Sciencemadness Discussion Board

Nitroguanidine

underground - 20-10-2013 at 00:22

I Saw from a pdf calling "Kitchen Improvised" a section of manufacturing the Nitroguanidine.
Here is what it says:

Obtain two clay flower pots with a small hole in their bottoms. Fitted to one of these is stainless steel tubing. A refractory
made from "firebrick" and fired by charcoal should be built. The flower pots will need to fit into this refractory and have
ample room around them to pack the charcoal. An air blower (e.g. hairdryer, vacuum cleaner is hooked up to blow air
through the coal to generate the heat needed. In the bottom flower-pot, a stainless steel screen will be needed to keep
from clogging the stainless steel tubing from the ammonia inlet tube. Place 200 grams of calcium carbonate (Limestone,
chalk) in the bottom flower pot, with the stainless tubing attached. Place the other flowerpot upside down directly on top
of the bottom pot. Place this in the refractory furnace and place a pyrometer or high temperature thermometer into the
hole in the top clay flower pot. Start the furnace and blow air through the burning charcoal until the temperature inside
the pots reaches 700 degrees C.. At this time begin to pass ammonia gas through the stainless tubing into the lime
inside. The temperature should never go over 820 degrees C. as the lime will decompose. The amounts needed in the generator are 170 G. ammonium nitrate fertilizer, 100 G.
sodium hydroxide and adding 100 ml water to the mixture. This water addition would be done in small portions to ensure
the absorption of the gas by the calcium carbonate. This gas needs to be generated slowly! When all the ammonium
nitrate has been added and the gas ceases to generate from the generator deprive the charcoal of oxygen to extinguish
the flame. Let the refractory furnace cool and remove the flowerpots from it. The black material in the bottom is calcium
cyanamide.
Place 216 grams of urea in a stainless steel pan. Heat until it begins to melt. Add in small portions 1300 grams
ammonium nitrate.
CAUTION: This is dangerous and extreme care should be used in this step. This mixture could explode if allowed to burn.
Water should be used if a fire does break out by immediate dilution and quenching of the reaction mixture!!
Keep the temperature of the melt at 120 degrees centigrade. When the addition of the ammonium nitrate is complete
and the mixture is liquid and at 120 degrees C. the calcium cyanamide from above is added in portions over a twenty
minute period. This mixtures temperature is held at 120 degrees C. for two hours and then diluted with 720 ml water.
This liquid is heated to 95 degrees C. and then filtered through several coffee filters or a "fast" filter paper. The liquid
thus obtained is allowed to cool to 25 degrees C. and then the crystals formed are filtered out. The liquid is reduced to
1/2 its volume by boiling. It is cooled and filtered and the crystals obtained are added to those from the first filtration.
These crystals are washed with 40 ml cold water. They are then dried in a shallow pyrex dish while heated in a hot oil
bath at 110 degrees C. for two hours. These crystals are guanidine nitrate (90% purity).
Immerse a one liter flask, containing 500 ml. concentrated sulfuric acid, in cracked ice. This acid is stirred until the
temperature drops to 10 degrees C. or less. In small portions, add 400 grams of dry guanidine nitrate to the acid with
stirring to keep the temperature below 11 degrees C.. When all the guanidine nitrate is dissolved, pour the now milky
liquid into three liters of cracked ice and water. Let this stand until the nitroguanidine is completely crystallized out of the
liquid. Filter these crystals out and dissolve in four liters of boiling water (distilled if possible). Allow to cool by standing
overnight and filter the crystals out. Dry these crystals by heating gently in a container placed in a pan of boiling water.
This dried material is then ready to store in a plastic container or to load into finished caps.

Has anyone try it ? it looks like it really does not needed Obscure chemicals. Nitroguanidine has a VoD of 8200 m/s at density of 1.70 g/cm3 ;)

caterpillar - 20-10-2013 at 01:32

As I know, aforementioned compound may be prepared without cyanamide at all- urea + AN + SiO2 ( silikagel as catalyst, transparent is better than opaque). And read this: https://sites.google.com/site/energeticchemical/nitroguanidi...

Fantasma4500 - 20-10-2013 at 09:24

interesting thread, there have often been demand for the synthesis of nitroguanidine from urea and AN!!

there was no mentions of final yield of this entire reaction from the source, right? because that would be very interesting..

not to go offtopic, this makes me think of anhydrous TACN which can be made in smaller amounts by melting AN and adding CuO and hexamine (not sure if that was nessecary for the formation of TACN tho)
a guy wrote about this in energetics about +6 months ago i recall it to be

anyhow, for the part with KOH, this is not easy to come by where im from, would NaOH be a decent substitute or did i miss something completely?

underground - 20-10-2013 at 09:54

I have seen an almost same process here on this forum

http://www.sciencemadness.org/talk/viewthread.php?tid=8911

The problem is that i can not find any source of sulphamic acid

BobD1001 - 20-10-2013 at 10:22

Step two of this synthesis produces nitroguanidine in what looks to be a much easier to perform experiment:

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

underground - 20-10-2013 at 11:13

Quote: Originally posted by BobD1001  
Step two of this synthesis produces nitroguanidine in what looks to be a much easier to perform experiment:

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


Very good topic, but i can not understand how he made the "dry silica gel"

caterpillar - 20-10-2013 at 13:34

Quote: Originally posted by underground  
Quote: Originally posted by BobD1001  
Step two of this synthesis produces nitroguanidine in what looks to be a much easier to perform experiment:

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


Very good topic, but i can not understand how he made the "dry silica gel"


Heat it up to 150-200 C. So simple. Silicagel can be found in many places.

golfpro - 20-10-2013 at 17:49

"Nitroguanidine has a VoD of 8200 m/s at density of 1.70 g/cm3"

Who says this?? wikipedia gives this a RE of 1.00, a velocity of 7400 at 1.55g/cm3.

