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ManyInterests
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Quote: Originally posted by PINKBOII  | | so i tried making NHN for first time, and when i add the nickel nitrate to the hydrazine freebase a green precipitate forms. i know its supposed to be
a purple color and this is not purple. how do i fix this. BTW i was not using the hexahydrate i was using the raw nickel nitrate from making it, im
guessing this is the problem but im not sure. also the green precipitate does NOT redisolve into solution. it just kinda sits there. one more note is
that i used H2O2 in the nickel nitrate synthesis and maybe converting the "NHN" to some sort of other nickel salt. |
I had that problem when I was first making NHN. The green is most likely nickel (II) oxide. What happened for me at the time is that my hydrazine
sulfate wasn't actually hydrazine sulfate at all, but almost completely sodium sulfate.
What was the process you used to make hydrazine sulfate? Or did you buy it?
I should update my notes and post them here for getting hydrazine sulfate done correctly and my NHN notes.
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Raid
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ok, yeah it was nickel 2 oxide, so i bought some hydrazine sulfate which its kinda expensive (100g for 20$) and i tried to make it and got really bad
yields. how do i fix the bad yield?
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Raid
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Also Manyinterests, do you happen to have a PDF or a method of synthesis that gives good yields?
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ManyInterests
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I tried to find the video that I found most informative, but it seems to be off youtube! Good thing I downloaded it!
I'll have to post my notes here:
| Quote: | 355 ml pool bleach (or 250 ml regular bleach selection)
75 ml 50% H2SO4 (add 37.5ml 98% H2SO4 to 37.5ml super cold water)
47.8 g NAoh
34.1 g urea (30ml or 40ml of distilled water to dissolve. use absolute minimum and make sure water is warm.)
0.75 g gelatine (takes 15 ml of warm water to dissolve this)
122 ml HCI
Dissolve urea and geltin seperately in the minimum water necessary (use distilled) be very careful not to use excess water. Then pour them into the
same container. Keep it cold and handy.
Get the fan started (this is where the deadly gasses start to form). Add the ice-cold bleach to ice bath (keep it super cold) and then add NAoh slowly
to it while stir vigerously (remove from ice bath and put on mantel) Do let let temperature rise above 20C.
Add the urea and gelatine to the container.., this is where the foaming starts. Be SUPER careful. After foam starts to subside cover with foil or
cling wrap to prevent hydrazine gas from escaping. Heat to 85 celsius for 5 minutes
Once solution is clear the hydrazine is ready. Remove from heat and put on another ice bath. It will still be fuming so be ultra careful.
After cooling, keep in ice bath. Add the HCI dropwise (BE VERY CAREFUL HERE! Also optional). Let it cool for a few minutes, then add H2SO4 and stir
for a few minutes. At this point it will cause the hydrazine sulfate to percipitate. Cool down to 15 celsius and you can do the vacuum filteration
after it is nice and cold for a while. (do not cool down to below 10C. We don't want the sodium sulfate that will percipitate at this point).
Put bleach in bottom of flask to neutralize any hydrazine that slips past. Neutralize further with dilute solution of calcium hypochlorite or sodium
hypochlorite (the same bleach you used to make it). Dry for several days before storing in tupperware
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This is for the hydrazine sulfate. Yes they are personal notes with personal reminders.
For my NHN synth here are the notes of my 2 last synths
| Quote: | synthesis on (DATE REDACTED)
30.15 grams of hydrazine sulfate
18.43 grams of sodium hydroxide
105ml of 95% ethanol (put 55ml first, then the 30 ml later and finally 25ml)
and 40ml of nickel nitrate solution that I made (with indeterminate amount of dextrin)
as of writing. Filtered and added around 250ml of ice cold distilled water and 100ml of 95% ethanol. Filtration is taking a while. Hopefully it will
come out dextrinated and require no crushing.
Note: I believe some hydrazine fumes were created. No harm was done. But this is something you need to be extremely aware of. It is possible that
gravity filtration is the superior choice in this case, as vacuum filteration doesn't seem to be doing this fast enough. You employed emergency
protocols of flushing that ethanolized hydrazine down the toliet. No harm happened. You will be A-OK.
Further note: Actually no, it was likely not hydrazine. Hydrazine has an ammonia scent and you know ammonia. It did smell like ethanol, but it might
have contained it. So your reaction was still good as it prevented any possible problem.
result was extremely finely powdered stuff. Just perfect!
