Sciencemadness Discussion Board

NIHT/NHHT Synth Suxess!

Hey Buddy - 7-12-2022 at 22:02

Nitroguanidine and Hexamine can be fragment-cyclized to 2-Nitriminohexahydro-1,3,5-triazine monhydrochloride (referred to in lit. as NHHT or NIHT) with hardware store muriatic acid under mild conditions and basic equipment.
NHHT is reported (without verification) to detonate at 9000m/s velocity with a density of 1.95g/cc (Yongzhong, Synthesis of Polynitrocompounds from Nitroguanidine, propellants, Explosives, Pyrotechnics 14, 150-152 [1989]).
It's futrther reported that the compound "explodes" on heating to 102 C. Other literature claims m.p. 189 C without mention of explosion.
This material came to attention during the failure to synthesize NTNT "new melt cast explosive", as a possible side reaction. Preparation of this compound was attempted by literature procedures by (me)hey buddy, repeatedly, without success. The reported high performance, simple preparation and ionic nature of this compound make it very unique in its class as a triazine, and its preparation would be beneficial to the arsenal of explosive material enthusiasts. As a compound, NHHT is regarded in the defense industry highly, and is "compared" with RDX and CL-14 as an approximate in that class. Whether this comparison is realistic or not remains unknown as this compound somewhat unfamiliar to explosive researchers, but because of its ease of preparation, should be.





Artboard 1.jpg - 254kB

[Edited on 8-12-2022 by Hey Buddy]

Successful Procedure

Hey Buddy - 7-12-2022 at 22:13

Successful rendering of NHHT was not precipitated by Metelkina's literature procedure in "2-Nitroguanidine Derivatives: X Synthesis and Nitration of 4-Nitrininotetrahydro-1,3,5-oxadiazine and 2-Nitrinino-1,3,5-triazine and their Substituted Derivatives". This procedure in my attempts failed repeatedly. At some point in time I found an old file saved on my computer titled "NIHT" which is referring to the same compound by different acronym. I have no memory of where this file came from. It is most certainly from a thread on SM from the past, but I cant find it. This procedure is in the attached picture. This procedure was successful scaled down, in many variations. The primary factor of success is closed vessel and long term reaction time.

NIHT_HCl.png - 299kB

Hey Buddy - 7-12-2022 at 22:27

Scaled down version:
150ml HCl (sunny side, muriatic)
8.2 g Nitroguanidine (NQ)
20 g Hexamine (Hx)

No cooling is employed in this reaction and it takes place at ambient temperature with exothermic response upon addition of hexamine.

Reaction is carried out in a 1000 ml boiling flask. Teflon tape is stretched across the opening of the boiling flask which allows the flask to off-gas but refuses entrance of air which can affect yield. The teflon tape was secured by wrapping it with some electrical tape around the boiling flask neck. This tape remained in place the entire 8 Hours of reaction to prevent ingress of air.

150 ml HCl is added into reaction vessel.
8.2 g NQ is added and stirred until entirely dissolved at room temperature.
20 g Hx is added to reaction vessel in one portion, stirring continues
Reaction vessel is closed from ingress of atmospheric air
Reaction is continued with stirring and without cooling for 8 Hours
Reaction media becomes banana colored and opaque
At conclusion of 8 hours, 500 ml dH2O is added to reaction to quench it
White opaque solution is precipitated
Filter and wash with dH20

NHHT*HCl is ionic and may have application as a high energy ligand in coordinated explosive complexes such as prospective complex: e.g. [M(NHHT)x(ClO4)y] / [M(NHHT)x(NO3)y]



_MG_9226.jpg - 167kB _MG_9221.jpg - 125kB _MG_9229.jpg - 187kB _MG_9230.jpg - 183kB



[Edited on 8-12-2022 by Hey Buddy]

underground - 7-12-2022 at 23:20

That is very nice. I had upload that file in the past, you can find it at the "trying for keto RDX" together with some other files. How much was your final yields ? Will you convert it to nitrate salt, then use H2SO4 for the dinitrate (NNHT) ?

[Edited on 8-12-2022 by underground]

Laboratory of Liptakov - 8-12-2022 at 04:28

It seems easy.....And the substance on filter is explosive, or only precursor ? I readed all twice. But is it not clear for me. Thanks.

underground - 8-12-2022 at 04:36

It is not. It is the HCL salt. The nitrate/perchlorate salt should be though.

Hey Buddy - 8-12-2022 at 08:46

Quote: Originally posted by Laboratory of Liptakov  
It seems easy.....And the substance on filter is explosive, or only precursor ? I readed all twice. But is it not clear for me. Thanks.


Sorry to be unclear. It is confusing researching the compound because there are contradictory statements in literature, and multiple acronyms. This method prepares the HCl salt. According to literature, the HCl salt detonates at 9000m/s. This is unverified and I can find little cross reference material supporting this. NHHT when nitrated with H2SO4 or NH4Cl produces NNHT which has a nitramine group at the number 5 triazine position. NNHT is considered a high energy insensitive secondary explosive.

The HCl salt has been of interest to me due to possible decomposition at 102 C as is claimed in literature, which in the case of "NTNT" was a concern. It appears this claim is incorrect about an explosive decomp at 102 C. My further interest in this material is the prospect of preparation of basic perovskite explosive complexes from NHHT as an easy ligand, because of its ability to form salts. The character of the NHHT*HCl is unknown and may be misreported where found. To the best of my understanding now, the HCl salt is still very high velocity in detonation and high density. I have not begun testing on the material yet, the first sample is drying and I prepared a 2x scale sample that is on filter right now. Theoretically, NHHT*HCl should serve as a high energy ligand in a perchlorate or nitrate complex and its sensitivity should be somewhat adjustable by experimenting with the oxidizer and metal of the complex.

I will add a yield when the first batch is dry. I can see now it is low yield, I think extending the reaction time will increase yield. Any yield at all is a good first step because I have failed to yield anything so many times in attempt of NHHT HCl. The second batch was left to react longer and I will post that info too when dry.

EDIT: I dried some on a pan at ~44 C but I didn't move the material around while drying, just left it on the pan, some of it turned yellow but appears not to be a major decomposition. 6 g was the total yield, which is lower than expected and is probably due to 8 hour reaction time 12 hours of reaction would probably yield more product. I would also recommend a larger washing with water bath at end of reaction to make less acidic.

