Making Iron Oxide

[A_W]

Yesterday I tried to make Iron Oxide (Fe2O3).
I followed the instructions from the Anarchists handbook: "Electrolyte a saltwater solution with two Iron nails connected to a 12v battery"
After 3 hours when dark Fe2O3 should start to collect at the bottom; some white, slimy shit appeared at the positive nail.
My question is: What the hell did I do wrong??????

-Sorry if my English sucks; I`m from Norway-

[Lagen]

Your book probably isn't a very reliable source of chemistry information. If you want the quickest, easiest way to make loads of iron oxide, try pouring some sodium hydroxide solution (lye) into circuit board etchant (ferric trichloride and hydrogen peroxide solution). It works wonders. (For use in thermite you should calcine the resultant iron oxide-hydroxide powder, but you should do the same with rust.) Or search for a topic entitled "Iron sulfate", you'll find more about other ways of making it.

[A_W]

Thank you very much for your help!!!
I totally agree; those anarchists handbooks are not very reliable.

[Lagen]

I just found out that the Iron Sulfate topic is not accessible now, I believe it should be in the July or August archive which still isn't up. Basically, you can use a solution of iron sulfate in place of the PCB etchant. What you will get will be a bluish-grey powder (iron hydroxide) which will slowly oxidize in air to form the brown oxide-hydroxide. The same thing will happen if you have a different formulation of etchant which doesn't use peroxide. (Sometimes there is even no iron at all, so ask before you buy.) You can add hydrogen peroxide to speed up the process, but not necessary. Baking the powder in fire to get the red form (for thermite) will speed it up enough.

You can get the iron sulfate in tree nurseries, and some garden shops, it's used to prevent the growth of moss. Most garden shops sell different (more expensive) preparations though. Ask at the nursery if they would sell you a bag.

About that crapbook recipe, the problem is that these books give recipes which might or might not work, depending on many circumstances, which they don't tell you. I think your pH got too high too fast and no chlorine was formed at the anode. But even if you maintain the pH, you mostly produce chlorate and hypochlorite. And electrolysis is slow. The chemical processes are much better.

If you have access to acids, try making your own iron sulfate or chloride. With hydrochloric acid, you must add the metal very slowly (not more than a few grams at a time) otherwise the acid will start to boil and give off lots of hydrochloric gas.

And I'm sure you know, the easiest way of getting the oxide is pottery (ceramics) shops.

[rikkitikkitavi]

try well sorted paint shops for Fe2O3, it sold as
a red paint filler, just like for pottery.

saw you where from norway. The red powder used to paint cottages in scandinavia is commonly Falu rödfärg or an other derivate. Normally you can buy the powder for making your own "antique" paint.

The main problem with preciptating Fe(OH) by mixing NaOH and Fe3+ is that the preciptate is formed as a volumnious mass with lots of water.
And it is a fucking mess to filter.

You need to stirr the solution well to get good results.

Better is to mix urea with Fe3+ salts. Heat it and voila! Fe(OH)x preciptates. As a nice solid mass that easily filters.

C(NH2)2+ H2O = CO2 + 2NH3 (upon heating)
3 NH3 + 3H2O + Fe(3+) = 3NH4(+) + Fe(OH)3

/rickard

[ January 06, 2002: Message edited by: rikkitikkitavi ]</p>

[BoB-]

I'm not sure if this made it into the Uber-chive, so I'll reprodue it here.

--------------------------------------------------
Originally posted by NBK2000


Why are you people doing these things the hard way? Just follow the process below and
you'll have all the rust you can handle.

I've followed it and it works, it's just slow because you have to wait for shit to settle but
actual work time is only a few minutes.

=========================================
Iron (III) Oxide the EASY way.

So you've read the anarchists cookbook on making thermite, you want iron (III) oxide but
don't want to run the risk of shorting out the electricity in your entire house, while at the
same time electrocuting yourself while choking to death on chlorine fumes.

Let's face it, getting Iron (III) oxide with electrolysis is dangerous, takes ages
(I had it hooked up for a few days in my garage and got less than an eighth of a gram of
rust), and if you don't have an AC to DC
converter your fucked.

You want a good chemical method for extracting Iron from stuff containing iron.

You will need:

2 glass jars
funnel
filter paper
ammonia or caustic soda (sodium hydroxide)
water
Iron sulphate plant food (or anything else containing iron)

1) Add some ammonia to a jar containing water, the ammount isn't important (you don't
need much water if your using
ammonia).

2) Get your Iron sulphate and crush it up
3) Add to the other jar and add just enough water to dissolve it.

Once again the ammount of water isn't important, just dissolve as much as you can
in a bucket and scoop out the solution as you need it.

4) Tip the contents of jar 2 into jar 1, now stir.

What do you see? green shit in the jar. The green stuff is Iron Hydroxide, now for those
of you doing either A-level chemistry or
GNVQ science, I will point out that iron hydroxide is unstable as it is lacking a third
oxygen molecule, hence it is Iron (II) Oxide.

