Professional Documents
Culture Documents
By
Hamideh Hajiha
University of Toronto
Hamideh Hajiha
Degree of Master of Applied Science
Department of Chemical Engineering and Applied Chemistry
University of Toronto
2009
Abstract
Multiple Effect Evaporators (MEE) are used in kraft pulp mills to concentrate
black liquor. In order to verify if the MEE is operating at an optimum condition, thermal
involved, this can be a challenging task. Thus, this work involved the study of operating
data from two Canadian pulp mills using Multivariate Data Analysis (MVDA)
techniques: Principal Component Analysis (PCA) and Partial Least Squares Analysis
(PLS). Moreover, the evaporation system was modelled using a dynamic simulation
software called CADSIM. MVDA determined that the thermal performance of the
evaporators was positively correlated with the weak black liquor flow rate and negatively
correlated with the steam pressure (to the first effect). The CADSIM model confirmed
these findings. Therefore, these two techniques show to be useful tools in identifying
ii
Acknowledgements
I would like to thank Professor Honghi Tran. Your guidance, support, weekly
meetings and continued challenges made all the difference for this project. I have learned
a lot over the past two years, and I am forever in your debt.
Daniel Saturnino, Thank you very much for all of your help with the CADSIM
portion of this project.
Many people helped with this project: Professor Tom Grace, Bill Downing,
Odessa Websdale, Denys Holik, and Jack Porter. I gratefully thank you for your support.
I would like to thank my parents, Narges and Mehdi, and my brothers, Hamed,
Mohammad, and Mory for supporting me throughout my life.
Many friends have contributed to my time over the past two years. I am greatly
thankful to Maryam, Fariba, Azadeh, Daniel, Sam, Pete, Sabrina, John, Tasha and Babak.
Finally, I would like to thank the Professors, Staff and Students in the Chemical
Engineering Department at the University of Toronto. You made my time here an
amazing experience.
iii
Table of Contents:
Abstract ............................................................................................................................... ii
Acknowledgements............................................................................................................ iii
List of Figures ..................................................................................................................... v
List of Tables ..................................................................................................................... vi
1. Introduction................................................................................................................. 1
2. Literature Review........................................................................................................ 3
2.1 Overview of Kraft Recovery Cycle .......................................................................... 3
2.2 Black Liquor Evaporators ......................................................................................... 5
2.3 Scaling Problem ...................................................................................................... 10
2.4 Multivariate Data Analysis ..................................................................................... 12
2.4.1 Principal Component Analysis (PCA) ............................................................. 13
2.4.2 Partial Least Squares Regression Analysis (PLS) ........................................... 23
3. Methodology ............................................................................................................. 26
4. Results and Discussion ............................................................................................. 28
4.1 Analysis for Mill A ................................................................................................. 28
4.1.1. Mill A Evaporation System ............................................................................ 28
4.1.2. MVDA ............................................................................................................ 33
4.1.2.1 PCA........................................................................................................... 40
4.1.2.2 PLS............................................................................................................ 42
4.1.2.3 Time Series Plots: ..................................................................................... 53
4.1.3. Dynamic Simulation ....................................................................................... 58
4.2 Analysis for Mill B ................................................................................................. 68
4.2.1 Mill B Evaporation System.............................................................................. 68
4.2.2 MVDA ............................................................................................................. 69
4.2.2.1 PCA........................................................................................................... 69
4.2.2.2 PLS............................................................................................................ 70
5. Limitations to Modelling .......................................................................................... 76
6. Conclusions............................................................................................................... 78
Reference .......................................................................................................................... 80
Appendix 1........................................................................................................................ 82
Scaling Problem in Mill A Evaporators........................................................................ 82
Appendix 2........................................................................................................................ 85
Boil-out – 1st Effect and 58% Flash Tank................................................................. 85
Boil-out Procedure:................................................................................................... 87
Appendix 3........................................................................................................................ 88
Appendix 4........................................................................................................................ 91
iv
List of Figures
v
List of Tables
vi
1. Introduction
In kraft pulp mills, multi-effect evaporators (MEE) are used to concentrate black
dissolved salts begin to precipitate from the system as they reach solubility. Precipitated
solids may deposit on the heat transfer surfaces, forming a layer of scale. Scaling of
liquor side heat transfer surfaces in black liquor evaporators has been a persistent
problem in many mills. It lowers the overall heat transfer coefficient and the available
heat transfer area of the evaporators, negatively affecting the thermal performance of
MEE. The severity of scaling varies from mill to mill, depending on liquor properties,
equipment design, and mill operation. It can be costly due to production losses associated
with equipment cleaning. In recent years, high energy costs have forced mills to explore
One of the main parameters affecting thermal performance for a given set of
multiple effect evaporators is scaling especially in the first effect and high solids
carbonate, and water-soluble sodium salts (burkeite and dicarbonate) [5]. Understanding
the mechanisms of scaling and the factors affecting it will help to improve the thermal
performance of MEE. The mechanisms are relatively well known [6, 7]. However,
operating variables that affect scaling are often not clear. This is because variables are
1
design, and operation. Since evaporators are an integral part of the chemical recovery
process, their thermal efficiency is likely affected by other factors in the recovery cycle.
untangle the relationship between various factors affecting evaporator scaling. MVDA
has been applied in various industries such as pharmaceutical, food and biotech
processes, mineral processing and pulp and paper [8-13]. The technique has been
scaling/plugging incidents in recovery boilers [14], and ring formation in lime kilns [15].
A similar approach may therefore be applied to examine the thermal performance of the
MEE system.
This thesis work is a first attempt to apply MVDA to the thermal performance and
Analysis (PCA), and Partial Least Squares (PLS) have been applied to better understand
parameters are examined through dynamic simulation (using software called CADSIM),
2
2. Literature Review
Kraft pulping and the chemical recovery process is composed of the following
units: cooking, washing, evaporation, burning, causticizing and calcining (Figure 1).
Wood chips are cooked with white liquor (NaOH + Na2S) in a digester at about 170 ºC,
to produce kraft pulp and weak black liquor, as seen in Reaction 1. Weak Black liquor
(WBL), the by-product of the chemical recovery cycle in the pulp and paper industry, is
composed of water, lignin, cellulose and inorganic sodium salts [16]. These chemicals
that, weak black liquor is separated from pulp in a washing unit. The black liquor is
diluted by the wash water and generally contains 14-17% solids. 95-98% of chemicals are
recovered in modern pulp washing units [17]. For each ton of pulp, 8-10 tons of weak
The resulting concentrated black liquor is burned in the recovery furnace to produce an
inorganic smelt of Na2CO3 and Na2S. The smelt is then dissolved in water to yield green
liquor, an aqueous solution of Na2CO3 and Na2S, as shown in Reaction 2. The green
liquor undergoes the causticizing process where Na2CO3 is converted into NaOH by
reacting with Ca(OH)2, as in Reaction 3. At this point, the original white liquor required
for pulping is recovered. In order to provide lime for the causticizing process, lime mud
(or precipitated CaCO3) is dewatered, dried and burned in a lime kiln to produce lime for
3
Wood
Lime
Lime Digester
Pulping
Kiln
Kiln
Pulp
White
Liquor
Washing
Washin
Lime
Lime g
Mud W eak
B la c k
Causticizin L iq u o r
Causticizing
g Plant 1 5 % s o l id s
Plan
Evaporators
t
Green Water
Liquor H ea vy
Recover
Recovery B la c k
Smelt y Boiler
Boile L iq u o r
r 7 0 % s o l id s
Figure 1: Kraft recovery cycle
The main reactions in the kraft process are listed below: [18]
Pulping
Combustion
Causticizing
4
2.2 Black Liquor Evaporators
Weak black liquor leaving the brownstock washers contains 13 to 17% dissolved
solids. In order to safely and effectively burn the black liquor to recover chemicals and
heat, the solids content must be at least 60%. Increasing the solids content improves the
recovery boiler thermal efficiency, stabilizes boiler operation and reduces sulfur
emissions. Emissions of total reduced sulphides (TRS) from the recovery boiler are
evaporation [18]. Heating value of black liquor ranges between 5800-6600 Btu/lb of dry
solids, which is low in comparison to other fuels, such as gas and oil [19]. Thus, a large
amount of water must be evaporated in order to increase the net fuel value of black
liquor. To accomplish this task, the most common types of evaporators presently used in
the industry are the rising film long tube vertical evaporators (LTV) and the falling film
evaporators (FF).
exchanger at the bottom and a vapour dome at the top. The tubes are typically 5 cm (2”
OD), 6.7 – 9.1 meters long, held in place by a tube sheet at the top and bottom [4]. Black
liquor enters the tubes from the bottom of the unit, where it is heated by the steam on the
shell side of the tubes. As the heated black liquor boils, the resulting water vapour helps
push the black liquor upward, until it reaches a deflector at the top where it is separated
from the vapour. All vapour domes have a deflector directly over the heating element to
break foam and initiate downward flow to the liquor. The concentrated black liquor exits
the unit through a liquor outlet at the bottom of the vapour dome. The fine black liquor
5
droplets entrained in the water vapour are separated by means of a demister as the vapour
Vapour
Demister
Vapour
Deflector Dome
Condensate Liquor
Outlet
Steam
Inlet
Condensate
Outlet Vent
Tubes
Liquor Inlet
and a vapour body at the bottom. Liquor is fed to the bottom of the evaporator where a
fixed level is maintained. Liquor rises to the top by means of a recirculation pump, and
flows down the tubes with gravity (Figure 3). The liquor and vapour mixture leaving the
tubes enters the dome at the bottom of the unit. The vapour is then separated from the
6
Falling film evaporators have a significantly smaller risk of scaling than the LTV
evaporators because no bulk boiling occurs inside the tubes; consequently, no dry spot
formation exists where scaling can initiate [19]. Falling film evaporators run at lower
steam pressures than the LTV evaporators, since steam does not have to push the liquor
upwards in the tubes. Consuming weaker steam minimizes the scaling caused by reverse
complexes [19].
