :(

I used the powerlabs procedure, however leave it in the reaction vessel for half an hour while stirring. I couldn't stir because the mixture evolved a lot of HNO3 gas and i was doing it inside.
Cooling does not seem to be necessary and is said to slow down the reaction resulting in incomplete nitration.
A high concentration of nitric would be good here, because there are six NITRATE groups that have to be attached.

[A-BOMB]

Isn't this some kind of flash product and wouldn't cotton balls do their cellulose I think? I've been up to late and woke up to early.

[vulture]

<a href="http://www.powerlabs.org/movies/ncburn.mpg" target="_blank">NC deflagration</a>

<small>[ March 26, 2002, 01:42 PM: Message edited by: vulture ]</small>

[A-BOMB]

Kingspaz how much of a yeild do you think you will get? And tell me if it works because I got the AN and the H2S04 so if it works I got a new project to do. I so bored! I've restorted to making baking soda and vingar bombs.

[Demolition]

I just tried the same method again,I used a smaller beaker this time (150mls) and the 10 grams of cotton fitted all in,however it was still a bit hard to stir.It is still nitrating now.I'll go have dinner now and then ill get it out when I finish,the temperature is hovering around 25 degrees.

[Demolition]

All up I left the cotton in the acid to nitrate for about 1 - 1 1/2 hours,I wanted it to be well nitrated,and not just partially.I washed it well and now its sitting in a large bottle of warm water and bi-carb soda.I think I'll leave it over night to make sure all the acid is neutralised.
Its a sort of yellowly/whitey colour,Im not sure if it will work or not,I'll test it tomorrow,weigh up the yield take some photos tomorrow or the next day. :)

[kingspaz]

glad yours worked demolition!
mine failed misrebly again...after leaving it to nitrate for 6hrs there wasn;t any change from 2hrs earlier so i added a load of water to it. the mixture then turned white and slushy! :confused:
i left it to settle and the result was a kinda white slime with little strings on cellulose in it...
dunno what the fucks going on. i scooped a load of it out and put it on the radiator to dry. its still drying now and when its dry i'll brun the lot because it doesn't look of feel nitrated at all. shouldn't it feel kinda like plastic? this is REALLY pissing me off now! :mad: :mad: :mad: ....5th time its failed now! i'l getting some KNO3 in a couple of weeks. i've finally found a source so i don;t have to make it anymore :) ...if it doesn;t work with the KNO3 then i know its the acid which is at fault.
i emailed powerlabs about it and they said that NH4NO3 + H2SO4 doesn't make nitric. this is clearly bullshit since i've made TNP with it.

[Demolition]

Thanks kingspaz :o
I took out a small piece (maybe an 1/8th of a cotton ball) and put it in the oven on low heat to dry it (its raining and cold outside).It was in there maybe for no more than 2 mintues.I took it out and seperated it into smaller pieces.I lit it.Very quick :cool: alot quicker than a similar amount of AP.I really didnt think that it would of worked.I love the smell after burning a small bit of NC. :D
The rest of it is still in the bi-carb-water solution.When the weather gets a bit better I'll take it out,also for safer storage.
Can anyone see any problems leaving it in the solution for a little while longer?Also if I nitrated 10 grams what should approximately the yield be? (does the cotton gain weight as its been nitrated or will the weight remain the same?)
My digital camera has gone for the day so I'll take some pictures tonight and put them up. :p

Kingspaz:Mine doesnt really look nitrated at all,It just looks mostly like normal cotton balls,it doesnt feel very plastic either?Thats why I doubted mine so much but I was wrong.It surprised me when I put my lighter to it and it flashed and it was gone. :D Make sure its very dry,maybe put a small amount in the oven just to make sure there isnt any moisture left in it.

[da man]

Be careful about keeping the temperature down! I just tried to make some cellulose hexanitrate, but i added the acids all in one dose and the acids weren't prechilled, the thing heated up heaps and nitrogen dioxide started to plume out. Idunked a few portions of water which eventually stopped it. I never expected the reaction to go that quickly!

