instructions of using eco-goldex e series reagent in e ... in e-waste gold stripping.pdf ·...
TRANSCRIPT
Prepared by
John Guo (P. Geo, Ph D)
Eco-Goldex.com
Tel: +1 438-825-5288
Email: [email protected]
Oct. 20, 2016
Instructions of Using Eco-Goldex E
Series Reagent in E-Waste Gold
Stripping and
Gold Recovery Procedures
Declarations and Notes
• Though Eco-Goldex is a low toxic chemical reagent invented for effective gold
extraction of various materials (gold ores, E-waste, sulfide concentrates…), it
does contain certain level of toxic and can cause harms to human body and
health problem if it is not properly handled.
• All precautions and safety protections at operation site should be exercised and
respected!
• Reagent should be stored at place where children can’t reach; reagent solution
should not intake and leaching/stripping operation should be conducted at open
space.
• This instruction is prepared for gold stripping dummies who don’t have much
background of gold leaching and procedures.
• If you already have a lab with cyanidation test facility or gold mine operation,
have your lab technician treats eco-goldex reagent the same way as cyanide
because eco-goldex reagent has the same operation conditions and procedures
as cyanide except eco-goldex is low-toxic and eco-friendly.
Chemicals and Tools Needed in Gold
Stripping Operation • Chemicals:
– Eco-Goldex E series (from eco-goldex, for gold stripping)
– Zinc strips (from eco-goldex, for gold precipitation)
– Gold Precipitation agent package (A,B,C) (or Ammonia solution)
(from your local supplier, catalyst work together with Zinc strips for
gold precipitation in pregnant solution)
– Sulfuric acid *( from your local supplier, for gold purification)
– Borax ( from your local supplier, for gold purification during refinery )
• Equipment/tools – Filter (filter paper) (we provide a special filtering paper for large scale filtering
purpose)
– stripping tanks/Pail /container(4-5)
– Heating stove
– Glass beaker, evaporating dish
– Crucible
– Torch/Muffle furnace
* HCI, H2SO4, HNO4 are all capable for gold purification purpose in this stage. But we consider H2SO4 is better
HCI is cheaper but not as strong as H2SO4, gold purified by HCI won’t reach 99%; HNO3 is strong but more expensive than H2SO4, it can make 99.8% gold as H2SO4. H2SO4 is good enough to purify impurities such as Zn, Cu, Fe, Ni… from gold to make 99.8% gold.
It is your decision which acid you will use in this stage.
Major Gold Stripping/Recovery Steps
Dissolving gold (stripping) from by eco-goldex E Series solution.
Separate stripping solution and the residual solid materials. The solution is also called Pregnant solution as it contains
gold (in anions format)
Au (Solid) 0
Au (solution) 3+
Precipitate Au from pregnant solution through Zinc strips (powder)
Purification
Au (solution) 3+ Au (Solid)
0
Stripping
Precipitation
Sponge gold Refinery
Filtering
Eco-goldex E Series Reagent Concentration in Solution
Many users ask this question, there is no direct answer for this
because it depends on how fast you want your gold stripping goes. If
you want to have very fast stripping, you need to have high E series
concentration, if time is not an issue, you can do stripping slowly, then
you can have lower E concentration in solution.
We give the following general guidelines:
• E series reagent weight ratio with water of 1-4 :100 (i.e. Add 1-4 kg
E reagent into 100 liter water) will give a moderate stripping speed.
• A role of thumb, If stripping is too slow, it means you need add more
E series into the solution.
• Hot water stripping solution (i.e. 40-60oC) will significantly increase
gold stripping speed.
• It is NOT recommended to recycle the stripping solution since
the effective components are ran out in the solution at the end
of the process; in addition, once gold precipitation agents
added into the pregnant solution, solution chemical property is
changed and the solution can’t be sent back to stripping
solution.
• It has been confirmed that Activated Carbon is NOT a good
candidate to recover gold from Eco-goldex E series product
derived pregnant solution.
• E co-goldex E series stripping solution is alkaline, it is safe
using steel tank.
