Log in

View Full Version : Nitrocellulose synthesis problem


-=007=-
2008-06-09, 01:51
In the last days I have been trying to make some nitrocellulose using the sulfuric acid\potassium nitrate method, but I having a few problems...when I mix the sulfuric acid with the potassium nitrate nothing happens, the potasium nitrate dont even dissolve and I am using concentrated sulfuric acid. Some reaction just happen when a put the cotton in the becker, the cotton turns red, then completly dissolves and everything turns into a jelly....can someone help me with this ?

FullMetalJacket
2008-06-09, 04:44
the solubility of KNO3 is pretty shit for these kinds of things... warm up your acid a little, then dissolve it and cool down slowly again.

or just swap KNO3 for NH4NO3

Eldorhan
2008-06-09, 08:23
I wouldn't even dare call that a "synthesis".


or just swap KNO3 for NH4NO3

What a wonderful idea...

-=007=-
2008-06-10, 04:53
Ok, could get the KNO3 to dissolve, but the cotton still dissolving when I put it in on the acid.....

Mokothar
2008-06-11, 19:39
And by cotton, do you mean cellulose cotton, or cellulose acetate cotton?

Sentinel
2008-06-12, 07:24
Are you SURE it's really cotton? Some "cotton balls" are really just synthetic fabric. Also, +1 for using AN instead of KNO3. AN is WAY better for getting HNO3 from H2S04

nuclearrabbit
2008-06-15, 18:40
What kind of acid are you using? Teknix site had a page about some H2SO4 he got that was thick like gel shit and didn't work at all for anything.

-=007=-
2008-06-17, 03:48
Yes I am sure it is 100% cotton, cause I bought it from a chem supplier and it burns like pure cotton. The sulfuric acid is 98,5 %, it is a clear liquid just a litte more dense than water. and i cant get AN , you need a license to buy it here. but anyway thanks....

nuclearrabbit
2008-06-22, 13:35
Mind posting your synth/procedure, that'll help a lot.

AprenticeChemistBITCHS
2008-06-22, 23:17
the solubility of KNO3 is pretty shit for these kinds of things... warm up your acid a little, then dissolve it and cool down slowly again.

or just swap KNO3 for NH4NO3

If you do decide to warm up the acid be damn carefull and make sure its cooled down before you start adding cotton. Runaway is not a fun fucking thing to experince. Ive made many many batchs of NC and only had a runaway once when I was making a nice big 100gram batch. Luckily it was in a fume hood and I got it undercontrol but runaway is not something you want happening. And if I remember correctly its more likely to have a runaway reaction if you're using the xNO3+H2SO4 methoud versus straight HNO3+H2SO4.


What excactly is the synth you are using? The only time ive ever had that shit happen was when I tried to nitrate a peice of cotton shirt or accidently used NON cotton cotton balls. Also have you ever made NC before? Because the cotton does get a little goopy when its in the acid until you wash it out and dry it.

xarf
2008-06-24, 09:11
Which reaction can run away? Cellulose -> NC?

Mokothar
2008-06-24, 11:57
Not really, but setting up the nitration mix is always a somewhat risky endeavour if you're heating it.

Nox aint got no friends ...

Sentinel owl
2008-06-25, 05:12
Basically, because the nitration process generates heat, the solution gets hotter, and if it gets too hot it will start spewing NOx fumes. White fumes at first, and if it runs away, scary red/brown ones. Never had one run away myself, although it fumes white if I don't cool it/mix in things slowly. My chem is a bit rusty but it has something to do with HNO3 breaking down. FYI this applies to all nitrations; that's why you do them COOOOOOLD

Eldorhan
2008-06-25, 19:54
You could apply that rule to every procedure that generates heat when it's not absolutely mandatory.

Heat = BAD.

AprenticeChemistBITCHS
2008-06-25, 21:41
Yes its the nitrocellulose reaction that can have a runaway. For those of you that don't know what a runaway is first don't try NC because you don't know enough and secondly know its not a fun thing. First off like stated it will start fuming brown/red fumes then it will will start making more fumes and it will start to "boil" Which means you know how when you boil water you get the bubbles and sometimes the water spills out or the bubbles pop and some water goes everywhere? Well imagine this with a mixture of HNO3/H2SO4. And of course lots of heat is generated so not only is the acid nice and acidy but its also hot. Luckily when I had this happen it was in a fume hood and I had a bucket of ice not to far so it wasn't to hard to keep it under controlled conditions and get the runaway to stop. But trust me it definatly leaves a big fucking pain in the ass mess, and if it had been in anything but that fume hood might have done some damage.

So the one step you do not want to forget is the ice bath. Seriously the extra miniute and ice is worth it.

frkonaleash101
2008-06-26, 00:42
Any nitration can cause a runaway if it isn't kept cool. you know it is running away when it starts spewing out brownish red gas and starts bubbling.

Eldorhan
2008-06-26, 08:33
Any nitration can cause a runaway if it isn't kept cool. you know it is running away when it starts spewing out brownish red gas and starts bubbling.

No, you know it's GOING to go haywire when it starts to fizzle and make little bubbles, meaning it's beginning to pump Nox and that you will soon have to bail out if you don't cool it ASAP.

Seriously if you wait for a cloud a brown fumes to start generating before you go "uh ? something might be wrong", you shouldn't even touch HNO3. Anyways if you go for that "method" of spotting a runaway nitration you won't survive long enough to testify about it.

A few times *might* be ok with good ventilation, but over time you'll end up frying your organs, so...

frkonaleash101
2008-06-26, 19:22
I never said to wait until the gases are bubbling out did I? No i dont think i did. I said you know you have a runaway when it is bubbling out gases. You want to cool it and stop it *before* it runs away. So a runaway is not when it just starts to bubble or disperse NOx. when it just starts means it is starting to run away not currently running away.