[Edited on 8-12-2022 by Hey Buddy]

Laboratory of Liptakov - 8-12-2022 at 10:04

Thanks. On paper is acidic salt of HCl. Is it explosive with low sensitivity (or unknown sensitivity).
Therefore is impossible do it neutralisation for example baking soda. Or using else alkaline neutralisation. (NaOH, KOH, NH4OH) ...?... this salt (NNHTxHCl) can react with HClO4...?...for create some better material? Thanks.

Hey Buddy - 8-12-2022 at 11:07

Quote: Originally posted by Laboratory of Liptakov  

Therefore is impossible do it neutralisation for example baking soda. Or using else alkaline neutralisation. (NaOH, KOH, NH4OH) ...?... this salt (NNHTxHCl) can react with HClO4...?...for create some better material? Thanks.


Should be able to use acid or double replacement reaction to change the anion with any negatively charged one like CLO4. It should be able to be neutralized relulting in the free base. It should be able to create lots of materials with different properties. The HCl should already be energetic. I will test hammer and burn test on the regular HCl salt and then try a Cu and Ni salt. I will do this with the guanidine thread also and post result. I will not be treating the NHHT with HNO3/HClO4 because my interest is to push away from these in reliance and simply learn metathetical reactions with acid salts to reduce reagents.

Microtek - 8-12-2022 at 23:17

The question is how labile such salts might be. I found that aminonitroguanidine nitrate loses nitric acid over time due to being a quite weak base. Seeing that NHHT*HCl is reportedly freebased by treating with hot 18% HCl, NHHT must be an exceedingly weak base.

Laboratory of Liptakov - 9-12-2022 at 02:58

HCl salt, preparation by description above. Run was 8 hours stirring at 17 Celsia. + 8 hours without stirring at 22 Celsia. . After this at 20 C no any precipitat in yellow solution. After cooling on + 5C arise precipitate. Vacuum filtered. HCl salt has not any energetic properties. Nothing burning, no flame on alu foil. Only smoke and smell similar as hexamine. Big hammer test repeatedly, but without any explo.





cipi.JPG - 198kB

acid saltNHHT.jpg - 249kB

underground - 9-12-2022 at 03:18

I was not expecting the HCL salt to be energetic. What was your yields? Try the nitrate/perchlorate salt. The nitrate salt probably can be treated with H2SO4 to form NNHT.

Laboratory of Liptakov - 9-12-2022 at 03:32

Nitrate/ perchlorate from HCL salt will examinate later. Within some days. Yield will measure also later. After dry process.

[Edited on 9-12-2022 by Laboratory of Liptakov]

Hey Buddy - 9-12-2022 at 19:44

Quote: Originally posted by Laboratory of Liptakov  
HCl salt has not any energetic properties. Nothing burning, no flame on alu foil. Only smoke and smell similar as hexamine. Big hammer test repeatedly, but without any explo.


I made an error. The Yongzhong P.E.P. article clearly claims that the HCl salt is Vd 9000m/s, explodes at 102 C. This misinformation has caused a lot of confusion for me. Maybe they mixed up their molecules?-- The comparison to CL-14 is to NNHT not NHHT as I suggested. I went back and found the NNHT power point where that comparison is made and realized my mistake, sorry about that.

Darn. Was really hoping the literature was accurate on this molecule being energetic. I tried a Cu ClO4 * NHHT --by CuSO4*5H2O + NH4ClO4 and had no precipitation. Tried isopropyl extraction that sometimes works with other combinations and got no crystals... I tried adding another ligand to see if it would co-precipitate. Now I just have a jar full of random non explsive things.

I made a second batch of NHHT*HCl, I will test it on big hammer and burn to double verify.
If the HCl salt is not energetic, but you do want it to be energetic, if you nitrate it in H2SO4 it should form an energetic compound. NNHT. Here is a defense industry power point on NNHT.
Attachment: Nnht.pdf (368kB)
This file has been downloaded 152 times

Microtek, I'm sure you're right. I'm unfamiliar with coordination chemistry. --This is off topic, but Microtek, do you think "Allantoin" could be interesting in typical perovskite coordination ie. allantoin metal perchlorate? I found some affordable as a womens cosmetic supply, so I ordered a bag of it.



allantoin.jpg - 93kB

[Edited on 10-12-2022 by Hey Buddy]

cause it looks kind of interesting to me... im curious, anyways...

[Edited on 10-12-2022 by Hey Buddy]

Microtek - 11-12-2022 at 01:34

I can't say that I'm any kind of expert in that area myself, but I agree that the molecule has the look of something that could be both dense and energetic if a few nitro groups were introduced. You could probably also just make a perchlorate or nitrate salt (searching on the web yields a few references to the nitrate but none that I can find to the perchlorate), but I think you need to experiment to establish the stability, hygroscopicity, etc.

Hey Buddy - 28-12-2022 at 07:51

I have finally gotten around to double-verifying NHHT is not energetic to burn nor hammer. Too bad. NHHT salts/complexes seem like the next step in exploration.

underground - 10-7-2023 at 12:33

I just spend few minutes to draw the derivatives form NQ/Urea + Hexamine

Also the Dinitrate/Diperch salts may also exist from the low nitrated derivatives

1.png - 46kB



[Edited on 10-7-2023 by underground]

Hey Buddy - 10-7-2023 at 14:18

The general theme of this thread was NHHT, but in the hopes of something more powerful from nitroguanidine. Here are some related compounds from nitroguanidine. The second paper has some (bis)nitroguanidine methane heterocycles that look pretty interesting and simple.

These images are all from the second polynitro paper. They report the open molecule [7] to be 1.93g/cc but have Vd @ 1.83g/cc of 9020 m/s but with a decomp only slightly over 100 C. Not sure if the hexamine/NQ/HNO3/H2SO4 would be more powerful, but you can take that molecule and treat it with NaOH then free it from the sodium to get [7]. Thats according to the article. Or you can use ammonia and leave the NH4 as cation. Hydrazine would be interesting.

The most interesting is the bis nitroguanidine [9], and molecule [11] which is a sort of dinitrimino heterocycle. Theres also [15] which is an oxadiazine, I have no idea how that would perform but it is interesting with the oxygen in the frame of the molecule.

