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watson.fawkes
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Silica around alkali and
alkali earth oxides is going to form a glass and lower the melting point. It's entirely possible the the main benefit of introducing silica is to get
the reaction into liquid phase much more readily. If that's so, an easy way to get a glass going to throw in some waste glass. It's standard procedure
when doing custom melts of glass to start with some melted glass whose proportion can be modified; it gets the melt going much quicker and saves
energy cost. Seems plausible that the same principle would apply if indeed molten glass is in fact the reaction medium here.
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Rogeryermaw
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after another run with the addition of NaCl i am completely convinced that it helps reduce the viscosity of the melt. i only used about 6-7% the
weight of the reactants and i would say all P4 had finished bubbling out in about half the time as usual. as usual blogfast, your science is strong! i
did take video and several snaps which i will make available after editing.
ok the video is available for those of you i sent the link to. i'm not sure who all should get it since you tube said i can only send it to 25 people.
i need your youtube screen name to give access to the videos.
[Edited on 25-9-2010 by Rogeryermaw]
[Edited on 25-9-2010 by Rogeryermaw]
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blogfast25
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Quote: Originally posted by Rogeryermaw  | as usual blogfast, your science is strong!
i need your youtube screen name to give access to the videos.
[Edited on 25-9-2010 by Rogeryermaw]
[Edited on 25-9-2010 by Rogeryermaw] |
Thanks, Roger, but far too much praise: people like me that have messed around with thermites and other metallurgical reactions understand the
importance of melt viscosity reducers, usually CaF2. In those, 'fluxing' is usually the difference between failure and success...
But for your, lower temperature, reactions the lower melting, more readily available NaCl may just have been the ticket... Just getting a bit of melt
going may lead to the reaction starting earlier and thus also finishing earlier...
And as Watson noted earlier, the silica may also contribute...
Re. your earlier comment:
| Quote: Originally posted by Rogeryermaw | this thought just occurred to me. when word gets out that P4 can be produced this way (mostly applicable to u.s. experimenters) NaPO3 may be as hard
to get as P4.
[Edited on 24-9-2010 by Rogeryermaw] |
If the worst came to the worst, sodium metaphoshate is easily synthesised. As long as we have access to phoshate, we have access to metaphosphate and
as long as we have access to good old bones, we have access to phosphate. No worries, really!
[Edited on 26-9-2010 by blogfast25]
[Edited on 26-9-2010 by blogfast25]
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Magpie
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| Quote: Originally posted by blogfast25 |
As long as we have access to phoshate, we have access to metaphosphate and as long as we have access to good old bones, we have
access to phosphate. No worries, really!
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This brings to mind a rare but brilliant satire by garage chemist:
"Another material worth banning: Bones. Everyone who reads up on phosphorus production will find out that animal bones once were the principal raw
material for it.
No more chicken wings at burger king, only boneless steaks and chicken filet, no whole turkey, etc...
Possession of a dead animal containing bones is only legal for registered and licensed butchers, every other person will be charged with unlawful
possession of a drug precursor."
The single most important condition for a successful synthesis is good mixing - Nicodem
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blogfast25
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@Magpie:
All this could end up increasing the murder rate. I'd start an illegal 'bone export business' now, get in from the ground up, you know?
Early bird catches the bone? ;-)
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Magpie
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I'm not sure if Roger agrees with this but I have the impression that using the NaCl flux is an important breakthrough in P production home
technology. When I did my limited experimentation using Al/NaPO3/SiO2 the voluminous foam generated looked like it could be a real problem. Also,
any method for getting the reactants into a liquid state at the lowest possible temperature sounds highly advantageous.
We should remember that the key to Charles Hall's breakthrough discovery of how to electrolytically produce aluminum was his use of cryolite
(Na3AlF6), a liquid producing flux for the Al2O3 ore.
Possibly use of other fluxes in Roger's technology could prove advantageous. Specifically I'm thining of CaF2 and cryolite. CaF2 is readily
available from pottery supplies distributors. Cryolite may be available there too. Also there are other fluxes, as any good book on pottery will
show.
I would experiment with CaF2 in my ceramic tubes if I wasn't concerned that it would eat a hole right through them.
