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Madog
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smile.gif posted on 27-5-2002 at 16:16
TACC


okay, i was reading about TACC the other day, i used to be very intertested in this but i just never got to make any because i got no CuSO4

i thought of my own method of preperation. it says that TACC is made by bubbleing amonia through a solution of Cu(ClO3)2

well, i figured maybe u could make it like this

Cu + 2HCl --> CuCl2 + H2

CuCl2 + H2O + (electricity) --> Cu(2+) + 2Cl(5+) + H2 + 2O(2-)

Cl(5+) + 3O(2-) --> ClO3(1-)

Cu(2+) + 2ClO3(1-) --> Cu(ClO3)2

Cu(ClO3)2 + 4NH3 --> Cu(NH3)4(ClO3)2

so, do u think this will work? i probaly have the last 3 reactions messed up but i know that if u electrolisize a XCl in a solution of water with the anode and cathode placed correctly (so the Cl bubbles over one, i forget the details) it will make XClO3

look in KIPE1 to see a thing on this being done with KCl

oh, and another thought. what about boiling CuCl2 with bleech or HTH?

edit: i fixed the crapy reactions

[Edited on 5/31/02 by Madog]




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kingspaz
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[*] posted on 23-7-2002 at 06:26


that seems like a good idea although i'm not sure how easily HCl would attack the copper. it may take a while to react all the copper and also some heating. maybe a better idea would be to use CuO powder from a pottery supply place:
CuO + 2HCl ---> CuCl2 + H2O
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PHILOU Zrealone
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[*] posted on 8-9-2002 at 12:29


Cu is related to noble metals in many regards and is corroded significantly only by strong oxydising acids.
So actually it is easier to get CuCl2 from Cu wire heated and dropped in Cl2 jar.But if you are patient, some should occure from HCl + Cu if in contact with O2...to add some H2O2 or HNO3 or H2SO4 will speed up the reaction significantly.
Grinding Cu to get Cu powder and heat it in a flow of O2 will give you CuO (black) that dissolves quite fast in conc HCl.

Unfortunately for you CuCl2 electrolysis only result in Cl2 evolution and Cu plating!

The Chloride to chlorate and perchlorate process is only true for alkaline and alkalinoheart metals like Li, Na, K, Mg, Ca, Sr, Ba that have metals that can't be isolated in water since they decompose it as soon as they are formed!
NaCl -aqua/eletrolysis-> Na + 1/2Cl2
Na + H2O --> NaOH + 1/2H2
Cl2 + H2O --> HOCl + HCl
HCl + NaOH --> NaCl + H2O
NaOH + HOCl --> NaOCl

NaOCl + NaOCl --heat --> NaOClO + NaCl
NaOClO + NaOCl --heat --> NaOClO2 + NaCl
NaOClO2 + NaOCl --heat--> NaOClO3 + NaCl
2NaOClO + NaOClO --heat--> 2NaOClO2 + NaCl
NaOClO + NaOClO --heat--> NaOClO3 + NaCl
2NaOClO2 + NaOClO --heat--> 2NaOClO3 + NaCl
3NaOClO2 + NaOClO2 --heat--> 3NaOClO3 + NaCl

To get Cu(ClO3)2 you should dissolve Cu(OH)2 or CuCO3 or CuO in a solution of HClO3 (HOClO2) made from Ba(ClO3)2 solution in distillated water and reacted with H2SO4.
HClO3 solution is strongly acidic and decompose over 35% so don't make it too concentrated (since the toxic and spontaneously explosive gas ClO2 will evolve: this gas is responsible of the explosion and fire when H2SO4 is dropped on KClO3/suggar mix and of the unstability of Chlorates towards sulfur and phosphor that contains traces of H2SO4 or H3PO4!).

If I were you, I would go for TACuP instead of TACuC.
Cu(NH3)4(ClO4)2 should be more stable, more powerfull about as sensitive as Cu(NH3)4(ClO3)2.

Ba(ClO4)2 + CuSO4 --> BaSO4(s) + Cu(ClO4)2
Cu(ClO4)2 + 4NH3 --> Cu(NH3)4(ClO4)2

Enjoy!

