Nitroguanidine Synthesis Essay


 Pages:  1  2  3
Author: Subject: Nitroguanidine
underground

Nitroguanidine


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



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...



Women are more perilous sometimes, than any hi explosive.
Antiswat



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



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
Hazard to Others





Posts: 177
Registered: 29-3-2013
Member Is Offline

Mood: No Mood



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





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





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



Women are more perilous sometimes, than any hi explosive.
golfpro
Banned





Posts: 179
Registered: 18-5-2013
Member Is Offline

Mood: Cap Sensitive



"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



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"




???





[Edited on 21-10-2013 by underground]
underground



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



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



VladimirLem
Hazard to Others





Posts: 204
Registered: 24-5-2010
Member Is Offline

Mood: Have no fear <Vlad> is here.



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 ) ...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



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.



Women are more perilous sometimes, than any hi explosive.
golfpro
Banned





Posts: 179
Registered: 18-5-2013
Member Is Offline

Mood: Cap Sensitive



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



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
Hazard to Others





Posts: 204
Registered: 24-5-2010
Member Is Offline

Mood: Have no fear <Vlad> is here.



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
Banned





Posts: 179
Registered: 18-5-2013
Member Is Offline

Mood: Cap Sensitive



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
Hazard to Others





Posts: 177
Registered: 29-3-2013
Member Is Offline

Mood: No Mood





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
Hazard to Others





Posts: 203
Registered: 10-5-2013
Location: Northern Europe
Member Is Offline

Mood: No Mood



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



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



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



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
Hazard to Others





Posts: 204
Registered: 24-5-2010
Member Is Offline

Mood: Have no fear <Vlad> is here.





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
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)

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

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

underground



Quote: Originally posted by VladimirLem  


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
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)

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

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
Hazard to Others





Posts: 204
Registered: 24-5-2010
Member Is Offline

Mood: Have no fear <Vlad> is here.



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
 Pages:  1  2  3


IUPAC Name

2-nitroguanidine

InChI

InChI=1S/CH4N4O2/c2-1(3)4-5(6)7/h(H4,2,3,4)

InChI Key

IDCPFAYURAQKDZ-UHFFFAOYSA-N

Canonical SMILES

C(=N[N+](=O)[O-])(N)N

MeSH Synonyms

nitroguanidine, nitroguanidine monopotassium salt

Depositor-Supplied Synonyms

Nitroguanidine, 2-Nitroguanidine, 556-88-7, 1-NITROGUANIDINE, Guanidine, nitro-, Picrite, N-nitroguanidine, N”-Nitroguanidine, Guanidine, N-nitro-, Guanidine, 1-nitro-, Picrite (the explosive), Guanidine, 1-nitro- (wet), .alpha.-Nitroguanidine, N1-Nitroguanidine, Nitroguanidine, wet, N(1)-Nitroguanidine, .beta.-Nitroguanidine, UNII-NAY6KWL67F, NSC 41036, CHEBI:39180, HSDB 5693, IDCPFAYURAQKDZ-UHFFFAOYSA-N, EINECS 209-143-5, UN0282, UN1336, AI3-16306, Nitroguanidine or picrite, dry or wetted with < 20% water, by mass, WLN: WNMYZUM, ACMC-1AUQS, AC1L1WRY, DSSTox_CID_4222, NAY6KWL67F, 1-nitroguanidine derivatives, 2-nitroguanidine derivatives, AC1Q28IM, DSSTox_RID_77331, DSSTox_GSID_24222, N17351_ALDRICH, KSC270M6H, UN 0282 (Salt/Mix), UN 1336 (Salt/Mix), ARONIS24123, Ex169, SCHEMBL107616, CHEMBL3187135, CHEBI:39181, CHEBI:84772, CHEBI:84773, CTK1H0663, MolPort-001-779-752, LTBB000482, NSC41036, Tox21_200886, BBL025828, NSC-41036, STL168029, [Oxido(oxo)hydrazono]methanediamine #, AKOS005111009, AKOS006223445, MCULE-1616315638, RP18820, RTR-019634, TRA0058682, NCGC00248865-01, NCGC00258440-01, AN-23689, CAS-556-88-7, LS-73828, OR021574, OR284513, DB-052774, TR-019634, FT-0632385, N0206, Z-0713, A830754, I14-1997, W-105552, 3B3-020200, Nitroguanidine or picrite, dry or wetted with <20% water, by mass, Nitroguanidine, wetted or picrite, wetted with not <20% water, by mass, Nitroguanidine or picrite, dry or wetted with <20% water, by mass [UN0282] [Explosive 1.1D], Nitroguanidine or picrite, dry or wetted with <20% water, by mass [UN0282] [Explosive 1.1D], Nitroguanidine, wetted or picrite, wetted with not <20% water, by mass [UN1336] [Flammable solid], Nitroguanidine, wetted or picrite, wetted with not <20% water, by mass [UN1336] [Flammable solid]

Removed Synonyms

CID11174

0 comments

Leave a Reply

Your email address will not be published. Required fields are marked *