Recirculating
Liquor
Steam
Inlet
Vapour
Outlet
Vent
Condensate
Outlet Drop
Separator
Liquor
Inlet
Dome
Liquor
Outlet
Recirculation Pump
that the latent heat of vapour is used multiple times. Each evaporator is called an effect in
this system. Live steam is only fed to the first effect, while the vapour generated in the
7
first effect is the heating medium in the second effect, and so on. In kraft pulp mills,
evaporation occurs in multiple effect evaporators (MEE), where steam and black liquor
flow counter-currently (Figure 4). Steam economy, defined as the ton of water
evaporated over the ton of steam used, increases as the number of effects increases (Table
1 lists measured steam economies for a practical operation). Table 1 shows specific heat
number is limited to six to eight evaporators. In case of rising film long tube vertical
(LTV) evaporators, the number of effects is limited to six, to keep the ∆T higher than 9.5
difference between the saturated vapour temperature and the liquor temperature. ∆T is
critical for long tube vertical evaporators, where a ∆T of less than 9.5 ºC will often cause
The evaporators operate at different pressures and are connected so that the
produced vapour in one is used as heating steam for the next one. Live steam is only fed
to the first evaporator body/effect. The weak black liquor feed usually splits between the
8
last two effects, where the liquor boils at lower temperature under vacuum. As the liquor
flows through the evaporators (from sixth to first), the pressure of the evaporator, boiling
Moreover, in order to bring the solids content from approximately 50% to 70-
80%, high solids concentrator(s) are placed after the evaporators, or integrated between
them.
A detailed layout and a process flow sheet are presented in the Result and
Discussion section regarding the studied mills. There is also an example of a severe
scaling problem and the mill’s initiative to solve said problem in Appendix A1.
9
2.3 Scaling Problem
liquor is concentrated, dissolved salts begin to precipitate from the system as they reach
solubility. Precipitated solids may deposit on the heat transfer surfaces, forming a layer
of scale. Severe scaling can interrupt black liquor flow, creating a bottleneck in pulp
production. Due to its low thermal conductivity, scale greatly reduces the heat transfer
The scaling in a kraft black liquor evaporator is of the following types: calcium
carbonate scaling, burkeite scaling, soap or fibre scaling, aluminum silicate and oxalate
Calcium scaling:
Calcium scales form mainly in the first effect. The rate of scaling strongly
oxalate and soap. Calcium ions become free when temperature reaches 90 – 130 ºC,
therefore causing calcium carbonate to form and precipitate on heating surfaces [4]. Since
calcium compounds are less soluble at higher temperatures, calcium scaling increases
when the liquor temperature is above 40 ºC [4]. Heat transfer surfaces can be the host for
10
nuclei formation as they have the highest temperature in the evaporator body [6]. Studies
Calcium ions restrain the nucleation of burkeite and dicarbonate, resulting in a higher
degree of super-saturation [20]. This type of scale is easily washable by circulating weak
Black liquor soap is a mixture of resin and fatty acids that is separated from weak
and intermediate black liquors to avoid scaling and foaming in the evaporators and
concentrators. High fibre content makes the separation of soap harder, since soap adheres
to the fibre surface. This type of scaling is common in the 2nd, 3rd and 4th effects [4]. To
reduce this type of scaling, soap is usually removed from the evaporators at the 3rd
effect.
Sodium aluminum silicate scales are hard, glassy and persistent. This type of scale
is usually found in first effect and final concentrators, and its amount is determined by
aluminum and silicate concentrations [4]. Generally, in North American mills, silicate
scaling is not a common problem due to its small input in the recovery cycle.
Oxalate scaling:
The oxalate ions are formed in the cooking and bleaching process. Sodium
oxalate particles can form in black liquor when the concentration exceeds 45% solids.
11
Also when evaporation is performed under vacuum at about 90 ºC sodium oxalate can
precipitate at 30-40% solids. To avoid this precipitation, the process temperature is raised
to about 110 ºC [21]. Calcium oxalate deposition is not a concern, since calcium is
Modern mills are equipped with various online instruments that continuously
collect data at high rates. These periodical measurements on various variables are stored
as large tables of data for long periods of time. Extracting information and analysis of this
data is necessary for understanding the behaviour of the system as well as recognizing
project goals for various systems. Principal Component Analysis (PCA) and Partial Least
Squares Analysis (PLS) are two such techniques that have been used extensively, having
gained wide acceptance in literature. PCA can visually monitor processes, compare
operational periods and determine which process changes work well for the system. This
procedure is a crucial first step towards the understanding of process. PLS can be used to
extract correlation information between variables and provide predictive models for the
process [3]. These two techniques, PCA and PLS, have already been used extensively to
model and monitor complex industrial processes [8-10, 22], including in the pulp and
paper industry [11], but have not yet been applied to multiple effect evaporators.
12
The challenges of multivariate data analysis involve dealing with dimensionality,
multicollinearity, noise and missing data. PCA and PLS are capable of handling large
amounts of highly correlated variables, missing data, noise, and mild nonlinearities [23].
SIMCA-P, a commercial software package available for MVDA, deals with all of these
problems as it uses all variables simultaneously, and uses projection method (explained in
section 2.4.1) to cope with missing data and noise. SIMCA-P finds correlations among
correlations are used to better understand the system, to find optimal operational
X increases. A causal relationship entails that a change in one variable, X, causes another
[3, 23-25]. The starting point for principal component analysis is a matrix with N rows
X = [x1 x2 x 3 ... x r ]
13
where x1 , x 2 , x 3... x r are vectors of data measured by r on-line process
instruments.
Principal component analysis finds lines and planes of closest fit to systems of
models a portion of the variability in the dataset. Each principal component equation has
a weight given to every variable in the dataset based on their contribution to maximize
the variability of the dataset. PCA simplifies tables of multivariate data by visualizing it
in low dimensional planes approximating the data in the least squares sense.
Prior to PCA, data are pre-processed to arrive at a useful model. Since PCA tries
to capture the maximum variability in the model, a variable with a large variability is
more likely to be expressed in the modeling than a variable with low variability. Thus
data are scaled so that all variables make the same contribution to the model. Data also
undergo mean centering, where the average value of each variable is calculated and then
subtracted from the data, making the interpretation easier. These pre-treatments are
linear equations, defining the principal components. Consider a matrix of industrial data,
X, with N rows (observations) and R columns (variables). The first principal component
(PC1) is a line in R dimensional space that best approximates the model, capturing the
14
maximum variability while trying to minimize the distance between itself and data points
with preference given to the inputs that are more important in explaining the model. Each
observation may now be projected onto this line to get a new co-ordinate called score, ti
(Figure 5). Each principal component equation has a weight given to every variable in the
dataset based on their contribution to maximize the variability of the dataset. In other
words, a principal component is a linear formula that combines all the variables to show
trends in the data, for example, PC #1 = 0.6 * (var 1) + 0.2 * (var 2) +….
PC #2
PC #1 PC #1
TTA TTA
The second PC is orthogonal to the first PC and orients itself to best approximate
the data in this direction. The two principal component lines form a plane, and process
data points are projected on the two dimensional model plane in the R dimensional
dimensional presentation of the multidimensional dataset (Figure 6). The x-axis (or t[1])
of the plot represents the first principal component, while the y-axis (or t[2]) represents
the second. In other words, PCA is a projection method which compresses all of the
15
number of orthogonal principal components. The reduction in dimensions of the dataset
allows one to visually study the behaviour of the system through the projection of the
I II
IV III
The most common use of PCA is in the conversion of a data matrix to a few
informative plots. The first few component plots, t1/t2 (XY plot of first and second PCs)
or t1/t3( XY plot of first and third PCs) display the most dominant patterns in the data set,
as they capture most of the information [24]. Scatter plot, t1/t2, shows how observations
are projected in to two dimensions (Figure 6). Each data point on this graph represents a
day’s worth of data for all of the variables while dealing with daily averages. The ellipse
represents a 95% confidence interval of the data. The center (origin; 0,0) of the graph
represents the average value across all variables. Points that are further away from the
16
origin are the ones that deviate greater from the average. It is important to note that
statistically it is expected N*0.05 observations will be found outside the 95% confidence
region. Points grouped together in the scatter plot have similar quality characteristics.
Observations close to origin have average properties and observations clustered together
and away from the origin have similar properties deviating from the average [3].
Principal component loadings express the orientation of the model plane in the R
dimensional space with respect to the original variables. Cosine of the angle between PC1
and original variable indicates the contribution and load of each variable. A second set of
loading coefficients indicates the direction of PC2 in relation to the original variables.
The loadings show how the variables are linearly combined to form the scatters. The
loading plot shows which variables are influential and also how the variables are
correlated [3]. Variables placed further away from the origin in the loading plot are more
influential on the model. Variables grouped together in the loading plot are directly
correlated with each other. From the arbitrary loading plot, Figure 7, one can conclude
that along PC1, steam flow rate to the 1st effect, placed at far left, is more influential than
level of the 2nd effect (shown as #2 EFFECT LEVEL), placed close to origin.
