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topic 22253

Refining of Palladium and making its salt


A discussion started in 2003 but continuing through 2019

2003

Q. Dear Sir,

I recover palladium from dragouts by electrolytic method, as a result this palladium contains traces of nickel, copper and Iron. Kindly suggest how to refine this palladium and convert to "di nitro di amine palladium" salt.

Note: please don't ask me to refer to refiners. Expecting a genuine answer from worthy candidates.

Panjala Mukesh Panjala Mukesh
     fashion jewelry mfgr.
Hyderabad, India



2004

Q. If anyone could help in making p-salt from the palladium metal.

Kumar Shah
manufacturer - Mumbai, Mahrashtra, India



2004

Q. HOW TO REFINE THE PALLADIUM AND PLATINUM.

DEAR SIR, I just know how to refine gold, but I'd like to expand my knowledge to refine platinum and palladium. PLEASE, any helps or tips that SIR can provide is appreciated.THANK YOU.

CHIN KOON LOONG
- G.TOWN,PENANG,MALAYSIA


2004

A. Hey there!

My father owns a precious metal refining company down here in Sydney Australia. I have been working there for 2 years now and only in the last 6 months have we started to refine platinum and palladium.

Best way is to dissolve the platinum and palladium in an Aqua Regia (4:1 Hydrochloric:Nitric) and set to simmer for about 2 hours. Platinum and Rhodium will not dissolve at room temperature. Once completed neutralize the nitric by adding a scoop of urea ( add slowly! ) and once frothing stops transfer into crystallization dishes and set to boil till liquid is down about halfway. Add ammonium chloride and stir and you will see a red/orange mud precipitate. That's your palladium/platinum. Of course its not as easy as it sounds but those are the basic steps.

Hope I helped a bit.

Elan Bension
- Sydney, Australia


Refining Precious Metal Wastes
by Hoke
from
Abe Books
or




"Recovery And Refining Of Precious Metals"
by C.W. Ammen
from Abe Books
or
info on Amazon

2007

A. Put your dirty Palladium in a bath of nitric acid (1 quart sulfuric to 1/2 cup of sodium nitrate if you want to make your own weak Nitric acid =30%) Once thoroughly bathed pour off the acid into a new container leaving the rest to be discarded, add Sodium chlorate to the acid and the Palladium will drop out looking yellowish then turn a blue/green. You can also drop it with dimethylglyoxime (DMG) out both Nitric and Aqua Regia...but it hard to find and really expensive.

I don't know if this what you are looking but it's what I know to do.

Damon Hunt
- Vancouver BC Canada



April 7, 2008

Q. Hello everyone,

I am working as a Chemist in one of Philippines precious metal refinery. I'm just 3 months hired but then our lab has no manual of analysing many things. I really have problem with the standard method of analysing palladium. Can anyone point me to a site or just send me a document that will enable me to really understand how to assay palladium.

nathan

Nathan MF
- Cebu, Philippines


September 18, 2008

A. When recovering Pt, Pd from spent Aqua Regia do not add urea as Platinum does not precipitate completely in the presence of nitrogen compounds, the classic method of boiling the acid to syrup to expel the nitric is the only way for a small scale operation to completely recover the platinum. As far as the Pd from dragouts the best method to quantitatively collect the Palladium is to digest the impure Pd in 50% nitric acid and selectively drop out the Pd with dimethylglyoximide.

Rick Hoff
- Hicksville, New York



June 1, 2009

Q. I am looking to learn how to separate palladium from raw ore. Can someone guide me in the right direction? please.

Mary Chavarin
- San Diego, California


June 4, 2009

A. I saw a post saying a small scale operation need to boil the acid to expel all the nitric acid to recover all the platinum, however I refine precious metal, and have been told that the platinum will not drop out of aqua regia unless there is a powerful oxidizer (i.e. nitric acid). We simply salt the aqua regia with ammonia chlorate to precipitate platinum.

