Tetramine copper perchlorate help?

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]

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...

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........LL

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 .

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]

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??

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. )
.....Dr.

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. .....Dr.

Philou´s generator TACP

Philou here describe all important. Pure Copper is not reactive, only his oxide. Very Interesting the plast type aparatus - philou - generator TACP. Very easy and cheap. I belive, that it will worked pretty quickly. Very fine wires ? Yes. In the plast jar can be use also very fine wire, copper coins or any pieces of Cu. Allways 2 minute shaking and after open and the jar slightly pressed. For adding oxygen. Recommend for 1,5 liter of plast container: 12g copper, 100g NH4OH 24%, 30g NH4ClO4. Output yield should be 33 - 36 grams of (dry) TACP. And almost all copper should be dissolved. Approximately 90 - 95 % of copper weight. Even it not much smell method. Open plast outdoor, mixing anyplace........Dr.

What would one expect?

Hello all,

Theoretically what would one expect of 2.3 grams (in a tube of lets say 6mm) of near max density 97% TACP and 3% wax (paraffin) initiated by 45mg (pressed) of SADS against a 1cm thick cast iron plate? I would expect a couple mm deep dent in the plate.

I have a few pictures of what I "think" it would look like. Would that indicate a low order detonation because the pictures show no dents, just removal of paint and a few scars?






Attachment: re.zip (3.4MB)
This file has been downloaded 697 times

Other Picture

Other pic

TACP test

TACP is not RDX or PETN. 15g TACP cube 20 x 20 x 20 mm, density 1,8 g/cm 3 (high pressed cube) easy made hole in 3 mm steel plate. Hole approximately 25 x 25 mm. On 10 mm steel thick , same cube made almost nothing. Therefore 2,3g TACP on 10 mm steel made only scratching on surface. Recommend plate 2 - 3 mm. And charge 10 - 20g. Similarly as kratomiter......Dr

Also why add paraffin wax...it will reduce the D2D ability and sensitivity to SADS.

Some of the scratches/scars are deeper...schrapnels of your detonator casing have thus accelerated and penetrated the iron what argues in favor of a detonation.

Also to penetrate the detonation has to be perpendicular vs surface...here it seems the detonator was laying on the side and initiated parallel to the iron surface(*)...it should have been standing straight and be initiated from above.

(*)Your picture is nice because it shows initiation occured from the right and detonation went to the left (all scratches are moving forward in a detonation process (like here) and they would be backwards in a deflagration process)...

[Edited on 24-8-2016 by PHILOU Zrealone]

Quote: Originally posted by MineMan

Also. The Vod is 7500ms according to LL, and the density is greater than RDX or PETN, shouldn't this be similar.... I am aware that for det pressure the Vod is squared....

The OB of Cu(NH3)4(ClO4)2 is +9.7%!

CuN4H12Cl2O8 --> CuO + 2 HCl + 5 H2O + 2 N2 + O2
MM TCuP= 63.5+(4*14)+(12*1)+(2*35.5)+(8*16) = 63.5+56+12+71+128 = 330.5 g/mol
Exces O2 = 32 g/mol --> + sign
OB = 32/330.5 = 0.097 or + 9.7%

The idea to increase the energy output by providing fuel is a good one ...obviously the detonation occured so the wax was a good way to provide protection against moisture and less sensitivity. SADS has already done most of the preparative work of D2D.
Would be nice to compare brisance of two equivalent detonators...waxed and unwaxed for example into a comparative sand crushing.
Maybe next time make use of liquid paraffin oil instead of candle wax to avoid the necessity to melt and overheat the complex...thus loosing some NH3.