PH Z
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Madog
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[*] posted on 8-9-2002 at 18:22


thanks!! i would like to synthisise some HClO4 and make various perchlorates includeing Cu(ClO4)2 and then TACuP. these compounds interest me

i wonder if there are any organic perchlorates that are sane to make. hmm, perhaps cellulose perchlorate or maybe hexamine perchlorate, that is something i have been thinking about for a while, seems like it would hurt me though.




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PHILOU Zrealone
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[*] posted on 10-9-2002 at 13:56


Cellulose perchlorate would be an ester of perchloric acid and is prone to detonate spontaneously upon standing...it is only something to play with in tiny amounts and to enjoy immediately; never store.
To see the power of HClO4; you put a drop of it on a sheet of toilet paper...paper will melt and make a kind of glue so rool it over itself and drop that in a fire outside...enjoy the lightnings and sharp cracks from a safe distance...this will show you the real power of perchloric esters and their potential hazard if they runnaway spontaneously in your lab/house!

Salts of amines and perchlorates are all safe until heated or in contact with a flame; moderately sensitive to shock but stil sensitive; very sensitive if transition complexating metals are involved --> primaries most of the cases or sometimes spontaneous ignition/explosion.

It is always a good idea to keep batches smaller than 10g and to dry them 1g at the time.I once had 500mg hydrazine perchlorate detonation in my kitchen on a hot plate (the stuff burn normally upon contact with a flame but shock on a hot plate...damn, my spoon was twisted arround my hand and flew spinning fast at 3 meters high,it had a notch on the side and my ears remember the noise).

Also while making use diluted acid and amines because neutralisation generates quite a lot of heat...if too concentrated heat can be excessive and opperate on nearly anhydrous amine perchlorate.Reaction of 20% concentration reactants is already quite hot!

PH Z
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[*] posted on 20-11-2002 at 08:21
TACC


Is this simple reaction a good idea to keep TACC
without destroing it, possibly in presence of a
suitable catalyst wich can beside separating the NaCl
from the mixture ?


[ 0,25 CuSO4 + 0,5 NaClO3 ] + [ NH4Cl + NaOH ] -->
[ 0,25 [Cu(NH3)4](ClO3)2 + 0,25 Na2SO4 ] + [ NaCl + H2O ]
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[*] posted on 10-12-2002 at 17:43


don't use H<sub>2</sub>O<sub>2</sub> in TACC batch Cu<sup>++</sup> reacts with H<sub>2</sub>O<sub>2</sub> to form Cu<sub>2</sub>O<sub>3</sub> and CuO<sub>2</sub>(out of topic this compound seems interesting as an oxidizer;))

[Edited on 16-3-2003 by KABOOOM(pyrojustforfun)]
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[*] posted on 11-12-2002 at 13:27
TACN


Does anyone here know anything about TACN? This seems to be easier to make then TACC due to a main precursor being a nitrate instead of sodium chlorate. I have been trying to find some good info TACN but its been hard, there even less info on this primary then TACC.
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[*] posted on 11-12-2002 at 22:32


There has been some discussion of TACN on the E&W Forum. All results seemed to indicate that it was very difficult to prepare, because it was extremely hygroscopic, and it needed to be anhydrous to exhibit much in the way of explosive properties.
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Marvin
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[*] posted on 17-12-2002 at 04:11


Same is true of TACC, it gets wet, its a write off, decomposes if you try to dry it, and loses ammonia anyway.
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[*] posted on 27-12-2002 at 19:53
formation of NH4ClO3?


After thinking about the standard procedure of synthesizing TACC, it has occurred to me that there is a possibility of producing NH4ClO3 while bubbling ammonia through the solution. Assuming that the chlorate does not completely react with copper compound, there will still be some residual chlorate ion left in the solution. My question relates more to ammonium chlorate than the actual TACC because i am curious as to how hazardous this compound would be if it indeed occurred in trace quantities. Also i have read little information about NH4ClO3 as far as its properties go, other than it being dangerously sensetive.

It seems that the risk may be lessened somewhat by letting the solution return to room temperature after refluxing and before filtering, so that extra unreacted chlorate would be filtered out as it precipitates from the solution.

