| Pages:
1
..
3
4
5
6
7
..
12 |
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
What to you mean by "decompose in nitric acid"
You can make RDX with just 99%Nitric acid and Hexamine, without Ac2O
|
|
|
roXefeller
Hazard to Others
Posts: 463
Registered: 9-9-2013
Location: 13 Colonies
Member Is Offline
Mood: 220 221 whatever it takes
|
|
Quote: Originally posted by underground  | | I was wondering if RDX can be made by mixing H2SO4 with an excess of Ammonium Nitrate, so all of H2SO4 is going to react, to form
pure HN03, and also the rest AN is also going to help the formation of RDX |
The excess of NH4NO3 is useful because it makes up the nitrogen deficiency in hexamine. The 1951 Bachmann article mentions around 30% of RDX contains
this supplemental nitrogen. They determined this by radioisotope N15 that the nitrate was made from.
But you need to distill the nitric acid away from the bisulfate. There is an equilibrium occurring within the bisulfate:
2HSO4 <--> H2SO4 + SO4
There's always acid lingering.
|
|
|
DubaiAmateurRocketry
National Hazard
Posts: 841
Registered: 10-5-2013
Location: LA, CA, USA
Member Is Offline
Mood: In research
|
|
Sorry I meant in sulfuric acid, typing mistake.
|
|
|
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
| Quote: Originally posted by roXefeller | | Quote: Originally posted by underground | | I was wondering if RDX can be made by mixing H2SO4 with an excess of Ammonium Nitrate, so all of H2SO4 is going to react, to form
pure HN03, and also the rest AN is also going to help the formation of RDX |
The excess of NH4NO3 is useful because it makes up the nitrogen deficiency in hexamine. The 1951 Bachmann article mentions around 30% of RDX contains
this supplemental nitrogen. They determined this by radioisotope N15 that the nitrate was made from.
But you need to distill the nitric acid away from the bisulfate. There is an equilibrium occurring within the bisulfate:
2HSO4 <--> H2SO4 + SO4
There's always acid lingering. |
H2SO4 + NH4NO3 --> NH4HSO4 + HNO3
Not any bisulfate at all, if you just let all the AN to react with H2SO4, will not end with pure NH4HSO4 and HNO3.
Not any H2S04 to destroy the RDX, or bisulfate.
[Edited on 2-4-2014 by underground]
|
|
|
Bert
Super Administrator
Posts: 2821
Registered: 12-3-2004
Member Is Offline
Mood: " I think we are all going to die. I think that love is an illusion. We are flawed, my darling".
|
|
underground, DubaiAmateurRocketry, roXefeller:
You each have a piece of a puzzle correct.
And another you're missing, or an incorrect assumption.
I'm betting between the 3 of you, a good answer to underground's question can shortly be had-
Start here: Chemical reactions are reversible, and go to an equilibrium.
Write as clearly as you can, ballance reactions (and check that they are what happens in the real world!), provide links to where you found concepts.
I'll watch you figure it out.
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).
|
|
|
Vikascoder
Hazard to Others
Posts: 309
Registered: 28-1-2012
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by TheAlchemistPirate | This guy already showed a way. | Quote: Originally posted by lucifer | I’ve made rdx with distilled 99% HNO3 and with methenamine,
The Yeild wasn’t bad, 74% (29,7gr rdx out of 25gr methenamine).
I,ve changed the nitration time in meglomainia’s method, to get a better yeild.
(info from urbanski).
Well I have already read this post but I want to know the accurate process which uses hexamine dinitrare and concentrated nitric acid to make rdx
Slowly ad 25gr methenamine to the HNO3, which went quite easy keeping the temperature under 30degr C
After that put the solution in a water bath of 60 degr C, letting the temperature of the solution rise to 55 degr C Keep it at this temperature for 12
minutes.
Then cool it down in a ice bad to 20 degr C
During this phase some rdx becomes visible in the solution.