The densities of metal containing primaries are always higher than convenional CHNO(Cl) energetic materials, but the metal is also detrimental on two aspects on VOD:
1°) The dead weight of metal or metal oxyd (here 63.5+16 = 79.5) is quite consequent (here about 24% of the weight) and doesn't increases the pressure (total volume of gases)
2°) The dead weight doesn't increase the quadratic speed of the exhaust gases (what is not beneficial to VOD and p).
The quadratic speed of the gaseous molecules increases when the average molecular weight of the molecules decreases...H2 displaying a MW of 2 is thus the best; then comes CH4 (MW16); then NH3 (MW17); then H2O (MW18),then HF(MW20) then CO and N2 (MW28), then O2 (MW32); then CO2 (MW44); then HCl (MW36.5); then Cl2 (MW71)...if CuO becomes gaseous it will require a lot of energy and display a MW79.5 and thus moves very slowly.

So metalic primaries will never be comparable to RDX or PETN in terms of output energy (work).

[Edited on 24-8-2016 by PHILOU Zrealone]

TACP

Quote: Originally posted by MineMan

Ok. Thank you for that explanation! Isn't TACP a secondary.... You refered to it as a primary? I like the idea of solid wax because it will decrease the impact and friction sensativity. What if I add a few drops of ammonia before coating the crystals?

The frontier between primaries and secondaries is sometimes trouble...so yes, stricto senson TACuP is more into the range of secondary because it doesn't detonate in minute amount (<1g) into the open or under slight confinement.

But the blablah about dead weight remains valid for any type of compounds 1^ary, 2^ary or 3^ary Explosives...true that the VOD and gas volume is much less important for primaries...only does matters the initiation ability of the secondary or tertiary...so for primaries the metal dead weight is stil OK.

[Edited on 25-8-2016 by PHILOU Zrealone]

About TACP sensitivity

TACP

TACP is pretty low sensitive. With wax very low sensitive. Therefore is use in system Berta. However pure TACP can have difficult DDT in diameter 6mm. Therefore is better using CHP. It is TACP 88%, HMTA 6% NH4ClO4 6%. Mixing under a few drops NH4OH on porridge, get on surface 80 C and evaporate. Arises soft material, partially crystals, partially as rubber. CHP worked in diameter only 4,3 mm. In copper cavity. General universal scheme is on Vimeo or YT system Berta. Berta detonator is possible trashing blow help the hammer on the anvil. Without explode, of course. //Not try it, everybody.// ..............Dr.

Right LL, I was not trying to accomplish DDT, but rather using a primary

Quote: Originally posted by MineMan

Yes, I am finding that in a 6mm tube 70mg only works a 1/3 to 1/2 of the time! Especially if you coat the TACP with 10% wax... Honestly, I am so sick of failures I think i will wrap the SADS in foil and surround it with TACP, that way the TACP will be on all sides of the primary instead of just one... SADS is amazing when made right... I feel bad even calling it a primary...

Quote: Originally posted by MineMan

All, I want to perform this synthesis again, but I cannot remember the proportions. I have forgotten my stiochemistry from college, can anyone point me to a good source where I can self teach my self how to optimize each reactant so I don't waste any (I think that is called stiochemistry). Also, I bought copper oxide to make it easier!

What are your reactants except CuO?
The proper name is "stoichiometry"

Yes you have to start with the chemical equations...then balance for equity of each atoms on both sides.
Chemical equations are like mathematic equations and can be added, simplified, multiplied or substracted

Because this equation is not the simpliest to start with stoichiometry, I will help you a bit

1°) one of the general rules of metal-acid-base-salt chemistry:
metal oxyde + acid --> metal salt + water
CuO + HClO4 --> Cu(ClO4)2 + H2O
after equilibration of the atoms
CuO + 2 HClO4 --> Cu(ClO4)2 + H2O

2°) another rule is that:
base + acid --> neutral salt + water
NH3 + H2O <--==> NH4OH (*)
NH4OH + HClO4 <--==> NH4ClO4 + H2O
By summing those:
NH3 + H2O + NH4OH + HClO4 <--==> NH4OH + NH4ClO4 + H2O
Then after simplification of H2O and NH4OH on both sides:
NH3 + HClO4 <--==> NH4ClO4 (thus a discrete form of NH3 and HClO4)
In the case of dry amines (base) and 100% concentrated acid the rule becomes:
amine + acid --> amine salt (s)