17
EVAPORATION SOUTH
EVAPORATION HSC
NORTH STEAM
HSC MASS
STEAM FLOW
MASS FLOW
0.4
I II
0.3 #3 EFFECT VAPOUR PRESSURE
%CAUSTICITY (CE)
0.1
MILL WATER TEMPSOAP SKIMMERCONDENSER
TO SURFACE TANK LEVEL
CHIP METER SPEED
p[2]
KAPPA #
-0.3
IV III
#1 EFFECT RECIRC PUMP LOAD
-0.4
Variables placed close together are positively correlated and when the numerical
value of one variable increases or decreases, the numerical value of other positively
correlated variables change the same way. Values on opposite sides of the plot origin are
negatively (inversely) correlated with each other. Based on the arbitrary example shown
in Figure 7, it may be concluded that 3rd effect vapour pressure and evaporation across
effects are positively correlated with each other. Combining the scatter plot and the
loading plot allows for interpretation of the PCA model. Both plots are divided into four
quadrants. Observation points in any quadrant of the scatter plot have higher values of
dimensional space. SIMCA P converts tables of data to plots by projecting the data onto a
18
information in the data is captured as patterns along these lines, planes and hyper planes
while similar data points fall close to each other. With MVDA the measured variables are
grouped together and are summarized by new variables called scores that capture
T
X =TP + E
where
T = [t 1 t 2 t 3 ... t k ]
[
P = p1 p2 p 3 ... pk ]
E = [e1 e2 e 3 ... e r ]
component loading matrix, E is a residual matrix, and the subscript k refers to the
number of PC’s calculated. The score matrix, T , contains the decomposed process data
while the loading matrix, P , identifies variables that are associated with processes in a
system.
Each PC captures some variability (information) in model, and having more PC’s
helps capturing more information from data points. An important question is “how many
principal components are really needed in a model?” This question is related to the
balance between the degree of fit and the predictability of a model. A quantitative
measure of the goodness of fit of a model is given by R2X, the explained variation. The
19
the prediction variation. Cross validation, CV, is used to estimate predictability of the
model with increasing number of principal components (CV is explained in the below
paragraph). The R2X and Q2X parameters follow different trends as the model
complexity increases (Figure 8). As the number of principal components increases, R2X
increases and approaches one, but it is not sufficient to have high goodness of fit. A valid
model should not have a large gap between R2X and Q2X [3, 26].
RR22X
Variance Explained
Q22X
Q
Cross validation is used to find the optimal model dimensionality and to test the
significance of a model. In CV, a portion of data is kept out of data set used for model
development. A number of parallel models are developed and used to predict the omitted
data and compare the predicted values with the actual ones. PRESS, prediction error sum
of the square difference between predicted and observed values, is a measure of the
predictive power of the tested model. In SIMCA P, CV is conducted for each consecutive
model dimension. For each additional dimension, PRESS is compared to the residual sum
20
of squares, RSS. When PRESS is not significantly smaller than RSS, the tested
Data Processing
Outliers (data points with abnormal operational conditions) are data points that are
usually located far from the other data points in the scatter plot and should be excluded
during model development to avoid result deformation. Outliers can negatively skew
process interruptions are some of the reasons behind the presence of outliers in large data
sets [11].
The data was screened using various multivariate analysis plots as well as
studying DModX and Hotelling T2 plots in SIMCA-P. DModX (Distance to the Model
deviation of the observation, and DModX values computed are specific to the dataset.
Observations with a DModX value twice as large as the DModX critical values are
outliers and are shown as spikes (Figure 9). Exclusion of these outliers from the dataset
through model processing, improves the model predictability. Hotelling’s T2 values are
computed for each observation as well. Hotelling’s T2 plot is used to define a 95% and
21
99% tolerance region and pinpoints the extreme outliers (Figure 10). Observations
outside the 95% ellipse defined by Hotelling’s T2 do not fit the model well either.
Detailed analysis of these outliers is necessary before removing them from the dataset.
33
22
DModX
D-Crit(0.05)
11
00
0 100 200 300
(Time) Days
Figure 9: A generic DModX plot with the horizontal line of D critical cutting points
22
60
50
40
Hotelling T2
30 T2Crit(99%)
T2Crit(95%)
20
10
0
0 100 Days 200 300
Figure 10: A generic Hotelling T2 plot with the horizontal lines of T2 critical cutting
points outside of the 95% and 99% confidence interval
In order to build a PLS model, variables of interest or variables that are hard or
costly to measure, are assigned as Y variable(s). In PCA, the principal components are
oriented in order to find the maximum variability in a dataset by projecting the process
time points onto a plane. On the other hand, in PLS the projection of X is done in a way
that it both approximates X well and correlates with Y. Thus the maximum covariance
between input and output variables is found [25]. A good PCA model could be converted
23
to a PLS model that best approximates the data and maximizes the relationship between
input and output variables [10]. PLS uses less principal components compare to PCA and
PLS provides various types of plots that can be used to assess the quality of a
model. Correlations are seen using coefficient plots. In the coefficient plots, X is centred
and scaled, while Y is scaled but not centred. The coefficient plot shows how strongly Y
is correlated to each input variable, X, since the data are scaled and centred, the
coefficients are comparable. A bar in the coefficient plot shows the correlation of each
input with that specific output, where bars above zero represented positive correlations,
and bars below zero represented negative correlations. If the error bar (the bar passing
through the correlation bar) passes through the zero line, a conclusive correlation has not
been found for that variable. From the arbitrary example, Figure 11, Y is positively
0.6
0.4
0.2
0
-0.2
Y -0.4
-0.6
-0.8
-1.0
-1.2
EVA PO R AT IO N AC R O SS E F F EC T S
ST EAM T E M P -#1 EF F EC T
M AN U AL VA LVE ST E AM -#1E F F EC T
X1 X2 X3 X4 X5 X6
24
Correlations found can be ranked based on their importance using the Variable
Importance for Projection, VIP plot (Figure 12). VIP compactly summarizes the
importance of X-variables both for the X and Y models. Not going into much detail
regarding mathematical formulas, VIP values are calculated for each x by summing the
squares of the PLS weights, wa, taking into account the amount of Y-varriance explained
in each dimension. There is always only one VIP for a given model and problem.
Observe that VIP values are all positive as it is a squared function of the PLS weights.
VIP values may be used for variable selection since variables larger than 1 indicate
“important” X variables, and values smaller than 0.8 indicate “unimportant” X variables
the model.
1.5
1.2
0.9
VIP
0.6
0.3
0
X1 X2 X3 X4 X5 X6
25
3. Methodology
This project consisted of three main tasks, mill visits, multivariate data analysis, and
dynamic simulation.
One week was spent at each of the two mills under study to accomplish the first
task. During this time, process flow sheets, P&IDs and guided tours of the mill helped to
better understand the process. Consulting with operators in the control room and
engineers on site facilitate recognizing the problem of scaling and thermal performance
of evaporators. The severity of the problem, the locations of occurrence, and procedure
taken to resolve the problem were among the topics explored in the visits to the mills. For
passing water or weak black liquor (low solids content) through them. This process is
The second task was to employ multivariate data analysis in order to determine
factors affecting thermal performance of evaporators and scaling. First, a list of variables
that may affect thermal performance and scaling of evaporators was created with the help
of a number of experts in the field. Second, daily averages for a period of one year were
collected for the selected variables. Third, the commercially available MVDA software,
SIMCA-P was used to determine correlations between scaling and operating conditions
of black liquor evaporators, processed mill data. This task was done for both mills, and is
26
The third task was to conduct dynamic simulation by CADSIM software. This
software has been used successfully for conducting experiments in heat and mass balance
in pulp and paper mills [27, 28]. After building the model of evaporation system in
CADSIM, process changes can be applied based on the MVDA results (what/if
scenarios) to verify the MVDA results, and to find the optimum operating conditions.
This task was only carried out for Mill A, due to insufficient data obtained Mill B.
27
4. Results and Discussion
The results of the mill visits, MVDA, and dynamic simulation of Mill A are presented in
The black liquor evaporation system at Mill A is a 1990 HPD unit consisting of a
five-effect falling film type evaporator, a 58% liquor flash tank, a high solids
concentrator (HSC), and a 70% liquor flash tank (Figure 13 and Figure 14). The system
was designed to process 467 metric tons/hr weak black liquor at 13.5% solids and 85°C
to produce 109 tons/hr of strong black liquor at 58% solids and 115°C during hardwood
pulping, and 15% more liquor during softwood pulping. In the past few years, however, it
The purpose of the evaporator system is to circulate liquor from the weak black
liquor storage tank through the five effects to 58% product storage. The circulation is at
such a rate that as much water and NCG's (non-condensable gases) as possible are boiled
The evaporation system starts with weak black liquor (WBL) from the brown
stock washers entering No. 1 and No. 2 WBL storage tanks. Weak black liquor is
received from the digesters after the pulp fibres have been washed in the brown stock
28
washers. WBL contains about 14 - 16% dried solids, which contains the inorganic
(Na2S), sodium sulphate (Na2SO4), calcium carbonate (CaCO3) and silicates. These
chemicals are the result of chemical reactions, which take place in the digester cooking
economically because they are costly to replace. By utilizing the evaporation process the
liquor can be concentrated to a density suitable for burning in the recovery boiler, where
Black liquor is useful as a fuel because it also contains organic compounds such
as lignin and tannins. These compounds give the liquor a heating value of about 14.5
multiple effects. These effects are shell and tube heat exchangers, which are connected by
vapour piping so that the water boiled off the liquor in the first effect, acts as heating
steam in the steam chest of the following effect. The liquor basically follows a reverse
One of two transfer pumps to the weak liquor flash tank, where solids
concentration is increased slightly, pumps the weak black liquor from the storage tanks.
(Figure 13) The liquor flows to the 5th effect vapour body where it is concentrated to
17% solids. The liquor flows through without a pump (by gravity) as the 5th effect
vapour body is at a lower pressure than the flash tank. The 5th effect recirculation pump
29
continuously circulates liquor through the 5th effect. From the 5th effect, the liquor is
pumped through a level control valve on the 5th effect to the suction line of 4th effect
recirculation pump.
