Recovering silver and palladium from MLCC:s

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joubjonn said:
Hey Necro,

Can you post your method when you finish? I would be interested since I have about a kg of MLCC's myself I would like to process. What's your plan with the Pd once you get it?
Click to expand...

Pd will be dried & stored, i dont have a good torch. unless someone close by wants to melt it for me ??? (Hint Hint)
 
necromancer said:
nevermind, this "is" Goran's post :oops:
Click to expand...
No, it's Noxx forum... and I have followed your posts with great interest. 8)

I'm sitting with a mess on my own that I created last summer. It looked good but I didn't let it sit in HCl as long as the first batch and when I added NaCl to it it turned into a thick mud with an unknown content. It probably is a mix of tin, palladium, lead, silver and copper in various oxidation stages and complexes with chloride and nitrate.
I tried to add a copper rod to cement palladium (the silver is in silver chloride form) and it somewhat worked, I got a palladium mirror on the surface and some branching palladium crystals on the rod after a couple of months. The mud changed color to white close to the rod (palladium chloride and nitrate cementing, depleting the mud), but the thick mud hindered circulation of the liquid so it was less than successful. The mud also locked in a lot of the cemented palladium metal particles.

Next idea I got was to treat it with NaOH to turn the silver chloride into silver oxide... and that is the stage it's in today. When I go on vacation I'm going to pick this experiment up and see what I can do to separate the metals. I also have another batch of MLCC:s that I'm going to process this summer. I guess I'm going to try the AR first to extract palladium and treat the left overs for the silver content.

As you see, it might be foolish to follow my advice on MLCC:s at this time... do it at your own peril! :mrgreen:

Göran
 
I could be wrong here,
But doesn't hokes say to use ammonium chloride for pgm's?
I understand the cl would conflict with ag in solution.
But it would be alot easier then using zinc to cement :)

Recently started collecying these, going back over 400 lbs (yes, 400) to scrape these small gems off.
I'll try a batch with smb and post my results and yeilds as well.
 
bgp_scrap said:
I could be wrong here,
But doesn't hokes say to use ammonium chloride for pgm's?
I understand the cl would conflict with ag in solution.
But it would be alot easier then using zinc to cement :)
Click to expand...

Hoke : Page 108 said:
If your palladium is pure, and if your standard solution was prepared
as directed, nothing will happen. This experiment shows
that palladium differs from platinum in that it is not precipitated
with ammonium chloride from an aqua regia solution from which
excess nitric acid has been boiled off.
Warm the mixture gently, and add a single crystal of sodium
chlorate. Or, dissolve a pennyweight of chlorate in a little warm
water, and add a drop at a time. There will be considerable fizzing,
and as it subsides, add another small crystal or another drop. The
solution should be just short of boiling. After the addition of a little
more of the chlorate, a change in color will be noted. Stir the
mixture with a glass stirring rod; soon a dark red precipitate will be
seen, floating on the surface and then sinking. Continue to add
chlorate, a little at a time until the liquid is almost colorless, and
then let cool. This red powder is palladium ammonium chloride chemically
much like the orange powder above.
Click to expand...

To me it was easier to use zinc to get all PGM:s in one go and collect the black powder until I have enough to warrant a separation and refining of the different metals. Even though the MLCC:s probably contained mostly palladium it was easier to add it together with other batches with other PGM:s. Some time in the future I'll refine it.

Göran
 
Goran, I have used your method twice, once with surface mount resistors and once with MLCC's. I have achieved good results ending up with a palladium nitrate solution. The only thing I did different was that I heated the HCL after soaking in room temperature HCL for two weeks. As soon as I heated it the reaction started again. I think it would be very hard to gage when all base metals have been removed without heating. Can hot HCL dissolve some palladium ? I thought HCL could only dissolve palladium if it is finely divided.
 
Rocky888 said:
Can hot HCL dissolve some palladium ? I thought HCL could only dissolve palladium if it is finely divided.
Click to expand...
It will readily dissolve oxidized palladium.

Harold
 
Harold,

Could the mlcc s first be boiled in hcl to remove tin and lead. Then crushed and roasted to convert the palladium to a oxide? Then you could leach the pd out and go after the silver with nitric once you expelled the free hcl? Or would the palladium require to high a tempeture to oxidize?

Regards
 
lunker said:
Harold,

Could the mlcc s first be boiled in hcl to remove tin and lead. Then crushed and roasted to convert the palladium to a oxide? Then you could leach the pd out and go after the silver with nitric once you expelled the free hcl? Or would the palladium require to high a tempeture to oxidize?

Regards
Click to expand...
I'm probably the wrong person to ask, although it would be my opinion that what you proposed wouldn't work well. If the palladium was sponge, with a lot of surface area, yeah, it might work, but solid pieces would experience only surface oxidation, so the process wouldn't really solve the issue.

Harold
 
So un-oxidized palladium will not be dissolved in hot HCl but will dissolve in very dilute AP (HCl + air bubbler)?
How much does palladium oxidase in H2O (from dilute acids)? I suppose it should not be much?
 
I believe that Pd is in form of paste sandwiched in a layers in them so it may be dissolved easier than if it would be like solid pellet or something like that.
 
Yes, it is, but i don't want it to dissolve. I'm depopulating RAM in HCl with air bubbler and i want MLCC to just fall of with chips so i don't need to extract small amount of Pd from large volume of solution rather accumulate them for future separate extraction of Pd.
If that is not possible I'm planning to do as Geo suggested with addition of grinding MLCC with gold flakes, then dissolve Pd in nitric, wash, filter, dissolve gold in AR or HCl/Cl....
Then I'll have concentrated solution of Pd and Au and poor solution of Pd with base metals. From that poor solution Pd would be extracted with Zn or just left for stock pot till I learn how to deal with it before disposal?
 
I think you are over thinking the amount of Pd in there. What you will have is a small amount of Pd mixed with gold and it will be a pain to remove. You are talking about a minuscule amount of Pd for this much work. You would be better served to remove the MLCCs before you put them in the AP.

Eric
 
I know it would be better but there is about 4lbs of memory so it would be a While to remove MLCC with flat screwdriver. More because i plan to process much more than 4lbs in the future so i must find faster method. Yes it is a small amount of Pd but it must be removed because of gold purity and when I already need to remove it I can try to collect it :)
 
Use heat gun, it takes about 15 seconds to heat stick and bang everything off. Much faster and efficient than using buckets of HCl.
 
If I understand this correctly, palladium will not dissolve in hot HCL unless it is finely divided or oxidized and it won't oxidize until it hits 800 degrees celcius. So what is palladium paste made from? Is it made from oxidized or finely divided palladium? When I processed some MLCC's I tested my base metal leach HCL with DMG and didn't find any palladium, but is that even a valid test when lots of base metals are present? Just wondering if I am losing any palladium before I process a larger batch. Any answers to my questions would be greatly appreciated.
 
Patnor, how hot can your heat gun get. Mine goes to about 520 C and it takes more like 25s for one side and few more for other side of ram stick.
 
Have no clue but I was using cheap lidl one and it was not good enough so then I bought more expensive one from hardware store and it is much better. I hold them really close and all it take is few seconds to solder soften, then nice bang on side of bucket and things are flying off. I was using hotplate and sand too and it was fast too, I started to lay them inside pan and by the time I lay last one first was teary to go, so I was constantly removing and putting them in and out.
 

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