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DubaiAmateurRocketry
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Quote: Originally posted by kratomiter  | I diluted the solution with water to make it easy to crystallize, but this can make unprotonated ANQ to crystallize also. Heated by flame on aluminium
foil it releases lots of white fumes, leaving litle residue.
I don't have any equipment to analyze it, but could be an interesting propellant if it's actually ANQ nitrate. |
ive never played with ANQ, try burn it, do you obtain the same result?
Do you have any thin volumetric tube ? You can try determine the density using it. Get a liquid that most likely will not dissolve this salt, like
benzene or hexane (I could be wrong), for the purpose.
If you obtained for example, nitroguanidine, the density is significantly lower. If say nitration failed and you still have ANQ, the density is also
significantly lower than actual ANQ nitrate.
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PHILOU Zrealone
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| Quote: Originally posted by DubaiAmateurRocketry | | Quote: Originally posted by kratomiter | I diluted the solution with water to make it easy to crystallize, but this can make unprotonated ANQ to crystallize also. Heated by flame on aluminium
foil it releases lots of white fumes, leaving litle residue.
I don't have any equipment to analyze it, but could be an interesting propellant if it's actually ANQ nitrate. |
ive never played with ANQ, try burn it, do you obtain the same result?
Do you have any thin volumetric tube ? You can try determine the density using it. Get a liquid that most likely will not dissolve this salt, like
benzene or hexane (I could be wrong), for the purpose.
If you obtained for example, nitroguanidine, the density is significantly lower. If say nitration failed and you still have ANQ, the density is also
significantly lower than actual ANQ nitrate. |
I would suggest the sink or float test of a single cristal into a saturated solution of ZnCl2 or NaI into water set at a density of 1.8
Then nitroguanidine (d= 1.71) or ANQ (d= 1.72) will float while ANQN (d=1.91) will sink...
[Edited on 25-5-2016 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Microtek
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Assuming that the ANQ nitrate dissociates completely on dissolving in water (not a given), recrystallizing from water would be equivalent with
recrystallizing ANQ from very dilute nitric acid - which is reported to give only ANQ. I recommend just washing the product with isopropanol and then
drying.
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kratomiter
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I'm sorry, I don't have any resource to determine the density. It was a mess because of the large amount of nitric acid. I'll repeat it again in the
future, now I'm busy.
Microtek: I didn't think it, but maybe you're right, depending on ANQ's pKa. My knowlegment in chemistry is low. Maybe could I differentiate between
ANQ or ANQ nitrate measuring the pH? ANQ nitrate should be fairly acidic.
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PHILOU Zrealone
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| Quote: Originally posted by kratomiter | I'm sorry, I don't have any resource to determine the density. It was a mess because of the large amount of nitric acid. I'll repeat it again in the
future, now I'm busy.
Microtek: I didn't think it, but maybe you're right, depending on ANQ's pKa. My knowlegment in chemistry is low. Maybe could I differentiate between
ANQ or ANQ nitrate measuring the pH? ANQ nitrate should be fairly acidic. |
Yes Microtek is right about dilution into water for recrystalization...it ruins your ANQN and sets HNO3 free
Determination of pH will be much less practical than density...
Because pH can be done with pH-meter but is not very effective for the regio below pH=1; same applies for pH-paper or pH indicators...
I doubt you don't have the resource to determine density...you simply need:
-a scale (the more sensitive, the lowest the quantity of solution you need)
-a graduated recipient (or a given volume recipient; ideally a volumetric flask (measuring flask or graduated flask))
-a salt that allow for an increase of density of the solution in the wished range (1.80 g/cm³)
-a test tube
-a single "large" Crystal (ideally >1 mm)
If you can work properly even a simple test tube will do in the place of the graduated recipient. Use demi water at 20°C to calibrate and set the
volume with a thin permanent ink pen...
Ideally the salt must be unreactive towards the compound, but since the measure is a fast test, even if some dissolves and react after a few seconds
with the solution, the measure has already be done.
Alternatively with a calibrated test tube, and a larger quantity of crystals, you can do a real density measurement...
