Sciencemadness Discussion Board

Tetramine copper perchlorate help?

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MineMan - 8-8-2016 at 14:16

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?

NeonPulse - 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.

kratomiter - 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]

PHILOU Zrealone - 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.


MineMan - 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?

kratomiter - 9-8-2016 at 15:10

It doesn't seem to be sensitive to impact or friction, just to flame.

MineMan - 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...

PHILOU Zrealone - 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)

MineMan - 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.

PHILOU Zrealone - 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.

MineMan - 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?

PHILOU Zrealone - 16-8-2016 at 15:25

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

green detonator

Laboratory of Liptakov - 18-8-2016 at 10:18

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

MineMan - 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?

DraconicAcid - 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.

PHILOU Zrealone - 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]

MineMan - 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...!

Don't Think It Worked...Ideas?

MineMan - 20-8-2016 at 18:02


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

MineMan - 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.

decompose TACP

Laboratory of Liptakov - 21-8-2016 at 01:00

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.

scarify NH3 /4

Laboratory of Liptakov - 21-8-2016 at 02:00

!!.....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.

kratomiter - 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.

MineMan - 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...

MineMan - 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?

PHILOU Zrealone - 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!

MineMan - 22-8-2016 at 10:04

Well I bought some copper oxide, but in the mean time (the 10 days it takes to arrive) I have attempted this preparation again, and used the crystals from last time, as they do turn into TACP when ammonia and copper is added. I have also used a copper wire ball/nest for more surface area and it seems to be working better, but I am still confused on a few things.

Is it necessary for constant stirring of the mixture like in LL's video?

What is the optimum temperature during the several hour duration for this reaction to take place?

Is an open lid necessary like in LL's video (he had a 2cm hole in the jar lid) for fresh air, because the ammonia evaporates off rather quickly and I would think that the AP provides the oxygen needed?

I will post some more pics later, for those that are on the edge of their seats!!

PHILOU Zrealone - 22-8-2016 at 11:18

You need air (O2) to allow for dissolution of the Cu!

The ammonia dissolves the "oxyd layer" (CuO, Cu2O, Cu(OH)2 and CuCO3) of the Cu metal...as the soluble complex Cu(NH3)4(OH)2 (deep blue); then the naked metal is reoxydised by the fresh air.

You also need agitation to allow for Cu pieces to come into contact with air (faster oxydation than with underwater diffusion)!

Try with euro-cents...it is iron-steel plated with Cu...add a little ammonia solution into a PE (polyethylen) bottle with the coins.
Don't put too much ammonia, but not too little eather...when the bottle lay down on the side the coins are into contact with air inside the bottle...when the bottle is straight the ammonia covers the coins.
Shake the bottle from time to time with a screw on top cap. If the bottle is hermetic...you will notice that it will depress (oxygen is consumed leaving N2; most ammonia remains into solution owing to its affinity for water and for the Cu(2+) complex).
From time to time allow fresh air to enter the bottle and to repressurize...so you get extra O2 for further oxydation and dissolution of the copper.
After a while (a few days/weeks) the ammonia will turn deep blue and the copper plated coins will become silvery and copper free.

[Edited on 23-8-2016 by PHILOU Zrealone]

kratomiter - 23-8-2016 at 08:48

I had success with very fine copper wires from electric cable, they were completely dissolved in less than 2 hours and now my TACP is pure.

Philou´s generator TACP

Laboratory of Liptakov - 23-8-2016 at 10:04

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.....:cool:...Dr.

What would one expect?

MineMan - 24-8-2016 at 08:10

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 620 times image_1.jpeg - 1.5MB

Other Picture

MineMan - 24-8-2016 at 08:17

Other pic :)

image.jpeg - 1.8MB

kratomiter - 24-8-2016 at 08:25

Maybe 1 cm thick iron is too much to make a hole in it, but 2.3 TACP at max density will go high order detonation for sure.
I detonated 2 grams of guanidine perchlorate with just 600 mg of TACP (unpressed, loose powder) in 6 mm copper tube against a thin aluminium plate (2 mm) and it made a big hole (>10cm).

