Preparation of elemental phosphorus

Direct Reduction of Phosphorus pentoxide to P4, possible?

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)?

Quote: Originally posted by Zachemophile

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

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.

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.

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]

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

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?

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.

pics

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.

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.

Well, apart from P, the products of the reaction are H2 and CO. Wouldn't those gases displace any O2 present? Also, I don't think there was any P2O5 to be seen.

If I recall correctly there was a fair amount of C left in the retort. Or at least a black slag, which should indicate that there was too much C or too little HPO3?

Anyway, I don't completely trust the starting materials, and I was more interested in finding out whether some kind of reaction would happen at all using my furnace.

I'll do a more careful test. Also, I might buy some phosphoric acid.



[Edited on 8-12-2013 by learningChem]

I found some papers (written by me), where I noted several experiments that I made in the past summer (or I intend to make).
I think that...these informations will be helpful:



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[Edited on 30.1.14 by bfesser]

I think I forgot to tell you something :
All operations involving white phosphorus should be conducted in the absence of light (especially short wavelength light) because white phosphorus can turn into red phosphorus, which is much less reactive.
...P₄ molecule is freaking annoying

[Edited on 31-1-2014 by DoctorZET]

Hmmm...I think it should also work with carbon tetrachloride/chloroform/benzene/toluene (this solvents can easily dissolve white phosphorus) but be careful with first two solvents (because, phosgene can be formed in the CO+H2 output flame).
Also you can try to collect P4 vapors in cold water, then boil the water and release the white waxy phosphorus sample into the flask. I'm not sure that it will work , unless I don't try this method yet. (there can be traces of H3PO4 and other phosphorous acids in water, but not in CS2 or other nonpolar solvents)
And yes, I did this experiment (on a small scale). I have got only 2-3 grams of phosphorus ... but my goal was not to obtain phosphorus.
Guess who was my source of phosphoric acid? >>> Answer is seven bottles of Coca-Cola.
First, I boiled all of the juice for 2 minutes (to destroy the carbonic acid), then added 30 grams of Ca (OH) 2 to precipitate calcium phosphate.
Then I added calcium phosphate in concentrated sulfuric acid, I distilled the mixture and voila! A few grams of almost pure phosphoric acid from Cola! (almost dry).
My goal was to determine experimentally how much phosphorus is in Coca-Cola.

To be sure, use acetylene instead of ethylene, but be careful! Acetylene can ignite/explode in the presence of an oxygen source (like NO2, N2O3, CuO, SnO2, PbO, H2O2 ,ClO2 ,HClO2 and, why not H3PO4 ) at that temperatures (600*C).

[Edited on 31-1-2014 by DoctorZET]

Awesome now I have a reason to get an acetylene tank! Now my welding supply company wont wonder why I only have an oxygen tank And toluene is definitely the most convenient for me, I can buy it by the gallon no problem. Cant wait to try this out!

I sure wish I had the patience and determination to want to figure out the phosphorus content of a bottle of coca cola, props for that ZET! Hope I get to see some more of those awesome sketches elsewhere on the forum too!

[Edited on 31-1-2014 by PeeWee2000]

better use calcium carbide
and there is another something:
3CuO+H3PO4+2C2H2 =(550*C)=> Cu3PO3+4CO+(7/2)H2+ [ KABOOM ],
where the 'kaboom' is the main problem...
then, the heat produced by first reaction activate this reaction:
Cu3PO3 <=(630-700*C)=> 3CuO+ P^
and the CuO is reintroduced in the process

[Edited on 31-1-2014 by DoctorZET]

[Edited on 31-1-2014 by DoctorZET]

Yeah It might not have all been fresh in my head in that last post though Luckily I'm only fantasizing right now, usually I'm pretty through with my safety though. And besides I dont actually have the money to buy an acetylene tank for a single reaction

Ok I spent 12 hours reading the topic and made some 11 pages of notes from what people were doing and thinking around there.

I noted that nobody didn't consider the Wöhler process of using electric furnace for this reaction. It certainly gives enough heat. My worry is that will the reaction mixture be conductive enough to allow current pass through. My idea is to make a tubular reactor as following:



The reactor volume would be 1-2L. To there, two tungsten electrodes with ceramic steel lined threaded plug is inserted according to picture. Also carbon rods could be used, but I've got some tungsten floating around. I would wanna test using direct microwave transformer pushing 1kW at 2000V to induce a gap width of about 10-20mm for electric arc. This way the arc wouldn't be dependent on the mixture's conductivity, but if it turns out it is well conductive once started, a voltage of 20-30V with high amperage(in scale of several dozens) should be used.

