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Rust synthesis.


Von Klemmung
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For a while, I've been looking for ways to create fe2o3/red iron oxide/ferric oxide, other than scraping it off the bottom of my car. :P

 

Then I chanced upon a page (which I, of course, can't find again) that suggested the following procedure.

 

First, make a solution of an iron salt in water. Then, add a hydroxide to the solution.

 

The solution should change its colour as a precipitate forms.

 

Upon drying, the precipitate should change its colour to that of rust.

 

So I decided to try some chemicals I have already, namely iron vitriol (sulfate AFAIK) and household ammonia/ammonium hydroxide.

 

The solution was a greenish/milky colour, just as the powder.

 

Upon adding the hydroxide, it turned greenish black immediately.

 

I filtered the solution, noticing a rust coloration on the edges of the filter.

 

The black precipitate was a bugger to dry out, but eventually turned out reddish-brown.

 

Now, I'm not really schooled in chemistry, but this is what I suspect was happening.

 

The addition of ammonium hydroxide caused an exchange of ions, leaving a precipitate of iron hydroxide (of a sort or two) and a solution of ammonium sulfate.

 

Drying out the (supposedly unstable) iron hydroxide, it decomposed into iron (ferric) oxide.

 

Can anyone verify the reaction, and/or explain the unwillingness of the hydroxide to dry out?

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u probably made mixture of things and some iron complexes. the best way is too take somethign iron, salt water, and dip the iron electrode and graphite one into salt watert then pass dc current through. red crap will accumulate in the water, which u can the dry out leaving you with very nice iron oxide. Put the iron on the anode.

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u probably made mixture of things and some iron complexes. the best way is too take somethign iron, salt water, and dip the iron electrode and graphite one into salt watert then pass dc current through. red crap will accumulate in the water, which u can the dry out leaving you with very nice iron oxide. Put the iron on the anode.

 

Thanks, but I forgot to mention "Cheap, easy and fast".

 

There are TONS of descriptions on the net dealing with electrolysis. And a rather humorous one about cars... Humorous...

 

Now, outdoors, I MIGHT try the vinegar/hypochlorite reaction, but I'm sorta put off by the idea of a chlorine generator.

 

But if this simple substitution method DOES work, I could make a couple of kilos of nice red fe2o3 in a day or so, as long as I dry it out correctly.

 

My initial impression of the reaction goes something like this:

 

xFexSO3x + xNH3xOHx + xH2O --> xFe2O3 + xNH3xSO3x + xH2o

 

Can anyone offer clarification?

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Ok.. Basicly the black green stuff is Fe(OH)2 . After exposer to air, It turns into Fe(OH)3 I believe, Which is reddish. I'm pretty sure you don't have Fe2O3 ... I tried the same thing. :-\ Of course, this is jsut what I was told. I don't understand The chemical pulling out another Hysdroxide form somewhere but I don't see it turning into Fe2O3 either.. so yeah. I could be wrong of course.

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u probably made mixture of things and some iron complexes. the best way is too take somethign iron, salt water, and dip the iron electrode and graphite one into salt watert then pass dc current through. red crap will accumulate in the water, which u can the dry out leaving you with very nice iron oxide. Put the iron on the anode.

 

 

I did this and I didn't get a pure anything. I had a mixture of red and grren blakc precipitate. After addition of NaOH, the red turned into the green black. This coincides with Von Klemming's experiment. I'm fairly certain Iron Oxide wasn't formed... I mean.. The possibilities are endless. Especially with the Chloride ions floating around (not to meantion reduced in favorable conditions)

My point is.. It's not as clean as your putting it.

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If you have the time, and want some iron oxide you can get a little bucket and put water in it and just stuff it with steel wool. Maybe even put a fish tank bubbler in there to get more oxygen in there. Should have a good aount in a few days.

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I don't understand why on earth you want Rust ? What's the use ? (none that I know). It doesn't smell great either !

 

Lots of uses, especially in this mixture called thermite, which is used in underwater welding and such. I can't really discuss all the details here, but you definitely should look into it yourself...

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I currently have 5 pounds of Iron Oxide that I'm willing to part with. I got it on ebay for thermite but I dont have money for aluminum powder. I understand this is extremly risky since you don't know me.. but I would sell it to you.. Your choice of course.. If you don't want to buy some... Like H2SO4 said... Steel wool and water will slowly create your Iron Oxide. I guess PM me if your interested in mine. I don't even know what a fair price is.. I think I payred 20 something.. Oh yeah. I didn't check the rules. If it is illegal to sell anything on here, just say so and Ill edit my post..

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More than one compound can be brown.... Iron hydroxide and Iron Oxide can be brown.. They can both NOT be too. Other than that, I havn't done sufficient testing to disprove your statement totally. I HAVE done electrolysis with both iron electrodes in a solution of NaCl and I got a nasty green precipitate. Definatly not Iron Oxide, Although There WAS a layer of what MAY have been Fe2O3 on top, it wouldn't be easy to seperate. After adding NaOH to the solution, The brown precipitate Turned into hte green crap. That's all the testing I've done. I will add iron hydroxide to my Iron oxide tonight. If it turns greenish black, I will concede that you can make SOME Fe2O3 with this method. (Although purifying this would be a pain.) If it does nothing, then that brown precipitate ovbiously wasn't Fe2O3.

 

Oh yeah, there was also some brown precipitate on the stell wool that I used as an anode... I will also test that. NOW, if your saying that heating this Iron hydroxide that you produce will convert to Iron Oxide.. You may very well be right I have no idea... Is this what yoru trying to say?

