Neo-6
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Possible convenient way of making phosphates and h2o2 OTC
I'm the type of guy who cant just walk thru local market's cleaning products section without checking all the labels and now i have collected some
potentially usefull info:
Dishwashing powders usually contain
5-30 % oxygen based bleaching agents
15-50 % phosphates
~5 % nonionic surface active tensides and enzymes
+ unreported amount just informed as 'some'
TAED, Some sodium silicates,sulfates and carbonates
So my first step is to do some research and wikipedia has good info, quoted from wikipedia article 'bleach'
''"oxygen bleach", which contains hydrogen peroxide or a peroxide-releasing compound such as sodium perborate, sodium
percarbonate, sodium persulfate, sodium perphosphate, or urea peroxide together with catalysts and activators, e.g.
tetraacetylethylenediamine and/or sodium nonanoyloxybenzenesulfonate. To bleach something is to apply bleach, sometimes as a preliminary step in the
process of dyeing. ''
So as my washing agent is solid and has TAED written on the box i assume it has per-compounds and TAED is the compound for breaking those down
forming h2o2.I also tried making soution of the powder using water in 2:1 solutions and the liquid makes the fizzing sound for long time.
So at this point i know i have source for phosphates and h2o2 that is cheap, easy to buy in bulk and available practicly everywhere all i need now is good way to isolate those compounds.
My process
First i make 1:3 solution of my powder and water and stirr it for a while.Small amount is left undissolved, and i fractionated that with a coffee
filter (witch last for about 7 minutes without breaking, i suppose this is due to ph, enzymes and other chemicals)
I try the solubility of the matter in coffee filter and notice it to be practically insoluble, white and mechanically tough.I just put that stuff in
jar to wait.
As this point i assume i have solution of phosphates and h2o2 and sodium sulphate and carbonate.I tested the ph of liquid(>10) witch isn't
supprise, but i just have excess ph paper.
As for isolating the h2o2 i see from wikipedia it has boiling point of 150 celsius.Also i see it's soluble in ether but i have precautions of mixing
strong oxidant with extremely flammable organic solvents
I'm open to suggestions
If h2o2 will decompose fully during distillation i would still be left with phosphates.Also i notice when solution is hot, it's clear and easy to
filter.When the solution is cooled it's no longer clear and it's becomes gel like.When reheated the liquid becomes clear again and has snow flake like
precapitate in it.Calcium phosphate maybe?
I'm going to retry this experiment and take pictures.Any suggestions or comments?
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entropy51
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| Quote: | | Any suggestions or comments? |
I don't know where you're located, but in many areas you can buy 30% H2O2, trisodium phosphate and phosphate-containing fertilizers at the hardware
stores.
You might want to do a little research regarding the distillation of H2O2.
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Neo-6
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Actually the phosphate isn't my primarily in my intrest, it's just comes as a byproduct witch i'd probably just make orthophosphoric acid of.But i
checked, as i live in rural area it could be bought in bulk very cheap.Actually the website also has ammonium nitrate 1000kg for 180 €, quite a new
year special
As for distilling the H2O2, thanks, it might not be so good idea.
I checked the solubilities of calcium phosphates and i strated thinking that technically it would be wise to use phosphate with low solubility,
because it would provide constant flow of it, rather than dissolving quickly.That would mean i could get decent quality hydrogen peroxide just by
dissolving dishwashing powder on water...
Buying it of course intrests me but the problem with that is i can find low concentrations of few percentages in pharmacies to be used as
disinfectants.Also buying it from pharmacies would be very expensive.I suppose they could order it for me as 30 %, but i would not want to give my
name, address and phone number...
I live in Finland, and here home chemistry isn't very acceptable socially...
