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7,666,371 Method for recovering metal values from metal-containing materials using high temperature pressure leaching

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US007666371B2

(12) United States Patent

Marsden et al.

(10) Patent No.:

(45) Date of Patent:

US 7,666,371 B2

*Feb.23,2010

(54) METHOD FOR RECOVERING METAL

VALUES FROM METAL-CONTAINING

MATERIALS USING HIGH TEMPERATURE

PRESSURE LEACHING

(75) Inventors: John 0 Marsden, Phoenix, AZ (US);

Robert E Brewer, Safford, AZ (US);

Joanna M Robertson, Thatcher, AZ

(US); Wayne W Hazen, Lakewood, CO

(US); Philip Thompson, West Valley

City, UT (US); David R Baughman,

Golden, CO (US)

(73) Assignee: Freeport-McMoran Corporation,

Phoenix, AZ (US)

(60) Provisional application No. 60/220,622, filed on Jul.

25,2000.

(51) Int. Cl.

COIG 3/00 (2006.01)

(52) U.S. Cl. 423/24; 423/26; 423/27;

205/580; 205/581

(58) Field of Classification Search 423/24,

423/26,27, 8, 22, 49, 54, 109, 139,21.5;

205/580,581,589,590,604,605,564,568

See application file for complete search history.

(56) References Cited

U.S. PATENT DOCUMENTS

( *) Notice: Subject to any disclaimer, the term ofthis

patent is extended or adjusted under 35

U.S.c. 154(b) by 81 days.

This patent is subject to a tenninal disclaimer.

5,698,170 A * 12/1997 King 423/24

5,895,633 A * 4/1999 King 423/24

* cited by examiner

Primary Examiner-Steven Bos

(74) Attorney, Agent, or Firm-Snell & Wilmer L.L.P.

(21) Appl. No.: 11/952,726 (57) ABSTRACT

Prior Publication Data

Filed: Dec. 7, 2007

Related U.S. Application Data

Division of application No. 101758,755, filed on Jan.

16,2004, now Pat. No. 7,473,413, which is a continuation

of application No. 09/912,922, filed on Jul. 25,

2001, now Pat. No. 6,680,034.

(22)

(65)

(60)

US 2008/0156656 Al Jul. 3, 2008

The present invention relates generally to a process for recovering

copper and other metal values from metal-containing

materials through pressure leaching operations. In accordance

with the various aspects ofthe present invention, metalcontaining

pregnant leach solutions from pressure leaching

operations need not be significantly diluted to facilitate effective

metal recovery using solvent extraction and electrowinning.

4 Claims, 3 Drawing Sheets

u.s. Patent Feb. 23,2010 Sheet 1 of 3 US 7,666,371 B2

100

)

102

104

~ METAL-BEARING MATERIAL

l'

~ REACTIVE PROCESSING

l'

106 ~",---__M_ET_A_L_R_E_C_O_V_E_R_Y _

FIG. 1

u.s. Patent Feb. 23,2010 Sheet 2 of 3 US 7,666,371 B2

200---i METAL-BEARING MATERIAL I

t

202___( COMMINUTION )

t

204~1 COMMINUTED MATERIAL I t

208

FLOTATION

210~ CONCENTRATED COPPER

SULFIDE-BEARING MATERIAL

212----( LIGHT REGRIND )

t

214~1 PRODUCT SLURRY I t

220----( PRESSURE LEACHING )

t

222~1 PRODUCT SLURRY I t

224___( FLASH )

t 282

226~1 FLASHED PRODUCT SLURRY I 280

( SM~LTER ) • 228 LIQUID/SOLID SEPARATION

METALS

L RECOVERY

TO FIG 2B 284

FIG.2A

230

FROM FIG 2A i

COPPER-CONTAINING

SOLUTION -----------------------------------------~

TO FIG 2A

~

7J).

•

~

~

~

~=~

232 CHEMICAL pH ADJUST

268

AGITATED TANK LEACH

rFJ =('

D

(..'D...

(.H

o....

(.H

""f'j

('D

?'

N

(.H

~

No

.... o

d

rJl

......:J

0-.,

0'1

0'1

W

......:J

="""'" N

254

""" /262 l HEAP LEACH )

FIG. 28

IIII

I

IIII

,,,

,

+ t

236

266

264

CHEMICAL pH ADJUST

US 7,666,371 B2

2

incomplete, resulting in the formation of ferrous sulfate, an

undesirable reaction by-product.

In high temperature pressure leaching, the sulfur contained

in the metal-bearing material (e.g., concentrate) typically is

converted to sulfate. In connection with such pressure leaching

processing operations, the copper typically is recovered

from the resulting solution by solvent extraction and electrowinning

techniques to provide a cathode copper product of

high purity.

