Catalytic Converter Refining with pictures

[Slayer-PGM]

Hello guys finally i have registered and posted my first post. first of all this is the most helpful forum i have ever seen. I have been on a couple of forums and I found this the most helpful and lots of details with experienced people and helping newbies like myself to full extent possible. Please allow me to introduce myself. My name is Zidan and I have been on this forum from last 4 months trying to grab the process regarding catalytic converter. I have Steve DVD as well in which he leach the cats using HCL/cl and AR. i have already started reading Hoke.Now the questions is that I know Steve uses whole honeycomb instead of crushed powder forum so i got my hands on the crushed catalytic converter (see pics). Its already been crushed and burned and Sieved. Now when I am touching it I can still fee the carbon on my hand. I am not sure if its carbon or ashes due to burning. Now its already burnt so will it affect recovery in hcl/cl or AR? Now by looking at the photo which would be the best method to start according to you guys? AR or Hcl/cl? I have DVD as well so I just need a head start. I am asking it because I dont want to mess up since I only got 1 kg of sample from him. If I can succeed I will get around 200 kg of it.
P.S : I am already using AR to extract gold from gold dust. I am familiar with AR and I saw Steve DVD as well and I am also comfortable with Hcl/cl.
Thank you

 

[solar_plasma]

Ofcourse you should wait, what the pro's will say, but I am pretty sure, you will need AR for this fine powder and leach many times. Whenever I have fine powder I use AR, because chlorox is much weaker compared to AR, even if you only use as much nitric as needed.

 

[Slayer-PGM]

Ofcourse you should wait, what the pro's will say, but I am pretty sure, you will need AR for this fine powder and leach many times. Whenever I have fine powder I use AR, because chlorox is much weaker compared to AR, even if you only use as much nitric as needed.

Thank you very much for the quick reply. Do I have to leach more than 1 time ? Heating would speed up the process I know I have read it many times on this wonderful forum but if I heat how much time will it take approximately and if I dont heat and keep the solution for a day or two will it give same yield?

According to me I will heat it and keep on checkng with Stannous chloride to check if its free from all PGM? Is that the actual process?

Thank you.

 

[solar_plasma]

Although this was about HCl/chlorox on whole honey combs, it illustrates very nicely any leaching process:

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=51&t=18293#p184317
(last passage about the tea bag)

*I love it*

Now this is, when you have whole combs in full strength chlorox, fine powder even with AR will be worse or at least equal, I think. So, 3 times minimum would be okay....but let's see, what the pro's will say.

 

[jimdoc]

Some gloves will be helpful.

Jim

 

[solar_plasma]

Read all safety informations, especially about the pgms, too. Never let dry pgm salts, if you can avoid it. Avoid any dust. I would leach in smaller portions in the same AR, so I don't have too much liquids to handle.

 

[butcher]

Leaching fine powders, powders can settle in the bottom of a vessel packing tightly together, making it more difficult for acids to do their work, in glass vessels heated from the bottom this can become a problem of overheating the bottom of the vessel resulting in a vessel breaking the bottom out because of uneven heating of the glass, keeping the fine powders in suspension, for leach to reach, or to keep from stressing the lab glass can be a problem unless stirred constantly. without heat the process can be more difficult to leach the PGM metals even though they are fine powders.

One option is the crock pot, to heat the solution, and stir solution every now and then during the leaching process, the crock pot heats from the sides of the crock, and will not suffer from thermal stress as lab glass will.

 

[Slayer-PGM]

Leaching fine powders, powders can settle in the bottom of a vessel packing tightly together, making it more difficult for acids to do their work, in glass vessels heated from the bottom this can become a problem of overheating the bottom of the vessel resulting in a vessel breaking the bottom out because of uneven heating of the glass, keeping the fine powders in suspension, for leach to reach, or to keep from stressing the lab glass can be a problem unless stirred constantly. without heat the process can be more difficult to leach the PGM metals even though they are fine powders.

One option is the crock pot, to heat the solution, and stir solution every now and then during the leaching process, the crock pot heats from the sides of the crock, and will not suffer from thermal stress as lab glass will.

Thanks for the reply. By crock pot you mean pressure cooker (I know its also called slow cooker but here its used for cooking fast because the heat inside will help to cook food faster)? Should I just heat the cooker with AR inside? Also how many times or hours you suggest? I was thinking coffee jug (the one used by Steve in his DVD). So I will go for pressure cooker or crock pot. Even on crock pot is there a specific type? Or I can use normal crock pot used by household ladies (i wont take mine, I will buy new )
I will keep on adding photos as I go on.
@Solar_Plasma
Thanks Solar. I will definitely Read all safety informations and infact already started it.
What exactly you mean by "Never let dry pgm salts, if you can avoid it."? I have Steve DVD so you can give reference from the CD if you want. I mean at what stage?

Thank you all once again.