Let it stand for 10 min.
Then add to the solution 400 ml of ice water
A lot more of rdx will precipitatet out of the solution.
Let this solution stand for 5 minutes
After filtering neutralised the rdx with 400 ml 5% sodium bicarbonate solution.
The yeild after completely drying was 29.7 gr which is if I am ride about 74%
|
|
Girls break promises like a small child breaks pencil tips so don't trust girl bcoz no girl=no tension
|
|
|
DubaiAmateurRocketry
National Hazard
Posts: 841
Registered: 10-5-2013
Location: LA, CA, USA
Member Is Offline
Mood: In research
|
|
You can not use H2SO4 because Hexamine decomposes in the presence of concetrated H2SO4 to form formaldehyde and ammonia. I dont know what Bert is
trying to say.
http://dspace.upce.cz/bitstream/10195/42530/1/MartinkovaZ_De...
|
|
|
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
| Quote: Originally posted by Bert | underground, DubaiAmateurRocketry, roXefeller:
You each have a piece of a puzzle correct.
And another you're missing, or an incorrect assumption.
I'm betting between the 3 of you, a good answer to underground's question can shortly be had-
Start here: Chemical reactions are reversible, and go to an equilibrium.
Write as clearly as you can, ballance reactions (and check that they are what happens in the real world!), provide links to where you found concepts.
I'll watch you figure it out.
|
Bert as i said, it was an idea. The concept was from my mind.
| Quote: Originally posted by DubaiAmateurRocketry | You can not use H2SO4 because Hexamine decomposes in the presence of concetrated H2SO4 to form formaldehyde and ammonia. I dont know what Bert is
trying to say.
|
I know that Hexamine decomposes in the presence of concetrated H2SO4, that is why i said to use an excess of ammonium nitrate, to convert ALL of H2SO4
to HNO3. Here is the ballance reaction
H2SO4 + NH4NO3 --> NH4HSO4 + HNO3
So at the end you are going to have a mix of NH4NO3/HNO3/NH4HSO4.
So i can not see any reason why RDX is going to decompose as long as there is not any more H2SO4 (It has already be converted to NH4HSO4 and HNO3 with
the presence of NH4NO3)
I hope that it is clear now.
|
|
|
VladimirLem
Hazard to Others
Posts: 204
Registered: 24-5-2010
Member Is Offline
Mood: Have no fear <Vlad> is here.
|
|
....well...and you re going to nitrate hexamine with that crap?
its the same problem that you have at the K6 synthgesis...to make these compounds you need really pure/high quality chemicals...espechially cause the
one step synthesis of hexamine needs a huge excess of HNO3 even if its 95%<...as i said, you could try this at making ETN but i guess you will
waste expensive stuff at making RDX this way
|
|
|
Bert
Super Administrator
Posts: 2821
Registered: 12-3-2004
Member Is Offline
Mood: " I think we are all going to die. I think that love is an illusion. We are flawed, my darling".
|
|
| Quote: |
I know that Hexamine decomposes in the presence of concetrated H2SO4, that is why i said to use an excess of ammonium nitrate, to convert ALL of
H2SO4 to HNO3. Here is the ballance reaction H2SO4 + NH4NO3 --> NH4HSO4 + HNO3 So at the end you are going to have a mix of NH4NO3/HNO3/NH4HSO4.
So i can not see any reason why RDX is going to decompose as long as there is not any more H2SO4 (It has already be converted to NH4HSO4 and HNO3 with
the presence of NH4NO3) I hope that it is clear now.
|
Clear. Understand exactly what you thought can happen, and why.
One of the best ways to find how well you've learned something is to try and teach it to someone else.
Who among you can explain clearly enough to underground WHY there is still going to be sulfuric acid present, or figure out what concept he need learn
to understand?
Why are YOU being asked if you can explain such things?!
