Reusing HCL/CL

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midaselm

Active member
Joined
Jan 24, 2013
Messages
26
HI All,

I think I may have messed up and would greatly appreciate any input from anyone who may have done similar or can lead me in the right direction.

I processed 6 catalytic converters over 2 initial attempts ( using 2 x 5 litre buckets )and recovered some black powers after much filtering . I had used zinc shavings and could not get the powder to settle so had to try filter it out , which took ages, but I managed to recover some black powder . I kept the waste liquid ( which was still dark cloudy from suspended PGM's) and left in a 5 gallon bucket for a week or two. When i returned the liquid had settled nicely (better than expected ) but had regained an orange/red colour (indicating that PGMS are being re-dissolved into solution ). I siphoned off the liquid into another bucket and collected the black powder that had settled .

I have read many posts on this site over past year or so , and, remembered reading that the acids can be reused ( but now think that may have been referring to AP method not hcl/cl ). So since I had 10 liters of stock pot already, i decided to make a second pass on the first cats, using the stock pot liquid which i split between three 5 litre buckets, adding more HCL and CL to bring down Ph levels and to each i added 2 second pass honeycombs . I didn't get much colour change in the liquid and presumed I recovered most PGM on the first pass. So I added fresh catalytic converters to each leech and kept adding CL over a week or two.

The leech is not really looking like its absorbing the PGMs ( not getting any redder in colour ). Testing with stannous, shows a dark green colour on q-tip which I think indicates palladium, but when tested on spot plate looks almost blue / black , but no sign of any red tint for Pt. Litmus paper test shows ph 1 .

Now I have 3 theories on whats happening , i) That the pgm's are being dissolved but are dropping out immediately because there is zinc already in the solution.
ii) The acid is dead / almost dead and can only barley get the palladium into solution and not the Pt/Rh.
iii) Everything is perfect:)

If its(i) that the PGM are dropping immediately . I'm thinking i need to Filter out the liquid and keep the filtrate which will be carbon,and PGMs and maybe redissolve in fresh HCL/Cl and attempt again.

or

If its (ii) dead acid. I will need to try drop whatever palladium / PGM's that are in solution now and dispose of waste ( after settling , siphoning and stannous testing and neutralization ), and use new HCL/CL leech on these converters .

or
If its iii) everything is ok . happy days !

I have attached a few pics of the stannous test using a spot plate , and q-tips . The pic shows samples of the three leeches , I added stannous to the spot plate and q-tips for each bucket, and left the other leach samples without stannous to have comparison beside .

Sorry about the long post and thanks in advance for any input or advice.

Ken
 

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At least it not i), to drop PGM:s with zinc is a replacement reaction, metallic zinc goes into solution while dissolved PGM:s becomes metallic and drops. As you have both filtered it and added more acid there should not be any more metallic zinc in the solution.

My gut feeling is that it probably is ii), but I have no experience with catalytic converters so don't take that as a trustworthy statement.

Göran
 
Sounds like you are on the right track to me.

Testing for Pt when Pd is present makes it very difficult to determine which is present, or if both are for that matter. The proper testing avenue is to remove the Pd first with DMG, then test the filtered solution with stannous chloride for Pt.

Finely divided Palladium will redissolve in acid. Precipitation with zinc requires the solution to be filtered shortly after precipitation to avoid the blacks from redissolving. The fact that the zinc precipitated blacks are redissolving indicates to me that your acid is still active, either keep using the acid for leaching, or use soda ash to adjust the pH to remove the excess acid before adding zinc.

Steve
 
In Hokes book she recommends removing the metal powders soon after it is cemented using zinc, if left sitting the metal will redissolve back into solution.
 
Cheers for the input Goran, im just getting started myself and all info helps . I was verging on thinking that the acid may be getting weak too but since Ive added a little bit more hcl cl it seems to be getting there now ....

Thanks Steve for more helpful advice yet again ! i think maybe because I didn't test on a spot plate last time that the reaction confused me this time, it actually goes red first but very quickly changes dark . I think the last batch i did tested on a swab turned a red colour and then only slightly darkened keeping a red , not near a much as this time , so im hoping my first batch was full of Pt !

Thanks Butcher , hoke is actually a fantastic read , very well written. Heres one to take a look at it any one has an elsevier or scribed account ( which i dont ), looks interesting and kinda recent . might be of some interest to someone .

http://www.elsevier.com/books/handbook-of-spent-hydroprocessing-catalysts/marafi/978-0-444-53556-6#
http://www.scribd.com/doc/78366895/Handbook-of-Spent-Hydro-Processing-Catalysts-Regeneration-Rejuvenation-Reclamation-Environment-and-Safety

Thanks again all ,
K
 
midaselm said:
Heres one to take a look at it any one has an elsevier or scribed account ( which i dont ), looks interesting and kinda recent . might be of some interest to someone .

http://www.elsevier.com/books/handbook-of-spent-hydroprocessing-catalysts/marafi/978-0-444-53556-6#
http://www.scribd.com/doc/78366895/Handbook-of-Spent-Hydro-Processing-Catalysts-Regeneration-Rejuvenation-Reclamation-Environment-and-Safety

Thanks again all ,
K
 

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  • 78366895-Handbook-of-Spent-Hydro-Processing-Catalysts-Regeneration-Rejuvenation-Reclamation-En...pdf
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Just thought id follow up and post some pics of the second stannous test I did on same batches..... it seems to be working , nice variety of colours in there !

again 3 different leech buckets represented by the 3 columns of plate in same order as first stannous pics (weaker solution from first test on right again on right column .)

hopefully will get them dropped later on this week .

thanks people.
 

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  • stannous 2.JPG
    stannous 2.JPG
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