3°) let us use equations from 1°) and 2°):
NH3 + HClO4 <--==> NH4ClO4
the reverse is also true, so
NH4ClO4 <==--> NH3 + HClO4
and doubled we get
2 NH4ClO4 <==--> 2 NH3 + 2 HClO4
Let us add
CuO + 2 HClO4 --> Cu(ClO4)2 + H2O
--------------------------------------------
2 NH4ClO4 + CuO + 2 HClO4 --> 2 NH3 + 2 HClO4 + Cu(ClO4)2 + H2O
Let us simplify the HClO4 on both sides
2 NH4ClO4 + CuO --> 2 NH3 + Cu(ClO4)2 + H2O

4°) Further work:
We know Cu⁽²⁺⁾ display a very strong affinity for ammonia and it does form a complex Cu(NH3)₄⁽²⁺⁾.
Cu⁽²⁺⁾ + 4 NH3 <--==> Cu(NH3)₄⁽²⁺⁾
We also know (see (*) above) that ammonia has a very strong affinity for water (1L water can dissolve 450L of gaseous NH3...see famous chemical coloured fountain)

So the following equation
2 NH4ClO4 + CuO --> 2 NH3 + Cu(ClO4)2 + H2O
can be written after doubling
4 NH4ClO4 + 2 CuO --> 4 NH3 + 2 Cu(ClO4)2 + 2 H2O
or after complexation of the NH3
4 NH4ClO4 + 2 CuO --> Cu(ClO4)2 + Cu(NH3)4(ClO4)2 + 2 H2O

Since only two moles of NH3 are produced by mole of CuO; only half of the Cu is fully complexed...
we thus have a lack of 4 NH3 to complexate the free Cu(ClO4)2...
Cu(ClO4)2 + 4 NH3 --> Cu(NH3)4(ClO4)2
By adding this equation to the previous one we get
4 NH4ClO4 + 2 CuO + Cu(ClO4)2 + 4 NH3 --> Cu(ClO4)2 + Cu(NH3)4(ClO4)2 + Cu(NH3)4(ClO4)2 + 2 H2O
or
4 NH4ClO4 + 2 CuO + Cu(ClO4)2 + 4 NH3 --> Cu(ClO4)2 + 2 Cu(NH3)4(ClO4)2 + 2 H2O
after simplification of Cu(ClO4)2 into both members (right and left) of the equation
4 NH4ClO4 + 2 CuO + 4 NH3 --> 2 Cu(NH3)4(ClO4)2 + 2 H2O
The later final equation can be divided by 2 since all numbers of moles are even numbers
2 NH4ClO4 + 1 CuO + 2 NH3 --> 1 Cu(NH3)4(ClO4)2 + 1 H2O
and by final simplification because chemist are lazy we don't write the "1" (like it is also often the case into mathematical equations because 1 is implicit: 1*X = X)
2 NH₄ClO₄ + CuO + 2 NH₃ --> Cu(NH₃)₄(ClO₄)₂ + H₂O

5°)Molecular masses:
So now by playing with atomic masses of atoms from the periodic table of the elements for N,H,Cl,O and Cu, you simply have to calculate the molecular mass of:
-NH3
-NH4ClO4
-CuO
-H2O
-Cu(NH3)4(ClO4)2

6°)Weight of each reactant and each product:
Multiply by the stoichiometric factors into the equation
-2 for NH3 and NH4ClO4
-1 for CuO, Cu(NH3)4ClO4 and H2O
to get the mass of reactants and products based on a molar base
Write those numbers below each reactants and products of the equation.

7°)Weight of reactants and products:
Check that the sum of all reactants from the right is equal to the sum of all products on the left of the equation for verification purpose...write that SUM number down for further use

8°)Percentage based weights:
Divide each reactants weight by the SUM number and multiply by 100.
Do the same for each product.
Now you get the ratio of reactants and products for 100g.