Craig Hirschey
precious metal refiner - St. Paul, Minnesota


August 10, 2009

A. I am an amateur refiner; I have been refining gold for several years; recently I have started to recover Pt from AR after the gold is precipitated. I do this by pouring the spent AR into a bucket and add some Al sheet metal. The Al will be absorbed into the solution and will precipitate all other metals in the solution, including a large quantity of Cu. I wash and dry the mud that I get from the AR then boil it in HCl. Wash and dry again then treat with AR. You will now see a quantity of Platinum Chloride (Red Foam) scoop the foam from the top and collect the red mud in the bottom dry and melt. There will be a very toxic smoke to be expelled when melting. Breathing the smoke can result in Platinosis. When melting there will be a lot of residue with small beads of Pt which will accumulate and render a larger bead. This process is a little tricky but it works. Pt melts at about 3000° f. I use Propane and oxygen which only gets to 3500f so I am not able to melt the Pt to a point where it will flow, but I can melt it enough to get very soft and bind together. One can wash the red mud with water; which will result in the Platinum Chloride turning to Platinum oxide and will go from red to black. Just dry and melt. It works for me. don't BREATH THE SMOKE!

Bruce Hannan
- Maryville, Tennessee



April 8, 2010 -- this entry appended to this thread by editor in lieu of spawning a duplicative thread

Q. Please help me I have recovered palladium but I can't refine it. please any one help me.

M Bilal M Madni
- Rawalpindi, Pakistan


January 3, 2011 -- this entry appended to this thread by editor in lieu of spawning a duplicative thread

Q. Dear sir,
Sir, I just want to know that I have a palladium in liquid state which is dissolved in nitric acid together with some other metal like silver, copper. Please tell me how can I make palladium separate from others, please do help me out of it.

Jitendra Rastogi
student - Meerut, U.P, India

----
Ed. note: Readers -- Please recognize that internet forums are giant one-room schoolhouses where schoolchildren and post doctorate chemists may view the same page. Jitendra posted his inquiry as a "student project" question, and it is important for people in his situation to recognize that while this page may describe some of the theoretical steps and formulas and reactions involved in refining palladium, as an aid to understanding chemistry, it is certainly not meant as instruction pages for untrained students to attempt the experiments.



January 12, 2011

Q. Dear Sir,
Sir, please tell me how can I make separate dissolved palladium from nitric acid in very fine purity.
Please tell me the process to make palladium salt and separated from other dissolved metal also in that liquid solution . I will be thankful to you

jeet sharma
jobshop employee - delhi



October 21, 2011

Q. Dear Sir,

How to recover Pd from nitric acid which contains Cu and Palladium?

Sara Sharala
Chemist - Malaysia


October 28, 2011

A. Dear Sara, Boil the PMG (Platinum Group Metals)that are in HNO3 solution with continued additions of HCl, Boil to almost dryness then add more HCl. After the third time start testing with starch/iodine paper. When all the NOx is gone (TAKE YOUR TIME), reconstitute the solution with water. If you have Pt in solution,recover it first. Use a saturated solution of Potassium Chloride. The Pt will come down as a yellow precipitate K2 Pt Cl4 Filter and wash this with cold saturated Potassium Chloride solution, it is slightly soluble. There are several ways to recover the Pd. The easiest is to ammoniate the solution with concentrated Ammonium Hydroxide in small additions, the Pd will first go to a Pink salt then with a further addition or two this will redissolve. How the Pd can be dropped by slowly adding HCl.At pH 3-4 (HN4)2 Pd Cl6 an orange yellow salt will precipitate. Filter and wash with cold saturated Ammonium Chloride solution, it is also slightly soluble. Save all your wash solutions and test for PMGs before discarding. DO NOT try to melt the salts, huge PM losses. Reduce in solution with Hydrazine, then melt. Bruce

Bruce Stewart
- West Grove Pennsylvania USA


March 14, 2012

A. Here are three low tech ways of separating copper and palladium:

1) Use Silver.

Silver is above copper, but below palladium, on the electromotive series, so adding silver to the copper/palladium solution will precipitate the palladium and leave the copper in solution. Remove the precipitated palladium and add sodium chloride to the remaining copper solution, and the silver will be recovered as silver chloride. This can be reduced back to metallic silver by various methods. Silver is expensive, and some will be lost in each cycle, so you will have to decide if this method is feasible for you.

