Sciencemadness Discussion Board

Nitrocellulose

liquidlightning - 26-7-2012 at 15:24

I want to nitrate some cellulose, however I don't have any H2SO4. The wiki says that the purpose of the H2SO4 is to act as a catalyst to produce the nitronium ion, NO2+.

My question is, can I use NaNO2 to produce the nitronium ion?

CaliusOptimus - 26-7-2012 at 16:17

No, but you can certainly use it to produce the nitrite ion NO2-

See Wiki

liquidlightning - 26-7-2012 at 17:15

Ohhhh I see, messed up the charges there. Nevermind.

Can something other than H2SO4 be used as a catalyst?

[Edited on 27-7-2012 by liquidlightning]

Ral123 - 26-7-2012 at 20:37

White fuming nitric will work alone. You wont get too high nitrated product but it'll be more stable once washed well. The excess nitric will evaporate. The nitrite will instantly give N2O3 witch can't make acid of any reasonable concentration.

detonator - 31-8-2012 at 23:31

In fact, the role of concentrated sulfuric acid is to prevent the fibers to swell and catalytic.
Conducive to the nitration reaction carried out.

Ral123 - 17-1-2013 at 09:08

Here's burn test in CO2 environment. Two nice dim flashes.
http://www.youtube.com/watch?v=zZEKmuty0Xc&feature=youtu...

hissingnoise - 17-1-2013 at 09:56

Quote:
I want to nitrate some cellulose, however I don't have any H2SO4.

Strong nitric acid will nitrate cotton, as ral123 said, but the water produced dilutes the nitrating power of HNO3!
So in this case H2SO4 binds the water to produce a more complete nitration . . .
Since the reaction is O-nitration, not C-nitration the nitrate ion rather than nitronium ion is the nitrating species!

Scientwisted - 27-3-2014 at 15:55

I apologize if this post is missed placed however I'm hard pressed to find a appropriate place for this post.
I am going to attempt my first NC esterification. Due to a near depleted stock of reagents and lack of funds I want to get the strongest possible nitration with the least amount of chemicals. I will be using 98% H2SO4 and KNO3 salt. Instead of using regular cotton or starch I was thinking of purchasing so flash cotton of reasonable quality as a starting material. I would use the typical nitration procedure then washing ,neutralizing, etc... I want feed back regarding my idea. Is it a good way to go from an economic stand point or is it dumb because of a greater risk of a runaway reaction?- Twisted

roXefeller - 27-3-2014 at 19:44

As you nitrate the cotton, increasing water from the esterification dilutes your reaction mixture which leads to less yield/less nitrogen content as you get longer use out of the pot. Use the typical procedure you have and separate your cellulose into separate portions, each getting nitrated, neutralized, and washed in an assembly line sort of process. The first pieces will be highest and after extended use of the acids at some point nitration will be sluggish, so the real question is how do you plan on figuring the nitrogen content? Nitrocellulose has that nice quality of reduced yield only showing up as reduced nitrogen content.

Scientwisted - 27-3-2014 at 19:53

That's a good point I didn't realize, but do u know what I'm saying? Instead of using just regular cotton as a starting point I would be using flash cotton(nitrocellulose of probably a medium-low nitrogen levels) that I could buy for relatively cheap.

TheAlchemistPirate - 27-3-2014 at 21:21

Flash cotton will already be nitrated as much as possible if you buy from a good source, all that will do is degrade the cotton. There is a limit on how much you can nitrate every material(such as glycerin,tnt, or cellulose), If I were you I would buy 98% sulfuric acid and make it with the normal way. It is possible to make nitrocellulose with just nitric acid you just need to keep it a low temperature, though it requires a huge amount of nitric acid and wont as good a quality as normal nitration. The main purpose of the sulfuric acid is to "pick up" the excess water created in this reaction, otherwise you will end up losing money from loss of concentrated nitric acid (a valuable chemical). If you have a distillation setup synthesize nitric acid using a nitrate salt and 98% sulfuric acid(look this up on youtube),or if you don't have a distillation setup slowly drop sulfuric acid on potassium nitrate in an ice bath (look this up too) and nitrate cellulose in that. Please refer to other threads about making nitric acid in these ways before attempting it yourself.

Bert - 28-3-2014 at 06:44

Quote: Originally posted by Scientwisted  
I am going to attempt my first NC esterification. Due to a near depleted stock of reagents and lack of funds I want to get the strongest possible nitration with the least amount of chemicals. I will be using 98% H2SO4 and KNO3 salt. Instead of using regular cotton or starch I was thinking of purchasing so flash cotton of reasonable quality as a starting material. I would use the typical nitration procedure then washing ,neutralizing, etc... I want feed back regarding my idea. Is it a good way to go from an economic stand point or is it dumb because of a greater risk of a runaway reaction?- Twisted



"Always begin with an end in mind"


I am curious as to the end you have in mind for the project. This has a great deal to do with how you go about things- I can think of several possibilities, laid out below in more or less the order of my personal level of approval and willingness to help you.


1. A research project?

First steps could be to look at litterature or results of previous experiments, formulate a hypothesis and write a procedure to test your concept. Got a hypothesis? Written a balanced equation?


