inspector5
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Iron oxide by electrolysis
Hello everyone. I have been lurking for a while but this is my first post.
I'm attempting to produce Iron(III) oxide for use as a catalyst in KNO3/Sugar propellant. I'm using info off of Wikipedia that says this:
Iron (III) oxide is a product of the oxidation of iron. It can be prepared in the laboratory by electrolyzing a solution of sodium bicarbonate, an
inert electrolyte, with an iron anode:
2 Fe + 3/2 O2 + H2O → 2 FeO(OH)
2 FeO(OH) → Fe2O3 + H2O
At about 200 °C, the iron(III) hydroxide converts into Fe2O3.
Not very detailed but I figured it was workable so I mixed up a roughly .6M solution of Arm & Hammer with RO water and hooked up the PC power
supply with the +5 going into a piece of steel wool and the ground going to a piece of CP titanium wire I had coiled up for another experiment. I was
getting good gas generation at the cathode and I believe the anode as well (it's kind of hard to tell with steel wool containing and obscuring most of
the O2). I let it run like that roughly 16 hours. I did not check the current at any point as the speed of reaction was not really a concern.
Now, I recall from Science Fair projects as a youngster that you can perform simple electrolysis of water with steel electrodes and fairly quickly
your cathode will begin oxidizing but my cell showed no signs change after those 16 hours so I switched over to a +12v leg and it is running at that
right now.
I was just wondering if anyone here could explain the lack of reaction at 5v for that period of time. I imagine I may be missing something basic in my
knowledge of what should be occurring.
Any advice, comments or criticisms are appreciated.
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starch
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How bouts burning some steel wool  j/k, well half
this looks so cool
http://www.youtube.com/user/NurdRage#p/u/0/5MDH92VxPEQ
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inspector5
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I have seen that video and actually I did burn a piece with what appeared to be similar in appearance to NurdRage's video. But what it resulted in was
not a homogeneous product. There appeared to be small spheres of un-oxidized steel along with very small pieces of the steel wool that would not be
easily separated with what I have for equipment. Also, I believe that method produces Iron(II,III) oxide (which would still work, though not quite as
well) or at best a mixture of the two and was hoping the electrolytic method would be a simpler way to achieve better purity.
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xxx
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Use solution NaCl and iron electrodes and your PC power supply
Black oxide at the anode and H2 at the cathode
Heat black oxide to get red oxide
Bicarbonate do not work even if you used strong power supply
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ScienceSquirrel
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Your best method is to start from iron II sulphate, readily available from eBay or garden centres as it is used for colouring concrete and correcting
iron deficency in soils, and sodium hydroxide.
Mix strong solutions of the reagents, then vacuum filter, wash and dry.
But iron oxides have lots of uses in pigments and glazes so why not just buy it?
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Arthur Dent
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And yet another technique to easily produce nice iron oxide for your rocket propellant experiment is also a question that I asked as one of my first
posts on this forum:
http://www.sciencemadness.org/talk/viewthread.php?tid=14731
...where I used some fine steel wool (previously washed a bit with acetone and dried) and poured some plain old bleach on it. After a few days, the
steel wool had just but disappeared and I was left with very fine Fe2O3 at the bottom of the vessel.
After filtering, washing and drying, you will be left with very fine brown iron oxide. The advantage of this technique is that you can make large
quantities of the oxide and it doesn't use electricity nor strong, dangerous chemicals. You can wave a magnet inside the suspended solution of water
and Fe2O3 particles to pick-up stray iron dust that hasn't reacted with the hypochlorite.
Robert
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Saerynide
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I once made ~100 g of very fine and very pure Fe2O3 (pure enough to run a beautiful thermite reaction that produced a bright shiny steel ingot ) very quickly using steel wool, bleach, and vinegar. The acid really kick starts
the reaction.
After, just decant, filter/wash, bake dry.
"Microsoft reserves the right at all times to monitor communications on the Service and disclose any information Microsoft deems necessary to...
satisfy any applicable law, regulation or legal process"
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inspector5
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xxx: I actually did try that and it worked. At first I was skeptical since the first references I found to that method were on youtube and I usually
take everything on there with a grain of salt but then I found some patents that described the same method so I gave it a try.
Science Squirrel: It is cheap but so am I and that combined with the fact that I live in BFE and don't want to pay shipping have set me on the idea of
making from things I already have but thanks for giving me an alternative prep.
Arthur Dent: I swear I really did UTFSE but somehow I missed that. But thanks, that sounds like the simplest method to produce a reasonable quantity.
Saerynide: I will try your method on a very small scale as I am somewhat apprehensive of mixing bleach with anything that accelerates the release of
chlorine gas.
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Saerynide
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Oh right, do it outside  Just leave it in a jar and let sit on the porch or
something. Give it a shake whenever you pass by to go out and it'll be done in no time. And of course, don't bake in the house. It smells VERY bad
when it dries (like rust and burnt vinegar lol), even when you wash it many times with clean water, the vinegar smell doesnt really come out...
[Edited on 12/22/2010 by Saerynide]
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inspector5
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I always do anything that releases or could release anything I wouldn't want to breathe outside or in my little (well-ventilated) shed depending on
the exact process and the length of time it takes but my main objection is just the indoctrination I've always received about not mixing bleach with
anything, which while cleaning your bathroom is a good rule but doesn't exactly apply the same to this situation. So I will (cautiously) try your
method.
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xxx
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"Bicarbonate do not work even if you used strong power supply ",my foolish wrong
I said that because i traid it with Na2CO3 ,first preceinceple iron oxide then begain O2 because anode will painting with iron oxide,perhaps that
occur only in basic solution
however I often prepare iron oxide from electrolysis (supply power laptop 20 volt and 3.5 amp) or i dissolve iron in HCl or H2SO4+water then add NaOH
Or Na2CO3 to precipitate Fe(OH2) green
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Arthur Dent
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Quote: Originally posted by xxx  | i traid it with Na2CO3 ,first preceinceple iron oxide then begain O2 because anode will painting with iron oxide...
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Sorry, I'm a bit confused... 
Robert
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xxx
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my english is bad so you will confused (traid=tried , my wrong)
i was try to paint anode with fe3o4 for preparation chlorate
i dissolved Na2CO3 in water then i added iron anode and cathode
at cathode H2
at anode iron oxide then painted anode with fe3o4 so stop precipitation iron oxide and began bubbled o2 i mean it stopped for oxidition iron
i tried too with naoh
hoever it failure in oxidaition NaCl and peeling off
i tried too to heated it with mixture NaOH+NaNo3 and it failure
i heated iron and when it become red i placed it in water several times . that little success
I thought you will confused again
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knowledgevschaos
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Probably a bit late but here goes:
Using carbonate or bicarbonate as an electrolyte has never worked for me, it seems to form a passivization layer that prevents the flow of current.
The only electrolyte that works without fail for me is potassium sulfate. Sodium chloride also works.
In one of NurdRange's videos he says something similar.
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