TACP test

Laboratory of Liptakov - 24-8-2016 at 09:11

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...:cool:...Dr

PHILOU Zrealone - 24-8-2016 at 09:27

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]

MineMan - 24-8-2016 at 10:23

Philou and LL great information. Yes Philou you are right about the placement, the 6cm tube was placed laying down on the plate and it was initiated in the way you suspect for this this thought experiment.

The wax idea was stolen from a rouge science post by Rosco Bondine. It serves a variety of reasons I believe.
-Takes the oxygen balence from 14.5 to about 0
-Increases the ease of compressibility
-protects the product from moisture
- reduces the sensativity.

I was worried the my product may of not been full power in this thought experiment, as I remember several color changes during filtering, drying, and some loss of ammonia when the product was heated during the wax coating process.

Also, I would like to add, do not use small copper wire for making this product, as it will become smaller and little thin pieces are impossible to filter out from the product!

MineMan - 24-8-2016 at 10:33

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....

PHILOU Zrealone - 24-8-2016 at 13:38

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.:P:):D;)
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]

MineMan - 24-8-2016 at 15:21

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?

kratomiter - 24-8-2016 at 19:26

TACP is a primary, see BERTA detonator from Dr. Liptakov in Youtube.

TACP

Laboratory of Liptakov - 24-8-2016 at 23:15

Pure TACP is in order as primary explosive. However, this order, this array is large. TACP + Wax can be really in order secondary. Will be less sensitive than pure ETN. Same example is TACP + HMTA. Arises soft material with very low sensitive on friction and and low sensitive on impact. However for this mix, laboratory tests from some university or professional laboratory is impossible find. I mean, that not exist. ..Dr.

PHILOU Zrealone - 25-8-2016 at 05:31

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 1ary, 2ary or 3ary 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

kratomiter - 3-9-2016 at 11:51

Today I was playing with SADS to test its ability to initiate explosives. 45 mg of SADS in a plastic straw (3 mm diameter) fully detonated MHN, but not TACP.
I know one test isn't enough, but TACP seems quite unsensitive.

MineMan - 3-9-2016 at 17:16

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...

TACP

Laboratory of Liptakov - 4-9-2016 at 11:07

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.// ........:cool:......Dr.

MineMan - 4-9-2016 at 13:17

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

MineMan - 6-9-2016 at 11:36

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!

PHILOU Zrealone - 7-9-2016 at 13:51

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...

Aluminium is highly reactive towards Ag(+) but also towards Cu(2+)...because of the huge oxydoredox potential of the two following reactions:
Al(0) + 3 Ag(+) --> Al(3+) + 3 Ag(0) + heat
2 Al(0) + 3 Cu(2+) --> 2 Al(3+) + 3 Cu(0) + heat
So it is unwise to allow for a direct contact between the Al foil and the SADS ... or with the TAC(u)P.

The heat generated may induce spontaneous explosion of the SADS and initiation of the rest of the charge upon storage.
Beware that it is not because nothing seems to happen for a few minutes, hours or days, that the sneaky thermodynamic is not at work and unexpectedly reveals its true nature (one day it may remain stable, but the other it will explode).

PHILOU Zrealone - 7-9-2016 at 14:00

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" ;)

MineMan - 7-9-2016 at 14:38

Ahh, that is good to know that TACP should also not contact Al, as I was employing Al for an end plug of the tube... I now see one of the reasons we don't want metal molecules in explosives...in addition to dead weight.

stoichiometry, ok I will use the proper word from now on. Reactants are:
CuO
Ammonium Perchlorate
Ammonia 26-29%

Honestly, I don't even know where to start, chemical equations maybe... But how do I know if I am leaving out any intermediate reaction? Or does only the final product and initial ingredients count? It is also not only for optimization that I want to learn this... I don't want to use too much of a reactant and have it left over in the product...

