Make Hydrazine Sulfate by the Hypochlorite-Ketazine Process - The Complete Guide

Ғылым және технология

In this video we make hydrazine sulfate by the hypochlorite ketazine process.
Warning: The reaction produces toxic gases and products. It also uses corrosive chemicals, gloves must be worn.
Hydrazine sulfate is a useful substitute for the more dangerous pure liquid hydrazine in chemical reactions. Simply adding in a stoichiometric amount of base will release the hydrazine in-site and allow for it to be use in for such purposes as reductions, azotizations and various other synthetic uses.
The process to make hydrazine sulfate is extremely simple: Start with 250mL of ammonia and add to it 100mL of methyl ethyl ketone. Stir and then slowly add 1/4 mole equivalent of sodium hypochlorite based bleach. if using 10% bleach then about 186g is needed. If using 6% household bleach about 310g is needed.
As the bleach is added the reaction will heat up and bubble vigorously, slow down the addition if it's bubbling too much. After all the bleach is added, keep stirring until the mixture stops bubbling. Then stop stirring and allow it to stand for a few hours or so until it separates into two clear layers. The top layer is methyl ethyl ketazine.
If after a few hours the solution is clear but there is no seperation, you may to perform an extraction with 100mL of toluene.
Separate it using a seperatory funnel or by careful decantation.
In a separate container, add 20mL of concentrated sulfuric acid to 100mL of water and stir. Then add the hot solution directly to the ketazine and keep stirring. The hydrolysis will generate crystals of hydrazine sulfate. Let solution cool to room temperature on its own and then filter off the crystals of hydrazine sulfate.
Acetone can be used in place of MEK, but you'll need to distill it off (use 50mL acetone in the reaction and distill 150mL of liquid) or extract it out with toluene into the acid solution.
Another process to make hydrazine sulfate is the hoffman rearrangement, a good procedure can be found in this thread: www.sciencemadness.org/talk/vi...
The complete discussion on hydrazine and how to make it can be found here: www.sciencemadness.org/talk/vi...
The message board itself, Science madness: www.sciencemadness.org
They are by far the best chemistry message board i have ever seen.

Пікірлер: 448

  • @NurdRage
    @NurdRage10 жыл бұрын

    Bleach has always had sodium hydroxide, it's a side effect of the manufacturing process (membrane electrolysis). But sodium hydroxide actually helps this process of making hydrazine. There is no wider conspiracy to alter clorox to "keep people like (me) from making hydrazine", this process still works and will work for the foreseeable future. But go ahead and keep calling me a dumb ass/asshole or whatever. I'll keep doing and teaching actual chemistry.

  • @alllove1754

    @alllove1754

    5 жыл бұрын

    Please do a Wolff-kishner!

  • @MrWoodwhitler
    @MrWoodwhitler11 жыл бұрын

    I have to thank you. I have impressed my chemistry teacher multiple times because of watching your videos.

  • @FourthRoot
    @FourthRoot13 жыл бұрын

    Although there have been many other influences, your channel is has played its part in rekindling my interest in becoming a chemist. Videos like these helped me learn enough chemistry on my own to pass my CLEP test with a high score and receive college credit necessary for my associates degree. I believe that that test was very influential in helping me land a job as a laboratory technician a month ago. Sadly I was just laid off, but I walked away with $2K, some experience, and a good reference.

  • @pavaluca
    @pavaluca13 жыл бұрын

    we appreciate all the hardwork you put into your videos nurd

  • @NurdRage
    @NurdRage12 жыл бұрын

    the consensus is that my bleach had an unusualy high salt content and salted out more of the ketazine. Yields can be improved if an extraction with toluene is performed.

  • @NurdRage
    @NurdRage13 жыл бұрын

    This has got be my most expensive video ever. Not because it's expensive to do, but because i failed SO MANY times and used up so much money in chemicals until i finally found the good cheap method in the video. At least all of you can benefit from my research :)

  • @TALOS7887
    @TALOS788713 жыл бұрын

    I don't understand almost 95.99% of what you're talking about but I like watching your videos.

  • @dr4cula
    @dr4cula13 жыл бұрын

    Even though I'm much more interested in physics and feel myself a lot better around stuff involving physics, I find your videos interesting enough to keep watching them ... And damn, even though I don't understand everything, it's still awesome to see how stuff can be made with fairly accessible stuff. Thanks for that and keep it up :)

  • @pixartist8190
    @pixartist819013 жыл бұрын

    Hey, I'm pretty clueless about chemics and I can't repeat any of your experiments, but I still enjoy watching them! Thanks for educating people :D

  • @cvasold
    @cvasold10 жыл бұрын

    Outstanding video! Thanks for taking the time to make it.

