Sciencemadness Discussion Board - Copper GABA Perchlorate

Copper GABA Perchlorate

Bfitzy - 8-7-2017 at 11:15

While reading about how copper would complex with organic amines such as hexamine and glycine, decided to try something else. I had gamma-aminobutyric acid on hand and tried using that. The preparation was as follows:
To a weak solution of ammonia was added about 10g of ammonium perchlorate along with two copper electrodes. The cell was run for a few days at about 15 volts. Next was added approx. 3g of GABA(purchased from a health foods store for about $17/6oz). The cell was left to continue running for another day, after which dark blue crystals began collecting at the electrides. These crystals we're collected and dried, and confinement tests with a couple milligrams in Al foil showed a great deal of energy.

A friction and shock sensitivity test was performed with a hammer and around 100mg of CGAP (my current name for the compound: Copper GAba Perchlorate). Under no conditions could I get it to detonate.

Anyone with advice, thoughts, questions et cetera is encouraged to comment.

Rosco Bodine - 8-7-2017 at 12:01

Freeform betaine could be neutralized with HNO3 and to the stirred hot betaine nitrate solution added in portions NH4ClO4. Betaine perchlorate should crystallize out from a supernatant solution of byproduct NH4NO3.

TACP -CGAP

Laboratory of Liptakov - 8-7-2017 at 12:19

Tetraamine copper perchlorate (TACP) is good energetic material self. Without organics amines. But of course his properties are a better or even much better with fuel- amines with which an easy create complex and takes their to self crystals. One from best is amino-guanidine, but of course is possible using hexa - methylene - tetra - amine (hexamine) , glycine or some different orgnics amines. Preparation is usually pretty easy. In ammonia water (10 -15% conc.) , is added for example 10g dry TACP + 10g organics amine. Glass container is closured and heated in water bath on 60 C to dissolving both compounds. Right setting of ratios, same as ratio against ammonia water is necessary set for best yield (from crystallisation) and properties of EM. But TACP takes organics amines into main complex always and easy. With hexamine is it confirmed in large span of ratios for example 2: 1 or 1:2. And result of properties are same. And the span conc. of hydroxide 10 - 25%. This is also your case. Works it almost self - auto - reaction. Dont forget, that this solution is Schweizer reagent. He also dissolves all organics compounds. Therefore is impossible for separation using paper filter. (contamination organics). And what. Your CGAP making some work ? Making the holes into steel ? Or some so something ? ..... :cool:

...LL

Rosco Bodine - 8-7-2017 at 12:21

TACP decomposes on dissolution into plain water. For what I was describing using betaine, no copper is needed for complexation, as the plain amine perchlorate by itself is interesting.

[Edited on 7/8/2017 by Rosco Bodine]

Laboratory of Liptakov - 8-7-2017 at 12:53

Our the answers (on GABA perchlorate) was walk cross over self in a short time.

Bfitzy - 8-7-2017 at 13:43

Have not had a chance to test it's effectiveness against steel. Unfortunately it is rather hot and dry where I live this time of year. Although I have worked with general pyrotechnic compositions and flash powders before, I have no experience with high explosives. What are some good methods for testing the substance? I.e. simple ways to make detonators/blasting caps with it?

Bfitzy - 8-7-2017 at 13:49

Also I'm working with what I have on hand which isn't a ton. As I said GABA was the only amino acid on hand. Speaking of, is there anything else copper will complex with other than nitrogenous substances? Right now I am mostly limited to copper Perchlorate salts and I don't have any hexamine.

Laboratory of Liptakov - 9-7-2017 at 00:14

On S-M is enough the study material how make detonators. If you will study threads and themes about it, early you will know enough, how to make any detonator and how to testing. Studing is much safetely, than testing without knowledge. And according your questions, you need firstly study a lot threads. Again I repeat. TACP is a good EM alone of self. Without anything. But his oxygen ballance is great + 14,5. Therefore is possible use practically any fuel 1- 10 %. Accordingly OB. Cellulose, any nitrocellulose, hexamine, flour, sugars, alcoholic sugars, carbon, sulphur, black powder, shotgun powder, oil, polyisobutylene, caramel and a lot next.
Result: Exploded it always..... :cool:

...LL

Laboratory of Liptakov - 9-7-2017 at 06:16

Here you can study how seems the holes from different mixtures. Even also diethylene glycole is possible use as fuel for TACP. And results are in basically identical against hexamine + TACP / called CHP. Slightly difference is, that CHP has the hole sharp edges from bottom, thus higher pressure of detonation. But diameters are identical. Conditions of tests are of course identical for all 3 attempts. Dr.