PHILOU Zrealone - 7-9-2016 at 16:23

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 :D

Because this equation is not the simpliest to start with stoichiometry, I will help you a bit :):D;):P

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]

MineMan - 8-9-2016 at 10:02

Wow, Thank you PH Z!!!:o 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!:D;)

ttrzllvr - 12-9-2016 at 03:16

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


kratomiter - 12-9-2016 at 06:35

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?

CGP and CGC

Laboratory of Liptakov - 12-9-2016 at 11:23

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...:cool:

Berta Bickford.jpg - 158kB

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

ttrzllvr - 12-9-2016 at 21:43

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%.

ttrzllvr - 12-9-2016 at 22:12

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...:cool:


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


I have different methods and goals. My primary goals is STABILITY (in the natural environment of course, I'm not interested in some childish laboratory or urban conditions), YIELD (wasting precious perchlorates to unstable and low yield compounds kilometers and kilometers from the "civilization"? No, thanks), AVAILABILITY - "innocent" dietary supplements will be still available (or a homemade gelatine). But of course I'll do other tests I'm interested in.

[Edited on 13-9-2016 by ttrzllvr]

[Edited on 13-9-2016 by ttrzllvr]

[Edited on 13-9-2016 by ttrzllvr]

Laboratory of Liptakov - 13-9-2016 at 01:21

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.

ttrzllvr - 13-9-2016 at 05:16

I'll do some tests with cardboard and/or plastic tubes. Brass cases are so damn unpractical and potentially dangerous especially when filled with a compound from unknown territory.

[Edited on 13-9-2016 by ttrzllvr]

ttrzllvr - 13-9-2016 at 05:22

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 :D

MineMan - 13-9-2016 at 05:49

Ok. We look forward to the results.

Laboratory of Liptakov - 13-9-2016 at 07:18

Ok. We look forward to the results.

ttrzllvr - 16-9-2016 at 06:56

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.

Laboratory of Liptakov - 16-9-2016 at 12:22

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

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

ttrzllvr - 16-9-2016 at 13:00

I found maybe the cheapest (?) glycine in Europe
http://4fitness.cz/vyhodna-baleni-a-naplne-proteinu/lglycin-...

If someone knows any cheaper source, let us know please.

Glycine

Laboratory of Liptakov - 17-9-2016 at 07:43

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

PHILOU Zrealone - 17-9-2016 at 16:21

Beware to the stability of Cu(ClO3)2...
I have searched for infos about it and found very little.

Why did I searched?
I did inserted some Cu powder or Cu salts into KClO3/S/C mixes to get green-blue colour during burning but the mixes strongly released chlorine smell while the original chlorate black powder was stable for ages (with unsoluble carbonate or hydroxyde as acid scavenger) and smell-less...since the only added parameter was copper I suspected the crossed salt Cu(ClO3)2 to be potential cause of troubles...

ttrzllvr - 17-9-2016 at 21:58

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.

PHILOU Zrealone - 19-9-2016 at 02:23

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 ;):P:):
-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.

Laboratory of Liptakov - 19-9-2016 at 03:01

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

Rosco Bodine - 19-9-2016 at 09:02

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

Attachment: US3296045 Tris-glycine Strontium Perchlorate.pdf (295kB)
This file has been downloaded 784 times

[Edited on 9/19/2016 by Rosco Bodine]

ttrzllvr - 19-9-2016 at 12:15

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 ;):P:):
-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.

ttrzllvr - 24-9-2016 at 06:23

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.

PHILOU Zrealone - 25-9-2016 at 02:01

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?

ttrzllvr - 25-9-2016 at 21:26

Some photos of preliminary tests here
http://tetrazolelover.at.ua/index/energeticke_zluceniny_kyse...
Be careful with the Cu GLY-perchlorate too, seems it is able to detonate from black powder fuse even in paper tubes.

