Sciencemadness Discussion Board - phosphate polymer

phosphate polymer

Magpie - 2-2-2013 at 17:43

A byproduct of the production of HI(aq) using the method of Argox (Rhodium archive) is a phosphate polymer. Using his method I have produced this polymer as shown in the picture below. Argox says that it is insoluble in water and non-polar solvents. I don't have any reason to not believe this but I'm hoping that someone here can suggest a successful solvent. I really would like to recover my 100mL flask. Thanks in advance.

Vargouille - 2-2-2013 at 18:15

Well, he says that mechanical action is required, but you might be able to solvate some of it by using hot 38-50% sulfuric acid.

DraconicAcid - 4-2-2013 at 12:03

Strong base should hydrolyze/depolymerize the phosphates.

kristofvagyok - 4-2-2013 at 12:31

Potassium hydroxide in isopropyl alcohol for one night? We clean almost everything with that mixture and it usually works(:

Magpie - 7-2-2013 at 13:53

Quote: Originally posted by kristofvagyok

Potassium hydroxide in isopropyl alcohol for one night? We clean almost everything with that mixture and it usually works(:

This is working and has turned the top 6mm into a liquid gel! For the first 2 days it appeared to do nothing but now today there is clearly degradation of the polymer. I used a 20% KOH in IPA solution.

Thanks to everyone who gave suggestions. I was going to try them all. I just picked kristo's first.

elementcollector1 - 7-2-2013 at 17:18

Try heating to speed things up?

BromicAcid - 7-2-2013 at 19:24

KOH / IPA for two days, of course it's coming off. You just removed the layer of glass around it

In terms of mechanical action give this a go, fill flask 1/2 full of methanol, add some rock salt, swirl and shake the crap out of it. This can work surprisingly well and is easy enough to try. So long as the salt is largely insoluble you can pick your solvent of choice.

Magpie - 7-2-2013 at 20:18

Quote: Originally posted by elementcollector1

Try heating to speed things up?

Heating might well speed things up, especially as it is sitting in my cold garage. But it is making good progress and I'm not in a hurry.

Magpie - 8-2-2013 at 18:35

Victory was prematurely declared.

It seems the gel was just precipitated KOH. Back to the drawing board.

Organikum - 9-2-2013 at 05:59

For speeding up hydrolysis of the polyphosphates - and thats the stuff what else might it be?- you need acidic conditions so the base treatment will have actually hardened the polymer (and eaten some glass). Give it heat an acid and lots of time. And there is no risk you loose your flask to the cure....

/ORG

unionised - 10-2-2013 at 03:55

Quote: Originally posted by Magpie

Quote: Originally posted by kristofvagyok

Potassium hydroxide in isopropyl alcohol for one night? We clean almost everything with that mixture and it usually works(:

Why use IPA rather than water?

Magpie - 15-2-2013 at 11:25

Quote: Originally posted by Vargouille

Well, he says that mechanical action is required, but you might be able to solvate some of it by using hot 38-50% sulfuric acid.

Quote: Originally posted by Organikum

For speeding up hydrolysis of the polyphosphates - and thats the stuff what else might it be?- you need acidic conditions so the base treatment will have actually hardened the polymer (and eaten some glass). Give it heat an acid and lots of time. And there is no risk you loose your flask to the cure....

Yes! Here's the results after a few hours heating with con sulfuric acid:

I even recovered an iodine colored working stir bar, which BTW was completely worthless in this application.