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Author: Subject: Microcrystalline cellulose nitrate(s)
plante1999
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Microcrystalline cellulose nitrate(s)

Is there anyone with actual experience, or data on the production, and the product of microcrystalline cellulose nitration. Is it soluble in acetone or alcohol ether? Is it less stable, and other information. The thread can also be used to report experimentations on the subject in a scientific fashion.

Rosco Bodine
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Yes a member of our forum ordenblitz applied for a patent for microcrystalline nitrocellulose

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Mood: Have no fear <Vlad> is here.

interesting...a few days ago i had the idea if it could work to substitute HMTD/AN* (mixture that detonates without detonator-cap) with NC/AN and getting a "save(r)" detonator, without using peroxides to ignite explosives...

could that work, mixing (MC-)(fine powdered-)NC/AN and then using it as a etonator-cap? or even MCNC itself, would be better, if it is really better to compress than normal NC

*i only tryed this a few times, much years ago...but still using HMTD as detonator

plante1999
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I could buy 1Kg of microcrystalline cellulose for 50$, but I don't have the money for it, or the need for 1kg of the cellulose, as such I will try to turn cotton into mcc using hydrochloric acid hydrolysis of amorphous zones. Speaking of nitrocellulose, I bought 100% cotton cloth today, for 3$ I had a few square feets, the objective is to make cloth of regular nitrocellulose, does anyone have experience with it?

Antiswat
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well plante, youre better off with using tissue paper, the cloth is much more dense cotton than the tissue paper will be, and ofcourse cotton wool is the least dense of them all
it will burn slow, but if you nitrate it properly it will burn completely
if its just for the purpose of getting a compact NC then i'd say its actually a good thing
i believe a more or less famous pyrotechnician youtuber has made a video about it, cant remember name tho, but it surely does burn slower

''the objective is to make cloth of regular nitrocellulose''
i took this as being a mistake, that you meant to make NC of cloth
also, i think there have been discussions and sure indications that less accepted and yet very well functioning initiation have been proved to work over and over again, like the idea of experimentalism, but there ARE alternatives out there, if you really do care to try

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plante1999
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My interest do not lie in detonation mind you, The main purpose is to burn, it is a bit complicated, but I want strong cloth made of nitrocellulose, as for the mcc, mostly to experiment on its properties.

plante1999
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I just burned down some of the cloth, and it left so much ashes, it was almost unbelievable, like 40% by weight, the ash are inorganic, and seams to contain quite a lot of zinc oxide (yellow coloration on heating). I'm ashamed, what can I do to find real pure natural cotton cloth.

Trotsky
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Make your own? Get yourself a pure cotton white shirt or something.

When you say you burned it and you were left with 40 percent of the original weight left in ashes, you're talking about nitrated cotton, right?

You're right, that is no good at all. Frankly it's unbelievable. You wouldn't have that much left with plain unnitrated cotton.

I doubt it contains any zinc oxide.

Was your material one hundred percent dry? Most people rush to the fun part and don't let it dry properly. With cotton balls it's a huge pain in the ass but this shouldn't be as bad.

How long did you let it sit in the nitration bath? If you want good NC you'll want to let it sit at least eight hours, better 12, wash then nitrate again. This way you'll go from 7 percent nitrogen to 10 or even 12 percent. If you do it right you can get very close to complete nitration and get really good clean burning material.

Also, how did you do the nitration? Sulfuric and ammonium nitrate or another nitrate salt? Mixed acid? For NC I think ammonium nitrate is best. Don't use good nitric acid for this reaction.
plante1999
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I meant the pure dry cotton cloth directly from the store. I also tried nitrating it after, but it also left the same residue, the nitrocellulose burned very fast tough. I used good nitric. I did many test with other 100% cloths, which all contained some synthetic (the nitrated product leave a carbon skeleton), or ashes.

But I finally found some real pure cotton cloth. I asked my grandmother about "Real' pure cotton cloth, and she gave me an used 60 years old dish washing cloth, that she had made with sugar bags back then. This cotton is really pure cotton, and on nitration burn fast leaving no residue.

I also cut a long but thin piece of it to use as a fuse, and rolled some to be used as a deflagrating charge. The charge was confined. When lighted, the fuse burn at a very reasonable speed, and the main charge made a nice firecracker. Success, I now need to nitrate the 50g of cloth.

Trotsky
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If it's leaving a skeleton like that you just don't have complete nitration. You need to nitrate it twice to get it to the point where you're left with almost no residue.

That or it was still wet. The last time I made any I was still heating my house, so I stuck all of the guncotton in front of a register and with a plastic sheet, I directed all of the air directly through the cotton. Letting it sit for 9 hours allowed it to dry well.

If I remember correctly properly dried guncotton won't ignite in a microwave, but wet guncotton will. Shit, I can't remember, there is a difference in the behavior of wet guncotton and dry guncotton under microwave radiation. I know the wet guncotton will burn in real short bursts. The bit of cotton will burn little parts of itself in real quick shots, but not the whole thing at once.

It could be dry to the touch but still burn like it was still wet.