  • @Danol12345
    @Danol1234513 жыл бұрын

    keep making vids!! youre really good chemist and love watching your vids!

  • @yuzukirules
    @yuzukirules13 жыл бұрын

    yay finaly another video ...Damn boy it was about time, agonizing wait, STOP making me wait...... YAYAYAYAYAYYAYAYAYAY

  • @NurdRage
    @NurdRage13 жыл бұрын

    @Libertarianist awesome to hear that my videos did some good. Good luck in your future endeavors and employment.

  • @tuxxedomask
    @tuxxedomask13 жыл бұрын

    I really enjoy this channel. The practical stuff about chemistry I love, i just absolutely suck at theoretical stuff.

  • @osintmachado
    @osintmachado13 жыл бұрын

    I know that took a lot of work, thank you. And keep doing great videos.

  • @HazMatLabz
    @HazMatLabz13 жыл бұрын

    Great video! And that's a very good thing to note about the excess of ammonia since it greatly reduces the chances of nitrogen trichloride/chloramines. Also just to note on that fact, is direct reaction with hypochlorites and urea almost directly forms NCl3.

  • @NurdRage
    @NurdRage12 жыл бұрын

    interesting, i'll be sure to keep an eye out for it in the smaller shops :)

  • @PattyMMelt
    @PattyMMelt13 жыл бұрын

    Freshman chemistry major here. I can't wait for the day when I totally know what you're talking about!

  • @MrBradshawbenjamin
    @MrBradshawbenjamin3 жыл бұрын

    I like the white with your outline as black effect, that was cool.

  • @ArtistBlade1972
    @ArtistBlade197213 жыл бұрын

    Excellent video!

  • @shodanxx
    @shodanxx13 жыл бұрын

    the dedication you put in documenting your efforts are commendable, I do not believe the good folks @sciencemadness are "looking down on you" just the fact that you explained this complex process in a way that a layman like me "got it" is impressive, you should seriously consider teaching professionally ! also thanks for revealing the secret ingredient of name brand epoxy thinner, that probably saved me hours of research, and that's another shop cleaning product to add to my list

  • @samkear
    @samkear13 жыл бұрын

    Another excellent video, thanks for posting!

  • @jeebersjumpincryst
    @jeebersjumpincryst13 жыл бұрын

    30 hours of video on the old one.... WOW! But good final job, and thanks so so much for posting - I LOVE yr vids! :)

  • @CHESEPOWER
    @CHESEPOWER13 жыл бұрын

    Nice video! Thank you for the information.

  • @silverblotter
    @silverblotter13 жыл бұрын

    very well explained

  • @guitarttimman
    @guitarttimman9 жыл бұрын

    why would someone look down on you? you obviously have a very good grasp on the subject.

  • @Nikolaii2571
    @Nikolaii257111 жыл бұрын

    I used to make mixtures of Calcium hypochlorite powder and Sulfur and watch the spontaneous combustion occur when I didn't know any better. When I was 15 years old, I attempted to produce a cherry bomb using the above mixture. The next thing I saw were both of my hands inside an orange ball of flame. Next, I ran around the table in a state of panic and shock. My hands looked like fried chicken with fingernails rolled up like scrolls. This experience taught me a healthy respect for fireworks.

  • @zignitz
    @zignitz13 жыл бұрын

    Hey congrats on getting to the ads level! I hope you get some decent revenue from this channel to fund future experiments!

  • @NurdRage
    @NurdRage13 жыл бұрын

    @xchainlinkx the better question is what is hydrazine itself used for, Hydrazine sulfate has very few specific uses, but it releases hydrazine when mixed with a base. So the hydrazine sulfate is used as a convenient "solid form" of hydrazine. kinda like instant cake mix. Hydrazine is used as a reducing agent in many chemical reactions, it can also make azines and pure anhydrous hydrazine can be used as rocket fuel.

  • @NurdRage
    @NurdRage13 жыл бұрын

    @xPyrotechx ah crud, you're right. i'll pull the video and fix the mistake when i have the time, probably next week. thanks for pointing it out.