I haven't found anything that could possibly beat EGDN, ETN, PETN or RDX as far as relatively simple to make/acquire the reagents/equipment for production.

I have been seeing inaccurate info on wikipedia lately as far as velocities go, is there one dependable source which gives the velocities of explosives?

underground - 20-10-2013 at 20:51

Quote: Originally posted by golfpro  
"Nitroguanidine has a VoD of 8200 m/s at density of 1.70 g/cm3"

Who says this?? wikipedia gives this a RE of 1.00, a velocity of 7400 at 1.55g/cm3.

I haven't found anything that could possibly beat EGDN, ETN, PETN or RDX as far as relatively simple to make/acquire the reagents/equipment for production.

I have been seeing inaccurate info on wikipedia lately as far as velocities go, is there one dependable source which gives the velocities of explosives?



http://en.wikipedia.org/wiki/Table_of_explosive_detonation_v...


"Used silica gel was prepared from liquid glass (sodium metasilicate) using the following procedure. Commercially available liquid glass is diluted 2-3 times, then 10-15% sulphuric acid is added. Solution forms non fluid galantine (it is essential that acid should be added in one portion, and solution should thicken, if H2SiO3 precipitate is formed, solutions must be more diluted and mixed more efficiently) witch is placed to the cold freezer for 2 days. On defrost galantine disperses to fine powder, witch is filtered, carefully washed and tempered to dryness. This silica gel was reused in guanidine nitrate process for 7 times, without loosing activity. Regeneration of silica gel was preformed by washing thoroughly with 1 liter of hot water and tempering"
Quote: Originally posted by caterpillar  

Heat it up to 150-200 C. So simple. Silicagel can be found in many places.



???





[Edited on 21-10-2013 by underground]

underground - 21-10-2013 at 06:38

Can somebody explain to me i little bit better how silica gel above is prepared ?

DubaiAmateurRocketry - 21-10-2013 at 07:06

Is it possible to carry out nitration to nitroguanidine to form oxygen positive materials ?

VladimirLem - 21-10-2013 at 09:38

Quote: Originally posted by golfpro  
"Nitroguanidine has a VoD of 8200 m/s at density of 1.70 g/cm3"

Who says this?? wikipedia gives this a RE of 1.00, a velocity of 7400 at 1.55g/cm3.


wheres the problem? 7400 at 1.55...you know the velocity rises much with every higher 0.1gram/cm at desensity?


@thread:

Has anyone practical knowledge about this compound?
is seems really interesting (less many and cheap chemicals needed compared to most nitrate esters/nitramines)....pretty cool VoD, brisance is okay too.

the problems i see is, that tests will end up with undetonated material all over the area (that shit is less sensitive than PURE ammoniumnitrate :o ) ...so, do anyone have good ideas for sensibilizing that stuff?


i thought of:
Strong ETN booster (30grams) - of course ;)
about 2-4% RDX and 2-4% ammonium nitrate at maincharge...but i dont like the fact that this stuff seems pretty sensitive to "acids"...so some substitute to this would be great

"phlegmatizing" it with in nitromethane/gasoline dissolved polyisobutylene (2-3%) and than pressing that stuff to around 1.6g/cm3

could that work?

caterpillar - 21-10-2013 at 13:05

Silicagel is used to keep some equipment dry- it gulps water steam. I found it in at nearly each box with science equipment (well, twice I met ceolite instead). this is why I think, that there is no need in its preparation. it is not very simple to press nitroguanidine due to the fibrous nature of its crystals. But read this: https://sites.google.com/site/energeticchemical/nitroguanidi... There is a complex of nitroguanidine and nitric acid- very powerful explosive. Dinitroguanidine exists too and according to aforementioned link, its ammonium salt is very powerful explosive.

golfpro - 21-10-2013 at 17:54

If it's true density is 1.7 than that would be good, but it has a low heat of explosion, I don't see it outperforming ETN at cast density in any way.

underground - 22-10-2013 at 02:23

Quote: Originally posted by caterpillar  
Silicagel is used to keep some equipment dry- it gulps water steam. I found it in at nearly each box with science equipment (well, twice I met ceolite instead). this is why I think, that there is no need in its preparation.


Ok so if i have correctly understand silicagel it should be something like this:

https://encrypted-tbn3.gstatic.com/images?q=tbn:ANd9GcSpxZLq...

And he says:
"340g of ammonium nitrate, 200g urea and 80g of tempered dry silica gel and heated up on oil bath to 195C"

So with the above chemicals mixing them and bring them to 195C you are going to form Guanidine nitrate ?

VladimirLem - 22-10-2013 at 08:14

Quote: Originally posted by golfpro  
If it's true density is 1.7 than that would be good, but it has a low heat of explosion, I don't see it outperforming ETN at cast density in any way.


No doubt its less powerful than ETN...but a bit faster as far as i know, and could be used in shaped charges (just at the cone must be 20%< other, more sensitive explosives integrated....the critical diametre of NirtoGua. is fucked up)
anyone know the exact/or calculated VoD of ETN....some says a bit above 7000....i dunno...

golfpro - 22-10-2013 at 15:56

wikipedia says anywhere from 7400-8100 depending on which page you look at.

I wish there was an official, reliable report for exact velocities of ETN and others.

