Pyrotechnical - 2021-06-25
Prep: http://www.sciencemadness.org/talk/viewthread.php?tid=15091 Edit: it’s sodium hypochlorite not sodium hypochlorate
Excellent, beginning to end. Thank you!
I Really appreciate it!!
Agreed!
Nice job my friend, I feel better via sulfate and sodium hydroxide with ethanol: the only flaw and that I don't get a concentrated product like yours
good job
At the 8th minute, we have finished making the hydrazine solution, or should we add hydrochloric acid and take out the sodium carbonate, or should we add hcl acid only when we want to convert the solution to sulfate??
Does hydrazine sulfate have the same properties as hydrazine solution with reduction reactions??
The HCl is used to rid of the sodium carbonate and then the sulfuric acid is used to form the sulphate salt I used HCl because sulfuric acid is more precious to me but you can use sulfuric acid for the whole thing. Hydrazine sulphate is still a good reducing agent but if a reaction calls for freebase hydrazine you most likely gotta use it.
Then calculating the volume in ml and weighing on a precision plate: so do you know the density in g / cm3 and then doing the proportion you know how much hydrazine hydrate keep expressed in %
Amazing, HELLO, isn't there air in the flask? Are you not worried that the hot steam of hydrazine hydrate will explode when it meets the air in the flask? May I ask, at the end, how much water did you add?
the hydrazine has too much water coming over with it to negate really any explosive risk. I didn’t add any water I only added some hydrazine freebase that I had laying around (probably about 20%) but you will need to add water, no specific amount just enough to dissolve it all pretty well, if the hydroxide is too concentrated it will eat your glassware a bit.
Why didn’t you use CaOCl instead of the NaOCl solution as CaOCl can be found in powder commonly and it should work
I mean I don’t see why it wouldn’t work, I ended up finding a synthesis using CaClO and urea, so it’s a feasible thing to try.
great vid! (and channel)
Appreciate it!
@Pyrotechnical Are you going to do a video about tetrazoles? would be cool!
In the future yes, just gotta get enough time to actually do it lol.
@Pyrotechnical Nice! I am looking forward too it
We know that hydrazine is powering the james webb telescope which will be powered for over 10 to 20 years ..my question is will there be a fuel such as hydrazine or something close to it that will be used to power our automobiles and home utilities ?
everything will probably be electric by the looks of it.
I love watching people way smarter than me
Is there a sinificant problem eg. Contamination from distilling the azeotrope from the bleach urea solution directly?
it’s 2-1 molar ratio so 100/130 = .76 mols of hydrazine sulphate so 40 x .76 = 30.4 x 2 = 60.8 grams of NaOH needed.
@Timothy Egoroff
Since it is always better with chemical equations..
Here is the developped answer from Pyrotechnical Science reply:
N2H4.H2SO4 + 2 NaOH --> Na2SO4.2H2O + N2H4
MM N2HSO4 = 130g/mol
MM NaOH = 40g/mol
MM N2H4 = 32g/mol
So for 1 mole of HS or 130g, you need 2 mole of NaOH or 80g.
This means that for each gram (130/130 = 1) of HS, you use 80/130 grams of NaOH (= 0.615g) and you potentially get 32/130 grams of N2H4 (= 0.246g)
Then 100g HS would require 61,5g NaOH (*) and deliver theorically 24,6g of N2H4.
(*) but a slight exces will not harm since most NaOH prills are an hydrate form and some NaOH has already reacted with atmospheric volatile acids or acidic generating non metal oxides (like CO2 anhydrous carbonic acid).
PHZ (PHILOU Zrealone from Science Madness forum)
Probably you may get some hydrazine from direct distillation of the basic mother liquor (usually bleach is stabilised with a few percents of NaOH already)...
But the yield might be lower (catalytic decomposition of hydrazine is faster at higher temperature by traces of metals (Cu or Fe for example) and it will be more dilluted since you have initially a more dilluted solution as starting material.
The precipitation and crystallization of hydrazine sulfate ensures a good level of purification and concentration in a single step.
If you decide to go for direct distillation... maybe opt for a colder distillation under vaccuum (reduced pressure) and maybe add a little heavy metal scavenger like ethylene diamine tetraacetic acid or salt (EDTA) or a little more gelatin... (they will complexate the multivalent metallic cations and reduce their detrimental effect onto hydrazine stability).
Avoid doing the warm distillation from HS and dry NaOH to get a more concentrated N2H4... it is corrosive to glass just like NaOH, flamable, toxic and quite volatile... better be on the safe side and keep some water.
I had 80% hydrazine (hydrazine monohydrate N2H5OH = N2H4.H2O) it is usually too concentrated for most reactions like hydrazine nitrate, hydrazine perchlorate, Ni(N2H4)3(NO3)2 (lilac NiHN), Co(N2H4)3(NO3)2 (orange brown CoHN) or reaction with AgNO2 (attempt to make AgN3 but got a silver mirror), Cu(NO3)2 (attempt to make CuHN)... the later two are unstable against hydrazine... I got partial pale turquoise blue CuHN success but most of the solution was a dark brown bubbling goo and most of the turquoise precipitate self ingnited on cold drying...it burns with a nice bright blue flame.