------------------------------------------------------------------------
------------------------------------------------------------------------
------------------------------------------------------------------------
The cheapest ingredient is NH3 so you can add a little exces...this also to prevent NH3 escape during process.

26-29% NH3 is 26 g - 29 g NH3 per 100g solution...
or since NH3 has a MW of 17 g/mol (=14+1*3)
--> 100g solution contains 26/17 - 29/17 moles of NH3 = 1,529 - 1,706 moles

[Edited on 8-9-2016 by PHILOU Zrealone]

Wow, Thank you PH Z!!! That must have taken you an hour to type!

Yes, several of those rules I had not learned... I will be mulling over this today and tomorrow, this is great!

Thank you!

Quote: Originally posted by ttrzllvr

You are wasting the Cu perchlorate http://tetrazolelover.at.ua/Unsorted/Cu_glycinate_perchlorat... http://tetrazolelover.at.ua/Unsorted/Cu_Glycinate_Perchlorat... Some info in English: https://www.youtube.com/watch?v=XwUqYtQzAt4

CGP and CGC

Copper Glycinate perchlorate and chlorate? Hmm... Interesting. If will be results from tests for use as detonators for classic secondary charges , it will be much more interesting. If it for this compounds will be requires only thin solid cover, for example hardened paper, or plastic tube, will be it better than system Berta in relatively thick copper. However still I am not see some one hole, or the holes in steel 2 mm thick. Or even 3 mm. I am waiting on results. I am curious. Here bottom:
Hole from sytem Berta - fuse type with Copper hexamine perchlorate. Dr...



[Edited on 12-9-2016 by Laboratory of Liptakov]

Quote: Originally posted by kratomiter

Quote: Originally posted by ttrzllvr   You are wasting the Cu perchlorate http://tetrazolelover.at.ua/Unsorted/Cu_glycinate_perchlorat... http://tetrazolelover.at.ua/Unsorted/Cu_Glycinate_Perchlorat... Some info in English: https://www.youtube.com/watch?v=XwUqYtQzAt4 Very interesting! Any English source to perform that synthesis?

There's probably just one source of impractical synthesis(if you want to wait a week for some crystals )
http://tetrazolelover.at.ua/Unsorted/Copper_gly-perchlorate_...
The Boussingault's mixed Cu(II) glycinate nitrate was my inspiration.
My method is to prepare Cu(II) glycinate first and react it with hot solution of copper perchlorate or chlorate and evaporate the solution on water bath to dryness. Yield is 100%.

Quote: Originally posted by Laboratory of Liptakov

Copper Glycinate perchlorate and chlorate? Hmm... Interesting. If will be results from tests for use as detonators for classic secondary charges , it will be much more interesting. If it for this compounds will be requires only thin solid cover, for example hardened paper, or plastic tube, will be it better than system Berta in relatively thick copper. However still I am not see some one hole, or the holes in steel 2 mm thick. Or even 3 mm. I am waiting on results. I am curious. Here bottom: Hole from sytem Berta - fuse type with Copper hexamine perchlorate. Dr... [Edited on 12-9-2016 by Laboratory of Liptakov]

Quote: Originally posted by Laboratory of Liptakov

Main goals should be some better. Plastic explosive or the detonator.

A (relatively) safe and stable detonator, yes. And it doesn't need to be hyperpowerful. But the plastic explosive??? As the main goal? Then I'm from another planet

Quote: Originally posted by Laboratory of Liptakov

Hmmm... Stability, Yield and Availability are only partially goals. Main goals should be some better. Plastic explosive or the detonator. Or both. Making prepare from CGP or CGC of course. Dr.