Anyone have any ideas as to exactly how hazardous the ammonia addition is to the copper chlorate solution in light of these concerns, or am i just being paranoid?
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Madog
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[*] posted on 28-12-2002 at 14:36


its insanely unstable. it is said that it will oxidise things in a similar fasion to Mn2O7. its *really* sensitive. if you are up to it and want to learn more about it perhaps you could make a solution of it, put it on some paper, and let it evaporate and see if the paper cauches on fire. im not sure if you can really isolate it. and if you could you would want to do it in really small quantities



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[*] posted on 28-12-2002 at 16:09


blazter, the remaining chlorate ions in the solution will be balanced by the remaining copper ions in solution thus a solution of copper chlorate. you can't have a solution with slightly more negative ions. to som extent NH4ClO3 probably does form but i'd say the instant it does it would likely revert back to the ions from which it was made.



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[*] posted on 29-12-2002 at 09:08


consider also that NH3 binds to Cu2+ in a complex ion, a very strong one to, meaning there is little free NH4+ in solution to form NH4ClO3.

One example. I was trying to dissolve
CuO in (NH4)2SO4 by boiling.

CuO(s) + (NH4)2SO4 => [Cu(NH3)2]2+ + H2O + [SO4]2-

Immediately a violett-blue complex formed, and after several hours of boiling all CuO had dissolved (I used 2 times excess (NH4)2SO4) but I could only smell the faintest of free ammonia.

/rickard
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chemoleo
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[*] posted on 26-7-2003 at 23:00
Copper tetraamine nitrate


hmm, I hope I am not totally mistaken but I seem to remember an experiment I did a long time ago - adding ammonia solution to a copper nitrate solution. I remember a colour change (so something HAS to happen), and isolating it by cyrstallising it/ evaporation.
The resulting crystal powder, as far as i remember, did sort of burn, leaving a brown residue (copper chloride/oxide?), but nothing like a fast burn or potential explosion if hammered hard... never pursued this tho. Any thoughts?
(oh, its coming back - I made this to create a blue flame, and it seemed to work to some extent if in a mixture with KClO3+sugar)
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[*] posted on 29-7-2003 at 09:12


is it going to work if i put some ammonia water instead of bubbleing ammonium ? im interested in TACC becose i have all the things i need. if somebody knows some good links where i can find info about TACC , post !!! i was already by magalomania .... ;)
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[*] posted on 29-7-2003 at 09:45


Ammonia solution will work in theory, but you'll have to carefully dry the product after making it. It is very water-soluble and won't work if it's damp.
It is better, though more complicated, to use alcoholic solutions, not aqueous. Form the copper salt by mixing alcoholic solutions of copper sulphate and the corresponding sodium salt (chlorate, nitrate, whatever). Sodium sulphate is insoluble in alcohol, so it pptes, leaving your copper salt in solution in the alcohol. The preferably bubble in dry ammonia, or add the strongest ammonia solution you can find, and evapourate to begin crystalisation. Filter the crystals out and dry them.
There are aminometal oxosalt complexes which work well, but I have never had a lot of luck with ammonia. I have used guanidine, nitroguanidine, and aminotetrazole and all of these form very promising substances with copper or nickel nitrate. The only problems I have with these are a very limited supply of guanidine/nitroguanidine, and aminotetrazole isn't very soluble in alcohol or water.
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[*] posted on 31-8-2003 at 04:21


rikkitikkitavi I think this reaction happend:
CuO(s) + 2(NH<sub>4</sub>;)<sub>2</sub>SO<sub>4</sub> => [Cu(NH<sub>3</sub>;)<sub>4</sub>]<sup>2-</sup> + H<sub>2</sub>O + 2[HSO<sub>4</sub>]<sup>-</sup> u boiled the solution causing some of the ammonia liberate. I think ammoniated copper salts don't just absorbs water becoming wet but form hydrate salts. for example when dissolving CuSO<sub>4</sub> in NH<sub>4</sub>OH then adding alcohol<br> Cu[NH<sub>3</sub>]<sub>4</sub>(SO<sub>4</sub>;)<sub>2</sub><b>.H<sub>2</sub>O</b> is precipitated.
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[*] posted on 22-3-2008 at 14:43


For every page I see about TACC, it says that it is decomposed by water. That means that you have to make it in an anhydrous solution. Every synthesis says to use either absolute methanol or ethanol. Do you think that you could use acetone or methyl ethyl ketone instead? And they say to use sodium chlorate, but do you think that you could use potassium chlorate?

