My copper tetra Amine Adventure

The best of run off chem and eye balling!

When cruising you tube I came across some testing of the above substance and figured it was nifty and cursory look into its making was mentally shelved for later use.

https://www.youtube.com/watch?v=YaCLTWsHEpI < Setting off

https://www.youtube.com/watch?v=Uj9BkyGo70w < One method of synthesis

https://www.youtube.com/watch?v=X65pAuLGlDo < Synth 2 (Basic method I am using)


Well Using the Nile reds method of making zeotropic Nitric acid such as adding water to the nitrate salt then reacting with the H2SO4 then re distilling collecting at 120c.

Nile red method: https://www.youtube.com/watch?v=KBeo8nww21g

Well he kept the weak fraction coming under the 120C mark for cleaning, but I decided to use scrap copper and make copper nitrate, Ok nifty but what to do with it?

Well I happened to have Ammonia on hand, at 3% So dump the two in and well pretty no crystals too much water.

Back to the nitric acid: From wally world you can get CaN/AM cold packs, So to get rid of the Ca I react with the Ammonia, I keep adding small amounts till no more precipitate forms leaving me with aqueous AN SO via Nile red method I just skip the water and pour in this now pure AN solution! Takes 2 boxes (4) cold packs to make 250Ml 68% nitric (Put the CaOH tot he side it can be handy)

So we have (NH4)2SO4, HNO, H2O, So set aside the HNO/H2O and set off to dehydrate the (NH4)2SO4 to a concentrated solution, so I set that aside and store for what ever.

Back to the tetra amine: So now I have my some what deep blue solution and some greenish precipitate, So too much water and not enough ammonia so what to do? Ah ha! yes I have Sodium hydroxide. So lets make a NH3 generator.

Dramatic Re-Enactment:




As you can see it was a good success but needed more ammonia but ran out of Sodium hydroxide, so back in the fridge it goes till I can get more. You can see the ammonium Sulfate has some minor contaminant but this has no effect on the gass generation.

The check valve is just a cheap air check valve to prevent suck back or rather slow it down (Remember you get what you pay for!)

But that is my interesting story of how to use waste products from one reaction to fuel another!

Will update as the adventure continuous! Looking forward to the end testing! Need a nice big pumpkin to soften up for some food grad chemistry!


[Edited on 2-4-2017 by XeonTheMGPony]

Like I said I was aware of the methods all ready there, but I wanted to find a use full way to dispose of waste products of my main reaction which was the Nitric acid.

So when you look at the over all reactions, you can skip some of the middle men So I take my header from the azeotropic distillate toss in scrap copper and let that react a few days til no more copper reacts.

Take out the copper, and chill in the fridge.

Take my fresh ammonium sulphate to make the NH3, I take my flask dump in NaOH till 1/4 of the bottom is full then drip in my (NH4)2SO4 till it stops producing gas, then reset and run again till sufficient ammonia is in solution.

Seems to work quite well, I just didn't have as much Hydroxide as I thought I did.

You definitely need to chill the copper nitrate solution befor ammonia addition and stirring helps but the bubbles will do a bit as well as steam is generated.

I just wanted to show a method to Jerry rig up an addition system when one lacks an addition funnel and such for a gas generator.

Thanks for your interest Will try to get pics of the generator running next time.

Quote: Originally posted by Elemental Phosphorus

How hard to detonate is TACN anyway? I know it will deflagarate with strong heat but how would one detonate it?

Got more NOH so this is how it looks after the second absorption run, I can now smell strong free ammonia from the solution, will do a third run once cool to saturate it.

All the material is now a nice dark blue with just a few specs of the lighter blue precipitate.

It seems, that your big problem is obtained ammonia water 24%. It is usual concentration for store and for next use. Instead it for you is not problem obtained HNO3. Notable country. Well, last way anyway, concentration ammonium water on 25% or more, is necessary at zero celsia adding NH3 gas. After increase NH3, will precipitate crystals TACN directly from solution. At zero C and concentration 28% will in jar pretty light blue water and huge amount TACN on bottom. Better is cooling solution for example on - 18C. Results will still better. And solubility NH3 of course highest.......Dr.