The electrodes should be inclined so the arc will initate at the bottom. A ballast of heating elements would be placed in the circuit so the fuse wont short out and the reaction energy is limited by the respectiveness of the mixture's temperature. The circuit would be fitted with power adjuster. The body of the vessel is stainless steel so it could become conductive and therefore require insulative placement.

Several reaction mixtures should be tested. First is the classic mixture of 10Al + 6 NaPO3 + 3 SiO2 ball milled. Another mixture consists of Ca3(PO4)2 + 3 SiO2 + 5 C. The heat from the arc should be more than sufficient to squeeze out what we want. No inert gas is required since at the moment of initiation, the small volume of the reactor is occupied by millimoles of reactive atmospheric gases and therefore burnt to oxides in the next second.

On the side would be the exhaust port where a steel tube is lead underneath water heated to 50-60C.

Another option consists the same reactor structure, but the heating is applied through the reactor wall, as in electric furnace or by coke bed. Steel merely holds up to 1200-1400C before becoming too soft and reactive, so it could be replaced with Al2O3+silicate or MgO refractory with proper fittings.

I'm interested in the practical scalability of this reaction, eg. could this produce WP in scale of several moles per run. In the posts regards towards too finely mixed reactants caused explosive initiation when the batch was scaled up slightly, which must be taken into consideration until bringing it up to several hundreds of grams, or even kilograms. The cost of the reaction is of another matter: if the reactants of Al and B could be substituted with carbon and SiO2, the cost and the trouble of making the reactants will decrease substantially. With the most expensive setup with fine Al and Boron, the cost and the trouble of making the reactants themselves can become a major limiting factor.

[Edited on 9-2-2014 by testimento]

Quote: Originally posted by thebean

I had an idea while I was reading this thread, but it sounds insane.

Ok Perhaps I'm just a dumb-ass. I've been following op on this +decade long thread as best I can. So far I've caught up to about 2010 or so so please understand me if I'm not up to speed on the recent posts. I eventually shall, but with such a phase lag involved it'll be a little while for me more to catch up. Perhaps a spin-off thread of sorts would be in order. I'm new here, so please fill me in for any my missing spaces as a newbie. So far the German garage chemist, blogfast, peach, Wack, and Roger have contributed so much in a "thread" that was pioneered more or less by Polverone and Bromic Acid long ago. These guys have poured heart and soul into making this fascinating substance, Phosphorus. which happens to be an element. Rather amazing how far mere scientific curiouity and perseverence will go. I've heard it before that the chemists were ahead of the physicists at the time in terms of new discoveries. Long Before the periodic table was discovered, chemists were at it discovering all sorts of things by mere good "detective work" .

About time there was a forum for chemistry like there's been for the Linux/GNU/BSD crowd forever.

Okay the facts from literature I know about Phosphorus:

Quote: from my old CRC Handbook of Chemistry and Physics, 62nd Ed 1981-1982
at. wt. 30.97376; at. no. 15; m.p.(white) 44.1 C, b.p. 280 C; sp. gr. (white) 1.82, (red) 2.20, (black) 2.25-2.69.
White P has twp modifications: alpha and beta with a transition temp of -3.8 C.
Discovered in 1669 by Brand, who prepared it from urine.
Never found free in nature, it is widely distributed in minerals.
Phosphate rock, which contains the mineral apatite, an impure tri-calcium phosphate, is an important source for the element.
Large deposits are found in U.S.S.R., in Morrocco, and in Florida, Tennessee, Utah, Idaho
etc, etc. Insoluble in water...

Yes, insoluble in ideal water, which contains no dissolved gases. Real water: O2(albeit slightly), and CO2(a lot).
An old edition of CRC, but doubt a whole much has changed...


Here's a naive thought to throw out to the crowd:
For a long time I've been reading posts about how this annoying obnoxious byproduct called phosphine is often obtained by all the prodigious attempts I've been reading here to make elemental phosphorus from crucibles at 500-100o degrees C. The thought comes to mind: can you make lemon-aid out of lemons somehow by reaction of phosphine, where P is in it's LOWEST oxidation state(P-III). and just oxidize that(perhaps in-situ somehow so you don't pass out by the fumes). with an alkene or alkyne, the simplest being ethylene or acetylene, respectively. If you get the stoichiometry and heat of reaction right, ought to get the stuff in gobs, right? Or...

