lab autoclaves - fathi habashi

7/26/2019 Lab Autoclaves - Fathi Habashi

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New EraPressure Hydrometallurgy8.Laboratory Autoclaves

for Hydrometallurgical Research

Fathi Habashi

Department of Mining, Metallurgical, and Materials Engineering

Laval University, Quebec City,Canada

[email protected]

Laboratory autoclaves forLaboratory autoclaves for hydrometalhydrometal--lurgicallurgical investigations are available in ainvestigations are available in a

variety of sizes, models, and materials ofvariety of sizes, models, and materials of

construction.construction.

They vary in sizes from 25They vary in sizes from 25 mLmL to 2 liters forto 2 liters for

laboratory studies and 5 to 50 gallons forlaboratory studies and 5 to 50 gallons for

pilot plant work.pilot plant work.


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They are essential tools for studying dissolution ofThey are essential tools for studying dissolution of

minerals at high temperature and pressure, andminerals at high temperature and pressure, and

hydrothermal precipitation reactions.hydrothermal precipitation reactions.

They can be equipped with gas inlet tube, coolingThey can be equipped with gas inlet tube, cooling

coil, agitators, etc. They may also incorporate ancoil, agitators, etc. They may also incorporate an

interchangeable chemically resistant lininginterchangeable chemically resistant lining

covering all interior surfaces.covering all interior surfaces.

Reactor operates up to 20Reactor operates up to 20 000000 kPakPa and 250and 250C.C.

AGITATED AUTOCLAVESAGITATED AUTOCLAVES

Agitated autoclaves are composed of aAgitated autoclaves are composed of a

container, a head, and an agitation systemcontainer, a head, and an agitation system

all inserted in an oven with a temperatureall inserted in an oven with a temperature

controller.controller.

Cooling coils and sampling tubes may alsoCooling coils and sampling tubes may also

be installed but other accessories such as abe installed but other accessories such as asafety valve and a vent are necessary.safety valve and a vent are necessary.


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AgitationAgitation

A stirrer drive with a pulleyA stirrer drive with a pulley

High torque magnetic drivesHigh torque magnetic drives


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High-torque magnetic drives

Magnetic drives aremagnetically coupled systemsuse high energy permanentmagnets in sealed enclosureswith no rotating seals toeliminate the troublesomeleakage problems whichsometimes arise with a packinggland in severe service,permitting long continuous runsat high pressure with little or noattention to the gland and drive.

A water cooling sleeve attachedto each drive protects the

components from excessivetemperatures arising from thereactor.


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The stirring shaft rotates inPTFE bearings and is rigidlyconnected to the internalmagnet. Both of thesecomponents are inside thepressure vessel.

The external magnet issupported by bearings androtates outside the pressurechamber. As a result of theoptimally utilized lines of forceof the magnetic field, theinternal magnet rotates insynchronization with theexternal magnet.


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Assembled Units

Using a pulley stirrerUsing magnetic stirrer


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Autoclave EngineersAutoclave Engineers

Autoclave Engineers specializes in pilotAutoclave Engineers specializes in pilot

plant size autoclaves.plant size autoclaves.


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The Zipper Clave reactorThe Zipper Clave reactor

The Zipper Clave reactor by Autoclave EngineersThe Zipper Clave reactor by Autoclave Engineersis manufactured inis manufactured in, 1, 2 and 4 liters., 1, 2 and 4 liters.

It is claimed to be the fastest, easiest opening andIt is claimed to be the fastest, easiest opening andclosing pressure vessel ever offered. No bolts toclosing pressure vessel ever offered. No bolts totorque, no clamps or rings. Instead, just raise thetorque, no clamps or rings. Instead, just raise thebody and push the spring section to close thebody and push the spring section to close thecover.cover.

To open, just pull the spring and lower the body.To open, just pull the spring and lower the body.Cover remains stationary, so there is no need toCover remains stationary, so there is no need tobreak cover connections.break cover connections.


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Closure is effected by resilient spring member (TheClosure is effected by resilient spring member (TheZipper) inserted through a circumferential groove in bodyZipper) inserted through a circumferential groove in bodyand cover. Simply release the safety sleeve and pull theand cover. Simply release the safety sleeve and pull theZipper to remove the cover. A quick release/safety lockZipper to remove the cover. A quick release/safety lockand cover safety device are provided to ensure that theand cover safety device are provided to ensure that thespring is fully inserted.spring is fully inserted.

The maximum pressure and temperature at which anyThe maximum pressure and temperature at which anyreactor can be used will depend upon the design of thereactor can be used will depend upon the design of thevessel and its material of construction since all materialsvessel and its material of construction since all materialslose strength at elevated temperatures. Autoclave design islose strength at elevated temperatures. Autoclave design is

under continuous improvement for better reliability.under continuous improvement for better reliability.