Laboratory of Liptakov - 27-9-2016 at 03:03

I recommend making mix PETN + Cu-Gly ClO4 (monohydrate) 1:1 behind use acetone and preparation the agglomerate 2x2 mm. And filling to plast or paper tube with cavity 6 - 8 mm. Should by detonate. Similarly as method on your pages. High pressed 0,25 g for output segmet. It is same as in system Berta. And 0,25g with low density about 50% crystaline. It should be brizant on target. However the plate 0,4 mm is very thin for measurement of detonators. If working this , must be in plate 2 mm thickness simply pure the hole. Minimal 4 mm of diameter. (from 0,25g brizant /mix) From detonator with cavity 6 mm. Dr.

[Edited on 27-9-2016 by Laboratory of Liptakov]

Peter Lustig - 30-9-2016 at 00:20

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]

system Berta

Laboratory of Liptakov - 30-9-2016 at 12:51

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....:cool:

PHILOU Zrealone - 30-9-2016 at 14:51

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]

Biuret might be interesting if able to coordinate/complexate...what is not sure because of its inherent acidity.
Do you have references for urea complexes? If yes then maybe biuret will do.
If it exists it would be Cu(BU)2(ClO4)2 with BU as H2N-CO-NH-CO-NH2 (or N3H5C2O2).
Cu(N3H5C2O2)2(ClO4)2 --> CuO + 3 N2 + 4 CO2 + 3 H2O + 2 HCl + H2

It would be more interesting to get the guanidine related biuret (H2N-C(=NH)-NH-C(=NH)-NH2) and that would for sure complexate strongly.

@Peter Lustig,
You wrote: "I have calculated, 6% Hexamin ist not enough for NH4 (Cu Hex2) (ClO4)3."
--> What do you mean by that, what have you calculated and enough for what?

Peter Lustig - 2-10-2016 at 01:16

I must korregieren, Biuren is harder than I thought. It forms the strong allkalischen a copper complex (biuret Wiki). Moreover, the production is not so simple.
I already have a new Ide, years ago I once dicyandiamide of fertilizer produced. This is simple and gives a clean product.With Chloratum there is a strong mix
For DCD there is information as a component in Exlposiv with strong oxidants as well as Lingant in complexes with oxidants. Patents for airbags. https://www.google.de/#q=dicyandiamid+komplex+patent
When I have time I will pursue the

I have enough guanidine nitrate, but it is not easy to produce free base. Another name for DCD is cyanoguanidine and thus very similar to the guanidine

My standard cap is 1,4g NHN with 0,1g SADS on top in a 223rem mag cartridge, but it is good to know alternatives....

In complex, the ratio of copper / hexamine 1: 1-2
TACP has 330,5g/mol 88g (88%) is 0,266mol Cu
Hex has 140g/mol 6g (6%) is 0,0428 mol Hex
0,266 / 0,0428 = 1 / 0,161 !!!
You get a mix of TACP and CHP ... what is good for the OB ...
https://www.degruyter.com/downloadpdf/j/znb.1981.36.issue-10...

ttrzllvr - 4-10-2016 at 23:03

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.


These, bis(biuret) perchlorate and chlorate compouds were prepared already years ago. If I remeber correctly, the Cu bis(biuret) chlorate is a pale bluish-green powder, poorly soluble in water, more a secondary than a primary, as I remember, its explosion was flashless. The perchlorate, blue crystals, was, I think, easily soluble in water and hygroscopic, but more energetic than the chlorate. But after years I'm not sure... I have still a bunch of biuret, maybe I'll try something again with it (especially I'm interested in aminobiuret through nitrobiuret). My method of its manufacture was similar to two methods in these patents:
US 2524049 http://www.freepatentsonline.com/2524049.pdf
US 3150177 http://www.freepatentsonline.com/3150177.pdf

A less known patent, maybe someone is interested in it (easily preparable, high performance aminoguanidine complexes with perchlorates, usable as powerful primary explosives, e.g. the nickel (II) di(monoaminoguanidine) perchlorate - 8175 m/s, 330 kbar at 90% of TMD, Trauzl test 39,6 cm3/g, min. initiating charge for PETN, less than 3 mg):
EP2450330 https://worldwide.espacenet.com/publicationDetails/originalD...