2. A technical exercise to acquire skill in manipulating the materials and apparatus of this branch of chemistry? (no new ground being broken in science, just paying dues, getting your chops and have some fun.)

Research what is (or was!) done with this synthesis in an intro to organic chemistry course. Find out why industry and science thought a student needed the exposure... Plan out your procedure, perhaps submit your plan to experienced people for a critique. Write up the procedure, execute while taking notes. Test your product, perhaps do additional labs with other methods/reactant concentration/dwell time to prove to yourself how different procedure, Nitrogen content and solubility are related. As follow up labs: PURIFY and the store several samples of the products to determine effectiveness of different purification procedures (or lack of same) and storage conditions? Do heat tests? Learn how to make a nitrometer? WRITE IT ALL UP AND POST IT BACK HERE. DOCUMENT, DOCUMENT, DOCUMENT!


3. A synthesis to produce materials for use in some further procedure?

What do you want to DO with nitrocellulose- make lacquer/collodion? Celluloid plastic? Propellant? High explosive? Magician's prop? A gelling agent/fuel for use with liquid explosives? Something new and radical, never before conceived of by the minds of men??? Research and write up a procedure.


4. I JUS WANNA BLOW SOMETHING UP! THE BIGGEST AND LOUDEST EVER!! THEN I'M GONNA PUT THE VIDEO UP ON YOOTOOB AND BE THE KEWLEST!!! WHY DO YOU KEEP SAYING "RESEARCH, WRITE UP" AND OTHER HARD THINGS LIKE THAT, I DO ENOUGH OF THAT IN HIGH SKOOL ALREADY!!!! JUST GIVE ME A RECIPE, I DON'T LIKE BORING READING, WRITING OR MATHS!!!!!

Oh, another one of those. I think I've got a toilet to clean or some other thing to do right now... Later!


* Hi, you several new guys on energetic materials- Are you getting the idea yet?

The site name includes the word "science". There are people here with considerable time and experience in the discipline... And oddly enough, the ones with join dates more than a week to 2 years in the past have been rather scarce in answering your questions. Why? What could the experienced ones want to see before deciding you're worth some time?

Conversely, why are the ones who are so quick to "teach what they have not yet themselves learned" motivated to do that- And how do you evaluate such information?

I am not by nature a sadistic bastard who enjoys baiting and abusing 15 year olds. I remember being 15 and desperately wanting to make something cool- And what happened when my friends and I tried half assed shit we didn't understand well enough.

Especially for you USA kids dealing with a totally dumbed down, emasculated, vinegar and baking soda level chemistry lab... I sympathize. But YOU need to learn to think very clearly about what you do if you want more- THERE IS NO RESET BUTTON HERE.

Scientwisted - 28-3-2014 at 08:50

Bert! That's wonderful I was waiting until you posted. I can't yet tell if you're crass by nature or just sullen by the "kewls" screwing up the threads with dumb questions. I'm actually a lab tech who's twice as old as you imagine me to be and I never upload videos. That being said I did want your advice. The reason is that I have long been intrigued by gun cotton and would like to do several experiments regarding the properties of the material.

The experiment:

Gun cotton is a nitrate ester that has seen widespread use due to the relative ease of manufacture and easy to obtain components. Aside from industry standards hobbyists have noted inconsistent results when attempting detonation of the substance. I will follow the scientific method and document, document, document etc... I will use NC in several physical states and as well as a few solvents to find which one most reliably and completely detonates. I am to use the same initiator (HMTD) in a yet to be determined quantity from a single batch (same lot # essentially).

I'm sure you know that in order to obtain accurate and consistent results I will need a good amount of highly nitrated NC that is essentially from the same batch (same high quality). RoXefeller mentioned that even on the same batch the nitrogen content of the cellulose may decrease. That is why I wanted to get industry grade NC. They even take a preliminary step of boiling the cotton in NaOH to strip off the vegetable wax. That's the kind of consistencies with subtle nuances that can make all the difference in the experiment.

As we say in the lab "the results are only as good as the sample" or in this case the starting materials. -Twisted

Bert - 28-3-2014 at 09:28

Short answer: blowing shit up. But pitched as research...

Maybe more later.

chemrox - 6-9-2016 at 16:41

@Scientwisted. Great sig! I want to borrow it for my "mood" It describes my general outlook and frame of mind. That last noun is used advisedly.

chemrox - 6-9-2016 at 17:06

The synthesis I have indicated the cotton should be dried at 100*C for two hours. Is this critical? What happens if the cotton is wetter? As in normal room humidity say 40% (the best I can do in my lab during rainy season, dehumidifier and all))

NedsHead - 6-9-2016 at 17:55

I've only ever dried nitrocellulose on a window sill or outside on a sunny day and it turns out fine, I do live in Australia though. according to wiki nitrocellulose has an auto ignition point between 159.85 and 169.85 degrees C

Laboratory of Liptakov - 17-9-2016 at 08:12

You take the sock, give into 3g NC and sock you deploy on hair dryer. Danger: You should be use for this attempt only a new and absolutely pure the sock. And dryer on low or half power. Process I estimate on 15 minute. Dr.