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View Full Version : From AN to Nitric acid. - Archive File


megalomania
June 21st, 2003, 05:04 PM
PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 07-01-2001 03:40 AM
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I recently visited an agricultural supplier and I found out that they sell 24-0-0 fertilizer, he also said it wass AN. I want to know about experiences with making high concentrations of nitric acid with AN and H2SO4 without a vaccume. I know I will have to purify the AN first and boil the H2SO4 down before mixing them, what would be the optimum mix for the two andwhat temp would I have to do this at? I dont have any money for glasware currently, but I plan on getting a cheap retort when I get some cash and then when I get alot more money (don't ask me how it will be a couple of months) I will try to order some jointed glassware from UGT. so I want to know what I could use as a distillation/receving flask. I was thinking like kurt saxon's mayo jar flask, as the boiling flask and I guess the receving flask dosent need to be sealed. does anyone know what tubing types I could use for this all I have read is surgical tubing but isn't that rubber witch gets dissolved my NA? please help me if you have experience in this field.


Tony Montana
Frequent Poster
Posts: 145
From: Australia
Registered: JUN 2001
posted 07-01-2001 04:34 AM
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An aspirator can be acquired reasonably cheaply(or made), and provides a half decent vacuum.
The improvised munitions black book states, 2 parts by volume Potassium nitrate.
1 part by volume Concentrated sulfuric acid.
It also states: If sulfuric acid is obtained from a motor vehicle battery, concentrate it by boiling it until white fumes appear.
The amount of nitric acid produced is the same as the amount potassium nitate you start with. Thus, for 2 tablespoonsful of nitric acid, use 2 tablespoons of potassium nitrate and 1 tablespoonful of concentrated sulfuric acid."
Dry potassium nitrate is added first,
followed by sulfuric acid and stirred into a paste. The heating of this paste produces red fumes(un-condensed nitric acid).
The black book uses a somewhat questionable method for condensing, using 2 coke bottles taped together at their openings. The bottle with the paste(distilling bottle) is put over a small flame, while pouring cool water over the other bottle(collecting bottle). While the obvious safety concerns ring out with this method, like bottles with acid breaking mid sythesis, I wouldnt do it, but hope it helps as it shows the most basic sythesis,I think you could get away with.

[This message has been edited by Tony Montana (edited July 01, 2001).]



wantsomfet
Frequent Poster
Posts: 239
From: EU
Registered: JAN 2001
posted 07-01-2001 05:57 AM
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Nitric acid from AN & H2SO4: At least one mole H2SO4 for every mole AN!
Jointed glassware should be used!
------------------
for best catfood visit:
kangaroooo.cjb.net



Donutty
Frequent Poster
Posts: 228
From: UK
Registered: SEP 2000
posted 07-01-2001 10:36 AM
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My glassware should be coming some time next week. I ordered everything needed for HNO3 productionm, so when I make some, I'll let you know how it goes.


John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 07-01-2001 12:22 PM
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AN is not the best for making nitric acid, NaNO3 and KNO3 are far superior, but it can be done. Everytime ive made nitric with AN though, some impurity has been in it which i cant figure out, but i cant make nitroglycerine with it even when its of high concentration.
Also, tony, if you get red/brown fumes when you produce nitric acid they are not uncondense nitric acid. They are nitrogen dioxide fumes and will not condense unless cooled to a very low temperature. What you want is for the nitric acid to become gaseous, when its gaseous it looks clear. Without a vacuum, though, some decomposition is inevitable which is why the nitric acid fumes and is red. It is possible to make clear white nitric under a vacuum.
The book is also wrong, measuring things by volume is fine with liquids but it doesnt provide accurate measurements with solids. KNO3 can be a fluffy powder or dense prills and the volume can differ alot with its density. In my experience 34mL (about 62.4g of 98%) sulfuric acid for every 58 grams of NaNO3 or 68g of KNO3 is the best ratio. In order to find how much AN to use youd have to figure out how many NO3- ions are in it and compare it with NaNO3 or KNO3 and adjust the amount. A normal aluminum coke can would certainly react with both nitric and sulfuric acid and that method would be foolish to try.
Edit: Pyro, when you buy from UGT look on Ebay and they are selling a full set of jointed glassware for distillation for $125. Thats 30 or 40 under their regular price and also buying through a money order is more anonymous than a credit card.

[This message has been edited by John456 (edited July 01, 2001).]



frostfire
Frequent Poster
Posts: 267
From:
Registered: SEP 2000
posted 07-01-2001 04:40 PM
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darn Donutty, you beat me at ebay....
it's not really wise to use the same name though (if it's really you)


Anthony
Moderator
Posts: 2383
From: England
Registered: SEP 2000
posted 07-01-2001 07:45 PM
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Now you mention it, I seem to have more success using KNO3 than NH4NO3 or NaNO3 in simple nitrations with H2SO4 although maybe since these are all fertilizer grade, the KNO3 is just purer (maybe easier to purify than the other salts?).
Anyway, when I get round to it I'll be in the same boat as you PYRO500 - HNO3 production on the cheap, I plan to use a glass bottle as the distilling vessel make a bung from fibreglass resin (I tested this at room temp and it was HNO3 proof) and use PVC aquarium tubing (H2SO4 proof, haven't tested with HNO3 yet) although I'll most likey use a glass elbow through the bung as I have a small amount of glass tubing.