5) Filter the green stuff out, use jar 2 to filter the liquid into. Save the green stuff.
(beyond this the steps are optional)

6) Add more water to jar 1, then add the green stuff, now stir.

7) Filter out the green stuff (should be turning brown)

8) Leave to dry, by the time it has dried it will have turned brown/red
in colour. This is pure Iron (III) Oxide, and it's as fine as flour.

Now wasn't that method much more simpler and quicker than hooking up all of the stuff
that you would need if you did it the other way?

If you want to do this on a mass scale, simply do the following:
Get two buckets, a bottle of ammonia and a large box of fertiliser
stuff (containg iron).

1) Tip the fertiliser stuff into the first bucket, with some water to
dissolve it all.

2) Tip the ammonia into the second bucket.

3) Tip the first buck into the second bucket and stir.

4) Filter and save the green shit. (Will oxidise compleatly in a few minutes).

Carrying out either of these methods takes less than five minutes to do.

(copied and pasted)

[Lagen]

Okay here's what I did. I took some saturated 45% FeCl3 soln. (55ml) and added 23g of urea (a slight stoichiometric excess). Started heating gently, at 98°C the urea dissolved and the reaction proceeded slowly at first. At 107°C the mixture became quite uncontrollable so for the rest of the time I ran it at about 100°C. After 90mins. the reaction was over, testing with aluminum foil there was no FeCl3 left, and the mixture was discoloured with fine brown precipitation (more in the form of a powder). Then the mix began boiling gently, but at 115°C it suddenly made a lot of froth, so I must have removed it from the heater. So when you do this, watch out near the end. Now it dries, so I don't know the yield yet.

Rickard, I think there are some good and bad points about both methods. Some people might not get urea very easily. Also, not everyone will want to take the time to do this process. The stuff tends to splatter, upon landing on the heater hydrochloric gas is given off, or it just corrodes the heater. So you need a flask and a return condenser. Anyone attempting to cover a beaker with aluminum foil will get an unpleasant surprise! But as you said, the stuff filters nicely.

On the other hand, I should imagine that people doing the hydroxide process would rather wash and decant their product, then boil it over a fire and, while still in the same container, bake it to get the hematite. Also maybe that the more voluminous stuff could have a higher specific area, but I would need some measurements to support that.

[nbk2000]

I took a cup of IRONITE plant food and tossed it in a 5 gallon bucket, covered with 2 liters of water, and stirred with my hands for a minute. After letting it settle, I poured off the water into a water cooler bottle.

I repeated the washing of the plant food twice (as described).

Then I added plain ammonia water a few ounces at a time to the solution which turned a very dark greenish color from the precipitation of fluffy gelatinous blobs.

The precipitate was very dark and voluminous, not settling out rapidly, but rather, staying suspended.

So I greatly diluted the solution by adding enough water to bring up the total volume to about 3 gallons.

This allowed the precipitate to seperate towards the bottom half, permitting titration with the ammonia to the end point.

After letting it settle for a couple of hours, I then used a siphon to suck up the greenish brown sludge from the bottom into a T-shirt filter in a bucket at a lower elevation.

The greenish mud rapidly clogs the filter so you have to keep scraping the mud off. Paper filters are impossible to use for this purpose.

I then spread out the (now) reddish mud into a very thin layer on a very large dripping tray in the sun to dry, scraping occasionally.

In the end I got about 2 ounces of slightly grainy red oxide powder.

My total cost would be about 25 cents for the iron I got and probably about 15 minutes of actual working time. Now that I know how to do it, I would wash the entire 10 pound box of plant food in a 5 gallon bucket so that I had 2 buckets full of the washings (10 gallons).

Then I'd pour half of these 2 buckets into another 2 buckets (4 half full total) to add the ammonia to it (premeasured from prior tests), stir, let sit, dilute up to a full bucket, let sit, then siphon through a large cloth filter.

Then oven dry the mud rather than wait hours for it to dry in the sun by itself since it form a hard crust on itself as it dries that keeps the insides wet.

This would get you about a pound of oxide for a half hours work, not counting wait time.

Or buy 25 pounds for $20 at the ceramics supplier.

[SATANIC]

i just found the stuff at a place called hardware house. they are australia wide for those in aussie, it's sold by the name 'builders oxide' and is used for colouring diy concrete / mortar. see the most recent catalogue in australia, it's $7.40 for one kg. ( right next to 500ml of HCl for $4.80)

[Mick]

sorry for been so dense, but what chemical did you find at hardware house?
(theres a few chems listed in this topic, and i don't know which one you found)


(Builders Oxide...Iron Oxide...2+2=? NBK2000)

[ January 11, 2002: Message edited by: nbk2000 ]</p>

[A-BOMB]

My grandfather is a stone and brick mason and has a few types of coloring like that, I'll get some and test it so see what it is. And what color was it black, grey, redish, light orange?

[RTC]

Who cares, try them all!

[mongo blongo]

Those who have tried NBK's method have probably had the problem of the shit getting on your hands and staining everything! It very hard to get rid of this stain with soap and water.
Does anyone know any better ways to get rid of the stain? It's a pain in the ass!

