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Rogeryermaw
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red phosphorus sublimes but i believe white boils so i may have only that as an option.
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metalresearcher
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A borosilicate retort won't work above 700oC it melts like plastic. And making P requires, as you know, a LOT more. These are OK when doing
experiments not above the 500 or 600s (dull red glow).
Maybe a quartz retort might do the job but this participates in the reaction.
EDIT:
http://www.qsiquartz.com/
sells quartz labware.
[Edited on 2010-10-31 by metalresearcher]
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blogfast25
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Quote: Originally posted by metalresearcher  | A borosilicate retort won't work above 700oC it melts like plastic. And making P requires, as you know, a LOT more.
[Edited on 2010-10-31 by metalresearcher] |
We're talking about distilling the product of Roger's efforts, NOT about using glass retorts for the production of P. White P has a boiling
point of 280 C, still quite high for a dangerous substance...
Roger: for a one stage distillation your retort would be fine. And that would get rid of most of the junk...
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Rogeryermaw
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of course the main concern here would be an even temp inside the retort or the P would just reflux...wonder if this might be a good time to try that
questionable design with a free or cheap junkyard microwave. no...with the need to inject inert gas things could get to complicated to keep safe.
perhaps woelen's test tube method has more merit in this case...of course as peach pointed out, i could use the P for synthesis and distill the
products of that synthesis to obtain a purified secondary product leaving the crap behind(in theory).
i do agree that this is a very high boiling point for a dangerous substance but we're reaching the same temps here as trying to purify sulfuric acid
which can be just as scary as far as what it will do to you in the event of catastrophic failure. i would hate to have either substance on my skin.
so...face shield, elbow neoprene gloves and full body covering. with the added risk of extremely horrid fire, i think this may have to be an outdoor
venture.
perhaps i could fill a production style retort with the product and run it like a production run. there will be loss but the P would distill over like
normal only cleaner...thoughts?
[Edited on 1-11-2010 by Rogeryermaw]
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peach
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With your sublimation point in mind, I'd go for the PCl3 and distill that at 76C.
The worrying thing about distilling the raw phosphorus is the flammability, the way it interacts with the atmosphere even as a solid and the high
temperatures involved.
Both are not good to breath in, with the PCl3 being more so. But dealing with the toxicity of the latter would be easier, for me, than the risk of it
bursting into flames with the added bonus of being slightly less dangerous to breath in.
PCl3 isn't a fire hazard, at all, according to the NFPA fire diamond.
Also, you'll probably want to clean up the PCl3 anyway, which may mean another distillation at the end. So it may be easier to skip the first, go to
the PCl3 and clean that up on it's own.
[Edited on 1-11-2010 by peach]
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Rogeryermaw
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that makes sound sense. i do have enough of the product that fairly clean to give it a go on a small scale.
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Enantiomer
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Interesting idea?
I have not ready the entire thread - it's huge! And if what I'm about to suggest has already been discussed somewhere I appologize in advance.
In the very first post in this thread the guy mentions, near the end of the post, something about using aluminum or magnesium powder. I'm not
extremely knowledgeable about chemistry. Specifically, I'm not real keen on what is meant by "reducing agent" in this context - since this is what he
is referring to in this part of his post. An idea did occur to me though that I would like to put forward.
Magnesium is flammable. Anything that burns has it's own temperature that it burns at. The need for high heat is an issue with the traditional methods
of priducing phosphurs. Perhaps there is some powder (maybe magnesium powder, maybe somthing else) that is flamable and that burns at about the right
temp for the traditional ways. If this were included in the mixture and ignited one would have an interal heat source that heats in the right temp
range. This is something that could considerable simplify and speed up the process (if it worked). I can also see the possibility of a few problems
with this idea too though. Such as: what kind of gasses the thing you were using for the heat souce emit and contamnation of the final product; side
rxns with the same, etc.
Any thoughts on this?
Enantiomer
Please don't eat the roses . . .
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12AX7
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Somewhere in this thread, you'll see thermite type mixtures used, where aluminum or magnesium reduce the phosphate directly. The phosphate itself is
a fine source of oxygen, no gasses required.