  • @Pap9
    @Pap913 жыл бұрын

    dude you are like.. the smartest persone i know:P do u memorize all "educational" stuff u say durring video or do u prepare for each vid?

  • @UristMcTubedwarf
    @UristMcTubedwarf13 жыл бұрын

    i have no idea what i would use that chemical for but i just like watching :)

  • @NurdRage
    @NurdRage13 жыл бұрын

    @Kendrana do a test for azides at various points in the reaction if you're unsure.

  • @acronus
    @acronus13 жыл бұрын

    @NurdRage Thank you very much for the effort and resources put into it, and all your video's in general.

  • @nattsurfaren
    @nattsurfaren13 жыл бұрын

    Thanks for a really good video NurdRage.

  • @MrSuednym
    @MrSuednym11 жыл бұрын

    When he pulled out a sep funnel, I immediately thought, well there's $123. My roommate broke one the other day, that's why I know the cost.

  • @abdelhakouinharoune7504

    @abdelhakouinharoune7504

    5 жыл бұрын

    It's been 6 years, anyone gave a shit yet ?

  • @NurdRage
    @NurdRage13 жыл бұрын

    @masterfish1234 The shape of the container just changes the rate of evaporation. i think the effect is negligible but if you should observe a significant difference let me know. :)

  • @AndreaEatsRainbows
    @AndreaEatsRainbows13 жыл бұрын

    The most things I've ever mixed are tea and sugar... But I love watching these videos:)

  • @anhero23
    @anhero2313 жыл бұрын

    @dr4cula physics major here. I agree, this guy definitely makes me look at chemistry in a new light.

  • @NurdRage
    @NurdRage13 жыл бұрын

    @Ibogaine306 it is, my actual addition funnel was in use somewhere else. But often the use of a piece of equipment defines its title :)

  • @NurdRage
    @NurdRage13 жыл бұрын

    @heydeech i don't recommend using a stir rod because then your hand will be over the mixture with the toxic and carcinogenic gases. You can use just a straight stirrer since heating isn't required.

  • @fredooor
    @fredooor13 жыл бұрын

    very interresting!

  • @NurdRage
    @NurdRage13 жыл бұрын

    @TakronRust nope, did you use diluted or concentrated sulfuric acid?

  • @NurdRage
    @NurdRage12 жыл бұрын

    yep, the stir bar is made of teflon, which is highly resistant to most solvents and chemicals

  • @klj2503
    @klj250313 жыл бұрын

    Excellent videos you make, thanks ! One question though: is this just proof of consept or what would you use Hydrazine Sulfate for in real life ?

  • @NurdRage
    @NurdRage12 жыл бұрын

    Go for it :)

  • @DarkBioCloud
    @DarkBioCloud13 жыл бұрын

    nice vid. It would be nice to see future videos based on creation of hard to find chemicals or producing common chemicals for less than the store prices. That would give people another route so if a chemical is hard to find or very expensive they can create it themselves from the raw materials(if they have access to them). Chemistry is all around us you don't always have to buy every chemical used if you create it yourself.

  • @SithMami
    @SithMami9 жыл бұрын

    This is amazing; thanks =]

  • @punckhole
    @punckhole13 жыл бұрын

    Chemistry is awesome!

  • @UC235
    @UC23513 жыл бұрын

    I have a video (actually 2 parts) up of a working Hofmann rearrangement for hydrazine sulfate. I borrowed a handy concept from this video which I would not have thought of without it. Thanks!

  • @NurdRage
    @NurdRage13 жыл бұрын

    @Kendrana There is, but since sodium azide is incredibly toxic, i don't think i'll be making a video on it.

  • @NurdRage
    @NurdRage13 жыл бұрын

    @JaiNobesIsARat it does have a methyl and ethyl group on either side of the ketone. Thus "methyl Ethyl ketone"

  • @Chlorate299
    @Chlorate29913 жыл бұрын

    These videos are incredibly fascinating, I just think it's funny that some of the chemicals used are almost impossible to obtain in a lot of places. For good reason :)

  • @typical_arthur
    @typical_arthur12 жыл бұрын

    I have no head for chemistry but this is really cool so i watch it anyway.

  • @NurdRage
    @NurdRage13 жыл бұрын

    @NADHHH Absolutely no idea at all, did you use diluted or concentrated sulfuric acid?

  • @phsycoklownkiller5
    @phsycoklownkiller512 жыл бұрын

    lol thks for telling us about the missing 2 you took all the fun of checking if your equations were balanced.