I wonder if maybe wrapping it in tinfoil before microwaving it might enable detonation... something to try with a small bit of guncotton and a microwave you don't need. The guncotton won't hurt it but the aluminum will.
plante1999
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Nah, I'm sure it is synthetic "elastane" fiber, when the bare cloth is burned it makes an arromatic-like flame with burning plastic smell. And as a proof, the pure cotton cloth from grandmother with the same nitration procedure leave no residue. It seams that most modern cloth contain synthetic.

malford
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Has anyone here ever tried detonating MCNC? I'm wondering if compressed MCNC would DDT.
Bot0nist
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In large enough quantity it would, but that would be impractical. If fully nitrated and pressed to a good density it should have no trouble detonating with a booster.

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I am left with a bunch of microcrystalline Cellulose and starch after
Extracting ASA from 1k of pills.
Is boiling water enough to separate starch ?
I am wanting to give McCN a try !!

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DubaiAmateurRocketry
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wonder how good a binder would be for MCNC and a/multiple liquid nitroester(s). So was his patent published?
Baffled
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I nitrated microcrystalline cellulose sold for diet purposes with mixed acids once, the product was slightly suloble in acetone, I believe I still have some very firmly stuck to the walls of an Erlenmeyer flask. I don't remember it being very energetic and I did not own the necessary hardware to characterize the product to check for possible mono- and dinitrated products.

Cellulase bioreactors might afford a green way to new interesting energetic materials having a better OB than plain old NC.
NeonPulse
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So yesterday i finally decided to nitrate some MCC.

Into a beaker i made a nitration mixture of 40g ammonium nitrate and 60ml sulfuric acid, adding the nitrate salt in small portions of freezer cold acid mixing thoroughly between additions and let this mixture sit in the freezer -26c overnight. due to the acids light brown colour the nitration mix was a clear orangey. anyway i removed tihs from freezer and let it warm up to around 23c.
Next i took 6.5g of the MCC in a dish i had it pre weighed in and and began to add this very fine powder into the mixture with good stirring much the same as one would nitrate ETN. The acid did seem to make the powder clump and stick together and i tried to break it up as much as possible but it still clumped up. the additions continued untill it was all in the nitration bath. There was no great temp spikes throughout the adding and with each half gram addition it was maybe 1-2 degrees jump with the end temp at 27c which was close to the ambient temperature anyway. I then continued stirring for around 30 mins breaking up the clumps to expose them to the acid. this was left to sit undisturbed for a further 20 mins and poured into 600mls of iced water. For filtration a buchner funnel is needed as the fine particles clog the filter paper. the collected powder was then neutralized in a bicarb solution, Re- filtered then boiled in a 2% bicarb solution for about 30 mins.

Finally this powder was again filtered and dried. The resulting powder took on a slight beige tint form the nitration and a burn test was done.
This stuff burned slightly faster than a double based gunpowder but left alot of black residual ash. No detonations from hammer strikes. It did dissolve in acetone but looked slightly opaque/pearly, not the clear lacquer like regular NC. Dissapointing! i was hoping for a clean burning end product. Perhaps it should have been left to nitrate longer....

I do plan to get 1-2g of this powder and attempt to nitrate it further but with mixed acids this time and see if it can burn any faster/cleaner, Although this step may be pointless it does not hurt to try.
Will upload some pics soon and the results of a second nitration attempt.

[Edited on 8-12-2014 by NeonPulse]

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Hennig Brand
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What was the strength (weight%) of your sulfuric acid? I made some MCNC a week ago or so, and coincidentally am in the process now of making a little double base propellant with it. I had clumping problems too, but found that if the MCC was forced through a fine kitchen sieve, which broke up any clumps, and then sprinkled into the nitration mixture with vigorous stirring, the clumping during the nitration could be nearly completely controlled. It definitely is different material than NC made from raw cotton.

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NeonPulse
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The sulfuric acid was around 98% the drain cleaner stuff boiled until it fumed heavily. I think this MCNC would be ideal as a propellant but if it is nitrated to the max since the barrels will foul up pretty fast. Hennig, how did yours burn? Was there much residual material left?

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Hennig Brand
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Pretty difficult to get to 98% sulfuric acid by boiling it down. Very dense fumes can be seen in the low 90s or less IIRC.

I was using 91% sulfuric acid and NH4NO3 and because a lot more MCC can be added to the nitration mixture than would have been possible with cotton I went overboard and added 60% more weight in MCC than I normally would have added in cotton. Estimated by mass increase the MCNC made is about 11.4% nitrogen, which is rather low. A smokeless propellant was made anyway (70% MCNC : 30% NG) and tested in a .22 cal. rifle. For the same propellant load weight as a commercial load the muzzle velocity was measured as 940fps which is much less than the ca. 1200fps the commercial load produces. The barrel also had much more fouling than usual. I guess I tried to nitrate too much material for the strength and quantity of the nitration mixture.

[Edited on 9-12-2014 by Hennig Brand]

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NeonPulse
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So I performed a second nitration on the mcnc I made and boy did it mahe a difference. I used mixed acids this time and it worked very well giving a slightly different product than the first time which filtered easily was bleached back t white and burned fast and clean. Testing impact sensitivity got a few small cracks and this stuff will likely detonate with a cap too since it coul be pressed easily I would say mixed acids are the way for this stuff as it probably went right into the mcc fully nitrating it. I put a burn test on the tube. Will link it here when I get home on the pc.

Where there is a will
there is a way.

AllCheMystery!