[Edited on 2-4-2014 by Bert]
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).
|
|
|
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
| Quote: Originally posted by Bert |
| Quote: |
I know that Hexamine decomposes in the presence of concetrated H2SO4, that is why i said to use an excess of ammonium nitrate, to convert ALL of
H2SO4 to HNO3. Here is the ballance reaction H2SO4 + NH4NO3 --> NH4HSO4 + HNO3 So at the end you are going to have a mix of NH4NO3/HNO3/NH4HSO4.
So i can not see any reason why RDX is going to decompose as long as there is not any more H2SO4 (It has already be converted to NH4HSO4 and HNO3 with
the presence of NH4NO3) I hope that it is clear now.
|
Clear. Understand exactly what you thought can happen, and why.
One of the best ways to find how well you've learned something is to try and teach it to someone else.
Who among you can explain clearly enough to underground WHY there is still going to be sulfuric acid present, or figure out what concept he need learn
to understand?
Why are YOU being asked if you can explain such things?!
[Edited on 2-4-2014 by Bert] |
Yea i understand. As roXefeller thried to explain, it is the equilibrium that it is going to occur, so always some H2SO4 will be in presence, that is
why distillation it is necessary
|
|
|
TheAlchemistPirate
Hazard to Others
Posts: 151
Registered: 25-3-2014
Location: The point of no return
Member Is Offline
Mood: Enigmatic
|
|
Earlier today I attempted to make nitric acid by nitrate salt and sulfuric acid distillation, but unfortunately, after I started adding sulfuric acid
it started to immediately boil and make tons of nitrous oxide gas. I used nurdrage's method, here are the things I did:
1. I preheated a two-necked distillation flask to 120 degrees C (with all the distillation apparatus set up)
2. I added 40 grams of KN03
3. I started to add 80 milliliters of H2SO4, but it started to start making NOx gasses, so I turned off my hot plate and sealed the opening.
It is now sitting in my garage, Im going to clean it tomorrow. Could someone tell me what I did wrong? In videos it didn't react early as fast.
[Edited on 4-4-2014 by TheAlchemistPirate]
"Is this even science anymore?!"
|
|
|
Zyklon-A
International Hazard
Posts: 1547
Registered: 26-11-2013
Member Is Offline
Mood: Fluorine radical
|
|
Don't preheat it.
|
|
|
TheAlchemistPirate
Hazard to Others
Posts: 151
Registered: 25-3-2014
Location: The point of no return
Member Is Offline
Mood: Enigmatic
|
|
Doesn't it make nitric acid when not heated? What if I preheated it to a lower temperature? One not high enough to make large amounts of nitrous oxide
gas?
"Is this even science anymore?!"
|
|
|
Bert
Super Administrator
Posts: 2821
Registered: 12-3-2004
Member Is Offline
Mood: " I think we are all going to die. I think that love is an illusion. We are flawed, my darling".
|
|
Oh yeah. NOx.
If you keep your Sulfuric acid in a freezer, adding the nitrate is a LOT less exciting...
[Edited on 4-4-2014 by Bert]
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).
|
|
|
TheAlchemistPirate
Hazard to Others
Posts: 151
Registered: 25-3-2014
Location: The point of no return
Member Is Offline
Mood: Enigmatic
|
|
I mean preheat it to a low temperature at first then after I pour it in, raise the temperature.
"Is this even science anymore?!"
|
|
|
Zyklon-A
International Hazard
Posts: 1547
Registered: 26-11-2013
Member Is Offline
Mood: Fluorine radical
|
|
You heat it only after you add the reagents in the flask, to distill it. you don't want the reaction to happen until everything is in the
controlled flask.
Keep the flask at RT (or below) until everything is inside and you are ready to distill.