In solvent extraction (or solution extraction or liquid ion

exchange, as it is sometimes called), the pregnant leach solution

typically is mixed with an organic solvent (i.e., an extractant),

which selectively removes the copper from the pregnant

leach solution. The copper-loaded extractant is then mixed

15 with an aqueous acid solution, which strips the copper from

the extractant, producing a solution stream suitable for electrowinning.

This resultant solution stream is highly concentrated

in copper and relatively pure, and typically is processed

into high quality cathode copper in an electrowinning circuit.

In general, electrowinning of copper consists of the electrolytic

deposition (sometimes called "plating") of copper

onto a cathode and the evolution of oxygen at an anode. In a

simple design of an exemplary electrowinning unit, a set of

cathodes and anodes are set in a reaction chamber containing

25 the copper-containing electrolyte. When the unit is energized,

copper ions are reduced onto the cathode (i.e., plated). Plating

ofcopper typically occurs on copper starter sheets or stainless

steel blanks. Anodes are quasi-inert in the electrolyte and

provide a surface for oxygen evolution. The copper plates

30 produced by the electrowinning unit can be in excess of99.99

percent pure.

Purification of copper from the pregnant leach solution by

solvent extraction has proven to be a successful means of

providing a concentrated copper solution suitable for elec-

35 trowinning of highly pure copper metal. However, prior art

teachings suggest the importance of ensuring that the acid

concentration of the pregnant leach solution is appropriately

controlled, often through neutralization, such as through the

use of lime or acid-consuming ore.

Still others have recognized that the use oflime to neutralize

the acid in the solution not only increases operating costs

due to lime consumption but also may result in the formation

of a low pulp density slurry, thus tending to make it more

difficult to recover the copper from that slurry. In response,

45 Placer Dome, Inc., ofVancouver, British Columbia, Canada,

has proposed in, for example, U.S. Pat. Nos. 5,698,170 and

5,895,633 methods to recover copper from copper-containing

materials, especially copper from copper sulfides such as

chalcopyrite, wherein a copper-containing solution contain-

50 ing an acid is contacted, that is, diluted, with an aqueous

diluent containing no more than about 5 grams/liter acid to

yield a diluted copper-containing solution having an acid

concentration ranging from about 2 to about 8 grams/liter

prior to the step of solvent extracting the copper from the

55 diluted copper-containing solution. In their patents, Placer

Dome requires the significant use of a diluting solution to

lower acid levels in the copper-containing solution sufficiently

for favorable equilibrium conditions during solvent

extraction, which technique Placer Dome suggests signifi-

60 cantly reduces copper losses relative to many existing processes

in which neutralization of the acid in the solution

before solvent extraction is employed.

To achieve these results, Placer Dome teaches that the

desired acid concentration ranges can be obtained when a

65 sufficient amount of diluting solution is contacted with the

copper-containing solution to yield the diluted copper-containing

solution. Specifically, Placer Dome teaches that the

(1)

FIELD OF INVENTION

CROSS-REFERENCE TO RELATED

APPLICATIONS

BACKGROUND OF THE INVENTION

1

METHOD FOR RECOVERING METAL

VALUES FROM METAL-CONTAINING

MATERIALS USING HIGH TEMPERATURE

PRESSURE LEACHING

The present invention relates generally to a process for

recovering copper and other metal values from metal-containing

materials, and more specifically, to a process for

recovering copper and other metal values from metal-containing

materials using high temperature pressure leaching

processes.

This application is a divisional application of U.S. patent

application Ser. No. 10/758,755 entitled "Method for Recov- 10

ering Metal Values from Metal-Containing Materials Using

High Temperature Pressure Leaching" filed on Jan. 16,2004

which is a continuation application ofU.S. patent application

Ser. No. 091912,922, entitled "Method for Recovering Metal

Values from Metal-Containing Materials Using High Temperature

Pressure Leaching," filed Jul. 25, 2001, now U.S.

Pat. No. 6,680,034, which claims priority to U.S. Provisional

Patent Application Ser. No. 60/220,622 entitled "Methods for

Recovering Copper and Other Metal. Values from Copper

Sulfide Concentrate Using High Temperature Pressure Oxi- 20

dation" filed on Jul. 25, 2000, all ofwhich are incorporated by

reference herein.

Smelting is one approach for recovering a metal, such as

copper, from a metal-bearing sulfide material. However, due

to the high cost of smelting, the copper sulfide minerals in an

ore body typically are first concentrated by flotation techniques

to provide a smaller volume for smelting. The concentrate

is then shipped to a smelter, which processes the con- 40

centrate pyrometallurgically at high temperatures to form a

crude copper product that is subsequently refined to a highly

pure metal.