Final yield after drying: 11.88 grams
Next synthesis (and hopefully final): (DATE REDACTED)
39 grams of hydrazine sulfate (all my remaining supply).
23.9 grams of sodium hydroxide
150ml of 95% ethanol (with 75ml added first, followed by the rest).
75 to 80ml of nickel nitrate solution.
This time no vacuum filteration (and outside!). Do it purely via gravity. Also in two containers as you will be putting in alot more stuff this time.
Gravity filtration takes hours when washing with the 250ml of water and 110 ml of ethanol.
Final yield after drying: 15.72 grams
Extra note on this one. The burn is not as quick. There might be something off with this batch. Some testing is required when making blasting caps
with it. If the 2nd batch successfully detonates a booster like ETN then it is good enough. Testing is needed to see its power in confinement. If it
goes DDT in a pen body with similar power, then that is all good and well. If it can set off a booster then it won't matter, but until then, the first
batch is vastly superior.
It could have been the choice of filteration.
To do: Do another filteration of the batch (now separated into two bits) via vaccuum filteration. Give it plenty of both water and alcohol.
Further notes after drying from second cleaning. Situation has improved. Perhaps not as much as the first batch, but still significantly better. For
future synthesis. Follow the first method. It is possible that too much ethanol was used, or that too much/too little nickel nitrate.
Final yield after cleaning and tests is 13.25 grams.
NOTEs: Next time DO NOT dextrinate it. It is unnecessary and might actually make it impossible to go full DDT.
FURTHER NOTES FOR SCIENCEMADNESS: Do not use plastic pen bodies as detonator caps. They won't work! |
Yes I know I have some anxiety notes written there. But it was a result of the discussion with Mineman and Laboratory of Liptakov on these forums when
it comes to disposing of the left over liquid.
At any rate, I have a gas mask now, so the issue will not repeat.
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Raid
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thanks!
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Raid
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also i forgot to ask if you think methanol would work for the reaction medium in place of ethanol, i have never seen it done but i think it might
work.
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ManyInterests
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That is a subject of experimentation! I am not sure. I know that Chemplayer tested both 95% ethanol and isopropyl alcohol (I don't know what
percentage, but safe to say it was probably 99% or 91%) and he said that ethanol was best.
I've never seen anyone use methanol for this. If you want to dare giving it a try, please do and report your findings!
Edit: for my hydrazine notes. I forgot to change his. The HCl (hydrochloric acid) is NOT optional. All synths I've done that didn't use it were
failures. use the HCl first to neutralize the solution before cooling and adding the sulfuric acid.
[Edited on 16-1-2023 by ManyInterests]
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Raid
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ok, ill try methanol today! and ill come back here and report my findings 
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Raid
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Ok, I tried methanol and it works. the yield seems is a bit lower but Im guessing that's because of the lower concentration of methanol I'm using. so
I'm going to say that its a safe bet to use methanol in place of ethanol, just use higher concentration for better yields.
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ManyInterests
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Great! Can you list the reagents and the amounts and the steps you took? I know I sound a bit obsessive, but I like using the forums as well as open
lab notes (for both myself and for future chemists).
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Raid
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I used your procedure but divided everything by 10 as to not waste reagents if this did not work. And instead of ethanol, I used methanol. the yield
was a bit lower then it should have been but I will still say that methanol is a viable replacement for ethanol if your don't care about a gram or
two.
but since you asked for the steps here they are.
3.9 grams of Hydrazine Sulfate was added to a 100ml beaker along with 2.39 grams of sodium hydroxide.
After that, i added 15ml of Methanol in the first addition. the solution heated up to the point the Methanol was evaporating so make sure to cover the
reaction mixture well. i allowed that to stir on the hot plate for around 30 min until somewhat cool. then i added an extra 10ml of Methanol to make
sure i freebased all the Hydrazine. and stirred for an hour. I left it on the hot plate for about a day to make sure all the sulfate salts crashed
out. then i pipetted off the supernate and put it in a test tube and heated it up to 65c when i added as little Methanol to the Nickel Nitrate as
possible. after the Hydrazine solution heated up to 65c,I slowly added the nickel nitrate solution aver the next 2-3 min. Then i gravity filtered the
solution and dried on a hot water bath.
