Sciencemadness Discussion Board
Not logged in [Login - Register]
Go To Bottom

Printable Version  
 Pages:  1    3  ..  6
Author: Subject: Tetramine copper perchlorate help?
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 8-8-2016 at 14:16
Tetramine copper perchlorate help?


I made according to LL's video, but during filtration I added water and all of the crystals dissolved and went through the filter, I take it, this molecule is soluble in water?

To recover should I just evaporate the water?
View user's profile View All Posts By User
NeonPulse
National Hazard
****




Posts: 415
Registered: 29-6-2013
Location: The other end of the internet.
Member Is Offline

Mood: Everclear or Neverclear. Can't decide.

[*] posted on 8-8-2016 at 16:43


If I remember correctly,Water decomposes this stuff and needs to be removed ASAP just vaccum filter the crystals and dry them with a paper towel. I'm not sure if they are hygroscopic but the mother liquor is so drying the crystals as soon as you can is ideal for the life of your product whose life is limited anyways.



Where there is a will
there is a way.

AllCheMystery!
https://www.youtube.com/channel/UCWbbidIY4v57uczsl0Fgv7w?vie...
View user's profile View All Posts By User
kratomiter
Hazard to Others
***




Posts: 105
Registered: 30-9-2012
Member Is Offline

Mood: No Mood

[*] posted on 9-8-2016 at 07:36


I have some experience with TACP: it is very soluble in water, so you must cool down the solution. Even this way, a lot of TACP remains dissolved, so the best way is to evaporate the solution to half volume(~80 ºC). The last time I did it I got an huge amount of TACP, somewhat contaminated with remaining Ammonium Perchlorate (blue color instead of dark violet) but still undergo DDT.
Many people says that water decomposes TACP, but it must be a slow process because I've been able to recover TACP from a heated solution.

BTW, if you see some unsoluble green salt (which I think is copper hydroxide) formed, you can remove it heating the solution, filtering it and the recrystallize your TACP.
It's a very useful primary explosive, my favourite at the moment.

[Edited on 9-8-2016 by kratomiter]
View user's profile View All Posts By User
PHILOU Zrealone
International Hazard
*****




Posts: 2879
Registered: 20-5-2002
Location: Brussel
Member Is Offline

Mood: Bis-diazo-dinitro-hydroquinonic

[*] posted on 9-8-2016 at 08:14


Yes soluble into water ... that was stupid!

You could evaporate your solution (into the cold or under middle warming) and reintroduce the solid or concentrated solution into your process.

Or if not too diluted...you may try to reduce solubility by adding methanol or ethanol.

I would make it from saturated Cu(ClO4)2 solution into demi water agitated into an hermetically sealed reactor and allowing dry NH3 (in excess) to enter little by little into the reactor...the complex should precipitate.





PH Z (PHILOU Zrealone)

"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
View user's profile View All Posts By User
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 9-8-2016 at 10:03


Quote: Originally posted by kratomiter  
I have some experience with TACP: it is very soluble in water, so you must cool down the solution. Even this way, a lot of TACP remains dissolved, so the best way is to evaporate the solution to half volume(~80 ºC). The last time I did it I got an huge amount of TACP, somewhat contaminated with remaining Ammonium Perchlorate (blue color instead of dark violet) but still undergo DDT.
Many people says that water decomposes TACP, but it must be a slow process because I've been able to recover TACP from a heated solution.

BTW, if you see some unsoluble green salt (which I think is copper hydroxide) formed, you can remove it heating the solution, filtering it and the recrystallize your TACP.
It's a very useful primary explosive, my favourite at the moment.

[Edited on 9-8-2016 by kratomiter]


Well, it looks like it is still going to work! I have evaporated with a hot plate and a pan, it has worked!

Primary explosive, I hope not, it is stuck to the bottom of the pan and I had to scrape it off with a plastic spoon...