The recovery of copper from copper sulfide concentrates

using pressure leaching has proven to be a potentially economically

attractive alternative to smelting. Pressure leaching

operations generally produce less fugitive emissions than

smelting operations, and thus, environmental benefits may be

realized. Further, pressure leaching circuits may be more

cost-effectively constructed on-site at a concentrator, eliminating

the expense associated with concentrate transportation

that smelting operations may require. Further, any by-product

acid produced in the pressure leaching circuit may be able to

be used in adjacent heap leaching operations, thus offsetting

some of the costs associated with purchased acid.

The mechanism by which pressure leaching processes

effectuate the release ofcopper from sulfide mineral matrices,

such as chalcopyrite, is generally dependent on temperature,

oxygen availability, and process chemistry. In high temperature

pressure leaching processes, that is, pressure leaching

processes operating above about 2150 c., the dominant oxidation

reaction is believed to be as follows:

If insufficient oxygen is present in the process vessel, the

conversion of iron to hematite (Fe20 3 ) generally will be

3

US 7,666,371 B2

4

ratio ofthe volume of copper-containing solution to the volume

ofdiluting solution must range from about I: 10 to about

I :500. In this manner, the acid generated in pressure leaching

is neutralized after, and preferably not before, solvent extraction

and electrowinning.

While Placer Dome's patented process is usable in many

situations, in cases where it is desirable to reduce operating

costs and/or the metal-bearing ore at a particular site does not

warrant such conditions, it would be desirable to obtain high

metal recovery in processes where such dilution is not

required.

SUMMARY OF THE INVENTION

While the way in which the present invention provides

these advantages over the prior art is described in greater

detail hereinbelow, in general, the process for recovering

copper and other metal values from a metal-bearing material

is improved, according to various aspects of the present

invention, in that the pressure leach solution need not be

significantly diluted before the copper and/or other metal

values are recovered, for example, through solvent extraction,

electrowinning, or other processes. In this manner, capital and

operating costs can be reduced without sacrificing the extraction

of copper or other metals.

Thus, in accordance with an exemplary embodiment ofthe

present invention, a process for recovering copper from a

copper-containing material generally includes the steps of: (i)

providing a feed stream containing copper-containing material;

(ii) pressure leaching the copper-containing feed stream

to yield a copper-containing solution; and (iii) recovering

cathode copper from the copper-containing solution using

solvent extraction and electrowinning without significantly

diluting the copper-containing solution. In general, recovery

processes in accordance with the present invention yield high

copper recovery, for example in excess of 98%, while at the

same time yielding various other important benefits.

BRIEF DESCRIPTION OF THE DRAWINGS

The subject matter of the present invention is particularly

pointed out and distinctly claimed in the concluding portion

of the specification. A more complete understanding of the

present invention, however, may best be obtained by referring

to the detailed description and claims when considered in

connection with the drawing figures, wherein like numerals

denote like elements and wherein:

FIG. 1 illustrates a general flow diagram of a metal recovery

process in accordance with one general embodiment of

the present invention;

FIG. 2A illustrates a more detailed flow diagram ofa metal

recovery process in accordance with one exemplary embodiment

of the present invention; and,

FIG. 2B illustrates further aspects of the metal recovery

process of FIG. 2A.

DETAILED DESCRIPTION

The present invention exhibits significant advancements

over prior art processes, particularly with regard to metal

recovery ratios and process cost advantages. Moreover, existing

metal recovery processes that utilize a conventional atmospheric

or pressure leaching/solvent extraction/electrowinning

process sequence may, in many instances, be easily

retrofitted to exploit the many commercial benefits the

present invention provides.

Referring to FIG. 1, in accordance with various aspects of

the present invention, a metal-bearing material 102 is provided

for processing in accordance with metal recovery process

100. Metal-bearing material 102 may be an ore, a concentrate,

or any other material from which metal values may

be recovered. Metal values such as, for example, copper, gold,

silver, zinc, platinum group metals, nickel, cobalt, molybdenum,

rhenium, uranium, rare earth metals, and the like may be

recovered from metal-bearing materials in accordance with

10 various embodiments of the present invention. Various

aspects and embodiments of the present invention, however,

prove especially advantageous in connection with the recovery

of copper from copper sulfide concentrates and/or ores,

such as, for example, chalcopyrite (CuFeS2 ), chalcocite

15 (Cu2 S), bornite (CusFeS4 ), and covellite (CuS). Thus, metalbearing

material 102 preferably is a copper ore or concentrate,

and most preferably, is a copper sulfide ore or concentrate.

