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Author: Subject: Ammonium Perchlorate manufacture
dann2
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[*] posted on 6-11-2007 at 15:00
Ammonium Perchlorate manufacture


Hello,

Two reads on AP industrial manufactute.
They are a bit old I suppose but good bedtime reading.




Dann2

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dann2
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[*] posted on 6-11-2007 at 15:01


and

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Xenoid
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[*] posted on 6-11-2007 at 20:09


Has anybody had any trouble opening these files?

I'm using a Mac with Version 12 Stuffit Expander and it stalls at fig 6.jpg in the first file and fig 24.jpg in the second file.

Regards, Xenoid
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[*] posted on 6-11-2007 at 23:01


Xenoid - make sure you add the .rar file type to the downloaded file. Worked for me...

Der Alte
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hashashan
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[*] posted on 7-11-2007 at 00:00


If anyone wants to use ammonium perchlorate from NaClO4 for pyrotechnic effects he might reconsider that.
You just can't get rid of the sodium that gets caught in the crystaline structure.
Thats why the only way to produce good quality AP is to make BA poerchlorate electrolyticaly and then convert it to AP
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[*] posted on 7-11-2007 at 08:55


Quote:
Originally posted by hashashan
Thats why the only way to produce good quality AP is to make BA poerchlorate electrolyticaly and then convert it to AP


Whats wrong with perchloric acid and ammonium hydroxide?
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[*] posted on 7-11-2007 at 13:16


That's OK as well, but not everyone has perchloric acid. This is a very expensive chemical, and in my opinion it would be highly uneconomical to make NH4ClO4 from HClO4.



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dann2
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[*] posted on 7-11-2007 at 14:48


Hello,
I have problems with both files and I posted them!
I deleted them first time as I realized they were corrupted. I reposted, they are still corrupted. They are OK on my end, somewhere between my pc, scimad.org and back (to a pc) there is a problem.

@DerAlt What do you mean by:
make sure you add the .rar file type to the downloaded file.

The files are viewable here too.

http://www.geocities.com/CapeCanaveral/Campus/5361/chlorate/...

http://www.geocities.com/CapeCanaveral/Campus/5361/chlorate/...

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[*] posted on 7-11-2007 at 14:50


Industry also uses perchloric acid for manufacture of ammonium perchlorate in addition to the older fractional crystallization methods from NaClO4 and an ammonium salt, or from other alkali perchlorates.
HClO4 is not as difficult to make industrially as one may think, it is made from NaClO4 solution and a large excess of strong HCl. NaCl is sparingly soluble in strong HCl and precipitates. The filtrate is distilled in vacuum and the HCl gas and azeotropic HCl recycled.
72% HClO4 then distills as the last fraction.
The process is not very practical in the lab since it is difficult to properly recover and concentrate the large amount of HCl gas and azeotrope.

On a lab scale, one could advantageously use a cation exchange resin to convert NaClO4 solution into HClO4 solution and neutralize this with NH3.
Cation exchange, if done correctly, is so thorough that it is used as an analytical method for determination of alkali metal ions, by exchanging them for H+ and titrating that.
You can certainly get pyrotechnic grade ammonium perchlorate from NaClO4 with this method- the yield will be nearly quantitative as well.
The disadvantage is that you can only make rather dilute solutions of mineral acids with ion exchangers. Also, again you need lots of excess HCl for regeneration of the exchanger, but only in dilute form, and you could distill the excess aqueous HCl from the effluent from exchanger regeneration if economic usage of HCl is a concern to you.

Preparative use of a cation exchanger for the preparation of different acids from their alkali metal salts is one of the ideas I have had in my mind for some time, and I have acquired 1kg of Wofatit KPS from ebay.
Brauer uses the ion exchange method to make perbromic acid from perbromate, and also mentions it as a method to obtain solutions of chloric acid from sodium chlorate. A journal reference was given for the latter procedure, which I acquired.
It doesnt actually give a procedure for chloric acid, but contains the general procedure for the preparations of acids with an ion exchanger, and details on how to prepare the exchanger bed, how much sodium a given weight of exchanger can exchange, regeneration procedure etc...
The only problem is that it uses a different exchanger resin (Wofatit KS) than I have, creating the need of obtaining information about the Wofatites (very old product line, one of the first organic resin ion exchangers commercially manufactured).

Preparative ion exchange offers some interesting possibilities, like converting KClO3 back into pure NaClO3 with practically 100% yield and preparing aqueous solutions of numerous inorganic and organic acids from their alkali metal salts.




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[*] posted on 7-11-2007 at 15:51
ammonium perchlorate purification


NaClO4 + NH4Cl ==>> NH4Cl04 + NaCl

If your looking for pure ammonium perchlorate from the above reaction then ion exchange as stated by garage chemist is the best method.

However, purification can achieved by the use of solvents to a lesser degree of purity with methanol and acetone.

http://www.sciencelab.com/xMSDS-Ammonium_perchlorate-9922929

Solubility:
Soluble in cold water, methanol.
Partially soluble in acetone.
Insoluble in diethyl ether.

Sodium chloride, NaCl is very slightly soluble in dry methanol and not soluble in acetone.