 

[butcher]

https://www.google.com/search?q=crock+pot&source=lnms&tbm=isch&sa=X&ei=ablSU57lA4XayAGgtIG4BQ&ved=0CAcQ_AUoAg&biw=1024&bih=618

crock pot or maybe called a slow cooker, are glazed ceramic pots with wire heating elements wrapped around the pot, inside a tin metal shell, they normally use a switch to power the two heating elements in low medium or high, being resistive heating if needed they can be modified for better control of heat with a dimmer switch or thermostatically controlled, or by lengthening the heating element for very low heating source like with the copper chloride leaching outdoors on those frigid winter nights.


Some of the new types have a glass lid, with a hole in the middle of the glass lid for a knob handle, this handle can be removed and a hose inserted for a type of distilling unit, or for attachment to a scrubber system.

These can be found in second hand stores in the kitchen section, they can be very useful in the lab, they come in many sizes from a cup or two , or in sizes to hold gallons of solution.

While you are in the second hand store you can find many other items to help out in your lab, much of my lab supplies can be found in the kitchen section of the second hand store.

 

[Slayer-PGM]

https://www.google.com/search?q=crock+pot&source=lnms&tbm=isch&sa=X&ei=ablSU57lA4XayAGgtIG4BQ&ved=0CAcQ_AUoAg&biw=1024&bih=618

crock pot or maybe called a slow cooker, are glazed ceramic pots with wire heating elements wrapped around the pot, inside a tin metal shell, they normally use a switch to power the two heating elements in low medium or high, being resistive heating if needed they can be modified for better control of heat with a dimmer switch or thermostatically controlled, or by lengthening the heating element for very low heating source like with the copper chloride leaching outdoors on those frigid winter nights.


Some of the new types have a glass lid, with a hole in the middle of the glass lid for a knob handle, this handle can be removed and a hose inserted for a type of distilling unit, or for attachment to a scrubber system.

These can be found in second hand stores in the kitchen section, they can be very useful in the lab, they come in many sizes from a cup or two , or in sizes to hold gallons of solution.

While you are in the second hand store you can find many other items to help out in your lab, much of my lab supplies can be found in the kitchen section of the second hand store.

I will surely go and check out. But if I dont find one can a coffee pot (Steve DVD) will be useful? I will heat it on low heat till reaction start and stannous test shows positive result. Crock pot is costly here.

 

[solar_plasma]

What exactly you mean by "Never let dry pgm salts, if you can avoid it."? I have Steve DVD so you can give reference from the CD if you want. I mean at what stage?

I mean, those salts are strong allergens. I knew it before, but I first got really aware of it, when I read this one: http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=51&t=9436

So, use and store them wet until you for real want to calcinate 'em.

 

[solar_plasma]

It will work at room temperature, it just takes longer. I guess you don't do this professionally, so time ist no issue. Let it work, stir from time to time, after days you will have the same effect with cold AR, as you would have with hours of warm AR. Just my two cents, and just my impression from the relatively few experiences I have done.

I almost only use higher temperature, when I want to demonstrate something in a school lesson. I leached a partly powdered big cat in the cold. I got 1g after a week of chlorox and 1g after some more weeks of leaching in AR. I guess there are 1 or 2 g more, I will get with rinsing waters.

 

[samuel-a]

Zidan,

Welcome to the forum. Good to know people are still doing their research before actual processing and not the other way around.

To your questions:
- I would first try to incinerate a sample again and look for smoldering residues.
Grab a sample and spread it thinly over a stainless steel tray. Now slowly heat the tray from underneath with a torch until it becomes red hot. If you can see particles which begins to burn and glow (and maybe even smoke), it means the powder was not properly incinerated. As you probably know, left over carbon will reduce yields.

- With a properly incinerated CC ashes, i would first start with hot dilute HCl leach with tumbling/stirring for 24-48 hours to leach out Pd oxides. Then introduce small amounts of Nitric for few more days. The key is to keep things warm and moving around.

- You would probably be best served doing a second leach with hot concentrated AR.

 

[Slayer-PGM]

Zidan,

Welcome to the forum. Good to know people are still doing their research before actual processing and not the other way around.

To your questions:
- I would first try to incinerate a sample again and look for smoldering residues.
Grab a sample and spread it thinly over a stainless steel tray. Now slowly heat the tray from underneath with a torch until it becomes red hot. If you can see particles which begins to burn and glow (and maybe even smoke), it means the powder was not properly incinerated. As you probably know, left over carbon will reduce yields.

- With a properly incinerated CC ashes, i would first start with hot dilute HCl leach with tumbling/stirring for 24-48 hours to leach out Pd oxides. Then introduce small amounts of Nitric for few more days. The key is to keep things warm and moving around.

- You would probably be best served doing a second leach with hot concentrated AR.