Tim
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Enantiomer
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Good ol' Tim
Sweeet!! I'll have to look for that.
Enantiomer
Please don't eat the roses . . .
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blogfast25
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| Quote: Originally posted by 12AX7 | Somewhere in this thread, you'll see thermite type mixtures used, where aluminum or magnesium reduce the phosphate directly. The phosphate itself is
a fine source of oxygen, no gasses required.
Tim |
Unfortunately that didn't really work though. I tried the direct reduction of calcium orthophosphate with Al powder, lit like you would light Classic
Thermite TM but I couldn't get it to ignite...
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plante1999
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| Quote: Originally posted by blogfast25 | | Quote: Originally posted by 12AX7 | Somewhere in this thread, you'll see thermite type mixtures used, where aluminum or magnesium reduce the phosphate directly. The phosphate itself is
a fine source of oxygen, no gasses required.
Tim |
Unfortunately that didn't really work though. I tried the direct reduction of calcium orthophosphate with Al powder, lit like you would light Classic
Thermite TM but I couldn't get it to ignite... |
this type of thermite rection need extremly high temperatur to go you could try to melt the alu with the orthophosphate, liquid have very high surface
area.
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blogfast25
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| Quote: Originally posted by plante1999 | | this type of thermite rection need extremly high temperatur to go you could try to melt the alu with the orthophosphate, liquid have very high surface
area. |
I tried lighting the calcium orthophosphate ‘thermite’ with a mixture of Al/KClO3/S as ignition pill. That ignition mixture burns to well above
2,500C, if that doesn’t light it then I dunno what does. I think the dissociation temperature for Ca3(PO4)2 === > CaO + P2O5 is too high, much
higher than for metaphospates (used throughout this thread) like Calgon.
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Sedit
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I'v done it,
Well sort of but you will see why im atlest a little giddy about it.
I took something called Nu-Calgon which is something that is used in micromat systems assuming it at this point to be Sodium hexametaphosphate and
shreaded Aluminum foil in a stainless steel crucible.
I laid out a layer of Aluminum and placed the Calgon product on top. I noticed sometime back that as this substance melts that when Al or Zinc is
place in it some form of gas came out that burned green on contact with air. When the material melts it has the consistancy of melted glass and these
gas bubbles where getting trapped on cooling only to ignite when the melt was crushed. The strong garlicy smell lead me to make a melt of this and
then quench the reaction with water when the most material seemed to be trapped.
After a few minutes to cool down I started to break the cake away from the stainless steel vessle and kept it in water to see if I could dissolve all
of the Calgon and leave some residue to perform test on.
After removing the melt and placing the stainless steel vessle aside I started to get a strong garlic smell after about 20 seconds and I could see
vapors rising from the still slightly damp bowl.
I took this into a dark place and to my delight the bottom of the bowl was glowing like a firefly.
===========================================================
Thats awsome looking and I hope I can make something of it in time but right now im a bit concerned about all that garlic smell I was just around now
assured I have contacted White Phosphorus I must take a few steps back and regroup my means of performing this synthesis to ensure my safety.
Any thoughts?
If I can perform this reaction at a low enough temperature im woundering if I can trap all the formed phosphorus under a water soluble layer of melt.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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blogfast25
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| Quote: Originally posted by Sedit | I'v done it,
Well sort of but you will see why im atlest a little giddy about it.
I took something called Nu-Calgon which is something that is used in micromat systems assuming it at this point to be Sodium hexametaphosphate and
shreaded Aluminum foil in a stainless steel crucible.
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Can you describe the Nu-Calgon product better?
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Sedit
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Im attempting to do so now.
Im not 100% sure but I believe this is the MSDS of the stuff I have,
http://www.nucalgon.com/assets/MSDS/English/4243.pdf
It states that its Sodium Phosphate tribasic. So if that is to be trusted, which its not until I pull up some more information from the container then
its nothing more then Trisodium Phosphate. The reason I don't really trust that is because it list no hazard decomposition products but I have clearly
seen it turn to what appears to be Phosphorus by boiling it with a blow torch. Adding Al, Mg, Carbon or Zn have increased the production of the
flammable gas I have been seeing. I still have to figure out what temperature this reaction is taking place at as well and as soon as I get my IR
thermometer back here which will be later tonight I will check it.
