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Author: Subject: Preparation of elemental phosphorus
Nitro-esteban
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[*] posted on 21-6-2013 at 12:58


It was just an idea... but I think its worth trying.
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Zachemophile
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[*] posted on 15-7-2013 at 10:50
Direct Reduction of Phosphorus pentoxide to P4, possible?


I would like to experiment with WP but I know the inherent difficulties of getting my hands on the stuff. Due to its use as a stand alone reducing agent in methamphetamine production it is not easily available in the modest quantity I would like. One option would be to obtain it from thermal decomp of red P, but this reagent is just as controlled for the same reasons. I have no intentions of converting cold pills to crank, but I'm sure they won't take my word for it.

As an alternative I have mulled over the idea of reducing the easily obtainable phosphorus pentoxide to condensable P4.

What dyu guys think? Id like to have a few pointers from more experienced chemist before I get started so that I don't waste my time / risk my life on procedures that won't work or will leave me severely injured.

Would LAH work as a reducing agent, or maybe Na + H2 (I think I would use amalgam rather than the pure metal)?

I'v heard carbon could work, in a kind of smelting type reaction, but I don't want to go anywhere near high temperatures when it comes to Willy Pete.

I realize the final product would contain quite a bit of oxide impurity, but I think I could get rid of most of it with a chromic acid treatment (although I've read from someone else's post that nitric would work the same or even better). Or should I condense it directly into acid solution?

Am I insane for even thinking this is possible? I've toyed with the idea of attempting the industrial kiln method of production (calcium phosphate, silicon dioxide, carbon and HIGH temperatures) but I'd rather not blow up.

Anyway just a little brain teaser for those of you that would appreciate a possibly easy way of producing WP at home or in the lab. If your advice is good I might live long enough to post my findings.

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[*] posted on 15-7-2013 at 11:03


Check out the sticky thread above.

BTW: in all likelihood: 'No heat? No phosphorus'.




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bfesser
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15-7-2013 at 11:28
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[*] posted on 15-7-2013 at 12:46


I would like to experiment with WP but I know the inherent difficulties of getting my hands on the stuff. Due to its use as a stand alone reducing agent in methamphetamine production it is not easily available in the modest quantity I would like. One option would be to obtain it from thermal decomp of red P, but this reagent is just as controlled for the same reasons. I have no intentions of converting cold pills to crank, but I'm sure they won't take my word for it.

As an alternative I have mulled over the idea of reducing easily obtainable phosphorus pentoxide to P4.

What dyu guys think? Id like to have a few pointers from more experienced chemist before I get started so that I don't waste my time / risk my life on procedures that won't work or will leave me severely injured.

Would LAH work as a reducing agent, or maybe Na + H2 (I think I would use amalgam rather than the pure metal)?

I'v heard carbon could work, in a kind of smelting type reaction, but I don't want to go anywhere near high temperatures when it comes to Willy Pete.

Am I insane for even thinking this is possible?
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[*] posted on 15-7-2013 at 12:57


Quote: Originally posted by Zachemophile  
Would LAH work as a reducing agent, or maybe Na + H2 (I think I would use amalgam rather than the pure metal)?
Wasting LiAlH<sub>4</sub> on isolating P? I don't even...

<img src="http://time2breakup.files.wordpress.com/2013/07/annoyed-facepalm-picard-l.png" width="300" />

Why don't you just read though this thread before posting strange ideas that likely won't work?

[edit]
Also, if you're going to continue saying things like "Willy Pete," we'll assume you're just a cook looking to be spoon-fed and your posts will be ignored or removed.

[Edited on 7/15/13 by bfesser]




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[*] posted on 15-7-2013 at 14:07


Quote: Originally posted by Zachemophile  

....easily obtainable phosphorus pentoxide ....


May I ask in what country (or continent) you live?




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[*] posted on 15-7-2013 at 15:07


IIRC, WP has nothing to do with metamphetamines. It's pretty useless for such things partially due to reason it's violently reactive.
It's RP together with iodine that's used to make HI in situ for various organic reactions (I think; I really never bothered to search on how to cook drugs), and while you can get small lumps of WP by thermal conversion and meticulous purification from RP, you can't really get RP from WP that easy.
In that regard, WP is less interesting to cooks, but it's also not very interesting to most k3wls as it's not something you can easily get and then force to react in a spectacular fashion without seriously jeopardizing health. It's more of a curious allotrope that glows in the dark and can make your life pretty miserable if you don't handle it with care. It's kind of like Gollum's precious. :)

But yeah, you won't get any allotrope unless you use heat, lots of it. There still isn't a process out there that is similar to the, now famous among amateurs, isolation of potassium without the whole mess.