Thanks for the help. I did what you said and bought the stainless steel plate and tried to heat it from below and as expected the powder started to burn more like some powder changed to red hot sphere. Not all but some. Please see the pics. Now what??
Thank you

 

[pgms4me]

Those glowing hot spots appear to be the carbon oxidizing. When I did cats, I took the powder or the combs and baked them in my hi-temp oven at 1000 degrees F for 1 hour. Anything above 800 but not over 1200 should be ok. Should only be done outside or in a small kiln that has vent to the outside. This helps to insure any sulpher or carbon compounds are vaporized. Good of you to post the pictures,it helps a lot.

 

[Geo]

I see that you said you bought the material already crushed. I am acquainted with a man that owns and open pit gold mine in Georgia. From his mine you can buy "paydirt". There is a guaranty that the dirt contains at least enough gold to cover the price of the dirt and sometimes people get lucky and find more than they paid for. To ensure that the dirt did indeed have the correct amount of gold, he would "salt" or sprinkle the sand with gold dust. To find twenty dollars worth of gold in a five gallon bucket of dirt would be hard for me to do.

Is there any chance that the material has been "washed" before it was sold? washing with hot AR removes almost all of the PM value while leaving the material undisturbed. If it were mine, I would test a small amount just to see whats in it.

 

[Slayer-PGM]

Those glowing hot spots appear to be the carbon oxidizing. When I did cats, I took the powder or the combs and baked them in my hi-temp oven at 1000 degrees F for 1 hour. Anything above 800 but not over 1200 should be ok. Should only be done outside or in a small kiln that has vent to the outside. This helps to insure any sulpher or carbon compounds are vaporized. Good of you to post the pictures,it helps a lot.

Thank you. Now I have a oven but that is normal household oven and max temperature is unknown but I doubt if it will go 1000 f. Also if i want to avoid the oven what else option do i have? can i just use large stainless steel plate and roast it the way I roast the above sample?
Thank you.

 

[Slayer-PGM]

Is there any chance that the material has been "washed" before it was sold? washing with hot AR removes almost all of the PM value while leaving the material undisturbed. If it were mine, I would test a small amount just to see whats in it.

I am 100% sure that its only burned, sieved and it has not processed in hot AR solution. How would you suggest me to do a sample? Like how much quantity? Also what procedure? Hot AR or HCL/Bleach and that too after burning? Thanks

 

[kurtak]

Slayer-PGM

All I can say is "good luck" with trying to leach & "recover" the PGMs from crushed CAT powders like this - as pointed out by butcher the leaching its self is some what of a problem - but the real problem is going to be recovering the leach from the powders - it is going to be a near impossible task if not impossible - even with a "good" vacuum filter set up

The problem is the "ultra" fine ceramic particle's which already exist in the crushed powder & by the time you are done with the leaching its going to brake down even finer - you will end up with a clay/cement like muck that is going to plug your filter so tight it won't pull (under vacuum) your leach through let alone any washing

At best you could get away with vacuum filtering a thin layer of material at a time (a cup to a cup & a half in an 8" filter funnel) but you are talking about processing 200 kg of material - you could "maybe" get away with it if you had a filter press but even then I think you would have a problem with plugging before you got all the leach washed out

About a year & a half ago I entered into a joint venture with a scrap yard with the idea of processing CATs for the PGMs (other then my self there was 3 other people involved that new something about PM recovery/refining) & we tried a number of different things for processing CATs - they were -----

(1) leaching whole CAT combs --- by far the most successful - at least here we where able to pull more value out then the price of selling the CATs out right - however the value was not great enough to cover wages - expense - &/or general over head

(2) leaching crushed CATs - near total failure due to the filtering problem - & we tried a number of different things to over come the problem (& we had a very big vacuum pump - made for running "large" dairy milking parlor systems) to the best of my knowledge the scrap yard still has a couple of buckets of this media stored with the leach still tied up in it

(3) caustic fusion - limited success - some problems - never completely worked out (I believe this is how the big boys do it - but not sure)

(4) smelting - some what successful - showed promise - but again never completely worked out - in fact I still have the anode bar from this - which tested positive for PGMs on the XRF --- this is the method I would suggest going with being as how your material is already crushed :!: :!: :!:

(5) caustic wash/leach - more of a drawing board idea with possibility - started never finished (would need to be done with whole CAT combs)

Bottom line - trying to leach CATs - for profit --- good luck (its not how the big boys do it & for good reason)

Leaching a few CATs as a hobby to learn about it & put some PGMs in your personal stash is one thing - trying to do it on a large profit making venture is a whole other thing & I can only wish you the best of luck --- for one thing - you will NEVER get all the PGMs out - & you are going to end up with a HUDGE amount of waste to deal with

Kurt

 

[maynman1751]

Kurtak, I have no idea what I'm talking about, but couldn't he siphon of the liquid, add more liquid, stir vigorously, let it settle, siphon....etc? Then this solution could be evaporated down to a manageable volume?????? I know a lot of the PM's will not be recovered, but some is better than beating yourself to death and ending up with nothing!!!!