Attachment: nitroguanidine derivatives.pdf (134kB)
This file has been downloaded 88 times

Attachment: nitroguanidine poly nitro compounds Zhuang.pdf (283kB)
This file has been downloaded 94 times
nq1.jpg - 337kB
nq2.jpg - 162kB
nq3.jpg - 54kB
nq4.jpg - 26kB
nq5.jpg - 47kB

Hey Buddy - 10-7-2023 at 14:45

Quote: Originally posted by underground  
I just spend few minutes to draw the derivatives form NQ/Urea + Hexamine

Also the Dinitrate/Diperch salts may also exist from the low nitrated derivatives





[Edited on 10-7-2023 by underground]


IIRC, microtek didn't think number 1 and 2 would be good candidates for further salts, although I didn't attempt it either way, I do have some NHHT sitting around... I sort of lost interest when I realized NHHT didn't explode on heat as claimed in a paper.

Did LL ever get aaround to testing NHHT nitrate perchlorates? He mentioned he might try that. Check the polynitro paper for [3] which is the product of mixed acid treatment. Probably would work with nitrate salt/H2SO4/. It is more realistic than any of the higher nitros requiring Ac2O. I suppose its possible the higher nitros such as 'z' rdx compound [2] may possibly be accessible without Ac2O via hexamine dinitrate route.

[Edited on 10-7-2023 by Hey Buddy]

[Edited on 10-7-2023 by Hey Buddy]

underground - 10-7-2023 at 15:41

The NHHT nitrate and perchlorate seems the most atractive to me since they would be dead easy to make

Hey Buddy - 10-7-2023 at 15:52

Quote: Originally posted by underground  
The NHHT nitrate and perchlorate seems the most atractive to me since they would be dead easy to make


Thats true. I have the HCl right now. Not sure the best bet to freebase? I could try NO3. Could also attempt NH4ClO4 driven displacement. Ive got a few grams of NHHT sitting around...

Do you think 3 and 4 are even possible? It seems unlikely to me.

[Edited on 10-7-2023 by Hey Buddy]

underground - 10-7-2023 at 16:03

To remove the hcl from NHHT you have to add a stronger base like NaOH in order to absorb the HCL . NHHT freebase will yield.

Another way is to dissolve NHHT HCL and silver/lead nitrate/perch at equal molarity. Lead hcl and Silver hcl will ppt out since they are almost insoluble in water. NHHT HNO3/HCLO4 will remain dissolved in solution

NHHT Nitrate added to Concentrated H2so4 most likely will yield 3-4 freebase.
The perchlorate salt ( 3 ) may exist since perchloric acid is a very strong acid. Not sure about 4

NHHT HCL molar mass:
C3H8N5O2Cl -->12.011*3+1*8+14*5+16*2+35.453= 36,033+8+70+32+35,453= 181,5 g/mol

NaOH molar mass is 40g/mol

So for every 181.5g of NHHT HCL you have to add 40g of NaOH to freebase it

Note that NHHT freebase may still be soluble in water. If that is the case then you have to evaporate all the water so you will end up with a mixture of NHHT and NaCL. Then extract the NHHT with an organic solvent.

The silver nitrate route would be the best though IMO

HCLO4 acid is stronger than HCL acid so adding an equal molar mass of NHHT HCL and HCLO4 will yield NHHT HCLO4. Upon evaporation HCL acid will go off


[Edited on 11-7-2023 by underground]

Hey Buddy - 10-7-2023 at 17:08

Ok AgNO3 metathesis it is then.

It worked okay. There is a bit of silver nitrate in filtrate. The AgCl was totally insoluble. I heated it up a bit to increase nitrate solubility for separation. Evaporating filtrate now...

[Edited on 11-7-2023 by Hey Buddy]

underground - 11-7-2023 at 01:56

Nice. Next step is to check its properties. The perchlorate salt has to be tested too. If you dont mind keep a little bit to ckeck if with H2SO4 will react at low temp (0c) to yield the 3/4 freebase (NNHT). 3/4 could also be tested and checked if the nitrate/perchlorate salt is possible.

Also the dinitratediperchlorate salt of NHHT may be possible.

This can be tested by reacting NHHT Nitrate with equal molar mass of 65% HNO3

[Edited on 11-7-2023 by underground]

Hey Buddy - 11-7-2023 at 08:15

Quote: Originally posted by underground  
Nice. Next step is to check its properties. The perchlorate salt has to be tested too. If you dont mind keep a little bit to ckeck if with H2SO4 will react at low temp (0c) to yield the 3/4 freebase (NNHT). 3/4 could also be tested and checked if the nitrate/perchlorate salt is possible.

Also the dinitratediperchlorate salt of NHHT may be possible.

This can be tested by reacting NHHT Nitrate with equal molar mass of 65% HNO3

[Edited on 11-7-2023 by underground]


"3/4" should come out as compound [3] (from polynitro paper). I dont think they can continue to hold the anions after the second nitro is added.

I suspect "5" is possible via HDN + NQ + HCl. If that were correct, 5 may have good performance with few steps. Is it possible to produce HDN without 65% NA? For instance a nitrate salt? If that were possible it would be very simple to produce "5". Z rdx decomposes at 50C which is Impractical but the nitimino with 2 nitrimines could Be much more thermally stable...

There were 2 g of NHHT converted to the nitrate, still have around 4g NHHT HCl remaining. If any of it shows promise I can whip up so more, i's pretty painless. I used quite a bit of water so it is still evaporating but I looked at it this morning and much of it has dropped out of solution already. The solution turned a tint of purple. I assume it is from reverted Ag in solution.

For NHHT nitrate, I think perhaps fire it into an Al block and dehydrate some with H2SO4 then fire that into Al for comparison? What mass of load is the standard for firing into Al cubes for comparisons, half gram?

Guess I need to prepare HDN to test if produces 5 with NQ...

[Edited on 11-7-2023 by Hey Buddy]

[Edited on 11-7-2023 by Hey Buddy]

underground - 11-7-2023 at 08:31

You can test a sample of ETN or RDX or whatever and compare to anything else. Note that density play a big role on performance.

Hey Buddy - 11-7-2023 at 08:54

I've got 1" 6061 Al block cubes. I think 500mg is common for a test like that. I can compare to melt ETN. I don't have a way to measure pressure for loading, but can try to just press it "real good".

Laboratory of Liptakov - 11-7-2023 at 10:29

After pressing don´t forgot do it mesurement of density of this 500mg. Radius x radius (in cm) x 3.14 x height (in cm)......:cool:

Hey Buddy - 11-7-2023 at 11:11

I filtered off some of the precipitate. unless it is very dense, it appears a low yield, small amount of material recovered. Gray contamination from silver in product.
In paper it is claimed dilute HCl 18% gives freebase product. Since the NHHT itself is not energetic, and requires minimally an oxidizer anion, it seems HNO3 would be more direct. Why not skip NHHT HCl and attempt nitrate from hex+NQ+HNO3? Further more, if HNO3 is used, HDN could be used in leu of hexamine, then use HNO3 as acid source...