Interesting that is NH3 so similar in ways on the PT dissolves in water easily while PH3 don't. If you thought PH3 is bad,
Arsine is insane: even more lethal, as gaseous, and less soluble than phosphine.
In any event, makes common sense the white form is waxy and less stable than the red form.
The P4 molecules are unlinked in white while they're somewhat polymerized in red. Question is, why does
that give it a red appearance and other difering properties such as solubility in Carbon Disulfide(if you're an organic
chemist, just about anything is soluble in CS2, but may not care since the stuff is so gross)
Perhaps it could be incorporated into some gift candle for some irritating relative
Could the paraffin "stabilize" the P like in the movies' pyro stuff

Quote: Originally posted by Polverone

Wow, don't everybody try to answer at once. Anyway, I've just found a very interesting document: US Patent 6207024 (accessible through www.uspto.gov) describes the production of elemental phosphorus from pyrolytic carbon and phosphoric acid, using microwaves to heat the reactants. The reaction takes place at much lower temperatures than the conventional arc furnace process. The problem (or problems), of course, is that the phosphorus still needs to be protected from oxidation, you need a relatively heat-resistant and microwave-transparent reaction vessel, and it's going to be tough to condense and collect the phosphorus if you're trying to come up with something using a domestic microwave oven. Microwave ovens are cheap at thrift stores, but there are still obstacles to overcome for performing this reaction at home...

Quote: Originally posted by aga

Would elemental phosphorous float or sink in Liquid aluminium (i.e. molten) ? If it sinks, the molten aluminium will protect it from Air as it cools ... https://www.youtube.com/watch?v=0uhI0NwlnL4 [Edited on 11-5-2014 by aga]

Quote: Originally posted by Polverone

Quote: Originally posted by ScienceHideout

Are you sure that that is correct, bromic acid? The delta H of AlP is negative. When we are talking about the reaction with LIQUID aluminum, the delta S is certainly negative, because we have a liquid turning into a solid (m.p.=2530 C) If both are negative, doesn't that mean that the enthalpy only drives the reaction, and the reaction is only favorable at low temperatures?

Quote: Originally posted by BromicAcid

Then how about : <s>float</s> <s>sink</s> <s>react</s> <b>distill</b>

Phosphorus.—This is obtained by heating phosphoric acid with carbon, or bone-ash or mineral phosphates with carbon and silica. In this way the phosphorus is liberated from the compound containing it, and is distilled and condensed outside the furnace. As this operation must be carried on in the absence of air, the electric furnace is particularly suitable, and has practically replaced all others.

The old method of making phosphorus consisted in heating bone-ash (calcium phosphate) with sulphuric acid, thus obtaining phosphoric acid or calcium metaphosphate. This was mixed with charcoal and heated in clay retorts, phosphorus being liberated as a vapor and condensed under water.

Bone-ash or natural calcium phosphate can be smelted directly (without the sulphuric-acid treatment) to yield phosphorus, if silica is added to combine with the lime, as well as charcoal to reduce the oxide of phosphorus, but this process could not be carried out until the introduction of the electric furnace, as the temperature required was higher than could conveniently be obtained in a retort. At the present time, bone-ash, or the minerals rock-phosphate, apatite, or wavelite, are mixed with silica and charcoal, and heated in an electric furnace, yielding phosphorus vapor, carbon monoxide and a liquid slag of calcium silicate. In some cases, however, the sulphuric acid process is still employed as a preparatory step.



A suitable electric furnace is that invented by G. C. Landis, and shown in Fig. 144. It consists of an iron box lined with vitrified bricks and having an inner lining of carbon blocks which form one electrode; the other electrode, E, being vertical. The charge of phosphate, carbon and silica is introduced by means of the hopper H and inclined tube J. The phosphorus vapor and accompanying gases pass out by the pipe O to suitable condensers, and the fused slag is tapped out below. The furnace is made gas-tight with the aid of water-seals for the cover and for the gland admitting the electrode; the latter being insulated from the furnace body at the point F. The vitrified bricks lining the furnace are laid in a nonabsorbent mortar such as a mixture of silicate of soda and powdered asbestos; this being intended to prevent absorption of the phosphorus. The carbon lining is composed of two layers of blocks, so that the inner set of blocks can be replaced, when worn away, without disturbing the outer layer. The inner tapping hole for the molten slag is plugged with a piece of wood, without any luting; an outer plug, which is luted, prevents access of air to the inner wooden plug. Two sets of tapping holes are provided so that one set can be used when the other has become worn out.

