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Author: Subject: Potassium Ferrocyanide from Potassium Nitrate and Iron Oxalate
j_sum1
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[*] posted on 25-9-2024 at 19:42


I have some experiment results. (Notable because I actually got to spend some time in the lab.)
Both based on cyanuric acid.



Experiment 1 – 350°C reaction between Iron oxalate, potassium carbonate, cyanuric acid and carbon

2FeC2O4 + 4C3H3O3N3 + 4K2CO3 +5C --> 2K4[Fe(CN)6] + 13CO2 + 6H2O

Heated 12g of FeC2O4 and other reagents in stoichiometric quantities over a butane burner in a cast iron crucible with loose lid.
Powdered mixture became fluidised releasing lots of gas. When temperature exceeded about 330°C a thick tarry substance was formed with continued bubbling. Above 350°C there was an odour of ammonia offgassing. Temperature was lowered and reaction continued until bubbling ceased.
Result was a solid cake which was scraped away with some difficulty with water. Filtering the suspension gave a dark residue that looked like FeO. Filtrate was cloudy and rust coloured and slightly acidic. No evidence of either ferrocyanide or ferricyanide. My suspicion was that the carbon did not react at all and that much of what I had obtained was merely decomposition products. This led me to attempt a lower temperature route.





Experiment 2 – Reaction between Iron oxalate, potassium carbonate, cyanuric acid and oxalic acid in aqueous suspension

FeC2O4 + 2C3H3O3N3 + 2K2CO3 + 5H2C2O4 --> K4[Fe(CN)6] + 14CO2 + 8H2O

Suspension was formed with 7.75g of FeC2O4 and other reagents in stoichiometric quantities in 150mL of water in a 500mL RBF. Mixture was stirred and refluxed for 12 hours.
Product contained quite a lot of solid that settled out. Filtering gave an acidic solution that was a lime-yellow colour (concidentally, the exact same shade as a K3[Fe(CN)6] solution I had on hand - at least to my eyes.)
Product was tested with Fe3+ and Fe2+ solutions and did not behave as either ferrocyanide or ferricyanide. Presence of oxalic acid could potentially have affected results. Further testing after neutralising revealed trace amounts of Fe(III) in solution but not the desired product.

Clean up suggested that very little of the iron oxalate or cyanuric acid had reacted. I suspect that my solution was mostly a ferro-oxalato complex in oxalic acid.


I am prepared to give up on iron oxalate as a starting material for obtaining ferrocyanide.

[Edited on 27-9-2024 by j_sum1]
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[*] posted on 26-9-2024 at 08:48


j_sum1

If you are willing to do it. Try PolyAcryloNitril.

I would love to see result.

I would do it myself and post the result but I currently don't have the means to perform it where I am.

...

It is sais that it should be heated withoit oxygen presence. Then it produces according to DATA as much as 10%-30% HCN.

It might be that you could take test tube and put a stopper and bubble the gaseous product into KOH

And then react this Cyanide to produce FerroCyanide

Edit

Polyacrylonitrile is also known as polyvinyl cyanide

[Edited on 26-9-2024 by Random]
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[*] posted on 26-9-2024 at 09:34


I thought the whole point of this thread was to make ferrocyanide without using HCN gas. There are many easier ways to make hydrogen cyanide, but the disadvantage is that they all produce hydrogen cyanide.



Quote: Originally posted by bnull  
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[*] posted on 26-9-2024 at 09:41


Quote: Originally posted by clearly_not_atara  
I thought the whole point of this thread was to make ferrocyanide without using HCN gas. There are many easier ways to make hydrogen cyanide, but the disadvantage is that they all produce hydrogen cyanide.


It seems less scary when using PolyAcryloNitrile.

...

You know. Imagine being near a fire with this plastic burning. You would not even know it.

Also FireFighting.
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[*] posted on 26-9-2024 at 17:51


Keep in mind that ferrocyanide itself decomposes into cyanide, carbon and iron when heated.
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[*] posted on 26-9-2024 at 19:25


One route to Cyanide could be also this route as it is inside Biological process. Is it Amgygdalin?

You know. There was this VIDEO on YouTube.

Dissolving Gold with Cherry Pits

...

I believe you need to get used to Cyanid. Of course it is scary if you deal with Concentrat.

...

You can use Dilluted SOLUTION. Turn Dilluted SOLUTION into FerroCyanid.
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[*] posted on 26-9-2024 at 20:30


Quote:
Imagine being near a fire with this plastic burning. You would not even know it.

Cyanide is highly flammable and rapidly consumed in a flame. The amount released would be much smaller than through pyrolysis. Even so:

https://journals.lww.com/euro-emergencymed/fulltext/2013/020...
"HCN from fire smoke is probably the most common cause of acute cyanide poisoning in developed countries"

Any use of ionic cyanides is very dangerous. Avoiding it is definitely worthwhile.




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[*] posted on 26-9-2024 at 21:29


Quote: Originally posted by Random  
j_sum1

If you are willing to do it. Try PolyAcryloNitril.

I don't have any, so that is not really an option.

Realistically, I will probably just buy some potassium ferrocyanide to replenish my stocks. The appeal was the possibility of a straightforward 1 pot synthesis using things I have a surplus of.
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[*] posted on 26-9-2024 at 21:45


You know. I was reading those Insectronics and Amphibionics books according to my personal memory inside 2006.

Was it 2006.

...

You know. You could build a simple Robot to do it for you.

It is a novel idea. Why risk your life with a toxic substance if you cam do it from distance.

It is a little bit offtopic but

...

You know. Things are changing.

In 2010 when I joined here the world did not have so many options.

Edit:

Getting experienced and courageous but not foolish in handling what we could mark as extremely dangerous substances is a process in itself.

Ontopic. A discussion could be why it is not possible or ehy it was not in this case possible to perform this from KNO3 and FeOxalat.

...

There were more how I could say ideas regarding this topic.

[Edited on 27-9-2024 by Random]

Edit2:

Processes behind various chemical reactions should be more deeply investigated. Which we could call mainstream scientific community is too...

Here I was interrupted in writing this post.

Between everything unlisted if they were capable they would also be here.

[Edited on 27-9-2024 by Random]
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