Lapis_infernalis
Harmless
Posts: 6
Registered: 10-3-2006
Member Is Offline
Mood: No Mood
|
|
Ammonium perchlorate from a electrolysis of Ammonium chlorate???
On the most good german chemistry boards the people become angry when you ask for synthesis of explosives or the starting substances. For this reason
I`m here.
My questions are what cathode and anode material I need, what concentration the diluotin need, toxicity, the amperage and if it still too dangerous
and I`ll blow myself up when I test this 
I can also make NH4ClO4 from NaClO4 (from a NaClO3 electrolysis) and a ammonia diluoton but I need Na+ free NH4ClO4 for blue stars
I hope you can answer my questions.
Sincerely yours Lapis_infernalis
Sorry for my bad grammar
|
|
|
PHILOU Zrealone
International Hazard
Posts: 2893
Registered: 20-5-2002
Location: Brussel
Member Is Offline
Mood: Bis-diazo-dinitro-hydroquinonic
|
|
Uses KClO4 colourles to pale lilas when in a flame.
Other flame colourisers overflow potassium.
NH4ClO3 as a base for NH4ClO4...not safe at all.
NH4ClO3 --> NH4ClO4 + NH4ClO2 + NH4ClO + NO2(-) + NO3(-) +NxOy + N2 + NCl3
Most products of this reaction goes inflame spontaneous...
NH4 chlorate may explode in solution!
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
|
|
|
MadHatter
International Hazard
Posts: 1332
Registered: 9-7-2004
Location: Maine
Member Is Offline
Mood: Enjoying retirement
|
|
NH4ClO4
Continue to make it from NaClO4. Ammonium chlorate is dangerously unstable, known to
explode by itself. I understand why you want to get the Na out because of the yellow colour
it gives to the flame. You'll have to use fractional crystallization a few times with distilled
water to purify the NH4ClO4.
As for anode and cathode materials, that subject has been covered extensively on this site.
Do a search on chlorates or perchlorates and you'll find your answer.
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
|
|
|
Lapis_infernalis
Harmless
Posts: 6
Registered: 10-3-2006
Member Is Offline
Mood: No Mood
|
|
On a german chemistry board someone had synthesis NaClO4 from NaClO3. He destroy the NaClO3 rests in the NaClO4 with hydrochloric acid. Would it also
act with NH4ClO3/NH4ClO2/NH4ClO???
I couldn`t imagine that a NH4ClO3 solution can explode!!!
Sorry for my bad grammar
|
|
|
chemoleo
Biochemicus Energeticus
Posts: 3005
Registered: 23-7-2003
Location: England Germany
Member Is Offline
Mood: crystalline
|
|
No, the point is that UNLIKE NaClO3, the NH4+ in the NH4ClO3 can be oxidised, i.e. to nitric acid and other things, or ammonia. This is why you would
be wasting your time trying to oxidise NH4ClO3 with electrolytic methods, as you won't get the correct product. Thus no need speculating on the effect
of HCl.
Better to use NaClO3-> NaClO4, and do the metathesis, i.e. with NH4Cl. Trickier, but there's no way around it.
[Edited on 10-3-2006 by chemoleo]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
|
|
|
garage chemist
chemical wizard
Posts: 1803
Registered: 16-8-2004
Location: Germany
Member Is Offline
Mood: No Mood
|
|
NH4ClO3 is explosive on its own. Heating it won't produce perchlorate, but an explosion instead.
To get Ammonium perchlorate, you have to follow the instructions for NaClO4 and add a saturated NH4NO3 solution to the NaClO4 solution. Cooling will
precipitate NH4ClO4.
To get the sodium out, it will have to be recrystallized from distilled water several times.
Recrystalization is an important process in chemistry, and done in nearly every synthesis. Guess why! It's a simple process for obtaining compounds in
a state of purity.
To directly get sodium- free NH4ClO4, perchloric acid is neutralized with ammonia solution. This will produce top quality NH4ClO4, suitable for all
purposes.
The perchloric acid can be obtained by distilling KClO4 with H2SO4. This must be done in vacuum, otherwise it will be dangerous.
And if you don't have platinum anode, you can pretty much forget about electrolytic production of perchlorates.
The process with graphite is very tricky, and only one member here has had success with it.
The easiest synthesis for perchlorates is thermal disproportionation of chlorate. Go look it up, it's in the german board too, under "Synthese von
Kaliumperchlorat".
[Edited on 10-3-2006 by garage chemist]
|
|
|
DeAdFX
Hazard to Others
Posts: 339
Registered: 1-7-2005
Location: Brothel
Member Is Offline
Mood: @%&$ing hardcore baby
|
|
Whats the tolerable amount of organic material when doing the chlorate --(heat)--> Perchlorate ?