About 80 per cent. or 90 per cent. of the phosphorus in the rock is extracted by this process, and the yield has been stated as 3.3 lb. of phosphorus per horse-power day.

Managed to make a small amount of white phosphorus today i added 50 mls of 47 % rust killer to 25 grams of crushed heat bead, and heated the mix up until it was like black lumpy honey ,then put it in a s/s retort i made at work from odd and sods, i then put it in my electric forge and after 3 hours of bubbling and self igniting fumes i was left with 1 gram of white phosphorus ,great but scary stuff .

will try mono ammonium phosphate next ,did a trial run and managed to get a tiny amount of WP so looks promising.

cheers nuxy

There called triclover unions we use them in product pipelines in food and pharmacutical factorys, they can have a nitrile or viton seal and the pipe to ferrel weld is a purge weld cheers nuxy

Just tried using mono ammonium phosphate mix was 25 gm crushed heat bead 12gm map and 10 gm garden lime hoped lime would convert to ammonium carbonate and make the phosphate react better, total yield was .4 grm lost some probably .1 grm before weighing ,ph tested retort residue tested acid on ph paper. cheers nuxy



[Edited on 13-8-2014 by nux vomica]

I am now noticing that you are not using any SiO2 or boria and therefore likely not forming any insoluble residue. This would nicely solve the problem of how to clean your expensive apparatus. If you can get your yields up I think you are onto something here.

Edit: Out of curiosity I calculated the %yields for your two experiments:

1st experiment. Assumptions: charge is 50ml of 47% H3PO4 and 25g of carbon. P content = 30.6g. %yield = (1g/30.6g)x100% = 10.3%

2nd experiment. Assumption: charge is 12g H2NH4PO4, 25g of carbon, and 10g of Ca(OH)2. P content = 3.2g. %yield = (0.5g/3.2g)x100% = 15.5%

Do these results look right?

[Edited on 13-8-2014 by Magpie]

Quote: Originally posted by Magpie

1st experiment. Assumptions: charge is 50ml of 47% H3PO4 and 25g of carbon. P content = 30.6g. %yield = (1g/30.6g)x100% = 10.3%

Got the new element off ebay fitted and have changed the retort setup to try and use gravity to make the phosphorus flow out easier,
Used 30 gp heat bead mix that had been used for another batch but that batch was run until exhausted of phosphorus so there shouldn't be any map residue left in it but the lime mix was still in it so don't no how much there actually was in it, 15 grams of map in granules like sugar mixed together with spoon then welded the retort shut and turned on forge.

Run took 45 min to get first sign of phosphorus then rest was out in another 50 min got a yield of 2.25 grams works out to a 56.25 %yield would be more one big blob caut on fire on surface of water when i let the water get to hot and the end of the retort tube must of had some left where i couldnt get it with a wire scraper cos i had a nice fire burning out of the tube after i had shut down cheers nuxy




[Edited on 31-8-2014 by nux vomica]

[Edited on 31-8-2014 by nux vomica]

That's a great yield - the highest I've seen. Phosphorus is hard earned as it resists mightily its separation from oxygen. That piece of phosphorus sitting on your scale looks angry.

I knocked together a second retort today so i can run several batches in the one day, never bothered to have my own tig at home as i can always use my work tig on my own jobs at lunch time but i have to wait till I'm back at work to refill the retort now i have gone away from the triclover fittings.