[Edited on 5-10-2016 by ttrzllvr]

PHILOU Zrealone - 7-10-2016 at 15:56

EP2450330 here http://www.freepatentsonline.com/EP2450330A2.pdf
or here http://www.freepatentsonline.com/DE102010050861A1.html

Rosco Bodine - 8-10-2016 at 22:22

Here is the patent EP2450330A2 and a machine translation to English


Attachment: EP2450330A2.pdf (436kB)
This file has been downloaded 594 times

Attachment: EP2450330A2 translation aminoguanidine complexed metal perchlorate initiators.pdf (55kB)
This file has been downloaded 846 times


MineMan - 9-10-2016 at 10:05

Huh, so they said that these could be used as a primary and a secondary explosive... I am guessing that would be achieved by pressing to different densities?

No data on friction sensitivity or the such though...

Seems like it could be pretty exciting though... Since I am not experienced in chemistry like some of the senior members on this forum, I don't want to be synthesizing a relatively unknown and unstudied compound. I will be an observer for now, until more tests are performed... but an excited observer.

Anyways, what I am saying is... hurry up chemistry gurus...and start experimenting, because 3mg for initiation of PETN is beautiful.

[Edited on 9-10-2016 by MineMan]

MineMan - 12-10-2016 at 13:51

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.....:cool:...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]

MineMan - 12-10-2016 at 21:33

Well,

I did this experiment and heated it up and let it sit in a hot water bath (near boiling) several times over several hours. I also added an extra 30ml of my ammonia, and an extra few grams of AP... because there was still copper oxide left.

Several hours later there was still copper oxide left, but I filtered it. The crystals are a very dark blue when wet (with the ammonia solution or the 91% alcohol used to filter) but when they dry they are a much paler blue... unlike my last batch...

Any ideas of what went wrong, it seems hard to get the really dark crystals (after drying)? Can anyone post pictures of their product so I can compare?

kratomiter - 14-10-2016 at 15:44

@MineMan Is your copper oxide lab grade? From my experience, pale blue TACP is due to lack of copper. Try dissolving some fine copper wire.
I'll post a photo tomorrow.

MineMan - 15-10-2016 at 15:59

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...:mad:

kratomiter - 16-10-2016 at 10:57

Your calculations seems to be right, are you sure your CuO is pure?
Fine copper wire dissolves quickly without agitation from my experience. I've never tried copper (II) oxide.

[Edited on 16-10-2016 by kratomiter]

TACP preparation

Laboratory of Liptakov - 16-10-2016 at 12:20

Here is easy method : all described...in video converter TeACP synthesis
https://vimeo.com/home/myvideos/page:2/sort:date/format:vide...

[Edited on 16-10-2016 by Laboratory of Liptakov]

Laboratory of Liptakov - 16-10-2016 at 12:40

Next method: Get 30g AP + 100g NH3 aq + 12g Cu wire dia. 1,5 mm into plastic 1,5 liter jar. Temperature increase on 35 C . Closing the jar. Shaking 5 minute. Open, get into the new air. And close again. Shaking, hold temperature in the bucket with water 50 C- for example. This procedure should by time about 30 - 60 minute. Decrease on zero or - 5 Celsia. Plast jar cutting and remove Cu wire, weight 1 - 3g. Other separe. Cut jar is possible using as the funnel. Yield should by minimal 30g dry TeACP.
Dr.