Figure 13: Black liquor flow path through evaporation system at Mill A
4th effect concentrates the liquor to 21% solids. A transfer pump draws liquor off
the suction line of the 4th effect recirculation pump and pumps it through either the
secondary reflux condenser or through the secondary reflux condenser bypass line to the
2nd effect vapour body. The secondary reflux condenser heats the liquor to 91°C. The
2nd effect concentrates the liquor to 27% solids. Liquor is recirculated through the 2nd
30
effect by the 2nd effect recirculation pump. From the 2nd effect the liquor flows to No. 2
The liquor is pumped from the flash tank to the soap skimming tank. The purpose
of the evaporator soap system is to recover tall oil soap from various points in the black
liquor system and to deliver this soap to the recovery boiler for incineration. This is
necessary to maintain the efficiency of the evaporator and concentrator heating surfaces
After soap removal, the liquor is pumped to the 3rd effect vapour body. Liquor is
recirculated through the effect with 3rd effect recirculation pump, concentrating the liquor
to 39% solids. The 3rd effect transfer pump draws liquor off the recirculation pump
suction line and pumps it through the primary reflux condenser to the 1st effect vapour
The 1st effect concentrates the liquor to 58 - 62% solids. The liquor is circulated
through the 1st effect by the 1st effect recirculation pump. Liquor, from the 1st effect,
flows into the 58% flash tank where the liquor temperature is reduced to 115°C. Liquor is
pumped from the flash tank by the 1st effect transfer pump to the 58% storage tank. The
name of the flash tank is an indication of approximate solids content of the liquor inside
it.
31
After the 58% storage tank, black liquor is further concentrated in the High Solids
Concentrator. HSC is composed of two heathers and a flash tank. Liquor concentration
Steam Flow:
Saturated steam enters the system at 325 kPa (143°C) through the HSC and the
1st effect. The vapour from the 1st effect is used as a steam source to concentrate the
liquor in the 2nd effect. The resulting vapour from the 2nd effect is, in turn, used to
concentrate the liquor in the 3rd effect, and so on. The same process principle is carried
through the 4th effect and the 5th effect. Steam pressure and temperature decreases as it
travels through the effects. The final vapour from the 5th effect is condensed in the
surface condenser to create a vacuum of –70 kPa to help drive steam and vapour through
Steam Primary
Reflux
TW
condenser
Cond. CW MW
SC
WW
HSC 1 2 3 4 5 WBL
FT
MW: Mill Water, TW: Tempering Water, CW: Cooling water, WW: Warm Water, Cond.: Condensate,
WBL: Weak Black Liquor, FT: Flash Tank, ST: Storage Tank, HSC: High Solids Concentrator
Figure 14: Schematic drawing of evaporator system at Mill A
32
At the outlet of the vapour system, there is a surface condenser, a shell and tube
heat exchanger that has cold mill water on the tube side and vapour out of the 5th effect
on the shell side. In this case the primary purpose of the surface condenser is to cool and
condense the vapour from the 5th effect and, in doing so, create a vacuum of
approximately -70 kPa in the 5th effect. The other effects have progressively higher
pressure where 1st effect operates at about 105 kPa of pressure. As the pressure decreases
through the evaporators (first to last), so does the boiling point of the water in the liquor,
4.1.2. MVDA
Daily average data of nearly 100 variables for a one-year period (January 1 to
December 31, 2007) were collected and analyzed using multivariate data analysis
A complete list of variables with their average, minimum and maximum values, and
standard deviation is provided in Appendix 3. These variables are categorized into three
groups: operational conditions around evaporators, mill production properties, and black
liquor properties.
Data Processing
The data was screened using various multivariate analysis plots and considering some
operation criterion. For example, periods of evaporator downtime due to cleaning were
taken out of data. Periods of start ups and shut downs were also taken out by studying
33
time series plots (graphs of the daily average of each variable during the investigation
period of the year 2007), eliminating the periods of abnormal operation for evaporators.
For example, if the average amount of steam temperature to the 1st effect was 139 °C,
data points with steam temperature of 20°C were definitely not acceptable (abnormal),
and were therefore excluded. As the purpose of this project is to observe important
(outliers) were necessary. Outliers are data points that are usually located far from the
other data points in the scatter plot, and were excluded during model development. An
example of an outlier is shown in Figure 15, marked by an arrow in the top left corner.
20
10
t(2)
-10
-60 -50 -40 -30 -20 -10 0 10
t(1)
Figure 15: Scatter plot showing an outlier in a red box at the top left corner
each outlier was investigated before its exclusion. Analysis of the coefficient plot of the
outlier marked in Figure 15, Figure 16, revealed that it had a lower recirculation
temperature, recirculation pump load and black liquor temperature to HSC, compared to
34
-20
-10
0
10
20
Production Rate
PRODUCTION
Chipmeter Speed
CHIP METER
WBL Storage Tank #1
WBL Storage Tank #2
WBL Flow to Flash Tank
WBL % Solids to Flash Tank
arrows).
Mass Flow BL Solids to Evaporators
WBL Temperature to 5th Effect
5th Effect Recirculation Temperature
4th Effect Recirculation Temperature
2nd Effect Recirculation Temperature
3rd Effect Recirculation Temperature
1st Effect Recirculation Temperature
5th Effect Level
4th Effect Level
2nd Effect Level
3rd Effect Level
1st Effect Level
5th Effect Recirculation Pump Load
4th Effect Recirculation Pump Load
2nd Effect Recirculation Pump Load
3rd Effect Recirculation Pump Load
1st Effect Recirculation Pump Load
Steam Flow to 1st Effect
Steam Temperature to 1st Effect
Steam Pressure to Evaporators
Control Valve Steam to 1st Effect
Manual Valve Steam to 1st Effect
1st Effect Vapour Pressure
2nd Effect Vapour Pressure
3rd Effect Vapour Pressure
4th Effect Vapour Pressure
5th Effect Vapour Pressure
Surface Condenser Pressure
1st Effect Boiling Point Rise
Evaporation Across Effects
Steam Economy Across Effects
Cooling Water Flow to SC
Tempering Water Flow to SC
TMPERING W
Mill Water Temperature to SC
Warm Water Temperature from SC
Clean Condensate Conductivity
Combined CondensateCOMBINED ConductivityC
Foul condensate
FOULConductivity
CONDE
2nd Effect Flash Tank Level
SBL Temp. Soap Skimmer Tank
2nd Effect Transfer Pump Load
Soap Skimmer Tank Level
Skimmed Liquor Pump Load
58% BL Storage Tank Level
58% Flash Tank Level
58% Flash Tank Discharge Temperature
BL Flow to HSC
Saltcake Addition
SBL % Solids
BL Temperature Into N. HSC Heater
BL Temperature Into S. HSC Heater
BL Temperature Out of N. HSC Heater
BL Temperature Out of S. HSC Heater
HSC Pressure
HSC Boiling Point Rise
Steam Flow to HSC Heaters
Steam Temperature to HSC Heaters
Steam Pressure to HSC Desuperheater
Control Valve Steam to HSC Heaters
Manual Valve Steam to HSC Heaters
Evaporation N. HSC Stem Mass Flow
Evaporation S. HSC Stem Mass Flow
Evaporation Across HSC
Hotelling’s T2 plot do not fit the model well either (Figure 10). Each of the outliers are
fit the model well (Figure 9). Observations outside the 95% ellipse defined by the
show the moderate outliers. For DModX, observations above the critical distance do not
plots in SIMCA-P (DModX, Hotelling T2, and Coefficient plot), and time series plot
35
represent abnormality in the system. Outliers were determined through studying various
In summary, the model development was carried out by excluding outliers which
(daily average values for each variable vs. time). DModX (Distance to the Model X)
Latent Heat of Water Out
CPwl
Q- Total Heat Transferred in Evaps
delta T
U- Overall Heat Transfer Coefficient
Wevap/Chipmeter Speed
U/Chipmeter
U/CHIPSpeed MET
Input Variables:
In multivariate data analysis, X variables are independent input variables that are
measured at the mill, and may have an effect on the thermal performance of evaporators
and scaling. Typical variables investigated in analysis of black liquor evaporators include
recirculation flow rate of black liquor, chemistry of black liquor such as carbonate to
sulphate mol ratio (C:S) and temperature. A list of input variables for this project was
decided based on the previous studies [6], and consultation with engineers at the mill.
Input variables include black liquor flow rate, temperature, and % solids; steam flow rate,
temperature, and pressure; total titratable alkali (TTA), % causticity, type of species used
(softwood vs. hardwood), kappa number, green liquor reduction, and effective alkali
Output Variables:
accommodate multiple outputs at once. Based on the mill experience, 4 Y variables are
used in this analysis. A brief description of each output variable with their relation to
system is its capability to evaporate water as measured by the evaporation rate, or more
appropriately, by the overall heat transfer coefficient. Since the objective of the
36
multivariate analysis is to look at the effects of scaling on evaporator performance, the
A high U value means the system is operating well, with a high rate of heat transfer.
The liquor level in the 58% flash tank indirectly indicates the extent of scaling in
the system. As scale forms around the vortex breaker in the 58% flash tank and in the
piping downstream of the 58% flash tank, it obstructs the liquor flow out of the 58% flash
tank. This causes the liquor level in the flash tank to increase until the flash tank is
37
flooded. A high liquor level in the 58% flash tank is an indication that scale deposition
has accumulated to the point where 58% flash tank level control has been lost.