In LL's videos it seems insensitive to friction, I thought this stuff was equivalent to PETN in sensitivity?
View user's profile View All Posts By User
kratomiter
Hazard to Others
***




Posts: 105
Registered: 30-9-2012
Member Is Offline

Mood: No Mood

[*] posted on 9-8-2016 at 15:10


It doesn't seem to be sensitive to impact or friction, just to flame.
View user's profile View All Posts By User
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 16-8-2016 at 12:17


All,

I used Ammonia Hydroxide, Copper Metal and Ammonium perchlorate... I think that produces TACN not TACP...?

Also is TACP the same as CHP? All of these acronyms...
View user's profile View All Posts By User
PHILOU Zrealone
International Hazard
*****




Posts: 2879
Registered: 20-5-2002
Location: Brussel
Member Is Offline

Mood: Bis-diazo-dinitro-hydroquinonic

[*] posted on 16-8-2016 at 12:25


Quote: Originally posted by MineMan  
All,

I used Ammonia Hydroxide, Copper Metal and Ammonium perchlorate... I think that produces TACN not TACP...?

Also is TACP the same as CHP? All of these acronyms...

TAC(u)N is Cu(NH3)4(NO3)2
TAC(u)P is Cu(NH3)4(ClO4)2
Starting from NH4OH, Cu and NH4ClO4, I hardly think you got nitrate anion forming ex nihilo or from weird oxydo-redox reaction between NH3 and HClO4.

C(u)HP is Copper hexamine perchlorate complex Cu(C6H12N4)(ClO4)2...so you need hexamine (hexamethylenetetramine from formaldehyde and ammonia)




PH Z (PHILOU Zrealone)

"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
View user's profile View All Posts By User
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 16-8-2016 at 12:50


Thank you for the reply PHILOU... it seems I made TACP... which would obviously make sense because of the ammonium perchlorate. The resultant product was beautiful blue crystals, however, I detonated 20grams of this in a 1/8" stainless steel pan, and it did not even dent it!! So 7500m/s... something went wrong.
View user's profile View All Posts By User
PHILOU Zrealone
International Hazard
*****




Posts: 2879
Registered: 20-5-2002
Location: Brussel
Member Is Offline

Mood: Bis-diazo-dinitro-hydroquinonic

[*] posted on 16-8-2016 at 12:58


What did you use to confine the TACP?

I suspect you did it in the open as a pile and thus not enough confinment to allow D2D...

Laboratory of Liptakov uses Cu pipes detonators and allow for pressing at various decreasing pressure to allow for efficient D2D into the Cu pipe.




PH Z (PHILOU Zrealone)

"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
View user's profile View All Posts By User
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 16-8-2016 at 13:09


It was in the open, but was detonated with a 1 gram ETN cap that did dent the pan. So I take it I did make TACP, then...

What is the best way to filter the TACP from the ammonium hydroxide solution, I added water and washed it with water... maybe that was the problem?
View user's profile View All Posts By User
PHILOU Zrealone
International Hazard
*****




Posts: 2879
Registered: 20-5-2002
Location: Brussel
Member Is Offline

Mood: Bis-diazo-dinitro-hydroquinonic

[*] posted on 16-8-2016 at 15:25


Filter and wash with a little methanol or ethanol and allow to dry in open air.



PH Z (PHILOU Zrealone)

"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
View user's profile View All Posts By User
Laboratory of Liptakov
International Hazard
*****




Posts: 805
Registered: 2-9-2014
Member Is Offline

Mood: cool.gif

[*] posted on 18-8-2016 at 10:18
green detonator


Philou write all important. TACP is possible wash and storage under ethanol or methanol. For his DDT is necessary solid cavity. And different density for filling. In close hermetic cavity, as dry crystals, is his stability 150 days by 15 Celsius. Confirmed. Worked after this time. Green detonator exist. But it is not NHN, is it TACP....:cool:....LL



Safety explosive Alfred Nobel 1867. Safety ecologic detonator Dr. Liptakov 2015.
View user's profile View All Posts By User
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 20-8-2016 at 12:03


Not sure where to get ethanol or methanol here in town. Ethanol can be bought as Everclear but that is over $15 for less than a liter.