Metal-bearing material 102 may be prepared for metal

20 recovery processing in any manner that enables the conditions

of metal-bearing material102-such as, for example,

composition and component concentration-to be suitable

for the chosen processing method, as such conditions may

affect the overall effectiveness and efficiency of processing

25 operations. Desired composition and component concentration

parameters can be achieved through a variety ofchemical

and/or physical processing stages, the choice of which will

depend upon the operating parameters ofthe chosen processing

scheme, equipment cost and material specifications. For

30 example, as discussed in some detail hereinbelow, metalbearing

material 102 may undergo comminution, flotation,

blending, and/or slurry formation, as well as chemical and/or

physical conditioning.

With continued reference to FIG. 1, after metal-bearing

35 material 102 has been suitably prepared, metal-bearing material

is subjected to reactive processing (step 104) to put a

metal value or values in metal-bearing material 102 in a

condition such that they may be subjected to later metal

recovery steps, namely metal recovery step 106. For example,

40 exemplary suitable processes include reactive processes that

tend to liberate the desired metal value or values in the metal

bearing material 102 from the metal-bearing material 102. In

accordance with a preferred embodiment of the present

invention, processing step 104 comprises pressure leaching,

45 preferably, high temperature pressure leaching. As used

herein, the term "pressure leaching" refers to a metal recovery

process in which material is contacted with an acidic solution

and oxygen under conditions of elevated temperature and

pressure. In accordance with various aspects of the present

50 invention, processing step 104 may comprise any type of

pressure leaching process.

As previously briefly noted, pressure leaching processes

are generally dependent upon, among other things, temperature,

oxygen availability, and process chemistry. While vari-

55 ous parameters for each may be utilized, in accordance with

preferred aspects of the present invention, the temperature

during pressure leaching preferably is maintained in the range

of about 170° C. to about 235° c., most preferably in the

range from about 200° C. to about 230° c., and optimally on

60 the order of about 225° C.

To maintain the temperature in this desired range, a cooling

liquid may be employed. As will be appreciated, pressure

leaching of many metal sulfides tends to be an exothermic

reaction, and the heat generated is generally more than that

65 required to heat the feed slurry to the desired operating temperature.

Excess heat may be removed and the desired operating

temperature maintained by contacting cooling liquid

US 7,666,371 B2

5 6

due to the lower volume of fluids which need to be handled

within metal recovery process 100.

Referring now to FIGS. 2A and 2B, a further exemplary

embodiment of the present invention is illustrated. In accordance

with this embodiment, a metal-bearing material 200,

preferably a copper-bearing material, is comminuted in step

202 to form a comminuted material 204. Preferably, metalbearing

material 200 comprises a copper sulfide-bearing

material.

Preferably, comminuted material 204 is subjected to froth

flotation (step 208) to separate copper sulfide-bearing materials

from gangue minerals. The flotation concentrate, namely

the concentrated copper sulfide-bearing material 210, is

obtained and preferably contains copper and other metals.

Further comminution ofconcentrated copper sulfide-bearing

material 210 may be necessary to yield a desired size

distribution for pressure leaching. As will be appreciated,

increasing the fineness of material 210 tends to increase the

reaction rate during pressure leaching, and thus may permit

the use of smaller, more economical pressure leaching apparatus.

Accordingly, material 210 has a particle size of about

80% passing less than about 150 microns, more preferably

less than about 100 microns, and optimally between about 30

to about 75 microns. In some instances, in order to achieve the

optimal particle size, or to expose fresh surfaces or to break up

lumps, a regrinding step 212 may be employed. During

regrinding step 212, solution (e.g., feed slurry 206 or otherwise)

may be added to the flotation concentrate 210 to facilitate

the grinding process.A product slurry 214 is then formed,

preferably with the addition of, for example, sulfuric acid,

dispersants, and the like prior to high temperature pressure

leaching (step 220). Preferably, product slurry 214 has less

than about 50% solids by weight.

Product slurry 214 is next subjected to high temperature

pressure leaching (step 220), preferably at a temperature in

the range of about 210° C. to about 235° C. in a sealed,

agitated, multi-compartment pressure leaching vessel with

oxygen overpressure of at least about 70 psig for about 1-3

hours. During pressure leaching step 220, oxygen preferably

is added continuously to the pressure leaching vessel to maintain

the oxygen overpressure optimal for the desired chemical

reactions to proceed That is, sufficient oxygen is suitably

injected to preferably maintain an oxygen partial pressure in

the pressure leaching vessel ranging from about 50 to about

45 300 psig, and more preferably in the range of about 60 to

about 150 psig. The total pressure in the sealed pressure

leaching vessel is superatmospheric, and can range from

about 300 to about 750 psig, and is preferably in the range of

about 400 to about 600 psig. A product slurry 222 is obtained

in a conventional manner therefrom.