The level of the 58% FT is controlled with a flow control valve on the liquor
outlet line of the flash tank. The operator selects a level set point: if the level indication
exceeds this set point, the valve will open to increase liquor flow out of the flash tank; if
the level indication falls below this set point, the valve will close to decrease liquor flow
out of the flash tank. The position of this control valve can be used as an indication of
scaling in the outlet of the 58% flash tank and/or the liquor line between the 58% flash
If scale builds up in the outlet of the 58% flash tank and/or in the liquor line
between the 58% flash tank and the control valve, it will restrict the liquor flow from the
flash tank, causing the flash tank level to rise in response to the changes. The flow control
valve will open up to increase liquor flow out of the flash tank. Eventually the control
valve position will reach 100%, and the flash tank level will keep rising until it is out of
control. At this point, the mill faces two options: i) reducing evaporation rate (amount of
water evaporated in the system) to reduce the amount of liquor going through the flash
tank; ii) performing a boil-out on the 1st effect and the flash tank together to remove the
scale build-up.
Liquor temperature at the discharge line out of the 58% flash tank is an indicator
for performance of the 58% flash tank. This temperature indirectly indicates scaling in
the system. As scale accumulates in the system and the level in the flash tank rises, the
38
pressure in the flash tank increases, making it more difficult for the liquor to flash.
Liquor leaving the first effect is fed to the 58% flash tank. In the flash tank, pressure is
reduced in order for the vapour to be flashed and separated from the liquor, resulting in
reduction in the liquor temperature. Once the flash tank is flooded due to scale
temperature.
Once flashing is no longer occurring in the 58% flash tank and hotter liquor is
exiting the flash tank as a result, flashing begins to occur in the atmospheric 58% storage
tank. The 58% storage tank is vented into the HVLC NCG (High Volume Low
via a separate vent line. Sufficient flashing in the 58% storage tank will cause the storage
tank to become pressurised. As the pressure in the storage tank reaches a pressure
sufficient to overcome the water seal in the pressure vacuum breaker, the water seal will
blow out and the tank will vent to atmosphere as well as to the HVLC NCG system.
suddenly spikes, venting to atmosphere is occurring, since this is normally just a measure
of atmospheric temperature. Once the gas has been vented, the pressure decreases causing
the water seal in the pressure vacuum breaker to reseal and the storage tank atmospheric
vent temperature to decrease. Thus, more frequent excursions of the 58% storage tank
39
Using these output variables, the performance of the evaporator system at Mill A
is expected to be directly related to the heat transfer coefficient across the effects, and
inversely related to the 58% flash tank liquor level, and the 58% tank discharge
temperature, and the 58% storage tank vent gas temperature. Performance of the
evaporators has an inverse relation with the scaling in the evaporators and need of boil-
out.
4.1.2.1 PCA
from January 2007 to January 2008. Seven principal components were calculated through
cross-validation accounting for 68% of the variability in the data. The first and second
principal components captured most of the variability in the data with 25% and 14% of
the total variability respectively. They can be plotted as the axes on a two-dimensional
graph, and the data points can be projected over these axes as a scatter plot, as shown in
Figure 17. The x-axis axis (or t[1]) of the plot represents the first principal component,
while the y-axis (or t[2]) the second. Each dot on the chart represents the information
generated from daily averages of all 98 variables for a specific day during the 12 month
period. It is numbered according to its date of the year, i.e. 1 means January 1, 2007, 32
means February 1, 2007 and so on. The ellipse represents a 95% confidence interval of
the data. The center (origin; 0,0) of the graph represents the average value across all 98
variables. The majority of the data points fall within the 95% confidence interval
indicating that the data can be used to build a good PLS model (Figure 17).
40
289
223
169 240 202
183
284 253 188191 167
282 201
5 3 286 287 165
168
164 171
271 272 273 45 205
281 283 252
290 5 187 221 254241 186 185 184
239
247 220 242163222
323 270 218
2 216
256
249 255 219 224
269 334 136 275 129 288
251 246 130 244 190243 225 203
332
250 40
67 128127245 24842 200
212 182
276 333 161 34 4 189 209 210
204
93
123 162 126 226
279
277 274 257
68 217291 699 61
122 94
215 95 38 125 208
280 278 214 8
199 69 213 172
15 211
262 358 292 326 65 104 103
258 352
312 320 121102 107
72 105 207 96
35 62 921239
331 314227
318
335 75 133 131
4364 132
206 11
268 309 356 63
198197 196 313 1 100 10
t[2]
362 361
336 363 120 181 71
76324325 97 13 7 9
0 267 340 238
308 349
337 319
315
194195 321 91 70 33327 98 16 14 41 36
106 37
299 146 322 346 345 108
66 73
265 348 317 347 316 193
32
351
355 350 259 60 364
365 74
339 353 357 330 329
175
237 266 338307 137
173 109 328
236 354 260 135
235 231
264 77 139
293 232 110
359 134 17
295 233 294 118119 176177 230
141
174 360
342 234 17918 180
50 11711490 113 229140
111 178
26114282 147
79 49 54138
341 3001458826 144 56
297296 263 112 55
298 83 80
-5 306 302 344
87 28 29
143
116
2352 57
24
303 343 89 58 22
301 78 30 31 27 21 59
305
304 86 25
85 81 84 20 19
In the scatter plot, trends, unusual behaviours, and other useful information were
seen. This was the best summary of the process behaviour, and was useful in the process
of building the PLS model. The majority of the data points fell within the 95%
confidence interval, indicating good performance of the model. The developed model had
R2 of 0.83 and Q2 of 0.63, indicating good predictability of the model. The loading plot,
Figure 18, helped interpreting the PCA model. The influence of variables and correlations
among them were revealed based on their position in the loading plot. For Mill A, the
influential variables, indicated by their positions further away from origin, were steam
quality (temperature, pressure and flow) to HSC, the type of wood species fed to digester
and product black liquor % solids. Analysis of scatter and loading plot revealed that data
points in the third quadrant (III) had a higher steam pressure, temperature, and flow to
evaporators, a higher WBL flow rate to weak liquor flash tank and a higher evaporation
across effects compare to the average.(variables are shown by arrows in Figure 18) Data
41
points in second quadrant (II) had a higher steam pressure, temperature, and flow rate to
HSC, a higher HSC boiling point rise, and higher product BL % solids compare to the
average.
TOTAL EA TO WOOD
-0.2 STEAM TEMP -#1 EFFECT
70% FLASH TANK VAPOUR PRESSURE STEAM PRESSURE TO EVAPS
4.1.2.2 PLS
A PLS model was built based on the above PCA model by assigning the overall
heat transfer coefficient U, 58% flash tank level, 58% flash tank discharge temperature,
and 58% storage tank vent temperature as output variables. Through the analysis, eight
principal components were calculated through cross-validation accounting for 78% of the
variability in the data. Correlations between input variables and each output variable were
shown in Figure 19, which correlates the overall heat transfer coefficient U with the top
15 input variables. Each output variable has its unique coefficient plot, where a bar shows
42
the correlation of each input with that specific output. As explained in section 2.4.2, the
height of each bar represents the strength of the correlation, i.e. a higher bar means a
stronger correlation. Variables represented by bars above the zero line are those that have
a positive correlation with U, whereas variables represented by bars below the zero line
are those with a negative correlation. For a given input variable, if its error bar crosses the
zero line, its correlation with the output variable is considered to be none or statically
unreliable.
From Figure 19 can be concluded that the heat transfer coefficient was positively
correlated with the weak black liquor flow to the weak liquor flash tank and was
negatively correlated with the WBL % solids to the weak liquor flash tank. Similarly,
-5
-10
Cooling Water Flow to SC
Figure 19: Coefficient plot for the heat transfer coefficient of Mill A
43
The summary of correlations among variables is presented in Table 2. The
number of variables affecting evaporator performance was reduced from nearly 100
Table 2: Correlations between output variables and top 10 input for Mill A
Output variables
58% Flash 58%
U- Heat 58% Flash
Rank Variables Tank Storage
Transfer Tank
Discharge Tank Vent
Coefficient Level
Temp Temp
1 Tempering Water Flow To SC, [L/s] -2.2 -1.7 -3.4
2 Total Water Evaporated Across Evaporators, [kg/hr] 5
3 WBL % Solids – Weak Liquor FT, [% solids] -3.3
4 Cooling Water Flow To SC, [L/s] 2.3 2.5
5 Steam Pressure To Evaporators, [kPa] -3.0 -1.1
6 4th Effect Recirculation Pump Load, [% load] 1.8
7 WBL Flow To Weak Liquor FT, [L/s] 3.7 -1.4
8 Mill Water Temperature To SC, [°C] -1.4
9 2nd Effect Transfer Pump Load, [% load] 2.3
10 Effective Alkali (EA) 2.9
Notes: FT=Flash Tank, SC=Surface Condenser, Blank=No correlation
Table 2 summarizes the correlations between each output variable and the top 10
important input variables. The number in each cell indicates the relative strength of the
correlation between the input variable (row) and the output variable (column) of that cell.
The numbers are specific to the model and are scaled to 5 for easier comparison. A higher
number indicates a stronger correlation, while the + and - signs that precede the number
respectively indicate positive and negative correlations. Blank cells (cells with no
44
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
1.8
2.0
Tempering Water TMPERING
Flow to SCW
Steam Temp to 1st Effect
Evaporation Across Effects
WBL % Solids to FT
Steam Flow to 1st Effect
Cooling Water Flow to SC
Steam Pressure to Evaporators
4th Effect Recirculation Pump Load
WBL Flow to FT
Manual Valve Steam to 1st Effect
Mill Water Temperature to SC
1st Effect Boiling Point Rise
Warm Water Temp from SC
2nd Effect Transfer Pump Load
70% BL ST #2 Level
ProductPRODUCT
BL % Solids BL
Mass Flow BL Solids to Evaps
WBL Temp to 5th Effect
Wash Residual EA
Evaporation S. HSC Steam Mass Flow
2nd Effect Recirculation Pump Load
Steam Flow to HSC Heater
5th Effect Vapour Pressure
45
Below, the results of main correlations for each of the four output variables,
and effect relations and are rather the result of change in combination of input variables.
water evaporated across effects, the cooling water flow rate to the surface condenser, and
the weak black liquor flow rate to the weak liquor flash tank. The heat transfer coefficient
was found to be negatively correlated with the % solids of the WBL and the steam
pressure to evaporators.