BTW 1.27gm NH4NO3 and 0.77gm H2SO4 make 1gm HNO3

Good luck and if at first you don't succeed, try again, then again, then cry and smash it up


[This message has been edited by Anthony (edited July 01, 2001).]



PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 07-02-2001 12:39 AM
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will aquarium tubing hold the heat? I think that it may melt, what is the optimum tempature to distill the paste at? I also can get calcium nitrate fertilizer 18-0-0 and I may get potassium nitrate fertilizer if I can find out where to get it from. does anyone that lives in the U.S. know what kinds of fertilizer has KNO3 in them, and what are the numbers on it. if I know the numbers I can mass dial the fertilizer company's and their stores to find suppliers. I think I really take advantage of free local calling (with a wardialer and a third phone line ) anyways, any one in the US please tell me where you get your KNO3 from.


c0deblue
Frequent Poster
Posts: 229
From:
Registered: JAN 2001
posted 07-02-2001 01:27 AM
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Fertilizer grade "pure" KNO3 is normally sold as 14-0-45 (the numbers can vary a little depending on the manufacturer). Our local agricultural supplier had none in stock, but could get it in one day from their supplier. The quoted price was $23.00 for 25 lb. I've heard of lower prices, but this is probably a typical range for retail outlets. Don't know if this was prills, granular or powder.
BTW, AN fertilizer is usually 34-0-0, so if the stuff your local supplier had was really 24-0-0 as you said (not a typo), it probably means its got a lot of inert material like chalk mixed with it. You'd first have to get rid of that.



Anthony
Moderator
Posts: 2383
From: England
Registered: SEP 2000
posted 07-02-2001 05:07 PM
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I've used aqaurium tubing for distillation at temps over 100*C, it goes a bit soft (so you can squash it with your fingers) but does hold up.


Donutty
Frequent Poster
Posts: 228
From: UK
Registered: SEP 2000
posted 07-02-2001 05:40 PM
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Thats strange, I thought I was the only Donutty about!!


Anthony
Moderator
Posts: 2383
From: England
Registered: SEP 2000
posted 07-02-2001 06:38 PM
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If you're talking about this post:
"My glassware should be coming some time next week. I ordered everything needed for HNO3 productionm, so when I make some, I'll let you know how it goes."

Then it's you, you daft git same number of posts and the first 5 digits of the IP's are the same.



Tony Montana
Frequent Poster
Posts: 145
From: Australia
Registered: JUN 2001
posted 07-03-2001 03:09 AM
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JOHN456: I may need to clarify my last post!
1. In my first post, the book (or I) did not say anything about applying a vacuum with the afore mentioned procedure. Therefore the fumes will be red.
2. Prilled KNO3 would be crushed into powder, if it was aquired that way. Making volume measurements more accurate.
3. A BOTTLE is glass
A CAN is aluminium
I say nothing about a CAN, I do refer to a bottle though.


PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 07-03-2001 03:53 AM
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I think I designed a vaccume still that might work, I just need to convert it to gif to upload and host the image of it


ALENGOSVIG1
Moderator
Posts: 782
From: Canada
Registered: NOV 2000
posted 07-03-2001 03:58 AM
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I have purchased a complete 24/40 distilling apparatus from united glass technologies and should arrive soon. should be great! i jut gotta rip the compressor outa that old fridge in the test field and make a vaccum.


Donutty
Frequent Poster
Posts: 228
From: UK
Registered: SEP 2000
posted 07-03-2001 04:35 PM
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Mmm.. Must be a coincedence! It's a small world, afterall...
Oh and nice one using your power as an Admin to view my IP and tell everybody!!



Anthony
Moderator
Posts: 2383
From: England
Registered: SEP 2000
posted 07-03-2001 05:07 PM
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Notice how yours and "his" post count is going up sychronously? Maybe someone used your computer and posted a message, but it's a very strange thing to post...
I think you should lay off whatever it is that's killing yout short term memory...

I didn't tell anyone your IP Besides it's a dynamic one, I presume your ISP always uses the same first 3 digits.

No more acetone fumes!



PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 07-03-2001 08:30 PM
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oops!
[This message has been edited by PYRO500 (edited July 03, 2001).]



PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 07-03-2001 08:31 PM
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here is my idea for A nitric acid still, I am assuming hardened fiberglass putty is acid proof does anyone think it looks workable? here is the location sorry I cant post it directly geocities wont let me.
to view it just cut and paste into the location bar.
"http://www.geocities.com/pyro2000us/hno3.jpg"


[This message has been edited by PYRO500 (edited July 03, 2001).]