[Edited on 16-10-2016 by Laboratory of Liptakov]

MineMan - 17-10-2016 at 12:39

LL,

I don't think you understand my question... I have watched that video countless times... but I don't have a ball mill to put the container in to rotate it continually. My understanding is the container has to be shaken nearly constantly or every few minutes when copper metal is used...

I do not understand your answer, are you saying the reaction only needs an hour to complete at 50C...?

Isn't 100g of NH3 overkill, from stiochiomistry I calculated 40grams of 25% NH3?

kratomiter - 18-10-2016 at 07:26

The more concentrated the ammonia is, the quicker the salt is formed.

PHILOU Zrealone - 18-10-2016 at 13:28

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.....:cool:...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]

From previous long post:
---------------------------------------------------------------
2 NH4ClO4 + CuO + 2 NH3 --> Cu(NH3)4(ClO4)2 + H2O

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
-----------------------------------------------------------------
So
-NH3 = 14+3*1 = 17 g/mol
-NH4ClO4 = 14+4*1+35.5+16*4 = 117.5 g/mol
-CuO = 79.5 g/mol
-H2O = 18 g/mol
-Cu(NH3)4(ClO4)2 = 63.5+17*4+99.5*2= 330.5 g/mol

From my equation one see that:
2*117.5 g of NH4ClO4 = 235 g
1*79.5g CuO = 79.5g
2*17g NH3 = 34 g (or 136g 25% NH3)

So for each g of CuO, one needs 2.956 g NH4ClO4 and 1.710g NH4OH 25%...
In your case with 22g CuO, you would need 37.62g NH4OH 25% and 65.03 g NH4ClO4...You have thus a little more NH4ClO4 and a little less NH4OH than wished.
I don't think it would matter much.

Of course to get the complex, you need all CuO to be dissolved.
Maybe you need more NH4OH to fully dissolve the CuO and then evaporate back to lower volumer; or more exposure time and shaking at ambiant T°. The affinity of NH3 for Cu(2+) is very high (see high Kc constant of complexation).

Otherwise the only explanation is that your CuO is unpure and something else is present.

specialactivitieSK - 2-11-2016 at 02:01

Melting organic compound of copper with AP ?

PHILOU Zrealone - 2-11-2016 at 03:33

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]

Just as interesting and probably more powerful/sensitive...
Glycine nitrate/NH4NO3
or
Glycine perchlorate/NH4ClO4

PHILOU Zrealone - 2-11-2016 at 03:38

Quote: Originally posted by specialactivitieSK  
Melting organic compound of copper with AP ?

Why not!
Cu (II) trinitrophenate and NH4ClO4? :cool::D;):P
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...

specialactivitieSK - 8-11-2016 at 07:28

THX

specialactivitieSK - 8-7-2017 at 03:08

???

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

Laboratory of Liptakov - 8-7-2017 at 05:44

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

PHILOU Zrealone - 8-7-2017 at 06:33

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)


As exposed by LoL,
What is your question or claim about this?

???
Cu + HMTA + NH4ClO4 will not give TACuP/hexamine complex at a significant rate...
You need water, air and NH3 (or NH4OH) to get something significant at a significant speed.

Maybe that heating nano Cu powder with HMTA and NH4ClO4 will cause an explosion...but I'm not sure the copper is needed at all since HMTA diperchlorate is already an explosive on its own.

NH4 will not be formed into your equation
NH4 doesn't exist alone...it needs a counter anion because it is NH4(+)....
Maybe NH3 and H(+)...then the H(+) needs to be catched by O2 itself oxydizing the Cu to CuO (thus a discrete form of Cu(2+)).

CuO + HMTA + NH4ClO4 will indeed provide some TACuP/hexamine...if water is present.

Are you sure about your calculations?
What is the meaning of it?
You wrote "( 10+22+37 = 63+5.6)"
To me it is
69 = 68,6 (if the dot is not a multiplication point)
or 69= 93 (if the dot is a multiplication point)
Anyway both are wrong...

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