Did you prepare a sample already? It is an interesting compound. I do not say your invention has no place on earth (Jára C. by tě pochválil), but some people want stability (also I'm radically not interested in commonly known energetic materials ).
Since the glycinate-chlorate is my invention, I focus primarily on it now. It is a challenge for me to develop a practically usable cupric chlorate based energetic material (ok, HATE me!) which is stable, nonexotic and cheap (and almost insensitive too). The ammine complexes are on the road of suiciders, so I focused on double salts. After a few years of research and making tests (I prepared a bunch of basic cupric chlorate or perchlorate energetic salts but I wanted a simple, non-hydroxy salt) I found the right compound maybe (HATE me twice!). If someone interested, here are some photos of an another test, 0,15g of CuGLYClO3.xH2O/0,15g PETN in a plastic tube
http://tetrazolelover.at.ua/CU_glycinate_chlorate_plastic_tu...
http://tetrazolelover.at.ua/Unsorted/CUGLYClO3_0.15_PETN_0.1...
Ignited by a black powder fuse. I guess the chlorate is a quite efficient obscure primary. I don't know the minimum initiating charge for PETN yet. But do not experiment with it! Still needs to be tested. Tests of perchlorate in plastic or paper tubes later. Then I'll make a new thread here (or someone else)...or not.

Other picture with 0,15 PETN ,.......It looks good!...........Dr.
Glycine is available?

[Edited on 16-9-2016 by Laboratory of Liptakov]

Glycine

Whow? ... Very cheap.. Cheaper than anything others. Cheaper than coffee. The big attempts waiting on everybody. .....Dr.

Quote: Originally posted by PHILOU Zrealone

Beware to the stability of Cu(ClO3)2...

Quote: Originally posted by ttrzllvr

Quote: Originally posted by PHILOU Zrealone   Beware to the stability of Cu(ClO3)2... I know. I meant the Gly-chlorate as a stabler and less sensitive replacement for TACC or as a "worst case" primary instead of organic peroxides. Of course, it is far from the ideal primary and no one should store it too long and in large quantities. I'm still testing it's stability. I prepared a few larger crystals to see possible changes easier. It has some smell, but the glycine I used was smelly too, even other chemicals have some... I must wait. I know the Gly-chlorate has no future, but the Gly-perchlorate seems to be very promising.

Amine perchlorates are:
-denser
-storage stabler
-less impact/shock and friction sensitive
-more powerful (if OB below or equal to 0)
-display higher VOD
than amine chlorate

But amine chlorate are more prompt to D2D than amine perchlorates and as such they must be closer to primaries.

Here you have several troubles:
1°) Cu(ClO3)2 stability concern..unknown behaviour?
2°) unknown stability of an organic ligand towards oxydoredox onto a catalytic metal core...this increases the sensitivity to heat/shock/friction ... but maybe also reduces the average life-time by lowering the activation energy necessary to induce decomposition?
3°) Unknown stability of amine chlorate...does it auto-oxydo-redox-ise to nitroso (-N=O) and chlorine oxydes (ClxOy) or amine dichlorides (-NCl2) upon time?
This is observed with NH4ClO3...what produces NCl3!

So first study :
-Storage stability
-Density of crystal and bulk
-Exact composition/formula
-Impact sensitivity
-Heat sensitivity (T° deflagration/detonation)
-DSC curve
-Initiating ability of known HE vs other common primaries
-Brisance (via sand crushing)
-VOD (via test plates and comparison with common HE) or Dautriche's or oscilloscope.

Each amino ligand is specific so must be done for each new compound although for certain compounds one may expect related properties owing to parenthood...like for example CH3-NH2 and H2N-CH2-CH2-NH2
--> Cu(H2N-CH3)4(ClO3)2
--> Cu(H2N-CH2-CH2-NH2)2(ClO3)2
what would be equal to Cu(H2N-CH2-)4(ClO3)2 and thus very close to the first one.

It is similarly as for copper hexamine perchlorate. I mean. Hexamine is classic organic compound? Thanks, Philou..Dr..