Quote: Originally posted by PHILOU Zrealone

What is NOH? Nickel oxyde hydride? A typo for NH4OH or NaOH? When using accronyms or abreviations..to avoid any confusion you should write somewhere into your text the name/meaning in extension. The use of NH3 or NH4OH to get rid of Ca(2+) into Ca/NH4 nitrate is not the best method since Ca(2+) tends to be complexated by NH3... 1°) Remember that EDTA (Ethylen diamine tetraacetic acid) complexates Ca(2+). 2°) Soluble Ca(NH3)x(NO3)2 may form with x = 1,2,4,8... (see complexation of NH3 by Mg, Ba, Ca, ... salts) So maybe you got some Ca(OH)2 precipitation (what is not that unsoluble BTW) but most of the Ca(2+) did remain into your initial reaction batch. Would be smarter to use Na2CO3 or NaHCO3 until no more unsoluble CaCO3 precipitates. Na(+) will not interfere into the Cu(NH3)4(NO3)2 process.

Today was filter day, some nice high density crystals followed by some nice fluffy ones!

So Now I need to boil down the mother liquor and hit it with ammonia gas again and add some more copper nitrate to get more crystals till all my waste copper nitrate is used up from the mercury cleaning!

Looks like you finely got TACuN

To speed up precipitation, collection and drying one may use methanol/ethanol dropped into the Cu(NO3)2 saturated solution and then introduce the concentrated NH3 solution (NH4OH)...

To speed up things further add a little diethyl-ether...

The cristals may be conserved dry for ages into an hermetical recipient under ether...
The ether layer is clear as water and the cristals very deep blue at the bottom...cristals dry faster when filtrated since ether is very volatile ==> at ambiant heat

TACuN

And after all what described Philou, hitting on the anvil. TACuN requires a bigger hammer. For confirming his properties.......Dr.

Just weighed out to 38.x grams, will ensure to do so for testing, thanks.

And hey 4 months is nothing when ignoring a beaker lol those crystals been sitting there for ages just haven't bothered to filter them out but with my shiny new glass powder addition funnel and bag of cotton balls handy figured take it for a test drive

PZ: Good news on the shelf life, I was suspecting they'd be short lived once dried! Hence why I left them in solution till I was ready to play with them. guess semi-hermetic will have to suffice as I tend not to weld things like ether cans

LL: Does it need to be wrapped in any thing like tin foil or paper? Or just a good sized crystal and a firm hit?

TACuN

Quote: Originally posted by XeonTheMGPony

Would methanol be compatible? As I have scant anhydrous ethanol and would rather not use it on that! Goat I need to get my vacuum desiccation chamber built! too much to do for one man! [Edited on 29-7-2017 by XeonTheMGPony]

Yes methanol compatible although a little more soluble inthere than into ethanol....maybe isopropanol could be another possibility but I have no experience with it...theorically should be better or equal to ethanol ;-).

Avoid aceton since it reacts with ammonia and will change the properties of the complex.

Spare the good ethanol to celebrate succes

Better use hermetic jar because otherwise the vapour pressure of TACuN will set NH3 free...any conserving food jar like jam jar, bolognese salsa jar, ... will do...after washing with liquid soap, warm water, rinsing and drying

TACuN

Why TACN?? the perchlorate is so much cooler.

Can someone please try to grow a large crystal of the TACP, it is so pretty, plus I would like to measure the det properties of a monocrystalline explosive. And they are so pretty. Any tips on how to do this other than cooling the solution slowly

The results!

Quote: Originally posted by XeonTheMGPony

The results!

Nice but to be more speaking and representative it is good to have a reference object next to the hole and the initial charge too.
So one can have an idea of the size of the hole vs charge vs reference
==> Nothing look more like a hole than another hole without references (2cm, 10 cm, 50cm, 1m...hard to tell)

Laboratory of Liptakov's (LoL) does it perfectly so maybe inspire from his schèmes, pictures, videos.

Quote: Originally posted by MineMan

Why TACN?? the perchlorate is so much cooler. Can someone please try to grow a large crystal of the TACP, it is so pretty, plus I would like to measure the det properties of a monocrystalline explosive. And they are so pretty. Any tips on how to do this other than cooling the solution slowly

Why not? ...
Almost everybody gets his first hands onto TACuN...the process is cheap, easy and beautifull.

Some people don't have easy access to ammonium perchlorate (AP), copper perchlorate or perchloric acid...to be able to make TACuP...and making those OTC is more labour intensive and cost more than obtaining nitrates or ammonium nitrate (AN)...