  • @htirah100
    @htirah10013 жыл бұрын

    my head blows up when reading the title

  • @cobrasniper555
    @cobrasniper55513 жыл бұрын

    THANK YOU!

  • @Zackbcom
    @Zackbcom13 жыл бұрын

    NICE!

  • @NurdRage
    @NurdRage13 жыл бұрын

    @remotecontrolaholic I have several hotplate/stirplates. That particular one is a few years old and yeah, the knob broke off.

  • @NurdRage
    @NurdRage13 жыл бұрын

    @insanic1 its called separatory, look it up in any major glassware supplier like chemglass

  • @NurdRage
    @NurdRage13 жыл бұрын

    @Palizasadomicilio I tried salting but it didn't work. Its a good idea though, but you should still go with either distillation if using acetone, or just go with MEK for phase separation.

  • @cooliscool2
    @cooliscool212 жыл бұрын

    Exactly. Hydrochloric acid is added dropwise to the isocyanic acid to produce chlorine gas. According to some instruction I found on the web the yield shoud be about 50%. I think I'm definitely going to give it a try.

  • @NurdRage
    @NurdRage13 жыл бұрын

    @61slugbug what concentration was the ammonia? greater than 20%?

  • @NurdRage
    @NurdRage13 жыл бұрын

    @1RadicalOne Go for it..... But since to make ~20g requires ~500mL of fluid, i don't think its economical to have a GIANT centrifuge for such small quantities. If you had that kind of money you could buy hydrazine directly. Its far cheaper just to let it sit.... Gravity is free :)

  • @Solingen1000
    @Solingen100013 жыл бұрын

    Thanks for all the great vids. I was wondering if there are any books you could recomend for an novice interested in chemistry? Once again...thanks.

  • @bj8161994
    @bj816199413 жыл бұрын

    Hey Nurdrage!! Love your videos, but when are you going to do the potassium chlorate via electrolysis video?

  • @jusTlikehmf2
    @jusTlikehmf213 жыл бұрын

    Nice, you have ads now. That's kinda awesome.

  • @KrazeyKraka
    @KrazeyKraka10 жыл бұрын

    This seems like it would be much better performed within a rig, rather than a beaker with a crystallization plate over the top.

  • @Andrew-my1cp

    @Andrew-my1cp

    4 жыл бұрын

    That's what I was thinking as well. I ordered a 3 neck RBF and was just thinking how easy it'd be to just set up a pressure equalizing addition funnel to one neck, a gas outlet that directs the produced gases through a scrubber solution to remove traces of highly toxic chemicals, and then the third neck could be used for a second pressure equalizing addition funnel. I see a lot of people making hydrazine inside of beakers and such and it's something I'd never try. I wouldn't want to trust cling wrap with my health haha.

  • @heydeech
    @heydeech13 жыл бұрын

    Great video! I was wondering, could a glass stir rod be used instead of a magnetic stirrer? my hotplate does not have a magnetic stirrer on it, I could always buy a stirrer alone since they aren't as expensive as the hotplate combo but would glass rod hand stirring work or does it need to remain covered?

  • @zenosxr
    @zenosxr12 жыл бұрын

    I'm a member at SM and I still love your video's, and have performed tons of syntheses of yours. BTW like the new videos with balanced equations and for SURE the ingredient annotations as I don't have to rewind and pause 50,0000 times. And the wife wants to know,, do you use a voice synthesizer to hide identity?

  • @NurdRage
    @NurdRage12 жыл бұрын

    That method produces highly contaminated hydrazine, almost inseperable from the isocyanuric acid.

  • @verzinsung
    @verzinsung11 жыл бұрын

    Useful video - thanks I suggest same (*2) molar quantity (50g) of NaHSo4 as acid rather than conc. sulfuric, being much safer to store and use.

  • @007rapz
    @007rapz13 жыл бұрын

    This must have taken a lot of work and research to make this video so i hope people appreciate that.

  • @NurdRage
    @NurdRage13 жыл бұрын

    @g3ov4n12 i suppose, any particular dye you'd like to see?

  • @NurdRage
    @NurdRage13 жыл бұрын

    @gabdcceddlappy its used for reductions and azotizations in organic chemistry. I will try to make luminol with it.

  • @bemanos12345
    @bemanos1234513 жыл бұрын

    nice video

  • @NurdRage
    @NurdRage13 жыл бұрын

    @yellowmetalcyborg vacuum distillation with rigorously cleaned all-glass apparatus.

