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Author: Subject: Nitration with Anhydrous Copper Nitrate
Motherload
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[*] posted on 22-2-2013 at 22:25


As far as I understand .... Any nitrations involving cupric nitrate require acetic anhydride.
They can only mono nitrate a deactivated aromatic ring.
What is the expected outcome for using cupric nitrate .... That would be better than conventional nitration for synthesizing energetics ?




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[*] posted on 22-2-2013 at 23:13


I got an idea, get the NO2 gas from the decomp, then cool it down to -11 degree to get N2O4, then put the dry CuO to get Copper nitrate :)
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[*] posted on 23-2-2013 at 01:25


Quote: Originally posted by Motherload  
As far as I understand .... Any nitrations involving cupric nitrate require acetic anhydride.

Unless you can manage to prepare anhydrous Cu(NO3)2 in the absence of water, which is not a simple thing to do.

Quote: Originally posted by Motherload  

They can only mono nitrate a deactivated aromatic ring.
What is the expected outcome for using cupric nitrate .... That would be better than conventional nitration for synthesizing energetics ?

Do not quote me on this, but I think I remember reading that nitrations with Cu(NO3)2 on aromatic rings give a higher ratio yield of the para- isomer, as the case may be, and are also less likely to oxidize any vulnerable functional groups.
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[*] posted on 23-2-2013 at 07:37


Quote: Originally posted by KonkreteRocketry  
I got an idea, get the NO2 gas from the decomp, then cool it down to -11 degree to get N2O4, then put the dry CuO to get Copper nitrate :)


I have mentioned that a couple of times in your copper nitrate synthesis thread.

@Anders
I know that ... I am posting in the "Nitration with Anhydrous Nitrate" thread regarding nitration with Acetic anhydride present.

[Edited on 23-2-2013 by Motherload]

[Edited on 23-2-2013 by Motherload]




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[*] posted on 23-2-2013 at 13:55


Quote: Originally posted by KonkreteRocketry  
I got an idea, get the NO2 gas from the decomp, then cool it down to -11 degree to get N2O4, then put the dry CuO to get Copper nitrate

I think it would probably work, but I am not completely sure. CuO might be too weak of a base in the absence of water. (Even if the gas is absorbed, you might only get some sort of double nitrate/nitrite salt, if the initial nitrite that forms is not in ionic form then further NO2 would then not be able to oxidize it to the pure nitrate.) For the reaction to proceed, you would also need some sort of liquid solvent that could dissolve either the initial solid reactant or the product, I am not sure what exactly that might be.

Edit: Woelen says the reaction does work...
Quote: Originally posted by woelen  
But in the 1960's the anhydrous salt was prepared by reaction of metallic copper with a solution of thoroughly dried NO2 in ethyl acetate at low temperature.


Makes me wonder how the reaction can produce nitric oxide without the copper nitrate just oxidizing it.

[Edited on 23-2-2013 by AndersHoveland]
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[*] posted on 5-5-2013 at 22:16


Excuse me, but I've already obtained the Anhydrous Copper Nitrate. Can we get back to nitration?



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[*] posted on 11-5-2013 at 20:32


Quote: Originally posted by APO  
Excuse me, but I've already obtained the Anhydrous Copper Nitrate. Can we get back to nitration?


So, you wanted a nitramine, correct? And I'm assuming you want to eschew acetic anhydride?

What substrates are you considering?

And political or nationalist signatures of any kind are a tendentious topic here. We post for the science, not the drama.

[Edited on 12-5-2013 by killswitch]
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[*] posted on 11-5-2013 at 21:55


Signature... Taken care of.

I would like to make Picric Acid from it, Anders said I could use it to nitrate phenol. Also Methenamine would be fun. I haven't maid any Acetic Anhydride yet, so that's not currently an option until I get Phosphorus Trichloride.




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[*] posted on 11-5-2013 at 22:21


Come on APO, you have listed in the last week that you want to make just about every single high powered explosive. Do you know the chemistry behind them that will prevent you from killing yourself? Why start so huge? Have you even done a nitration before? I'm guessing not since you ask if there is a nitric acid that won't burn your skin, you should wonder how HE's will rip your skin off, and figure out a blast shield/loading mechanism.

Do some acid-base extractions, make nitrocellulose for damn sakes. Everyone here is concerned about your wants and needs man can you not take a hint? Tell me ONE experiment you have done pertaining to basic knowledge of any energetic.

There are fun things you can do other than risking your life with these compounds. What chemicals are in your possession right now and I'll tell you something k3wl you ran reasonably do to improve your skills. Do you even own a beaker, a Flask..? what do you have in your lab, maybe a GC-MS unit?

EDIT 1: Fixed errors.