But then you need a solvent in what your compound doesn't dissolve and that is lighter than your compound --> d<1.6
1°)Weight tube empty (E)
2°)Weight tube with demi water up to calibration line (W)
3°)Empty the tube and dry the tube
4°)Fill tube with solvent up to line and weight (S) then add rod then weight(S+R)
5°)Introduce crystals into the tube by tiny portions while stirring with the rod (to take bubbles away)
6°)Weight tube+solvent+crystals+rod (T)
7°)Lift the rod above tube and allow all drops to fall into tube; then take excess solvent above the line away with a pipette and replace the rod in
tube...then weight.(T')
With all this you know that density of water arround 20°C is approx 1.00 g/cm³; so:
a) W-E is the weight of water (=volume) under the line
b) (S-E)/(W-E) is the density of S vs water (dS)
c) T-(S+R) is the weight of crystals you added
d) T-T' is the weight of displaced solvent
--> Since you know dS you may find the volume of displaced solvent = (T-T')/dS = (T-T')*(W-E)/(S-E)
--> you can find the density of your compound = weight of crystals/volume displaced
= (T-(S+R))*(S-E)/((T-T')*(W-E))
[Edited on 27-5-2016 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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kratomiter
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Thank you PHILOU for your clear explanation, but the yield was low, so I have make the salt again and then try to measure the density.
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Microtek
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I just found this (theoretical) paper on the intercalation compound between hexagonal boron nitride (used in lubricating systems so it should be
possible to procure it) and fuming nitric acid.
The compound has given very high values in calculations with thermochemical code, far in excess of current high performance energetics. However, I
haven't been able to find any experimental accounts.
Attachment: Intercalated BN_HNO3.pdf (2.6MB)
This file has been downloaded 1085 times
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MineMan
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Microtek, you got me excited there... But this paper is 21 years old, surly we would have heard more on this by now if it were sucsussful.
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PHILOU Zrealone
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| Quote: Originally posted by MineMan | | Microtek, you got me excited there... But this paper is 21 years old, surly we would have heard more on this by now if it were sucsussful.
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The mix HNO3/BN may be very powerful but unpractical owing to the corrosive, toxic and hazardous fuming HNO3.
A bit like Axt's ANNMSA mix:
AN = NH4NO3 (ammonium nitrate)
NM = CH3-NO2 (nitromethane)
SA = H2SO4 (concentrated sulfuric acid)
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Microtek
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It is also possible that the method that was used in estimating the performance parameters (VOD 18 km/s and Pcj 640 kBar) was not suitable for this
system, and grossly overestimated the performance.
Still, the report on page 6 of this thread (first post on that page, by Franklyn) titled "The Future of Warheads Armor & Ballistics" was published
in 2007, and the table in the report that lists the BN/HNO3 intercalated compound is based on a Swedish military report from 2006, so it was thought
possible 10 years ago.
So, the point I'm trying to make here, is that given that the precursors are cheap and readily available (ebay has lots of postings for hexagonal
boron nitride), perhaps it would be worth an experiment or two. I have ordered a paper that hopefully has some experimental details on the proces of
making intercalated compounds of BN and Brønsted acids.
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MineMan
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Yah! I am excited to hear your results and updates. 18km/s... even if the real value is 9500m/s I will be excited.
Does anybody have any idea of the VOD of Axt's mixture?
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nitro-genes
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That's amazingly fast, I presume the boron nitride's incredible speed of sound is one of the properties of the BN-HNO3 composition that makes it this
fast?
Somewhat off topic maybe, but similar: If you would have a reducable (high energy potential) ceramic like material with very high speed of sound and
powder it like using aluminium powder, would it be possible to have thermobaric effects with almost no loss of brisance?
Something like this, a corrosion resistant magnesium/lithium alloy with very high energy potential:
http://www.asminternational.org/news/industry/-/journal_cont...
Or use dopes to increase material hardness and speed of sound, like this:
https://www.newscientist.com/article/dn11093-diamond-loses-i...
Or would the speed of sound be negatively affected by inhomogenity and only be that high in single compound materials?
[Edited on 1-9-2016 by nitro-genes]
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Microtek
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So, now I've had the opportunity to read an experimental paper on the preparation of intercalates of hexagonal boron nitride and a number of Brønsted
acids. It's a good news/bad news situation:
The good: The preparation of intercalates is extremely simple; you simply add hBN (which they bought from an abrasives company in a particle size
range of up to 10 um, and used without any additional treatment) to the desired acid in a test tube, stir it with a glass rod, let it settle and
decant the excess acid. Then the slurry is heated to dryness, at atmospheric pressure or lower.
The bad: Using nitric acid does not yield any sign of an intercalated compound... However, perchloric acid does. I would suppose that the intercalated
compound of hBN and perchloric acid is comparable to the one with nitric acid. It is often the case in papers that use computational methods to
predict explosive performance, that perchlorates are omitted. This is probably due to the thermochemical code not working well with this class of
salts, so I am guessing that this may also be the reason that it was the HNO3 intercalate that was mentioned in the paper on future energetics.