What about isopropyl alcohol in 90% concentration? I would assume the other 10% is water...will that destroy my TACP through hydrolysis? If there are any other chemicals such as acetone I could use, please let me know, also, how would I go about figure out which chemical would be best to wash off the ammonia?
View user's profile View All Posts By User
DraconicAcid
International Hazard
*****




Posts: 2980
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Online

Mood: Semi-victorious.

[*] posted on 20-8-2016 at 12:14


I don't the 10% water would be a problem, but it shouldn't be too hard to dry to rubbing alcohol.



Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
View user's profile View All Posts By User
PHILOU Zrealone
International Hazard
*****




Posts: 2879
Registered: 20-5-2002
Location: Brussel
Member Is Offline

Mood: Bis-diazo-dinitro-hydroquinonic

[*] posted on 20-8-2016 at 12:19


Isopropanol is OK...although better use a product you know all its content even the 10%! Eventually distill it first.

Eventually do your own ethanol from sugar, fruits and yeast --> distillation. Suggar is quite cheap especially if it comes from free fruits of your garden :D.

Aceton is reactive towards ammonia so:
-it will pollute your product with (CH3)2C=NH and polycondensation products of aceton on itself (NH4OH is quite basic)...
-aceton may also take some of the complexated NH3 from you complex.

[Edited on 20-8-2016 by PHILOU Zrealone]




PH Z (PHILOU Zrealone)

"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
View user's profile View All Posts By User
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 20-8-2016 at 15:39


Don't have any of the equipment to distill either the Isopropanol or make the Ethanol. I used 50g of AP and 150ml of ammonium hydroxide (29%) and about 30 grams of copper tubing. I am letting this solution sit in the sun for a few hours and it is gradually turning a darker blue, although all of the AP is not yet dissolved despite my efforts of allowing the solution to sit in a near boiling water bath.. kind of gave up on that part.

Hope this works well...!
View user's profile View All Posts By User
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 20-8-2016 at 18:02
Don't Think It Worked...Ideas?



Well,

I put the solution in a very hot water bath one more time to try to dissolve all of the remaining AP (Ammonium Perchlorate). I then put the solution in a cold water bath of salt and ice and a lot of crystals the size and texture of table sugar perciptiated, I then washed the crystals with the 91% Isopropyle alcohol.

But the crystals are a pale blue and white (especially when dry) (see picture)... not like the last batch I made...infact there were a few crystals attached to the copper tubing that were much deeper in color (see picture), which is what all of the last batch looked like.

In the picture to the right you can see the lighter abnormal crystals in the background too.

These pale crystals still burn with an electric blue color, but more slowly, and they leave a discolored yellow residue behind.. they burn slow at first, then turn into an ember like charcoal.

I gave the ratios I used in the post above... and I would like to make TACP successfully again, I am not sure what went wrong, but I stayed home all day today to make this, so I am really upset.

Any ideas??




Lighter Blue.jpeg - 2.1MB Deeper Blue.jpeg - 2MB
View user's profile View All Posts By User
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 20-8-2016 at 18:23


Well, I put a few of the lighter colored crystals on the rough rock (as you can see in the picture on the left with my hand holding the copper tube) and hit them with a hammer, they still explode, but feebly compared to the dark blue crystals!

I believe the dark blue crystals to be the true TACP... and it really doesn't take a hard hit with the hammer on the rough rock, it seems actually a little more sensitive than SADS.

