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Author: Subject: HMX, FOX-7, TKX-50, e.t.c
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[*] posted on 11-11-2013 at 10:25


I told you- in aforementioned pdf boys said, that reaction goes between dinitrourea and hexamine (more precisely, with products of its nitrolysis). It means, that mixed acid must be strong enough. I do not think, that two vessels are good idea- most likely, without dinitrourea hexamine will be completely destroyed. You may read elsewhere, that sulfur acid destroys nitramines like RDX and this compound requires pure nitric acid and cannot be obtained, using usual mixed acid. Two vessel method, as described here: Synthesis, characterization and thermal studies of keto-RDX or k-6.pdf uses poly phosphorus acids just because they wanted to preserve fragments of hexamine.



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[*] posted on 11-11-2013 at 11:34


When you are going to use a mixed acid, there is also there some H2SO4, so what about that, it does not destroy the K-6 ?
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[*] posted on 12-11-2013 at 03:48


Quote: Originally posted by underground  
When you are going to use a mixed acid, there is also there some H2SO4, so what about that, it does not destroy the K-6 ?


It appears, that doesn't. Try it. I can repeat- concentration is crucial. People made this process under permanent control and they found, that at some time quantity of RDX and K-6 reaches its maximum. Then it goes down. Therefore, regime must be precisely reproduced.




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[*] posted on 12-11-2013 at 05:27


Caterpillar have you ever made K-6 ? or are you going to do ?
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[*] posted on 12-11-2013 at 10:56


Negative. It would be interesting, but all my equipment with chemicals are leaved in my past live. I made RDX twice more or less successfully, but not K-6. I knew so few, when I was young. Now when I'm reading description of such procedures, I want to realize some of them, but now even sulfur acid is problem for me.



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[*] posted on 12-11-2013 at 12:03


Quote: Originally posted by caterpillar  
but now even sulfur acid is problem for me.


Dear caterpillar,

*Sulfuric acid

Dany.
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[*] posted on 12-11-2013 at 20:30


Dear Dany, thanks for the correction. (I can take it only as a small revenge for my own). English is not my mother's tongue, and when I'm typing and typing quickly, I make some rather stupid mistakes. (off topic- few years ago we received electrolyte for ours accumulators. Concentrated solution of KOH + some LiOH. One bottle was especially heavy. After dilution an accumulator was flooded with this "electrolyte" and immediately foam went out of it. That heavy bottle contented sulfuric acid. I should have taken couple of litres...)



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[*] posted on 12-11-2013 at 20:36


Quote: Originally posted by caterpillar  
Dear Dany, thanks for the correction. (I can take it only as a small revenge for my own)


:)

Dany.
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[*] posted on 13-11-2013 at 02:23


I was thinking to make some aminonitroguanidine nitrate

guanidine nitrate from AN/U with Silica gel as a catalist -->

nitroduanidine with conc. H2SO4. -->

aminonitroguanidine with hydrazine sulfate -->

( It shoul be easy to make some hydrazine sulfate if you should have some MEK http://www.youtube.com/watch?v=UB7vwIFCnR0 )

aminonitroguanidine nitrate

ANG +HNO3 --> ANGN with dilute nitric acid. If it is concentrated to any extent it could oxidize the hydrazine. ANG is a much better base than nitroguanidine, so ANGN would be much more "stable"

So what do you think guys ?







[Edited on 13-11-2013 by underground]
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[*] posted on 13-11-2013 at 14:49


It is a long way to Tipperary... When (and if) you have made nitroguanidine, we'll discuss the next. And if I'm correct, conversion of nitroguanidine to aminonitroguanidine requires hydrazine hydrate (or even pure hydrazine). And preparation of any salt of hydrazine is a little bit tricky.



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[*] posted on 13-11-2013 at 23:08


I do not know about if it requires pure hydrazine, but i want to believe that hydrazine sulfate will work. Better with some experience about that subject will answer to us. You can easily made some hydrate from hydrazine sulfate but i do not want to work with that think.

In case that hydrazine sulfate does not work, you can made some aminoguanidine nitrate, but i do not know the performance of that stuff, i believe it should have something close to 9000m/s
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[*] posted on 14-11-2013 at 01:33


Believers go to a church. A scientist must know. From one russian forum: hot water solution of hydrazine reacts with nitroguanidine, producing nitroaminoguanidine. I have a solid guess, due to the nature of your questions, that your own experience in HE is very low. In such case, start with something simple.



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[*] posted on 14-11-2013 at 02:24


Quote: Originally posted by
 
Believers go to a church. A scientist must know. From one russian forum: hot water solution of hydrazine reacts with nitroguanidine, producing nitroaminoguanidine. I have a solid guess, due to the nature of your questions, that your own experience in HE is very low. In such case, start with something simple.