I wonder if citric acid or acetic and ammonium nitrate could be used for NHHT*NO3


[Edited on 11-7-2023 by Hey Buddy]

Hey Buddy - 11-7-2023 at 11:16

Quote: Originally posted by Laboratory of Liptakov  
After pressing don´t forgot do it mesurement of density of this 500mg. Radius x radius (in cm) x 3.14 x height (in cm)......:cool:


Yes I will caliper the vessel and index the depth of load after pressing. Is 500 mg the standard that you use? ~8mm cylinder, SS? I hope there is enough NHHT NO3 to make 500mg...
BTW, what does "cool" emoji face mean? I always see you use it, but I don't understand. I imagine you are sun-bathing at a pool while typing on SM.

underground - 11-7-2023 at 12:17

Most likely the nitrate salt is quite soluble in water. Try to evaporate more water or to clean it up, redissolve, filter the contamination and evaporate. Did you use sticiometric amount of silver nitrate to NHHT HCL. ?

AgNO3 169,8g/mol
NHHT HCL 181,5 g/mol

So for every 1,8g of NHHT HCL you have to add 1,7g of AgNO3


You should have end up with more product when you convert it to HNO3 salt from HCL since the molar mass of the molecule have been increased. The crystal structure of nitrate salt may be quite dense

From metathesis you get 100% yields. If you did not then something is off. Maybe your NHHT HCL is not pure or something.

I am not sure if HNO3 can be used. HCL is used to break up Hexamine to methylamine. RDX is actually an isomer of 3 molecules of nitromethylamine so maybe HNO3 will work. Hexamine broke up in process to methylamine and react with NQ to form NHHT HCL. 2 moles of methylamine and 1 mole of NQ form NHHT. If the temperature go high other methylamine products may produced like dimethylamine and trymethylamine. Maybe you got some ammonium HCl as contamination.


[Edited on 11-7-2023 by underground]

Hey Buddy - 11-7-2023 at 14:25

Quote: Originally posted by underground  
Most likely the nitrate salt is quite soluble in water. Try to evaporate more water or to clean it up, redissolve, filter the contamination and evaporate. Did you use sticiometric amount of silver nitrate to NHHT HCL. ?

AgNO3 169,8g/mol
NHHT HCL 181,5 g/mol

So for every 1,8g of NHHT HCL you have to add 1,7g of AgNO3


You should have end up with more product when you convert it to HNO3 salt from HCL since the molar mass of the molecule have been increased. The crystal structure of nitrate salt may be quite dense

From metathesis you get 100% yields. If you did not then something is off. Maybe your NHHT HCL is not pure or something.

I am not sure if HNO3 can be used. HCL is used to break up Hexamine to methylamine. RDX is actually an isomer of 3 molecules of nitromethylamine so maybe HNO3 will work. Hexamine broke up in process to methylamine and react with NQ to form NHHT HCL. 2 moles of methylamine and 1 mole of NQ form NHHT. If the temperature go high other methylamine products may produced like dimethylamine and trymethylamine. Maybe you got some ammonium HCl as contamination.


[Edited on 11-7-2023 by underground]


Of course, stoichiometric. There must be something wrong with this NHHT. The remaining filtrate was left to evaporate, the last time I looked at it, it had some additional salt precipitating. Went back to check again, decomposition, brown syrup. It has to be the NHHT. The silver was made from bullion dissolved in HNO3. The stuff I use for SADS. That leaves bad NHHT as the only possibility, drying temp was pretty low. Recovered salt is very little, I haven't weighed it but it's too little to do repeat tests. Will have to try some other methods and prepare new NHHT. Might as well just try other simple methods to find out if any of them work


Update:
Made a batch of HDN. Plan to test:
1) NQ/HDN/HNO3
2) NQ/hexamine/HNO3
3) NQ/hexamine/HClO4

There are a lot of compounds in this series. Have to parse logical potentials.
I figure with possible issues of NHHT HCl to NO3, due to possible bad NHHT, eliminate crossover of HCl to NO3 for now, instead focus on unknown products from plausible routes, and since it isn't really known what the products are, just perform the process and fire the resulting products into Al witness blocks and compare effect. RDX and etn as controls for comparison.
After the effects are compared from the various products, simple processes like nitrate displacement from HCl can be attempted and those products fired to compare against the known witness blocks.
I need a break from demoralizing amino acids for a bit anyways...

[Edited on 12-7-2023 by Hey Buddy]

underground - 11-7-2023 at 20:55

I do not this there would be any different using HDN over Hexamine since you are going to reflux it wil 65% NA. You will just end up with the same products. It will be just like using a stronger acid like 67% NA. You just adding more HNO3 moles into the mixture. HDN is good when used for RDX

[Edited on 12-7-2023 by underground]

Hey Buddy - 11-7-2023 at 21:03

Quote: Originally posted by underground  
I do not this there would be any different using HDN over Hexamine since you are going to reflux it wil 65% NA. You will just end up with the same products. It will be just like using a stronger acid like 67% NA. You just adding more HNO3 moles into the mixture. HDN is good when used for RDX

[Edited on 12-7-2023 by underground]


Are you certain there is no possibility of a dinitrimine nitrimino triazine? Via HDN?-- I need to prepare rdx, so I just made a big batch of hdn, so there is plenty of extra for tests. And for Al block controls for anything comparable to rdx. For tests of NQ/hexamine, I would use 99% HNO3 not 65% as in a nitrate. Surely there is a potential of a dinitramine, there is a trinitramine and a mononitramine, the tri is from acetic anhydride in their limited tests, analogous to Bachmans rdx, then they find a mono nitramine from mixed acid, it seems that HDN and high test HNO3 would derive a dinitramine if not a trinitramine analogous to KA process for RDX via HDN. Is that not logical?
It seems worth a look since HDN is so fast to make

[Edited on 12-7-2023 by Hey Buddy]

[Edited on 12-7-2023 by Hey Buddy]

underground - 11-7-2023 at 21:37

If you are going to use 99% NA then yes it is worth it. I was talking about 65% NA. You could even try to Add H2SO4 to the mixture since with NQ you will end up with Z-RDX.
I was just thinking to try the compounts step by step for example NHHT nitrate/perch then NNHT etc compare them, check there properties and performance then decide with worth the most.

