Refining my wastes

[jeneje]

Hello all,
I need some help with my waste solutions. I have approx. 200gallon of AP, AR, HNO3, and HCL all mixed together. Yes I know i screwed up. I will take the flack over that. Anyway, i have read that I can use steel to drop all the PMs and copper out of solution. My question is once i have done this, should i recover the sludge and reprocess using HNO3 to disolve base metals again as CM hoke refers to, and will my PMs still remain in the sludge to refine with AR.
When i first joined the forum i was as many on here, head strong and knowed more then anybody else :roll: WRONG!! since then i have taken the time to redo my lab(made it safer) and now begining to have an understanding of the correct processes. "slow learner here"
I do want to say that i have learned alot from the wise folks on here and hope to continue to learn, while i do make mistakes, i am grateful for all who is willing to teach. Any help here is welcome and I am truly thankful.

Ken

 

[gold4mike]

I think you'll do better to cement everything first with copper.

Once you're confident the PM's are out, then drop with iron/steel to get the copper out.

If you drop all of it at the outset you'll use more acid and generate more waste again trying to eliminate the base metal (copper) that is mixed in with your PM's.

 

[jeneje]

I think you'll do better to cement everything first with copper.

Once you're confident the PM's are out, then drop with iron/steel to get the copper out.

If you drop all of it at the outset you'll use more acid and generate more waste again trying to eliminate the base metal (copper) that is mixed in with your PM's.

Thanks gold4mike, i do have a copper bus bar i can use. Does all solutions that i have mixed up with one another make a difference as far as dropping the pms? I do know now to seperate the different ones.

Thanks
Ken

 

[butcher]

As long as it is acidic the copper will replace the valuable metals from solution.

 

[Geo]

use copper first (copper pipe will work) keep an eye on the pipe, if it deteriorates to the point of falling apart pull it out and replace it. after a time when no more copper dissolves, syphon or decant solution down to within a few inches from the bottom careful not to disturb any powders on the bottom. stop just short of the powder and add water (depending on the amount of powder and solution) double the volume with water and let everything settle. decant or syphon again to a different container (add this solution to your now barren spent copper solution) again add water and settle. decant leaving powder. this solution is added to the first. repeat last step till water stays clear. decant and discard last rinse and collect powder to process later. now you can add a piece of steel to your spent solution. leave steel in solution until solution clears to a very light lime green. decant this solution or syphon to a container that will hold solution and have two thirds free space for the reaction to neutralize the solution. add lime dust or soda ash slowly until theres no reaction. the spent solution is now safe to discard safely.

 

[etack]

I would use iron with that much volume and acid it could take a lot of cooper. If you use large pieces of sheet metal it could be quick then put the cooper sponge in the new stock bucket to be used up when new acid is added. you PMs will still be there.

Eric

 

[butcher]

The only copper it will use to cement is the amount needed to replace the valuable metals, and the amount of copper needed to saturate the free acid with copper, adding iron first would contaminate the values.

You can work in batches, start with clean 55 gal barrel siphon off acid solution into this barrel adding copper to this barrel (you may already have salts of some values in the containers the acids are sitting in now, decanting the solution and collect them).

Once you finish one barrel, and get the copper sludge from using the iron cementation process, you can use this recovered copper to cement the next batch.



Another suggestion is use this acid solution in crock pot method to remove base metals from other scrap, heating the solution will also concentrate it, so the volume of waste can be reduced, this will cement any values (along with some unwanted stuff that can be cleaned up), this will lower volume of your waste,
The powders from the crock pot will need more clean up later, it is a little bit more of a challenge but can be done, once you understand the principles Hoke’s book teaches, I have used my used solutions to remove components from circuit boards, cooking the copper chloride solution to almost a thick syrup, some dilution to precipitate copper I chloride, the mix of lead, silver, copper and other values and trash in these powdered chlorides, these put into container that my next batch of used solution is added to (used solution to help clean up these powders)and stirred well and heated, saturating this batch of used solution and cleaning up the powders some, decanting this solution goes to the crock pot.

The powders are boiled in water and lead and some other metals removed, then neutralized, then dried on hot plate and incinerated with propane torch in the same corning dish, cooled and a boil in HCL, diluted kept warm while powders settle and lead copper and tin are removed, this is repeated till no more color, then the powders are again dried and incinerated for recovery of silver gold and other values.

This is a bit hard to explain in detail but I can have several containers powders being upgraded, while waste acids are downgraded, waste acids moving from container to container in one direction (toward dirty waste disposal, and the powder moving from container to container toward being cleaned up values in the opposite direction.

You would be surprised at how much dissolving power your spent waste has, and these eventually become solutions of metal chlorides higher in the reactivity series as you continue to use them, filtering the solutions with tin is much easier when solutions are concentrated, and warm. These filters are also kept for processing, I even keep my fairly clean lead salts and tins salts in separate containers, even my powders are used in my recovery (like the copper powders, the copper I chloride powders are handy to replace values from solutions.

 

[jeneje]

Thanks guys for all the help. I have learned alot again. I am bookmarking this post for referance and would suggest all new member to do the same.
Thank you all very much.

