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

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: http://www.sciencemadness.org/talk/viewthread.php?tid=757&*

The complete discussion on hydrazine and how to make it can be found here: http://www.sciencemadness.org/talk/viewthread.php?tid=1128

The message board itself, Science madness: http://www.sciencemadness.org

They are by far the best chemistry message board i have ever seen.

Category:

Science & Technology

Tags:

• YouTube editor
• Synthetic
• organic chemistry

[TheQgvFactor]

Well, I know Bleach + Ammonia creates Musterd Gas, so how safe is this to do, if it were done inside of a fume hood with a Chemistry teacher (all safety precautions taken, gloves worn)?

[NurdRage]

@TheQgvFactor which moron told you the blatant lie that bleach and ammonia make mustard gas? It makes toxic chloramine, but certainly not mustard gas.

[98JMA]

@ConorC96

He's a research chemist.

[Raddan2010]

I hope to be an accomplished chemist someday. NurdRage, you're my inspiration.

[98JMA]

@Si3z3 Did you bother to even watch the video?

[Si3z3]

@NurdRage ive heard that bleach and amonnia make mustard gas but i always thought it made chlorine gas

[Chirimorin1]

@TheQgvFactor In general, when done in a fumehood with proper safety precautions, none of the gas will escape into the room. Your chemistry teacher should know how to do this stuff safely.

[98JMA]

@dariumzleso

Possibly, although you will need to make sure that whatever acid you use can protonate one of the amines on the hydrazine. Also, you would have a significant loss in yield with the monohydrochloride salt, as it is much more soluble than the sulfate.

The best way to find out things like this is just to experiment on a small scale until you find a procedure that you like.

[dariumzleso]

@98JMA

Ok, thanks.

I suppose this basing procedure is also suitable for other compounds, right?

an HCl salt instead of a sulfate for example

[98JMA]

@98JMA

neoprene gloves and have a lot of experience handling these materials. The distillation must also be carried out under argon or nitrogen, as pure liquid hydrazine reacts violently with air and sometimes moisture.

[98JMA]

@98JMA

If you attempt this yourself, though, be extremely cautious - pure hydrazine attacks glass at elevated temperatures, so a metal still must be used, it is incredibly toxic, highly corrosive, a skin sensitiser, a known carcinogen and has dozens of other highly adverse health effects. DO NOT attempt unless you have access to a very powerful fumehood or glovebox, are wearing full PPE, including a face shield, full PVC suit and respirator, chemical splash goggles and heavy

[98JMA]

@dariumzleso

Not exactly. Look at this balanced equation;

N2H4(H2SO4) + 2 NaOH = Na2SO4 + 2 H2O + N2H4

As you can see, one mole equiv. of hydrazine sulfate reacts with two mole equiv. of base, so, you need to use twice the molar amount of NaOH as you do the Hydrazine Sulfate. For example, if you used, say, 30g of hydrazine sulfate, then you will need to use 18.44g of NaOH.

[dariumzleso]

@98JMA

I'm studying chemistry but i'm italian so there might be some misunderstandings.

however, like you say, i have to calculate the number of moles of base that stoichiometrically fits the moles of the sulfate ion (SO4), right? not the interely hydrazine sulfate.

for example, x grams of hydr. sulfate ---> moles of sulfate ions in it = moles of base to be used. Correct?