The heat transfer coefficient was a calculated variable in this study, as explained
in section 4.1.2. It is noteworthy that some of the input variables were involved in the
calculation of the heat transfer coefficient, and thus their observed correlations in the
model were expected theoretically. The heat transfer coefficient, U, was calculated based
Q Wevap λ o + WWL Cp WL (To − Ti )
on Equation 1, U = = . As a result, U would be expected to
A ∆T A (TSat − TCond . − ∑ BPR )
correlate positively with evaporation rate and weak liquor flow rate since both are in the
numerator. Also U would be expected to correlate negatively with steam pressure since
These correlations were found through multivariate data analysis as well. Nonetheless,
finding the expected correlations supports the validity of model and its results.
MVDA showed positive correlations for the cooling water flow rate to the surface
condenser with the heat transfer coefficient. The operation of the surface condenser has a
great influence on the performance and efficiency of the evaporators and, consequently,
scaling in them. There are two choices for maximizing the efficiency of the multiple
effect evaporators: i) increasing the temperature of steam to the 1st effect (which can
result a radical increase in scaling in tubes), and ii) lowering the pressure in the effects.
46
Lowering the evaporator pressure subsequently lowers the boiling point rise of the liquor.
This allows boiling to occur at lower temperatures, thus enabling the system to extract
more heat energy out of the vapor and use it efficiently. Since the surface condenser
condenses the vapor faster than vapor chest of evaporators due to the use of cooling water
as a cooling medium, the cooling water flow rate and temperature are important variables
regarding performance of the surface condenser. The surface condenser is operated under
vacuum in order to lower the pressure in the effects. This is the prime purpose of the
surface condenser. The second purpose of the surface condenser is to condense the vapor.
The last purpose is to act as a heat exchanger. The water used to condense the vapor picks
up the heat and this warm water is then transferred to the warm water tank in pulping.
The heat transfer coefficient was found to be negatively correlated with the %
solids of the WBL and the steam pressure to evaporators. Fewer solids mean the presence
of more water in the system. The explanation behind the increase in the heat transfer
coefficient with the decrease in the WBL % solids may be that the extra water passing
through tubes reduces chance of solids build up. As a result less solids form scale in the
tubes and the heat transfer coefficient and performance of the evaporators is improved.
A decrease in the steam pressure correlated with increase in the heat transfer
coefficient. Lower pressure saturated steam has lower temperature. This results in a
47
∆T decreases, the heat transfer coefficient increases (Q=UA∆T), explaining the negative
2. The 58% flash tank level was positively correlated with the effective alkali
(EA). This may be explained by the fact that a higher EA means a higher boiling point
rise of the liquor, making it more difficult to flash in the flash tank and thus resulting in a
The 58% flash tank level was negatively correlated with the tempering water flow
rate to the surface condenser, the steam pressure to the evaporators, and the mill water
temperature to the surface condenser. The tempering water is added to the mill water to
surface condenser to regulate the cooling water flow to surface condenser. The tempering
water flow is typically low during winter months. Since the tempering water is remote
from the 58% flash tank, the negative correlation between the tempering water flow and
the 58% flash tank level suggest that the scaling problem around the 58% flash tank was
3. The 58% flash tank discharge temperature is positively correlated with the 4th
effect recirculation pump load, and the 2nd effect transfer pump load. This may be
explained by the fact that as the system fouls up, the liquor needs to be circulated at a
higher rate in these effects in order to achieve the same thermal efficiency.
48
The 58% flash tank discharge temperature is negatively correlated with the
tempering water flow to the surface condenser. Warmer months, with higher tempering
water flow rate, seem to perform better. This result is in agreement with the correlation
found for the other output, the 58% flash tank level.
4. The 58% storage tank vent temperature is positively correlated with the cooling
water flow rate to the surface condenser. This is understandable, since both high 58%
storage tank vent temperature and high cooling water flow rate can be caused by scaling
around the 58% flash tank and storage tank. As scaling becomes more severe, the vent
temperature increases as explained earlier. The system therefore requires more cooling
water to maintain sufficient vacuum in the 5th Effect to be effective. Interestingly, the
surface condenser and the 58% storage tank are located far from each other in the
The 58% storage tank vent temperature is negatively correlated with the
tempering water flow rate to the surface condenser, and the weak black liquor flow rate to
the weak liquor flash tank. Here again in warm months, with higher tempering water flow
rate, seem to have less vent leaving the 58% storage tank. The study also shows that it is
more desirable to have a higher weak black liquor flow rate to the weak liquor flash tank,
since the system experiences less vent incidents under this condition.
Considering all the correlations simultaneously, Table 2, it can be seen that some
of the input variables showed correlation with more than one output and were more
49
dominant in the model. The water flow rate to the surface condenser, the weak black
liquor % solids, and the weak black liquor flow rate to the evaporators were found to be
the dominant parameters in the PLS model of the evaporators of this mill based on the
loading plot and the VIP plot. These variables have both high weights in the loading plot,
and rank high in the VIP plot. The output variables were different measures of a similar
phenomenon of possible scaling and pluggage in the evaporation system. Therefore, input
variables that show common correlations to the output variables deserve more attention.
These variables were further analysed in the dynamic simulation model for optimization
Among the correlations found by MVDA, some were more interesting for the mill
personnel including the relation between effective alkali (EA) and the heat transfer
coefficient, water flows in the surface condenser and problems in the 58% tanks. On the
other hand, some correlations such as relation between the heat transfer coefficient and
WBL flow rate also were predicted by the heat transfer formula, Equation 1, and may
50
Effect of Data Intervals
Correlations captured by MVDA models are highly dependent on the data used.
Frequency of collected data can significantly affect the results of analysis [3]. For this
project, daily averages of operational variables were used. The time interval of one day
was selected since it was believed to be sufficient for studying the evaporator operation,
according to mill experts. However, in order to test the appropriateness of the frequency
of data, smaller intervals of data were also analysed. The results of analysis for daily and
hourly averages for the months of October and November for Mill A are shown in Table
3 and Table 4.
Table 3: MVDA results of daily average for period of Oct-Nov 2007 Mill A
Output Variables
Rank Input Variables U - Heat 58% Storage 58% Flash 58% Flash
Transfer Tank Vent Tank Discharge Tank Level
Coefficient Temperature Temperature
1 Caustic Flow to White Liquor ST -4.4 -3.8
2 Surface Condenser Pressure 4.2
3 Steam Flow to 1st Effect -0.7 -1.0
4 WBL Flow to Weak Liquor FT 1.2
5 Foul Cond. Temp to Stripper Pre-heater 3.0 5.0
6 2nd Effect Recirculation Pump Load -1.3
7 Cooling Water Flow to SC 1.2
8 Tempering Water Flow to SC -2.4
9 WBL % Solids to Weak Liquor FT -1.8
10 1st Effect Level -3.1 -3.7
Notes: ST=Storage Tank, FT=Flash Tank, Cond.=Condensate, Temp.=Temperature, SC=Surface Condenser, Blank=No correlation
51
Five of the top ten significant variables, numbers 1, 4, 7, 8 and 9 in Table 3, were
common for both analyses. The rest of the important variables found in the analysis of the
hourly average data, which were not in the top 10 variables of the daily analysis, were in
agreement with the results obtained from the daily average data as well. Both analyses
demonstrated same trend and agreeable correlations. It was concluded that using daily
averages data for the multiple effect evaporators was an adequate time interval.
Table 4: MVDA results of hourly average for period of Oct-Nov 2007 Mill A
Output Variables
52
4.1.2.3 Time Series Plots:
In time series plots, daily average values of variables were plotted vs. time for the
year 2007. A line passing thorough the data points of these plots showed the overall
average value over the year. Data points falling above the average line had values higher
than the average and those below the line had values lower than the average value for that
plots of periods of higher and lower amounts of the output variables in comparison to
800
700
U (KJ/m hr-C)
2
600
500
400
1/1/07 1/4/07 30/6/07 28/9/07 27/12/07
Date
53
The average value of the overall heat transfer coefficient is 560 kJ/(m2h°C),
ranging between 0 and 1324 kJ/m2h°C. It was high, about 660 kJ/(m2h°C), during the
months of May and June, and low, about 540 kJ/(m2h°C) during the month of September.
Since the heat transfer coefficient is inversely related to scaling, a higher value is desired
Figure 22 shows contribution plots for periods with high and low heat transfer
coefficients. Input variables that have opposite relations for the high and low U periods
are more interesting. As an example, looking at the fourth input variable from left to right
in Figure 22, WBL flow to flash tank, was above average (indicated by a bar above zero
line) during periods with high U, and below average during periods with low U. It was
therefore concluded that weak black liquor flow rate to flash tank was related to the heat
transfer coefficient. Input variables with opposing values were the interesting variables in
this study. From Figure 22, high U periods operated at a lower WBL % solids to flash
tank, and a lower recirculation pump load, a higher steam temperature, pressure and flow
rate to the 1st effect, a higher WBL flow rate to the flash tank, a higher cooling water flow
rate to the surface condenser, a higher WBL temperature to the 5th effect, and higher
vapour pressure in effects than during the low heat transfer period.
