Making ammonium persulfate

[The_Rsert]

Hello,
Has somebody information about ammonium persulfate?
I have some sodium perulfate, ammoniumnitrate, NH4OH and ammonium chloride.
Is possible to synth. it with the chemicals?

I need some ammonium persulfate, because I want to make some copper persulfate(neutralising ammonium persulfate with copper carbonate) to synth. tetraamincopper(2)persulfate.

[Mumble]

Well, ammonium persulfate is a common etchant of circut boards. It is used as an alternitive to FeCl3 and Sodium Persulfate. I've heard of people making it from the interation of solutions of an alkali persulfate and Ammonium Chloride. I never heard the results of the proceedure though. I imagine that you could possibly crystalize the persulfate out with low temps as NaCl doesn't change in solubility much. Ammonium Persulfate decomposes in water so you may want to wash with alcohol or acetone.

The other way to do it is electrolysis of ammonium sulfate in dilute sulfuric acid. That is all the detail I have about that method.

[hereno]

According to here http://www.sciencemadness.org/talk/viewthread.php?tid=1778&page=1

Cupric persulphate has not been isolated, but its tetramino- and tetrapyridine derivatives, [Cu,4 base]S2O8, have been prepared (Barbieri and Calzolari, Z. anorg. Chem., 1911, 71, 347).


Thus, you can't make CuS2O8 by precipitating from ammonium persulfate, only seems isolatable as its complex. Theres no need at all to convert the Na2S2O8 to the ammonium salt anyway! Use it as is, Na2S2O8 solubility = 55g/100ml @ 20°C.

[Mendeleev]

But maybe they made some progress since 1911.

[nbk2000]

I'd hope chemical science has advanced at least just a little in the last century! :p

[hereno]

Im quite sure that in 1911 they knew how to precipitate salts from solution :rolleyes: If it were as simple as mixing ammonium persulfate with copper carbonate (<-Is THAT even isolatable!) it would be well known. Anyway the point is that there is no need to isolate it anyway, if your aiming for the complex.

[FUTI]

I thought that CuCO3 isn't isolable when I was student...and guess what, I was wrong. It can be made;) It's on you to find how hereno.

EDIT: BTW I had an impresion that heavy metal salts as Ag, Fe and others can promote decomposition of persulfate in solution, so I wouldn't use Cu salt with ammonium-persulfate anyway! Think about it and tell us if you find something interesting, I never research subject to deep.

[Mumble]

Generally it exists as a complex with copper hydroxide, also known as basic copper carbonate. I've heard something about heating CuO in a CO2 atmosphere, but it reverts to the hydroxide complex on contact with moisture.

What I really don't understand is why use Copper Carbonate(I assume you have the basic complex). Did you plan to boil the mixture and have the ammonium carbonate decompose and leave the system? The persulfate would without any question decompose under these conditions. If you just were making a solution, the insolubility of the copper carbonate would severely push the equilibrium to the left. Your best method would be to heat or reflux the sodium persulfate and anhydrous copper sulfate under methanol, filter off the sodium sulfate and anything remaining and bubble dry ammonia into the methanol. The crystals will precipitate. This is the best way I know to prepare the tetraamine copper (II) complexes anhydrously. You don't have to deal with them becoming wet and about as useful as an explosive as table salt. This would be the best of any chance of preparing the compound you are hoping to acheive.

[hereno]

Question, Is the problem with aqueous solutions that the water forms a ligand with the complex replacing NH3, or is it because its a hydrated salt?

According to the link above, the formation of the complex you want can be done in aqueous solutions. Why dont you just try mixing stoichiometric proportions of NaS2O8/CuSO4.5H2O/NH4OH and try to precipitate it, no point getting complicated if it isn't warranted!

[The_Rsert]

OK, i have just testet making Tetraamincopper(2)persulphate!
It works very well! Thanks!

Picture of yield of 5g copper sulphate:
http://members.fortunecity.de/potatoguns/TACPersulfat.jpg
The crystalls were very wet an some ice was in the filter, too.
The "washing-water"(I don't know the right English word for this) was beautyful coloured :)
http://members.fortunecity.de/potatoguns/WaschwasserTACPersulfat.jpg

[metal dragon]

Off topic but here is a movie of the tetra amine copper persulphate burning.
The soultion that the crystals are filtered from is a very nice purple.


http://www.infernolabs.co.uk/filehost/teraaminecopperpersulphate.AVI

[The_Rsert]

Picture of yield of 5g copper sulphate:
http://members.fortunecity.de/potatoguns/TACPersulfat.jpg
The crystalls were very wet an some ice was in the filter, too.
The "washing-water"(I don't know the right English word for this) was beautyful coloured :)
http://members.fortunecity.de/potatoguns/WaschwasserTACPersulfat.jpg

The links are now deleted.
The new link is:
http://members.fortunecity.de/potatoguns/TACPersulfat.html