[Edited on 9-7-2017 by Laboratory of Liptakov]

PHILOU Zrealone - 9-7-2017 at 09:43

Quote: Originally posted by Bfitzy

While reading about how copper would complex with organic amines such as hexamine and glycine, decided to try something else. I had gamma-aminobutyric acid on hand and tried using that. The preparation was as follows:
To a weak solution of ammonia was added about 10g of ammonium perchlorate along with two copper electrodes. The cell was run for a few days at about 15 volts. Next was added approx. 3g of GABA(purchased from a health foods store for about $17/6oz). The cell was left to continue running for another day, after which dark blue crystals began collecting at the electrides. These crystals we're collected and dried, and confinement tests with a couple milligrams in Al foil showed a great deal of energy.

A friction and shock sensitivity test was performed with a hammer and around 100mg of CGAP (my current name for the compound: Copper GAba Perchlorate). Under no conditions could I get it to detonate.

Anyone with advice, thoughts, questions et cetera is encouraged to comment.

You have Something moderately energetic because you have the perchlorate, the copper and complexating fuel...

Sadly is your fuel too present in proportion...as such overfuelled composition burns slower/deflagate less and detonates with much more difficulty...

Long story short...Oxygen Balance (OB) is too negative...

GABA is H2N-CH2-CH2-CH2-CO2H...(or C4H9NO2)
The NH2 is far enough from the acidic CO2H group to be basic enough and complexating....

1 mole C4H9NO2 needs 5,25 moles O2 to fully burn to H2O, N2 and CO2
2 C4H9NO2 + 10,5 O2--> 8 CO2 + 9 H2O +N2

Cu(ClO4)2 only afwords 4 O2 per mole or 3,5 O2 and 1 of Cl2
Cu(ClO4)2 --> CuCl2 + 4 O2
Cu(ClO4)2 --> CuO + 3,5 O2 + Cl2

Assuming the complex is tetracoordinated
Cu(H2N-C3H6-CO2H)4(ClO4)2
you have thus 4 GABA (that would need 4*5,25 O2 = 21 O2 to fully burn) for one Cu(ClO4)2 (that can only afword 4 O2)
==> You are thus lacking a lot of oxygen hence the crappy energetic results.

Working with lower molecular (less carbonaceous) amino acids will be beneficial...
Optimum being aminoglycollic acid H2N-CH2-CO2H (amino-acetic acid/glycine or if it was stable carbamic acid H2N-CO2H)...thus bringing OB from very negative to closer to zero balance.

Working with multiple complexating amino groups into a single molecule is also a way to reduce the amount of aminated molecules into the complex and thus the fuel % into the complex.
Cu(H2N-CH2-CH3)4(ClO4)2 = Cu(C2H7N)4(ClO4)2 = CuCl2N4O8-C8H28
Cu(H2N-CH2-CH2-NH2)2(ClO4)2 = Cu(C2H8N2)2(ClO4)2 = CuCl2N4O8-C4H16

BTW all your complication to use lectrodes and 15 volts are useless...eventually you may decompose the GABA by oxydation and lose its NH2 via oxydation products.

If you don't have access to commercial ammonia... hint...make your own from own human body production ;-)
==> urea hydrolisis afwords 2 equivalents of ammonia ;-)

[Edited on 10-7-2017 by PHILOU Zrealone]

Laboratory of Liptakov - 9-7-2017 at 11:12

In urea (piss) you have even derivates of guanidine 0,01%. But main is making NH3 from urea. Nice process. Only insert some heated energy. All others is free and very cheap. Best is a morning urea with a high concentration. I hope, that ammonia water will free available buy still a long times....

...LL

[Edited on 9-7-2017 by Laboratory of Liptakov]

Bfitzy - 9-7-2017 at 12:03

PHILOU, +1 on your post, that was really helpful. However, I am keeping my oxygen balance higer in the overall composition by having a large excess of TACP in the product, just like LL's CHP. I already know that I probably added way too much GABA. I did not take the time to measure out molar ratios. I can do the work balancing the equations, but I am just not super familiar with how the tetraaminecopper complex interacts so I decided against that at this point.
Keep in mind that there is also a significant conc of AP still in the powder. Recrystallizing TACP is a little wasteful so there's still leftover reactants slowing it down some.

Bfitzy - 9-7-2017 at 12:08

Here's a picture of the fractionally crystallized product.

Laboratory of Liptakov - 9-7-2017 at 13:21

If has something create a quality cocrystal (fuel- TACP) or even a new energetic compound, is necessary that was a both reagents in solution complete dissolve. Regardless on losses. Thats normal, even in proffesional description are yields for example only 70% on insert TACP. Therefore will your yield worse. And without counting still worse. For example only 30% on inserted reagents. I see a lot the excuses. Dot.

PHILOU Zrealone - 10-7-2017 at 02:33

Quote: Originally posted by Bfitzy

PHILOU, +1 on your post, that was really helpful. However, I am keeping my oxygen balance higer in the overall composition by having a large excess of TACP in the product, just like LL's CHP. I already know that I probably added way too much GABA. I did not take the time to measure out molar ratios. I can do the work balancing the equations, but I am just not super familiar with how the tetraaminecopper complex interacts so I decided against that at this point.
Keep in mind that there is also a significant conc of AP still in the powder. Recrystallizing TACP is a little wasteful so there's still leftover reactants slowing it down some.