Still not sure what went wrong? Also the lighter crystals in the above right picture became much whiter after they fully dried.
View user's profile View All Posts By User
Laboratory of Liptakov
International Hazard
*****




Posts: 805
Registered: 2-9-2014
Member Is Offline

Mood: cool.gif

[*] posted on 21-8-2016 at 01:00
decompose TACP


Preparation copper oxychloride for blue stars: Putting, TACP into cold destilled water. 1g to 100 g water. And bubble pipe air (O2) through. After 60 minutes Arises in water not dissolve copper oxychloride. Preparation CuO for blue stars: Putting 1g TACP to boiling destilled water 200g. After 10 minutes arises black CuO, which is not dissolve in water. Same conditions are for TACN. According temperatures and reaction condition, (short times - partially reaction) arises combination both compounds oxychloride + CuO and partially stay also TACP (or TACN. )
...:cool:..Dr.




Safety explosive Alfred Nobel 1867. Safety ecologic detonator Dr. Liptakov 2015.
View user's profile View All Posts By User
Laboratory of Liptakov
International Hazard
*****




Posts: 805
Registered: 2-9-2014
Member Is Offline

Mood: cool.gif

[*] posted on 21-8-2016 at 02:00
scarify NH3 /4


!!.....Basic properties of TACP is smell ammonia gas. At 15 Celsius slightly, at 50 C much more. ...!
Crystalls smell always. Wet, or total dry. Do not washing in pure water. Is possible washing only in cold (5C) ammonia water concentration 6%. Or washing in methanol, ethanol, acetone. Best explosive properties has slihgtly wet TACP with 1 - 3% ammonia water (24%) between crystals. TACP can exploded even with 15% ammonia hydroxide (water concentration 6 - 25%) between crystalls. Or partially into crystalls. Molecule NH4 hold all molecule TACP together. Pure water pluck and scarify NH4 from molecule TACP. Ammonia water 6% and more, allways return molecule NH4 into TACP. ..:cool:...Dr.




Safety explosive Alfred Nobel 1867. Safety ecologic detonator Dr. Liptakov 2015.
View user's profile View All Posts By User
kratomiter
Hazard to Others
***




Posts: 105
Registered: 30-9-2012
Member Is Offline

Mood: No Mood

[*] posted on 21-8-2016 at 06:30


@MineMan Same problem here with the last batch I made. I'm almost sure that deep blue crystals are pure TACP.
The pale blue colour could be due to a lack of ammonia or copper ion, I don't know for sure but I think is the second one.
View user's profile View All Posts By User
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 21-8-2016 at 07:26


Dr. Liptakov,

I don't understand your points...but I did not dilute the solution with water at all. I used 30% NH4, and then washed with 91% alcohol. Before I even washed the crystals they were of the pale blue color...

Kratomiter, you are right, the deep blue is pure TACP, after more test I can hardly get the light blue crystals to burn...
View user's profile View All Posts By User
MineMan
National Hazard
****




Posts: 455
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 21-8-2016 at 08:40


Ahh... the boiling point of Ammonia is 25 Degrees C. I must of boiled off all of the ammonia in the hot water bath. Plus, out where I live it is about 50 Degrees C in the sunlight, which is where I had my solution. LL... I thought in one of your videos though you said to heat it to 70 Degrees...?

It looks like I better add more ammonia to compensate or tape the holes in the lid shut so it cannot evaporate, all though in LL's video those holes seem to have a purpose... but I would think the AP could provide the oxygen?
View user's profile View All Posts By User
PHILOU Zrealone
International Hazard
*****




Posts: 2879
Registered: 20-5-2002
Location: Brussel
Member Is Offline

Mood: Bis-diazo-dinitro-hydroquinonic

[*] posted on 21-8-2016 at 11:20


Obviously...
Not enough exchange surface between Cu and media
--> reduce your Cu pipe into dust...
--> Or make immediately Cu(OH)2 or CuO
to allow for better immediate reaction with NH4ClO4 and NH4OH!




PH Z (PHILOU Zrealone)

"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
View user's profile View All Posts By User
 Pages:  1    3  ..  6

  Go To Top