Product slurry 222 may be flashed (step 224) to release

pressure and evaporatively cool product slurry 222 through

release of steam to form a flashed product slurry 226. Flashed

product slurry 226 preferably thereafter has a temperature

ranging from about 85° C. to about 100° C. Solution recovered

from steam generated from flashing step 224 may be

cooled and used as process make-up solution (not shown).

In accordance with further aspects of this preferred

embodiment, after product slurry 222 has been subjected to

atmospheric flashing (step 224) using, for example, a flash

tank, to achieve approximately ambient conditions of pressure

and temperature, flashed product slurry 226 may be

further conditioned in preparation for later metal-value recovery

steps. In some cases, use of a heat exchanger may be

advantageous to cool the slurry such that solid-liquid phase

separation may take place. Preferably, one or more solidliquid

phase separation stages (step 228) may be used to

with the feed slurry in the reactor vessel. The cooling liquid

can be recycled liquid phase from the product slurry, neutralized

raffinate solution, fresh make-up water, or mixtures

thereof, or may be provided by any other suitable source. The

amount ofcooling liquid added during pressure leaching will

vary according to the amount of sulfide minerals reacted (and

thus the heat generated by the pressure leaching reaction).

The duration of pressure leaching in any particular application

depends upon a number of factors, including, for

example, the characteristics ofthe metal-containing material 10

and the pressure leaching process pressure and temperature.

Preferably, the duration of pressure leaching in accordance

with various aspects of the present invention ranges from

about less than I hour to about 3 hours, and optimally is on the

order of about forty-five (45) to ninety (90) minutes. While 15

any reactor vessel for pressure leaching may be used, preferably

an agitated, multiple-compartment pressure leaching

vessel is employed.

In accordance with various aspects of the present invention,

processing step 104 via pressure leaching of metal- 20

bearing material 104 produces a product slurry having a relative

y high acid and metals content, and is characterized by

high metal (e.g., copper) recoveries through metal recovery

step 106. For example, no less than about 98% of the metal

(e.g., copper) in the preferred chalcopyrite and other copper 25

sulfides can generally be recovered through pressure oxidation

utilizing the above-described conditions.

Contrary to prior art processes, such as for example the

aforementioned Placer Dome processes, where significant

amounts of diluting solution are combined with the pressure 30

leaching liquor to reduce the acid concentration, in accordance

with various aspects ofthe present invention, dilution is

not used, or if used, relatively low dilution ratios are used. In

cases where low dilution of the pressure leaching product

slurry is employed, dilution ratios of less than about I: 10 35

metal containing solution to make-up solution are employed.

Preferably, dilution is conducted such that the dilution ratio is

on the order of between about 1:4 and about 1:8 of metalcontaining

solution to make-up solution.

40

With continued reference to FIG. 1, in accordance with

various aspects ofthe present invention, metal recovery step

106 preferably comprises conventional solvent extraction and

electrowinning (SX/EW). It should be appreciated, however,

that other metal recovery processes may be used.

Where metal recovery step 106 comprises SX/EW, such

processing preferably is conducted in a conventional manner.

As such, suitable extraction reagents should be employed.

Preferably, such extraction reagents include aldoxime,

aldoxime/ketoxime mixtures and/or modified aldoximes. For 50

example, particularly preferred solvent extraction reagents

include LIX reagents, such as, for example, LIX 622N, which

comprises a mixture of 5-dodecylsalicylaldoxime and tridecanol

in a high flash point hydrocarbon diluent, available

from Cognis Corporation; LIX 984, also available from Cog- 55

nis Corporation, which is a mixture of 5-dodecylsalicylaldoxime

and 2-hydroxy-5-nonylacetophenoneoxime in a high

flash point hydrocarbon diluent; or M-5774, available from

Avecia, an Acorga™ solvent extraction reagent, which comprises

a modified aldoxime (5-nonyl salicylaldoxime). Other 60

suitable solvent extraction reagents, however, may be

employed.

As will be appreciated by the disclosure set forth herein,

metal recovery process 100 enables various advantages over

recovery processes wherein more significant dilution is 65

required. For example, by using relatively low dilution ratios,

lower operation costs potentially can be obtained, primarily

US 7,666,371 B2

7 8

ditions are selected such that the solvent extraction reagents

collect the copper in copper-containing solution 230. The

copper-bearing reagents are then subjected to more acidic

conditions to shift the equilibrium conditions to cause the

copper to be exchanged for the acid in a highly acidic acid

stripping solution (not shown). Various process stages may be

used, as necessary, to provide a suitable stream to feed the

electrowinning process and to yield a substantially barren

solvent for re-use in the extraction process. During solvent

10 extraction 252, copper from copper-containing solution 230

may be loaded selectively onto an organic chelating agent,

such as the aforementioned aldoximes or aldoxime/ketoxime

blends. Preferably, an extraction reagent, such as LIX 984 or

Acorga® M-5774, is dissolved in an organic diluent to result

15 in the extraction of copper from metal-containing solution

which can be recovered through conventional electrowinning

(step 254) to yield the desired metal product 256. As previously

mentioned, LIX 984 is a mixture of 5-dodecylsalicylaldoxime

and 2-hydroxy-5-nonylacetophenone oxime in a

20 high flash point hydrocarbon diluent, which forms complexes

with various metal cations, such as Cu2

+. Other solvent

extraction reagents may be used in accordance with various

aspects of the present invention. Such extraction reagents

should, however, be selected to facilitate suitable extraction

25 and subsequent stripping operations.