Quote: Originally posted by PHILOU Zrealone

Amine perchlorates are: -denser -storage stabler -less impact/shock and friction sensitive -more powerful (if OB below or equal to 0) -display higher VOD than amine chlorate But amine chlorate are more prompt to D2D than amine perchlorates and as such they must be closer to primaries. Here you have several troubles: 1°) Cu(ClO3)2 stability concern..unknown behaviour? 2°) unknown stability of an organic ligand towards oxydoredox onto a catalytic metal core...this increases the sensitivity to heat/shock/friction ... but maybe also reduces the average life-time by lowering the activation energy necessary to induce decomposition? 3°) Unknown stability of amine chlorate...does it auto-oxydo-redox-ise to nitroso (-N=O) and chlorine oxydes (ClxOy) or amine dichlorides (-NCl2) upon time? This is observed with NH4ClO3...what produces NCl3! So first study : -Storage stability -Density of crystal and bulk -Exact composition/formula -Impact sensitivity -Heat sensitivity (T° deflagration/detonation) -DSC curve -Initiating ability of known HE vs other common primaries -Brisance (via sand crushing) -VOD (via test plates and comparison with common HE) or Dautriche's or oscilloscope. Each amino ligand is specific so must be done for each new compound although for certain compounds one may expect related properties owing to parenthood...like for example CH3-NH2 and H2N-CH2-CH2-NH2 --> Cu(H2N-CH3)4(ClO3)2 --> Cu(H2N-CH2-CH2-NH2)2(ClO3)2 what would be equal to Cu(H2N-CH2-)4(ClO3)2 and thus very close to the first one.

These are well known facts. But thanks anyway . Already for a couple of years the philosophy behind my interest in some energetic materials is other than scientific, so personally I do not need to know everything about the compound. Stability (alone, in the presence of metals, natural plant or animal organic matter, human sweat and blood, soil, some minerals, secondary explosives or other pyrotechnic compounds), friction sensitivity (on metals, hard soil, stones, wood, textile materials, leather...) and initiating ability (from PETN to some less sensitive AN formulations) is what I need to know.

Quote: Originally posted by ttrzllvr

Ok, other tests done with the Cu GLY-perchlorate. If someone interested (you know where to find it). No doubt, the compound has a future.

I have tried to find it onto your website but it is not easy... can you point me out the right direction where to look for?

system Berta

Peter: Biure as ligand unfortunately, not try it. Without minimal 20 tests is impossible say what it will making. However, Copper hexamine perchlorate is tried almost 1000x. Always making, worked without failed. Basic prepare is the porridge under ammonium hydroxide usually 24%. Mix for porridge is TACP 88%, hexamine 6%, NH4ClO4 6%. This porridge is put on hot inert plate, 80 Celsius. From porridge during hot process arises dry, but relatively soft material. With low sensitive on friction. Even is possible scratching this material helping steel mapboards at this temperature and get dry material from plate. Recommend at 20 Celsia, of course. After is necessary making agglomerate 2x2 mm. Next steps are see in picture here return page. Agglomerate is possible store in closure in the jar on 1 month. And after filling again, without changes of properties. This process is all confirmed. Always is better preparation small amount. For example 4,4 TACP, 0,6g hexamine, 0,6g AP. Dr. ...LL....

Quote: Originally posted by Peter Lustig

Complex compounds such as M(Amin- Lingant)(ClO4)2 are very interesting. What do you think about Biure as Lingand? I'm trying to prepare Biuret. @LL I have calculated, 6% Hexamin ist not enough for NH4 (Cu Hex2) (ClO4)3. System Berta is still interesting. [Edited on 30-9-2016 by Peter Lustig]

Quote: Originally posted by Peter Lustig

Complex compounds such as M(Amin- Lingant)(ClO4)2 are very interesting. What do you think about Biure as Lingand? I'm trying to prepare Biuret.

