arthur2647
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What is this whole "nitration" thingy about?!
Hi, I'm new here, just have a few questions. Before I give my situation and questions, i apologize if I'm interrupting. I tried to synthesize NG with
more of dilute acids, around 40 percent sulfuric acid and potassium nitrate. I filled the beaker with around 50ml of the acid and added around 15 g
nitrate to it. To this i added about 1-2ml of glycerin drop by drop. Shortly after adding I was presented with a subtly sweet smell which I guess is
the NG. But i don't believe I ever achieved the tri- ester form. As well I could see a hazy zigzag line where the glycerin hit the acid as it trailed
down to the bottom.
During the nitration which i left for about 90 minutes, I did see
a few bubbles here and there form on the top and also some very slight haze in the top layer. However after i added some cold water to this, it all
vanished and i was left with a clear solution. Actually to be honest, I did this experiment twice. The first time i was left with tiny clear bubbles
(~20) spread out on the bottom after adding cold water, and they would not dissolve in water. The second time i was left with just that clear
solution.
So in the end this got me really interested in terms of the action of these acid mixtures on the glycerin. It seems that the glycerin is acted upon
almost instantly but I'm guessing the acid just loses potency quite fast. It makes me wonder how much more concentration do i really need to get a
decent nitration.
If you guys have any ideas or input, thanks.
[Edited on 17-9-2015 by Bert]
[Edited on 17-9-2015 by Bert]
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Bert
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Start at the beginning of this thread, read the whole thing... Don't waste any more chemicals until you have done that.
Look for the Phokion Naoum book in the sciencemadness library:
http://library.sciencemadness.org/library/index.html
Read the relevant chapters (or better yet, the whole thing!).
FAR too dilute sulfuric acid.
Battery electrolyte?
http://www.sciencemadness.org/talk/viewthread.php?tid=19117
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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arthur2647
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Thanks...it is true, its from battery acid. But part of that large journal , it does mention if you add excess sulfuric acid it can counterbalance the
lower hno3 amount. I have to say it doesn't really matter to me if i make the tri ester or not. I just want to understand the chemistry behind
nitration more. It does seem though that the most concentrated acids are the best. I just don't see a lot of literature on potential of these lower
acids. For example with excess sulfuric acid would it manage to make the di ester, since i know the first OH group is not hard to nitrate.
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ecos
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try to buy more concentrated sulphuric acid or you can concentrate it yourself by boiling or distillation :
https://www.youtube.com/watch?v=tgUH0HXrOKE
boiling is faster and would give you concentration till 80% as far as i remember !
FYI- avoid nitroglycerin since you don't have experience with EM. better to deal with nitrocellulose !
[Edited on 3-9-2015 by ecos]
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Tabun
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OK!I'm getting tired of this.These 2 names,TNT and dynamite has been so raped and they are so freaking popular that you can't google them without
getting firecrackers,minecraft and the like : nothing on the subject(well...almost).Can somebody tell me about the tube dynamite is put in?How thick
is it?What is it made of?Carboard or what?Is it pressed in there?
Yea...I know : "What dynamite?".Just try to make it general.
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Hennig Brand
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I think a lot of different things have been used, and I am not an expert on that, but I have found that common kitchen grade waxed paper works well.
Make tubes by rolling 2 -3 layers, or whatever you deem appropriate, onto a former (e.g. cardboard tube or dowel of the right size). One end can be
folded in and sealed and the dynamite can be spooned in and pressed in increments (normally fairly light pressing depending on dynamite type). Loading
is very easy and fast especially once the cartridges get over 3/4" to 1" or so.
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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arthur2647
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so back to my last post, any ideas. dynamite is cool and all but i dont need that
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Hennig Brand
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Do some reading, there is a tremendous amount of information on NG even in this thread alone. The esterification of glycerin by nitric acid is an
equilibrium reaction and I am fairly sure there is equilibrium data which you could avail yourself of if you searched a bit.
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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arthur2647
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well i did some reading, but my hope of coming here was that people would like to have a discussion about things. Basically i know i need
concentrated acid to make the final nitrated form reliably. I just haven't come across in my reading much about dilute acids. All i found was mainly
that dilute mix of acids can create glycerin mononitrate. But i haven't found if its possible to create more.
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Joeychemist
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That would require you to have something worthwhile to discuss...
Quote: Originally posted by arthur2647  | | Basically i know i need concentrated acid to make the final nitrated form reliably. I just haven't come across in my reading much about dilute acids.
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Nitroglycerin and Nitroglycerin Explosives By Naoum
You might want to check out the chapters on nitratring acids and the Homologous and Related Nitric Esters 
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ecos
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| Quote: Originally posted by arthur2647 | well i did some reading, but my hope of coming here was that people would like to have a discussion about things. Basically i know i need
concentrated acid to make the final nitrated form reliably. I just haven't come across in my reading much about dilute acids. All i found was mainly
that dilute mix of acids can create glycerin mononitrate. But i haven't found if its possible to create more.
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do you have a problem to concentrate the diluted acids your self ?
you will find a lot of videos on youtube on how to concentrate nitric acid or sulphuric acid.