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Berghofautoclaves

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 AspectsEngineering Aspects

ValvesValves

AccessoriesAccessories

ValvesValves

Valves used in autoclaves have nonValves used in autoclaves have non--

rotating stems to minimize leakage.rotating stems to minimize leakage.

Because stem tip does not rotate onBecause stem tip does not rotate on

contact with body seat, the 2contact with body seat, the 2--piece Nonpiece Non--

Rotating Stems designed by AutoclaveRotating Stems designed by Autoclave

Engineers eliminate the galling andEngineers eliminate the galling and

scoring of stem and seat usuallyscoring of stem and seat usuallyassociated with conventional rotating stemassociated with conventional rotating stem

valves. Thus, one of the major causes ofvalves. Thus, one of the major causes of

valve leakage and failure is avoided.valve leakage and failure is avoided.


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AccessoriesAccessories

The safety head houses the rupture disc. ToThe safety head houses the rupture disc. To

prevent the action of corroding vapors, theprevent the action of corroding vapors, the

discs can be coated on one or both sidesdiscs can be coated on one or both sides

with Teflon or gold. Such coatings andwith Teflon or gold. Such coatings and

lining increase the minimum rupturelining increase the minimum rupture

ratings available in a given disc.ratings available in a given disc.

A dial thermometer.A dial thermometer.

A connecting tube.A connecting tube.


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Acid Digestion BombsAcid Digestion Bombs

The acid digestion bombs are small nonThe acid digestion bombs are small non--

agitated autoclaves that are meant foragitated autoclaves that are meant for

conducting rapid semiconducting rapid semi--quantitative tests atquantitative tests at

high temperature and pressure.high temperature and pressure.

They may be equipped with a heatingThey may be equipped with a heating

mantle but more often they can be heated inmantle but more often they can be heated in

a laboratory oven thus the temperaturea laboratory oven thus the temperature

inside the bomb is not precisely known.inside the bomb is not precisely known.


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Parr bombsParr bombs

Parr bombs contain a Teflon cup and areParr bombs contain a Teflon cup and areavailable in two sizes: 25available in two sizes: 25 mLmL and 125and 125 mLmL..

They can be heated in an oven.They can be heated in an oven.

The 125The 125--mL bomb has a safety rupture disc builtmL bomb has a safety rupture disc builtinto the head which protects the bomb and theinto the head which protects the bomb and theoperator from the hazards of an unexpectedoperator from the hazards of an unexpectedexplosion from accidental overloading.explosion from accidental overloading.

Should the pressure in the bomb accidentallyShould the pressure in the bomb accidentallyreach the 23reach the 23 000000 kPakPa range, a pair of thin,range, a pair of thin,

frangible discs (frangible discs (InconelInconel + stainless steel) will+ stainless steel) willrupture.rupture.

15025014 000125

1502508 00025

Maximum working

temperature, C

Maximum working

pressure, kPaSize, mL


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Microwave acid digestion bombsMicrowave acid digestion bombs

Microwave acid digestion bombs are made of aMicrowave acid digestion bombs are made of amicrowave transparent polymer which has goodmicrowave transparent polymer which has goodmechanical strength at temperatures up tomechanical strength at temperatures up to150150C, and serves as a heat insulator for theC, and serves as a heat insulator for theTeflon sample cup.Teflon sample cup.

Since heating is developed internally within theSince heating is developed internally within thecup, temperatures in the outer, high strengthcup, temperatures in the outer, high strength

body will seldom exceed 50body will seldom exceed 50C.C.This type of autoclave is characterized by fastThis type of autoclave is characterized by fastdigestion times, can operate at temperatures updigestion times, can operate at temperatures upto 250to 250C, and pressures to 8000C, and pressures to 8000 kPakPa..


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BerghofBerghofbombbomb

BerghofBerghofbomb is a stainless steel pressurebomb is a stainless steel pressurevessel with 10vessel with 10 mLmL Teflon sample holder,Teflon sample holder,

heated from below by a heating coil.heated from below by a heating coil.

Operating temperature up to 180Operating temperature up to 180C.C.


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Materials of ConstructionMaterials of Construction

The choice of the material ofThe choice of the material of

construction of an autoclave dependsconstruction of an autoclave depends

on the operating medium whetheron the operating medium whether

acidic or alkaline, the temperatureacidic or alkaline, the temperature

range, and the presence or absence ofrange, and the presence or absence of

oxidizing atmosphereoxidizing atmosphere..