BobD1001 - 22-10-2013 at 16:14

Quote: Originally posted by underground  

Ok so if i have correctly understand silicagel it should be something like this:

https://encrypted-tbn3.gstatic.com/images?q=tbn:ANd9GcSpxZLq...

And he says:
"340g of ammonium nitrate, 200g urea and 80g of tempered dry silica gel and heated up on oil bath to 195C"

So with the above chemicals mixing them and bring them to 195C you are going to form Guanidine nitrate ?



Just follow procedure from the link to the synthesis I posted earlier in the thread. It takes time, heat, mixing, and a recrystallization if I remember correctly, but will form guanidine nitrate. I will likely be doing this synthesis this weekend, as I have been wanting to experiment with it for small rocket engines (such as the old Jetex brand) for some time now. Has anyone here successfully or otherwise experimented with guanidine nitrate rocket propellants?

Dornier 335A - 23-10-2013 at 00:40

The density of ETN was measured to 1.719 (±0.0025) g/cm3 with a gas pycnometer in "Characterization and Analysis of Tetranitrate Esters". Its VoD calculated with Cheetah 6.0 at that density was 8206 m/s.

underground - 23-10-2013 at 02:29

Quote: Originally posted by BobD1001  

Just follow procedure from the link to the synthesis I posted earlier in the thread. It takes time, heat, mixing, and a recrystallization if I remember correctly, but will form guanidine nitrate. I will likely be doing this synthesis this weekend, as I have been wanting to experiment with it for small rocket engines (such as the old Jetex brand) for some time now. Has anyone here successfully or otherwise experimented with guanidine nitrate rocket propellants?


Yes i just wondering if i am going to use silicagel as i am going to buy like that one
https://encrypted-tbn3.gstatic.com/images?q=tbn:ANd9GcSpxZLq...
if it is going to work



Quote: Originally posted by caterpillar  
Silicagel is used to keep some equipment dry- it gulps water steam. I found it in at nearly each box with science equipment (well, twice I met ceolite instead). this is why I think, that there is no need in its preparation. it is not very simple to press nitroguanidine due to the fibrous nature of its crystals. But read this: https://sites.google.com/site/energeticchemical/nitroguanidi... There is a complex of nitroguanidine and nitric acid- very powerful explosive. Dinitroguanidine exists too and according to aforementioned link, its ammonium salt is very powerful explosive.


I finally bought something for absorbing the moisture but it looks that it is calcium chloride:(


I was thinking to buy that one
http://www.ebay.co.uk/itm/Flower-Drying-Silica-Gel-500-gm-/3...

Is it going to work ?

[Edited on 23-10-2013 by underground]

underground - 23-10-2013 at 08:15

Ok, lately i bought some urea as a fertilizer, and i was trying to make some urea nitrate as it is easy to make it. I add 2moles of AN and 1mole of H2SO4 and then i let the reaction to go. After i filter the liquid and surely was hno3 as long as it produce a lots of fumes if i blow to it and also really reacts with copper. Then i add some urea fertilizer into the acid but nothing was happened!! So what is going on...

[Edited on 23-10-2013 by underground]

underground - 3-11-2013 at 00:29

Is there any other chemical to react between AN/UN to form guanidine nitrate ? as long as i can not find anywhere here silica gel (except Internet)

VladimirLem - 3-11-2013 at 07:08

Quote: Originally posted by underground  
Is there any other chemical to react between AN/UN to form guanidine nitrate ? as long as i can not find anywhere here silica gel (except Internet)


there is no need for urea nitrate to make guanidine nitrate.
you have to reakt ammonium nitrate with urea
and as far as i know, i ve seen the same synthesis, without silica gel...but cant find it anymore...
another synthesis way is with Calcium cyanamide and ammonium nitrate...

and, if you want to make Nitroguanidine...i dont know if this is a good choice....as you said, ETN is much stronger....NitroGua. is less sensitive and better to handle (saver), but that stuff isnt easy to ignite...without a strong booster and added sensitizers, this will be a fail cause its less sensitive than -pure- ammonium nitrate :mad:
and dont be naive...you woundnt get 8200m/s....if you get 6-7000m/s im proud on you so if you wand performace stay at ETN (and please dont melt that shit:o)

i wonder what exactly you are going to do with this HEs?

if you are going to make shaped charges or something else, this would make sense but i dont think so....you will earn much easier success (simple detonations) with AN, carbon containing stuff and lets say up to 5 percent of ETN as sensitizer

there is no huge differece between 1kg ANNM and stuff with more brisance...both will fuck shit up...i think at my first, really huge charge...i made some 600g ANFO underground before and no load BANG...so ....hey, letz put 1.5 kg ANNM-AL at thouse tree and beeing just 30 metres away in cover....i thought the apocalypse just started:D:o

if you really want to see differences (performace) at explosives make shaped charges...

underground - 3-11-2013 at 12:31

Quote: Originally posted by VladimirLem  
Quote: Originally posted by underground  
Is there any other chemical to react between AN/UN to form guanidine nitrate ? as long as i can not find anywhere here silica gel (except Internet)


there is no need for urea nitrate to make guanidine nitrate.
you have to reakt ammonium nitrate with urea
and as far as i know, i ve seen the same synthesis, without silica gel...but cant find it anymore...
another synthesis way is with Calcium cyanamide and ammonium nitrate...

and, if you want to make Nitroguanidine...i dont know if this is a good choice....as you said, ETN is much stronger....NitroGua. is less sensitive and better to handle (saver), but that stuff isnt easy to ignite...without a strong booster and added sensitizers, this will be a fail cause its less sensitive than -pure- ammonium nitrate :mad:
and dont be naive...you woundnt get 8200m/s....if you get 6-7000m/s im proud on you so if you wand performace stay at ETN (and please dont melt that shit:o)

i wonder what exactly you are going to do with this HEs?

if you are going to make shaped charges or something else, this would make sense but i dont think so....you will earn much easier success (simple detonations) with AN, carbon containing stuff and lets say up to 5 percent of ETN as sensitizer

there is no huge differece between 1kg ANNM and stuff with more brisance...both will fuck shit up...i think at my first, really huge charge...i made some 600g ANFO underground before and no load BANG...so ....hey, letz put 1.5 kg ANNM-AL at thouse tree and beeing just 30 metres away in cover....i thought the apocalypse just started:D:o

if you really want to see differences (performace) at explosives make shaped charges...