Solvent extraction step 252 and electrowinning step 254

may also involve various solvent stripping and recycle operations

(both ofwhich are not shown) which can be operated in

a conventional manner. Preferably, no less than about 98% of

30 the copper in copper-containing solution 230 is recovered as

cathode copper product 256 by solvent extraction 252 and

electrowinning 254.

With continued reference to FIG. 2B, electrowinning step

35 254 also preferably proceeds in a conventional manner to

yield a pure, cathode copper product 256. In accordance with

the various aspects of this embodiment of the present invention,

a high-quality, uniformly plated cathode copper product

256 may be realized without subjecting copper-containing

40 solution 230 to significant dilution prior to solvent extraction.

As those skilled in the art will appreciate, a variety ofmethods

and apparatus are available for the electrowinning of copper

and other metal values, any ofwhich may be suitably used in

accordance with this embodiment of the present invention.

Raffinate solution 260 from solvent-extraction step 252

may be used in a number of ways. For example, all or a

portion ofraffinate 260 may be used in heap leaching operations

262. In some cases, in accordance with various aspects

of this embodiment of the present invention, use of raffinate

50 260 in heap leaching operations 262 may be desirable inasmuch

as raffinate 260 may have higher acid levels and in some

cases thereby more advantageously affecting heap leaching

operations 262. Alternatively, the pH ofraffinate solution 260

may be chemically adjusted, such as is shown in step 264 and

55 the resulting product sent to impoundment (step 266). In

accordance with yet another aspect ofthis embodiment ofthe

present invention, raffinate solution 260 may be agitated in a

tank leach operation (step 268).

With reference again to FIG. 2A, ifthe metal content ofthe

60 washed solids, that is residue 280, from solid-liquid separation

step 228 is sufficiently high to warrant further processing,

the metals contained therein may be recovered through conventional

means such as, for example, through smelting (step

282) or established precious metals recovery processing (step

65 284). If, however, the metals content ofresidue 280 is too low

to justifY further treatment, the residue may be sent to an

impoundment area (step 286).

separate solubilized metal solution from solid particles. This

may be accomplished in any conventional manner, including

use of filtration systems, counter-current decantation (CCD)

circuits, thickeners, and the like. A variety offactors, such as

the process material balance, environmental regulations, residue

composition, economic considerations, and the like, may

affect the decision whether to employ a CCD circuit, a thickener,

a filter, or any other suitable device in a solid-liquid

separation apparatus. However, it should be appreciated that

any technique of conditioning flashed product slurry 226 for

later metal value recovery is within the scope of the present

invention. Preferably, flashed product slurry 226 is subjected

to solid-liquid phase separation (step 228) to yield a resultant

liquid phase copper-containing solution 230 and a solid phase

residue 280.

Flashed product slurry 226 is suitably subjected to solidliquid

phase separation (step 228), by multiple stages of

counter current decantation (CCD) washing in thickeners.

Wash solution and a suitable flocculent may be added as

desired during step 228. In accordance with one alternative

aspect of this embodiment of the present invention, flashed

product slurry 226 may be thickened in a primary thickener to

recover approximately 95% or more of the soluble copper in

a high grade pregnant leach solution. In this case, primary

thickener underflow then proceeds to a multiple-stage CCD

washing circuit, and wash solution and a suitable flocculent

may be added as required (not illustrated).

Referring now to FIG. 2B, in order to optimize solution

extraction ofthe copper, the pH ofcopper-containing solution

230 from solid-liquid phase separation step 228, in accordance

with various aspects ofthis embodiment ofthe present

invention, preferably is adjusted to a pH of about 1 to about

2.2, more preferably to apH ofabout 1.2 to about 2.0, and still

more preferably to a pH of about 1.4 to about 1.8. This

adjustment may be accomplished in a variety of mauners. In

accordance with one aspect of the present invention, coppercontaining

solution 230 is subjected to a chemical pH adjustment

step 232, which optionally can be followed by further

solid-liquid separation (step 234) to yield a final metal-containing

solution 236 for solvent extraction. In such case, the

residue 238 from step 234 can be impounded (step 240) or

otherwise disposed of.