I have the chance to get 20% 5L hydrazine hydrate before its regulation in Europe.
Hopefully I have under hand about 500g HS... and bleach and urea are not yet regulated.
Urea can be got quite pure from Ad-blue additive for Diesel engine (8€ for 5 liters saturated urea solution (about 350g/L)... and bleach can be bought for 1€ to 8€ for 5L depending on the concentration of active chlorine 5° to 50° (about 110 g NaOCl per liter).
This makes hydrazine super OTC and cheap.
Bleach can be done from simple electrolysis in a single cell or from bubling and absorption of a known weight/volume of Cl2 (easily made from HCl and MnO2 or KMnO4 or trichloroisocyanuric ring) into cold saturated NaOH solution without much problem.
Urea from ad-blue will probably disappear within the EU due to the restriction of diesel motor engine in 2030 and benzine in 2035... better store some if you can... sothat we can drive with hydrazine motors ;o).
We can also recycle our own urine (manure) (about 30g/L urine) but it is better to take the ammonia or the urea as fast as possible out of the urine by distillation, salification or precipitation to get rid of the smelly fermentiscible impurities.
My researches points towards urea cyanurate, urea nitrate and urea oxalate for precipitation ... for rapid isolation. I need to investigate other salts but informations on solubility or uronium salts are scarce and hard to find...
Nile Red and others have tried but their attempts were quite labour intensive and stinky because of the handling of fermented/oxidised and heated/burnt organic matters.
PHZ (PHILOU Zrealone from Science Madness forum)
@Philouz Louis hi, I drip vaporisation distilled the rough solution of the reacted naoh and hydrazine sulfate h2o, my 2 nech 1l conical flask got chewed up so bad the whole bottom is now GONE -$35, anyway i have been thinking, could this be from the excess of naoh? Would it make a diference to add under molar quantity of naoh next time to drip vaporisation distill the solution, last night i had to visit the energency room for possible inhalation of hydrazine hydrate when the bottom released solution onto the hot plate slowly.
@O K A Y
Solid (or concentrated solution of) NaOH and concentrated hydrazine are corrosive to glass ... NaOH dissolve it as sodium silicate... I imagine hydrazine makes also a kind of hydrazinium silicate.
Very strange you got such a fast corrosion... it may happen but after several runs.
Your 1L two neck conical flask must:
-be already in service for a long time... used and abused... with micro-cracks.
-be of low quality glass (chinese one?)
-non heat resistant glass (no pyrex)
-pyrex but the heat difference between heating source and glass/HS-NaOH-Na2SO4-H2O-N2H4 was too high and stressfull for the heat resistant glass(*).
Or cooled too fast from hot to ice...
(*) I twice had the problem with pyrex... from nearly red hot calcination of a salt to under tap water... bottom of test tube broke... and calcinated product down the drain... yes I felt stupid..
Second time was with a big 5L thick distillation flat bottom pyrex balloon (30 cm) with a long neck of 35 cm and 8cm diameter... heated via gas flame on the kitchen stove. The to be distillated liquid was fermented fruit juice but with much pulp despite filtration through a T-shirt thight tissue/fabric. I had done it a few times without troubles...but this time the pulp had sedimented to the bottom and eventually burnt above one of the metallic branch of the burner that was dark red and holding the glass balloon..then calcinated the pulp against the glass... bubbles did form there and insulated the burning pulp further... with no refluxing liquid able to flow back due to the dense pulp above it and almost no agitation... the glass became a local red hotspot vs the cooler glass arrround... thus a temperature of probably 1000°C difference in a few centimeters... of course... the crack noise was sharp and crack from the hot point upside on 19 cm... I turned fast the heat off and I prayed that the glass balloon will hold enough time for me to siphon the nearly boiling liquid back to my 50L fermented juice drum (lifting it and pouring was not an option). Hopefully the cristal PVC flexible tubing for the siphoning did hold on the all process... it was damn hot and a bit softened;
the crack didn't extend further... (I still have that glass balloon as a reminder how I was stupid)...it is still in one piece with that long crack.
Conclusions:
1) Never distillate a very viscous slurry or sedimenting liquid without agitation, without a flame diffusion /heat homogenizing plate especially if in large quantity... better distillate the supernatant liquid and press filter the pulps (burned pulp gives also a bad taste to your alcohol).
2) Pyrex resist heat if relatively homogeneous... but doesn't stand large temperature differences/shocks... better let it cool down at its own pace.
Wait, does this mean if a gardener accidently dropped urea in bleach they would make hydrazine. Lol.
Kinda but not really
Chemistry of Questionable Quality - 2021-07-29
Awesome video! I'm planning a hydrazine sulphate synthesis this month and anything related is helpful. I'm not sure I have the balls to store hydrazine in liquid form though.