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Peter Lustig
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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]
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Laboratory of Liptakov
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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....
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite (2024)
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PHILOU Zrealone
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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?
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Peter Lustig
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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...
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ttrzllvr
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| 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.
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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]
"We are shaping the future - as we are able, as we need, as we want..." - Me
"Inventing is a relay race." - Me
"Try this, try that... Why don't try it yourself? I know what I need to try." - Me
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PHILOU Zrealone
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EP2450330 here http://www.freepatentsonline.com/EP2450330A2.pdf
or here http://www.freepatentsonline.com/DE102010050861A1.html
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Rosco Bodine
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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
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MineMan
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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]
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MineMan
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| 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]
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MineMan
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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?
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kratomiter
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@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.
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MineMan
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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...
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kratomiter
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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]
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Laboratory of Liptakov
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TACP preparation
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]
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite (2024)
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Laboratory of Liptakov
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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]
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite (2024)
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MineMan
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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?
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kratomiter
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The more concentrated the ammonia is, the quicker the salt is formed.
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PHILOU Zrealone
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| 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] |
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.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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specialactivitieSK
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Melting organic compound of copper with AP ?
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PHILOU Zrealone
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| 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
PH Z (PHILOU Zrealone)
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PHILOU Zrealone
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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...
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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specialactivitieSK
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THX
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specialactivitieSK
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???
Copper hexamine perchlorate : Cu + Hexamine + A.P.
Cu + C6H12N4 + 2NH4ClO4 = Cu (C6H12N4)(ClO4)2 + 2NH4
( 10+22+37 = 63+5.6)
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Laboratory of Liptakov
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And it is some question or some result how to make or how to counting before preparation ? ........LL
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite (2024)
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PHILOU Zrealone
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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...
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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