First of all, thanks VladimirLem for your response
If the stuff is like that you describe above, it is better not to made it, i was thinking something like ETN substitute, as it is going to cost much more less than ETN... But if it is so difficult to detonate better not try to make that..

I am sorry but i really do not know what are the shaped charges, i saw a sticky theme but it is really long... so can you tell me about that with only few words to start with ?

VladimirLem - 3-11-2013 at 13:16

well...its an special kind of explosive device to focus the released energy of the detonation at one small area....in short: its an armour piercing device

http://en.wikipedia.org/wiki/Shaped_charge
http://www.youtube.com/watch?v=qqMoFx0uwpo
http://www.youtube.com/watch?v=LudNqf56AFo
http://www.sciencemadness.org/talk/viewthread.php?tid=10575

caterpillar - 3-11-2013 at 14:51

Guanidine nitrate (nitroguanidine as well) may be not very interesting itself, but it is the start point for many interesting compounds. Guanidine nitrate-> nitroguanidine-> aminoguanidine-> aminotetrazole-> nitriminotetrazole or nitroguanidine nitrate-> dinitroguanidine and so on. There are many much simpler ways to make loud bang, but it is interesting for boys, who love chemistry.

DubaiAmateurRocketry - 4-11-2013 at 03:58

Quote: Originally posted by caterpillar  
but it is interesting for boys, who love chemistry.


What do you mean? Is there any girls who like energetic materials ?

caterpillar - 4-11-2013 at 12:32

Quote: Originally posted by DubaiAmateurRocketry  
Quote: Originally posted by caterpillar  
but it is interesting for boys, who love chemistry.


What do you mean? Is there any girls who like energetic materials ?


I met one at a russian forum. And here http://www.sciencemadness.org/talk/viewthread.php?tid=8144&a... NatashaJurievna might be a girl (I'm not sure, of course).

underground - 4-11-2013 at 12:37

Quote: Originally posted by VladimirLem  
well...its an special kind of explosive device to focus the released energy of the detonation at one small area....in short: its an armour piercing device

http://en.wikipedia.org/wiki/Shaped_charge
http://www.youtube.com/watch?v=qqMoFx0uwpo
http://www.youtube.com/watch?v=LudNqf56AFo
http://www.sciencemadness.org/talk/viewthread.php?tid=10575


Ok i make some searching and i can say that shaped charges are really interesting. Also i can only almost everywhere see the conical shape charge, and how we are going to know how it is going to work better ? For example degrees of the cone, how much explosive must be used, outer diameter, length.. distance from the target e.t.c.

Also can you give to me a picture about the sticky theme of the unconventional shaped charges to understand it better ?

NeonPulse - 4-11-2013 at 13:48

Underground you should take time to read the dc thread.it is full of helpful info on shaped charges. I learnt a lot there,it just takes a bit of time to go through all the pages. It is worth the time if you want to learn more.a lot of tests and results to help build sc's that work.

underground - 4-11-2013 at 22:25

Quote: Originally posted by NeonPulse  
Underground you should take time to read the dc thread.it is full of helpful info on shaped charges. I learnt a lot there,it just takes a bit of time to go through all the pages. It is worth the time if you want to learn more.a lot of tests and results to help build sc's that work.


OK NeonPulse, thanks a lot, i appreciate that.

caterpillar - 6-11-2013 at 13:38

Back to the topic: read this, if you can. http://www.exploders.us/sprawka/67.html and http://www.exploders.us/sprawka/68.html . Nitroguanidine and dinitroguanidine. There is another route to nitroguanidine- melt urea with ammonium sulphamate. Urea 300 gr, ammonium sulphamate 1148 gr. 225-245°C, 30 minutes with further nitration of obtained guanidine sulphate with mixed acid. Good news is that this mixture cannot explode, when you heat it.

underground - 7-11-2013 at 22:24

Quote: Originally posted by caterpillar  
Back to the topic: read this, if you can. http://www.exploders.us/sprawka/67.html and http://www.exploders.us/sprawka/68.html . Nitroguanidine and dinitroguanidine. There is another route to nitroguanidine- melt urea with ammonium sulphamate. Urea 300 gr, ammonium sulphamate 1148 gr. 225-245°C, 30 minutes with further nitration of obtained guanidine sulphate with mixed acid. Good news is that this mixture cannot explode, when you heat it.