Purification/recrystallization of NHHT HCl could end up with better understanding and progress of the derivatives. Most of the contamination comes from the Hex/NQ rnx. The next steps are clear

99% NA needs equipment and it would be hard to make in big quantities. On the other hand NHHT HNO3 / NNHT can be made without special equipment from cheap and available materials at large quantities. If NHHT HNO3 has better performance than TNT then it is worth it. Even if it will end up with poor performance NNHT is one step dehydration from NHHT HNO3 with H2SO4.
The only issue for NNHT production is to find out the best way of NHHT HCL production and purification.

AgCL can be converted back to Ag metal with NaOH and table sugar. Ag powder/ Ag2O could possibly react with AN to make AgHNO3 again

The H2SO4 used for the dehydration of QN to NQ and NHHT HNO3 to NNHT could be reused and reconcentrated by boiling. It is never consumed. So in theory only urea AN and Hexamine are going to be consumed for making NNHT without any special equipment.

Just my opinion

[Edited on 12-7-2023 by underground]

Laboratory of Liptakov - 12-7-2023 at 01:44

Hey Buddy
Usually I am at sun-bathing at a pool while typing on SM......:cool:
For basic measurement I use aluminium block and 1000mg in diameter 8 mm.
At this conditions should by give ETN at least 5 mm of deep of crater.

table deep.jpg - 995kB

[Edited on 12-7-2023 by Laboratory of Liptakov]

Hey Buddy - 12-7-2023 at 03:29

Quote: Originally posted by underground  


99% NA needs equipment and it would be hard to make in big quantities. On the other hand NHHT HNO3 / NNHT can be made without special equipment from cheap and available materials at large quantities. If NHHT HNO3 has better performance than TNT then it is worth it. Even if it will end up with poor performance NNHT is one step dehydration from NHHT HNO3 with H2SO4.
The only issue for NNHT production is to find out the best way of NHHT HCL production and purification.

The H2SO4 used for the dehydration of QN to NQ and NHHT HNO3 to NNHT could be reused and reconcentrated by boiling. It is never consumed. So in theory only urea AN and Hexamine are going to be consumed for making NNHT without any special equipment.

Just my opinion

[Edited on 12-7-2023 by underground]


Good points, in that case the first one to test would indeed be NHHT nitrate. AgNO3 should be avoided because it is not as common of nitrate source. Should rather attempt route from common nitrate source such as Na/K or NH4NO3. HDN can be tested after hexamine is tested, I will just use to prepare RDX for control test on Al block for now.

Hey Buddy - 12-7-2023 at 03:34

Quote: Originally posted by Laboratory of Liptakov  
Hey Buddy
Usually I am at sun-bathing at a pool while typing on SM......:cool:
For basic measurement I use aluminium block and 1000mg in diameter 8 mm.
At this conditions should by give ETN at least 5 mm of deep of crater.



[Edited on 12-7-2023 by Laboratory of Liptakov]


Do you know the type of Al you have used in past, if it is common like 6061 or something else? I have 6061 right now, but if you are using other one I should use that, because 6061 may yield differently than other Al under this pressure/force. I believe 6061 may be a bit softer than some others but is most common.

underground - 12-7-2023 at 04:43

Quote: Originally posted by Hey Buddy  
Quote: Originally posted by underground  


99% NA needs equipment and it would be hard to make in big quantities. On the other hand NHHT HNO3 / NNHT can be made without special equipment from cheap and available materials at large quantities. If NHHT HNO3 has better performance than TNT then it is worth it. Even if it will end up with poor performance NNHT is one step dehydration from NHHT HNO3 with H2SO4.
The only issue for NNHT production is to find out the best way of NHHT HCL production and purification.

The H2SO4 used for the dehydration of QN to NQ and NHHT HNO3 to NNHT could be reused and reconcentrated by boiling. It is never consumed. So in theory only urea AN and Hexamine are going to be consumed for making NNHT without any special equipment.

Just my opinion

[Edited on 12-7-2023 by underground]


Good points, in that case the first one to test would indeed be NHHT nitrate. AgNO3 should be avoided because it is not as common of nitrate source. Should rather attempt route from common nitrate source such as Na/K or NH4NO3. HDN can be tested after hexamine is tested, I will just use to prepare RDX for control test on Al block for now.


For metathesis to work you have to find a soluble nitrate salt and an isoluble HCL salt. If you want to avoid AgHNO3 then freebase the NHHT with NaOH is your best alternative.

How much NHHT HNO3 you got? Did you did a flame test ?

[Edited on 12-7-2023 by underground]

Hey Buddy - 12-7-2023 at 10:25

Quote: Originally posted by underground  

For metathesis to work you have to find a soluble nitrate salt and an isoluble HCL salt. If you want to avoid AgHNO3 then freebase the NHHT with NaOH is your best alternative.

How much NHHT HNO3 you got? Did you did a flame test ?
[Edited on 12-7-2023 by underground]


of nitrate sources, NH4NO3 should be considered firstly because it's most common and has gaseous cation. K/Na are second most common. For those two salts with metal cation, K/NaNO3 metathesis seems best route.
For NH4NO3 however, it seems possible that free based NHHT could be heated with ammonium nitrate, or alternatively, a method from Metelkina:

"...heating the reagents in 18% hydrochloric
acid at 50–55°C for 3 h we isolated a compound which
was assigned the structure of nitrimine (IX)"

they are referring to the free base NHHT via dilute HCl, therefore it may be possible to simply heat NQ/Hexamine/18% HCl to 55 C for 3 hours, and isolate the freebase, followed by boiling with NH4NO3 (NHHT decomp is reported at 200 C). Or perhaps even heating NH4NO3 along with the other reagents initially. Or maybe a combination of the two, heating the reagents to produce NHHT, then without separating NHHT, add the NH4NO3 to the solution.

If any of that were possible, it would be the absolute minimum process to achieve the nitrate salt. And dead easy. It seems too simple to be possible, but it may be possible, with the catalytic action of heat and the fragmenting of the hexamine into a triazine in solution. NH4NO3 may just release NH3 and produce the nitrate on the triazine.

As for AgNO3 attempt, there isnt much. Most decomposed. What's there has Ag contamination not worth separating. I can try a burn test, to see if it is different than the NHHT... over all, need to simply use fresh materals to eliminate variables. NHHT sample is a year old...


Burned the attempted NHHT*NO3 it had no notable energetic reaction. Assumption is a bad sample...