Alternatively, or in combination with the method described

above, the pH of copper-containing solution 230 may be

adjusted through dilution (step 250). In contradistinction to 45

the prior art methods that rely on significant dilution, in

accordance with the present invention, when dilution is

employed, low dilution ratios ofmake-up solution to coppercontaining

solution 230 are used. Dilution step 250 may be

accomplished by dilution with process solution, fresh water

or any other suitable liquid vehicle at dilution ratios of copper-

bearing solution to make-up solution of less than about

1: 10, and more preferably on the order of between about 1:4

to about 1:8. Once the pH of the copper-containing solution

230 has been appropriately adjusted, metal recovery preferably

is achieved by solvent extraction (step 252), ifnecessary,

using relatively high concentrations of extractants in the

organic diluent, followed by electrowinning (step 254).

In accordance with the present invention, in some instances

copper-containing solution may be directly electrowon. Ifthe

properties of solution 230 permit, electrowinning step 254

may be performed directly (that is, without first subjecting

solution 230 to solvent extraction).

When appropriate, solvent extraction, in accordance with

preferred aspects ofthis embodiment ofthe present invention,

is conducted prior to electrowinning and is conducted in a

generally conventional fashion. Typically, equilibrium con9

US 7,666,371 B2

10

The present invention has been described above with reference

to various exemplary embodiments. It should be

appreciated that the particular embodiments shown and

described herein are illustrative of the invention and not

intended to limit in any way the scope ofthe invention as set

forth in the appended claims. For example, although reference

has been made throughout this disclosure primarily to

copper recovery, it is intended that the invention also be

applicable to the recovery of other metal values.

What is claimed is:

1. A metal recovery process comprising the steps of:

a) providing a metal-bearing material in a slurry fonn;

b) subjecting said slurry to flotation to fonn a concentrated

metal-bearing material;

c) pressure leaching said concentrated metal-bearing material

at a temperature in the range of about 170° C. to

about 235° C. in an oxygen-containing atmosphere in a

pressure leaching vessel to fonn a product slurry;

d) separating said product slurry into a metal-bearing solution

and a solids-containing residue;

e) adjusting the pH of said metal-bearing solution to a pH

ofless than about 2.2 by combining said metal-bearing

solution with a make-up diluting solution to yield a

pH-adjusted metal-bearing solution, wherein the ratio of

said metal-bearing solution to said make-up diluting

solution is in the range of from about 1:4 to about 1:8;

f) solvent extracting and electrowinning said pH-adjusted

metal-bearing solution to yield an acid-containing raffinate

solution;

g) applying said acid-containing raffinate solution in a heap

leaching operation.

2. The process of claim 1 wherein said step of providing a

metal-bearing material comprises providing a copper con10

taining material.

3. The process of claim 2 wherein said step of solvent

extracting and electrowinning comprises solvent extracting

and electrowinning said pH-adjusted copper containing solution

to yield an acid containing raffinate solution and copper

15 cathode.

4. The process ofclaim 3, wherein said step ofadjusting the

pH of said metal-bearing solution comprises combining said

metal-bearing solution with a make-up diluting solution to

yield a pH-adjusted metal-bearing solution wherein the ratio

20 of said metal-bearing solution to said make-up diluting solution

is in the range of from about 1:4 to about 1:8 and the pH

of said pH-adjusted metal-bearing solution is from about 1.4

to about 1.8.

* * * * *

w Roma�v�sr�^D��areast-font-family: HiddenHorzOCR'>Plaster of Paris, 1% 70 No Change

 

Pitch Coal, 1% 76 12% Decrease

Na3P04012H20,1% 75 10% Decrease

Toner

1Higher value indicates less dust.

2Untreated raw coal light transmittance was 68% at 60 sec. Less than 5%

change after treatment was indicated as no change.

Dust Suppression

Agent

48- by 200-mesh

PRB Coal

Plaster of Paris

Na3P04012H20

11

US 7,208,023 B2

12

imparting a second electrostatic charge to the first fraction,

wherein the second electrostatic charge is opposite

the first electrostatic charge; and

mixing the first and second fractions.

2. The method, as claimed in claim 1, wherein the first

fraction is less than about 20% by weight of the total bulk

material.

3. The method, as claimed in claim 1, further comprising

reducing the particle size of the first fraction before the step

of imparting. 10

4. The method, as claimed in claim 1, wherein the step of

imparting comprises,

placing the first fraction in an electrostatic field of at least

about I kV/cm;

raising the temperature of the first fraction in the electro- 15

static field to between about 30° C. and about 300° c.;

and

maintaining the first fraction in the electrostatic field and

at the raised temperature for between about 5 minutes

and about 600 minutes. 20

5. The method, as claimed in claim 1, wherein the step of

imparting comprises treating the first fraction with a corona

discharge.

