| Pages:
1
..
4
5
6 |
B(a)P
International Hazard
Posts: 1139
Registered: 29-9-2019
Member Is Offline
Mood: Festive
|
|
Quote: Originally posted by ManyInterests  |
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).
|
Where did they say they used isopropyl alcohol to liberate hydrazine? My understanding was they dissolved hydrazine sulfate in water then added sodium
hydroxide to pH 8, heated the solution, then added the nickel nitrate solution. The isopropyl alcohol was used to wash the product.
|
|
|
Cubane538
Harmless
Posts: 18
Registered: 30-7-2023
Member Is Offline
|
|
| Quote: Originally posted by ManyInterests | 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. |
Here you can see the video..
Attachment: 20230801_073927~2.mp4 (4.7MB)
This file has been downloaded 292 times
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
| Quote: | | Where did they say they used isopropyl alcohol to liberate hydrazine? My understanding was they dissolved hydrazine sulfate in water then added
sodium hydroxide to pH 8, heated the solution, then added the nickel nitrate solution. The isopropyl alcohol was used to wash the product.
|
I stand corrected. I was confusing videos in my mind with one where Chemplayer freebases hydrazine with IPA and Ethanol in two separate attempts.
I did remember that Raid said he did liberate it with just water. I might do that next time if it is easier. Just keeping in mind that the pH needs to
be 8 or thereabouts. I'm probably going to continue to use the old ethanol method since it worked for me quite a few times.
| Quote: | Here you can see the video..
Attachment: 20230801_073927~2.mp4 (4.7MB)
This file has been downloaded 3 times
|
I always lit my NHN from the top and not the bottom, but that is some slow burning stuff. I think there is something wrong with it, but sadly I cannot
tell what... :\
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
I need to bump this thread back up due to a series of rather... irritating events. I wanted to make more NHN and since I had been quite experienced in
making it and seen numerous setbacks and know how to deal with them, but my last two synthesis, especially my latest, has been a failure and I really
don't understand why.
So here are the number of reagents used:
Hydrazine sulfate: 43.25g
95% ethanol: 150ml
sodium hydroxide: 26.4g
I had freebased my hydrazine the same way as I done before. Added the ethanol to the sulfate, mixed it thoroughly, then added the sodium hydroxide (I
did it in one fell swoop). Everything was put in the fridge for days so it was ice cold to begin with, and I did it while everything was in an ice
bath to keep things cool. The temperature never rose above 9C the whole time.
I mixed in a covered beaker and allowed it to settle, then mixed and such for 35 minutes to allow all the hydrazine to freebase. Then I filtered off
the sulfate into a flask and heated it up (also covered) with strong stirring. I need to mention that the heating on my mantle is a bit unpredictable.
When it was reaching the 60C the temperature then almost immediately shot up to 75C. Also since I was doing this on a windy day on my balcony, my
flask tipped as well, it loosed up the plastic wrap that I was using to seal it and I saw fumes come out (no inhalation, I am fine). But when I added
the nickel nitrate solution (I added more water to it, but it is still very emerald green, as pictured).
I am really confused as to what is happening here. My last attempt worked, but it yielded barely 4g. The last successful time I made it was in 2022
and I made two attempts that yielded 11.4g (of excellent quality NHN) and of 15.5g (of poor quality NHN that I had to get rid of) respectively. All
other previous successful synthesis of mine also yielded much higher amounts of high quality NHN.
The first times I attempted they failed due to my hydrazine synthesis not working. But when I made the hydrazine sulfate for this they absolutely WERE
hydrazine. I am really baffled.
Any thoughts? Any help?
Edit: Maybe I freebased my hydrazine wrong and it was destroyed by the temperature spike?
Edit2: when I added the nickel nitrate to the hydrazine solution It didn't turn torquoise blue. It remained green. Normally in a successful synthesis
it would be immediately purple.
Edit3: upon further thing, this probably is a hydrazine issue. Either the original synthesis, or I was too cavalier with the freebasing.