Fore composition sake ...would be more beneficial to make:
-"pure" dry TACuP
-"pure" dry TGABACuP
- and to mix it into desired ratio.

Why?

I'm affraid that mixing radomly TACuP/ GABA/AP composition will result in unknown compounds...that sadly are all in comparable shades of blue...thus difficultly discernable without due chemical analysis...

GABA is also not the simplest complexation agent to use because it can interact with itself as a zwiterionic species thus its carboxylic acid group blocking/interracting strongly with its own basic amino group...

Also keep in mind that at a discrete level all those reactions are in fact dynamic equilibrii complexations, precipitation, acido-basic reactions.

1°) you may have cocrystallisation but in what %?

2°) you may have only one of the components that is dropped out because it's solubility product is lower than the other...

3°) you may have complex complexation fight...thus GABA expelled in favor of NH3 or the contrary

4°) you may have internal self complexation of Cu(2+) gamma-amino butyrate ==> Cu(O2C-CH2-CH2-CH2-NH2)2
The two NH2 folds onto the Cu(2+) metallic core thus yielding a cycloheptaring (°-Cu-O-C-C-C-C-N-°)
Then there are two complexating sites eventually available for two GABA..
==> Cu(°)2(GABA)2(-O2C-C3H6-NH2°)2 (the ° is to show the complexation link)

5°) You may have unclear transition complexes...precipitating alone or mix thereof
Cu(NH3)4(ClO4)2
Cu(NH3)3(GABA)(ClO4)2
Cu(NH3)2(GABA)2(ClO4)2
Cu(NH3)(GABA)3(ClO4)2
Cu(GABA)4(ClO4)2
Cu(°)(NH3)3(ClO4)(GAB°)
Cu(°)(NH3)2(GABA)(ClO4)(GAB°)
Cu(°)(NH3)(GABA)2(ClO4)(GAB°)
Cu(°)(GABA)3(ClO4)(GAB°)
Cu(°)2(NH3)2(GAB°)2
Cu(°)2(NH3)(GABA)(GAB°)2
Cu(°)2(GABA)2(GAB°)2

6°) you may have internal migration of the perchlorate anion to the amino group...
Usually the stronger acid tries to bond to the stronger base (yeah natural selection/mating at molecular level ( :cool:

)
So it is well possible that
Cu(H2N-C3H6-CO2H)(ClO4) <==> Cu(O2C-C3H6-NH2) + HClO4 <==> Cu(O2C-C3H6-NH3ClO4)
(here I have left aside the rest of groups to allow for a better visual understanding of the problem)
So the cabroxylic acid attacks the Cu core to make a carboxylate and set at the sametime some HClO4 free that then is ready to attacks the NH2 basic group to make an organic amine perchlorate...

Bfitzy - 11-7-2017 at 13:26

I finally decided to just buy hexamine and glycine. I may continue with this path later, but I will seriously consider a simple mix of TACP and TGABACuP. Thank you for your advice, that was all incredibly helpful information. Hopefully once I take some organic chemistry classes in college I'll have a little better understanding of how complexation works. And PHILOU, you're totally right because in all my batches I'd get a ton of color variance as well as super unpredictable sensitivities.

Rosco Bodine - 12-7-2017 at 00:05

Betaine or TMG (trimethylglycine) is cheap about twenty bucks a kilo

http://www.sciencemadness.org/talk/search.php?token=&src...

http://www.sciencemadness.org/talk/viewthread.php?tid=4176&a...

http://www.sciencemadness.org/talk/viewthread.php?tid=4176&a...

http://www.sciencemadness.org/talk/viewthread.php?tid=6334&a...

PHILOU Zrealone - 12-7-2017 at 02:57

Quote: Originally posted by Rosco Bodine

Betaine or TMG (trimethylglycine) is cheap about twenty bucks a kilo

http://www.sciencemadness.org/talk/search.php?token=&src...

http://www.sciencemadness.org/talk/viewthread.php?tid=4176&a...

http://www.sciencemadness.org/talk/viewthread.php?tid=4176&a...

http://www.sciencemadness.org/talk/viewthread.php?tid=6334&a...

Sole problem with betain is its high carbonaceous counterpart vs the single nitrogen...
(CH3)3N-CH2-CO2H is comparable to (CH3)4N + CO2
Thus nearly same OB as tetramethylammonium salts...

Would be nice to bring some oxygen providing groups into the side carbonaceous chains or to get more oxygen containing anions than ClO4(-) and C(NO2)3(-)...in a way to get closer to 0 OB...
==> pentanitroethan anion (-)C(NO2)2-C(NO2)3 (= C2N5O10)...thus afwording 6 active O atoms per anion instead of 4 for perchlorate or nitroformiate
==> ((O2N)3C-CH2-CH2)3N-CH2-CO2H (tris-trinitropropyl-glycine)
==> etc.