 

[4metals]

Jeneje

Mixing the wastes isn't the end if the world. This has been pretty well covered before and I'm sure you're up to the task.

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=47&t=1300

 

[Oz]

Another good resource to keep yourselves EPA compliant as a Conditionally Exempt Small Quantity Generator.

http://www.epa.gov/osw/hazard/generation/cesqg.htm

You will also need to read up on your state’s regulations, they may be stricter than the EPA minimum guidelines.

 

[jeneje]

Hello all, I have run into a snag. Some of the buckets i had in the begining i did not put a copper bus bar in before i put metal in them. When i went to add them today, i noticed a thick rust sludge in the bottom. So now...i am thinking about filtering the sludge and use a crock pot and re-dissolve the material in HCL to remove all the base metal and start over using the copper bus bar first to drop my pgm's. My question, is this the right approach to the prolbem to recover the pgm's or is it to far gone now. Any help here is appreciated.

Thanks
Ken

 

[etack]

HCl wont dissolve Cu.

I would wash it with hot water till it runs clear. Than I would use poor mans AR on it slowly. using only enough nitrate to dissolve most of the Cu. then test solution and if barren pour off and do it again. when you only have your PMs at the bottom collect and refine.

This is what I would do.

Or you could melt into an anode and refine in a Cu cell.

Eric

 

[Oz]

HCl wont dissolve Cu.

Acid Peroxide does just that using HCl, you can skip the H2O2 and it will just tak a bit longer to get going.

 

[NoIdea]

Hi All - I may be mistaken, but wont the nitrate, in the origional brew, need to be delt with before the use of copper to drop the pm's?


Deano

 

[butcher]

The nitrate and acidic solution would form (a form) of aqua regia, even so, the values in solution would cement on copper once nitric and the acid was saturated with copper (the acids used up in making copper salts dissolved into solution).

Powders from my stockpots are washed and neutralized rinsed and dried then incinerated before treatment to remove base metals.

Depending on powders, I sometimes reuse the powder from the previous stock pot in the next (newly formed) fresh stock pot, the new waste put into these powders cleans up some of the base metals in these powders from the previous stock pot, and cement values from this newly added waste acids (I am not sure how I explained this makes sense).

 

[jeneje]

Hey all, i may not have posted the right prolbem, when i first started refining my material - my waste solution was put into five gallon buckets, (thinking all of my pm's were gone from the solution :roll: ) i put metal in the waste buckets thinking i could retrieve my copper and it would neutralize my solution and i would have copper salts.
What i got is buckets that have un-disolved metal chunks mixed with pm's in sludge that did not drop. With that said - if i understand this right i can filter off the solution, let the sludge dry and re-disolve again to recover the pm's or incinerate the sludge and process again.

Thanks
Ken

 

[Geo]

incinerate the sludge and then pulverize and use a magnet to remove any iron. i would screen it and pulverize again and repeat the magnet until it all is screened. then (depending on weight, if pounds, do smaller batches) boil in hcl until the solution turns black. decant and repeat until the solution remains clear.if you do a few ounces at a time it may be easier.as you do a batch add any undissolved metal together in one container until all the material has been treated. rinse with water until water stays clear. dry and incinerate and digest in hot dilute nitric acid to remove silver and palladium and then process whats left in cool AR to recover the gold. anything left will be PGM's.

 

[jeneje]

incinerate the sludge and then pulverize and use a magnet to remove any iron. i would screen it and pulverize again and repeat the magnet until it all is screened. then (depending on weight, if pounds, do smaller batches) boil in hcl until the solution turns black. decant and repeat until the solution remains clear.if you do a few ounces at a time it may be easier.as you do a batch add any undissolved metal together in one container until all the material has been treated. rinse with water until water stays clear. dry and incinerate and digest in hot dilute nitric acid to remove silver and palladium and then process whats left in cool AR to recover the gold. anything left will be PGM's.

Thank you Geo, That was what i needed to know. After learning to use copper first to drop my pm's i am getting alot more gold then ever before. I now treat my waste with copper before metal. Again thanks a bunch.

 

[goldenchild]

I wouldn't process the waste in large barrels. I think you would have an easier time handling everything in 5 gallon buckets. I think you mentioned that you were. This way it won't get overwhelming. Unless of course you are set up to process 55 gallon drums. I've learned the hard way to try and manage wastes ASAP after reactions :roll: Waste management and processing is my least favorite part of all this and takes a long time if you are trying to do it properly. Large volumes compounds it.

 

[jeneje]

I wouldn't process the waste in large barrels. I think you would have an easier time handling everything in 5 gallon buckets. I think you mentioned that you were. This way it won't get overwhelming. Unless of course you are set up to process 55 gallon drums. I've learned the hard way to try and manage wastes ASAP after reactions :roll: Waste management and processing is my least favorite part of all this and takes a long time if you are trying to do it properly. Large volumes compounds it.

Yes you are right goldenchild, i too am learning to deal with waste asap, this mess is from a year ago and yes i am trying to do it the right way. I think by summers end it will be all gone and i will be back on track to a better way of dealing with it.
Ken