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Author: Subject: Precipitation of TACN (tetraamine copper nitrate)
Triflic Acid
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[*] posted on 9-6-2021 at 17:43
Precipitation of TACN (tetraamine copper nitrate)


Made a solution of this explosive earlier today. I currently have it in solution, but am not sure how to get it out. I don't have much isopropanol left, (and trying to conserve it) like the usual preps call for, but I have loads of ethanol-methanol fuel alcohol. Could I precipitate the TACN using this fuel alcohol instead? I really don't want to use up my iPOH.



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XeonTheMGPony
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[*] posted on 9-6-2021 at 19:47


I boil it down, then gas with ammonia then salt out or evaporate the remaining water
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Triflic Acid
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[*] posted on 9-6-2021 at 20:03


Won't plain boiling destroy the ammonia ligands? And I really don't like the thought of evaporating something under a stream of ammonia.

[Edited on 10-6-2021 by Triflic Acid]




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MineMan
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[*] posted on 9-6-2021 at 20:31


It should reform when the ammonia is added.
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[*] posted on 10-6-2021 at 04:53


Ok, so basically make copper nitrate solution, then boil down and last gas w/ ammonia?



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[*] posted on 10-6-2021 at 06:22


Actually, I'd really prefer to be able to use alcohol to get it out of solution. At this point, given the lack of info about ethanol being used to precipitate, I think I'm going to give up and use iPOH.



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[*] posted on 10-6-2021 at 07:33


[Cu(NH3)4]SO4 is often precipitated out using EtOH or MeOH. I think that this will work for nitrate also.



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[*] posted on 10-6-2021 at 08:54


Ok, I'll test that on a small scale this afternoon. More results coming shortly.



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[*] posted on 10-6-2021 at 15:55


Quote: Originally posted by Triflic Acid  
Ok, so basically make copper nitrate solution, then boil down and last gas w/ ammonia?[/rquote

That's the ticket! Make it a super concentrate and most will crash out, the rest gets salted out easily.
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[*] posted on 12-6-2021 at 12:49


Cool the aqueous solution to -10 ° C for 8 hours. If the concentration of NH4OH in the solution is about 20-25%, the yield is 95% or more. The next operation is only the filtration of TACN crystals. Do not use paper. The solution dissolves everything organic. It's a Schweizer reagent. If the concentration of NH4OH in the solution is low, for example 10%, bubble the cold solution with ammonia gas. The more concentrated NH4OH, (and the colder) the higher the yield.



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[*] posted on 12-6-2021 at 14:13


In the end, I found a really old bottle of iPOH, and just used that. So, no test of ethanol. Also, cooling to just 5C in an ice bath for 1 and a half hours worked to give me a good amount.



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[*] posted on 17-6-2021 at 23:58


I said that. No ethanol is needed. Another interesting fact is that TACN can be very easily converted to TACP. Simply mix dry 10g TACN + 10g NH4ClO4. And add 60g NH4HO 25% aq.
Within an hour, at the lab. temperature, the TACN changes to TACP Directly before your eyes. Highly soluble NH4NO3 will in solution. Therefore TACP requires recrystallization. 10g TACP + 30g NH4OH 15%. The ratios are not specified exactly, but it works reliably. It's a nice reaction to the look. How dark TACN crystals change to light blue TACP. According to the different colors, it is easy to determine the correct ratio / time / temperature / for complete conversion. Like with litmus paper. TACN crystals are in solution almost black, but TACP light blue. Is not necessary dissolving all TACN. Reaction run in mode dark crystal to light crystalb directly.




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[*] posted on 18-6-2021 at 04:40


Attachment: TACN.pdf (1.5MB)
This file has been downloaded 285 times
Attachment: TACN4.pdf (10kB)
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