[Edited on 28-10-2009 by Neo-6]
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entropy51
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| Quote: | | That would mean i could get decent quality hydrogen peroxide just by dissolving dishwashing powder on water... |
Well, it might make decent quality dishwater. | Quote: | | I suppose they could order it for me as 30 %, but i would not want to give my name, address and phone number... |
Well, just to take the first Google hit, they do sell wood bleach in Finland. One of those bottles is NaOH solution, the other bottle is H2O2, probably 30% or so. I don't know about Finland, but in
the US (where home chemistry isn't very acceptable either), the only thing you need to give them is some cash and you can take some really decent H2O2
home.
There's a thread on this forum about making H3PO4 from fertilizer type phosphates.
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aonomus
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Distilling H2O2 isn't the greatest idea because of the chance of a runaway decomposition right?
I heard that you can concentrate H2O2 by slowly freezing it so that water freezes but H2O2 doesn't, and slowly increases in concentration...
As for phosphates, can you not take trisodium phosphate with conc. HCl and distill off H3PO4?
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DJF90
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Distil H3PO4? Not likely. It'll condense to give you other phosphoric acids (di, tri, meta and even poly...) polyphosphoric acid is a useful dessicant
with similar dehydrating properties to P2O5, although not quite as strong.
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entropy51
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You can make H3PO4 by distilling H2SO4 with phosphates. There's a thread here in which Magpie relates his successful preparation.
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aonomus
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Thread located here: http://www.sciencemadness.org/talk/viewthread.php?tid=2923&a...
My only thoughts are, what about substituting the (Ca)3(PO4)2 with Na3PO4? does the solubility of CaSO4 vs NaSO4 play a role in the distillation?
Magpie also mentions that he made a dilute solution of phosphoric acid and concentrated via vacuum distillation, presumably because the
resulting salts are quite insoluble and might make a mess of things that won't allow full mixing?
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entropy51
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Looks like I was wrong: apparently Magpie distilled off the H2O under vacuum to concentrate his acid, if I understand that thread correctly.
I think the Ca salt was used because the insoluble sulfate can be filtered off if the chemistry gods are agreeable, but as Magpie described it's
messy. Otherwise you have the soluble Na2SO4 in the product, and DJF90 is correct about not being able to distill the H3PO4 off.
Maybe OT, but I've seen products in the hardware store that contain H3PO4. I've never tried them since I have H3PO4, but might be viable for those
who don't.This cleaner is listed as 37% H3PO4 with no other ingredients. Might the rest be H2O?
[Edited on 11-11-2009 by entropy51]
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aonomus
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[edit]
So it occurs to me that any excess sulfate that doesn't precipitate out as calcium sulfate, will just distill as sulfuric acid along with the water...
Also from the looks of it, this method seems to be an ok way of preparing phosphoric acid so long as you get the dilute phosphoric acid, and you have
a cheap source of sulfuric acid that is clean enough. Bone ash (Ca3(PO4)2) is cheap on ebay, and would be an easy route, now I want to try this
myself...
[/edit]
[Second edit]
It just occured to me that you'd be forming plaster of paris, so you would want to work quickly to filter off the dilute phosphoric acid before the
plaster sets.
[/edit]
Some 'pH down' phosphoric acids are mixed with a dye and some citric acid sometimes. Apparently solvent extraction is an option when trying to remove
the dye, but I'm not sure about the citric acid's solubility.
Also, hydroponics stores can sell 35% H2O2, but I'm worried that it might be mixed in with some other stuff...
Then again, what can be stable under 35% H2O2 and not catalyze decomposition or get bleached itself?
[Edited on 11-11-2009 by aonomus]
[Edited on 11-11-2009 by aonomus]
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Formatik
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Quote: Originally posted by entropy51  | | Maybe OT, but I've seen products in the hardware store that contain H3PO4. I've never tried them since I have H3PO4, but might be viable for those
who don't.This cleaner is listed as 37% H3PO4 with no other ingredients. Might the rest be H2O? |
If it's colorless that could tell you. H3PO4 cleaners tend to have impurities like dyes and even odorants added to them.
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