Agitating is always a
plus for stripping as this
will increase solution
dynamics and
accordingly chemical
reactions in the solution
water
Prepare proper volume of water
in a tank
Alkaline water
Add E series reagent based on the ratio proposed above into water, agitating
water make sure reagent dissolved well. stirring solution if necessary
Step 1: prepare gold stripping solution
1 2
Note: though you don’t need to adjust pH value in the stripping solution, but make sure never add acid into the solution!
For most common gold bearing E-waste (CPU, RAM, Pins, electronic circuit boards…) , eco-goldex reagent concentration is about 1-4% (which means add 1-4 kg E series reagent in 100 liter water) for moderate stripping speed.
Watch video about how to prepare the leaching solution on youtube
• Warm to Hot water temperature: 40-
60oC is perfect.
• Room temperature works well if you
don’t want to pursue fast stripping
speed.
Stripping solution can be prepared in
advance to ensure complete dissolving
of the reagent (i.e. 2 -3 hours before
stripping)
4 gallon alkaline leaching solution
Once stripping solution is prepared with proper quantity. Make sure
E-waste materials are completely submerged into the solution.
Stirring if necessary and check the surface color visually to see
whether stripping is done. When E series concentration is high, the
stripping is going very fast, 10-30 seconds depending on the
thickness of the coating.
Notes: by visually checking the surface of the electronic parts to decide the stripping time and make decision should more E reagent be added into the solution to speed up stripping process.
5
Step 2: Stripping
stripping usually goes very fast
when stripping starts then slow
down as effective components
consumed quickly.
Step 3: Filtering 1. upon satisfaction of the stripping result, stop agitation and filter the solid and pregnant solutions.
3. Properly dispose residual solid after pregnant solution is transferred to storage tank and restart a new tank stripping if necessary.
Pregnant solution
2. Using a filter pump to transfer the leaching (pregnant) solution to a storage tank for gold precipitation
Depends on your situation, the filtering process can be as simple as just pouring out pregnant solution into a solution storage and dismiss the residual solid waste to another storage bins as shown in next page.
• Once stripping is done, filtering the pregnant solution from the residual waste
materials. Retain the pregnant solutions. This filtering is to separate waste solid from
pre solution, these solids are metals that may contain Cu, Pb, Ni, Fe…, it should be
removed from preg solution as much as you can.
• You need only to filter the preg solution, As long as it contains no solid materials,
preg solution may looks dirty, that is fine.
• Make sure rinse the residual solids with water before dismiss.
How to know you have gold in your preg solution
• Your stripping test materials are usually in small quantity (n lbs
~ nx10kg). You need to expect how much gold you may recover
in theoretical condition( assume 100% recovery);
• Your gold quantity is usually small (~ grams) in the solution
unless you cumulate your stripping solution in one batch
process or process large amount of materials;
• Two methods to tell you have gold or not in the pregnant
solution:
– Qualitative : using Stannous chlorite coloring method;
– Quantitative: send your pregant solution to a qualified lab to assay
gold concentration in the solution .
This color indicates there is gold in the solution.
Before Stannous chlorite solution added
After Stannous chlorite solution added
A simple Stannous Chlorite Color reaction method can be effective to tell whether there is gold in the leaching solution .
(note, this method works well only when Au concentration is high enough in the solution; if Au concentration is low,
color reaction may be not obvious.)
In E-waste gold stripping, visual checking can tell
whether gold is dissolved or not.
Before stripping
Original chip
After stripping completed
Chip is partially stripped
Step 4: Precipitation
The following chemicals and materials are needed to precipitate
gold from pregnant solution:
• Zinc strips (some people like to use zinc powder, it is the
same function, but zinc strips will avoid you solution filtering
process after the zinc precipitation is done) .
• Ammonia solution (NH3.H2O), or
• Gold precipitation package A,B,C.