Demolition: yes the cotton would of gained weight, i'm not sure exactly how much but with 6 nitrate groups attached to it i imagine a fair bit, about 50% at an estimate, maybe more!

<small>[ March 28, 2002, 05:40 AM: Message edited by: da man ]</small>

[Demolition]

When I added my H2SO4 to the HNO3 the temperature rose quickly to about 60-70 degrees.No nitrogen dioxide was released for me however throughout the whole nitration white HNO3 vapour (correct me if im wrong)was given out.The actual nitration itself gave out hardly any heat at all.

[da man]

Yes i definately think that was the problem! I added the nitric acid to the cellulose, then i added the sulphuric acid, i think that is what created enough heat to cause the nitric acid to decompose. I think the reason why the sulphuric acid heats up when it meets the 70% nitric acid is because the sulphuric acid forms hydrates with the water in the nitric acid which causes heat from the rapid reaction. its the only explanation i can think of but can someone with more experience in chemistry please correct me if i'm wrong.

Demolition, i just tested some of the nitrated cellulose which i have been nitrating for about 2 hours and it only burnt reasonably slowly, like ping pong balls, so i assume it has formed celluloid. It's a mostly yellow colour with patches of white in it. I'm going to leave it nitrate further over the night and test it again in the morning.

[Demolition]

da man:I only nitrated mine for about 1 1/2 hours.All of that time the cellulose was submerged under the acid.Looking at my NC again I would have to say that the colour is more whitey than yellow. (check out the photo) Did you dry it well?Last night I tested a small amount,It didnt even burn,after leaving it over night this morning it was alot drier however it still burned very slowly,I suspected only partially nitrated cotton,not willing to give up I put a small amount in the oven,after 2 minutes on low I pulled it out and made a long string like piece from the cotton (approx 4 cms long,3mm wide) When I lit it it flashed and was gone. :)
Maybe there is still some moisture in your cotton.

<a href="http://www.angelfire.com/retro/explosives/NC.gif" target="_blank">http://www.angelfire.com/retro/explosives/NC.gif</a>
Heres the photo of my NC in a water-bi-carb solution. <img border="0" title="" alt="[Wink]" src="wink.gif" />

<small>[ March 28, 2002, 06:54 AM: Message edited by: Demolition ]</small>

[Mr Cool]

If you can't get it to work, make sure that what you are using is PURE cellulose (not paper, which contains bleaches, white pigments like titanium dioxide, and often adhesives as well). I use absorbent cotton wool, the only processes this goes through before being sold are washing and drying, after being picked off the cotton plant.
If it still isn't very good, first boil the cotton in conc. NaOH for half an hour or so, then wash it fully in distilled water, to remove any grease that might be present on the surface of the fibres.

And yes, you MUST make sure the nitrated product is TOTALLY dry! Even low water contents seem to affect the burning quite a lot. Although I doubt they'll do much harm to the detonation.
I wouldn't recommend oven drying more than a few grams, this stuff can catch fire at ridiculously low temperatures (about 150*C IIRC).

[vulture]

I remember someone claiming that i makes the DDT (Deflagration Detonation Transition) in rather small amounts and quickly when confined.
Would be a nice alternative for flash or maybe even a primary if this is true.

[kingspaz]

thanks guys, i'll leave it to dry for a few days or put it in the oven before i waste any more acid in further attempts. once i know it works i can make it again whenever then.
vulture, i have also heard that claim, i am however sceptical about this. surely if this was the case then wouldn't it detonate in guns?

[vulture]

I mean it does detonate in guns no? I wouldn't know what could cause the high muzzle velocity otherwise...