Some things are still basically the same as when invented. Aluminium and phosphorus production, for example.

May I suggest reading at least 25% of this thread? It should not be that hard.




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[*] posted on 15-7-2013 at 15:09


I had an idea. What if we reduced sodium phosphate with zinc powder in a closed iron container over flame. This would form zinc phosphide. Cautiously remove the residue, place in an enclosed flask with sealed tubing, add hydrochloric acid, and pass the resulting PH3 gas into a solution of FeCl3. This might oxidize the phosphine to phosphorous, though I do not know. I am not sure what other reaction could happen.
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[*] posted on 15-7-2013 at 15:39


Zachemophile,

The production of Red Phosphorus, via the reduction of phosphates via LiAlH4, has been reported on......here. As I recall, there is some, but too much information in the literature about it. Anyway, reputedly, it can be done.

Quite likely, if the reduction can be performed with LiAlH4, it can also be performed with NaAlH4. If you have a Parr-type pressure reactor, NaAlH4 can be produced. (And, if required, that material can be used to produce LiAlH4.)





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[*] posted on 15-7-2013 at 21:32


I wonder... do you think it might be possible to reduce triethyl phosphate dissolved in ether with aluminum foil, by passing anhydrous HCl gas into the solution?

Afterwards, hydrolyze the ester to phosphorous acid, which might then be easier to further reduce than the phosphate. Woelen remarked something about this in another thread:
Quote: Originally posted by woelen  
Indeed, the highest oxidation state salts and acids usually are much less reactive than the salts (and acids) of lower oxidation states:
- nitrite is more reactive than nitrate
- sulfite is more reactive than sulfate
- chlorate is much more reactive than perchlorate
- bromate is more reactive than perbromate
- phosphite is more reactive than phosphate, although the difference is less than with the other examples above.

As an example, nitrite can act as either an oxidizing agent or reducing agent, it is fairly reactive. Sulfur dioxide typically acts as a reducing agent, but can readily oxidize H2S.

I wonder if it might be easier to reduce phosphite also.

[Edited on 16-7-2013 by AndersHoveland]
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Nitro-esteban
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[*] posted on 26-8-2013 at 13:07


Perhaps phosphorus can be obtained from malathion.
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[*] posted on 28-9-2013 at 17:29


For all the chit-chat, it doesn't seem to be impossible to perform the industrial process in small scale:


2 Ca3(PO4)2 + 6 SiO2 + 10 C → 6CaSiO3 + 10 CO + P4

700g Calcium phosphate + 360g silicon dioxide + 120g carbon → 30 grams of phosphorus

Oh dear, heating a kilogram buttload of waste soil up to 1500C all only just for a neatly 30 grams of white waxy accumulant? Bring that all way up to 100 kilograms for getting only 3kg out? Aww f*....

Another source cites using microwave at 540C - possibly manageable with conventional heating too:

1 4H3PO4 + 16C → 6H2 + 16CO + P4

98g phosphoric acid + 192g carbon → 30 grams of phosphorus

I remember seeing a 25-liter trunk of decent quality phosphoric acid in some sort of cleansing ware shop so whenever I'd have a need for some phosphorus, I might give it a shot and let you know.

[Edited on 29-9-2013 by testimento]
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[*] posted on 30-9-2013 at 16:11


Quote: Originally posted by testimento  
For all the chit-chat, it doesn't seem to be impossible to perform the industrial process in small scale:


2 Ca3(PO4)2 + 6 SiO2 + 10 C → 6CaSiO3 + 10 CO + P4

700g Calcium phosphate + 360g silicon dioxide + 120g carbon → 30 grams of phosphorus

Oh dear, heating a kilogram buttload of waste soil up to 1500C all only just for a neatly 30 grams of white waxy accumulant? Bring that all way up to 100 kilograms for getting only 3kg out? Aww f*....

Another source cites using microwave at 540C - possibly manageable with conventional heating too:

1 4H3PO4 + 16C → 6H2 + 16CO + P4

98g phosphoric acid + 192g carbon → 30 grams of phosphorus

I remember seeing a 25-liter trunk of decent quality phosphoric acid in some sort of cleansing ware shop so whenever I'd have a need for some phosphorus, I might give it a shot and let you know.

[Edited on 29-9-2013 by testimento]


In case the carbon isn't quite enough to bring the reaction up to the desired heat, one could always use silicon carbide powder from a rock shop.

The only problem I can see is the CO - what on earth would you do to get rid of that? Leave oxygen in the reactor to turn it into relatively harmless CO2?
Also, could I request that source?