Like what ? I have already prepare some ETN, few things are more powerful than ETN, also i do not have a plenty of chemicals... and we can not judge nothing until we will try it, maybe will work, maybe not. Also guanidine nitrate and nitroguanidine are enough more simple, i will start from them anyway !!
But steel aminoguanidine nitrate can be made.
I was wondering if nitroaminoguanidine can be made from aminoguanidine to eliminate the uses of hydrazine.

caterpillar i am waiting you... :D




[Edited on 14-11-2013 by underground]
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[*] posted on 14-11-2013 at 14:14


Go ahead. Reduction of nitroguanidine yields aminoguanidine, yeah. Read carefully the first tread at this very forum: 5-ATZ(5 aminotetrazole...) I do know nothing about nitration of aminoguanidine. Read literature or try it yourself. But the very first stage- preparation of guanidine nitrate- has some, let's say, underwater stones. Hot mixture of urea with AN may explode. You need some thermostat or you'll have to stay near, breathe with ammonia and switch power on and off. Stirring is usefull too. Silicagel should be transparent, it works better then opaque. Smash it to small pieces. That's all what I know.



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[*] posted on 14-11-2013 at 21:38


So it should be better to make the silica gel fine powder correct ?

Also here is a description about AGN

http://www.sciencemadness.org/talk/viewthread.php?tid=12938

"The nitrate, NH2C(=NH)NHNH2*HNO3, crystallizes from water in large plates, from alcohol in needles, and melts at 144°C; it is only sparingly soluble (12 parts in 100) in water at 16°C. "

edit:

caterpillar, here is a description on how to make nitroaminoguanidine with hydrazine sulfate


"200ml water was heated to 60�C and 11g NQ were added while stirring. 15.3g hydrazine sulfate, 100ml water and 6.90g NaOH were mixed and stirred until everything had gone into solution. This solution was slowly poured into the agitated and heated NQ-solution/suspension. Heating (60�C) and stirring was continued during half an hour. After 15 minutes all the NQ had dissolved. The liquid turned orange and during the experiment I smelled ammonia:
HN=C(NH2)(NHNO2) + H2N-NH2 ---> HN=C(NHNO2)(NHNH2) + NH3

So after these thirty minutes, the solution was neutralised with concentrated hydrochloric acid (approx. 6ml HCl 29% was used). The liquid was allowed to cool to 5�C (fridge) and was left so for one hour for full precipitation of the NAQ (the colour... how should I say: slightly pale yellow - "blanc cass�" - light off-white colour?), . It was then filtered and washed with two portions of 15ml cold distilled water. Dried at 80�C. Yield: 7.25g or 57.6% yield. "

[Edited on 15-11-2013 by underground]
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[*] posted on 15-11-2013 at 05:29


Yeah, but what happens with hydrazine sulfate in presence of NaOH? It turns out to hydrazine, of course. Problem is, where to get any salt of hydrazine. Its preparation is not very simple, as I know. NaOCl + urea, something like this. You have no need to make powder from silicagel- small pieces 1-2 mm in size would be enough. Reaction of sulphamic acid (or its ammonium salt) with urea with further nitration of guanidine sulfate surely is safer, then melting AN with urea. I can only repeat: when (and if) you have made nitroguanidine, you'll think about the next stages.



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[*] posted on 15-11-2013 at 06:15


Quote: Originally posted by caterpillar  
Problem is, where to get any salt of hydrazine. Its preparation is not very simple, as I know. NaOCl + urea, something like this.


Very easy if you are going to have some MEK

http://www.youtube.com/watch?v=UB7vwIFCnR0

:D:D

Also take a look on this

http://www.sciencemadness.org/talk/viewthread.php?tid=18487

[Edited on 15-11-2013 by underground]
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[*] posted on 15-11-2013 at 13:40


Then what the problem is? Go ahead.



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[*] posted on 16-11-2013 at 00:17


I just want to know those products, like aminonitroguanidine - ANGN how toxic and harmful are going to be, and it is a little bit difficult to find any informations about those EM. But surely i would try.

[Edited on 16-11-2013 by underground]
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[*] posted on 16-11-2013 at 05:31


There seems to have no extreme toxic groups in ANGN, however most explosives are harmful to you so you should really just synthesize, burn or detonate them in small scale.

This article might be providing some interesting energetic oxidzier and explosives with its derivatives.

Abstract
1-Amino-3-nitroguanidine (ANQ, 2) was synthesized via hydrazinolysis of nitroguanidine (1). An appropriate Lewis structure of ANQ is drawn based on VB calculations. Due to its basicity, it can be protonated by strong mineral acids or acidic heterocycles. In order to synthesize new energetic materials the nitrate (3) and perchlorate (4) salts of 1-amino-3-nitroguanidine were synthesized by protonation of 2 with 40% nitric acid and 60% perchloric acid, respectively. 5-Nitrimino-1,4H-tetrazole obtained by reacting 5-amino-1H-tetrazole with 100% HNO3 was used to synthesize the nitriminotetrazolate salt 5. Furthermore, the dinitramide salt 6 of 1-amino-3-nitroguanidine was synthesized by metathesis reaction of silver dinitramide and 1-amino-3-nitroguanidinium chloride. The dinitroguanidinate salt 7 was synthesized by protonation of 2 with 1,3-dinitroguanidine, which was prepared from nitroguanidine in anhydrous nitric acid/N2O5. All compounds were fully characterized by single-crystal X-ray diffraction, vibrational spectroscopy (IR and Raman), multinuclear NMR spectroscopy, mass spectrometry, elemental analysis, and DSC measurements. The heats of formation of 2–7 were calculated using the atomization method based on CBS-4M enthalpies. With these values and the experimental (X-ray) densities several detonation parameters such as the detonation pressure, velocity, energy, and temperature were computed using the EXPLO5 code. In addition, the sensitivities towards impact, friction and electrical discharge were tested using the BAM drophammer, friction tester as well as a small-scale electrical discharge device. A Koenen test with 1-amino-3-nitroguanidinium nitrate (3) was carried out in order to evaluate its explosive performance and shipping classification.


