Fantasma4500
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NH4ClO4 and other ClO3 easy
i somewhat randomly found a way to make Ba(ClO3)2 ..
the procedure was following
ammonium tartrate and potassium chlorate is mixed, this produces nearly insoluble potassium tartrate and ammonium chlorate
ammonium chlorate will upon mixing with other carbonates produce ammonium carbonate and fx. Ba(ClO3)2 if BaCO3 is
used..
ammonium tartrate is made by NH4OH in exess added to tartaric acid
but now the more interesting idea of this...
NH4ClO4.
ofcourse you could just use KClO4 instead of KClO3, and then mix it with ammonium tartrate, and then very controlled evaporate
off the water, only slight impurity by potassium tartrate..
NH4ClO3 is a bad idea to try and isolate / dry as it tends to have properties that are very hard to tame, if its possible at
all.. but there shouldnt be anything bad about boiling NH4ClO3, tho i would go with less than 100*C just in case..
i havent tried this yet myself, tho.
but imagine that you can use this for practically any chlorate you might want to make!
Cu(ClO3)2 for TACC perhaps?
im planning to try and make lithium chlorate
i found this synthesis so to say here..
http://www.amateurpyro.com/forums/topic/4608-non-electrolyti...
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virgilius1979
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If you want Cu(ClO3)2 it's better to react NaClO3 and CuSO4 in methanol, which precipitates the Na2(SO4) and leaves the Cu(ClO3)2 in solution; you may
than bubble NH3 to get TACC.
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AndersHoveland
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Quote: Originally posted by Antiswat  | i somewhat randomly found a way to make Ba(ClO3)2 ..
the procedure was following
ammonium tartrate and potassium chlorate is mixed, this produces nearly insoluble potassium tartrate and ammonium chlorate |
Ammonium chlorate has a low solubility itself. (most ammonium salts tend to be very soluble, but ammonium chlorate and perchlorate have anomalously
low solubilities) This is likely to interfere with the separation, since some ammonium chlorate will likely precipitate out with the potassium
tartrate.
Indeed, it is fairly easy to precipitate out ammonium chlorate from a mixture of sodium chlorate and ammonium chloride.
One note of warning for those who may not be aware: NH4ClO3 has a much lower stability than NH4ClO4. Ammonium perchlorate is perfectly safe here, but
there may be some explosion hazard from the NH4ClO3. Because of safety, it is often recommended not to mix ammonium compounds with solutions
of chlorates, but it can be a very useful route to make metal chlorates. I would just suggest using some caution, and to redisolve the ammonium
chlorate precipitate (after separatation) back into another solution of water as soon as possible. Either use the solution quickly, or keep it out of
sunlight.
While many chemistry books recommend keeping certain light-sensitive reactions away from sunlight, what they often fail to mention is that exposed
fluorescent tubes not covered by acrylic diffusor panels are just as bad (I mention this because more and more people are using those awful spiral CFL
bulbs that leak out ungodly ammounts of UV radiation)
[Edited on 10-3-2013 by AndersHoveland]
I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
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woelen
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Anders, you're not right about the low solubility of the ammonium chlorate and perchlorate salts. I remember some time ago also that you wrote a post
about the very low solubility of NH4ClO4. This compound actually dissolves in water very well, but it is hardly hygroscopic. This makes it an ideal
compound for purification and isolation. NH4ClO3 also is quite soluble, I tested this with NaClO3 and NH4Cl.
@Antiswat: Using KClO4 as a starting point for making other perchlorates hardly is possible. Solubility of KClO4 is very low, when compared with
KClO3. KClO4 is hardly useful in aqueous chemistry, due to its low solubility in water at room temperature.
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Fantasma4500
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| Quote: Originally posted by virgilius1979 | | If you want Cu(ClO3)2 it's better to react NaClO3 and CuSO4 in methanol, which precipitates the Na2(SO4) and leaves the Cu(ClO3)2 in solution; you may
than bubble NH3 to get TACC. |
true.. but for this KClO3 doesnt work, and NaClO3 isnt really that common as KClO3..
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Fantasma4500
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| Quote: Originally posted by AndersHoveland | | Quote: Originally posted by Antiswat | i somewhat randomly found a way to make Ba(ClO3)2 ..
the procedure was following
ammonium tartrate and potassium chlorate is mixed, this produces nearly insoluble potassium tartrate and ammonium chlorate |
Ammonium chlorate has a low solubility itself. (most ammonium salts tend to be very soluble, but ammonium chlorate and perchlorate have anomalously
low solubilities) This is likely to interfere with the separation, since some ammonium chlorate will likely precipitate out with the potassium
tartrate.
Indeed, it is fairly easy to precipitate out ammonium chlorate from a mixture of sodium chlorate and ammonium chloride.
One note of warning for those who may not be aware: NH4ClO3 has a much lower stability than NH4ClO4. Ammonium perchlorate is perfectly safe here, but
there may be some explosion hazard from the NH4ClO3. Because of safety, it is often recommended not to mix ammonium compounds with solutions
of chlorates, but it can be a very useful route to make metal chlorates. I would just suggest using some caution, and to redisolve the ammonium
chlorate precipitate (after separatation) back into another solution of water as soon as possible. Either use the solution quickly, or keep it out of
sunlight.
While many chemistry books recommend keeping certain light-sensitive reactions away from sunlight, what they often fail to mention is that exposed
fluorescent tubes not covered by acrylic diffusor panels are just as bad (I mention this because more and more people are using those awful spiral CFL
bulbs that leak out ungodly ammounts of UV radiation)
[Edited on 10-3-2013 by AndersHoveland] |
i checked up on it, and to my relief, while potassium tartrate's solubility is about 2g/100 mL (KClO3 alike) NH4ClO3's solubility is about 30g / 100
mL at about 20-30*C
NH4ClO4 is about 10g/100 mL
its acceptable i'd say.. with some careful recrystallization it should work very well, tho..
but yes.. dont isolate the NH4ClO3 (!!!)
or well if, then do it under very controlled conditions, very sturdy drying surfaces etc.
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Fantasma4500
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| Quote: Originally posted by woelen | Anders, you're not right about the low solubility of the ammonium chlorate and perchlorate salts. I remember some time ago also that you wrote a post
about the very low solubility of NH4ClO4. This compound actually dissolves in water very well, but it is hardly hygroscopic. This makes it an ideal
compound for purification and isolation. NH4ClO3 also is quite soluble, I tested this with NaClO3 and NH4Cl.
@Antiswat: Using KClO4 as a starting point for making other perchlorates hardly is possible. Solubility of KClO4 is very low, when compared with
KClO3. KClO4 is hardly useful in aqueous chemistry, due to its low solubility in water at room temperature. |
yes, thats one thing that should be considered that it doesnt dissolve straight away.. not sure but i think they used potassium chlorate/perchlorate
in the link i added to the thread.. anyways KClO4's solubility is nearly the same as KNO3's at 20*C, tho you need to add 80*C extra when using KClO4
but they said to use boiling water..
otherwise just heating it up and letting little by little react should work aswell.. its been done with insoluble oxides/carbonates with non-acids
before and ive tried it a few times tho i cant recall anything specific..
anyhow its possible and should give a decent result.. surprised that theres nothing yet that makes this too easy making of NH4ClO4 impossible.. just
seem too easy to make this way??
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