http://www.goldnscrap.com/index.php/gold
Oddzielenie kwasem solnym i
utlenienie miedzi do chydrochlorku miedzi.
Chlorek
miedzi(II),
CuCl2 – nieorganiczny
związek chemiczny, sól kwasu
solnego imiedzi na
+2 stopniu
utlenienia.
Dihydrat chlorku
miedzi(II) ma postać szmaragdowozielonych kryształów. W tej formie
występuje jako rzadki minerał eriochalcyt.
Otrzymać go można poprzez roztworzeniewęglanu
miedzi(II) w kwasie
solnym.
Bezwodny
chlorek miedzi występuje w postaci brązowego ciała stałego
(minerałtolbachit).
Można go otrzymać spalając miedź w nadmiarze chloru lub
poprzez odwodnienie dihydratu za pomocą stężonego kwasu
siarkowego.
Wodne roztwory chlorku
miedzi(II) są zielone, natomiast w dużym rozcieńczeniu mają barwę
niebieską.
W
obecności nadmiaru jonów chlorkowych tworzy związki kompleksowe:
CuCl3-(czerwony) i CuCl42- (żółty)[4].
Pozostaje złoto, z którego
robimy wodę królewską, a potem z niej wytrącamy złoto.
Film z procesem (3 części):
http://www.youtube.com/watch?v=iCmXLXrAtto
http://www.youtube.com/watch?annotation_id=annotation_2862129675&feature=iv&src_vid=iCmXLXrAtto&v=Hv4CcaTVJqY#t=1m59s
http://www.youtube.com/watch?annotation_id=annotation_2194426549&feature=iv&src_vid=iCmXLXrAtto&v=0yOBdkxk1IE#t=3m39s
Złom elektroniczny
http://www.goldnscrap.com/index.php/scrap-cpu-a-chips
redukcja złota z wody
królewskiej za pomocą SMB ( pirosiarczyn sodu )
http://www.bimberhobby.pl/product.php?id_product=48
Before
explaining how to perform this process, it's probably be better if we
first talk about why use it in the first place.
As
you probably know, there are many reducing agents that will reduce
ionic gold into the metal, such as: SMB (Sodium MetaBisulfite),
copperas (Iron II Sulfate), Sulfur Dioxide Gas (SO2), Hydroquinone,
formaldehyde, hydrazine Sulfate and many more… each has its own
applications and pro's / con's.
The
Oxalic/Oxalate process is very selective for reducing Gold ions and
it is used when very high purity (9999 and higher) Gold is desired.
But due to the nature of this process which involves changing the
acidity of the solution (which may form oxides/hydroxides of base
metals and interfere the process), It is used almost exclusively as a
re-refining process, sometimes referred to as "polishing"
step. When in most cases the Gold will be reduced from an Aqua Regia
solution the 1st time with the use of SMB or SO2 Gas,
get washed and dissolved again, filtered and then reduced the
2nd with Oxalic Acid.
Important:
This is not a Recovery process, this is a final step of Refining.
High
purity Gold of 9999 and higher could be made with simple setup (as
you can view in the video below) that even a hobbyist refiner could
build himself, let alone a proper and well organized laboratory.
Who
needs this process and why?
Research
and processing labs can utilize this process to produce high purity
gold powder to be used either as is or as precursor for preparing
gold based catalysts. Considering the prices charged by large vendors
for precious metals powders, the cost saved by this process is
enormous.
Refiners
would rather use this process for producing small amounts of bullion
gold, amounts too small which doesn't justify setting up an
electrolytic refining cell (Wohlwill process).
The
use of Oxalic acid is also called for as a first refining step when
large amount of PGM's are in solution with the gold, such in the case
of dental gold.
WARNING:
The process described here involves highly corrosive and toxic
chemicals and should only be done outside or in a fume hood. Using
all the safety gear such as Gloves, goggles and a respirator is
mandatory.
The
process:
Gold
powder which had been refined once (dissolved and dropped out of
solution with SMB) was dissolved again by means of Aqua Regia in the
usual manner and filtered through a slow/medium speedFilter
paper
.