If it works, the compound with perchloric acid could have the advantage of being much less volatile than nitric.
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MineMan
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Ok, any reports of experimental VOD or volume of gas produced?? Please keep us updated.
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PHILOU Zrealone
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| Quote: Originally posted by nitro-genes | That's amazingly fast, I presume the boron nitride's incredible speed of sound is one of the properties of the BN-HNO3 composition that makes it this
fast?
...
Or would the speed of sound be negatively affected by inhomogenity and only be that high in single compound materials?
|
The speed of sound into a dense hard mono-cristal is not the same as the speed of sound into a powdery material surrounded by a gas or by a
liquid...the weakest link will prevail into the speed of sound for this second case...thus the gas or the liquid...and into the present BN/HNO3
case...the HNO3 what should not be that fast (although into the range of km/s but below the 2-3 km/s what is weak in comparison of detonating
explosives).
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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PHILOU Zrealone
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| Quote: Originally posted by MineMan | Yah! I am excited to hear your results and updates. 18km/s... even if the real value is 9500m/s I will be excited.
Does anybody have any idea of the VOD of Axt's mixture? |
It must be between 6500 and 8000 m/s and more probably between 7000 and 7500 because of its brisance described by Axt.
CH3-NO2 alone already goes to 6300 m/s @ d= 1,14 ...
But here we are denser because of the free HNO3, the H2SO4, NH4NO3 and NH4HSO4.
Also part of the NH4HSO4 produced is a dead weight.
Into the mix one may consider the partial formation of NH2OH (hydroxylamine from CH3-NO2 and acid) whose nitrate has a VOD of 8000 m/s...
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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PHILOU Zrealone
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The volume of detonation gases can be calculated from the chemical equations...
10 BN + 6 HNO3 -->5 B2O3 + 3 H2O +8 N2 (11 moles of gases)
8 BN + 3 HClO4 -->4 B2O3 +3 HCl + 4 N2 (7 moles of gases)
The volume of gases will not be exceptional because of the solid/liquid B2O3.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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alkynes of trouble
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Interesting explosive, DPX-26. RDX performance but much less sensitive.
http://onlinelibrary.wiley.com/doi/10.1002/anie.201608723/ab...
Can somebody provide the paper?
| Quote: |
The reaction of 3-amino-5-nitro-1,2,4-triazole with nitrous acid produces the corresponding diazonium salt. When the diazonium salt is treated with
nitroacetonitrile, a subsequent condensation and cyclization reaction occurres to produced 4-amino-3,7-dinitrotriazolo-[5,1-c][1,2,4] triazine
(DPX-26). X-ray crystallographic analysis shows that the DPX-26 has a density of 1.86 g cm−3, while it is calculated to have a heat of formation
of 398.3 kJ mol−1. DPX-26 is predicted to approach the explosive performance of RDX but displays significantly better safety properties.
Oxidation of DPX-26 using hypofluorous acid produces 4-amino-3,7-dinitrotriazolo-[5,1-c][1,2,4] triazine 4-oxide (DPX-27), which is also predicted to
be a high-performance material with enhanced safety properties. |
[Edited on 11-11-2016 by alkynes of trouble]
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PHILOU Zrealone
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| Quote: Originally posted by alkynes of trouble | Interesting explosive, DPX-26. RDX performance but much less sensitive.
http://onlinelibrary.wiley.com/doi/10.1002/anie.201608723/ab...
Can somebody provide the paper?
| Quote: |
The reaction of 3-amino-5-nitro-1,2,4-triazole with nitrous acid produces the corresponding diazonium salt. When the diazonium salt is treated with
nitroacetonitrile, a subsequent condensation and cyclization reaction occurres to produced 4-amino-3,7-dinitrotriazolo-[5,1-c][1,2,4] triazine
(DPX-26). X-ray crystallographic analysis shows that the DPX-26 has a density of 1.86 g cm−3, while it is calculated to have a heat of formation
of 398.3 kJ mol−1. DPX-26 is predicted to approach the explosive performance of RDX but displays significantly better safety properties.
Oxidation of DPX-26 using hypofluorous acid produces 4-amino-3,7-dinitrotriazolo-[5,1-c][1,2,4] triazine 4-oxide (DPX-27), which is also predicted to
be a high-performance material with enhanced safety properties. |
[Edited on 11-11-2016 by alkynes of trouble] |
There is a place for that into the forum 
Reference section: Wanted references, book or articles
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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PHILOU Zrealone
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| Quote: Originally posted by PHILOU Zrealone | | Quote: Originally posted by alkynes of trouble | Interesting explosive, DPX-26. RDX performance but much less sensitive.
http://onlinelibrary.wiley.com/doi/10.1002/anie.201608723/ab...
