Synthesis of Hydrazine Sulfate: Part 1

[98JMA]

Can I use bleach instead of the hypochlorite solution?

[lexichronicle2]

Emulsions sometimes split if given a ride through the freezer :P

Domestic freezer will reach a solid -30C if left on super freeze for a good while. It may take a day or two to cool all the contents from -18 down to the limit, as the pump has zero heat moving capacity at -30C

[ChemCrazy81]

Can you mix the MEK directly with the urea and then add the hypochlorite like in the ketazine process?

[98JMA]

@ChemCrazy81

Try it and tell us!

[g3ov4n12]

I dont got it, why you heated when you were pouring the hypochlorite/hydroxide?

[UC235]

@g3ov4n12 I only heated after mixing the two solutions and the foam subsided. The color change indicates the reaction progress and it will not go colorless without heating nearly to boiling.

[NADHHH]

3) Is heating essential when you add urea to bleach solution? I am planning to do this step outside (and thus have very limited heating options) because I do not have sophisticated equipment as you have and I really do not want to breath those hydrazine fumes.

[NADHHH]

2) Can I use oxalic acid / oxalate in addition to gelatin for more efficient chelating of transition metal ions? I think they may be pain in the ass because I use cheap household / technical chemicals (from chemical store I can get ~10 times more expensive).

[NADHHH]

1) I have a lot of cheap (2 USD/kg) fertilizer grade urea and it contains ~2% biuret impurities. I already recrystallized it. Heating in water bath to ~100C made solution strongly alkaline and some ammonia gas was also generated. So more of urea got polimerized to biuret. Can it bet efficiently seperated from urea by recrystallization? Can biuret inerfere with this reaction?

[NADHHH]

Hello UC235!

Great video (as all your videos)! I will repeat this with some modifications (acetone instead of butanone followed by acetone azine extraction with toluene). I have some questiens:

[UC235]

@NADHHH 1) Biuret may lower yield; I don't know. Biuret has much lower water solubility than urea, though they may act differently when mixed. Prepare the solution with excess urea and more water and filter any solid.

2) Don't use oxalate. Sodium oxalate is poorly soluble and may precipitate causing problems. If you have EDTA or a salt of it, use that. If not, stick to gelatin.

3)Stirring when mixing the solutions is critical. After, heating almost to boiling to finish the reaction is necessary.

[ConorC96]

Also, how do you get the ethyl methyl ketone?

[UC235]

@ConorC96 MEK is easy to find in the hardware stores where I live. I'd go with dye additive urea for the most pure material, though it certainly isn't reagent grade.

[ConorC96]

Where can you come by the urea

[UC235]

@ConorC96 Fertilizer, certain instant cold packs (others are ammonium nitrate), and it is sold as an additive for applying certain types of dyes to fabrics. The latter two sources will likely give you a more pure starting material. I use urea sold as a dye additive. When melted, it became somewhat brown indicating that it wasn't totally pure. I recrystallized it from mixed denatured alcohol and water (with significant loss, but it is cheap) and it no longer discolors when melted.

[ConorC96]

@UC235 Which gives you the most pure urea?

[kuro96inlaila]

Great videos!

[TakronRust]

Your glassware looks immaculate. It doesn't look like it's ever been used. lol

[UC235]

@TakronRust I take good care of my equipment. It wasn't free. Also, especially with organic chem, sometimes small traces of contaminants can mess up a reaction so you get used to cleaning everything very thoroughly.

[Aranwu]

@UC235

Any useful tips on how to clean the glassware thoroughly? :D



[lexichronicle2]

@Aranwu There are absolutely tons of methods, ranging from biological washing powder (which works extremely well on tars) to things that are carcinogenic and explosion hazards. The method of cleaning it depends on what's in it to begin with. The more extreme methods aren't always the best.

Common options are, biological, KOH / NaOH (in water or alcohol), sulphuric, hydrochloric, nitric, nitric and ethanol, chromic acid, persulphate and sulphuric, piranha and heat, oh... & a brush on a stick

[RatkoUSA]

@UC235 Do you cook your glassware in the oven after cleaning? I've found that doing so for approximately 30 minutes at 450-475 degrees removes most traces of contaminants and water left behind from the washing process.

[UC235]

@RatkoUSA I usually use the convect setting at ~130C to dry the glass in a short amount of time.

[TheMaDMAli]

hahaha you reffed, sciencemadness, biggup

[hkparker]

Great job!

[NurdRage]

Nicely done!

[acidum984]

Eagerly waiting for part 2 and aftermath of entire process!

So far nice work. (as usually)