[Edited on 1-10-2013 by elementcollector1]




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[*] posted on 30-9-2013 at 17:22


CO would pass the condenser, at which point it could be flared off (along with any pesky P4 / PHx fumes), or just vented.

CO burns easily in air, sustaining a dim blue flame.

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[*] posted on 30-9-2013 at 17:32


Quote: Originally posted by testimento  


2 Ca3(PO4)2 + 6 SiO2 + 10 C → 6CaSiO3 + 10 CO + P4

700g Calcium phosphate + 360g silicon dioxide + 120g carbon → 30 grams of phosphorus



What if you used sodium hexametaphosphate (empirical NaPO3)?

4 NaPO3 + 2 SiO2 + 10 C → Na2SiO3 + 10 CO + P4

408 g NaPO3 + 120 g silicon dioxide + 120 g carbon → 30 grams phosphorus

As to the CO, can't you absorb it in concentrated NaOH solution to get sodium formate?

[Edited on 1-10-2013 by Cheddite Cheese]

[Edited on 1-10-2013 by Cheddite Cheese]




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[*] posted on 1-10-2013 at 20:23


According to Mellor, phosphoric acid is reduced with carbon in fireclay retorts "heated to redness".

What temperature would that be in celcius?

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[*] posted on 2-10-2013 at 06:43


Around 700-800C (think MP of aluminum).

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[*] posted on 5-10-2013 at 12:00


I have some yellow phosphorus for sale if any one is interested.



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[*] posted on 9-10-2013 at 14:09


Quote: Originally posted by elementcollector1  
The only problem I can see is the CO - what on earth would you do to get rid of that? Leave oxygen in the reactor to turn it into relatively harmless CO2?
Also, could I request that source?


Presuming the CO won't react the gas phase / solidified phosphorus, it will be bubbled out of the reaction through the water trap, and it can be vented via tube outside, ejected via exhaust fan or directed into a separate burner air intake to be burned.

I remember this was actually cited in this very topic in some form of patent which dictated that reaction scale.

https://en.wikipedia.org/wiki/Black-body_radiation
http://911research.wtc7.net/cache/wtc/analysis/fires/metcolo...
http://physics.info/color/ (this one has excellent chart)

The black-body radiation is explained in this article, including the temperature color indicators. It seems to be the most common method of showing up the temperature chart since few people have access to high-temp thermoprobes, allowing them to actually measure the reaction temps anything in excess of 350C where conventional mercury thermometers compete.

[Edited on 9-10-2013 by testimento]
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[*] posted on 3-11-2013 at 20:34
reduction of metaphosphoric acid


I used a ceramic retort loaded with some 2 grams of metaphosphoric acid and carbon (burnt flour). There's phosphorous coating the glass tube but the yield was almost nothing.



p.jpg - 140kB
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[*] posted on 3-11-2013 at 20:40


pics

p2.jpg - 209kB p3.jpg - 93kB
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[*] posted on 16-11-2013 at 10:00


A simple way to obtain a SAMPLE of white phosphorus is by scraping out the (impure) mixture of red phosphorus from the sides of matchboxes (or if you can obtain pure red P4 just as good). Now put the red P4 in a testube whose mouth has been firmly sealed with a piece of cotton. Take this apparatus and heat lightly for a few moments until you see a white-yellow substance condensing on the cotton. Voila, white phosphorus.

;)
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[*] posted on 26-11-2013 at 00:51


Please post useful info or do not post at all. Your last post about boiling piss does not add anything to this thread, it just derails it and makes you look like a k3wl.



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[*] posted on 5-12-2013 at 13:36


Quote: Originally posted by learningChem  
I used a ceramic retort loaded with some 2 grams of metaphosphoric acid and carbon (burnt flour). There's phosphorous coating the glass tube but the yield was almost nothing.



You know, looking at this I'm tempted to see what happens if you scale it up. The setup is fine, but the yield is, as stated, very low. The maximum possible yield of phosphorus from a mixture of (assuming) 1.3g H3PO4 and 0.7g C would be about 0.41g phosphorus, and because you didn't use vacuum or inert gas, your yield is likely much lower than that. So, if you scale it up to 50g phosphoric acid and 25g carbon, and assume a yield of 10% (a reasonable, if low assumption IMO), your expected yield would be 1.6g of phosphorus.




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[*] posted on 6-12-2013 at 18:21


What was the heat of your reaction.
Also would this be a viable route (it seems to simple)
PH3+3NH3==>(NH4)P
and then decompose the ammonium phosphide (I cant find if it does decompose, but it seems likely)




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