  • @DragonisRed1
    @DragonisRed18 жыл бұрын

    Hi. You mentioned at the end of video that there's Peroxide process. Is process the same with hydrogen peroxide? Or there must be some additional catalyst? Thx

  • @NurdRage
    @NurdRage13 жыл бұрын

    @JaiNobesIsARat you can use sodium bisulfate pool acidifier instead, though you're product will be contaminated with sodium sulfate if you don't use enough water. But if you use too much water it'll give a poor yield. MEK is also known as 2-butanone.

  • @NurdRage
    @NurdRage13 жыл бұрын

    @UC235 did you give credit where its due? :)

  • @JavDSilva
    @JavDSilva13 жыл бұрын

    @NurdRage sorry i got exited and forgot to say great research and thank you very much

  • @toxicore1190
    @toxicore11909 жыл бұрын

    does this work with acetone as well? never mind didnt watch the video until the end sorry :D

  • @jazerazo
    @jazerazo13 жыл бұрын

    Thanks.

  • @Sheynan55
    @Sheynan5513 жыл бұрын

    wow! thx!! i love ur vidoes.. but i dont think i will try this video this time just cuz is a very high level of chemistry.

  • @NurdRage
    @NurdRage13 жыл бұрын

    @inurfac Have you seen many research labs and meth labs in your time to know the difference?

  • @NurdRage
    @NurdRage13 жыл бұрын

    @Kendrana From what i know of azides, they aren't formed under these conditions, but i could be wrong.

  • @lucasmaugeri5372
    @lucasmaugeri53728 жыл бұрын

    If two layers were not formed many hours after the addition of hypochlorite to ammonia / MEK (I did it dissolving flavourless gelatin, on an ice bath and dropwise), so I extract with toluene... should I get rid of the toluene before performing the hydrolysis with diluted H2SO4? If so, could this be performed by simply boiling it away (or distilling)? How stable is the methyl ethyl ketazine to heat?

  • @drakenbakken
    @drakenbakken13 жыл бұрын

    "they probably look down on me, ah well" rofl can't wait to see some of the stuff your going to do with this now

  • @hkparker
    @hkparker13 жыл бұрын

    I will be trying this and the luminol synth in the next coming weeks. Probably wont film it as there is no need for a worse shot version of the same reaction but I will let you know how it goes.

  • @98JMA
    @98JMA12 жыл бұрын

    It is necessary to form the methyl ethyl ketazine (butanone azine), yes. As he mentions, acetone can be used instead but fractional distillation must be used as opposed to simple phase separation.

  • @JackSinger
    @JackSinger11 жыл бұрын

    Can you give us a tour of your lab?

  • @mamooshaa
    @mamooshaa13 жыл бұрын

    Could you please make a video in which you take the hydrazine sulfate and incorporate it into a simple fuel cell? that would be so cool!!! Thanks.

  • @ReapingMiner
    @ReapingMiner12 жыл бұрын

    I used your method of making hydrazine with 2 small alterations. I used

  • @JavDSilva
    @JavDSilva13 жыл бұрын

    wait nurd what? too esay already, and i jus fount where to buy it all for less than $15 great video keep it up

  • @putinslittlehacker4793
    @putinslittlehacker47933 жыл бұрын

    I know this video is 9 years old but I'm praying you still respond to your comments, I have been able to purify 30% peroxide from that oxaxlean percarbonate powered bleaching agent, what catalsits would work for the peroxide proses?

  • @NurdRage
    @NurdRage13 жыл бұрын

    @ignilc they've referred to my videos as "pure crap and confusion spreading" and they've called me a mediocre chemist and a clown. So it's doubtful they would read anything i post, let alone use it.

  • @norscience
    @norscience13 жыл бұрын

    @Nurdrage: What catalysts are needed for the process using H2O2 instead of bleach? I don't see why this reaction won't proceed without any catalysts? I prefer using 35% peroxide (of which I have a lot) to using 6% bleach. PS: Great video. I absolutely love these more advanced videos dealing with organic chemistry. Keep it up! PPS: Nice to see you on the Sciencemadness board. :)

  • @skyebuddha
    @skyebuddha13 жыл бұрын

    Thanks

  • @NurdRage
    @NurdRage12 жыл бұрын

    you mean using chlorine gas? i tried to do that but the yield was incredibly low. But if you can get it to work then go for it :)

Келесі