Everything are in other language than English so can not understand them.... But i can really understand your topic ;)

[Edited on 8-11-2013 by underground]

caterpillar - 8-11-2013 at 20:33

Well, one can understand formulas, even written in foreign language (to say nothing about the Chinese one). But, if russian texts are problem for you, some info can be found just under your nose: http://www.sciencemadness.org/talk/viewthread.php?tid=8911

underground - 8-11-2013 at 22:05

Quote: Originally posted by caterpillar  
Well, one can understand formulas, even written in foreign language (to say nothing about the Chinese one). But, if russian texts are problem for you, some info can be found just under your nose: http://www.sciencemadness.org/talk/viewthread.php?tid=8911


Yes i have already see that and it has already posted at the beginning of that thread :)

caterpillar - 9-11-2013 at 02:49

Well, it means that you already know enough. But to start with preparation of calcium cyanamide is too problematic for us, poor kitchen (garage?) chemists. And as you may see, it is not necessary at all. (BTW, aforementioned process might be realized simpler- CaC2 plus dry nitrogen. But this reaction requires 1000 Celsius too...)

underground - 9-11-2013 at 03:08

It looks like AN/U/Silica gel is the best way but something is wrong with the reaction

He uses almost 1:1 ratio of moles of AN and Urea (340gr AN and 320gr U ) but this reaction produces water, not CO2 and ammonia

CH4N20 + NH4NO3 = CH6N403 + H20

It needs 2 moles of Urea and 1 Mole of AN to produce CO2 and NH3

2CH4N20 + NH4NO3 = CH6N403 + CO2 + 2NH3

So something is going wrong here

franklyn - 6-2-2014 at 01:49

A study of the detonation parameters of bulk density Nitroguanidine and Aluminium powder mixtures

www.chemikinternational.com/pdf/2012/01_2012/CHEMIK_2012_p50-57.pdf


[Edited on 7-2-2014 by franklyn]

underground - 6-2-2014 at 16:02

Quote: Originally posted by franklyn  
A study of the detonation parameters of bulk density Nitroguanidine and Aluminium powder mixtures

www.chemikinternational.compdf201201_2012CHEMIK_2012_p50-57.pdf

.


franklyn your pdf link does not work for me at least.

underground - 7-2-2014 at 02:44

Ok franklyn, thanks :)

http://www.chemikinternational.com/pdf/2012/01_2012/CHEMIK_2...

underground - 13-2-2014 at 07:04

I was trying to make some nitroguanidine by dehydration of quanidine nitrate with H2SO4 but it looks like i end up with guanidine sulpate !! I mix 200gr of GN with 500gr of H2S04. After that the temperature was rised a little bit. The SA started to produce some fumels like with nitrate salts and was bubbling like a coca cola... After i drop that mixture into 300ml of water and some white crystals were formed, it was about 140-150gr. I washed and neutralized them with some sodium bicarbonate, wased them again with some water and acetone for drying faster. That salt it does not burned at alll, guanidine nitrate burnes better than that... also it melts really dificult, more than GN, and when it melts and decomposes, some white solid perticipates is formed... So what is that at all ?

[Edited on 13-2-2014 by underground]

DubaiAmateurRocketry - 13-2-2014 at 10:35

That is probably nitroguanidine, I think thats how it should behave. nitroguanidine isnt very energetic, have you tried to test the density yet?

underground - 13-2-2014 at 10:53

No i do not, how can i do that ? Guanidine sulfate has a melting point of 290-293 °C wich is more suitable with that i have, also i can not find anywere the density of Guanidine sulfate!

[Edited on 13-2-2014 by underground]

DubaiAmateurRocketry - 13-2-2014 at 11:22

Quote: Originally posted by underground  
No i do not, how can i do that ? Guanidine sulfate has a melting point of 290-293 °C wich is more suitable with that i have, also i can not find anywere the density of Guanidine sulfate!

[Edited on 13-2-2014 by underground]


get a measuring cylinder and add water, then add 1ml of NQ, see how much gram increased, you will need a scale up to 0.01 gram though, i guess you do?

underground - 13-2-2014 at 11:37

Quote: Originally posted by DubaiAmateurRocketry  

get a measuring cylinder and add water, then add 1ml of NQ, see how much gram increased, you will need a scale up to 0.01 gram though, i guess you do?


Ok i will try it tomorrow and i will tell you the results.

Dornier 335A - 13-2-2014 at 12:10

Nitroguanidine made by pouring a solution into water looks a lot like asbestos. An it is indeed very difficult to ignite.
You could measure its melting point. NQ lies around 240°C and guanidine sulfate between 290°C and 293°C.

underground - 13-2-2014 at 15:30

Indeed it looks like asbestos, so it looks like i have some NGuanidine here. I will do the DubaiAmateurRocketry's density test to see what we have here. How much possible is with this way to form GS rather than NG ?

DubaiAmateurRocketry - 14-2-2014 at 05:06

You should have nitroguanidine, nitroguanidine is not energetic and can be bought easily so im not surprised, however it can detonate with a booster.

I did not find guanidine sulfate's density, but nitroguanidine is 1.72 g/cm³. Guanidine sulfate might have a similar density so im not sure if this is a good idea hehe.

[Edited on 14-2-2014 by DubaiAmateurRocketry]

underground - 14-2-2014 at 06:57

Quote: Originally posted by DubaiAmateurRocketry  
You should have nitroguanidine, nitroguanidine is not energetic and can be bought easily so im not surprised, however it can detonate with a booster.

I did not find guanidine sulfate's density, but nitroguanidine is 1.72 g/cm³. Guanidine sulfate might have a similar density so im not sure if this is a good idea hehe.

