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Author: Subject: Hydrazine
Sir_Gawain
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[*] posted on 7-4-2024 at 17:49


The temperature is less important than the presence of enough water to start the reaction. There should be a visible reaction and temperature spike. I’m not the best at the freebasing myself, and I blame my low sodium azide yields on that.



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[*] posted on 7-4-2024 at 18:15


Quote: Originally posted by Sir_Gawain  
The temperature is less important than the presence of enough water to start the reaction. There should be a visible reaction and temperature spike. I’m not the best at the freebasing myself, and I blame my low sodium azide yields on that.


Hmm, that could also be a major problem, since the ingredients were dry and the alcohol was also dry.

So what do you recommend? I will give my previous successful synthesis from 2022:

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)

I took the above from my old notes.

So please tell me what you did to get a good freebase? I have never added water to my freebasing before. All videos I see on the matter all use alcohol, sodium hydroxide, and hydrazine sulfate and nothing more. Should I add like 15ml of water or something?

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[*] posted on 7-4-2024 at 18:25


IIRC, alchemystery uses some water in his potassium azide video. You just add the hydrazine sulfate to the ethanol and slowly add sodium hydroxide while stirring. If the reaction doesn’t start, you add water a few drops at a time until it does. If you add all the sodium hydroxide at once, then initiate the reaction with water, it heats up so much it boils. I’ve had this happen once, and it was terrifying.



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[*] posted on 7-4-2024 at 18:34


I will look up that video if I don't already have it (I download any chemistry video I find interesting).

I think this was my mistake in the previous two synthesis. added everything all at once, which was wrong, and then made everything too cold. I will stand that the coldness is a factor, too.

In all honesty I am not sure how the reaction would look like, or I have seen it but I forgot. I made some hydrazine sulfate that I am still precipitating out. I moved my setup indoors as it is mostly hydrazine sulfate, but I have my apartment well ventillated (and the beaker is well covered) in order to allow all the stuff to precipitate at 15C and not allow it to go under 10C. By next weekend I should have everything fully ready to try again.
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[*] posted on 7-4-2024 at 19:14


Quote: Originally posted by ManyInterests  
I will look up that video if I don't already have it (I download any chemistry video I find interesting).

I think this was my mistake in the previous two synthesis. added everything all at once, which was wrong, and then made everything too cold. I will stand that the coldness is a factor, too.

In all honesty I am not sure how the reaction would look like, or I have seen it but I forgot. I made some hydrazine sulfate that I am still precipitating out. I moved my setup indoors as it is mostly hydrazine sulfate, but I have my apartment well ventillated (and the beaker is well covered) in order to allow all the stuff to precipitate at 15C and not allow it to go under 10C. By next weekend I should have everything fully ready to try again.


Once you have added the first portion of hydroxide you need to stir until you see the reaction start (some white vapour will be visible and the vessel will warm), note that it takes a long time to get going. If you have been stirring for 15 minutes with no evidence of a reaction starting, try a little water (maybe 5% of your ethanol volume), keep stirring until you see the reaction commence. The formation of the sodium sulfate hydrate with later additions of sodium hydroxide will remove the water.
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[*] posted on 8-4-2024 at 05:06


Thank you for that information. So adding all the ethanol and mixing the hydrazine sulfate first. Then the hydroxide piecemeal. If I don't see what you are describing, add water dropwise until something reacts.

Yesterday I did the longest hydrazine sulfate synthesis I ever did. Most of the time it was waiting for things to cool down. My.mantle overshot the temperature again (it peaked at 91C) but I saw plenty of sulfate formation. I let it cool until it was at 23C before it got too late. I brought the setup inside (with lots of plastic wrap to prevent any gas escape. Overnight it cooled down to 14C and currently I still have it unfiltered at 16C since I had to go to work. Once I return to it I will put it in a ice bath and cool to just barely over 10C before filtering to prevent much sodium sulfate formation.