[Zambosan]

The high pressure forces the bullet out, but the process is still deflagration, albeit under high temp & pressure. In fact, NC is preferred for cartridge ammunition because it has a burn rate that is very easy to predict when the extruded grains are of a uniform size. This is in contrast to black powder, which is much more unpredictable.

[da man]

I think in guns it is gelled with nitroglycerine to slow down the rate it burns, if it did detonate it would probably burst the chamber and it would detonate the nitroglycerine it's with, and that wouldn't be good! :D But i think it could very well detonate by itself!

[kingspaz]

in the gun, the NC burns very fast. its this rapid expansion of hot gasses produced which pushes the bullet out. if it detonated it would have a shattering effect blasting the gun to pieces. if it could detonate without nitroglycerine then there wouldn't be single base powders which contain only nitocellulose.

BUT, both single and double base powders can detonate from a cap. i blieve the velocity of detonation for nitrocellulose is 7100m/s....that seems high to me but thats what i remember!
double base is much more powerful since it contains nitroglycerine, which is added to the NC to give it a neutral oxygen balance resulting in lower barrel wear since no corrosive by products of incomplete combustion are produced.

<small>[ March 28, 2002, 06:17 PM: Message edited by: kingspaz ]</small>

[nbk2000]

Here's a process I ran across in a old chemistry book from the 1800's. If someone could test it out and see if it works, that be great, because I was thinking of including it in my book and want to know if it actually works or not.

++++++++++++++++++++++++++++++++++++++++++++++++++ ++++++++++++++++++++

Add 6 fluid ounces of Sulphuric Acid to 1 fluid ounce of Distilled Water in a glass jar, then add 3.5 ounces of powdered Potassium Nitrate, gradually stirring it in with a glass rod until the lumps disappear and the mixture becomes transparent.

Do this mixing outdoors. If you see any red fumes, STOP! Get upwind and wait for the fumes to stop. After a few minutes wait, you can resume slowly adding more nitrate.

Place a thermometer in the mixture, and when it indicates between 145° and 150°F., the cotton should be immersed. If the acid mixture isn't hot enough, warm it in a hot water bath.

Take 4 grams of clean cotton, and separate it into 10 or 12 puffs, and immerse the puffs separately, and leaving the cotton in the mixture for 10 minutes. Should the temperature fall to 140°F, heat the jar in boiling water, and maintain it between 140° and 150°F.

After 10 minutes remove the cotton with plastic tongs, and squeeze out as much of the acid as possible between two sheets of polyethylene plastic or glass.

Quickly add the mass into a large amount of clean, cold water, separating the mass so as to wash it thoroughly and quickly. Next, boil the cotton in a saturated solution of baking soda for several minutes. Complete the washing by rinsing for several hours in running water, then spread it out to air dry.

[kingspaz]

well, its dry, and fucked up! it burnt like regular cellulose. ah well, i think the exceptionly long time i left it in the acid may have screwed with it. i'll try it again when i have time, but i need to purify more H2SO4 first :(
i'll use the same method but instead of leaving it for 30 minutes and getting a partial nitration i will leave it for 1hr and hopefully it'll work then!

[da man]

One thing that i have found affects the performance of cellulose hexanitrate is nitrogen oxides and nitric acid present in it. If your nitrated cellulose is yellow it means it contains alot, it should be white. To get the nitrogen oxides and nitric acid out you can add urea to a solution containibg the nitrated cellulose. I get alot of it out though by boiling it in a solution of sodium bi-carbonate, it burns ALOT better when it doesn't contain the impurities, whereas the yellow parts just burn like celluloid or cotton!

[Demolition]

When I first got my NC out of the acid and put it into water the colour of the water turned quite yellow,however after washing it in cold water a few times and then 3 more times in hot-bi-carb solution the colour of the cotton returned to white and the water remained clear.

Funny how you dont notice something until someone points it out. <img border="0" title="" alt="[Wink]" src="wink.gif" />

[Mr Cool]

NBK: I'm just going to finish a batch of TeNN I'm doing (I need to do the last step...), then I'll try that method. So I should have a verdict to give you by the end of the day.