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ManyInterests
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| Quote: Originally posted by PINKBOII | I used your procedure but divided everything by 10 as to not waste reagents if this did not work. And instead of ethanol, I used methanol. the yield
was a bit lower then it should have been but I will still say that methanol is a viable replacement for ethanol if your don't care about a gram or
two.
but since you asked for the steps here they are.
3.9 grams of Hydrazine Sulfate was added to a 100ml beaker along with 2.39 grams of sodium hydroxide.
After that, i added 15ml of Methanol in the first addition. the solution heated up to the point the Methanol was evaporating so make sure to cover the
reaction mixture well. i allowed that to stir on the hot plate for around 30 min until somewhat cool. then i added an extra 10ml of Methanol to make
sure i freebased all the Hydrazine. and stirred for an hour. I left it on the hot plate for about a day to make sure all the sulfate salts crashed
out. then i pipetted off the supernate and put it in a test tube and heated it up to 65c when i added as little Methanol to the Nickel Nitrate as
possible. after the Hydrazine solution heated up to 65c,I slowly added the nickel nitrate solution aver the next 2-3 min. Then i gravity filtered the
solution and dried on a hot water bath. |
Did you cool down all the reagents before mixing? I always cooled everything down and kept it in an ice bath when mixing with also keeping most of the
beaker covered with cling film while mixing it. ( I keep only as little as needed uncovered to stir properly while covering everything in order to
stop the hydrazine from escaping).
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Raid
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the only thing that i left cool was the freebase hydrazine. after stirring for like an hour I left if to sit for a day to cool to room-temp but I
guess you could cool in the freezer for faster synthesis. it also should help the Sulfate contamination.
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Raid
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Does anyone think you could use water for the reaction medium in place of the ethanol?
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Hey Buddy
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Accidental Hydrazine Nitrate
I got really lazy and attempted to make some NHN with nickel nitrate solution still acidified and hydrazine in alcohol. It precipitated white
Hydrazine Nitrate in EtOH solution and rejected the nickel which stayed in solution. I thought it was obvious but none the less interesting as there
is no hypergolic reaction in the alcohol medium.
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ManyInterests
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| Quote: |
Does anyone think you could use water for the reaction medium in place of the ethanol? |
I really don't see how that would work. Water and ethanol are fairly different solvents and I am not sure if it'll work to freebase hydrazine.
| Quote: | | I got really lazy and attempted to make some NHN with nickel nitrate solution still acidified and hydrazine in alcohol. It precipitated white
Hydrazine Nitrate in EtOH solution and rejected the nickel which stayed in solution. I thought it was obvious but none the less interesting as there
is no hypergolic reaction in the alcohol medium. |
Yeah, this is why I was advised to use an excess of nickel metal to use up all the nitric acid. At first I was thinking of find the 'right' balance
until I realized it is smarter to just salvage the left over nickel metal for later use.
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Raid
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I have seen a procedure on freebasing hydrazine to hydrazine hydrate with water and I think i'll try it out. It is said to work well as long is a PH
is adjusted accordingly.
It is said that hydrazine sulfate in water is acidic with a PH of 3 and you need to all a hydroxyl group to increase its PH to 11. Then it said to
filter to get rid of sulfate contamination.
I will probably chill it to 0-5c to make sure sulfate contamination is at a minimum.
Ill report back the results.
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Raid
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ok, i just tried the process i talked about above and it works very well, Its much faster and better then using an alcohol.
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ManyInterests
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Nice!
So let me see if I can possible recreate what you are saying.
Say I would get water (distilled of course) and add some HCl to get the pH to 3, then add some sodium bicarbonate (or sodium hydroxide) to get it to
11, then chill it and then filter it out any solids, then add that water to the hydrazine sulfate and mix to freebase?
After that, of course, it is warming to 40C and adding the room temp nickel nitrate I assume. I was told not to use dextrin anymore and not to heat to
65C.
Am I on the right track?
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Raid
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you don't need to add HCL, the hydrazine sulfate is acidic in water. I used NaOH to get the ph to
Note: I have tested it with heating to 65c but it does not seem to do anything different if you were just to use no heating.
all the patents i have seen say the same thing.
I would also recommend chilling the solution if the freezer for around 5-7 hours (longer if you want) that should precipitate out the sulfate salts
and you should get a better and more pure yield.