Notes: 1. Using Ammonia solution or the gold precipitation package A, B,C depends on their
availability at your local suppliers. 2. These two chemicals (package) service the same purpose of helping precipitation of
gold onto zinc strips. Without them, gold won’t precipitate with zinc strips. 3. Quantity of ammonia solution added in pregnant solution is 20-40% in volume; 4. Quantity of package A,B,C refers to next page. 5. Quantity of Zinc strips is about 10 times of gold to be precipitated from preg solution
About the gold precipitation package
The package is composed of three chemicals A, B, C: A: citric acid; CAS No: 77-92-9; B: Ammonium fluoride, CAS No: 12125-01-8; C: Magnesium sulfate, CAS No: 7487-88-9 the mixing ratio of the three chemicals is: A:B:C = 2.5:1.5:1
• 1 liter of pregnant solution needs 20 grams A, 12 grams B and 8 grams of C.
• Add proportional gold precipitation agent A,B,C into the pregnant solution
based on the volume of the pregnant solution to be precipitated.
• Ammonia solution has better gold precipitation than the package A,B,C.
• We provide the package here as an option since Ammonia solution is not always available in some countries. The three chemicals A,B,C are all solids, this make their transportation are more acceptable in some countries as well.
Gold precipitation from pregnant solution
Pregnant solution (measure volume and estimate Gold contents in it to determine the package quantity or the volume of Ammonia solution and zinc strips will be added)
Add Zinc strips in the pregnant solution.
i.e. if 4 grams in pregnant solution, add 40 grams of zinc
strips.
Add gold precipitation agent package (A,B,C)
Or Add 25-40% ammonium solution (NH3.H2O)
• A,B,C is proportionally mixed according to the ratio of 2.5 A: 1.5B: 1C.
• 1 liter of pregnant solution need 20grams A, 12 grams B and 8 grams of C.
• Add gold precipitation agent A,B,C into the pregnant solution.
Gold Precipitation Agents
The package is composed of three chemicals A, B, C: A: citric acid; CAS No: 77-92-9; B: Ammonium fluoride, CAS No: 12125-01-8; C: Magnesium sulfate, CAS No: 7487-88-9
Agent 1: Chemical package
Just add industrial grade ammonium solution into the pregnant solution. The proportion is about 25-40% of the volume of the pregnant solution. The criterial is that when ammonium solution percentage is right, the zinc strips added in the pregnant solution should change color quickly, if no obvious color change, it indicates too much E series concentration still in the pregnant solution, then continue add ammonia solution.
Gold Precipitation agents
Agent 2: Ammonium solution (NH3.H2O/ NH4OH)
!! Agent 1 and agent 2 can be alternatively used. It depends on their availability from your local market. !! Remember Ammonia is restricted for shipment by air, it will be better buy locally.
Zinc Strips Precipitation • Add zinc strips into the catalyst agent (ammonia /package A,B,C)
regulated pregnant solutions;
• The amount of zinc strips is as follows:
weight (zinc strips) = 10 times Au to be Precipitated from pregnant
solution.
i.e.
if 6 grams of Au expected from preg
solution, then add 60 grams of zinc
strips into Preg solution.
• The precipitation time should be
About 2-3 hours depends on the
quantity of pregnant solution.
It is recommended to test Au contents
in diluted preg solution before disposal.
• Second time precipitation of the diluted
Preg solution is recommended to maximize
gold recovery
Normal Zinc Precipitation process
2-3 hours precipitation to ensure complete Au-Zn exchange. If you put Zinc strips in the pregnant solution too long, Zinc strips will be broken into small pieces as the solution is too alkalinic. If that does happen, don’t worry, as gold is still at the bottom. Filter the solution to get your gold.
After 3 hours
This photo shows the reason why we recommend to use zinc
strips not zinc powder (if zinc powder is used, another filtration is
required. With zinc strips, you just need to pickup them easily)
Diluted preg solution
Au Loaded zinc strips
Add new zinc strips into the diluted preg solution will help improve gold recovery (second precipitation)
• Use clean water to rinse the Au loaded zinc strips;
• Recover the rinse solution into the diluted preg solution to have the second time precipitation to avoid loss of gold.