I was extremely patient with this one and I hope for a high yield.
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[*] posted on 12-4-2024 at 08:50


I'm going to get ready for an NHN synthesis and I will do follow your instructions and do everything slowly and steadily. If water is needed I will do slightly less than 5% of the ethanol. I really want this to succeed. I want to make one final NHN synthesis and get it all done. I want to make more hydrazine sulfate as it will be useful in the future, but for now I just want to make one final bit of high quality NHN and call it a day for NHN synthesis.
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[*] posted on 12-4-2024 at 10:35


What was your hydrazine sulfate yield?



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[*] posted on 12-4-2024 at 13:03


Quote: Originally posted by Sir_Gawain  
What was your hydrazine sulfate yield?


69.65g. My best yet. Doing it slowly and patiently paid off.

but what didn't pay off was using to make nickel hydrazine nitrate. I really don't understand it, but this time I am confident it is not a failure of freebasing, I am certain it did freebase. What I did see happening as I was heating the ethanolized hydrazine was that when my mantle switched off heating at 58C. It went completely nuts and shot up to 75C (AGAIN! Third time!) and I saw some kind of steam coming out of my flask which I thought I covered up and a lot of bubbling in the flask.

This has to be the reason: My hydrazine got fucked from the heat and simply escaped. When I added some nickel nitrate solution it went straight to green again and with none of the purple goodness. Meaning all the hydrazine was destroyed in the process.

This is entirely the result of my new mantle. I need to find a work around for this. I simply cannot afford to keep having these failures.

For my hydrazine sulfate synth, I followed the instructions in a video that is no longer on youtube. But here are the reagents:

Quote:
355 ml pool bleach (or 500 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


I did 3 times that amount to great success. It worked quite well the last time as well. I filtered after I cooled everything down to 10C and no more, so the amount of sodium sulfate left is minimal.

I'm sorry, but I am very upset right now, and I must apologize for the foul language but I am VERY unhappy at this I made NHN successfully many times and these failures are costing me and frustrating me. I did everything right, but the heating did it in and destroyed my hydrazine. Please tell me I am correct...

[Edited on 12-4-2024 by ManyInterests]
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[*] posted on 12-4-2024 at 14:21


What’s the purity of your nickel nitrate? That’s about the only major variable I can think of.



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[*] posted on 12-4-2024 at 14:40


I bought it from a chemical supplier. It is very pure. I dissolved it in distilled water with 0.04% the weight of the nitrate with dextrin.

It is not the nickel nitrate, I am very confident that it isn't. So far I've done this three times. The first time I did it it worked... but I got a very poor yield. Only 4g when I was expecting around 15g or so. The second time there was also a big nothing. Then there was this time, and this time I am very confident that the problem is the heating now, since I am certain that the hydrazine freebased well. There was heat coming out and I saw a clear change in the hydrazine sulfate to look like the sticky thing I'd expect out of sodium sulfate in that situation.

It is the heating. The first time I tried to heat them I used a cheap hotplate stirrier, but it never went beyond 40C. Probably due to it being very cold outside. So I transferred it to my mantle to get it to heat to the necessary temperature but I also had a similar runaway. I've had those runaways in all instant.

I am prepping for another hydrazine sulfate synthesis, the next time I do this, I will use my cheap hot plate stirrer again since the weather is MUCH warmer than the last time. If I need to heat it up. I will only use my mantle until it reaches 45 or 50C (I set my mantle temp to 51C, but it did not stop until 58C, then the runaway happened at 60C. This means my thermometer is probably not accurate. I will use a hot water bath to get it to the appropriate temperature.

It was probably the heat and the destruction of the hydrazine that was the culprit in all cases. NHN can be made at room temperature, but the results will be chunky and will need additional crushing. When done at a higher temperature it will have the consistency of talcum powder and will need very little grinding.

At this point I am willing to compromise, I'm sick and tired of all these failures, especially for something that I thought I had accomplished years ago.
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