[Edited on 3-4-2023 by Raid]
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Raid
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After longer and more testing with freebasing using distilled water, I have noticed that when adding the Ni(NO3)2 to the N2H4 it will sometimes
produce a non-energetic salt that has all of the same qualities as regular NHN. One of the main differences it that it does not deflagrate like
regular NHN, instead it will just burn and some of it will fly away. It will deflagrate with heating under it. I have not tried to detonate it.
I have a few reasons why this would happen most of which could be traced back to my own fault.
The first thing that I have done is add an alcoholic solution of Ni(NO3)2 to the N2H4 in H20, this could have caused the less energetic salt. I will
be fixing this mistake later today and reporting on what I find.
Also, when adding the alcoholic solution to the N2H4 it forms a bit of a supernatant that can be easily broken upon mixing the solution. This does not
happen when using all EtOH for the reaction medium. I'm guessing that this is caused by the difference in density or water content (most likely
density).
If you're wondering if this freebasing technique works well I can say that it does, if your not sure what I'm talking about scroll up and look for
where I talk about it. The only downside is that your getting more sulfate contamination with the hydrazine, this can be fixed by chilling it until
the sulfates crash out. This has its own problem because the water will freeze if your using a freezer.
The best method I have used is distilling it. This will take out most of the impurities. If you don't want to do any of these then I would recommend
buying hydrazine sulfate from Amazon or HiMedia, The prices are cheap for hydrazine sulfate. I got 100g for $16 which I thought was a reasonable
price. Store-bought Hydrazine Sulfate is much purer compared to synthesizing it yourself and will reduce the chance of metal contamination by lots. If
you don't want to buy it, I would reccomend freebasing the N2H4 and then distilling it untill you get your desired consentration then you can get the
sulfate or chloride if desired. This is one of the easiest ways to reduce the contamination of DIY hydrazine sulfate.
Moving on to the theoredical synthesis.
One thing I would like to point out to people is that using the Cl salt of hydrazine (Hydrazine Dihydrochloride or Monohydrochloride) is MUCH better
than the sulfate. It will make your end product much better and reduced the chance of getting your Ni(NO3)2 turned in to NiSO4. You may be wondering
if this same thing could happen with with the Chloride instead of the Sulfate, In all of my testing with this it takes considerably more Cl ions in
solution to convert the Ni(NO3)2 to NiCl2. If your using the Hydrazine Dihydrochloride for the NHN synthesis then having the nitrate converted should
not be much of a problem.
I have seen many people on youtube using a synthesis where the N2H4 is added to the Ni(NO3)2, I'm not sure if this is just used to make large batches
of NHN or what. If someone could find where they got this synthesis it would be very helpful.
Thanks for reading
[Edited on 14-4-2023 by Raid]
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Cubane538
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Few days back I made some NHN by adding hydrazine (extracted from hydrazine sulphate and dissolved in ethanol) in Nickel nitrate solution.
When I filtered and dried the product I observed that the colour is violet - blue instead of Liac!!
I also did flame test and it was burning well.
But I'm in confusion wheather it is NHN or something else!!
[Edited on 31-7-2023 by Cubane538]
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ManyInterests
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How fast does it burn? Does it instaneously vanish with a bright flash? Then that is probably good enough.
I need to make more NHN soon, since I am running out. The last time I made it, one of the batches I made seemed sub par. I wonder how well it would
work as a cap on its own. I need to test them.
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B(a)P
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I recently saw this on youtube.
https://www.youtube.com/watch?v=enJAVGGTPQ4
Interestingly they use hydrazine sulfate directly (using sodium hydroxide to generate the hydrazine in the solution) with nickel nitrate. I have not
tested this approach myself, curious if anyone else has though?
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ManyInterests
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That's how I've been doing it all the time. He used Isopropyl alcohol while I used ethanol. It is possible to use methanol as well, but ethanol has
the best yields.
When I freebase my hydrazine sulfate with sodium hydroxide and ethanol, I also need to filter out whatever solids that are left behind (my process for
hydrazsulfate always has a little sodium sulfate in it). One thing that he is doing that I must do next is add nickel nitrate until I get that excess
added and used up all my hydrazine freebase. since I didn't know you could do that (and easily get rid of the surplus, since NHN is water insoluble).
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