EDIT 2: This just happened today, here is a picture of my thumb after a tiny drop of 70% nitric acid got on me, I didn't notice until it was hurting and at that time I could see some meat was eaten under the yellow stain. After I washed my hands the yellow skin fell off and now I have this little hole.


[Edited on 5-12-2013 by chemcam]




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[*] posted on 12-5-2013 at 14:46


That's not so bad.



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[*] posted on 12-5-2013 at 14:56


Quote: Originally posted by APO  
That's not so bad.


Yeah, nothing to be afraid of, just respect it and it will respect you. I was being lazy and didn't put my gloves on while filling up my 250mL reagent bottle from a large 2.5L bottle. The drop got me when I took the funnel out.




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[*] posted on 12-5-2013 at 16:26


Ever work with fuming nitric acid?



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[*] posted on 12-5-2013 at 16:34


Yes I have made it many times. I haven't spilled it though, I always wear gloves with WFNA and RFNA. The ACS 70% that I have even fumes quite a bit.



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[*] posted on 12-5-2013 at 20:41


Do you use a respirator?



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[*] posted on 12-5-2013 at 21:19


Quote: Originally posted by APO  
Do you use a respirator?


No I dont use a respirator only use very nice goggles. When I do a reaction that fumes heavily like NO3 or similar I have 2 large fans that push the vapors out of the garage. Never have fans suck the vapor or you will have problems. I also have a fume hood but at the moment it needs repairs, I ran the fan solid for a long time with no speed regulation and it burnt out.

EDIT: Hey APO with these kind of questions that nobody else benefits from why don't you just u2u them to me instead. I'm not an asshole or anything, but a smart-ass sometimes.

[Edited on 5-13-2013 by chemcam]




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[*] posted on 13-5-2013 at 02:40


Quote: Originally posted by APO  
Signature... Taken care of.

I would like to make Picric Acid from it, Anders said I could use it to nitrate phenol. Also Methenamine would be fun. I haven't maid any Acetic Anhydride yet, so that's not currently an option until I get Phosphorus Trichloride.
What are you talking about? Please be realistic. A 13 year old boy getting phosphorus trichloride?
Are you really interested in chemistry or do you just want to boast about dangerous and hard to obtain chemicals to impress others?

Could you post a list of chemicals you have now and as others asked, could you also tell what kind of equipment you have? You know? Stuff like PCl3 is not for little kids.




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[*] posted on 13-5-2013 at 02:57


He was saying that President Obama "sucks".

Simply quoting, not saying my opinion.




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[*] posted on 13-5-2013 at 13:51


First of all Woelen, Phosphorus Trichloride can be made from slow addition of gaseous Chlorine to elemental Phosphorus, and second of all, I'm truly interested in chemistry and I'm editing a lab tour video as we speak to silence some of my critics.



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[*] posted on 13-5-2013 at 16:27


APO, I can tell ytou are very interested in chemistry, but I really doubt wha you have is anhydrous copper nitrate under argon. I know thats what the seller said it was, but I am 99.99% sure it is a hydrate.

Good luck friend.




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[*] posted on 13-5-2013 at 16:56


Damn.



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[*] posted on 13-5-2013 at 16:59


Quote: Originally posted by APO  
Damn.


Can you post a picture of what you have, in the bag.




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[*] posted on 13-5-2013 at 17:03


Will do in my lab tour.



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[*] posted on 13-5-2013 at 21:30


Quote: Originally posted by APO  
Will do in my lab tour.


Well i'll be damned, APO has very, very nice glassware and reagent collection is okay for beginner, some stuff you have is too risky. I wish I had a soxhlet extractor though!

I still hope you do not start with energetics, in your video you mention acetone peroxide, I wouldn't recommend that because at your age you cannot fully comprehend the risk-to-benefit ratio and if you lose a hand your whole life will be ruined which I said in some other thread but good advice can be repeated. I see you also have some methenamine, HMTD is pretty sensitive too if that's in your to-do list.

In your video you sound very intelligent, maybe too intelligent for your age, you have just enough knowledge to get yourself into trouble. =] Good Luck in your quest young friend.

EDIT: Who or where did you buy your tert-Butanol from? I can't find small amounts like that. Are you in America?

[Edited on 5-14-2013 by chemcam]




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[*] posted on 14-5-2013 at 06:36


I mentioned Acetone Peroxide if I gained enough balls for that, but I'm aware of the risks so If I don't expect more that milligram amounts if I do make some. I know Hexamethylene Triperoxide Diamine is sensitive as well, but in it's pure state it's said to be more stable. Yes, I live in the US, and I bought the Tertiary Butanol from eBay.

For everyone else, here's my lab tour video:

https://www.youtube.com/watch?v=rPBep_rOuJE




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[*] posted on 14-5-2013 at 06:40


It will be deleted one month from 5/13/13 for personal reasons.



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