I have made copper sulfate and I can get potassium chlorate. I made the copper sulfate by electrolysis of magnesium sulfate with copper pipe as electrodes, and filtering. I know I can get potassium chlorate from armstrong's mixture. I just want to make sure the synth will work before I use up some of my limited acetone or MEK.




So... what did you do over the weekend?
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[*] posted on 22-3-2008 at 14:46


Quote:
Originally posted by Zelot
I made the copper sulfate by electrolysis of magnesium sulfate with copper pipe as electrodes, and filtering. .


You do not have copper sulfate. Your precipitate is copper hydroxide. You will need to dissolve this in sulfuric acid and then crystallize to get copper sulfate.




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[*] posted on 22-3-2008 at 21:57


Are you sure that it won't make copper sulfate? Then where does the SO4 ion go? The magnesium from the MgSO4 changed into MgO, and lots of blue crystals were formed. I guess it could be CuOH, but I'm not sure.

BTW, if I had sulfuric acid, I wouldn't bother with TACC.




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[*] posted on 22-3-2008 at 23:44


cathode
H2O+2e- -->2H2 +2OH-
anode
Cu-->Cu2+ +2e-

Cu2+ +2OH- --> Cu(OH)2
also Mg2+ +2OH- -->Mg(OH)2
The electrolysis will initially produce Mg(OH)2 and the copper ions will stay in solution, but as the electrolysis continues, or if the solution is stirred, the copper ions will reach the cathode side of the cell and precipitate out as the hydroxide. You would need a divided cell to isolate pure CuSO4

However, if Mg2+ has a much higher mobility(which I don't particularly want to calculate now) than Cu2+ it will be attracted to the cathode faster, but that would still leave your copper(II) in solution, you would have to evaporate to isolate it, you would not obtain it by filtering unless your solution was quite concentrated

Tell me more about how the experiment was done, you may have done it differently than I am envisioning, leading you to somehow isolate CuSO4.




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[*] posted on 23-3-2008 at 08:31


Well, I got a glass jar, and dissolved as much epsom salts as I could into it. Then I cut two sections of copper pipe and connected those to the 1 amp charger. I submersed the pipes, and bubbles of hydrogen and oxygen came out. I left it to do its thing and left for school. When I got back, the anode was completely dissolved, there were crystals growing on the cathode, and a layer of crystals on the bottom of the jar. I put the stuff through a couple of coffee filters, and dried the crystals in the oven.

The anode and cathode were not that far apart. Maybe an inch or two. There was also a white powder growing on the cathode, which I assumed to be Mg(OH)2.




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[*] posted on 23-3-2008 at 12:49


Ok, the concentration issue is what did it. Your concentrated MgSO4 electrolyte means that the copper sulfate would crystallize out as it is formed. I assumed dilute electrolyte. It may still have Mg(OH)2 contamination, so you could dissolve your copper sulfate crystals in water, filter out the insolubles and then crystallize the filtrate and that should clean it up a bit.



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[*] posted on 24-3-2008 at 03:43


"For every page I see about TACC, it says that it is decomposed by water. That means that you have to make it in an anhydrous solution"

No it can be made in aequous solution. Just make a conc. solution of copper chlorate (can be made from Ba(ClO3)2+CuSO4) and pass in ammonia until saturated. Cool down in the fridge. Plenty of blue crystals will form upon cooling.

It is useless stuff tough and possibly dangerous to store. It decomposes even in a sealed glass jar. Make the perchlorate complex - it keeps well for years and isn't moisture sensitive. Or go for the nickel chlorate, it keeps perfectly well too and due to its very low solubilty it precipates even from dilute solution.

Btw. the corresponding zinc ammine is useless as well (hygroscopic and decomposes within weeks).
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