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Zr 95.5 min, Hf 4.5 max,Co 2.5Zirconium Grade 705

Ti 99 min.Commercially pure titaniumTitanium Grade 4

99Nickel 200

W 4.0, Co 2.511615.56.5Hastelloy C-276

Co 1.01281662Hastelloy B-2

15.5768Inconel 600

Cu 31.5661.2Monel 400

Cu 3.5, Nb

1.0 max.

2.025203435Carpenter 20Cb3

Si 1.02.025171265T316 Stainless Steel

OtherMnMoCrNiFe

Major elements, %

Table A.2 provides a set of multiplierswhich can be used to convert 350Cpressure ratings for any T316SS vessel tohigher or lower temperatures.

It can also be used to determine thecorresponding 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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0.610.650.760.981.20Zirconium Grade 705

0.60 at 16C0.630.811.201.20Titanium Grade 4

0.34 at 316C0.360.510.640.75Titanium Grade 2

1.161.161.171.201.20Carpenter 20Cb3

0.60 at 316C0.600.600.600.60Nickel 200

1.20a1.20a1.20a1.20a1.20aHastelloy C-276

1.20a1.20a1.20a1.20a1.20aHastelloy B-2

1.20a1.20a1.20a1.20a1.20[1]Inconel 600

1.191.201.201.201.20Monet 400

1.001.041.091.131.13T316 Stainless Steel

35030020010025

Temperature, CMaterial

[1]Standard designs cannot be rated higher than 1.20 without checking all aspects of the design.

Stainless Steel 316Stainless Steel 316

Sulfuric, phosphoric, and nitric acids readilySulfuric, phosphoric, and nitric acids readilyattack T316SS at elevated temperatures andattack T316SS at elevated temperatures andpressures. Halogen acids attack all forms ofpressures. Halogen acids attack all forms ofstainless steel rapidly, even at low temperaturesstainless steel rapidly, even at low temperaturesand in dilute solutions. Although T316SS offersand in dilute solutions. Although T316SS offersexcellent resistance to surface corrosion byexcellent resistance to surface corrosion bycaustic, stress corrosion cracking can occur.caustic, stress corrosion cracking can occur.This phenomenon begins to appear atThis phenomenon begins to appear at

temperatures just above 100temperatures just above 100C. T316SS offersC. T316SS offersgood resistance to ammonia and to mostgood resistance to ammonia and to mostammonium compounds. Halogen salts canammonium compounds. Halogen salts cancause severe pitting in all stainless steels.cause severe pitting in all stainless steels.Chlorides can cause stress corrosion cracking.Chlorides can cause stress corrosion cracking.


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Carpenter 20CbCarpenter 20Cb--33

Carpenter 20CbCarpenter 20Cb--3 is an enriched grade of3 is an enriched grade of

stainless steel, designed specifically forstainless steel, designed specifically for

use with dilute (up to 30%) sulfuric acid atuse with dilute (up to 30%) sulfuric acid at

elevated temperatures. It can also be usedelevated temperatures. It can also be used

for nitric and phosphoric acid systems asfor nitric and phosphoric acid systems as

well as for all systems for which T316SS iswell as for all systems for which T316SS is

suitable.suitable.

MonelMonel

400400

MonelMonel 400 is an alloy of two400 is an alloy of two--thirds nickel and one thirdthirds nickel and one thirdcopper.copper.

For many applications it offers about the same corrosionFor many applications it offers about the same corrosionresistance as nickel, but with higher maximum workingresistance as nickel, but with higher maximum workingpressures and temperatures and at a lower cost becausepressures and temperatures and at a lower cost becauseof its improved machine ability.of its improved machine ability.

It is used for caustic solutions because it is not subject toIt is used for caustic solutions because it is not subject tostress corrosion cracking in most applications includingstress corrosion cracking in most applications includingthe presence of chloride ions.the presence of chloride ions.

It is also an excellent material for fluorine, hydrogenIt is also an excellent material for fluorine, hydrogenfluoride and hydrofluoric acid systems.fluoride and hydrofluoric acid systems.

As would be expected from its high copper content,As would be expected from its high copper content,MonelMonel 400 is rapidly attacked by nitric acid and ammonia400 is rapidly attacked by nitric acid and ammoniasystems.systems.


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InconelInconel 600600

InconelInconel 600 is a high nickel alloy offering600 is a high nickel alloy offeringexcellent resistance to caustic and chloridesexcellent resistance to caustic and chloridesat high temperatures and high pressuresat high temperatures and high pressureswhen sulfur compounds are present.when sulfur compounds are present.