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wait a minute

i know that if you use salt as an electrolyte, oxygen doesnt form at the anode until after a bunch of chlorine has. and i know that if you use a copper anode to try to make copper oxide (also useable in thermite, I'm told), and put salt in the water, you get copper chloride (neat green color :) ), not copper oxide. Does chlorine bond in this way with iron, or just with copper? I would assume you wouldnt want any iron chloride crap in your thermite.

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ok ill crarify the method. get dilute salt slution, dip in 2 iron electrodes, hook them up to dc current. mine was 30 volts adapter. id run that for a few hours, the bucket would be full of stuff floating around. id poaur the stuff in a cup, then let it settle, then pour off the execc, and repeat. after a while i had like a cup of the gunk still in water. id set that under a lamp for a day or two, and id get a good amount. after u dry it its like brow, but after u heat it in a dish its nice and red.

 

 

ps: my crappy avatar is an example of my iron oxide

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get dilute salt slution' date=' dip in 2 iron electrodes, hook them up to dc current. mine was 30 volts adapter. id run that for a few hours, the bucket would be full of stuff floating around. id poaur the stuff in a cup, then let it settle, then pour off the execc, and repeat. after a while i had like a cup of the gunk still in water. id set that under a lamp for a day or two, and id get a good amount. after u dry it its like brow, but after u heat it in a dish its nice and red.

[/quote']

 

I did somenthing similar, but not the same. I had a 30 V DC adaptor too. I striped the copper wire of insulation and put it in an electrolyte of plain tap water. The other electrode was an old iron nail connected witha croc. clip. I kept on getting loads of reddish/brownish stuff. After the whole vessel was like dark brownish, I emptied it and filled it up with clean water again to continue, since I have no use for whatever the substance was. It smelt like Iron though. I am presuming it is Fe2O3.

 

On another occasion, I kept on elctrolysing sea water! with different electrodes( the last and longest used was the iron nail) until the solution was of a similar colour to that mentioned before. I removed as much excess liquid and left the vessel to evaporate. Two days later, I was left with a crust of solid with liquid beneath it. On turning, atirring and leaving for another day, I formed a fine red/brown powder, again smelling of Iron. What could this be?

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Got this from another forum...

 

"Sarevok - making rust

 

You can simply mix a saturated solution of an hydroxide (such as sodium hydroxide, "lye") or of ammonia to a saturated solution of an iron salt (such as iron sulfate, chloride, nitrate, anything - as long as its soluble, that's it). Ferric hydroxide will precipitate. You then filter it and leave it to dry; ferric hydroxide is unstable and turns to ferric oxide (rust) as it dries."

 

Therefore, Akcapr, I concede this debate :) So you can Make Fe2O3 that way, I also heard on a forum that Bleach and Vinegar (2:1 ratio) Will disolve steel wool very quickly. So.... There ya go.

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I know you never said it wouldn't you were pressing that it WOULD.. lol. Right now I am electrolysing Steel wool in NaCl solution. I should get Iron Chloride which will immediatly precipitate Iron Hydroxide.. Correct. So the drying and heating should Yeild Fe2O3. Perfect.. maybe.

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Hey guys, I don't have a bunsen burner or a gas stove or an alcohol lamp or any kind of labware to heat my useless brown iron hydroxide. I want to heat it to make my iron oxide but I don't want to use my mom's cookware and my stove is electric making it hard to heat things evenly. What would you guys recommend?

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Speaking of this, I just did a little experiment. I electrolyzed steel in NaCl. I got this yucky black color (as I did before). After decanting and refilling with water once, the color remained the same. I headed out to a festival and a few hours later to find the water rust-colored. So now I'm continually decanting to get rid of residual NaCl. I believ eeverything is working nicely, although I'd like a higher amperage power supple than my crappy 12 Volt AC adapter. This takes forever. After that, I jsut need to test it. Unfortunatly, thus far I have found it near impossible to make aluminum powder by chemical means. As for putting it through a mill, I don't have one of those either..

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Hey guys, I don't have a bunsen burner or a gas stove or an alcohol lamp or any kind of labware to heat my useless brown iron hydroxide. I want to heat it to make my iron oxide but I don't want to use my mom's cookware and my stove is electric making it hard to heat things evenly. What would you guys recommend?

 

This one is a bit fiddly, but certainly doable and dirt cheap.

 

Run a search for "soda can stove".

 

You should find instructions for converting 2 empty soda cans into a nifty little spirit burner.

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Got this from another forum...

 

"Sarevok - making rust

 

You can simply mix a saturated solution of an hydroxide (such as sodium hydroxide' date=' "lye") or of ammonia to a saturated solution of an iron salt (such as iron sulfate, chloride, nitrate, anything - as long as its soluble, that's it). Ferric hydroxide will precipitate. You then filter it and leave it to dry; ferric hydroxide is unstable and turns to ferric oxide (rust) as it dries."

 

Therefore, Akcapr, I concede this debate :) So you can Make Fe2O3 that way, I also heard on a forum that Bleach and Vinegar (2:1 ratio) Will disolve steel wool very quickly. So.... There ya go.[/quote']

 

YOU FOUND IT!! :D

 

Still, I'm not sure the Fe2O3 is pure, since there's still some blackish residue, and the roasted powder doesn't go RED-red.

 

I guess I'll try the electrolysis next (scrounged a few transformers AND remembered the old car battery charger lying around).

 

Otherwise, it's the Steel Wool Wait... Or find a quiet place to chlorinate...

 

THX guys! I got some new angles on the matter.

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