*********************************
About your monocrystalline TACuP...
Instead of slow cooling...you may:
1°) Make a saturated solution of TACuP and introduce a seeding cristal...then allow for slow evaporation...like common large Crystal growing techniques...

2°) Make a saturated solution of TACuP with a seeding cristal into it (into a tiny recipient) and allow for a slow migration of solvent (by natural evapo-condensation) into a closed large recipient holding the volatile solvent (methanol or better ethanol or even better isopropanol).
The volatile solvent will evaporate into the closed volyme condensate into the saturated TACuP solution (the TACuP solution will evaporate some water into the surrounding and thus concentrate a little)...so you get two effects into the solution...a slight concentration and a solubility drop (induced by the solvent)...this results into crystallization that is easier onto the already present seeding crystal...the later will thus grow.
Usually the solvent condensate at the surface of the liquid into the inner tiny recipient...you thus observe a concentration gradient (upper layer is paler even colorless-clear at a certain stage) while the bottom is deep blue like initial TACuP...during crystallization the amount of dissolved TACuP diminishes and as a consequence the solution becomes paler and paler (the blue color fades).

3°) You work with a saturated TACuN solution and you introduce slowly drop by drop a saturated AP solution into the media...until it becomes slighly milky/turbid ==> then you add a few drops of water to make it clear again (to be on the edge of precipitation of TACuP.
Again you put a seeding Crystal of TACuP (suspended into the fluid), and you allow for slow introduction of saturated AP solution drop by drop under slow agitation (1 drop per 5 minutes)...
TACuP is less soluble than TACuN and hence it will precipitate and this process is easier onto the already present seeding Crystal...the solution of TACuN will become paler and paler...but it needs to be refreshed somehow also slowly.
At the end into solution you will have AN, TACuN and a little TACuP and AP...
This later process is less convenient that the previously exposed.

4°) You need 3 recipients...and tubings (see drawing below)

-The nr 1 contains crystals of TACuP and a saturated solution of TACuP
-The nr 2 contains a seeding crystal suspended into saturated solution of TACup
-The nr 3 contains initially water...but it will enrich itself into TACuP of lower concentration than the saturated solution.

The third recipient may be slighly heated to ensure evaporation of water that will condensate into the first..
When this happens the same volume of saturated TACuP solution will be displaced into the second recipient holding a seeding crystal...what will grow...and depress concentration of the saturated TACuP soluation a little...
When this happens the same volume of less saturated TACuP solution will fall into the third recipient.

From time to time when concentration into the third recipient becomes too saturated it can be refreshed by new water and the initial content evaporated to regain TACuP crystals recyclable into the first recipient...

The syphons needs to be amorced by introducing some saturated fluid into them...

In principle no heat is needed (since vapor pressure of the third recipient will be higher than the first as long as there is a difference in concentration between recipient 3 (dilluted) and 1 (saturated)) but this may help the process to be a little faster...

Thus on end was in basically the mole, who maked the hole in clay. I knowed it. Nothing TACP, only the mole. .......LL

Quote: Originally posted by XeonTheMGPony

I'm not interested in re-inventing the wheel. not going to waste time messing about with chlorates of any type! The Tetra amine is a fun way to get rid of waste chems till I have better use for them, the point of creating this threads for those starting out can see how you can use the by product of one reaction to fuel another so lets keep it on that topic please! That or specifics to tetra amine copper nitrate.

TACuP

Thanks for complex explain.......................LL

Well some new toys arrived so figured I'd deal with the last beaker of blue slurry and close this venture down as all the mercury been don, only thing left is to distill it in a hydrogen atmosphere to reduce any oxides.

Some fun pics.

Addition funnel
SS Keck clips
Nice new clamp.
Hallow plugs.
And a gift from a friend but not shown is a beauty full mercury therm that goes to 110c
And of course my shake n bake lab mantle and temp control!

Quote: Originally posted by XeonTheMGPony

And forgot to add a fun dose of irony, my source for ammonia was fire extinguisher powder, ABC type to be exact [Edited on 16-11-2017 by XeonTheMGPony]

Quote: Originally posted by XeonTheMGPony

that's why it needs to be stirred and refluxed, then the hydrophobic parts settle out on top like a weird jelly moose so just have to filter and discard of the sludge any way you wish.