[Edited on 7-4-2024 by ManyInterests]
[Edited on 7-4-2024 by ManyInterests]
[Edited on 7-4-2024 by ManyInterests]
|
|
|
Sir_Gawain
Hazard to Others
Posts: 457
Registered: 12-10-2022
Location: [REDACTED]
Member Is Offline
Mood: Stable
|
|
Are you sure the free-basing reaction took place at all? If your reagents are dry and cold enough, the reaction may not start. What’s your source of
hydrazine sulfate and nickel nitrate?
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
| Quote: Originally posted by Sir_Gawain | | Are you sure the free-basing reaction took place at all? If your reagents are dry and cold enough, the reaction may not start. What’s your source of
hydrazine sulfate and nickel nitrate? |
That could be my problem. It could have been too cold. All regents were very cold except for the nickel nitrate solution, it was at room temperature.
The Hydrazine sulfate I made myself with the Hoffman rearrangement of urea. The nickel nitrate was purchased from a chemical supplier online. It was
Nickel(II)nitrate hexahydrate.
I had successfully made hydrazine sulfate many times before and they all made NHN. At this point I will believe that you are right. No freebasing
occurred because everything was too cold.
Edit: This is one aspect that I as unaware would happen. I had no idea that that freebasing needs some decent temperature. I remember being warned
that it can get hot and you can lose your hydrazine, I didn't store ingredients in the fridge previously, I think this was the mistake I made this
time. Not my nickel nitrate solution being too concentrated or maybe even the temperature spike on the mantle.
[Edited on 7-4-2024 by ManyInterests]
|
|
|
Energetics-testin
Hazard to Self
Posts: 53
Registered: 7-6-2022
Location: Canada,Quebec
Member Is Offline
Mood: in love with EM's <3
|
|
Found this video a week ago and finally was able to make NHN pretty easily, the quality of the NHN is alright but not the best.
Apparently using alcohols will always favor the formation of chunky "impure" slightly violet NHN and not the beautiful pink some people get.
Using potent solutions, Good temperature & H2O to freebase the hydrazine sulphate, Will apparently favor the formation of the talcum like
consistency and not a grainy sand-like "powder".
https://youtu.be/1jOWAA67z-I?si=T6mTCvDJQjk0GH3S
"I dont claim this method to be safe or better,its just that its the only one that worked for me, So I wanted to share."
|
|
|
Microtek
National Hazard
Posts: 872
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
@ManyInterests: I encourage you to find a copy of the book "Small scale synthesis of Laboratory Reagents with reaction modeling" by Leonid Lerner.
It has excellent and very thorough guides for preparing hydrazine sulfate (from urea and hypochlorite), freebasing the hydrazine and using it to
prepare sodium and potassium azide, as well as many other useful preparations. You can preview the book here:
https://www.routledge.com/Small-Scale-Synthesis-of-Laborator...
|
|
|
EF2000
Hazard to Others
Posts: 153
Registered: 10-5-2023
Location: The Steppes
Member Is Offline
Mood: Taste testing the Tonka fuel
|
|
| Quote: Originally posted by Microtek | @ManyInterests: I encourage you to find a copy of the book "Small scale synthesis of Laboratory Reagents with reaction modeling" by Leonid Lerner.
|
A bit of Eastern European magic, then a bit of pdf compression, and voila.
Found it on Nexus (bot in Telegram), also available on Anna's Archive: https://annas-archive.org/md5/23e6ee80c42c2419e4b176bbc6d1d3... and library.lol: lol
Attachment: leonid-lerner-small-scale-synthesis-of-laboratory-1.pdf (2.5MB)
This file has been downloaded 249 times
Wroom wroom
"The practice of pouring yourself alcohol from a rocket fuel tank is to be strongly condemned encouraged"
-R-1 User's Guide
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
Thank you guys, Turned out my issue was more due to the awful PID on my mantle that overheated my freebased hydrazine. I managed to resolve the issue,
I freebased a lot better (by adding warmer ingredients and the sodium hydroxide in three parts instead of all at once) and I freebased a lot of
hydrazine, I also used my rather crappy hotplate (it is cheap... you get what you pay for...) in combination with a hot water bath that kept the
temperature from 60 to 69C while I added all the nickel nitrate that I could... and I made a good batch of very pure, very high quality NHN.
And thank you for the book. I always get as many as I can.
|
|
|
| Pages:
1
..
4
5
6 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