[Edited on 13-7-2023 by Hey Buddy]

MineMan - 12-7-2023 at 19:28

Updates please!

And this out performs HMX? 9000m/s @ 1.8 when crystal density is 1.95?

underground - 12-7-2023 at 19:32

Guanidine and urea with Hexamine most likely will yield the corresponding triazine. The dinitrate salt of the triazine into H2SO4 will yield 3 freebase ( NNHT ) and 10 freebase skipping the QN to NQ step. 10 freebase has the same OB as RDX

The most important part obviously is to cyclise urea/guanidine with hexamine to form the corresponding triazine. From that point on you can choose how much you want to nitrate it.

[Edited on 13-7-2023 by underground]

Hey Buddy - 12-7-2023 at 20:27

Quote: Originally posted by MineMan  
Updates please!

And this out performs HMX? 9000m/s @ 1.8 when crystal density is 1.95?


We don't know. There is also a dinitrimino dinitramine reported at 9250m/s @1.88 out of possible 1.96.
I botched a metathesis of Silver nitrate with an old NHHT sample back from beginning of this thread. Now back to square one.
Discussing strategy to test the family tree of possible molecules from this NQ/hexamine root. There are lots of things to test. The literature isn't accurate, metalkina is probably the most accurate. He doesn't give characteristics of the compounds. the pyro, prop. & explosives article appears to be inaccurate on reported performance, however, there appear to be several possible 9km+ compounds from NQ/hexamine. Triazines and broken triazines, and an oxadiazine.

I think Underground and I agree it best to begin simple and try least effort/complexity to most. In search of easy quick high velocity explosive. I'm going even further trying to get a nitrate from NH4NO3 boiling.

Made a big batch of HDN for a control comparison with rdx, but
I thought HDN decomposed at 170 C. Apparently it exhumes nitric acid at lower temp because I tried drying over elevated temperature and this morning the hexamine was in a puddle of nitric acid in the drying dish. I should have just let the acetone dry out on vacuum.

It seems the order of testing is nhht salts like nitrate and perchlorate, then attempt higher nitrated variants all the way up to the z-rdx with a nitrimino in the triazine #6 position, low temp 50c decomp, but high performance. Then comes fractured NNHT via base, then (bis)NQ, after that (bis)NQ heterocycles.
At least, it seems like thats the plan. I'm wiring a residential house, so I'm preoccupied at the moment, but thinking about this at night. I think thats about everything for update up to speed.

[Edited on 13-7-2023 by Hey Buddy]

Hey Buddy - 12-7-2023 at 20:43

Quote: Originally posted by underground  
Guanidine and urea with Hexamine most likely will yield the corresponding triazine. The dinitrate salt of the triazine into H2SO4 will yield 3 freebase ( NNHT ) and 10 freebase skipping the QN to NQ step. 10 freebase has the same OB as RDX

The most important part obviously is to cyclise urea/guanidine with hexamine to form the corresponding triazine. From that point on you can choose how much you want to nitrate it.

[Edited on 13-7-2023 by underground]


Will simply have to attempt each compound and fire it into Al to compare effect. Theory is good for planning but in practice, it will have little bearing on effect. Must fire them all and compare.:cool:

Now I understand cool face emoji. Feels gud man.

underground - 12-7-2023 at 21:12

Quote: Originally posted by Hey Buddy  

Now I understand cool face emoji. Feels gud man.


LoL

Laboratory of Liptakov - 12-7-2023 at 22:09

Hey Buddy........Most likely it is 6061. But you still need a reference crater from ETN. At least one, preferably two. Whatever the aluminum, soft or hard, it is always essential to have a reference sample of known EM. And perform all other tests under the same conditions with the same aluminum. Same pad, same blast pit, same sawdust cover, same amount of primary and so on.

I'm explaining it here for at least the tenth time. And then someone comes with a picture of an old rotten wooden board with a gaping hole and a pile of chips around it.

Hey Buddy - 13-7-2023 at 14:56

Quote: Originally posted by Laboratory of Liptakov  
Hey Buddy........Most likely it is 6061. But you still need a reference crater from ETN. At least one, preferably two. Whatever the aluminum, soft or hard, it is always essential to have a reference sample of known EM. And perform all other tests under the same conditions with the same aluminum. Same pad, same blast pit, same sawdust cover, same amount of primary and so on.

I'm explaining it here for at least the tenth time. And then someone comes with a picture of an old rotten wooden board with a gaping hole and a pile of chips around it.


Patience is the virtue of the master. --I noticed that you are measuring depth of crater, have you attempted measuring water volume by either weighing mass of water from a filled crater on a scale? It may give more resolution in reading for comparisons.

underground - 19-7-2023 at 02:42

I found a Chinese paper for NNHT production. They claim that NNHT det Velocity is 9094m/s. I managed to translate it with an online Chinese to English translator.




Quote:

2-Nitroamino-5-nitro-hexahydro-1,3,5-triazine (NNHT) is a
It is a new type of insensitive explosive, which has attracted people's attention in recent years[1,2].
The molecular structure of NNHT contains both nitro and amino groups, both of which can form
Intermolecular and intramolecular hydrogen bonds have low sensitivity; its density, collision
The impact sensitivity, detonation velocity and specific impulse are respectively 1.88 g·cm-3
, 89 cm, 9094
m•s-1 and 238 s[3~5], it can be seen that it is an insensitive and
Energetic materials with high energy density.
Currently, the United States uses it in gun propellants to make it weapon-resistant
can be improved. The application of NNHT in the M30A1 formulation can make the propellant
The propellant power of propellant is increased by 8%. While NNHT increases the burning rate of propellant, it also
The flame temperature is lowered, and the gunpowder power is increased[6].
In 1990, Huang et al. [3] first designed and synthesized 2-nitroamino-5-
Nitro-hexahydro-1,3,5-triazine (NNHT), its synthesis[7], crystal structure
and molecular geometry[8] have been reported in China. The literature[9, 10] reports are based on
Nitroguanidine, terbutylamine and formaldehyde as raw materials, through Mannich condensation reaction
To obtain 2-nitroamino-5-tert-butyl-hexahydro-1,3,5-triazine (NBHTA),
Then the target compound was obtained through chloride ion catalyzed nitrification reaction (Scheme
1). Wang Bozhou et al. [9] improved the process to increase the Mannich shrinkage
When the combined reaction temperature reaches 82 ℃, the yield can reach up to 89%;
NBHTA was nitrated with industrial nitric acid instead of pure nitric acid, and at 20 °C, the yield
No. 2 Li Yongxiang et al.: A new method for the synthesis of 2-nitroamino-5-nitro-hexahydro-1,3,5-triazine (NNHT) 257
up to 88%; the total yield of the reaction was up to 78%.
Scheme 1
In order to reduce the cost, a new synthetic route (Scheme 2) was adopted in this paper.
NNHT was synthesized from urotropine, nitroguanidine and hydrochloric acid.
In the nitrification reaction, concentrated nitric acid is directly used for nitrification, which is less than the original process.
The raw material ammonium chloride; the raw material terbutylamine in the original process is more expensive, and the market price is
22,000 yuan/ton, while urotropine is much cheaper, and the market price is 99.9%
6800 yuan/ton, the cost of the product is greatly reduced; the revenue of the target product of this route
The yield can reach 64.3%, although the yield is lower than the original process, but the overall average
On balance, the new process is still very economical, saving costs while also
Facilitate the expansion of production scale.
Scheme 2
1 Experimental part
1.1 Instruments and reagents
Beijing Analytical Instrument Factory IR-8400S spectrometer (potassium bromide tablet
method) to test the infrared spectrum of the product; using Element2VARIOEL element
Determination of C, H, N content by element analyzer; Determination by Bruker-AV400
1HNMR and 13CNMR; using Dalian Elite P230 high performance liquid phase
Chromatography to test the purity of intermediates and target products, STA-449C heat fraction
The melting points of intermediates and target products were determined by analyzer.
Hexatropine, methanol, N,N-dimethylformamide, hydrochloric acid (37%)
All were analytically pure; concentrated nitric acid (98.5%) and nitroguanidine were all industrial grade.
1.2 Synthesis of hydrochloride NIHT•HCl (1)
Add 20 mL (0.239 mol) of 37% hydrochloric acid into 100 mL
In the flask, weigh 7 g (0.048 mol) urotropine and add it to hydrochloric acid, stir
Mix; weigh 5 g (0.048 mol) of nitroguanidine, slowly add four-port burner
bottle, stirred at room temperature; after mixing evenly, the temperature was raised to 38 °C, and stirred
Reacted for 3 h; during the reaction, the solution gradually turned milky white;
warmed, filtered, washed with 10 mL of methanol, and dried to obtain an intermediate product
NIHT•HCl is a white powder.
1.3 Purification of intermediate product NIHT•HCl (1)
The intermediate product NIHT•HCl is the hydrochloride, choose concentrated hydrochloric acid for
Purification, using analytically pure concentrated hydrochloric acid to dissolve the water-insoluble intermediate product,
Solubility is small at room temperature, it can be dissolved by heating, and dissolved when the temperature rises
The degree of solubility increased significantly, and then cooled down to room temperature, crystals were precipitated, washed and dried.
Yield 78.3%, purity 98.5%. m.p. 189 ℃.
1.4 Synthesis of NNHT (2)
Add 5 mL (0.118 mmol) of 98.5% concentrated nitric acid into a four-neck flask
medium, ice-salt bath (salt bath formula: 100 g H2O: 20 g NH4Cl: 40 g
NaCl) to -10~-12 ℃; then weigh 1 g (0.01 mmol)
Slowly add NIHT·HCl into concentrated nitric acid, and keep warm for 30 min to increase the reaction
The temperature was 2-3 °C, and the reaction time was 1 h; filtered, washed with water, and vacuum-dried,
The target product was obtained as light yellow powder with a yield of 82.1% and a purity of
98.3%. m.p. 207 ℃ (literature value [10] 207 ℃); 1
H NMR δ: 9.27
(s, 2H, 2×NH), 5.32 (s, 4H, 2×CH2); FT-IR (KBr) ν:
3330, 3216 (N—H), 3123, 3047, 2972 ​​(C—H), 1607 (C—
N), 1572 (NO2) cm-1
. Anal. calcd for C3H6N6O4: C 18.95,
N 44.20, H 3.18; found C 19.58, N 43.91, H 3.21.
2 Results and discussion
2.1 Factors affecting the synthesis of hydrochloride NIHT•HCl (1)
Synthesis of NNHT from Nitroguanidine (NQ) and Hexamethamine (HA)
The first step in the pathway is ring opening by HA, providing nitroguanidine
The CH2NHCH2 group forms a triazine ring, which is then combined with a molecule of HCl to form
Hydrochloride. It is also possible that methenamine reacts with concentrated hydrochloric acid to form formaldehyde and
Ammonium chloride and urotropine have the properties of tertiary amines, thus possessing
Mannich reaction conditions, so the reaction principle is fundamentally the same as Scheme 1
are consistent. The product formed, NIHT·HCl, is para to the N=C double bond
N—H combined with one molecule of hydrochloric acid.
When synthesizing NIHT•HCl, use industrial grade and analytical pure concentrated salt respectively
Acids were used for the synthesis reaction, and the two did not have much influence on the product yield, while
By changing the reaction time to 3, 5, 7, 9, 10 h and the reaction temperature to 30,
38, 50, 55, 70, 80 ℃. The effects of reaction time and temperature on the production
impact on yield.
258 Organic Chemistry Vol. 31, 2011
2.1.1 Effect of reaction time
The order of addition is: concentrated hydrochloric acid → urotropine → nitroguanidine, the reaction temperature
at 38°C

When the temperature is low (<50 °C), with the increase of the reaction temperature, the reaction
The yield rate also increases. This is because the Mannich condensation reaction is a
Endothermic equilibrium reaction, the effect of temperature on the reaction yield depends on the reaction rate
and equilibrium conversion are two factors. When the temperature is lower, the reaction reaches equilibrium
When the conversion rate is low, and it takes a long time. Because the reaction at low temperature
It should be difficult to reach equilibrium, so the conversion rate is low, resulting in low reaction yield.
As the temperature increases, the reaction speed increases and the conversion rate increases accordingly. When
When the temperature rises above 50 °C, with the increase of reaction temperature, the reaction rate
The rate is accelerated, but hydrochloric acid will volatilize to a certain extent with the increase of temperature, resulting in the dissolution
The decrease of the acid concentration in the liquid makes the reverse reaction of the salt formation reaction possible,
On the contrary, it leads to the decrease of the yield of salt. Therefore, the reaction yield increases with the temperature
After the maximum value appears, it gradually decreases. In addition, due to the temperature rise of the reaction system
A certain side reaction occurs after high temperature, which also affects the yield to a certain extent.
Therefore, the yield of the intermediate product reaches the maximum at 50 °C