2) Use Oxygen.

Use zinc or aluminum to drop both the copper and palladium from solution. Wash this several times and dry. Spread both metals on a non-reactive surface and heat. Copper oxides at fairly low temperatures to copper oxide. Remove this with dilute hydrochloric acid, leaving the palladium.

3) Use ammonium hydroxide.

Add sodium hydroxide to the copper/palladium solution. This produces blue green copper hydroxide, and a dark colored palladium hydroxide. The copper hydroxide is soluble in ammonium hydroxide, leaving palladium hydroxide, which, with heat, will decompose to palladium oxide and finally to palladium.

You can find the physical and chemical properties of these reactions on line, along with such things as oxidation and decomposition temperatures.

No matter how carefully you process the two metals, some copper will always remain, so be prepared to repeat the refining process until you reach the purity which you require.

Gary L Kissler
- Kooskia, Idaho, USA



December 6, 2011

Q. I have many gallons of expired liquid Pd/Sn plating activator in an HCl solution and I wish to extract the Pd from it. I've located some similar procedures but nothing specific to PGMs containing Sn. Has anyone forum reader seen a procedure for this?

Peter Dylazo
- Vancouver BC



November 16, 2012

Q. Dear sir ,
I am interested to recover palladium from copper, nickel, lead, tin electronic scrap. The content of copper is around 35% and that of Pd 10%

With regards

Debabrata Mohanty
precious metal refining company - Mumbai, Maharastra, India



January 21, 2013

Q. Hi all...
I'm new here and found this useful site where I can find my answers.
So, I've got a huge amount of powder in which palladium and iron is involved.
Now I want to separate the palladium from that powder.
I don't know what to use and what's the process.
Please somebody help me.

Safin Khan
- India



August 3, 2013

Q. I am looking to learn how to produce palladium nitrate [Pd(NO3)2] from palladium metal. Can someone guide me in the right direction? please

Mahboobe Asadi
- Tehran, Iran


January 23, 2014

A. Refining platinum and palladium is a process that requires patience. I recover platinum, Palladium and rhodium from catalytic converters. The process is as follows:

After de-canning the substrate material, I drop the substrates into a drum of hot soapy water and allow them to soak for about two hours (this helps to remove some of the sulfur and excess hydrocarbons). Next, using a water hose and nozzle I rinse the substrates which removes the carbon and sulfur. I then shake out the excess water and allow the substrate to dry for two days. The substrates are then crushed in a small ball mill to a fine powder and I roast these powders in a brick oven at 400 °C, which burns off the remaining hydrocarbons and sulfur. After cooling, the powders are placed into a fermentation barrel and I cover them with a 50/50 mixture of 3% hydrogen peroxide and 32% hydrochloric acid. I add about 100 ml of houshold bleach cover and then agitate the barrel every few hours for about a week adding bleach every other day. I then filter the liquid into a beaker and heat to a low boil which removes excess chlorine and reduces the solution. After cooling you can precipitate leached PGMs with zinc, keep adding zinc in small amounts until the solution is clear. Your PGMs will precipitate as a black powder. Siphon off the solution leaving the black powders; wash the powders first with water, and then with HCl 32% to remove excess zinc. Afterwards, dissolve the black precipitate in a small amount of Aqua regia and again precipitate the black PGMs with zonce, repeat washes and re-dissolve in AR a second time.

Now you are ready to separate the metals. First precipitate your platinum salts with Ammonium chloride. Filter the yellow salts and save the solution, you can test the solution for palladium with DNG test solution, precipitate with zinc again and wash. Redissolve the palladium in AR and precipitate with sodium chlorate or chlorine gas to produce the brick red palladium salts. Again save the solution.

Your Platinum and palladium salts should be heated to 800 °C to make the sponge (separately, of course). To produce the Platinum and palladium metals from the sponge will require heating to 1800 °C. The metals produced are .999 pure and can be poured into graphite moulds to produce coins or bars, your choice. Hope this helps. Be careful and be safe. always work with a fume hood or outdoors -- the fumes are deadly.

David Singleton
- Tibro, Sweden


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