I tried to make it into a retort and capture the off gas in H2O but have so far had no luck.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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blogfast25
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So Na3PO4. Yes, that would react with Al or Mg at elevated temps. to yield P4. But isolating the P is the whole art, Sedit...
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Sedit
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Isolation, esp on a small scale will be a task in itself without a doubt. I know the TSP is soluble in water so thats a start but then there will be
other contaminations to deal with.
Like I said I tryed a simple retort but can not seem to get anything to come out which strikes me as odd because it can be seen forming rapidly in an
open system yet getting anything to come out the other end seems like a no go.
On a larger scale and a good enough heat source I don't think it will be that hard to produce P4 at all but I still have some small scale test to run
before I wrap a retort made of pipe fitting in nichrome wire and jack the heat up. The who Potassium thread has got my brain scambling for means of
performing something simular in a solvent based lower temperature setting.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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S.C. Wack
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| Quote: Originally posted by Sedit | | The reason I don't really trust that is because it list no hazard decomposition products but I have clearly seen it turn to what appears to be
Phosphorus by boiling it with a blow torch. |
Well I don't think those conditions apply to the msds. Perhaps your product is not virgin pure and in fact contains something organic.
Perhaps checking the pH can aid some in identity.
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Sedit
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Im highly doubtful of organics because it looks like shattered glass. Im almost positive now that what I have is TSP but your right and a PH test
would be good, I just hope my PH tester is still working because I stuck it into to strong of an acid the other day and it started to bubble
violently. I may have to resort to PH strips.
Either way Im just excited to see elemental Phosphorus glow.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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Polverone
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Looks like glass, easily melts under torch flame, MSDS reports solution is only faintly alkaline... this is not trisodium phosphate, despite a message
to that effect later in the MSDS. It's some sort of polyphosphate/metaphospate. That's good news, actually. It's similar to what Rogeryermaw has used
with success before.
PGP Key and corresponding e-mail address
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Sedit
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That is great news, Let me look for his synthesis and ill try to repeat it word for word.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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Magpie
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Here's some more information from Nu-Calgon's website:
http://www.nucalgon.com/assets/prodlit/3-70.pdf
This is good news if it is reasonably priced and OTC.
The old consumer product Calgon ("Calgon take me away") doesn't seem to be available anymore. Most likely due to concerns about phosphate
contamination of surface waters.
The single most important condition for a successful synthesis is good mixing - Nicodem
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Sedit
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I just did a quick search since I do not know the price since its been sitting in my shop for about 5 years or more but the search shows them selling
8oz packets for 24$. This is not what I have but I believe the same product. Mine is contained in a one liter jug or so. Im pretty sure your local Ace
or plumbing shop would have it and I would not doubt Large chain stores to have something simular.
Now I must find a good source of fine Silica if I want to proceed since I have read in this thread it would increase yeilds to something I may be able
to capture.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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blogfast25
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Silica: finely ground sand (preferably desalinated and decarbonated) or dry ground silicagel (these little sachets you get with electronic appliances)
will do. Grind in a granite mortar and pestle.
Overall reaction:
12 Na3PO4 + 18 SiO2 + 20 Al === > 18 Na2SiO3 + 10 Al2O3 + 3 P4
Try heating a fine mixture of Nucalgon, silica and Al powder in a steel crucible on direct flame (Bunsen). Once reaction starts (stop heating!),
burning jets of P4 should boil off, forming P2O5 smoke. Do it in the dark (to see the phosphorescence) and outside (don’t breathe the P2O5).
That’s what happened when I used NaPO3 (Na metaphosphate – ‘old calgon’) in that set up.
For ideas in P4 isolation read this thread! Trust me, it’s the HARDEST bit!
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Jor
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I recently bought a lump (about 20 grams) of white phosphorus. It is covered with some red material. Is this red phosphorus?
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