This is the main Chloroauric Acid solution we will be working with in
this process.
-
The Gold solution is placed in a high quality borosilicate
beaker or
in a boiling
flask (with
tapered ground joint) and the flask is placed on a hot
plate/mantle on
medium heat. Make sure the solution level will not exceed two thirds
of the flask volume.
-
In another beaker, weight out Oxalic
acid (dehydrate).
The amount of Oxalic acid needed is 1.15
gram for
every 1
gram of
expected gold metal.
This ratio represents a 20% excess in Oxalic acid to ensure all of
the gold is reduced in case there's too much nitric acid left in the
original AR solution.
-
Add the Oxalic acid to the gold solution and turn up the heat of the
hotplate/mantle until a gentle boil has reached. A boiling flask with
tapered ground joints enables you to connect a condenser (Graham)
and an addition
funnel (see
video below), but if you are boiling the solution in an open mouth
beaker, you should cover it with a watch glass. The addition of
reagents will be done through the spout with a pipette.
-
Now prepare a concentrated Sodium
Hydroxide (NaOH)
solution in another beaker. Simply add some NaOH prills/powder and
dissolve it with warm water until no more is dissolved. Either by an
addition funnel or by manually adding it with a pipette, start adding
the NaOH solution to the gold solution. Remember you are adding a
strong base to a strong acid which produce a violent exothermic
reaction, thus the addition must be done SLOWLY
and DROPWISE.
You
may notice some precipitation of brown powder before you even add any
NaOH, but that's just about as far as it will go without pH
adjustments. At this point, you may also notice brown Nitrogen
Dioxide (NO2 – toxic gas) formed in the reaction vessel which is
the result of left over excess Nitric acid from the original Aqua
Regia solution. If the gas cloud formed is very thick, it's probably
a result of way too much Nitric being used and you might want to
consider adding more Oxalic acid and or even start over.
It
is pointless to try and determine just how much NaOH is needed, so
your main indicator for the reaction completion is the color of the
solution. As you add NaOH you will notice more and more
brownish/black suspension being formed that will slowly coagulate.
Keep adding NaOH solution until you can no longer notice the
yellow/orange hue of the solution and the bubbles.
-
Once the process is done and all of the gold had precipitated out,
the solution would normally be either colorless or with just a faint
color of blue/green. If there's a significant coloration to the
solution, then you probably should consider repeating the process all
together. Remember, this process is all about purity.
At this
point, the pH of the now barren mother liquor should fall anywhere
from 0-2.
-
If you used a boiling flask, it is recommended that you now transfer
the powder and the barren solution to an open mouth beaker so it will
be easier to wash. It is suggested that you will allow the gold
suspension to settle to the bottom first. It takes several hours…
Even better, let it to settle overnight.
-
The following day, slowly decant the barren waste solution either
through a filter or into a settling tank to be discarded later.
Washing
cycles are done in the usual manner:
-
Cover the gold powder with Hydrochloric acid (HCl 25-31%) and boil
for few minutes, let cool and settle, now decant and repeat two more
times at least.
-
Cover the gold powder with Ammonia solution (NH4OH 10-25%) and boil
for few minutes, let cool and settle, now decant and repeat one more
time at least.
-
Cover the gold powder with boiling hot Distilled Water
and swirl it around for few minutes, let cool and settle, now decant
and repeat 3-5 times.
You
can combine all of the above washes with the barren mother liquor and
filter it all at once just in case some gold powder slipped through.
Also, keep in mind that sometimes, the HCl washes may dissolve some
of the gold. You can precipitate it later with SMB.
Remember
you must make sure the combined washes solution is acidic, otherwise
you risk forming Ammoniacal gold complexes which can turn explosive.
You can test the solution with a simple pH test strips.
-
After the last distilled water wash is decanted, place the beaker on
a hot plate and set it on low heat until the gold powder is
completely dry. The color of the powder should be very light brown.
-
Depends on what you want to do, you can now use the gold powder as is
or melt your gold in a new and clean crucible.
-
Sit back, have a beer and enjoy your success :)
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