http://www.znaturforsch.com/ab/v67b/0066.htm

I can not get the paper.. I wish i could read about it.

The dinitramide and nitrate salt sounds very interesting !

This one also ... what is the compound ? http://www.sbir.gov/sbirsearch/detail/274771


[Edited on 16-11-2013 by DubaiAmateurRocketry]
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[*] posted on 16-11-2013 at 12:34


I did synthesized FOX-7 in my lab as a high school student. I would say that it's not that kind of explosive that owns a lot of power. I detonated about 1.5g sample of FOX-7 with 0.5g LA as primary explosive in a paper tube, the link of the video is here:
http://v.ku6.com/show/1TqbsOv_fG0u8OVA.html
It is just normal. A little bit weaker than RDX but very stable and insensitive.
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[*] posted on 16-11-2013 at 13:48


Quote: Originally posted by exoto  
I did synthesized FOX-7 in my lab as a high school student. I would say that it's not that kind of explosive that owns a lot of power. I detonated about 1.5g sample of FOX-7 with 0.5g LA as primary explosive in a paper tube, the link of the video is here:
http://v.ku6.com/show/1TqbsOv_fG0u8OVA.html
It is just normal. A little bit weaker than RDX but very stable and insensitive.


Try to make some ANGN ;)
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[*] posted on 16-11-2013 at 22:53


Quote: Originally posted by exoto  
I did synthesized FOX-7 in my lab as a high school student. I would say that it's not that kind of explosive that owns a lot of power. I detonated about 1.5g sample of FOX-7 with 0.5g LA as primary explosive in a paper tube, the link of the video is here:
http://v.ku6.com/show/1TqbsOv_fG0u8OVA.html
It is just normal. A little bit weaker than RDX but very stable and insensitive.


您好, 居然能在这里能碰到中国人, 有QQ吗?



And for you @underground, this paper is really one of the easiest way to synthesize furoxan compounds. 1 step reaction using an cinnamyl alcohol, sodium nitrite, AcOH, and water.

Link :

http://www.beilstein-journals.org/bjoc/content/pdf/1860-5397...




[Edited on 17-11-2013 by DubaiAmateurRocketry]
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[*] posted on 16-11-2013 at 23:00


Quote: Originally posted by exoto  
I did synthesized FOX-7 in my lab as a high school student. I would say that it's not that kind of explosive that owns a lot of power. I detonated about 1.5g sample of FOX-7 with 0.5g LA as primary explosive in a paper tube, the link of the video is here:
http://v.ku6.com/show/1TqbsOv_fG0u8OVA.html
It is just normal. A little bit weaker than RDX but very stable and insensitive.


Eh, a lot of the low sensitivity explosives have a higher critical diameter than something more sensitive. I really doubt you can see FOX7's full performance at 1.5g. For example, RDX and PETN, same masses at the same density, lets say around 400mgs, despite RDX having a higher det velocity, guess which will make a greater dent? PETN.
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[*] posted on 19-11-2013 at 00:17


Quote: Originally posted by The_Davster  
Quote: Originally posted by exoto  
I did synthesized FOX-7 in my lab as a high school student. I would say that it's not that kind of explosive that owns a lot of power. I detonated about 1.5g sample of FOX-7 with 0.5g LA as primary explosive in a paper tube, the link of the video is here:
http://v.ku6.com/show/1TqbsOv_fG0u8OVA.html
It is just normal. A little bit weaker than RDX but very stable and insensitive.


Eh, a lot of the low sensitivity explosives have a higher critical diameter than something more sensitive. I really doubt you can see FOX7's full performance at 1.5g. For example, RDX and PETN, same masses at the same density, lets say around 400mgs, despite RDX having a higher det velocity, guess which will make a greater dent? PETN.


Yes. I plan to synthesis more of FOX-7, say, 100g in the future. And I may use 20g~30g sample to do the detonation experiment and compare it with same amount of RDX and other explosives.
I work on several other synthesis as well such as LLM-105 and DNPP. LLM-105 was successfully synthesized but in small scale. DNPP is still in process. I m kind of interested in their performance in real world.
also, 5-aminotetrazole nitrate is one of the explosive we have scaled up. Its performance is a shock to me. 44g of it feel like a grenade.
Here is the link:
http://www.woopie.jp/video/watch/89a2aba27837602c?return=aut...
Many of us are interested in 5-ATNO3. It is surprisingly insensitive but meanwhile powerful
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