The single most important condition for a successful synthesis is good mixing - Nicodem
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Rogeryermaw
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what i have noticed about the use of NaCl as a flux is that it seems to reduce the viscosity of the melt and therefore allows the P4 vapor to escape
more easily thus reducing the necessary burn time in the furnace. cut my time in half at least.
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Magpie
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| Quote: Originally posted by Rogeryermaw | | what i have noticed about the use of NaCl as a flux is that it seems to reduce the viscosity of the melt and therefore allows the P4 vapor to escape
more easily thus reducing the necessary burn time in the furnace. cut my time in half at least. |
Yes! A viscosity reducer. That makes perfect sense. By reducing the viscosity the formation of foam is reduced, or eliminated. As, you say it also
allows the P4 to escape easier.
By eliminating the foam it should be possible for me to increase the charge size without plugging the outlet of the retort.
The single most important condition for a successful synthesis is good mixing - Nicodem
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blogfast25
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| Quote: Originally posted by Magpie |
We should remember that the key to Charles Hall's breakthrough discovery of how to electrolytically produce aluminum was his use of cryolite
(Na3AlF6), a liquid producing flux for the Al2O3 ore.
Possibly use of other fluxes in Roger's technology could prove advantageous. Specifically I'm thining of CaF2 and cryolite. CaF2 is readily
available from pottery supplies distributors. Cryolite may be available there too. Also there are other fluxes, as any good book on pottery will
show.
I would experiment with CaF2 in my ceramic tubes if I wasn't concerned that it would eat a hole right through them. |
The cryolite in Al production has a slightlly different function: the electrolyte bath is a eutectic mix of Al2O3 and Na3AlF3 with a much lower
melting point than Al2O3 (2054 C !!). Without the cryolite the Hall-Heroult process would basically have to run at above 2054 C. Now it runs at about
700 C (off the top of my head).
CaF2 (fluorite) would be no use in the phosphate reaction because it's MP is too high (about 1500 C) and it would either not really melt or not be
very low in viscosity. NaCl is probably ideal...
But it is widely used in aluminothermy ('thermite' in common language) where to allow separation between the slag (contaminated alumina) and the
molten metal you need to reach the melting point of both the metal and the slag (whichever is the highest). Adding CaF2 which melts well below the
2054 C MP of alumina much reduces the viscosity of the melt and so promotes the metal (which is insoluble in the alumina) to coalesce out and collect
in a molten puddle at the bottom of the melt. There isn't a metal that I have produced using aluminothermy (Cu, Fe, Cr, V, Mn, Ti, Nb, Si, FeTi, FeV,
FeSi) that didn't need a good dollop of CaF2 in the formulation to actually obtain valuable lump metal and not just fireworks...
[Edited on 27-9-2010 by blogfast25]
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blogfast25
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Roger, I watched the vids with great interest, thanks for putting them up.
One possible improvement, re the air flow regulation. 'On - off' works fine of course but here's a little trick I use for a very small lump charcoal
furnace which is aired with an inverted Hoover. That too blows far too much air, so I cut it down to a continuous regulator as follows. The tuyere (as
it is known in the lingo of the furnacistos) is the pipe running into the furnace, connected to the blower. I cut it about three feet away from the
entry into the furnace and fitted a funnel onto it at the end facing away from the furnace. Now I simply direct the blower onto the funnel and by
adjusting the distance between the blower outlet and the tuyere funnel I can regulate the airflow like the best up there. Simple but effective!
Finally, I'm not sure why you want to keep the vids private. P4 has no major uses in bomb making or drug making. Why not make your design available
commercially, either as blueprints or as actual pre-a-porter reactors? Land of the Free, no?
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Rogeryermaw
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as for the blower, one of these days i was planning on putting a dimmer switch in line to control the motor voltage. since it is a straight wired
motor i don't think the changes in voltage will hurt it. or i have also considered using the engines from one of my ducted fan model airplanes. i do
like your funnel idea...would be cheaper and i already have the parts to make that happen!
as to making the vids public, here in the states methamphetamine production is out of hand and one of the ways they make it is by reduction of
ephedrine by hydriotic acid produced in situ by reacting iodine with red phosphorus. that's whats holding me back from releasing this to the the
world. i do agree with you that withholding useful info is a sickening practice but i'll be damned before i will give those stinkin' meth punks
another way to ruin chemistry for the rest of us.