<small>[ March 19, 2002, 05:39 PM: Message edited by: mongo blongo ]</small>

[kingspaz]

hmmmm.....very dilute HCl would work. it would react with the oxide to make iron chloride which is soluble i *think*. if it is soluble then the HCl will rinse it off....when i say dilute i mean about 0.5% solution. don;t put it on your face or brocken skin!.....infact don't wash in acid!

[mongo blongo]

Thanks, Im gona try it! :)

[nbk2000]

vinegar may work also, and is much safer.

[mongo blongo]

Yup, they both seem to the trick.
Thanks. :)

[Smkymcnugget420]

I took a cup of IRONITE plant food and tossed it in a 5 gallon bucket, covered with 2 liters of water, and stirred with my hands for a minute.

Found this at: http://en.allexperts.com/q/Lawns-725/question-Ironite-1.htm


"There's so much wrong with Ironite, I don't know where to begin. Let's start with the Environmental Law Foundation lawsuit detailed in their press release posted on the internet, "Ironite Sued for Toxics in Fertilizer and False Advertising" (http://www.envirolaw.org/poison.html).

The problem: "'Ironite' is made from mine tailings from a proposed Superfund site in Humboldt, Arizona." That site is the Iron King copper mine. The toxic waste-based product is LOADED with 2 things they don't tell you about: Arsenic and Lead. In fact, there's so much Arsenic and Lead in Ironite that it qualifies as Hazardous Waste, based on government tests in Oregon."

Will the Arsenic & Pb effect the reaction, or be released somehow? Sorry I'm not a big Chemistry buff so I don't really know how to approach the problem, I am studying though so hopefully I'll be of more use to the forum soon.

I found all kinds of chemicles here, lots of "______" oxides:

http://www.baileypottery.com/shipping-policies.htm#Web

They do international orders but its expensive.

[Bacon46]

I purchase Fe2O3 at my local home improvement store in the form of red powdered concrete dye. I doubt if the feds are ever going to ban iron oxide.

If you really want to make it yourself, I was reading The Do it Yourself Gunpowder Cookbook by Don Mclean. In it there is a paragraph or two on making Fe2O3. I have never tried this but it seems like it would work, and be very easy and inexpensive.

In it he states:

“If you have fine steel wool you can make Iron Oxide very quickly. Clean the steel wool with solvent (it comes from the factory lightly oiled) and dry it. Fluff it apart and hang it in a closed jar with a small bottle cap full of HCl at the bottom, and it will turn to rust almost overnight. When it is completely rusted, crush it in your hand like a Shredded Wheat biscuit and sift it through a fine screen.”If you hung the steel wool close to a running chlorate cell you could kill two birds with one stone and make chlorate and Fe2O3 without expending any additional energy.:D

Thanks to Mr Science for providing The Do it Yourself Gunpowder Cookbook, and all of the other interesting torrents he has uploaded.

[chemdude1999]

I'm still chuckling at the thought of banning rust.

As a side note, I digest many water samples at work in a nitric acid solution. The hot block is in a fume hood, of course. It is one of the older styles with metal fixtures up top. After many years of use, there is now a steady supply of finely powder oxide at the bottom near the back of the hood. Years of acid vapors has compromised the roof ducting. I usually just wipe it up and throw it out.

[rangegal]

I get my rust from an old 55 gallon drum in my backyard. Doesn't provide enough for any good size of thermite obviously (although I have made thermite from it). I use it for my KN/SU rockets.

Filled up this little vial from just half an hour of scraping.
http://img521.imageshack.us/img521/8593/dscf3384smalljs6.jpg

[futuredictator]

I just use the electrolysis method. I wrap a 12v AC adapter's positive (i think) wire around about 5 iron nails, and dunk it in a plastic bottle full of water and a dash of sodium hydroxide. then just fray the negative wire, so there's more surface area, and dunk it in as well. But make sure the negative and positive wires/ nails don't touch or arc. The nails are usually decomposed in about 2-3 days, mix it up until it's an even color, then I pour it all into a foil pan and leave it out in the sun to evaporate. After it's dry, just crush it up in a bowl, or if you're special, a ball mill. This obviously takes awhile, but I'm really in no rush.

[ChippedHammer]

Just go to any large hardware store and look in the concreting section, I picked up red and black iron oxides for $7 a kilogram.

[Polumna]

Hi

Another good way to make Fe2O3/O4 is to get some ironwool from your supermarket ( I got mine ( 500g) for 3€), then take a battery or a blowtorch and burn it inside your mortar&pestle.
The resulting ironoxide is very brittle and you can grind it up in your mortar&pestle very easy.

I tried it in thermite and it worked very good.

[tmp]

I'll have to go with ChippedHammer on this one. I get red iron oxide for $2
LB. from my local pottery supplier. For me, there's no point in making it
myself. Even the steel wool would cost me more !

[PeterB2]

Out of curiosity, what kind of oxide (i.e. in which oxidation state is the iron) is produced by simply burning steel wool? Would it depend at all on how fine the wool is or other reaction conditions?