[Edited on 14-2-2014 by DubaiAmateurRocketry]


Yea, i also make that thought. But for what i have read i believe it is NG I was thinking if i can move now to NG nitrate :P

VladimirLem - 14-2-2014 at 09:19

Quote: Originally posted by DubaiAmateurRocketry  
nitroguanidine is not energetic


what is this supposed to mean?

i dont think they put it in cartridges cause it looks so nice :D




underground - 14-2-2014 at 09:43

Quote: Originally posted by VladimirLem  

i dont think they put it in cartridges cause it looks so nice :D


xaxaxaxaxa!! realy funny!! :D :D

[Edited on 14-2-2014 by underground]

Explosive performance of nitroguanidine

Gargamel - 20-12-2015 at 13:13

If you have guanidine nitrate, nitroguanidine could easily be prepared.

Apart from being a useful raw material for a lot of other things and also as a propellant:

How would it perform as a high explosive for shaped charges and other interesting experiments?
I found velocity figures from 6750 to 8200m/s, that sounds useful, even though it's not as energetic as the more common HEs.

I wonder how it behaves in practice concerning the typical problems one encounters, like achieving the right density, critical charge diameter and sensitivity to initiation.


Any practical experience?

The_Davster - 20-12-2015 at 13:21

One major problem with guanidine nitrate (EDIT: typo, meant nitroguanidine, thanks philou!) is that its morphology (needles) makes it very difficult to get anything approaching a reasonable density for application in shaped charges.

Better to turn it into 5-AT, and make the nitrate salt. That has around 8800 m/s and density 1.8 if I remember correctly.

[Edited on 20-12-15 by The_Davster]

PHILOU Zrealone - 20-12-2015 at 14:45

@ The_Davster,
Nitroguanidine, not guanidine nitrate!

From Explosives 4th revised and extended edition, Josef Köhler and Rudolf Meyer

p248 and 249
Nitroguanidine (H2N)2C=N-NO2
MW: 104.1 g/mol
Enthalpy of formation: -213.3 kcal/kg
OB: -30.7%
%N: 53.83%
Volume of detonation gases: 1075 L/kg
Heat of explosion (H2O gas): 687 kcal/kg
specific energy: 98 mt/kg
density: 1.71 g/cm³
melting point: 232°C = 450°F (decomposition without deflagration)
lead block test for 10g: 305 cm³
VOD at max density and confinement: 8200 m/s
impact sensitivity: up to 49 Nm --> no reaction
friction sensitivity: up to 353 N pistil load --> no reaction
critical diameter of steel sleeve test: 1 mm --> no reaction ... Thus very insensitive even if confined!
Soluble in hot water but almost unsoluble in cold water. Sparingly soluble in alcohol and insoluble in ether.
Readily soluble in alkali (formation of salts NQ is a nitramine NH2-C(=NH)-NH-NO2).
Excellent chemical stability and not very sensitive to shock or impact.

The_Davster - 20-12-2015 at 14:49

thanks! I typed the wrong compound

underground - 20-12-2015 at 15:10

Does anyone know the properties of aminoguanidine nitrate ? Aminoguanidine can be made by reduction of nitroguanidine. Then just neutralize it with HNO3

Nitroguanidine looks to be an interesting nitramine

[Edited on 20-12-2015 by underground]

Bert - 20-12-2015 at 21:28

Gargamel-

I have merged your new nitroguanidine thread with another nitroguanidine thread.

If you please. If you don't have an actual lab you conducted to report on, or time to give the references /links to show your sources of information leading to questions- and the topic has been repeatedly discussed, with multiple pre existing threads...POST YOUR QUESTION IN AN EXISTING RELATED THREAD.

Thanks-

PHILOU Zrealone - 21-12-2015 at 04:31

Quote: Originally posted by PHILOU Zrealone  
@ The_Davster,
Nitroguanidine, not guanidine nitrate!

From Explosives 4th revised and extended edition, Josef Köhler and Rudolf Meyer

p248 and 249
Nitroguanidine (H2N)2C=N-NO2
MW: 104.1 g/mol
Enthalpy of formation: -213.3 kcal/kg
OB: -30.7%
%N: 53.83%
Volume of detonation gases: 1075 L/kg
Heat of explosion (H2O gas): 687 kcal/kg
specific energy: 98 mt/kg
density: 1.71 g/cm³
melting point: 232°C = 450°F (decomposition without deflagration)
lead block test for 10g: 305 cm³
VOD at max density and confinement: 8200 m/s
impact sensitivity: up to 49 Nm --> no reaction
friction sensitivity: up to 353 N pistil load --> no reaction
critical diameter of steel sleeve test: 1 mm --> no reaction ...

Thus very insensitive even if confined!
Soluble in hot water but almost unsoluble in cold water. Sparingly soluble in alcohol and insoluble in ether.
Readily soluble in alkali (formation of salts NQ is a nitramine NH2-C(=NH)-NH-NO2).
Excellent chemical stability and not very sensitive to shock or impact.


From same book p 166:
Guanidine nitrate (H2N)2C=NH.HNO3
MW: 122.1 g/mol
Enthalpy of formation: -767 kcal/kg
OB: -26.2%
%N: 45.89%
Volume of detonation gases: 1098 L/kg
Heat of explosion (H2O gas): 482 kcal/kg
specific energy: 77 mt/kg
density: ??? g/cm³ (1.436 from Wikipedia)
melting point: 215°C = 419°F (deflagrate at 270°C = 518°F)
lead block test for 10g: 240 cm³
VOD at max density and confinement: ??? m/s
impact sensitivity: up to 50 Nm --> no reaction
friction sensitivity: up to 353 N pistil load --> no reaction
critical diameter of steel sleeve test: 2.5 mm

Thus very insensitive but more than NQ because it will blow a 25mm diameter pipe recipient with a 2.5 mm hole heated by Bunzen burners while NQ doesn't with 1mm (Nitroglycerin does it at 24 mm)!

Soluble in alcohol and/or water.