[Edited on 27-9-2010 by Rogeryermaw]
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Magpie
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@blogfast
I do not doubt your expertise and experience in the area of using fluxes, etc, and do realize that these minor additives may very well serve different
functions depending on the situation at hand. But I was under the impression that many fluxes used for ceramic work are successful because they lower
the melting point of both the substrate and the flux, the ultimate being a eutectic composition.
I have been reading some about glass making. One problem they have to deal with is the inclusion of gas bubbles. To eliminate this they use
fining agents to reduce the melt viscosity. This facilitates the release of the gas bubbles. Among the fining agents mentioned the most
user friendly appeared to be sodium chloride and sodium sulfate. Although I believe the sulfate could release SO2 gas in a reducing environment.
So, as you say, NaCl may be optimum for the case at hand.
@Roger
I wanted to add my twist on air flow regulation: Place a tee in your airline, using the straight section for the airflow to the furnace. On the
branch leg place a valve, ideally a globe type for finer regulation, but a ball valve would likely suffice. The airflow then is easily controlled by
how much you spill through the valve on the tee.
[Edited on 27-9-2010 by Magpie]
The single most important condition for a successful synthesis is good mixing - Nicodem
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blogfast25
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| Quote: Originally posted by Magpie | But I was under the impression that many fluxes used for ceramic work are successful because they lower the melting point of both the substrate and
the flux, the ultimate being a eutectic composition.
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Yes, that's correct. Even cryolite is occasionally used in glazes and some potters stock it.
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blogfast25
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@Roger:
That's fair dos I guess. Here in Europe we can buy powdered red P but I guess we don't have crystal meth problem, or at least not as large...
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Rogeryermaw
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i will say this though. i trust your judgment, blogfast, and you have the info to watch the vids anytime you want. you can share it with whom you see
fit. i trust your motives and don't think you will misuse it. same goes for all of you i have shared this with. i would like to see responsible home
chemists have access to P4. as Polverone put it, "Phosphorus and its compounds are invaluable reagents for a variety of laboratory procedures, and
it's also just plain nifty."
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Rogeryermaw
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| Quote: Originally posted by Magpie |
@Roger
I wanted to add my twist on air flow regulation: Place a tee in your airline, using the straight section for the airflow to the furnace. On the
branch leg place a valve, ideally a globe type for finer regulation, but a ball valve would likely suffice. The airflow then is easily controlled by
how much you spill through the valve on the tee.
[Edited on 27-9-2010 by Magpie] |
not bad Magpie! much like the wastegate on a turbocharger!
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peach
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One of the ways? It seems to be the ONLY way most of them know.  That recipe is
over a century old.
I don't mind if drugs are Hofmann's problem child, but I do mind when that child cuts the phone off harvesting the copper. If you hear a can of 9%
larger fall from about telephone pole height, that's more likely the lesser spotted, reclusive heroin addict out foraging for berries; addict slang
for scrap metal.
With all this furnace talk, have you guys read Dave Gingery's "How to build a gas fired furnace"?
I bought it when I was about 14, along with "How to build your own lathe".
The gas fired furnace one, he tells you all about making your own refractory from firebricks, clay and other things. There's a blue print for a
working out the book furnace with a removable lid, and instructions on how to make the formers and ram the refractory. As well as details, drawings
and measurements for building a centrifugal blower and some rough information on green sand casting.
The blower, you may as well buy one or scrounge one from the tip (modern combi boilers have a £100+ high heat one in the top, and the boilers end up
at the metal scrap yards; ask for 'berries' and remember to say 'berry merry munch' when the deal is done).
The furnace dimensions and details are easily changeable. If you google for anything like DIY / Furnace / Gas / Dave Gingery / Gingery you'll find
tons of pages. And there's the hobbicast group on yahoo groups.
I just thought the design could be easily manipulated to make a more permanent retort furnace.