Organic material being dust, hair and so on. Tolerable meaning the maximium amount before your kitchen stove is a smoldering crater.
[Edited on 11-3-2006 by DeAdFX]
|
|
|
MadHatter
International Hazard
Posts: 1332
Registered: 9-7-2004
Location: Maine
Member Is Offline
Mood: Enjoying retirement
|
|
(Per)chlorate
Ammonium chlorate is so unstable, that in the United States it is FORBIDDEN to be transported
by any means. I don't even want to be near it !
When decomposing chlorate to perchlorate, the amount of tolerable organic or any flammable/
combustible matter is ZERO. One member here already reported that a dumbass heated
KClO3 mixed with sucrose in a test tube. The mixture exploded !
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
|
|
|
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".
|
|
ammoniu8m perchlorate from perchloric acid
Source:The Perchlorate must be free from Chlorate.
A saturated solution of Sodium Perchlorate was poured into two and one half times its volume of pure HCl (density 1.20). After thorough agitation the
Sodium Chloride was allowed to settle, the the clear liquid was siphoned off, and the Sodium Chloride drained in a funnel by suction, and washed with
a little more acid. The solution containing HCl and Perchloric acid, with a little salt of Na was evaporate until dense white fumes of Perchloric acid
began to appear. The liquid was found to be completely free from HCl. At this point the concentration of the Perchloric acid is approx. the density of
the dihydrate, about 70%.
The acid above may contain small amounts of NaClO4 which may ppt out of solution. The acid can be distilled (use a Kieldahl bulb) if necessary.
It is not advisable to store Perchloric Acid, make and use as required.
Uses of Perchloric acid
Perchlorates are the salts of Perchloric acid. Most of the Perchlorates can be produced by Perchloric acid and the Chloride or Nitrate of the metal
and heating to drive off the HCl or HNO3 formed.
All of the Perchlorates can be formed by reacting the appropriate Hydroxide or Carbonate with the acid. This method of production is not used because
of the expense of Perchloric acid compared to Sodium Perchlorate, but it gives very pure Perchlorates.
[Edited on 12-3-2006 by Bert]
|
|
|
Lapis_infernalis
Harmless
Posts: 6
Registered: 10-3-2006
Member Is Offline
Mood: No Mood
|
|
OK
I`ll made my NH4ClO4 from a NaClO4 solution and NH3.
NaClO4 + NH4OH --> NH4ClO4 + NaOH
But than I need a water-unsoluble compound it can easy made from the sodium hydroxide solution and the ammonium perchlorate must not be changed.
Every sodium salt I know is water soluble. 
Sorry for my bad grammar
|
|
|
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
You might add HCl to make NH4Cl and use that solution while hot to precipitate NaCl. When hot, the NH4ClO4 should be more soluble, allowing you to
evaporate the solution and remove NaCl in the process. Then you can cool it and precipitate NH4ClO4.
Na2SO4 might also be an option, but I don't remember if it's less soluble than NH4ClO4.
Tim
|
|
|
MadHatter
International Hazard
Posts: 1332
Registered: 9-7-2004
Location: Maine
Member Is Offline
Mood: Enjoying retirement
|
|
NH4ClO4
After filtering you product, you should let it dry then dissolve in anhydrous acetone. NaOH is
insoluble in that. Filter or centrifuge - whatever is necessary to keep the NaoH out and then
evaporate. Fractional crystallization in H2O will work but keep in mind that NH4ClO4
decomposes above 66C.
[Edited on 2006/3/22 by MadHatter]
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
|
|
|
SAM4CH
Hazard to Others
Posts: 162
Registered: 16-7-2004
Location: TA
Member Is Offline
Mood: PERFECT
|
|
Is ammonium perchlorate decomposes in boiling water ">90C degree", I ment if I try to evaporate solution contains NH4ClO4 to get larg yeild is
there any problem!!!?
What about purification my ammonium perchlorate from any ammonium chlorate remains in last product if my sodium perchlorate solution was contains
small amount of chlorate!?
Sam
|
|
|
MadHatter
International Hazard
Posts: 1332
Registered: 9-7-2004
Location: Maine
Member Is Offline
Mood: Enjoying retirement
|
|
Chlorate
It's critical that any traces of sodium chlorate be destroyed before making NH4ClO4, otherwise
you invite an explosion. As for boiling down a water solution of NH4ClO4, I wouldn't know because
I've always used acetone.
You could boil down under vacuum if you can keep it below 66C.
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