--------------------------------------------------------------
Not asked but related to amino-guanidine nitrate...

From same book p379
Triaminoguanidine nitrate (H2N-NH-)2C=N-NH2.HNO3
MW: 167.1 g/mol
Enthalpy of formation: -67.07 kcal/kg
OB: -33.5%
%N: 58.68%
Volume of detonation gases: 1206 L/kg
Heat of explosion (H2O gas): 876 kcal/kg
specific energy: ?? mt/kg (must be >98 since VODG is bigger just as heat of explosion while energy of formation is less exothermic)
density: 1.5 g/cm³
melting point: 216°C = 420°F (decomposition-dflagrate at 227°C = 440°F)
lead block test for 10g: 350 cm³
VOD at 0.95 density and confinement: 5300 m/s
impact sensitivity: 4 Nm
friction sensitivity: over to 120 N pistil load --> crackling
critical diameter of steel sleeve test: ??? mm

Thus much more sensitive!

Prepared by reacting 1 mole of guanidine nitrate with 3 moles of hydrazine hydrate at 100°C for 4 hours.The reaction is accompanied by the liberation of ammonia.

--------------------------------------------------------------
From Donald Haarmann (The Wizzards is In) VOD tables updated by Formatik in 2008
> Triaminoguanidine nitrate (TAGN)
VOD 5300 at 0.95
and 7930 at 1.46
LBT 350/117% vs TNT
Ref K&M and 2700 T28

> Guanidine nitrate (GN)
VOD 3700 at ??
LBT 10% vs TNT
LBT 110-140 thus vs TNT 36-46%
Ref 2700 G151 and Urbanski (2)

> Guanidine perchlorate
VOD 6000 at 1.15
VOD 7150 at 1.67
LBT 400 vs TNT 133%
Ref Urbanski (2) and Davis and 2700 G152

K&M= Köhler and Meyer
2700 = PATR 2700 Encyclopedia of Explosives and Explosive Items Vol.
Davis = Tenney L. Davis; The Chemistry and powder of Explosives (1943)
-----------------------------------------------------
Conclusions?
1°)Aminoguanidine nitrate must display properties between GN and TAGN.
2°)One can see that the enthalpy of formation of nitrate salt of amine is large, this comes mainly from the neutralization heat of the base by the acid...most amine salts display such effect.
3°)The enthalpy of formation and heat of explosion goes up (less negative) by passing from GN to NQ (a kind of dehydratation)...this fact comes from less water into the molecule...water in exhaust gases reduces the heat of explosion.
4°)The enthalpy of formation and heat of explosion goes up (less negative) by introducing hydrazine into the molecule see GN and TAGN; this fact comes from endothermicity of hydrazine and that the N-N bond will form very stable N#N (dinitrogen) after burning releasing a lot of energy
5°)Perchlorates are better than nitrates, more dense salts results, better OB and energy output --> more sensitive and higher VOD or lead block tests.
6°)Triaminoguanidine perchlorate must be a killer but also quite sensitive :D :cool:


[Edited on 21-12-2015 by PHILOU Zrealone]

ecos - 21-12-2015 at 05:11

Biguanide diperchlorate has VoD of 8490 m/s according to US4340755 A


vod.JPG - 82kB

[Edited on 21-12-2015 by ecos]

PHILOU Zrealone - 21-12-2015 at 06:03

Good Ecos!

Biguanide diperchlorate (BGDP) H2N-C(=NH)-NH-C(=NH)-NH2.2HClO4 is a kind of dimer of guanidine perchlorate (H2N-C(=NH)-NH2.HClO4)
H2N-(C(=NH)-NH)1-H .HClO4 (VOD 7150m/s at 1.67 g/cm³)
H2N-(C(=NH)-NH)2-H .2HClO4 (VOD 8490m/s at 1.91 g/cm³)

Now we need to find datas for:
-dinitro biguanide O2N-NH-C(=NH)-NH-C(=NH)-NH-NO2
-biguanide dinitrate H2N-C(=NH)-NH-C(=NH)-NH2 .2HNO3
-biguanide dinitroformiate H2N-C(=NH)-NH-C(=NH)-NH2 .2HC(NO2)3

-bisguanidine dinitrate H2N-C(=NH)-NH-NH-C(=NH)-NH2 . 2HNO3
-bisguanidine diperchlorate H2N-C(=NH)-NH-NH-C(=NH)-NH2 . 2HClO4 (probably stronger than BGDP)
-bisguanidine dinitroformiate H2N-C(=NH)-NH-NH-C(=NH)-NH2 . 2HC(NO2)3
-dinitro bisguanidine O2N-NH-C(=NH)-NH-NH-C(=NH)-NH-NO2
And azo dérivatives
H2N-C(=NH)-N=N-C(=NH)-NH2 . 2HNO3
H2N-C(=NH)-N=N-C(=NH)-NH2 . 2HClO4 (probably even stronger)
H2N-C(=NH)-N=N-C(=NH)-NH2 . 2HC(NO2)3
O2N-NH-C(=NH)-N=N-C(=NH)-NH-NO2

Formamidine dérivatives:
-formamidine nitrate H2N-CH=NH . HNO3
-formamidine perchlorate H2N-CH=NH . HClO4
-formamidine nitroformiate H2N-CH=NH . HC(NO2)3
-nitroformamidine O2N-NH-CH=NH
-aminoformamidine nitrate H2N-CH=N-NH2 . HNO3
-aminoformamidine perchlorate H2N-CH=N-NH2 . HClO4
-aminoformamidine nitroformiate H2N-CH=N-NH2 . HC(NO2)3
-nitroaminoformamidine O2N-NH-CH=N-NH2
-O2N-NH-CH=N-N=CH-NH-NO2
-diaminoformamidine dinitrate H2N-NH-CH=N-NH2 . 2 HNO3
-diaminoformamidine diperchlorate H2N-NH-CH=N-NH2. 2 HClO4
-diaminoformamidine dinitroformiate H2N-NH-CH=N-NH2 . 2 HC(NO2)3