54
Low U Period High U Period
0
0
-1
0
1
-3
-2
-1
0
1
2
Chipmeter Speed
WBL Storage Tank #1
WBL Storage Tank #2
WBL Flow to Flash Tank
WBL % Solids to Flash Tank
BL Mass Flow to Evaporators
WBL Temperature to 5th Effect
5th Effect Recirc. Temperature
4th Effect Recirc. Temperature
2nd Effect Recirc. Temperature
summarized below.
transfer coefficient
3rd Effect Recirc. Temperature
1st Effect Recirc. Temperature
5th Effect Level
2nd Effect Level
5th Effect Recirc. Pump Load
4th Effect Recirc. Pump Load
2nd Effect Recirc. Pump Load
3rd Effect Recirc. Pump Load
1st Effect Recirc. Pump Load
Steam Flow to 1st Effect
Steam Temperature to 1st Effect
Steam Pressure to Evaporators
Manual Valve Steam to 1st Effect
1st Effect Vapour Pressure
2nd Effect Vapour Pressure
3rd Effect Vapour Pressure
4th Effect Vapour Pressure
5th Effect Vapour Pressure
Surface Condenser Pressure
1st Effect Boiling Point Rise
Evaporation across Effects
Cooling Water Flow to SC
Tempering Water Flow to SC
Mill Water Temperature to SC
Warm Water Temp. from SC
Clean Condensate Conductivity
Combined Condensate Conductivity
Foul condensate Conductivity
2nd Effect Flash Tank Level
SBL Temp. -Soap Skimmer Tank
2nd Effect Transfer Pump Load
Soap Skimmer Tank Level
58% BL Storage Tank Level
BL Flow to HSC
SBL % Solids
BL Temp. to N. HSC Heater
BL Temp. to S. HSC Heater
BL Temp. from N. HSC Heater
BL Temp. from S. HSC Heater
HSC Pressure
HSC Boiling Point Rise
Steam Flow to HSC Heaters
Steam Temp. to HSC Heaters
Steam Pressure to HSC De-SH
Control Valve Steam to HSC Heaters
Manual Valve Steam to HSC Heaters
N. HSC Steam Mass Flow
S. HSC Steam Mass Flow
condenser, and a higher steam flow rate and temperature to the HSC heaters.
Evaporation across HSC
70% BL Storage Tank Temperature
70% Flash Tank Vapour Pressure
Product BL % Solids
70% BL Storage Tank #1 Level
70% BL Storage Tank #2 Level
1100 KPa Steam Flow to Ejectors
Figure 22: Comparison of contribution plots for periods with high and low heat
55
The average value of the 58% flash tank level is 52%, ranging between 0 and 91%
effective alkali-to-wood ratio, a higher tempering water flow rate to the surface
to scaling in the flash tank. Days with low 58% flash tank level (good days) had a lower
(Figure 23). A high 58% flash tank level indicates improper flashing which could be due
Similarly, periods of higher and lower amounts of the other output variables in
% Causticity
EA-to-Wood
Species into Chipmeter
MCC EA
Wash Residual EA
KAPPA #
58% FT Level (% Level) 100
80
60
40
20
1/1/07 1/4/07 30/6/07 28/9/07 27/12/07
Date
Figure 23: Time series plot of the 58% flash tank level
The average value of the 58% flash tank discharge temperature is 118°C, ranging
between 15 and 127 ° (Figure 24). Days with low 58% flash tank discharge temperature,
good days, had similar contribution plots as days with high 58% flash tank discharge
temperature (bad days). Good days had slightly lower product BL % solids and relatively
56
130
58% FT Discharge Temp (oC)
120
110
100
1/1/07 1/4/07 30/6/07 28/9/07 27/12/07
Date
Figure 24: Time series plot of the 58% flash tank discharge temperature
The average value of the 58% storage tank vent temperature is 26°C, ranging
between 12 and 48 °C (Figure 25). Days with low 58% storage tank vent temperature,
good days, had lower warm water temperature from surface condenser, a lower effective
alkali-to-wood flow rate, a lower product BL % solids, a lower 5th effect vapour
pressure, and a lower 1st effect recirculation pump load. These days had a higher
tempering water flow rate to the surface condenser, a higher steam pressure to
57
50
58% BL ST Vent Temp (oC)
40
30
20
10
0
1/1/07 1/4/07 30/6/07 28/9/07 27/12/07
Date
Figure 25: Time series plot of the 58% black storage tank vent temperature
Information obtained from the time series plots can help mill personnel with
running the mill. The coefficient plots for good and bad days revealed which variables
were significant and determined their correlation to each of the output variables.
Application of these findings and control of significant variables forces the mill to fall
In addition to multivariate data analysis, mass and heat balance was performed on
the evaporation system of Mill A using CADSIM, a windows application that allows one
to create a process flowsheet drawing, add process information, and then run the process
as a simulation [28]. (Figure 26) Process simulation in CADSIM was carried out to verify
the MVDA results and to find the optimum operation conditions. What/if scenarios were
58
conducted for a number of important variables using CADSIM model based on the
MVDA results. This was done by increasing or decreasing the average amount of one
selected variable at a time and observing the effects on the system, mainly on the output
variables. For example PLS found a negative correlation between the heat transfer
coefficient and the WBL % solids, thus the WBL % solids was reduced and changes on
Comparing measured data with the calculated data from the CADSIM model
59
Table 5: Comparison of measured data with calculated data from simulation model of Mill A
Average Value Value
Variables Unit
Measured Calculated
WBL % Solids – Weak Liquor Flash Tank % solids 15.2 15.2
Mass Flow BL Solids To Evaporators t/hr 83.1 83.1
#5 Effect Recirculation Temperature °C 73 75
#4 Effect Recirculation Temperature °C 82 85
#3 Effect Recirculation Temperature °C 107 101
#2 Effect Recirculation Temperature °C 111 113
#1 Effect Recirculation Temperature °C 136 132
Steam Flow To #1 Effect t/hr 76.2 78.4
Steam Flow To HSC Heater t/hr 19.3 24.9
Steam Temperature To HSC Heaters °C 146 143
Steam Pressure To HSC Heaters Desuperheater kPa 338 395
#1 Effect Vapour Pressure kPa 103 101
#2 Effect Vapour Pressure kPa 43 40
#3 Effect Vapour Pressure kPa -12 -14
#4 Effect Vapour Pressure kPa -47 -48
#5 Effect Vapour Pressure kPa -64 -66
BL Flow To HSC (Liquid volumetric) L/s 26 28
58% Flash Tank Discharge Temperature °C 118 120
SBL % Solids % solids 59 59
BL Temperature Outlet HSC Heaters °C 139 138
HSC Pressure kPa 101 101
Steam Economy Across Effects & HSC 4 3.9
Product BL % Solids % solids 71 71
Total Water Evaporated Across Evaporators t/hr 398 406
Cooling Water Flow To Surface Condenser L/s 391 360
Warm Water Temperature From Surface Condenser °C 51 56
60
200
R2=0.998
150
Simulation predictions
100
50
0
-100 -50 0 50 100 150 200
-50
-100
Mill measurements
daily and hourly analysis based on the MVDA results. These scenarios were investigated
using the CADSIM model to find the optimum operation values for Mill A. To study
effect of each input variable on the system, changes of 5, 10, 15 and 20% to the average
amount of selected input variables were made at a time. The system was then left to reach
steady state. Comparison of the system conditions under changes in each input variable
with the average conditions determined the effect of that variable on the system. The
following input variables were changed in the dynamic simulation model: WBL % solids,
WBL flow to the weak liquor flash tank, steam pressure to the evaporators, mill water
temperature to the surface condenser, cooling water flow rate to the surface condenser
and tempering water flow rate to the surface condenser. The results of CADSIM
simulations resulted from change in the listed input variables are presented below:
61
1 - WBL % Solids:
Based on the mill data, on average weak black liquor with 15.2% solids entered
the system with the average heat transfer coefficient of 5670 kJ/hr.m2.°C, and steam
consumption of 103 ton/hr from 294 kPa steam at 143 °C. Based on the MVDA results, a
negative correlation between the WBL % solids and the heat transfer coefficient exists.
As % solids decreases, fewer solids are present to precipitate and form scale. Also, fewer
solids means more water in the system, and as liquor with higher water amount passes
through the tubes, the deposits are washed from the heating surfaces (tubes) and the
reduction in the heat transfer coefficient after reaching equilibrium (Table 6). Reducing
% solids meant more water in the black liquor. Thus higher amount of water was
accessible for evaporation, resulting in higher steam consumption. The other output
Input
WBL % Solids -5% -10% -15% -20%
62
Examining the dynamic values of the heat transfer coefficient, it was observed
that there was a slight decrease in U few minutes after the change was introduced to the
system. After that, the system reached a steady state within 40 minutes (Figure 28).
5000
4000
U (kJ/m2.hr.C)
3000
2000
1000
Time (min)
Figure 28: Heat transfer coefficient vs. time as WBL % solids reduces by 5%
the effect of the WBL % solids on the heat transfer coefficient. Change in the amount of
solids in WBL, changes solids deposition and scale formation in the evaporation system
at the mill. Since CADSIM assumes a clean system with no scale formation, its results
can be different from the results of the analysis of the real system by MVDA.
63
2 - WBL Flow to the Weak Liquor Flash Tank:
On average, the WBL flows at 547 ton/hr (about 464 ton/hr of water for 15.2%
solids black liquor). Based on the MVDA, the WBL flow to the weak liquor flash tank is
positively correlated with the heat transfer coefficient, and negatively correlated with the
58% flash tank level. To verify the MVDA results, the WBL flow to the weak liquor
flash tank was increased in CADSIM. Dynamic simulation showed that an increase in the
WBL flow resulted in an increase in the heat transfer coefficient. This result was in
agreement with the MVDA results (Table 7). Higher WBL flow means higher amount of
liquor is passing through the system, thus recirculation in the evaporators’ body increases
and chance of solids build up decreases. As the flow increases, the overall heat transfer
coefficient increases. The dynamic simulation did not show any correlation between the
WBL flow to the weak liquor flash tank and the 58% flash tank level.
