Hi all,
First time poster, long time lurker (actually thats a lie i joined a few weeks back.)
i purchased a groundwater remediation machine that had been dropped off a forklift (literally, not a euphemism), after consuming $30 worth of grinder blades i ended up with 70kg of 'cat ox', a sud chemie product i have the msds for (<1% Pt, <1%pd, <1% propriety metal oxide, <1% propriety promoter, remainder al2o3).
After scrapping the 300kg of stainless (0.70c/kg, so sad all 314 as well) i began reading.
Many papers later, chanced upon a sth korean gem
recovery of platinum and palladium from spent petroleum catalysts by a hydromettalurgical method, panpan sun, manseung lee, (kor. J. Met. Mater), Vol 51, No 12, pp873-881
The authors (aside from being descendants of gold panners), (because his name is PanPan), focused on finding a method for recovery of the pt/pd without dissolving the alumina,......
Anyway, did about 15ish 50g trials, figured upon a method, scaled up to 1kg, ppt out the 'black powder' using Al chunks (43g), took this to gold buyer for free xrf
Black powder has pt 35.9%, pd 12.5%, fe 7.6%, Cu 28.1%, Pb 2.0%, Rh 3.6%, Zn 3.8%
So i treated another 7.5kg of catalyst, obtained a further 400g of 'black powder, i am going to assume its assay is similar.
As an organic chemist i am finding this first foray into pgms pretty relaxing, i mean unless you pour the stuff down the sink you cant destroy an element (although i have read of volatisation losses). That said, the volume of your solutions (20 liter drums labeled 'may contained pt', 'may contain pd', 'probably doesn't contain much but just in case keep') can build up very quickly. I can just see myself dragging those suckers through two house moves and procrastinating doing anything with them.
Now for the spoon feeding request. I have done some evenings of reading, but know how can be better by far, and i have none.
To purify the above 'black powder' i intend the following, but would gladly welcome any advice
Cover the powder in 20% HCl and digest @50C for an hr with stirring, i believe this will dissolve the fe, cu, pb (pbcl2 being soluble in strong Hcl solns) and Zn, filter, wash twice with boiling water, dry weigh (this is my check to ensure the correctish amount of mass has been lost).
The pt/pd/rd ppt is then dissolved in a minimum of hot A.R. (5pt hcl, 1 pt Hno3, 1 pt water??, it appears AR is different in every lab, advice?)
Evaporated on a steam bath, HCl added, thrice repeated.
Add Nh4Cl solution (what concnetration of Nh4Cl soln is best here?) until no more orangy ppt appears upon further addition, chill to 10C, filter, wash filtrate thrice (with cold clean Nh4Cl solution), dry orange powder, heat slowly in an evaporating basin to 370C (in the dining room whilst mother in law is eating), then more rapidly to 900C, testing the fumes for colour (white good, yellow, other colours bad, Pt volatilisation).
What remains should be Pt sponge, about 130g.
From above separated orangy ppt solution is passsed a slow stream of cl2 gas until no more ppt forms or the gas ceases to be adsorbed in any way. Solution chilled overnight, yellow ppt filtered washed (Nh4Cl soln again i assume), dried and heated gently as with orangy ppt above.
What remains should be about 60g of palladium sponge
The filtrate and all Nh4Cl washings from above are evaporated to dryness in an excess of Hcl, then treated with ethanol, producing some double salt of Rh/NaCl, a red powder. This powder is dried and then heated (temp here?) in a glass tube with a stream of H2, the resultant Rh metal and Nacl is washed clear of the Nacl and dried.
Comments anyone?
First time poster, long time lurker (actually thats a lie i joined a few weeks back.)
i purchased a groundwater remediation machine that had been dropped off a forklift (literally, not a euphemism), after consuming $30 worth of grinder blades i ended up with 70kg of 'cat ox', a sud chemie product i have the msds for (<1% Pt, <1%pd, <1% propriety metal oxide, <1% propriety promoter, remainder al2o3).
After scrapping the 300kg of stainless (0.70c/kg, so sad all 314 as well) i began reading.
Many papers later, chanced upon a sth korean gem
recovery of platinum and palladium from spent petroleum catalysts by a hydromettalurgical method, panpan sun, manseung lee, (kor. J. Met. Mater), Vol 51, No 12, pp873-881
The authors (aside from being descendants of gold panners), (because his name is PanPan), focused on finding a method for recovery of the pt/pd without dissolving the alumina,......
Anyway, did about 15ish 50g trials, figured upon a method, scaled up to 1kg, ppt out the 'black powder' using Al chunks (43g), took this to gold buyer for free xrf
Black powder has pt 35.9%, pd 12.5%, fe 7.6%, Cu 28.1%, Pb 2.0%, Rh 3.6%, Zn 3.8%
So i treated another 7.5kg of catalyst, obtained a further 400g of 'black powder, i am going to assume its assay is similar.
As an organic chemist i am finding this first foray into pgms pretty relaxing, i mean unless you pour the stuff down the sink you cant destroy an element (although i have read of volatisation losses). That said, the volume of your solutions (20 liter drums labeled 'may contained pt', 'may contain pd', 'probably doesn't contain much but just in case keep') can build up very quickly. I can just see myself dragging those suckers through two house moves and procrastinating doing anything with them.
Now for the spoon feeding request. I have done some evenings of reading, but know how can be better by far, and i have none.
To purify the above 'black powder' i intend the following, but would gladly welcome any advice
Cover the powder in 20% HCl and digest @50C for an hr with stirring, i believe this will dissolve the fe, cu, pb (pbcl2 being soluble in strong Hcl solns) and Zn, filter, wash twice with boiling water, dry weigh (this is my check to ensure the correctish amount of mass has been lost).
The pt/pd/rd ppt is then dissolved in a minimum of hot A.R. (5pt hcl, 1 pt Hno3, 1 pt water??, it appears AR is different in every lab, advice?)
Evaporated on a steam bath, HCl added, thrice repeated.
Add Nh4Cl solution (what concnetration of Nh4Cl soln is best here?) until no more orangy ppt appears upon further addition, chill to 10C, filter, wash filtrate thrice (with cold clean Nh4Cl solution), dry orange powder, heat slowly in an evaporating basin to 370C (in the dining room whilst mother in law is eating), then more rapidly to 900C, testing the fumes for colour (white good, yellow, other colours bad, Pt volatilisation).
What remains should be Pt sponge, about 130g.
From above separated orangy ppt solution is passsed a slow stream of cl2 gas until no more ppt forms or the gas ceases to be adsorbed in any way. Solution chilled overnight, yellow ppt filtered washed (Nh4Cl soln again i assume), dried and heated gently as with orangy ppt above.
What remains should be about 60g of palladium sponge
The filtrate and all Nh4Cl washings from above are evaporated to dryness in an excess of Hcl, then treated with ethanol, producing some double salt of Rh/NaCl, a red powder. This powder is dried and then heated (temp here?) in a glass tube with a stream of H2, the resultant Rh metal and Nacl is washed clear of the Nacl and dried.
Comments anyone?