Filled one retort with 15grm map and 30 grm heat bead mix, and the second one with 15 grm map and 30 grm heat bead mix plus 5 grms of garden lime interesting to see if there is differencece with the lime to no lime Other photo is a page from old book from 1920,s that has some info on phosphorus production . cheers nuxy

I find that the phosphorus was condenseing around the triclover fitting and not flowing out, a smaller tube hopefully makes the gasses flow through quicker and wont form a heat sink effect,

I thought that the lime would form ammonium carbonate but i see the heat makes the ammonia volitize out leaveing H3PO4 in the retort (took better photos of pages ).
cheers nuxy

Right the results are in but not sure how accurate they are, for the retort with lime i got 1.35 gms of phosphorus, and for no lime 1.75 grms, the no lime retort seemed to also be really reacting well as there was a lot of phosphorus being wasted and burning up in the air after passing through the water used a new element and think temp was to high measured at 945 deg c with probe, you get the same effect if you heat the outlet with a gas torch the phos seems to volatile and wont condense and just passes through the system, will play with settings when i get a chance cheers nuxy

Had three more goes for the return of 2, 2.3, 2.65 grm phosphorus used a glass tube leading into the water and found the phosphorus condensed on the glass and will run down the tube if you heated gently with a gas torch occasionally much better way to do it.

Took a pic of map and coke mix didnt crush them up but mix and seal in retort, arc welded tube at home useing 2.5 m/s rods.

Cleaned all the phosphorus up in chromic sulfuric acid mix total is 15.48 grm dont even really need that much so might see if i can turn it into red phos seems a bit more usefull and stable than the white version cheers nuxy.



[Edited on 26-9-2014 by nux vomica]

[Edited on 26-9-2014 by nux vomica]

Quote: Originally posted by j_sum1

I'm late to the discussion and haven't read the whole thread so forgive me if this has been covered before. If the purpose is to obtain a small sample for element collection (ie, volume created is not critical) then there is a straightforward method. Red Phos can be gotten by scraping matchboxes after first loosening the glue with acetone. Tedious, impure, but possible. Purifying and converting to white Phos is easy. Place a small sample of red phos in a glass tube with sealed end or a small test tube. Bung the other end with cotton wool or similar. Heat the red phosphorus in a flame until it sublimes. It will deposit on the cotton wool. Removing the bung should demonstrate self ignition in air. If you want to keep your sample then you need to use a longer glass tube. Place a cooling collar around the tube to force the phos to deposit in the location you desire. Then ampoule your sample by melting the tube on either side of the sample. You won't get more than a few milligrams this way, but if that's all you need then this method is a cinch.

Quote: Originally posted by Azane

Perhaps phosphorus trichloride could be reacted with a metal phosphide...? AlP + PCl3 --> 1/2P4 + AlCl3

this worked

Im not sure if preparation of black phosphorus crystals has been discussed but I'm very curious as to how it its created. I know extremely high pressure is applied or gas phase transport.
Please share some info or refer to one of the 48 pages of this thread

Photo from smart-elements

[Edited on 5-11-2014 by nhindori]

Monopotassium way?

Quote: Originally posted by Molecular Manipulations

You supply phosphates but think they were made from phosphorous? Common man, nobody makes phosphates from elemental phosphorous.

Quote: Originally posted by Magpie

But IIRC elemental P is used by the carbonated beverage industry for making phosphoric acid. This is likely a way to obtain the purity they require.

Quote: Originally posted by blogfast25

2 NaPO3 + SiO2 + 10/3 Al ---> Na2SiO3 + 5/3 Al2O3 + 2 P

Quote: Originally posted by Rogeryermaw

6(NaPO3) + 10Al + 3SiO2 = 3Na2SiO3 + 5Al2O3 + 6P

Quote: Originally posted by Rogeryermaw

i have done it!!!!!!!! i will post pics soon as i clean and solidify it all. they will be up tonight!!!

Quote: Originally posted by j_sum1

I am still not extremely clear on the process: in particular the reason for the NaCl and SiO2 in the reaction vessel. I think the receiving vessel has water in it, but again I am not sure. Anyway, the whole process looks reasonably accessible. I'd love some more insight if anyone has any. (Or refer me back to the sections of this thread that I have missed.)

Quote: Originally posted by Assured Fish

Does anyone know the exact temperature range at which this reaction takes place 2NaH2PO4 --> Na2H2P2O7 + H2O And also the following 3Na2H2P2O7 --> (NaPO3)6 + 3H2O I would guess its up around 700°C but the wiki doesn't specify nor can i find anywhere that does tell me. I also realize that it would be a hell of a lot easier to just buy sodium hexametaphosphate but for the sake of science it would be good to know the temp range required to undergo hydrolysis of monosodium phosphate to disodium pyrophosphate and so forth just in case sodium hexametaphosphate cannot be aquired.