[kingspaz]

my NC was pretty acidic, well he stuff that didn;t work. it was kinda yellow and started reacting with the paper it was on...
ah well, i will try again when i get time. thanks for the help guys!

[Demolition]

After a couple of days drying I weighed my NC.Approx ~ 13 grams. :)
Ill try and detonate some later during the week.

[Mr Cool]

NBK: I didn't try that method after all, because that's a hell of a lot of acid for 4g of cotton! There's 15 times more KNO3 than is theoretically necessary...
I'll stick to my method, since my source of H2SO4 is expensive and somewhat variable in availability.

[nbk2000]

Ever heard of "ratios" and "scaling down"?

[Mr Cool]

Yes.
If I scaled it down, I'd only get a tiny bit of NC. But with the same amount of acid I could get more from a different method. I was just checking that you hadn't made a mistake when you copied it down, because that is a ridiculous excess.

[nbk2000]

That's exactly the way it was.

Remember, it's coming from a 19th century book, so that's a factor. I'd try it (if I had the acid) as is, then try it with half as much acid the next time, and see if there's any difference.

Try it with half or third of the acid and see if it works.

Don't forget, the extra acid may be needed because of the water.

[vonK]

I've been having problems washing my nitrocellulose. When I stick it in water it disintergrates leaving a milky solution with tiny bits of nitrocellulose floating around.
I use 80ml of 98% H2SO4 with 20g KNO3 and three and a half cotton balls (thats all that will fit). Each cotton ball weighs 10.5 grains(1 grain = 0.065g ?), they came from a hospital and the pack says they were sterilised with ethylene oxide.
Can anyone tell me why this happens?

Thanks
Kurt

[kingspaz]

same thing happend to me. i believe it was due to it being left to nitrate for too long. i left mine for 6 hours and that milky shit was the result. i think 45-60 minutes would be the best nitration time. i haven't the time to experiemnt further and make another attempt <img border="0" title="" alt="[Frown]" src="frown.gif" />

[vonK]

No, that can't be the problem.
I left mine for only 30mins and what little I did manage to get at the end, burnt slowly like plastic.
I will try again today but I will put the nitrocellulose in a funnel and pour the water over it rather than submersing it under water.

[vonK]

Well, my idea wasn't much of a success.
I made a nitrating mix but fucked up somewhere and added to much NaNO3 to my H2SO4.
As it was cooling the mix started to solidify so I added some cotton balls before it became completely solid.
While the cotton was nitrating I made my funnel. I cut the top 1/4 of a plastic Coke bottle, where it starts to taper towards the mouth and punched the lid full of tiny little holes.
after 30 mins I put the nitrated cotton (coated in crap) in the funnel and and poured water over it. It seemed fine so I poured NaHCO3 solution over it and then more water. I then picked up nitrocellulose and squeezed out most of the water.
After drying it in the oven for 30 mins I tested some in a flame. It burst into flames but it was nowhere near as quick as HMTD, I quess it wasn't completely nitrated.
I then tried again using proper ratios and KNO3 instead of NaNO3. This time when I poured water over the nitrocellulose the filtrate came out milky and my nitrocellulose slowly dissappeared.
I think the problem is, that highly nitrated cellulose breaks into tiny little pieces in the water, I'm not sure why but this is what seems to be happening.

[Demolition]

Here are my results :
1-I tried to set off about 5 grams of NC using a approx ~ 4 gram AP det,the detonator fired,no detonation of the NC.
2-A .22 magnum shell pressed with AP failed to detonate about 4 grams of NC (the NC was pressed around the det in a small plastic tube) The det fired perfectly,no detonation.
3-Thinking that detonator is not strong enough I tried about 4 grams of NC using a fuse this time,sealed in a thickish plastic tube.This time a small bang however no where near the amount of damage or the amount of noise that 4 grams of NC would do when detonated,the tube was also left almost intact also.