Another possibility is to concantenate the side arms thus taking H atoms away...and providing more relative oxygen to burn the rest...
HO2C-CH2-N(-CH2-CH2)3N-CH2-CO2H
Each HO2C-CH2-N(CH2)3 units may keep one oxoanion...
==> 3 less H atoms per unit

Thus if you get the idea a DABCO related bis-betaine diperchlorate, dinitroformiate or dipentanitroethanate

[Edited on 12-7-2017 by PHILOU Zrealone]

Bfitzy - 14-7-2017 at 16:15

So, PH Z, what would you recommend as the best? Grainger does sell sodium azide for about $60/250G, but that's a little pricey. I bought hexamine and glycine, but is there just something simple I should stick with instead? I'd rather stay away from common organonitrate explosives because I dislike having the FBI knocking on my door.

PHILOU Zrealone - 15-7-2017 at 01:34

Quote: Originally posted by Bfitzy

So, PH Z, what would you recommend as the best? Grainger does sell sodium azide for about $60/250G, but that's a little pricey. I bought hexamine and glycine, but is there just something simple I should stick with instead? I'd rather stay away from common organonitrate explosives because I dislike having the FBI knocking on my door.

I'm not a FBI nor USA specialist...but I think that no real matter the type of energetic material/explosive you do (make/synthetize) or handle...(depends onto local legislation/regulations)...they might sooner or later knock onto your door...

Depends strongly onto your behaviour, potential treat to the society, Noisyness/stinkyness/dnagerousness for neighbourghood, quantities involved...

*********************

250g for 60 dollars...that is not too expensive...and it may allow you some primaries fun for years...if you don't work on too big quantities at the time.

Nice glycine and hexamethylenetetramine are very nice acquisitions for a home chemist...

Hexamine
--> dinitrate, diperchlorate, dinitroformiate
--> N,N', N"-trinitroso-cyclo-hexa-triamine (R-salt)
--> RDX/HMX
--> energetic perchlorate complexes HCuP (CHP) for example
--> binary mixes with chlorates/nitrates/nitrites of alkalies or amine nitrate, perchlorate...

glycine
--> nitrate, perchlorate, chlorate(?), nitroformiate
--> energetic complexes nitrate, perchlorates, chlorates (?)
--> binary mixes with chlorates(?)/nitrates/nitrites of alkalies or amine nitrate, perchlorate...

[Edited on 15-7-2017 by PHILOU Zrealone]

Laboratory of Liptakov - 15-7-2017 at 09:07

Quote: Originally posted by Bfitzy

You can be almost sure, that this forum is under 24 Hrs monitoring. But important is sentence, what Philou described. It depends on your behavior. On types of your questions and similarly. If you will rummage again and again only in 1g of anything during a few years and bring here positive informations, nothing knocking on your door. If you put here a question how to make 1 Kg TATP, knocking will during 24 Hrs.... :cool:

...LL

Bfitzy - 15-7-2017 at 13:33

Well that's my whole reasoning behind wanting sodium azide as a precursor to silver and lead azide. I need only minute quantities to set other things off compared to stuff like CHP.
I have to do a lot of stuff at my house, and even though I have been doing pyro in my backyard for 3 years and have never had a complaint from my neighbors, I'd rather not take chances. I have other places I can go to do bigger tests, but that's not my end goal.

Bfitzy - 16-7-2017 at 00:51

So as far as initiators go... Would this work as a shaped charge? And yes I can make stuff with things other than plastic. Would this in theory work or would the way that explosives work not do that

Bfitzy - 16-7-2017 at 00:53

Also I took the time to draw out what I believe the copper glycine Perchlorate complex looks like. I am becoming quite the fan of it.

[Edited on 16-7-2017 by Bfitzy]

PHILOU Zrealone - 16-7-2017 at 03:40

@Bfitzy,
Your pictures are of low quality...and hard to read maybe need some improvement...

==> Hint, use Paint program from Windows or equivalent drawing program (that allows for beautiful colored geometrical drawing with text...) and once done...(make a copy of the drawing under another name and convert from bmp to jpeg (so you have original in the case you need to make modifications into the drawing or in the case you need the same kind of drawing for another drawing))....

;-)...I'm not strong enough at chinese or japanese

...but I think I was able to read "Shockwave"

"Also I took the time to draw out what I believe the copper glycine Perchlorate complex looks like."
Except for quality of the drawing/picture...it is nice... but glycine is amino-acetic acid (H2N-CH2-CO2H) and not 3-amino-propanoic acid (H2N-CH2-CH2-CO2H)...thus one carbon too much

...
To write simplified molecular drawings requires extreme care because to add an extra (or to forget a) carbon atom happens quite easily...