[Edited on 4-4-2014 by Zyklonb]
|
|
|
TheAlchemistPirate
Hazard to Others
Posts: 151
Registered: 25-3-2014
Location: The point of no return
Member Is Offline
Mood: Enigmatic
|
|
Oh, I didn't know that I had to cool it. I never saw a tutorial mentioning that, and I have researched this procedure for weeks. Thanks for replying,
btw nothing was damaged, and I left the area for a while to let the gas escape to outside ( I live in a remote area )
"Is this even science anymore?!"
|
|
|
DubaiAmateurRocketry
National Hazard
Posts: 841
Registered: 10-5-2013
Location: LA, CA, USA
Member Is Offline
Mood: In research
|
|
Why would one heat it? If you add KNO3 to sulfuric acid slowly and control the temperature, you would be fine. HNO3 boils at around 80 degree
Celsius, therefore as bert said, adding KNO3 to sulfuric acid that was kept in a freezer sounds like a very good idea. Have any one tried freezing the
KNO3 too? does it help?
|
|
|
TheAlchemistPirate
Hazard to Others
Posts: 151
Registered: 25-3-2014
Location: The point of no return
Member Is Offline
Mood: Enigmatic
|
|
I thought that distilling the KNO3 and the H2SO4 would be better than simply adding the two chemicals together while they are cold, for the following
reasons:
1. Better purity
2. Better yield
3. Higher concentration
4. less dangerous
I did run into a problem today though, after washing the equipment I noticed that the ground glass stopper in my two-necked boiling flask was stuck. I
noticed small crystallization between the glass. I heard this happens when you don't apply vacuum grease to the joints, but I did apply it and all my
other joints were fine. Is there a simple way to get the stopper off?
"Is this even science anymore?!"
|
|
|
Zyklon-A
International Hazard
Posts: 1547
Registered: 26-11-2013
Member Is Offline
Mood: Fluorine radical
|
|
Heat it up with a heat gun or similar device. The outer joint will expand slightly, and before the inner joint.
|
|
|
Bert
Super Administrator
Posts: 2821
Registered: 12-3-2004
Member Is Offline
Mood: " I think we are all going to die. I think that love is an illusion. We are flawed, my darling".
|
|
Heat gun doesn't work super well-
Best bet is soak a liquid into the joint, if you use heat it has to be FAST and tightly focused.
See here: http://onlinelibrary.wiley.com/store/10.1002/9780470141045.a...
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).
|
|
|
TheAlchemistPirate
Hazard to Others
Posts: 151
Registered: 25-3-2014
Location: The point of no return
Member Is Offline
Mood: Enigmatic
|
|
I am heating the flask in boiling water right now, I will take it out in a few minutes. That link doesn't want to work with my computer for some
reason, sorry for going completely off topic. UPDATE: The boiling water did nothing,not sure why I thought thatd work. I am now freezing the flask,
tomorrow I will use a propane torch on the female joint and try to pull out the male one...
[Edited on 5-4-2014 by TheAlchemistPirate]
"Is this even science anymore?!"
|
|
|
Bert
Super Administrator
Posts: 2821
Registered: 12-3-2004
Member Is Offline
Mood: " I think we are all going to die. I think that love is an illusion. We are flawed, my darling".
|
|
Try a penetrating solvent capable of dissolving grease & displaceing water before whipping out the torch, working glass with heat is an art
learned over a big pile of busted glass in my experience!
I bought a used vacuum dessicator with a totally frozen valve, grease had turned to rock. Soaking the frozen joint over night with Kano "Kroil" allowed me to get it apart easily the next day.
Don't be in a hurry... You can always break it later of you want!
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).
|
|
|
TheAlchemistPirate
Hazard to Others
Posts: 151
Registered: 25-3-2014
Location: The point of no return
Member Is Offline
Mood: Enigmatic
|
|
Ok, Im now soaking it in a high-power grease remover. I made sure to check this thread before I tried heating it. Also, could someone answer my
question about the efficiency of directly adding cold H2SO4 to KNO3?
"Is this even science anymore?!"
|
|
|
| Pages:
1
..
3
4
5
6
7
..
12 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