Although it can be recommended for aAlthough it can be recommended for abroad range of corrosive conditions its costbroad range of corrosive conditions its costoften limits its use to only those applicationsoften limits its use to only those applicationswhere its exceptional characteristics arewhere its exceptional characteristics arerequired.required.

HastelloyHastelloy

BB

--22

HastelloyHastelloy BB--2 is an alloy rich in nickel and2 is an alloy rich in nickel and

molybdenum which has been developedmolybdenum which has been developed

primarily for resistance to reducing acidprimarily for resistance to reducing acid

environments, particularly hydrochloric, sulfuricenvironments, particularly hydrochloric, sulfuric

and phosphoric.and phosphoric.

Its resistance to these acids in pure form isIts resistance to these acids in pure form is

unsurpassed, but the presence of ferric andunsurpassed, but the presence of ferric and

other oxidizing ions in quantities as low as 50other oxidizing ions in quantities as low as 50

ppmppm can degrade the resistance of this alloy.can degrade the resistance of this alloy.


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HastelloyHastelloy CC--276276

HastelloyHastelloy CC--276 is a nickel chromium276 is a nickel chromiummolybdenum alloy having a broadestmolybdenum alloy having a broadestgeneral corrosion resistance of all commonlygeneral corrosion resistance of all commonlyused alloys.used alloys.

It was developed initially for use with wetIt was developed initially for use with wetchlorine, but it also offers excellentchlorine, but it also offers excellentresistance to strong oxidizers such as cupricresistance to strong oxidizers such as cupricand ferric chlorides, and to a variety ofand ferric chlorides, and to a variety ofchlorine compounds.chlorine compounds.

Nickel 200Nickel 200

Nickel 200 is one of the designations ofNickel 200 is one of the designations of

commercially pure nickel.commercially pure nickel.

It offers the ultimate in corrosionIt offers the ultimate in corrosion

resistance to host caustic environments,resistance to host caustic environments,

but its applications are severely restrictedbut its applications are severely restricted

because of its poor machine ability andbecause of its poor machine ability and

resultant high fabrication costs.resultant high fabrication costs.


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TitaniumTitanium

Titanium is an excellent material for use withTitanium is an excellent material for use withoxidizing agents, such as nitric acid, aquaoxidizing agents, such as nitric acid, aqua regiaregia,,and other mixed acids.and other mixed acids.

It also offers good resistance to chloride ions.It also offers good resistance to chloride ions.

Titanium may burn vigorously in the presence ofTitanium may burn vigorously in the presence ofoxygen at elevated temperatures and pressures.oxygen at elevated temperatures and pressures.

While there have been many successfulWhile there have been many successfulapplications in hydrometallurgy where oxygen andapplications in hydrometallurgy where oxygen andsulfuric acid are handled in titanium equipment,sulfuric acid are handled in titanium equipment,

the danger of ignition is always present and mustthe danger of ignition is always present and mustbe protected against.be protected against.

ZirconiumZirconium

Zirconium offers excellent resistance to hydrochloric andZirconium offers excellent resistance to hydrochloric andsulfuric acids but as withsulfuric acids but as with HastelloyHastelloy BB--2, oxidizing ions2, oxidizing ionssuch as ferric, cupric, and fluorides must be avoided.such as ferric, cupric, and fluorides must be avoided.

Zirconium also offers good resistance to phosphoric andZirconium also offers good resistance to phosphoric andnitric acids, and to alkaline solutions as well.nitric acids, and to alkaline solutions as well.

Grade 702 containing hafnium is the standardGrade 702 containing hafnium is the standardcommercial grade offering the best resistance to mostcommercial grade offering the best resistance to mostcorrosive agents.corrosive agents.

Grade 705 containing small amounts of both hafniumGrade 705 containing small amounts of both hafniumand niobium has better strength than Grade 702,and niobium has better strength than Grade 702,allowing higher working pressures, but the corrosionallowing higher working pressures, but the corrosionresistance of Grade 705 is not as good as Grade 702.resistance of Grade 705 is not as good as Grade 702.


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PRESSURE HYDROMETALLURGYPRESSURE HYDROMETALLURGY

LABORATORIESLABORATORIES

AutoclaveAutoclave

assembly unit inassembly unit in

operationoperation


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HighHigh--pressure hydrometallurgical laboratorypressure hydrometallurgical laboratory

Titanium autoclaves in a hydrometallurgical pilot plant at

Colorado School of Mines Research Institute, Golden, Colorado


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INCO miniINCO mini

plantplant


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MINTEK, South AfricaMINTEK, South Africa

*Ortest Metallurgical Research, Perth, Aust ralia.


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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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lab autoclaves - fathi habashi

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