Attachment: A Novel Synthetic Method of 2-Nitroimino-5-nitro-hexahydro- 1,3,5-triazine NNHT).pdf (268kB)
This file has been downloaded 141 times

[Edited on 19-7-2023 by underground]

underground - 25-7-2023 at 16:03

Considering the easy of making NNHT- NIHT HNO3/HCLO4 and their potential, it really amazes me the fact that still nobody want to explore those energetics

Microtek - 21-1-2024 at 06:44

I gave NIHT a shot recently:

Hexamine (3.5 g, 25 mmol) was added to hydrochloric acid (37%, 10 ml) with stirring. When the hexamine was mostly dissolved, nitroguanidine (2.5 g, 24 mmol) was added in small portions over the course of 10 minutes. No exothermicity was seen.
The temperature was raised to 38 C, and kept at 38.0-38.5 C with stirring for three hours. When the temperature was raised, almost all of the solids were dissolved, but after about 30 minutes, a white powdery precipitate was formed. The reaction was done in a fume hood as it evolves a lot of formaldehyde.

After three hours, the mix was allowed to cool to 5 C, and was filtered, washed with ethanol on the filter, resuspended in ethanol, refiltered and left to dry overnight. The collected product weighed 4.871 g, which is more than the used guanidine can account for. In an effort to purify the product, it was added to 50 ml of distilled water and heated to dissolve it (the Metelkina paper does this). On cooling, small, white crystals precipitated. These were collected by filtration, dried and weighed. Only 0.987 g had precipitated from the recrystallisation. In order to determine the solubility of the isolated compound, an excess of the solid was added to distilled water, stirred for 5 minutes at 21 C and centrifuged. The solution was then decanted into a pre-weighed petri dish, and the water was evaporated at 70 C. Re-weighing the petri dish showed 10 mg of solids had been dissolved in the water, indicating a solubility of 1 g per liter of water at 21 C.
A second saturated solution was prepared and treated with AgNO3 soln, but gave no AgCl precipitate. This indicates that the product recovered from the recrystallisation is not NIHT*HCl but probably the free base.

On the assumption that the solid was in fact NIHT free base, 0.15 g was mixed with an equivalent amount of HClO4, 50% and evaporated to dryness at 70 C. This gave a syrupy material that hardened to a candy like substance on cooling. It burns energetically and without smoke or residue, and is quite sensitive to hammer blows. It is also quite hygroscopic, and absorbed enough moisture to turn liquid after 12 hours at 45% relative humidity and 21 C.

Laboratory of Liptakov - 21-1-2024 at 08:47

Incredible exact description. Pity that final material is hygroscopic.....:cool:

underground - 21-1-2024 at 12:09

Quote: Originally posted by Microtek  
I gave NIHT a shot recently:

Hexamine (3.5 g, 25 mmol) was added to hydrochloric acid (37%, 10 ml) with stirring. When the hexamine was mostly dissolved, nitroguanidine (2.5 g, 24 mmol) was added in small portions over the course of 10 minutes. No exothermicity was seen.
The temperature was raised to 38 C, and kept at 38.0-38.5 C with stirring for three hours. When the temperature was raised, almost all of the solids were dissolved, but after about 30 minutes, a white powdery precipitate was formed. The reaction was done in a fume hood as it evolves a lot of formaldehyde.

After three hours, the mix was allowed to cool to 5 C, and was filtered, washed with ethanol on the filter, resuspended in ethanol, refiltered and left to dry overnight. The collected product weighed 4.871 g, which is more than the used guanidine can account for. In an effort to purify the product, it was added to 50 ml of distilled water and heated to dissolve it (the Metelkina paper does this). On cooling, small, white crystals precipitated. These were collected by filtration, dried and weighed. Only 0.987 g had precipitated from the recrystallisation. In order to determine the solubility of the isolated compound, an excess of the solid was added to distilled water, stirred for 5 minutes at 21 C and centrifuged. The solution was then decanted into a pre-weighed petri dish, and the water was evaporated at 70 C. Re-weighing the petri dish showed 10 mg of solids had been dissolved in the water, indicating a solubility of 1 g per liter of water at 21 C.
A second saturated solution was prepared and treated with AgNO3 soln, but gave no AgCl precipitate. This indicates that the product recovered from the recrystallisation is not NIHT*HCl but probably the free base.

On the assumption that the solid was in fact NIHT free base, 0.15 g was mixed with an equivalent amount of HClO4, 50% and evaporated to dryness at 70 C. This gave a syrupy material that hardened to a candy like substance on cooling. It burns energetically and without smoke or residue, and is quite sensitive to hammer blows. It is also quite hygroscopic, and absorbed enough moisture to turn liquid after 12 hours at 45% relative humidity and 21 C.


Could you determine what the remaining 4g into the solution is ? Is there any possibility to be NIHT HCL and the rest 1g to be the NIHT freebase ? Cause 1g of product seems a bit low.

[Edited on 21-1-2024 by underground]

Microtek - 21-1-2024 at 23:21

I'm sure that a lot of the crude material was in fact NIHT*HCl. I would say that NIHT is probably a very weak base, which coupled with the very low solubility of the free base means that recrystallising it from water gives free NIHT. Aminonitroguanidine nitrate shows the same tendency. It migt be better to recrystallise from hydrochloric acid. It's also possible that the crude material could be nitrated without purification but without sophisticated analytical equipment, I think it is usually preferable to eliminate as many unknowns as possible.

underground - 22-1-2024 at 03:06

True. Will you continue more on this subject ? Let us updated pls.

Edit. Due to low solubility of NIHT freebase, adding NaOH to your crude product then recrystalize it out from water would yield NIHT freebase. I wonder if NIHT HNO3 could exist. Dehydration /nitration of NIHT HNO3 with H2SO4 will yield NNHT which has similar or better performance than RDX

Edit2. Keep in mind that oxygen ruin the reaction for NIHT HCL production. It is better to seal the reaction beaker with a membrane or a balloon to keep oxygen out.

[Edited on 22-1-2024 by underground]

Microtek - 22-1-2024 at 03:27

Precipitating the free base with NaOH might be a good idea, I'll try that at some point.

I did cover the beaker with a plastic film, so I don't think too much air would have gotten in (diffusion through tiny gaps is very slow without a pressure differential). For my next run I can use a sealed apparatus to see if it makes a difference.