Cellulose Nitrate?

[ninefingers]

I've tried Cellulose Nitrate and CHN several ways; nothing works. Has anyone any positive experience with this? Thanx Dan-oh

[MurderSkillz]

Several ways how? Care to explain what you are even trying to do with it?

[that guy]

My best results were letting it sit in the acid for about 6 hours. I've used KNO3 and NaNO3 with the same result. I've found that my nitrocellulose gets extremely hard during the process, but after cleaning (washing in cold water and boiling in NaHCO3 solution), it's more like cotton again. It's probably been bout 6 months and I don't recall the ratios that I used, but I do remember cooling the acid before the cotton was added and letting it raise with the addition.

If your cotton dissolves, you may be using too much H2SO4. You should be able to use RFNA. H2SO4 protonates HNO3. No water is necessary.

[X-ray Cat]

I've needed a LOT of tries with nitrate-salts/sulfuric acid mixes for it to work for nitrating. Your sulfuric aswell as your salt needs to be in the precise right condition (dry and pure) and in the precise right quantities.. This also goes for the amount of cotton that should be added.
Some tips that might help you:
-I always seem to find that the amount of cotton that goes with an acid bath is way to much in the synths i find on internet. Following problems will be low nitration of the cotton with a slowburning product as a result plus a very tough job in stirring the cotton through the acid. Try using less cotton.

-Try making nitric acid with your sulfuric acid and nitrate salt. Nitric acid mixes always seem to work for me. Never had a problem with it, nitrate salts have given me a LOT of problems with nitrating. Nitric acid isn't that much of a problem to make, there are fairly easy and uncomplicated improvised setups to do so. I think there actually should be a few setup descriptions on this site (including the use of martini-glasses or kitchen foil or the combi). If any members out there remember it, post a link in this thread please, tihiii!!

[that guy]

Originally Posted by X-ray Cat

I think there actually should be a few setup descriptions on this site (including the use of martini-glasses or kitchen foil or the combi). If any members out there remember it, post a link in this thread please, tihiii!!

As per request, my setup closely resembles the one pictured here: Preparation of formic acid - HomeChemistry

I use a one gallon jar instead of a beaker, so it's completely OTC. It's not tempered glass, so temperature adjustments must be made slowly, and an oil or water bath is necessary. I've also found that I have to wrap teflon tape around the martini glass/gallon jar connection to keep water out. Otherwise, water condenses on the outer rim of the martini glass and can slowly leak in.

The wine glass is a huge advantage over the "beaker inside beaker" method IMO. I tried it once, and the inside jar wanted to float, so I had to put glass shards in it to weight it down. Also, It appeared that the product was constantly refluxing because the receiver was sitting in hot acid. It seemed to lead to quite a bit of decomposition.

[ninefingers]

Originally Posted by MurderSkillz

Several ways how? Care to explain what you are even trying to do with it?

wouldn't YOU like to know! You're not dealing with a "Newbie" "kid" here.

[willi-wurm]

i tried just for fun once, by just mixing H2SO4 with NH4NO3, and let it cool, and left the cotton in there. every half hour id take one out, and Id test some. i got best results after 2 hours of nitration. also i observed a slight orange tinge before neutralizing. i also noticed that anything over six hours of nitration started to go all... squishy, and after neutralizing, it completely vanished! very strange.

can you neutralize it with weak NaOH solution? im low on bicarb.

i did it once out of boredom, and the next time to make nitrocellulose laquer for some APNC.

[X-ray Cat]

Originally Posted by willi-wurm

\ also i observed a slight orange tinge before neutralizing. i also noticed that anything over six hours of nitration started to go all... squishy, and after neutralizing, it completely vanished! very strange.

can you neutralize it with weak NaOH solution? im low on bicarb.

i did it once out of boredom, and the next time to make nitrocellulose laquer for some APNC.

Thats your cotton getting oxidized due to low concentration nitric. NaOH I think will probably fuck it up by hydrolisation.