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roXefeller
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They do like discussions, but not leading questions on century old compounds that have been researched exhaustively. Sulfuric acid only has a role in
dehydrating, so you should ask, how concentrated does it need to be to function as a dehydrator. The question isn't really about strength of nitric
acid because it's water component effectively dilutes the sulfuric acid more. It is the same as adding 97% NA to 30% SA if you add 70% NA to 60% SA.
Patent research that you should do, would indicate that industry finds little value in concentrations of SA below 70% as a dehydrator in these ester
reactions. A tangent question would be, how is glycerin mono- or di-nitrate created and what strengths are employed there. You can find it. I (and
the other advanced users and mod's) don't want to spoonfeed knowledge of dangerous compounds to people who aren't willing to research mundane details,
it's an ethics and site liability thing. If you really want a discussion, ask questions that are more meaningful or match the experience of those
whom you are probing.
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Bert
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| Quote: Originally posted by arthur2647 | well i did some reading, but my hope of coming here was that people would like to have a discussion about things. Basically i know i need
concentrated acid to make the final nitrated form reliably. I just haven't come across in my reading much about dilute acids. All i found was mainly
that dilute mix of acids can create glycerin mononitrate. But i haven't found if its possible to create more.
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First: go read the forum FAQ:
http://www.sciencemadness.org/madscifaq.html#2.1_Board_topic...
Next: Go to the forum library.
http://library.sciencemadness.org/library/index.html
Download these books for a start:
Phokion Naoum: Nitroglycerin and Nitroglycerin Explosives
Tenney L. Davis: Chemistry of Powder and Explosives
Read about your topic there. Come back and ask questions, provide references for WHERE the information you ask to clarify came from. Then, you may
post outside of "beginnings".
And I GUARANTEE you, you'll get to have a discussion under those terms-
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Bert
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Thread Moved
17-9-2015 at 10:08 |
ave369
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Here's the resident forum researcher on Boiling the Bat! (battery acid). And a little how-to.
1. Flask
The best container to boil down H2SO4 is a round-bottom flask. If you have one, the heating method is a non-issue: you can even heat it directly on a
kitchen gas stove, if you have a tripod or stand. If you have an electric stove, a conical Erlenmeyer flask could be preferable, but these are not as
crackproof as round-bottom flasks. A thin sand bath is preferable if you use an Erlenmeyer flask on a kitchen electric stove.
If you do not have any flasks, it gets harder. Jars can be used, but they are very prone to thermal cracking, so a very thick sand bath is recommended
if you use a jar. One of the best vessels for this purpose is a thick glass casseroling dish, it is nigh uncrackable.
2. Boiling chips
Pour the Bat into your chosen container. Toss some boiling chips into it once you start heating. Boiling chips are pieces of porous material that make
the process of boiling continuous and calm, as opposed to not boiling, overheating and suddenly going "POOF!". This is called bumping, and sulfuric
acid loves to do it. Without boiling chips, you will hear gunfire from your flask and the acid may even be forcefully ejected from it. So use boiling
chips: small pieces of brick, pumice, some kinds of porcelain will also do. They will make your boiling calm, like you are boiling an egg.
One thing to remember about boiling chips is that heating should be continuous for them to be effective. If you boil your acid, let it cool down and
heat it again, boiling chips may refuse to work. If this happens, toss some fresh ones in.
One final thing to remember about boiling chips: do NOT toss them in when the acid is already bumpily boiling! It will make it boil extremely
vigorously and, possibly, be ejected from your vessel.
3. The Mist.
It's that Mist! The infamous, dreaded Mist!
What the Mist is? It is a mixture of H2SO4 vapors, SO3, H2O, and SO2. It starts to form when your boiling acid reaches the threshold of 80%. It is
extremely noxious, carcinogenic and smells like pure pain and hell. It is milky white in color. You can usually smell the Mist long before it actually
touches your nose (and it is not a good thing at all to let it anywhere near your face!)
What to do when you detect it? Depends on what do you need the acid for. If you need it for things like Glauber's acid syntheses, you can stop right
here. 80% acid will be enough.
If you need it for nitrations, you need much more than that. You have to somehow get around the Mist. Here's a few common methods:
* Devise a remote control of your heating appliance. Once the Mist emerges, open all windows in the room, evacuate the room and watch over the process
through the glass in the door. Turn off the heating when 30 minutes/1 hour/2 hours etc pass.
* Use a retort, and redirect the Mist into a trap flask filled with bicarbonate of soda. This will thwart the Mist and turn it into harmless steam.
* Put a reflux condenser on your flask when the Mist starts to form. This makes the Mist much less intense, but does not stop it completely (a reflux
condenser long enough to stop the Mist right in its tracks also stops the boiling down of acid, returning all the water down).
* Distill the acid. You need very good glassware to do this.
I'm also researching various ways to get around boiling down over 80% and produce 98% or oleum another way. So far, I've yet to find an easy and fun
way to do so. Pyrosulfate pyrolysis requires very high temperatures and sacrificial glassware. Distillation of acid mixture is so far a very
experimental method, and I'm still unsure of what to expect from it.
[Edited on 17-9-2015 by ave369]
Smells like ammonia....
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