New Era

Pressure Hydrometallurgy
8.Laboratory Autoclaves
for Hydrometallurgical Research

Fathi Habashi
Department of Mining, Metallurgical, and Materials Engineering

Laval University, Quebec City,Canada

Fathi.Habashi@arul.ulaval.ca

Laboratory autoclaves for hydrometallurgical investigations are available in a

variety of sizes, models, and materials of
construction.
They vary in sizes from 25 mL to 2 liters for
laboratory studies and 5 to 50 gallons for
pilot plant work.

 They are essential tools for studying dissolution of

minerals at high temperature and pressure, and
hydrothermal precipitation reactions.
They can be equipped with gas inlet tube, cooling
coil, agitators, etc. They may also incorporate an
interchangeable chemically resistant lining
covering all interior surfaces.
Reactor operates up to 20 000 kPa and 250C.

AGITATED AUTOCLAVES
Agitated autoclaves are composed of a
container, a head, and an agitation system
all inserted in an oven with a temperature
controller.
Cooling coils and sampling tubes may also
be installed but other accessories such as a
safety valve and a vent are necessary.

Agitation

A stirrer drive with a pulley

High torque magnetic drives

High-torque magnetic drives

Magnetic drives are
magnetically coupled systems
use high energy permanent
magnets in sealed enclosures
with no rotating seals to
eliminate the troublesome
leakage problems which
sometimes arise with a packing
gland in severe service,
permitting long continuous runs
at high pressure with little or no
attention to the gland and drive.
A water cooling sleeve attached
to each drive protects the
components from excessive
temperatures arising from the
reactor.

 The stirring shaft rotates in

PTFE bearings and is rigidly
connected to the internal
magnet. Both of these
components are inside the
pressure vessel.
The external magnet is
supported by bearings and
rotates outside the pressure
chamber. As a result of the
optimally utilized lines of force
of the magnetic field, the
internal magnet rotates in
synchronization with the
external magnet.

Assembled Units

Using a pulley stirrer

Using magnetic stirrer

Autoclave Engineers

Autoclave Engineers specializes in pilot

plant size autoclaves.

The Zipper Clave reactor

The Zipper Clave reactor by Autoclave Engineers
is manufactured in , 1, 2 and 4 liters.
It is claimed to be the fastest, easiest opening and
closing pressure vessel ever offered. No bolts to
torque, no clamps or rings. Instead, just raise the
body and push the spring section to close the
cover.
To open, just pull the spring and lower the body.
Cover remains stationary, so there is no need to
break cover connections.

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 Closure is effected by resilient spring member (The

Zipper) inserted through a circumferential groove in body
and cover. Simply release the safety sleeve and pull the
Zipper to remove the cover. A quick release/safety lock
and cover safety device are provided to ensure that the
spring is fully inserted.
The maximum pressure and temperature at which any
reactor can be used will depend upon the design of the
vessel and its material of construction since all materials
lose strength at elevated temperatures. Autoclave design is
under continuous improvement for better reliability.

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Berghof
autoclaves
Berghof developed a
special conical
flange closure which
assures uniform
tightening and a
reliable seal by
means of two simple
hand screw.

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Engineering Aspects
Valves
Accessories

Valves
Valves used in autoclaves have nonrotating stems to minimize leakage.
Because stem tip does not rotate on
contact with body seat, the 2-piece NonRotating Stems designed by Autoclave
Engineers eliminate the galling and
scoring of stem and seat usually
associated with conventional rotating stem
valves. Thus, one of the major causes of
valve leakage and failure is avoided.

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Accessories
The safety head houses the rupture disc. To
prevent the action of corroding vapors, the
discs can be coated on one or both sides
with Teflon or gold. Such coatings and
lining increase the minimum rupture
ratings available in a given disc.
A dial thermometer.
A connecting tube.