[Edited on 16-7-2017 by PHILOU Zrealone]

Bfitzy - 16-7-2017 at 04:32

Forgive me' I've been up 20 hours straight so far and I was working with what I could pull together lol

Laboratory of Liptakov - 16-7-2017 at 08:56

Only for information, was tested TACP in crystallisation process 1:1 with guanidine nitrate. Result are crystals (blue) without detonatable properties.
Also was tested nitroguanidine in a same process. Result are difficulty fibre -
filling energetic material, which has detonatable properties. However about 30% weakly, than pure TACP. And about 40% weakly than CuHP in same others conditions.... :cool:

...LL

PHILOU Zrealone - 16-7-2017 at 12:41

Quote: Originally posted by Laboratory of Liptakov

Only for information, was tested TACP in crystallisation process 1:1 with guanidine nitrate. Result are crystals (blue) without detonatable properties.
Also was tested nitroguanidine in a same process. Result are difficulty fibre -
filling energetic material, which has detonatable properties. However about 30% weakly, than pure TACP. And about 40% weakly than CuHP in same others conditions.... :cool:

...LL

Try with guanidine perchlorate (GP) instead of GN and NQ and all your problems will be resolved...

Guanidine perchlorate is a powerful and sensitive HE...
(H2N)2C=NH.HClO4 --> HCl(g) + CO2(g) + 2 H2O(g) + 1/2 H2(g)

Same must be true with guanidine-copper (II) perchlorate...
Cu((H2N)2C=NH)2(ClO4)2 (bis-guanidino-copper perchlorates BGCuP...

BGCuP must be better performing than TACuP and equally or better than HCuP...

Introduce guanidine or guanidine hydrate into a solution of Cu(ClO4)2...if the complex doesn't precipitate on its own...add cold ethanol and eventually ether (diethyl-ether)...

NQ (nitroguanidine) may be used as its salt...
H2N-C(=NH)-NH-NO2 + NaOH --> H2N-C(=NH)-N(NO2)Na + H2O

Copper nitroguanidinate must me a primary or D2D compound...
H2N-C(=NH)-N(NO2)Na (aq) + CuSO4 (aq)--> Cu(N(NO2)-C(=NH)-NH2)2 (s) + Na2SO4 (aq)

Aminonitroguanidine (H2N-NH-C(=NH)-NH-NO2) must be interesting compound for complexation of Cu perchlorate or as its perchlorate; nitroformiate or nitrate salts admixed with TACuP or HCuP...
==> Cu(ANG)2(ClO4)2, Cu(ANG)3(ClO4)2 or Cu(ANG)4(ClO4)2
==> ANG.HNO3, ANG.HClO4, ANG.HC(NO2)3; the first is a very powerful HE...no doubt the perchlorate will be even better and the nitroformiate arround the perchlorate.

Would be nice to test nitroformiate as anion with copper and related complexes
TACuNF (Cu(NH3)4(C(NO2)3)2)
HCuNF
BGCuNF
MANGCuNF, BANGCuNF or TANGCuNF (if mono, bis or tetra complexes)

Laboratory of Liptakov - 16-7-2017 at 13:09

I am only soldier on chemical field. I have only guanidine nitrate and nitroguanidine. I do not know, how from this making guanidine perchlorate. Of course, that I have NH4ClO4 and TACP. Your brilant a huge source and all options are for my almost incomprehensible. So much equation. But I know, that making aminoguanidine carbonate is pretty difficult from nitroguanidine. Thus, how to make guanidine perchlorate from entire description is for me incomprehensible. Any way, thanks for all........... :cool:

...LL

PHILOU Zrealone - 16-7-2017 at 15:11

Quote: Originally posted by Laboratory of Liptakov

I am only soldier on chemical field. I have only guanidine nitrate and nitroguanidine. I do not know, how from this making guanidine perchlorate. Of course, that I have NH4ClO4 and TACP. Your brilant a huge source and all options are for my almost incomprehensible. So much equation. But I know, that making aminoguanidine carbonate is pretty difficult from nitroguanidine. Thus, how to make guanidine perchlorate from entire description is for me incomprehensible. Any way, thanks for all........... :cool:

...LL

Yes sorry...a lot of chemistry...but hard to speak about this without equations...

Guanidine perchlorate is very very soluble into water and hard to dehydrate...
It can be made from:
Guanidine chloride + sodium perchlorate --> NaCl + GP
This means that solubility of Guanidine Perchlorate > Guanidine Chloride /Sodium Perchlorate > Sodium Chloride.

It can be made alternatively from:
Guanidine carbonate / NH4ClO4 --mild heating --> GP + CO2(g) + NH3(g)
Guanidine carbonate / HClO4 --> GP + H2O + CO2(g)
Guanidine carbonate + Cu(ClO4)2 --> CuCO3(s) + GP (precipitation of CuCO3)
Guanidine / HClO4 --> GP + H2O
Guanidine / NH4ClO4 --> GP + NH3(g)

How to make guanidine...
Guanidine nitrate + KOH --> KNO3(s) + Guanidine (hydrate/hydroxide)
Guanidine nitrate + NaOH --ethanol--> NaNO3(s) + Guanidine
Guanidine nitrate + dilluted H2SO4 --heat/vaccuum distill--> Guanidine sulfate + HNO3 (g)
Guanidine sulfate + Ba(OH)2 or Ca(OH)2 --> Guanidine + BaSO4 or CaSO4 precipitate.
....