I've read the book tons already and it's just been sat on the shelf for aaaaaaages. As a thank you for making the video and letting me watch it, you
can have my copies for free if you like Roger.
I just found my refractory bricks and an empty propane can.
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Rogeryermaw
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[rquote=188511&tid=65&author=peach
One of the ways? It seems to be the ONLY way most of them know. That recipe is
over a century old.
I don't mind if drugs are Hofmann's problem child, but I do mind when that child cuts the phone off harvesting the copper. If you hear a can of 9%
larger fall from about telephone pole height, that's more likely the lesser spotted, reclusive heroin addict out foraging for berries; addict slang
for scrap metal.
[/rquote]
man that is more real than you know. there was a trolley system in downtown that has been shut down because the wiring has been ripped out twice and
on the news(when i was working on the spawar contract building security equpiment for national guard aviation bases) in hawaii about the (i think it
was the H3 highway) new highway construction where the ice heads stole the wiring for the new lighting system along the highway...they have no
scruples at all!
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peach
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They are funny guys. And truly dedicated to recycling, sometimes before it's ever been used for the intended purpose they're that eager.
I saw two guys in Scotland at one point pulling up all the tiles in an abandoned house. The police turned up and one of them refused to be arrested or
get in the car until he'd got his sandwich and can of beer back in his hands. Then he shut up and jumped in the car. Simple folk. All for £40 and a
few more hours dribbling in a chair, numb to the world. Poor boys.
"If it's nailed down, they'll probably steal the nails as well"
[Edited on 28-9-2010 by peach]
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blogfast25
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@Roger:
Any chance of a P4 yield estimation? You know, P out divided P in x 100?
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Rogeryermaw
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well at roughly 5.1 grams of phosphorus in 102 grams of 6(NaPO3) with a return of at least 4 grams per run (since we scaled it up) it's close to 78%.
there must be losses to atmosphere etc but the return is fairly high.
on the second attempt with the scaled up design the haul looked physically larger but i did not weigh it.
[Edited on 29-9-2010 by Rogeryermaw]
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Strepta
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@Rogeryermaw:
Roger, what was the the mass (in grams) of the NaPO3 you used in the experiment which yielded 4 g of P? If you used a mole (102 grams) there would be
about 31 grams of P available.
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peach
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102 grams is 0.166 moles of the hexa phosphate (611.7g/mol). 6 phosphors in each mole, so it'd yield 0.996 moles of P.
He's yielding P4, making that 0.249 moles of that allotrope. At 123.88g/m for P4, that's 30.8g (matches with above 0.996 of P). And a yield of around
13%. Unless my 1.30am brain has gone dead on me and I've made a mistake.
13% still beats 0%, particularly for such a tricky element. Add to that, he's only just got the thing going! Extra roasting may yield more.
| Quote: | | In 1669, German alchemist Hennig Brand attempted to create the philosopher's stone from his urine, and in the process he produced a white material
that glowed in the dark. |
^^^^^^^^^^^^^^^^^^^^^^
That reminds me of when we made yogurt in Chemistry and someone astutely asked, "Why was he eating the white curd on a cow's tits in the first place?"
[Edited on 30-9-2010 by peach]
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Rogeryermaw
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wow. you are correct sir. thank you for making me check my math! i guess that actually works out to about 13%. now i have to run it again and see what
the yield turns out to be. if you look you'll see where i goofed up. i calculated for 1/6th mole of HEXA metaphosphate and translated that to 1/6th
mole of phosphorus. 1 sixth hexa is the same as 1 mole meta in this case so at 1 sixth mole times 6 atoms phosphorus per mole = 1 mole phosphorus. so
thank you for catching that! and at 4+ grams out per 31 grams in yield is roughly 13%. again as i said on the most recent attempt the yield looked to
have larger physical volume but i did not weigh since i was working on the video. so yield is not spectacular but since it yields something we can't
buy in the states any at all is better than what i started with.
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Strepta
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@Rogeryermaw:
Roger, you stated earlier that the NaCl reduced the "burn time" in your furnace by about half. How did you determine that the reaction was complete?
Are you listening for the gas bubbles in the receiver?
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