Can somebody provide the paper?
| Quote: |
The reaction of 3-amino-5-nitro-1,2,4-triazole with nitrous acid produces the corresponding diazonium salt. When the diazonium salt is treated with
nitroacetonitrile, a subsequent condensation and cyclization reaction occurres to produced 4-amino-3,7-dinitrotriazolo-[5,1-c][1,2,4] triazine
(DPX-26). X-ray crystallographic analysis shows that the DPX-26 has a density of 1.86 g cm−3, while it is calculated to have a heat of formation
of 398.3 kJ mol−1. DPX-26 is predicted to approach the explosive performance of RDX but displays significantly better safety properties.
Oxidation of DPX-26 using hypofluorous acid produces 4-amino-3,7-dinitrotriazolo-[5,1-c][1,2,4] triazine 4-oxide (DPX-27), which is also predicted to
be a high-performance material with enhanced safety properties. |
[Edited on 11-11-2016 by alkynes of trouble] |
There is a place for that into the forum
Reference section: Wanted references, book or articles |
Now available thanks to Solo into the reference section...
Alkyne of troubles was too lazy to do it   ...so I did it
Don't forget to add the ".pdf" at the end to be able to read it (under adobe...or other pdf reader)
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Laboratory of Liptakov
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active plasticizer
With successful was synthesized active plasticizer from hexamine and NH4CLO4. His properties show on same bonding effect as classic plasticizers as is
oil and polyisobutylene rubber (PIB). However his oxygen balance is - 86, against classic (PIB), where is - 346. His properties will next researched.
Seems, that is non hygroscopic. Basic preparation is of course slightly dangerous. On the "Philou's" testing spoon is insert 0,2g hexamine and 0,2g
NH4ClO4 and 3g H2O. By 100C is all dissolve and run evaporate water. Heating is increase to cca 250 - 280 C (no measured). From both compound firstly
arises partially heterogenous mixture, which after a few seconds is changed on transparent slightly brown solution. In this point is is necessary
heating stopped and "Philou" spoon is insert on water level. After 10 second temperature decrease on 20C and plasticizer is ready to use. If is
plasicizer heated over 350 - 400 C, his color changed on black and bubbled. After bubbling material deflagrated with a same effect as ETN, which is
heated. Thus very long and fast flame. Very effective. In closure alu foil not show detonation properties. Against ETN. Very interesting is, that by
ratio 66% AP and only 33% hexamine, arises sparse material, which making the drip. Which is weird. Should be exactly conversely. In basic ration 1:1
has material properties and color almost same as density the Honey. But smell is, as old the Coyote.
......Dr....
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
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MineMan
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LoL,
How did you come up with this idea?? Interesting.
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Laboratory of Liptakov
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active plasticizer
The plasticizer was discovered during the examination of the mother liquor from the reaction - recrystalisation from copper hexamine perchlorate.
But one test, nothing test. 10 test = 1 test. 100 test can bring relevant results or half of truht. Last attempts show, that for example flour,
requires 40% this plastificator, which is too for some applications. But because every gram of this plasticizer content 50 % NH4ClO4, and 50% one from
best energetic fuel, is posssible maybe some construction final energetic mixture, with OB - 20, or even near zero. Because is possible adden only
oxidizer, AN, or AP and slightly Al, and plastic material is ready to testing. Dr.
[Edited on 2-8-2017 by Laboratory of Liptakov]
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
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Laboratory of Liptakov
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Next attempts show, that this plasticizer is very hygroscopic if is mixed with some energetics materials. Examination stopped. Dr.
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
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Mr.Greeenix
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-Ammonium-dinitroguanidine (ADNQ)
-1,7-diamino-1,7-dinitrimino-2,4,6-trinitro-2,4,6-triazaheptane (APX)
Both Materials possess very good detonation parameters:
APX (Vdet = 9540 m·s–1, pC–J = 395kbar, Qv = –5935 kJ·kg–1)
ADNQ (Vdet = 9066 m·s–1, pC–J = 332 kbar, Qv = –5193 kJ·kg–1),
with moderate safety parameters:
APX: IS ≥ 3 J, FS ≥ 80 N and ESD ≥ 0.1 J
ADNQ: IS ≥ 10 J, FS ≥ 252 N and ESD ≥ 0.4 J,
Two very interesting compounds, however preparing dinitroguanidine seems to be a problem i think.
Attachment: (ADNQ) and APX.pdf (905kB)
This file has been downloaded 915 times
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