Laboratory of Liptakov - 16-7-2017 at 23:33

1) Well, from entire is easy Guanidine nitrate + NaOH --------in ethanol--------NaNO3 (will soluble in ethanol ) + Guanidine will precipitate in ethanol ? Pure Guanidine is unstable I mean. OK, can stay as precipitat in ethanol 2x washing.
2) Guanidine as porridge in ethanol mixing with NH4ClO4. Heating on 78 C and try, what happends.
3) Guanidine as porridge in ethanol mixing with NH4ClO4. Mixing ethanol with water 1:1 and heated on 80 C and waiting what happends.
4) .....If happend nothing, All pour into toilet......... :cool:

..........LL

PHILOU Zrealone - 17-7-2017 at 03:36

Quote: Originally posted by Laboratory of Liptakov

1) Well, from entire is easy Guanidine nitrate + NaOH --------in ethanol--------NaNO3 (will soluble in ethanol ) + Guanidine will precipitate in ethanol ? Pure Guanidine is unstable I mean. OK, can stay as precipitat in ethanol 2x washing.
2) Guanidine as porridge in ethanol mixing with NH4ClO4. Heating on 78 C and try, what happends.
3) Guanidine as porridge in ethanol mixing with NH4ClO4. Mixing ethanol with water 1:1 and heated on 80 C and waiting what happends.
4) .....If happend nothing, All pour into toilet......... :cool:

..........LL

Guanidine is soluble into ethanol just like NaOH while NaNO3 must be relatively unsoluble....sole unknown is solubility of guanidine nitrate...but if it is not soluble into ethanol...one may start into water...
1°) NaOH + Guanidine nitrate into minimum water quantity at ambiant T°--> NaNO3 + guanidine hydrate
Maybe NaNO3 will already start to precipitate.
2°) Add Ethanol to precipitate even more NaNO3

Procedure will work better with KOH since KNO3 is much less soluble into water and ethanol than NaNO3

.
Take the solid away by filtration and wash with a little cold ethanol.

You thus have a guanidine hydrate solution into water/ethanol...
==> that you can use to complexate Cu(ClO4)2...or other complexing metal salts (nitrate, chlorate, iodate, bromate, perchlorate, nitroformiate, nitramide, dinitramide,...of Cu, Co, Cd, Zn, Fe, Ni, Cr, ....)
==> that you can exchange ligand with Cu(NH3)4(ClO4)2 (TACuP)...
Guanidine is a stronger base than NH3 and it is less volatile so NH3 will be kicked off the solution and off the complex and be replaced by guanidine...
Good venting is needed for the NH3 (or allow to flow into an acid containing recipient to recover the NH3...HNO3? --> NH4NO3) or recycle into another TACuP process

==> that you can allow to react with an ammonium salt to displace NH3....
NH4ClO4 will provide Guanidine perchlorate and NH3 gas...
If heating is done...better stay onto the low heat...

I have had deliquescent moist hydrazine perchlorate (200 mg)(what must be quite similar to GP) detonating onto a thick stainless steel dessert spoon while heating it onto a mild cooking flame...the spoon had a notch onto the side and was twisted into a loop (I was holding it) but the shock was so strong I couldn't hold it and it lifted into the air spinning at high speed...of course ears ringing, flame blown off. :cool:

...that was younger time fun...hopefully without damages other than the spoon

[Edited on 17-7-2017 by PHILOU Zrealone]

Laboratory of Liptakov - 17-7-2017 at 05:17

Huhaha...200mg destroyed the spoon ? In hands ? Flying spoon? Twisted into the loop ? Fantastic attempt. I consider a great Hero. If you survived with all parts ./.
Well, is time for try something from description.....God with us.......

.....LL
Thanks for all.... :cool:

[Edited on 17-7-2017 by Laboratory of Liptakov]

symboom - 17-7-2017 at 14:57

This thread makes me want to spend time around the vitamin shelf
Thinking of combinations with other amino acids

Also for glycine
Technical grade glycine is sold for use in industrial applications; e.g., as an agent in metal complexing and finishing.

Glycine
GABA
Lysine
Serine

The essential amino acids are histidine, isoleucine, leucine, lysine, methionine, phenylalanine, threonine, tryptophan, and valine

In contrast, non-proteinogenic amino acids are amino acids that are either not incorporated into proteins (like GABA, L-DOPA, or triiodothyronine)

Maybe a amino acid that has a close stucture as glycine
Could make other double salts or complexes

Complex salts of nickel and copper lysine perchlorate was attempted no percipitation

potential semiorganic material was synthesized from the amino family, and single crystals of l-leucinium perchlorate (LLPCl) were grown by slow solvent evaporation at room temperature. From single-crystal XRD, it was found that LLPCl crystallizes in a monoclinic system.

recently synthesized iodates of arginine and lysine,
The paywall wont let me read it