• The rinsed and Au-loaded zinc strips are ready for purifying.
Step 5: Purification • Put Au loaded zinc strips into a plastic pail, and then add
proper amount of clean water;
• Slowly add sulfuric acid into the pail and slowly stirring the
zinc strips.
• the zinc strips will be dissolved in the diluted sulfuric acid
solution;
• The purpose of this step is to remove the extra zinc metals and
other soluble metals.
Pre-added water will act as a diluting solution to prevent strong reaction between Zinc and sulfuric acid
Always gloves!
Slowly add high concentration of sulfuric acid (H2SO4) into the pail to dissolve loaded zinc strips
Gentle stirring the solution still all Zinc strips are dissolved and become small tiny particles
Add sufficient clean water to dilute sulfuric acid to prepare filtering. Strong sulfuric acid will damage the filer paper if not diluted properly
!! Strong and dangerous gas released, do this in open space or in well
ventilated space !! If it is possible, you may add minor
HNO3 to remove other impurities here before adding water,
Filtration of the primary gold dust
These tiny black dusts are primary gold with impurity
Make sure dry this dark sludge as much as you can to remove water from it. As extra water in sludge may cause the next purification solution spill over under heated condition.
Second time purification
Carefully pouring high concentration of H2SO4 into a 2L glass beaker, amount of H2SO4 depends on the filtered primary gold dust, enough to submerge all solid materials
Slowly put the filtered primary powder including the filtration paper into the beaker with H2SO4 solution. You should see the filter paper will be dissolved quickly.
H2SO4 only
Make sure not much water in the sludge, it will cause spill when heated
98% H2SO4
This shows what it looks like after the filtration paper is dissolved with the dark tiny primary gold dust in the strong H2SO4 solution
• Sitting the beaker onto a stove to
cook the sulfuric acid to remove
other metals (Cu, Fe, Ni…).
• Slowly rise stove temperature to
prevent possible beaker burst.
• Use an evaporating dish cover the
beaker
An evaporating dish cover the beaker will depress smog!!
Double safety container! In case the beaker is broken, the gold will be in this container.
stove
• Cook the H2SO4 solution till the solution color changes to brownish red from dark.
• This process is critical to ensure high purity of your gold!
• The longer time you cook, the more impurity metals (Cu, Ni, Fe…) will be removed by H2SO4, and the higher purity of your gold.
• Through this cook process, your gold should have at least 99.8% purity!
smog
Note the solution color changed after ~30 minutes cooking
• After 30-40 minutes cooking, remove the beaker carefully to an open space to let the solution cool down.
• You should see a brownish color mud-like sediment sitting at the bottom of the beaker. this is the sponge gold!
• Note: this solution is very acid! You have to use special filter paper to filter the solution. Retain the brownish mud
Sponge gold
!! Make sure to rinse the sponge gold
several times and thoroughly with
water to remove residual acid !!
Transfer your sponge gold to filter
paper, and then to a crucible
Sponge gold in a crucible and
ready for refinery
borax
Don’t forget to add borax
to remove other
impurities
1.05 kg
In just 3 hours
We recommend a portable Intermediate Frequency (IF) melting furnace for gold /Ag refinery for SSM gold miners
Au/ Ag smelting crucible
Au/Ag crucible in work
Au/Ag crucible in work
Process capacity: 1-200 kg per run, 20-30 minutes (hot start)
3 Residual Materials and Solution Treatment
follow your local government policy/regulation how to treat the residual materials.
• Eco-goldex E reagent itself has no significant
residual materials need to be treated.
• The residual diluted preg solution after precipitation
may contain Zn2+ ,Pb2+, Fe3+… in the solution. The
solution itself is alkalinic and should be neutralized
before disposal.
• The sulfuric acid wash solution is very acidic and
should be stored and handle properly;
• The acidic solution can be reused in zinc strip
dissolving stage.
• The solution contain a lot of metallic anions(Cu, Ni,
Fe…)
• The residual metal materials can be resold or treated
properly at designated dump site