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Author: Subject: potassium cyanide
GrayGhost-
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[*] posted on 4-8-2018 at 16:12
potassium cyanide


I tempt synth potassium cyanide from termic process KNO3 + 4C = KCN + 3 CO , Carbon was obtain from sugar calcinated, like grain was coarse I grindin in my mortar ( and pestle obvious) , mixture both components and warm with my oxyacetileic torch.

1) first run performed y little recipient of iron and was ignited with much smoke.

2) second run performed in this artefact.



7xrQVp3.jpeg - 289kB


and same result mixture ignited again.

The artefact is composed by long tube is reaction chamber, glass with oil actuate like valve avoid intake oxygene, the short tube is security chamber is when cool down suck oil and remain in this chamber and avoid contaminate of final product.


Im thinking in use carbon of coarse grain for avoid ignite again.

I m need suggestions please.




[Edited on 5-8-2018 by GrayGhost-]
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Foeskes
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[*] posted on 7-8-2018 at 02:06


Maybe use excess carbon and purify the product with CH3OH
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[*] posted on 7-8-2018 at 07:43


Quote: Originally posted by Foeskes  
Maybe use excess carbon and purify the product with CH3OH


I used excess carbon, but ignite.

The residue pour in water, carbon was precipitated, the liquid clear mixtured with diluited muriatic acid, and fizzing. Is this CNH? I dont have courage for smell :D.

in 3° test use wet mixture, because steam displace oxigen of chamber, and again ignite.

I think use more coarse grain of carbon.

[Edited on 7-8-2018 by GrayGhost-]
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Foeskes
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[*] posted on 7-8-2018 at 15:41


To be honest I think if you heating a mix of carbon and KNO3 long enough, it'll always ignite. It's likely carbon dioxide from the formed potassium carbonate. The main problem about this reaction is that Cyanide's are reducing agents and your melting it with a oxidizing agent maybe if you heat the ignited mix with charcoal even longer. Maybe you should use the urea method.
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[*] posted on 7-8-2018 at 17:26


Quote: Originally posted by Foeskes  
To be honest I think if you heating a mix of carbon and KNO3 long enough, it'll always ignite. It's likely carbon dioxide from the formed potassium carbonate. The main problem about this reaction is that Cyanide's are reducing agents and your melting it with a oxidizing agent maybe if you heat the ignited mix with charcoal even longer. Maybe you should use the urea method.


the next idea

4 run charcoal coarse grain.

5 run mineral carbon type coke.


The urea methode is for ferrocyanide or is other more direct?




[Edited on 8-8-2018 by GrayGhost-]
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[*] posted on 7-8-2018 at 18:05


There is an extensive discussion and good information on the various methods of cyanide production, including the urea method, in this thread:

http://www.sciencemadness.org/talk/viewthread.php?tid=23

I would not recommend heating a mixture of potassium nitrate and carbon/charcoal in a semi-sealed metal tube. The mixture is like sulfur-less black powder, and the metal tube is like a pipe bomb if it gets clogged. Very dangerous.




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GrayGhost-
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[*] posted on 7-8-2018 at 18:27


Well i find the patent of Mr Kellner, he use arc electric furnace, melt previosly the nitrate and mix with carbon for produce nitrite, then go to electric furnace.


US patent 579988. citaded by Polverone.

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Boffis
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[*] posted on 8-8-2018 at 02:20


Could you dilute the K nitrate with potassium hydroxide to reduce the tendency to deflagrate. Then leach the residue with a small amount of alcohol to preferentially remove the excess KOH.

Alternatively how about using potassium cyanurate and charcoal?

K<sub>3</sub>C<sub>3</sub>N<sub>3</sub>O<sub>3</sub> + 3C &rarr; 3KCN + 3CO

K3C3N3O3 + 3C -> 3KCN + 3CO

Does anyone know why all of a sudden the subscripts won't display correctly in HTML

[Edited on 8-8-2018 by Boffis]

[Edited on 8-8-2018 by Boffis]
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GrayGhost-
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[*] posted on 8-8-2018 at 08:10


Quote: Originally posted by Boffis  
Could you dilute the K nitrate with potassium hydroxide to reduce the tendency to deflagrate. Then leach the residue with a small amount of alcohol to preferentially remove the excess KOH.

Alternatively how about using potassium cyanurate and charcoal?

K<sub>3</sub>C<sub>3</sub>N<sub>3</sub>O<sub>3</sub> + 3C &rarr; 3KCN + 3CO

K3C3N3O3 + 3C -> 3KCN + 3CO

Does anyone know why all of a sudden the subscripts won't display correctly in HTML

[Edited on 8-8-2018 by Boffis]

[Edited on 8-8-2018 by Boffis]



The trick is NO2K not NO3K according to patent. I dont have acces to KOH, NaOH . Is forbidden and /or restricted here.

Can preparate cyanurate with DCCA ?
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Foeskes
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[*] posted on 8-8-2018 at 14:47


https://youtu.be/xz7i11XC9wk
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[*] posted on 9-8-2018 at 06:03


Quote: Originally posted by GrayGhost-  


The residue pour in water, carbon was precipitated, the liquid clear mixtured with diluited muriatic acid, and fizzing. Is this CNH? I dont have courage for smell :D.

[Edited on 7-8-2018 by GrayGhost-]


O MY GOD ... DON'T TRY TO ADD ACID TO CYANIDES. THAT'S NOT A GOOD TEST !! Use iron chlorides in dilute conditions !! The Prussian Blue test
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AJKOER
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[*] posted on 10-8-2018 at 15:01


Here is a good historical account of methods, mostly at elevated temperatures, see https://www.911metallurgist.com/blog/how-to-make-cyanide .
-------------------------------

Did come up with a 'radical' idea based on the possible action of the hydrogen atom radical on cyanate at low pH absence oxygen. Likely paths include:

.H + OCN- = OH- + .CN

Or: .H + OCN- = .OH + CN- (most probable being reverse of Eq (12) in the Haynes reference below)

Or: .H + OCN- = .OHCN- (which could interestingly be akin to the chlorine .OHCl- radical anion)

If .CN is created, possible further reactions:

.CN + .CN --> (CN)2

(CN)2 + H2O --> H2C2O4 + NH3 (which could produce an insoluble oxalate precipitate)

.H + .CN = HCN

.CN + H2O = .OH + HCN
......

Some background on the cyano radical see https://en.wikipedia.org/wiki/Cyano_radical and https://www.sciencedirect.com/science/article/pii/0010218077... Also, see https://aip.scitation.org/doi/10.1063/1.463945 for other suggested (unexpected?) reactions.
-------------------------------------

Sources of .H include:

Fe --> Fe(ll) + 2 e-

Fe(ll) --> Fe(lll) + e-

H+ + e- = .H

.OH + H2 = H2O + .H

and also, heating H2 to high temperatures, and photolysis of pure hydrogen,....or ELECTROLYSIS of water in the presence of an oxygen scavenger.
----------------------------------------

Performing a search on electrolysis involving cyanates finds an old mining method to recover ore claiming 'Cyanide Regeneration' employing an oxygen scavenger (KI is recommended). See Engineering and Mining Journal, Volume 90, Ocober 8, 1910, discussing the 'The New Clancy Cyanide Patents', at
https://books.google.com/books?id=wIogAQAAMAAJ&pg=PA701&... .

The author of the process notes a major well known obstacle in working with cyanates, to quote:

"when cyanates are allowed to stand for any considerable time, or are retained in solution, they are converted into ammonia and potassium carbonate, and are transposed by the lime used in the cyanide process into insoluble carbonates or by the action of sulphuric acid in the ore into sulphates—so that the original cyanide finds itself eventually in the residue dumps in the form of sulphates or insoluble carbonates."

The Clancy method further involves also the addition of an amide compound to quote:

"To show the action of these amide compounds, take, for example, urea (carbamide) and add this to a solution of a cyanate (such, for example, as potassium cyanate) and electrolyze this mixture between inert electrodes. After a few minutes the said mixture will be transformed into one which will dissolve the precious metal in alkaline solution. "

The role of amide in recent work ("Bifurcate localization modes of excess electron in aqueous Ca(2+)amide solution revealed by ab initio molecular dynamics simulation: towards hydrated electron versus hydrated amide anion." by Zhang R, Bu Y., see https://www.ncbi.nlm.nih.gov/pubmed/27351489 ) suggests a promotion of solvated electron activity. See also https://www.sciencedirect.com/science/article/pii/0146572484... .

Bottom line, one may find this old Clancy method as a path to convert CNO- to CN-, which I discovered based on my 'radical' idea.

Related chemistry, see https://www.911metallurgist.com/chemistry-cyanogen-compounds... .

[Edited on 11-8-2018 by AJKOER]
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