[Edited on 18-7-2017 by symboom]

[Edited on 18-7-2017 by symboom]

[Edited on 18-7-2017 by symboom]

[Edited on 18-7-2017 by symboom]

Laboratory of Liptakov - 18-7-2017 at 09:27

Perchlorates with metal and organic amines are a large way. Huge the tree with a lot a branches and hundreds of flowers, inflorescences. And some from them are great a new energetics materials, which waiting on self own the discovery..... :cool:

...LL

PHILOU Zrealone - 18-7-2017 at 13:03

Quote: Originally posted by Laboratory of Liptakov

Perchlorates with metal and organic amines are a large way. Huge the tree with a lot a branches and hundreds of flowers, inflorescences. And some from them are great a new energetics materials, which waiting on self own the discovery..... :cool:

...LL

LoL is not only an energetic researcher but also a poet

Laboratory of Liptakov - 19-7-2017 at 05:52

I seems, that Copper guanidine nitrate is possible transformed directly on Copper guanidine perchlorate. Results from detonators, respectively from output segments, show on better results, than Copper hexamine perchlorate. Pure ETN is of course slightly better. However, if anyone hasn´t hexamine and HNO3, is it good way, how making something, what will works. NH4ClO4 is condition always. Also is researched nitroguanidine, also he show a interesting properties. Entire is it only a start of research of the filed of the copper perchlorates, with the guanidine. Unfortunately this substance require yet classic primary 300mg charge. Against CuHP, which works always in solid cavity as mono material.
Details will describe later..... :cool:

....LL

[Edited on 19-7-2017 by Laboratory of Liptakov]

PHILOU Zrealone - 19-7-2017 at 10:59

Quote: Originally posted by Laboratory of Liptakov

I seems, that Copper guanidine nitrate is possible transformed directly on Copper guanidine perchlorate. Results from detonators, respectively from output segments, show on better results, than Copper hexamine perchlorate. Pure ETN is of course slightly better. However, if anyone hasn´t hexamine and HNO3, is it good way, how making something, what will works. NH4ClO4 is condition always. Also is researched nitroguanidine, also he show a interesting properties. Entire is it only a start of research of the filed of the copper perchlorates, with the guanidine. Unfortunately this substance require yet classic primary 300mg charge. Against CuHP, which works always in solid cavity as mono material.
Details will describe later..... :cool:

....LL

[Edited on 19-7-2017 by Laboratory of Liptakov]

Nice first results...thank you for the infos ...

That was fast...only 2 days...we write, you read, you understand, you design experiment, you experiment and already results ...Hat down...bravo.

I think I know who you are...but I can keep a secret...(The Flash

)

symboom - 19-7-2017 at 11:26

Hexamine Nickel perchlorate burns like black powder Copper hexmethyltetramine perchlorate burns some where in the middle of flash powder and black powder copper guanidine perchlorate sounds interesting seems like it is not as reactive and needs a boosted from what I understand a simple flame wont ignite it same with guanidine nitrate ammonium nitrate and hexamine nitrate which burns as the only. One would think because it has a fuel and a oxidizer it would be flammable and burn

[Edited on 19-7-2017 by symboom]

[Edited on 19-7-2017 by symboom]

Laboratory of Liptakov - 19-7-2017 at 13:47

Results well, thanks for the Hat....:-).....Relevant results require a lot attempts. Important is testing in solid cavity behind a same conditions. Thus for example, output segment by standard conditions (For ETN 500mg Hi pressed) give diameter hole ( into 2mm steel plate) 8,2 mm with a short and pretty sharpnes edges.
It is reference hole for comparation. Guanidine or hexamine "salts" give diameter 7,2 mm. Well, if is all right. Sometimes is hole from guanidine "salts" only 5,2. But it same pay for hexamine " salt". Thus according last attempts, are results not clear, what is own better. However, Nitroguanidine is possible mixed with TACP under ethanol for example in ratio NG 25 /TACP 75 and this, relatively heterogenous (fibrous) mix has D2D properties. And better output parameters than pure TACP. But worse than CuHP. Behind absence hexamine, is thus possible experimentation with salts on guanidine base. But if someone can prepared guanidine nitrate (nitroguanidine) so also can relatively easy preparation also hexamine. According all, is hexamine - TACP still better than guanidine - TACP. Aminoguanidine was not try, also same glycine. Of course, almost all, what is reactive fuel, can be mixed in stechiometry with TACP and results will almost always better, than pure TACP. But basic conditions are testing in solid cavity, not burning on air only. Burning test (at this compounds) showe nothing about they detonation parameters.....Dr.

PHILOU Zrealone - 19-7-2017 at 17:16

True...ignition and flame propagation in the open is only one aspect of the properties of a compound...
The effect of ignition under confinement (multiple aluminium foil layers or detonator casing) will reveal deflagration or even detonation power...

Typical examples are:
-nitrocellulose...what burns a bit like black powder in the open but deflagrates or detonates once confined...
-Nickel hydrazine nitrato complex (NiHN) what burns fiercely into the open but deflagrates or detonates strongly once confined a little...