6. The method, as claimed in claim 1, wherein the bulk

material is a bulk fuel material. 25

7. The method, as claimed in claim 1, wherein the bulk

material is coal selected from the group consisting of

bituminous coal, subbituminous coal and lignite.

8. A method of treating a solid particulate material,

comprising: 30

a. separating the material into first and second fractions,

wherein the first fraction comprises less than about

10% of the total material;

b. reducing the particle size of the first fraction;

c. placing the first fraction in an electrostatic field of at

least about I kV/cm;

d. raising the temperature of the first fraction in the

electrostatic field to between about 30° C. and about

300° c.;

e. maintaining the first fraction in the electrostatic field

and at the raised temperature for between about 5

minutes and about 600 minutes;

f. cooling the first fraction to ambient temperature while

maintaining the electrostatic field;

g. removing the first fraction from the electrostatic field

when the material temperature is at ambient temperature;

and

h. mixing the first and second fractions.

9. A method to control dusting in a bulk material having

a first electrostatic charge, comprising:

placing a charge control agent in an electrostatic field of

at least about I kV/cm;

raising the temperature of the charge control agent in the

electrostatic field to between about 30° C. and about

300° c.;

maintaining the charge control agent in the electrostatic

field and at the raised temperature for between about 5

minutes and about 600 minutes; and,

mixing the bulk material with a charge control agent

having a second electrostatic charge opposite the first

electrostatic charge, wherein the amount of the charge

control agent is between about 0.1% and about 20% by

weight of the bulk material.

* * * * *

fam�� H�^D��OCR'>a) providing a feed stream comprising an elemental

 

sulfur-bearing material and a dispersant wherein said

dispersant comprises at least one of a surfactant,

ground sand, mineral processing tailings, or combination

thereof, and wherein said elemental sulfur-bearing 25

material comprises an elemental sulfur-containing residue

from a pressure leaching operation carried out at a

temperature in the range of about 1400 C. to about 1800

c.;

b) pressure leaching at least a portion of said feed stream 30

at a temperature in the range of about 2200 C. to about

275 0 C. in an oxygen-containing atmosphere in an

agitated multiple-compartment pressure leaching vessel

to form a product slurry comprising a sulfuric acid

solution;

c) separating at least a portion of said sulfuric acid 35

solution from said product slurry to yield a residue;

d) recovering at least one metal value from said residue.

2. The process of claim 1 wherein said step of recovering

at least one metal value from said residue comprises recovering

at least one precious metal from said residue.

3. The process of claim 1 wherein said step of pressure

leaching at least a portion of said feed stream comprises

pressure leaching at temperatures above about 2350 C.

4. A treatment process comprising the steps of:

a) providing a feed stream comprising an elemental 45

sulfur-bearing material-wherein said elemental sulfurbearing

material comprises an elemental sulfur-containing

residue from a pressure leaching operation

carried out at a temperature in the range of about 1400

C. to about 1800 c.; 50

b) pressure leaching at least a portion of said feed stream

in the presence of a dispersant wherein said dispersant

comprises at least one of a surfactant, ground sand,

mineral processing tailings, or combination thereof, at

a temperature in the range of about 2200 C. to about

275 0 C. in an oxygen-containing atmosphere in an 55

agitated multiple-compartment pressure leaching vessel

to form a product slurry comprising a sulfuric acid

solution;

c) separating at least a portion of said sulfuric acid

solution from said product slurry to yield a residue;

d) recovering at least one metal value from said residue.

5. The process of claim 4 wherein said step of recovering

at least one metal value from said residue comprises recovering

at least one precious metal from said residue.

6. A process for recovering metal values from an elemental

sulfur-bearing solid residue of a pressure leaching pro

='fo�`�ie�^D��nt-family:"Times New Roman","serif";mso-fareast-font-family: HiddenHorzOCR'>at a temperature in the range of about 220° C. to

 

about 275° C. in an oxygen-containing atmosphere in

an, agitated multiple-compartment pressure leaching

vessel to form a product slurry comprising a sulfuric

acid solution;

c) adding a dispersant during said pressure leaching step;

d) separating at least a portion of said sulfuric acid

solution from said product slurry to yield a solid

residue;

e) recovering at least one precious metal value from said

solid residue.

17. The process of claim 16 wherein said step of providing

an elemental sulfur-bearing material comprises providing an

5 elemental sulfur-containing residue from a pressure leaching

operation carried out at a temperature in the range of about

140° C. to about 180° C.

18. The process of claim 16 wherein said step of pressure

10 leaching comprises pressure leaching at a temperature of

about 235° C.

* * * * *


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