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Acid Digestion Bombs

The acid digestion bombs are small non-

agitated autoclaves that are meant for

conducting rapid semi-quantitative tests at
high temperature and pressure.
They may be equipped with a heating
mantle but more often they can be heated in
a laboratory oven thus the temperature
inside the bomb is not precisely known.

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Parr bombs

Parr bombs contain a Teflon cup and are

available in two sizes: 25 mL and 125 mL.
They can be heated in an oven.
The 125-mL bomb has a safety rupture disc built
into the head which protects the bomb and the
operator from the hazards of an unexpected
explosion from accidental overloading.
Should the pressure in the bomb accidentally
reach the 23 000 kPa range, a pair of thin,
frangible discs (Inconel + stainless steel) will
rupture.

Size, mL

Maximum working
pressure, kPa

Maximum working
temperature, C

25

8 000

150250

125

14 000

150250

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Microwave acid digestion bombs

Microwave acid digestion bombs are made of a
microwave transparent polymer which has good
mechanical strength at temperatures up to
150C, and serves as a heat insulator for the
Teflon sample cup.
Since heating is developed internally within the
cup, temperatures in the outer, high strength
body will seldom exceed 50C.
This type of autoclave is characterized by fast
digestion times, can operate at temperatures up
to 250C, and pressures to 8000 kPa.

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Berghof bomb
Berghof bomb is a stainless steel pressure
vessel with 10 mL Teflon sample holder,
heated from below by a heating coil.
Operating temperature up to 180C.

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Materials of Construction
The choice of the material of

construction of an autoclave depends

on the operating medium whether
acidic or alkaline, the temperature
range, and the presence or absence of
oxidizing atmosphere.

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Major elements, %
Fe

Ni

Cr

Mo

Mn

Other

T316 Stainless Steel

65

12

17

25

2.0

Si 1.0

Carpenter 20Cb3

35

34

20

25

2.0

Cu 3.5, Nb
1.0 max.

Monel 400

1.2

66

Inconel 600

76

Hastelloy B-2
Hastelloy C-276
Nickel 200
Titanium Grade 4
Zirconium Grade 705

Cu 31.5
15.5

66

28

6.5

15.5

16

Co 1.0
W 4.0, Co 2.5

99
Commercially pure titanium

Ti 99 min.

Zr 95.5 min, Hf 4.5 max,Co 2.5

Table A.2 provides a set of multipliers

which can be used to convert 350C
pressure ratings for any T316SS vessel to
higher or lower temperatures.
It can also be used to determine the
corresponding ratings for vessels of the
same design made of other materials.
No pressure vessel should be operated
above these maximum temperature limits.

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Material

[1]Standard

Temperature, C
25

100

200

300

350

T316 Stainless Steel

1.13

1.13

1.09

1.04

1.00

Monet 400

1.20

1.20

1.20

1.20

1.19

Inconel 600

1.20[1]

1.20a

1.20a

1.20a

1.20a

Hastelloy B-2

1.20a

1.20a

1.20a

1.20a

1.20a

Hastelloy C-276

1.20a

1.20a

1.20a

1.20a

1.20a

Nickel 200

0.60

0.60

0.60

0.60

0.60 at 316C

Carpenter 20Cb3

1.20

1.20

1.17

1.16

1.16

Titanium Grade 2

0.75

0.64

0.51

0.36

0.34 at 316C

Titanium Grade 4

1.20

1.20

0.81

0.63

0.60 at 16C

Zirconium Grade 705

1.20

0.98

0.76

0.65

0.61

designs cannot be rated higher than 1.20 without checking all aspects of the design.

Stainless Steel 316

Sulfuric, phosphoric, and nitric acids readily
attack T316SS at elevated temperatures and
pressures. Halogen acids attack all forms of
stainless steel rapidly, even at low temperatures
and in dilute solutions. Although T316SS offers
excellent resistance to surface corrosion by
caustic, stress corrosion cracking can occur.
This phenomenon begins to appear at
temperatures just above 100C. T316SS offers
good resistance to ammonia and to most
ammonium compounds. Halogen salts can
cause severe pitting in all stainless steels.
Chlorides can cause stress corrosion cracking.

