Determination of BlackDetermination of BlackDetermination of Black Determination of Black Liquor Evaporation Liquor Evaporation

Properties via Testing Properties via Testing with the Bench Topwith the Bench Topwith the Bench Top with the Bench Top

ReactorReactorReactorReactor

Bench Top ReactorBench Top ReactorBench Top ReactorBench Top Reactor

Used primarily to study crystallizationUsed primarily to study crystallizationUsed primarily to study crystallization Used primarily to study crystallization behavior during evaporationbehavior during evaporation

Allows controlled evaporation of blackAllows controlled evaporation of black Allows controlled evaporation of black Allows controlled evaporation of black liquor and other solutionsliquor and other solutionsI t t ti t tiI t t ti t ti Instrumentation to measure operating Instrumentation to measure operating conditions and particle size distributionconditions and particle size distribution

Filtered samples taken to collect crystals Filtered samples taken to collect crystals for analysisfor analysis

Main VesselMain Vessel Vessel (2.5 liter) Vessel (2.5 liter)

fabricated from SSfabricated from SS Well stirred with Well stirred with

magnetically coupled magnetically coupled mixermixermixermixer

Flanged top plate with Flanged top plate with inlet, outlet and probe inlet, outlet and probe connectionsconnectionsconnectionsconnections

Connections for pressure Connections for pressure transducer, pressure transducer, pressure , p, prelief valve, relief valve, thermocouples and other thermocouples and other accessaccessaccessaccess

Evaporation in Bench Top ReactorEvaporation in Bench Top ReactorEvaporation in Bench Top ReactorEvaporation in Bench Top Reactor Electrical heating jacket Electrical heating jacket

d PID C t ll lld PID C t ll lland PID Controller allows and PID Controller allows operation up to 150 operation up to 150 °°CC

Evaporation rates of up toEvaporation rates of up to Evaporation rates of up to Evaporation rates of up to 6 g/min 6 g/min –– using water using water cooled condenser cooled condenser

Sample outlet at bottom ofSample outlet at bottom of Sample outlet at bottom of Sample outlet at bottom of vesselvessel

2 micron stainless steel 2 micron stainless steel filter used to remove salt filter used to remove salt crystals from liquorcrystals from liquor

Lasentec FBRM ProbeLasentec FBRM ProbeLasentec FBRM ProbeLasentec FBRM Probe

Particle size measuredParticle size measured Particle size measured Particle size measured by length of reflected by length of reflected laser signal from laser signal from

Laser Diode

Detector Fiber Optic

Beam Splitter ggrotating beamrotating beam

Particle size distribution Particle size distribution Sapphire Window

Laser Beam

Optics Rotating at

calculated by softwarecalculated by softwareCrystallization indicated Crystallization indicated

p ga Fixed HighVelocity

yyby rapid increase in by rapid increase in particle count ratesparticle count rates

Example FBRM DataExample FBRM Data

Crystal FilterCrystal Filter 2 micron stainless steel filter2 micron stainless steel filterUsed to remove salt crystals from liquorUsed to remove salt crystals from liquory qy qCrystals cleaned and analyzed to Crystals cleaned and analyzed to

determine salt speciesdetermine salt speciesdetermine salt speciesdetermine salt species

Boiling Point RiseBoiling Point RiseBoiling Point RiseBoiling Point Rise

During steadyDuring steady--state evaporation thestate evaporation theDuring steadyDuring steady state evaporation the state evaporation the boiling point rise (BPR) can be measuredboiling point rise (BPR) can be measured

BPR equals the difference between theBPR equals the difference between the BPR equals the difference between the BPR equals the difference between the measured temperature and the boiling measured temperature and the boiling temperature of water at the measured temperature of water at the measured ppvapor pressure vapor pressure

Correlation can be derived from data to Correlation can be derived from data to express BPR as a function of the liquor express BPR as a function of the liquor solids contentsolids content

Crystallization and BPR AnalysisCrystallization and BPR AnalysisCrystallization and BPR AnalysisCrystallization and BPR Analysis

Evaporation from 35% to 65% Solids Evaporation from 35% to 65% Solids FBRM particle data to determine FBRM particle data to determine

crystallization pointscrystallization points Boiling Point Rise as a function of solids %Boiling Point Rise as a function of solids % Boiling Point Rise as a function of solids %Boiling Point Rise as a function of solids %Requires 4 liters of BL at 35Requires 4 liters of BL at 35--40% solids40% solids

Bench Top Reactor Bench Top Reactor Modified with Flow Loop Modified with Flow Loop

and Viscometerand Viscometerand Viscometerand Viscometer••Added recirculation loop Added recirculation loop with viscometerwith viscometer••Data Acquisition via FBRM Data Acquisition via FBRM qqsystemsystem••Allows for measurement ofAllows for measurement ofAllows for measurement of Allows for measurement of viscosity and boiling point viscosity and boiling point rise over range of solidsrise over range of solidsrise over range of solidsrise over range of solids

Brookfield TT100 ViscometerBrookfield TT100 Viscometer Rotating concentric cylinders

provides defined shear measurement

Torque Sensor produces 4-20 mA linear signal

Thermocouple at viscometer outlet provides temperature

Typical Viscosity and BPR CurvesTypical Viscosity and BPR Curvesyp yyp y

Viscosity, BPR and Crystallization Viscosity, BPR and Crystallization A l iA l iAnalysisAnalysis

Evaporation from 35% to 72% SolidsEvaporation from 35% to 72% Solids Evaporation from 35% to 72% SolidsEvaporation from 35% to 72% Solids FBRM particle data to determine FBRM particle data to determine

crystallization pointscrystallization pointscrystallization pointscrystallization points Boiling Point Rise as a function of solids %Boiling Point Rise as a function of solids % Viscosity data over range of testViscosity data over range of test Viscosity data over range of test Viscosity data over range of test

conditions (with correlation equation)conditions (with correlation equation)Requires 8 liters of BL at 35Requires 8 liters of BL at 35 40% solids40% solidsRequires 8 liters of BL at 35Requires 8 liters of BL at 35--40% solids40% solidsComplete chemical analysis of black liquor Complete chemical analysis of black liquor

available from IPST analytical groupavailable from IPST analytical groupavailable from IPST analytical groupavailable from IPST analytical group

IPST Contact InformationIPST Contact InformationIPST Contact InformationIPST Contact Information Steve LienSteve Lien

404404--894894--66746674 Steve.Lien@ipst.gatech.eduSteve.Lien@ipst.gatech.edu@ p g@ p g

Shipping Address:Shipping Address:

Institute of Paper Science and TechnologyInstitute of Paper Science and TechnologyGeorgia TechGeorgia Techgg500 10th St. NW500 10th St. NWAtlanta, GA 30318Atlanta, GA 30318Attn: Steve LienAttn: Steve Lien