[Edited on 8-11-2007 by WizardX]




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[*] posted on 7-11-2007 at 23:31


As far as i know its hard to get rid of Na because Na perchlorate is close in sizes to AP. Thats why i thought that Ba perchlorate would be supperior because its molecule is much much larger
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[*] posted on 8-11-2007 at 01:38
Lithium perchlorate


I wish I can remember the patent number but there is a patent that talks about using lithium chloride and electrolyzing this until you get lithium perchlorate. This is turn is reacted with ammonium carbonate to precipitate lithium carbonate.



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[*] posted on 8-11-2007 at 03:02


that is a good idea, I thought about it ... even if ill have Lithium ions they won't do any harm. However Lithium here is 4 times more expensive then Barium.... so ......
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chloric1
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[*] posted on 8-11-2007 at 14:42


DAMN IT! :mad: So where are you and why is lithium so high? I mean it is rarer and supposed to be more expensive than barium but not THAT much.



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[*] posted on 8-11-2007 at 23:57


Im in Israel. Were not rich in minerals.
Besides If ill go to a chem shop itll be about 8 times more expensive.
However barium is quite cheap here ... 4$ for 2 pounds of barium carbonate
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[*] posted on 9-11-2007 at 11:22


Lithium simply isnt cheap, even in bulk amounts. The extraction from natural sources is expensive due to the low concentration in all natural sources, and only economic because byproducts can be marketed as well.
Anything below 20$ for 1kg lithium carbonate is a good price, I think. The cheapest technical grade Li2CO3 from a pottery supplier I found was EUR 10,35/kg.


[Edited on 9-11-2007 by garage chemist]




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[*] posted on 9-11-2007 at 15:10


garage chemist-Well here in the USA I can get lithium carbonate from a pottery supplier for $7.50 per pound or $35 for 5 pounds. When you exchange the dollar for the Euro and convert metric to American Standard, it comes out to be very close to your cost over there. No advantage over here. I would set up something with hashashen but he is better ordering from Europe or Isreal if the pottery grade is available there.



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[*] posted on 9-11-2007 at 19:49
Lithium Perchlorate patent


Hello,
Chloric1 mentioned a patent for Li Perchlrorate. Attached below.
The price of Lithium is not so important (if you are making Ammonium Perchlorate) as you will recycle Li. (reduce, reuse, recylce you know, or is that plastic :D)

Anyhow I read somewhere that Lithium salt could be converted very easily into Perchlorate becasue of the very small size of the Li ion. Cannot remember where I read this but it does not seem to make sense to me as the Li is a spectator ion. Perhaps the larger ions (Na, K) physically get in the way more of (Per)Chlorate formation at an anode surface?


Wonder would Li Perchlorate form easily at a Graphite surface?


Dann2

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[*] posted on 10-11-2007 at 07:46


If you're after NH4ClO4 for rocketry you might as well settle for LiClO4 if you're making it anyway. Hell of an oxidizer and very high oxygen content.



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[*] posted on 10-11-2007 at 09:07


LiClO4 is also soluble in organic solvents like diethyl ether and THF and the solutions are conductive. It is the best salt you can use if you want to explore lithium metal production by electrolysis in nonaqueous solvents.



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[*] posted on 28-1-2008 at 13:27


Ok guys ... suppose I got a NaClO4 + NaCl + Na2SO4 solution .... how can I get AP from it.
Adding NH4NO3 resulted nothing.
Anyone care to share his experience please

and garage chemist .... what will happen to the ClO4 ? where will it go?
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[*] posted on 28-1-2008 at 14:20


Quote:
Originally posted by hashashan
Ok guys ... suppose I got a NaClO4 + NaCl + Na2SO4 solution .... how can I get AP from it.
Adding NH4NO3 resulted nothing.
Anyone care to share his experience please

and garage chemist .... what will happen to the ClO4 ? where will it go?


WTF? Am I missing something here? the ClO4 will go with your ammonium ion. You see ammonium perchlorate is still soluble in 0°C water to the extent of 11% IIRC. That may seem hard to isolate but keep in mind ammonium perchlorate is MUCH more soluble in boiling water. You would be wise to mix equamolar amounts of ammonium salt with your sodium perchlorate and boil down until the solution is a bit hazy. If you used ammonium nitrate then you have no worries as, on cooling, ammonium perchorate will deposit before any sodium nitrate. If,however, you use ammonium chloride remember sodium chloride is only moderately soluble in boiling water so you will have to filter through a heated funnel then cool. In both cases you need to dissolve your crude ammonium perchlorate in a minumum of boiling distilled water at least once if not more to get a respectable pure product.




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[*] posted on 28-1-2008 at 14:58


@chloric : the ClO4 was refered to garage chemist with the Li production.

now about what you said ... the sodium sulfate and chloride wont interfere? I am worried about the sulfate .. it is as soluble as the AP
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[*] posted on 28-1-2008 at 15:44


yeh sorry about that. I forgot to mention your sulfate. It seems you have a real mess:(:(. Your sulfate will deposit right along with your AP. The only answer is to deposit everything you can by cooling and add VERY warm (50°C) acetone,after decanting, to dissolve out the AP and hope for the best. It may take MANY treatments. Methanol should work to.

[Edited on 1/28/2008 by chloric1]

[Edited on 1/28/2008 by chloric1]




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[*] posted on 28-1-2008 at 15:51


Damn this AP ... I already precipitated the ClO4 as the K salt.
Anyway ... Suppose I make my perch from NaCl .. and then I destroy the remaining chlorate with Sulfite.. So there is no possible way to precipitate the Ammonium salt in a normal way?
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