John456
Frequent Poster
Posts: 105
From:
Registered: MAR 2001
posted 07-04-2001 12:03 AM
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Tony-
I know you didnt say anything about a vacuum, but the red fumes arent nitric acid vapors, there are some vapors among them that condense and thats why a vacuum is preferred for better yields. it would probably be accurate enough measuring by volume if it was powdered but id still rather measure it by weight =) Sorry about the bottle, English is not my first language and i sometimes confuse bottles with cans especially when i see aluminum cans of coke in the stores everyday.


simply RED
Frequent Poster
Posts: 242
From: HELL
Registered: OCT 2000
posted 07-04-2001 06:20 AM
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Someone said that making HNO3 from NH4NO3 and H2SO4 can be dangerous because some nitramines form....


PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 07-04-2001 02:23 PM
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any comments on my still?


Donutty
Frequent Poster
Posts: 228
From: UK
Registered: SEP 2000
posted 07-04-2001 04:39 PM
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Would probably work if the tubes were uniform ( unlike the drawing ). I prefer to use professional stuff though because (I hope) you can trust it! (and it looks good)


PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 07-04-2001 05:53 PM
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in the drawing I was trying to imply that the tubing is in coils between the jars. it was hard to duplicate the drawing and I was tired so it looked kinda funky I do not have the money for expensive glassware so I decided to desingn a vaccume still that could work for many purposes. I am assuming that the fumes of the solution that are the least volitle will condense in the first jar and then the fumes that need to be cooled more will go to the second jar and so on till the fumes are condensed, the aquarium air manifold lets the vacume suck in air to keep from getting such a high vaccume that all liquids evaporate.


Anthony
Moderator
Posts: 2383
From: England
Registered: SEP 2000
posted 07-04-2001 06:27 PM
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Looks good. The onlt thing I can think of is that, depending on the strangth of the vacuum, the liquid HNO3 might not go up the tubing and into the jar (it'd collect at the bottom of the U's between the jars). Also, no provision to stop HNO3 vapours getting into the vacuum pump (unless it's expendable?)


PYRO500
Moderator
Posts: 1513
From: somewhere in florida
Registered: SEP 2000
posted 07-04-2001 08:06 PM
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I was thinking of sunig small tubing, 1.5 or 2 mm inner diamater tubing that would have the liquid pressed out of it easily, if there is still liquid in the tube I will release the vaccume by opening all the valves in the air manifold and unstoppering the distillation flask then I will slowly close the valves and let the vaccume pull the HNO3 into the jars. I plan on having awater aspirator powered by a pool pump if I can find one cheap and I wont have to worry about the vapors ruining the pump. the air manifold allows me to slowly open pathways for the air till the vaccume is just enough to lower the boiling point of the liquid so it will only boil when above room tempature.

neo_philosopher
June 27th, 2006, 02:32 PM
My way of translating AN into Nitric acid is like this-

1) dissolve alot of AN into a bucket of water
2) Perform electrolysis with copper electrodes.
3) Boil till all the water is gone. usually turns from green
to blue
4) decompose at ~180C and dissolve the gases in water

electrolysis makes ammonia and copper nitrate. I like to buy a
big chunk of copper from a scrap yard, use that on the positive
end and just a wire close to the surface on the neg. end.

See, weird compounds come alive with impurities, I think its like:

[Cu(NH3)4]SO4

this kind makes the solution green, once the temp is over 140 it releases
the final ammonia making blue copper nitrate liquid. Decomp is like this-

Cu(NO3)2 -> CuO + NO2 + O2

so perfect gas solution is made for water dissolving.

All it needs is to cool it down a bit. its better than any other metal decomp. b/c its the coldest. Cheap, simple. Although the power supply needs to be high amps, I found out that computer power sources can dish out 10amps for 12v+. so I use two sources in parallel and the neg in ground. 20 amps at 12v is good enough to make alot of copper nitrate. Just a warning, sometimes I had the result that the CuNO3 decomposed very rapidly... very rapidly indeed- BOOM

The_Duke
June 29th, 2006, 04:19 AM
Why bother... :rolleyes:

neo_philosopher
March 10th, 2007, 09:17 PM
I would bother because not only electrolysis is good for making copper nitrate, but also you can just heat ammonium nitrate and copper or copper oxide and that releases ammonia. Then you have a cyclic process which only uses AN and outputs in one phase NH3 and in the next NO2 + O2. AN in, HNO3 out

Squizzy
April 1st, 2007, 12:25 AM
Why not convert the AN into Sodium nitrate using Sodium Hydroxide. Much safer making nitric acid from that than AN.
I ve used a cast iron camp oven (dutch oven) as a reaction vessel instead of glass vessel. Drilled a hole and used a conventional distillation head , condensor and receiving flask. To seal the camp oven use clay lute around the rim and the distilation receiver hole. Heat the oven to burn off any organics and oils.
Afterwards theres only a bit of surface rust on the oven after it dries mainly.
I used gas burner to gently heat the oven