Oxaladiamidine dérivatives:
-bisformamidine dinitrate H2N-C(=NH)-C(=NH)-NH2 . 2HNO3
-bisformamidine diperchlorate H2N-C(=NH)-C(=NH)-NH2 . 2 HClO4
-bisformamidine dinitroformiate H2N-C(=NH)-C(=NH)-NH2 . 2 HC(NO2)3
-bisnitroformamidine O2N-NH-C(=NH)-C(=NH)-NH-NO2
And
Diamino dérivatives of oxaladiamidine...
Tetramino dérivatives of oxaladiamidine...

Triguanide dérivatives H2N-(C(=NH)-NH)3-H
H2N-C(=NH)-NH-C(=NH)-NH-C(=NH)-NH2
--> dinitrate, diperchlorate, dinitroformiate, dinitro-

Thus stil a lot of simple compounds to discover/study with very potent explosive abilities probably over RDX, PETN...and maybe over HMX or CL-20

[Edited on 21-12-2015 by PHILOU Zrealone]

underground - 21-12-2015 at 07:00

Do anyone know any info for aminoguanidine nitrate ?

PHILOU Zrealone - 21-12-2015 at 09:17

Also related to aminoguanidine...diamino-tetrazine H2N-C(NN)2C-NH2
--> mononitrate, monoperchlorate, mononitroformiate and maybe dinitrate, diperchlorate, dinitroformiate.

Also dihydrazino-tetrazine H2N-NH-C(NN)2C-NH-NH2
--> mononitrate, monoperchlorate, mononitroformiate and maybe dinitrate, diperchlorate, dinitroformiate.

PHILOU Zrealone - 21-12-2015 at 09:24

Quote: Originally posted by underground  
Do anyone know any info for aminoguanidine nitrate ?

-It has the formula H2N-C(=NH)-NH-NH2. HNO3
-It must display properties between those of guanidine nitrate and triamino guanidine nitrate...probably closer to TAGN.
--> d close to 1.5, VOD > 7500 m/s, Impact sensitivity in the range 3 < x < 10 Nm

Other infos
-Aminoguanidine can be made from equimolar cyanamide and hydrazine mix; and from guanidine with one hydrazine equivalent.
-Free aminoguanidine easily turns into diamino-tetrazine by air oxydation...

[Edited on 21-12-2015 by PHILOU Zrealone]

underground - 21-12-2015 at 09:39

Quote: Originally posted by PHILOU Zrealone  
Quote: Originally posted by underground  
Do anyone know any info for aminoguanidine nitrate ?

-It has the formula H2N-C(=NH)-NH-NH2. HNO3
-It must display properties between those of guanidine nitrate and triamino guanidine nitrate...probably closer to TAGN.
--> d close to 1.5, VOD > 7500 m/s, Impact sensitivity in the range 3 < x < 10 Nm

Other infos
-Aminoguanidine can be made from equimolar cyanamide and hydrazine mix; and from guanidine with one hydrazine equivalent.
-Free aminoguanidine easily turns into diamino-tetrazine by air oxydation...

[Edited on 21-12-2015 by PHILOU Zrealone]


I was thinking of making Aminoguanidine from nitroguanidine by reduction of nitroguanidine with zinc in acetic acid

http://www.sciencemadness.org/scipics/Engager/TzOTC/Syntheti...

Not the use of toxic hydrazine at all

diamino-tetrazine looks very interesting, what about diamino-tetrazine dinitrate ?

Praxichys - 21-12-2015 at 11:16

Here's a thread I made a few years back which contains a ton of info on these guanidine compounds:

http://www.sciencemadness.org/talk/viewthread.php?tid=17908

Gargamel - 23-12-2015 at 09:50

Sorry Bert, I must have overlooked this thread.

I'm specifically after the practical usefulness of nitroguanidine.


The whole zoo of related compound that can be made with it is interesting, but of rather academical interest, because I cannot get the other precursor materials in quantity.
Guanidine nitrate and sulphuric acid - OK, but not the rest.


By "Quantity" I mean amounts an amateur experimentor would work with, like 10g - 20g SCs.

PHILOU Zrealone - 23-12-2015 at 12:41

Quote: Originally posted by Praxichys  
Here's a thread I made a few years back which contains a ton of info on these guanidine compounds:

http://www.sciencemadness.org/talk/viewthread.php?tid=17908

Interesting, thank you for pointing this out!

So DougTheMapper and Praxichys are two faces of the same coin :o, a kind of schizophreny :P or simply loggin lost or the will to change?

Chisholm - 24-6-2017 at 04:15

So my vacuum pump has failed, and I'm having to do gravity filtration of the nitroguanidine in a Buchner funnel. This is an extremely slow process due to the fine particle size.

I want to preserve the liquid, so I can boil it down to recover the sulfuric acid, but I'm concerned about the stability of nitroguanidine in acid. I know that the concentrated solution from the addition of guanidine nitrate to sulfuric acid, if left to stand, eventually fails to produce nitroguanidine upon dilution (CoPaE). But is NQ degraded in 25-20% sulfuric acid?

[Edited on 6-24-2017 by Chisholm]