Quote: Originally posted by Assured Fish

Ok so this thread is old and dead but ill post here. 169C 2NaH2PO4 -------> Na2H2P2O7

Quote: Originally posted by Assured Fish

Quote: Originally posted by Assured Fish   Does anyone know the exact temperature range at which this reaction takes place 2NaH2PO4 --> Na2H2P2O7 + H2O And also the following 3Na2H2P2O7 --> (NaPO3)6 + 3H2O I would guess its up around 700°C but the wiki doesn't specify nor can i find anywhere that does tell me. I also realize that it would be a hell of a lot easier to just buy sodium hexametaphosphate but for the sake of science it would be good to know the temp range required to undergo hydrolysis of monosodium phosphate to disodium pyrophosphate and so forth just in case sodium hexametaphosphate cannot be aquired. Ok so this thread is old and dead but ill post here. 169C 2NaH2PO4 -------> Na2H2P2O7

Hello all! I'm a new member and if it's ok with the forum I'd like to try a few different approaches to making white P4. I have a new camera coming in a few days for doing HD 1080P videos as my current one sucks. My plan is to tape the experiments then upload them to a proxied YT account. This way I can stay anonymous but also show people VIDEOS of this reaction going with many different tweaks to it.

There are mainly 4 different things I'll be doing here:

1) Using HHO (oxyhydro gas) + MAP coolant + AIR propane to test and run experiments at any temperature up to 2500C - 5000F. My HHO torch is 3 cells at 4-5 LPM (each cell) with 3, 12V-75A chargers. I finally fried a breaker a couple days ago so right now the torch is only running on 1 cell. What you see in the pic is a baby flame around 4-5LPM. Which on its own can boil & cut steel. But when everything is connected I get a surge of roughly 12-15LPM HHO on top of the MAP gas which is extraordinarily hot and cuts through 1/4" steel like butter. It really is powerful. When I change the tip to .035 the flame is at least 14+ inches. Which you'll see when I get my breaker fixed & get some advice from the electrician.

The main benefit of HHO is that the water (fuel) really does last forever. So there's no need to refill any gas tanks. The torches aren't really "cheap", but you can set up a powerful hobby torch for $150-$300 (or cheaper if you build the cells yourself). I should mention too, my goal is to use HHO just for testing. I want my final method to rely on simple air-MAP gas accessible by anyone.

2) Instead of using pure AL powder (500 mesh) I want to test a mixture of 50% AL, 20% MG, 30% C. I have a theory I'll talk about in #4.

3) When my camera gets here I'll be replacing all text & pics with video.

4) I'm going to start with a few "normal" reactions first. Then I'm going to set up a "rocket distiller". I believe one of the big problems with this reaction is the RELEASE of heat energy in the form of >>>pressure. I believe for every unit of energy that escapes in the form of pressure, that's 1 less unit the AL has to not only keep the sodium silicate and aluminum oxide molten and finishing their reactions.... but to CONTINUE & COMPLETE the process of reducing P4O10 to WP.

I believe this is a serious problem! Why? Because I've set this reaction of many times on a small scale by igniting it with either HHO or air-MAP. I notice the reaction will fire off (then I pull the heat away on purpose to see how far it goes on its own). Then when I add air-MAP the reaction starts up again. However, there is this weird threshold where the slag stops releasing WP with the air-MAP (at 1100C). I noticed when I add HHO at this point the reaction goes almost double the time. Like under it's own energy it goes for 3-5 seconds. MAP makes it go another 3-5 seconds as you see more WP liberate. But when you just keep the MAP there the reaction dies and the WP stops being liberated. When HHO is added the reaction goes off again vigorously for nearly double the length of time. Around 12-15 seconds.

My hypothesis is this:

AL - will burn up and get the reaction going as normal.
MG - will make the mix more reactive, will burn faster, hotter and create more pressure.
C - As the AL & MG are doing their thing, the C will be displaced as gas OUT of the vessel. This will conserve energy by lowering the weight of the slag and also add pressure that can be "recycled". Plus C produces cleaner WP.

I believe if this is done right, and I get the right %'s we may see some interesting things. For instance, if this goes off like a rocket there will be a very HOT & efficient afterburn. That should be capable of driving the reaction COMPLETELY to the right under it's OWN thermal energy.