Quote: Originally posted by Laboratory of Liptakov

Philou here describe all important. Pure Copper is not reactive, only his oxide. Very Interesting the plast type aparatus - philou - generator TACP. Very easy and cheap. I belive, that it will worked pretty quickly. Very fine wires ? Yes. In the plast jar can be use also very fine wire, copper coins or any pieces of Cu. Allways 2 minute shaking and after open and the jar slightly pressed. For adding oxygen. Recommend for 1,5 liter of plast container: 12g copper, 100g NH4OH 24%, 30g NH4ClO4. Output yield should be 33 - 36 grams of (dry) TACP. And almost all copper should be dissolved. Approximately 90 - 95 % of copper weight. Even it not much smell method. Open plast outdoor, mixing anyplace........Dr.

It ended up working... I think the color is very dependent on how dry the TACP is and if there is any ammonia left.

But here is my main problem, there is always copper oxide left in the TACP... and it is a pain to separate out (and expensive with all of the alcohol it takes!

I tried this again a few days ago, except I used and excess of all reactants (NH3, AP) except the CuO, which I purposely used a deficiency to ensure none was left over in the product. It still was! Even after heating the solution to near boiling, and letting it react for 2 days!

Any ideas??, really fed up... I would just use copper wire, but I don't have a magnetic stirrer, or have the time to shake the jar every 5 min for 4 hours...

I am really frustrated, and would like some help...

TACP preparation

Quote: Originally posted by MineMan

Quote: Originally posted by Laboratory of Liptakov   Philou here describe all important. Pure Copper is not reactive, only his oxide. Very Interesting the plast type aparatus - philou - generator TACP. Very easy and cheap. I belive, that it will worked pretty quickly. Very fine wires ? Yes. In the plast jar can be use also very fine wire, copper coins or any pieces of Cu. Allways 2 minute shaking and after open and the jar slightly pressed. For adding oxygen. Recommend for 1,5 liter of plast container: 12g copper, 100g NH4OH 24%, 30g NH4ClO4. Output yield should be 33 - 36 grams of (dry) TACP. And almost all copper should be dissolved. Approximately 90 - 95 % of copper weight. Even it not much smell method. Open plast outdoor, mixing anyplace........Dr. LL, from my calculations that seems like WAY too much NH4OH!!!, which is really the expensive component for me. Is this a scenario where the stiochomitry is not valid because we nee a lot more NH4OH for the ammonium perchlorate to dissolve? Philou, from the help you gave me earlier I calculate what is necessary for 100 grams of product (95g TACP and 5g H2O). Does this look right? AP: 68g NH3 (25%):35 grams CuO: 22grams But this seems nothing close to what LL is using...? [Edited on 12-10-2016 by MineMan]

Quote: Originally posted by Rosco Bodine

Glycine forms an adduct 1:2 with ammonium nitrate as does hexamine, and both may also form an adduct 1:2 with ammonium perchlorate. The weight proportion for glycine and NH4ClO4 1:2 molar would be 1 gram / 3.13 gram An interesting experiment would be to mix glycine and NH4ClO4 as a slurry wet with enough water to allow long stirring at mild temperature, and then evaporate at mild temperature the water. If there is an adduct of glycine and NH4ClO4 it could have interesting energetic properties. See US4746380 for the glycine adduct with NH4NO3 http://www.sciencemadness.org/talk/viewthread.php?tid=29&... The adduct for hexamine and NH4NO3 is described in US3166452 Glycine forms an adduct with Strontium Perchlorate which is useful as a red flare composition. It would be no surprise if that adduct is also detonable. See US3296045 attached [Edited on 9/19/2016 by Rosco Bodine]

Quote: Originally posted by specialactivitieSK

Melting organic compound of copper with AP ?

Why not!
Cu (II) trinitrophenate and NH4ClO4?
Just kidding...too sensitive

The melting of Cu acetate and NH4ClO4 might be interesting but do it in tiny quantity just in case...Cu tends to catalyse many decomposition reactions...

And it is some question or some result how to make or how to counting before preparation ? ........LL

Quote: Originally posted by specialactivitieSK

??? Copper hexamine perchlorate : Cu + Hexamine + A.P. Cu + C6H12N4 + 2NH4ClO4 = Cu (C6H12N4)(ClO4)2 + 2NH4 ( 10+22+37 = 63+5.6)