Laboratory of Liptakov - 20-7-2017 at 13:39

Last tests show, that Tetraamine copper perchlorate with hexamine gived best results as D2D mixture against mixtures with guanidine nitrate or nitroguanidine. Therefore is in vain here explained entire variants, what all was tested with guanidine - TACP. Yet, that on air his mixtures show pretty fast burning, more fast than CuHP. In solid cavity are his properties always weaked, than any mixtures TACP - hexamine. Therefore I here describe basic preparation CuHP, respectively Tetraamine copper perchlorate - hexamine clathrate.
10g TACP + 10g hexamine is dissolved in 50g ammonia water 25%. (Ammonium hydroxide 25% in aq.) In closure jar is temperature increase on point of boiling to dissolving both compounds. Or behind use reflux cooler without any cover cap. Instantly after dissolving stop heating. Cooling should by take of about 3 hours from +60 C to - 5C.

Important: For separation crystalls is impossible use paper filter, which is destroyed during a few seconds. Solution is Schweizer reagent and decompose all organics materials. You use Buchner or very fine stainless sieve of eyes 0,1 - 0,05 mm. Or synthetic the cloth.

Yields should by 10g CuHP. Water filtrate is possible recycled on hexamine, NH4ClO4 and CuO. Solution simply boiled to dry. All compounds is possible use directly with next charges, respectively dry mix is counting and insert as hexamine 7-9g. Small amount AP + CuO is not necessary re-counting. Thus, for next charge is added only 1g pure hexamine, 9g old, and 10g TACP. Evaporate on glass, ceramic, not on stainless plate, which is reactive during hard drying process. Thats is basic preparation. All values are not critical. Is possible use A. hydroxide only 10%, and only of 30 - 60g. ON basic 10g TACP is possible insert only 5g hexamine. TACP takes hexamine always into own crystalls almost in same concentration. Any way, any ratios, results are always great. Is even possible making mix so, what you take simply 4,3g TACP (all fine powder), add 0,3g AP, add 0,3 hexamine, pour on it a few drops of ammonia water to consistency the porridge. 1 minute mixing by the spoon. This mix is pour - insert on stainless plate and by 80 Celsius evaporated. Smell it entire as hell and coyote together, but on plate in basically run process super fast recrystallisation. From porridge is almost instantly transparent blue water, (principle recrystal) and after 3 minute of course dry crystalls. Is it very fast, dangerous, but results are best. Also here is values not critical. Is possible added only 0,2 - 0,4 hexamine without AP.
However described method 4,3 +0,3 + 0,3 show best properties.... :cool:

...Dr

[Edited on 20-7-2017 by Laboratory of Liptakov]

copper glycine perchlorate

Laboratory of Liptakov - 22-1-2018 at 01:56

For Cu (GLY) ClO4 is possible use same method as for here is described Cu(HEX) ClO4 ? Thus 10g TACP + 10g glycine heated 60C in NH4OH 24% ? For example in 50g ammonia water? Cooling on - 5C and separe crystals ? Thanks for any reply... :cool:

Rosco Bodine - 22-1-2018 at 13:16

Quote: Originally posted by Laboratory of Liptakov

For Cu (GLY) ClO4 is possible use same method as for here is described Cu(HEX) ClO4 ? Thus 10g TACP + 10g glycine heated 60C in NH4OH 24% ? For example in 50g ammonia water? Cooling on - 5C and separe crystals ? Thanks for any reply... :cool:

There was a reply in the NPED thread
http://www.sciencemadness.org/talk/viewthread.php?tid=24817&...

If what I believe is likely will happen does happen, perchlorate will displace nitrate and the amines will displace ammonium to some extent ....and what is the equilibrium there I am not sure.

A shared or mixed "ammonia value" complex is possible, where half of the coordination with copper is one "ammonia value" amine compound and the other half is coordinated with a different "ammonia value"amine compound.

For example methylamine will replace and displace 2 of the 4 ammoniums, and perchlorate will displace the nitrate for a precursor, and these are probably solubility driven reactions.

copper glycine perchlorate

Laboratory of Liptakov - 23-1-2018 at 00:22

Thank you. Yes, I know. I've studied all 5 the links from the recommended link, before a some days. But I did not find the answer. However, Thank you for explaining NH Group's behavior.... :cool:

.....LL

Rosco Bodine - 23-1-2018 at 01:10

I should have posted these links before

http://tetrazolelover.at.ua/index/energeticke_zluceniny_kyse...

translate
https://translate.google.com/translate?sl=auto&tl=en&...

https://books.google.com/books?id=Tt8JAAAAIAAJ&pg=PA152&...

http://www.hoboes.com/pub/Prohibition/Drug%20Information/Mis...

http://www.orgsyn.org/demo.aspx?prep=CV1P0531

Laboratory of Liptakov - 23-1-2018 at 10:15

Thanks for all, Rosco...... :cool: