Phosphorus extraction. (completed) :)

[YT2095]

I`m just average I guess, thnx for the compliment though, I have a fan club of One at least )

 

I seriously reccomend NO ONE try doing this at home though!, I must be either immune or very lucky again as 50mg+ of Phosphorous is lethal !!!

 

Don`t do it! ))

[aommaster]

Oh, don't worry, I won't be ABLE to!

[YT2095]

actualy it`s ridiculously easy! don`t underesstimate the simplicity!

I`ll say no more about that

[Crash]

Indeed, and well done again

[jsatan]

I know this is digging up an old thread, but more info the better,

 

couldnt you have put the white phos under water then leave sunlight to change it to red phos?

that's got to be safer than heating it to 250c or whats ever it needs, lol.

 

Btw I came across this thread via google, I wasnt looking at phos glowing.

[budullewraagh]

according to my phosphorus allotropy chart, if you take cubic white p and heat to 44.1 celsius, it can liquify (and supercool). from here, one can heat the reaction to 300 celsius or expose to light or x-rays

[jsatan]

I know this isnt something YT would want to answer, but after you made the phos acid you added carbon.

How did you get from this to phos?

I'd go with the light, seems safer to me, I wouldnt want to heat it, lol.

[budullewraagh]

the carbon reduces the phosphoric acid to phosphorus. carbon monoxide is formed. i would imagine that there would be some formaldehyde and other carbon-oxygen-hydrogen compounds that would facilitate the reduction of phosphorus with a 3:4 hydrogen:oxygen ratio

[jsatan]

aha Thats better,

I had it in my head that it was (H)nP not H3PO4.

I was thinking as he said charcoal works as well, I thought the carbon was being turned into hydro carbons, I was like wth.

My chem isnt that good,

But I'm learning,

[jsatan]

So (just from a quick read and think)

you "dry the phos acid

to turn it back to "Phosphorus pentoxide, P2O5 (P4O10)" add carbon and you're done?

what temp does this have to be at?

[budullewraagh]

i would imagine that high temperatures would be required as effectively you're doing a thermite. i would imagine that it would be a good idea to dry the phosphoric acid. interestingly, 88% H3PO4 has a great deal of the anhydride in it

[jsatan]

I've got about 1litre of phosphoric acid from my hydroponic growing etc.

Yeah as far as I know I'll have to boil the water out of it to make the H3PO4 into the oxide, but thats changing it alot.

I've got 85% phos acid.

 

Would it require more heat than ironoxide alu mix?

 

I've manage to make that work just using ironoxide powder and alu foil chopped into bits.

I'v got a hot head which is used for glass working.

uses mapp gas and it got the alu white hot easy, but if its hotter than that in a test tube then that even for pyrex is hot. Not that it would bother the pyrex but thats a hell of alot of heat.

 

come'on YT be a sport,

Pm me, please.......

[jsatan]

Doesnt heating phos acid to remove the water make pyrophosphoric acid metphos acid?

how would I get it back to phos oxide?

That is what I'm aiming for isnt it?

[jsatan]

hummm. I think I've figured it out.

phos acid + carbon heat it till about 130c (I think this is the temp) and what comes of will be E-phos and others co2 etc.

this needs to collected with out contact with air.

So using phos acid thats is of high concentration or water work.

I'm getting there,

Its good fun trying to unlock the puzzle.

[jsatan]

YTI may be wrong but from what Ive been reading you get phosphine as well as a misty gas.

What did you do with yourd, burn it?

 

Also you must of had this up to a very high temp, 1800c range If I thinking right.

 

I havent found anyway of doing it using phos acid apart from using lead but this isnt very good, so they say.

 

I've read alot of forums and most people find it much harde then just adding phos acid and carbon and heating.

 

Strange, you there YT?

[YT2095]

I`m here

 

what exactly was your method, I only wrote mine down basicly, did you leave the carbon and the conc phos acid to stand a while? I left mine for just over 24 hours ontop of a room heater to make sure it was completely dry and intimately mixed as absorbed into the pores of the carbon, then gently heated it over a flame after to drive off any excess moisture, as soon as there was the garlic type smell I capped the tube with a bleeder pipe, THEN you turn up the heat, the carbon will start to Glow dull red at 1`st then bright orange, leave it like for a good five minutes, if you`re in a darkened room you`ll actualy see tiny green "Sparkles" appear towards the top end of the tube and a perfectly horrid smell. let it cool slowly, the glow will still be there and more so if you uncap the tube!

it really isn`t hard, it takes alot of patience and the results vary, from lame to WOW!

keep the quantities small, don`t try and scale it up. basicly that`s all there was to it, I`m sure I`ve not forgotten anything, as for 1800c I`ve no way of measuring the flame temp, I used a propane/butane mixed gas and forced air in my burner (home made burner too).

 

now then you mention using Lead? I`ve not tried that method before, how does that one go?

 

oh and something else I forgot, before I actualy did any of this, I used some of the black mix on a tile and tried to burn it in open air in the dark and noticed the green flame, and if you have a ceramic crucible with lid, do it in there with the lid on after

[jsatan]

aha thank YT. No I didnt let it dry.

I didnt think the water would go from the phos acid.

Yeah I dont thin you would of reach the 1800c with a propane burner.

I think is working the same way as someone else came up with.

carbon (poly type) with phos acid put in a microwave, lol.

I'll set up my make shift fume hood.

Yeah your phos acid will be much more pure then mine from a quick think.

Thanks for the inof, I'll mull it around in my head for a bit,

So you didnt get any misty smoke coming off?

Headache in the making.

[YT2095]

I did get the misty smoke when I did open reactions, and when that smoke was subject to a flame it had that dull yellow green color typical of Phosphorus compounds, the "smoke" itself did not glow though, only stuck of garlic (another sign).

as for 1800c on a forced air but/prop burner, no idea at all mate, it will certainly allow you to melt borsilicate glass to a near liquid state though (as it did with my tube when I heated the stuff).

[jsatan]

yeah soft glass will melt about 900c, well melt isnt the right word, lol. as it a not a solid.

 

I was thinking aout making my self a clay pot for it.

So you didnt get a headache?

(I work with glass as a side hobby, )

[budullewraagh]

absolutely. yt, i have much respect for you. cheers!

[YT2095]

Hmmm.. it would seem I owe you all an appology of sorts.

 

I`ve atempted to re-create my experiment again, using activated charcoal and a purer Phosphoric acid in my synth (I have better stuff now).

 

it failed.

 

and so without reserve Sorry to each, there must have been some other element or contaminant that i overlooked and/or didn`t factor in.

 

but Pure Charcoal and H3PO4 does NOT work, there must be something else present in the original synth that I wasn`t aware of

 

 

given time I`ll find out was this contaminant likely was, I can think of a number of things right away, and so I`ll do my best to try and establish Which one or oneS are responsible, I only wish I knew which brand of BBQ Charcoal I bought!???

 

sorry if I wasted anyones time with this, but I`de be remiss if I DIDN`T put the record straight

[budullewraagh]

Don't give up yet!

 

Think of it- the industrial method involves SiO2 taking the cation and an O out of phosphate salts, then thermiting with carbon, so you're definitely on the right track- instead of using the SiO2 you do the same thing by removing water. How extensive were your efforts to get this to work? Theoretically the carbon should do thermite with the P2O5/P4O10. Perhaps you had too much oxygen present in your atmosphere?

[Sebbass69]

Sorry to hear it didn't work - it would be awesome if there was a way to make phosphorus in home labs...

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Just as a quick idea, if there was a polar solvent that could dissolve P2O5 and conducted electricity, you could use electrolysis to isolate the phosphorus, but I'm not sure such a solvent exists.... and water won't work, because it reacts with P2O5 -