My goal is to also make this reaction easier for people who don't have access to a lot of resources. For all we know, 1 tweak to the reducing powder or the way the reaction burns (making it burn like a rocket) may produce higher yields in much less time. This can also CONTROL the release of gas coming out of the distiller. And another issue is short distillers which is why I *may add a spiral distiller on my final model.

So far I've successfully ran this reaction many times but all on small scales under 5gms. Using a small retort with thin walls which I accidentally melted. I've also used tricalcium phosphate (mixed damp rid with TSP) + C + SiO2. Just to prove it works which it does but the available P4 is low, the reaction conserves no energy, my current retort can't handle the heat.... which is why I use NAPO4 now like everyone else.

Let me show some pics of things....


This is 1 cell of HHO (4+LPM) with a drip of MAP to color it blue.


This is a thick steel reducer that I cut in half. Then I realized the camera was just a big white screen so I had to let it cool (you can see the back where it snapped off)


This is my HHO torch which is semi-dismantled at the moment.


THIS is what I need feedback on. I built 2 retorts. 1 big that's not done yet and 1 small. This is my smaller one that I want to begin doing larger chargers in (25+gms).


It's crude but I'm gonna hit the back cap with MAP gas and the middle with a cooled burst of HHO. I did NOT weld the copper distiller to the steel because the threads on that adapter connect to my bigger retort (it can be reversed for larger hundred gm charges).

What I did to connect the copper pipe is put it in the reducer with a small gap around the pipe (like 2mm). Then I used a small flat screwdriver and quite a bit of AL foil to pack it in tight all around the pipe down to the bottom. After that I poured SiO2 dust all around the pipe. Then I hammered the dust down hard ass possible going in circles packing it down. Then I put another layer of foil up top and hammered that down to sandwich the SiO2 dust between 2 layers of very tightly packed foil. So basically it's like a rock of SiO2 powder crammed between the pipes that effectively seals out air. This way down the line when I'm ready to scale I just hammer/wrench out the pipe and connect it to my bigger retort then use the small retort as the distilling side.

The thing is... I'm a bit worried as to whether a "seal" like this will hold up.

I've seen the amount of smoke just a few gms produces. The first time I tried AL I did it open air in my home with no ventilation... my whole house filled up with smoke. I immediately opened all the windows and threw fans in. Then I started testing the same volume in my bathroom in a small retort. With a respirator on my face and small fan vent on the ceiling.

My "ventilation" now is a fan in the window (bathroom fan isn't powerful enough for large charges). I can't do this outside. It's too cold. Nosey neighbords, etc. So it has to be done inside. I've already heated the pipe with MAP and HHO to see how it holds up and as long as I keep enough coolant in the line the pipe stays bright orange-yellow and doesn't melt. You can also bang on it and it doesn't deform unless you turn down the MAP gas. My concern though is at higher weight the reaction itself could melt the AL. Then I'm left with just SiO2 and I'm hoping worse-case-scenario that will stop any breach of O2.

Finally, I've thought about flooding the retort with CO2 gas. As I saw someone else in this thread do that and that will allow me to test the retort with smaller amounts first. The problem is he did that around 750C in a testube. I'll be slightly under the melting point of steel (1300C?). From what I understand, CO2 gas is no longer "inert" at these temperatures. As in, the AL with burn in CO2 like oxygen inside the retort? They say not to put out MG fires with CO2 so this has to apply to AL as well, right?

Sheesh, so many things that could go wrong I think I'll just start small maybe 15gms and see how that holds up.

My end goal is to build a "quick fire rocket distiller" so safety & engineering are huge concerns here. When I switch to the rocket model I'll test very small amounts first on video. I know many on here will be concerned with clogging. But I think good engineering will stop that.

If people have thoughts or comments feel free to LMK.

Thank you!

ps. I realize this thread is extremely old. But this is the ONLY THREAD on the internet that sufficiently covers this topic. And the 1 thing this thread really lacks is videos. So even if my hypotheses are wrong at least others will get to see this done on video in detail. With me tweaking as many variables as possible till I'm hitting 80% yields both consistently & efficiently as possible... in a way that is accessible to most people (my end goal is to make this work with only air-MAP and no HHO). Wish me luck. :-)

pss. I will continue with pics only until my cam arrives.





[Edited on 9-2-2016 by BluePlanet1]