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Carpenter 20Cb-3
Carpenter 20Cb-3 is an enriched grade of
stainless steel, designed specifically for
use with dilute (up to 30%) sulfuric acid at
elevated temperatures. It can also be used
for nitric and phosphoric acid systems as
well as for all systems for which T316SS is
suitable.

Monel 400
Monel 400 is an alloy of twotwo-thirds nickel and one third

copper.
For many applications it offers about the same corrosion
resistance as nickel, but with higher maximum working
pressures and temperatures and at a lower cost because
of its improved machine ability.
It is used for caustic solutions because it is not subject to
stress corrosion cracking in most applications including
the presence of chloride ions.
It is also an excellent material for fluorine, hydrogen
fluoride and hydrofluoric acid systems.
As would be expected from its high copper content,
Monel 400 is rapidly attacked by nitric acid and ammonia
systems.

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Inconel 600
Inconel

600 is a high nickel alloy offering

excellent resistance to caustic and chlorides
at high temperatures and high pressures
when sulfur compounds are present.
Although it can be recommended for a
broad range of corrosive conditions its cost
often limits its use to only those applications
where its exceptional characteristics are
required.

Hastelloy B-2
Hastelloy B-2 is an alloy rich in nickel and
molybdenum which has been developed
primarily for resistance to reducing acid
environments, particularly hydrochloric, sulfuric
and phosphoric.
Its resistance to these acids in pure form is
unsurpassed, but the presence of ferric and
other oxidizing ions in quantities as low as 50
ppm can degrade the resistance of this alloy.

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Hastelloy C-276
Hastelloy

C-276 is a nickel chromium

molybdenum alloy having a broadest
general corrosion resistance of all commonly
used alloys.
It was developed initially for use with wet
chlorine, but it also offers excellent
resistance to strong oxidizers such as cupric
and ferric chlorides, and to a variety of
chlorine compounds.

Nickel 200
Nickel 200 is one of the designations of
commercially pure nickel.
It offers the ultimate in corrosion
resistance to host caustic environments,
but its applications are severely restricted
because of its poor machine ability and
resultant high fabrication costs.

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Titanium
Titanium

is an excellent material for use with

oxidizing agents, such as nitric acid, aqua regia,
and other mixed acids.
It also offers good resistance to chloride ions.
Titanium may burn vigorously in the presence of
oxygen at elevated temperatures and pressures.
While there have been many successful
applications in hydrometallurgy where oxygen and
sulfuric acid are handled in titanium equipment,
the danger of ignition is always present and must
be protected against.

Zirconium
Zirconium offers excellent resistance to hydrochloric and
sulfuric acids but as with Hastelloy B-2, oxidizing ions
such as ferric, cupric, and fluorides must be avoided.
Zirconium also offers good resistance to phosphoric and
nitric acids, and to alkaline solutions as well.
Grade 702 containing hafnium is the standard
commercial grade offering the best resistance to most
corrosive agents.
Grade 705 containing small amounts of both hafnium
and niobium has better strength than Grade 702,
allowing higher working pressures, but the corrosion
resistance of Grade 705 is not as good as Grade 702.

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PRESSURE HYDROMETALLURGY
LABORATORIES

Autoclave
assembly unit in
operation

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HighHigh-pressure hydrometallurgical laboratory

Titanium autoclaves in a hydrometallurgical pilot plant at

Colorado School of Mines Research Institute, Golden, Colorado

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INCO mini
plant

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MINTEK, South Africa

*Ortest Metallurgical Research, Perth, Australia.

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Zeton
Canada

Selected Suppliers

Parr Instrument Company

Autoclave Engineers, Inc.
Pressure Products Industries, Inc.
Berghof America, Inc.

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Thanks

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