Im not too sure what is going on,after each failed detonation ive lit the rest of the NC remaing and it flashed and burnt quickly.I can only think that the cotton absorbs the blast and there for does not detonate.Does anyone have any ideas??? :confused:

[Mr Cool]

I'm not sure what's wrong, but NC is/was always used wet as an explosive. I think this is mainly for safety from sparks, but it would help to propagate the shock wave.

[kingspaz]

would be 'fluffy' nitro cellulose be simliar to pumice in that it could 'stop' the shockwave? maybe cast nitrocellulose would be easier to initiate - uniform density.

[Hystrix]

I don't understand why do you call it "HEXAnitrocellulose"? Afaik the cellulose's monomer (glucose) has only 5 OH-groups, and 2 of them are used for linking to cellulose. So, we can prepare trinitrocellulose only.
Btw: Urbanski describes pentanitroglucose and octanitrosaccharose (and other saccharides' nitroesters), they are very unstable <img border="0" title="" alt="[Frown]" src="frown.gif" />

[kingspaz]

ah, there does seem to be a problem! i've just draw a pic of a glucose monomer, i crossed off the two OH groups used to bonding leaving only 7 possible nitro groups locations :confused:
this is assuming all other hydrogens ans OH groups are removed and replaced by nitro groups. i don't see how this could work :confused: :confused:
anybody want to have a shot at an explination?

[A_W]

The reason why you get problems with the nitrocellulose "dissolving" in the water, leaving a milky "solution" behind is very likely to be the (extremely) long nitration time.

10 minutes are recuired to make dinitrocellulose, and 15 minutes for making trinitrocellulose. Leaving it for hours, will probably destroy the explosive, making other useless compounds.

Properly made nitrocellulose is not supposed to look or feel like plastic. It looks very similar to regular cotton, wich is why it makes a great chemistry demonstration :D .

The reason why some of you get nitrocellulose that burn like regular cotton, is probably because the nitrocellulose has not been neutralized properly. Try washing it in several NaHCO3 baths until it stops bubbling, and then wash with water. I got some bad results with un-neutralized NC. When I washed it with NaHCO3, it burned like smokeless powder (and this was only left in the acid for 3 minutes!)
Hope this helps :)

<small>[ August 30, 2002, 01:47 PM: Message edited by: A_W ]</small>

[A-BOMB]

Well I distilled some HN03 a few days ago and this morning I desided what to do with it so I tried the formula from powerlabs and put in one cottonball and let it nitrate for 15 minutes because I think I didn't have that concentrated HN03 or H2SO4. So heres a pic of it nitrating, I just washed it a hour ago and its drying now. So I'll tell you how it works out.

<img src="ftp://ewf:sd332gf@209.195.155.80/-=Uploads=-/Linked%20Pictures/Picture%2052.jpg" alt="" />

[A_W]

Nice work A-BOMB :) . If the acids were concentrated (98%/68%), leaving it for 15 minutes should give you a piece of trinitrocellulose. I don`t know if the acids HAVE to be completely concentrated, but home-destilled HNO3, should be quite strong (I think).

[Mr Cool]

To try and answer the qn. about why good NC can be called cellulose hexanitrate:

A glucose molecule has 5 hydroxyl groups, take two off for it to join to it's neighbours and it has three left. So this part of the cellulose polymer can be nitrated 0, 1, 2 or 3 times.
The hexanitrate refers to two of these units joined together. I suppose this is because it's possible to have NC with, for example, an average of 2.5 nitrates per monomer, but you could hardly call it cellulose di-and-a-half-nitrate, so they use two monomers and call it pentanitrate. I dunno what you'd do if you had an average of 2 1/3 nitrate groups per monomer...
That's why I think it is anyway. I could be wrong.
The N% is a much better scale to use.