Input
WBL Flow to Weak Liquor FT 5% 10% 15% 20%
58% FT level - - - -
Examining the dynamic changes of the 58% flash tank level in CADSIM, it was
observed that the tank was over filled 5 minutes after increasing the WBL flow, and took
100 minutes to return to the normal steady state operational conditions (75% level). This
is shown by a spike at the beginning of the level vs. time plot (Figure 29). Important to
note is the fact that the results on the level of flash tanks in CADSIM are not reliable.
64
This is partly due to CADSIM’s limitation on enabling users to place level indicators on
the flash tank. In order to measure the level of the flash tank in this CADSIM model, the
flash tank was combined with a storage tank. A level indicator was then placed on the
storage tank to measure the level of the two combined tanks. This approach may not be
accurate, but it was the best solution under the limitations of CADSIM, since it provided
the closest reading for the level of the flash tank in the simulation model. Moreover, the
control strategies used for the level of the 58% flash tank in the CADSIM model are not
the same as those used at the mills. Though CADSIM does not allow for the placement of
valves in the model, the mills themselves have such valves before and after each flash
tank. These limitations of the dynamic simulation decrease the reliability of results
100
Level (% of tank)
50
0
05 100 200 300 400 500
Time (min)
Figure 29: 58% Flash tank level vs. Time as WBL flow increases by 5%
65
3 - Steam Pressure to Evaporators:
Based on the mill data, steam is fed to the evaporators at 294 kPa and 140°C on
average. Results of MVDA revealed a negative correlation between the steam pressure
and the overall heat transfer coefficient and the 58% flash tank level. Changes were made
the steam pressure feeding the evaporators. Similar to other input variables; 5, 10, 15 and
20% changes were made to the steam pressure at first. However, it was observed that
simulation model could not operate when changes to the steam pressure were greater than
10% (the model would have negative heat transfer coefficient values and overflow in the
58% flash tank). As a result smaller changes of 1, 2, 3, 4, and 5% were made to the steam
pressure to study the behaviour of the system. The CADSIM analysis showed that
reducing the steam pressure to the evaporators caused slight negative changes in the heat
transfer coefficient of the 2nd-5th effect, while creating a larger positive change in the 1st
effect. This resulted in an overall positive change on the heat transfer coefficient (Table
8).
Input
Steam Pressure to Evaps -1% -2% -3% -4% -5% -10%
Output Heat Transfer Coefficient 0.26% 0.53% 0.82% 1.13% 1.45% 3.45%
66
4 – Mill Water Temperature to Surface Condenser:
Based on the MVDA, there is a negative correlation between the mill water
temperature and the 58% flash tank level. However, no correlation was observed in the
dynamic simulation. Operation of the surface condenser was explained in section 4.1.2.2,
explaining that it is responsible to create vacuum in the 5th effect. It is worthy of note that
the surface condenser in this simulation is considered to be completely separate from the
multiple effect evaporators. To run the CADSIM model, pressure of evaporators was
required to be specified, thus pressure of each effect was fixed to the average value based
on the mill data. Having fixed pressure in CADSIM’s evaporators means that the surface
condenser can not affect pressure in evaporators any longer. As a result, changes in the
surface condenser do not carry over to the evaporators’ body in the CADSIM simulation.
However, in the mill situation, operational conditions in the surface condenser affect the
vacuum in the fifth effect (which is not a fixed value as it is in this simulation), and
Based on MVDA, correlations exist between cooling and tempering water flow to
the surface condenser and the heat transfer coefficient, the 58% storage tank vent
temperature and the 58% flash tank level. However, no correlation between the output
variables and cooling and tempering water flow to the surface condenser was observed in
the CADSIM simulation. Again, this could be due to separation of the operational
conditions in the surface condenser from the evaporators’ performance in the CADSIM
67
4.2 Analysis for Mill B
An analysis similar to the one performed for Mill A was also performed for Mill
B. Data collection and data processing were carried out correspondingly. Below, only the
The evaporation system at Mill B was similar to that of Mill A (Figure 30). The
main difference was that Mill B used rising film LTV evaporators instead of falling film
evaporators, and had two high solids concentrator placed after the multiple effect
evaporators. At Mill B, 263,000 L/hr of black liquor at 14% solids is processed using
86,000 lb/hr steam at 60 psig and 330° F to produce 105,000 L/hr of 45% solids black
liquor.
Stripper
6 5 4 3 2 1
Vapour
Steam
Liquor to
Condensate Concentrator
Weak Black
Liquor
68
4.2.2 MVDA
A daily average data of 49 input variables for a two-year period were collected
and analyzed using multivariate data analysis techniques. From these variables, 16 were
related to the black liquor properties, 12 to the steam properties, 11 to the mill operation
and 10 to the liquor chemistry. A complete list of variables with their average, minimum
For this mill, three variables were assigned as outputs; the amount of water
evaporated, the amount of steam consumed, and the steam economy (steam economy
being the ratio of the amount of water evaporated to the amount of steam consumed). Due
to insufficient data, the heat transfer coefficient was not used as an indication of thermal
performance of evaporators (as done for Mill A), and thus steam economy was used as
typical steam economy for six effect evaporators is around 5 [17]. To compute the steam
the difference between the amounts of water in the flow of product black liquor of MEE
4.2.2.1 PCA
from January 2004 to Sept. 2006 for the evaporators. Seven principal components were
69
calculated through cross-validation accounting for 83% of the variability in the data. It is
explaining the model is specific to each data set, and thus these values are different from
Mill A. The first 2 PC’s captured most of the variability in the data with 43% and 13% of
4.2.2.2 PLS
A PLS model was built based on the PCA model by assigning three factors of
interest as Y variables. These variables were: the amount of water evaporated, the amount
of steam consumed, and the steam economy. As mentioned in section 4.2.2, due to
insufficient data, the heat transfer coefficient was not used as an indication of thermal
70
performance of evaporators and scaling; therefore, steam economy was used as the best
alternative option. In the analysis, seven principal components were calculated through
The correlations among variables were determined from the coefficient plots of
the PLS model. The number of factors affecting evaporator performance was reduced
from 49 variables to 10 of the most important ones. The summary of correlations among
variables is presented in Table 9. The presence of correlations for most variables was
uncertain in this model as the error bars for most variables passed through zero line in the
coefficient plot (as explained in detail in section 2.4.2). This meant that there was either
no correlation or there was not enough data in the model to determine the correlation.
Analysis of longer period of time, or shorter intervals (hourly averages) might have
improved the accuracy of the results for Mill B. Unfortunately; Mill B was not able to
correlations based on the theoretical principle of evaporation. For example, the weak
black liquor % solids were negatively correlated with the three outputs. High % solids
meant less water in the weak black liquor. Since there was less water to be evaporated,
the amount of water evaporated was negatively correlated with the % solids of the weak
black liquor. Higher WBL % solids also meant that less steam was required for the
system. Since WBL % solids had negative correlation with the amount of both the water
evaporated and the steam used, it might mislead one to conclude that WBL % solids has
71
no correlation with steam economy (considering the cancellation of correlations of
numerator and denominator, as the steam economy is the ratio of the two). However,
WBL % solids was negatively correlated with the steam economy, since the correlation
with water was stronger than it was with steam. Therefore, according to MVDA,
Table 9: Correlations between output variables and top 10 input for Mill B
Output Variables
Rank Input Variables Water Steam Steam
Evaporated used Economy
1 Steam Flow to Evaporators +1.5 +5 -1
2 Weak Black Liquor %Solids to Evaporators -4 -2 -3
3 Weak Black Liquor Flow to Evaporators +1 +3
4 Product Liquor Flow -3 -2.5
5 First Stage Stripper Feed -2.5 -2
6 Black Liquor to Total Heat Recovery Unit (THR) +1 +1
7 Black Liquor Flow to Concentrator +1 +1
8 Concentrator Product Liquor Flow +1.5 +1
9 Steam Temperature to Evaporators +1
10 Weak Black Liquor Temperature -1 +1
Note: Blank squares indicate no correlations.
Below, the results of main correlations for each of the three output variables,
numbered from 1 to 3, are discussed. (Refer to Figure 30 for the schematic drawing of
evaporation system.)
1. The amount of water evaporated in MEE correlated positively with: the steam
flow rate to the evaporators, the WBL flow rate to the evaporators, the black liquor flow
72
rate to the total heat recovery unit (THR), the black liquor flow rate to the concentrator,
the concentrator product liquor flow rate, and the steam temperature to the evaporators.
Overall, it can be concluded that there is a positive correlation between the amount of
steam and black liquor were higher (greater than average) throughout the system.
Increasing the flow rate enhanced heat transfer. As more WBL was processed through the
system, more water was available for evaporation. A higher steam temperature also
More water was evaporated as more black liquor was fed to the total heat
recovery unit, THR. In the THR unit, oxygen is added to the black liquor to increase its
The amount of water evaporated correlated negatively with the weak black liquor
% solids to the evaporators, product liquor flow rate, and first stage stripper feed. Higher
dry solids means less water was available for evaporation, shown by a negative
correlation here. A low product liquor flow rate could suggest that the liquor has spent a
longer time in the system for evaporation, as the product exits the system at a lower rate.
This would give the liquor a longer retention time, and increase its chances of
73
evaporating water. A longer retention time means higher recycling in the system, which
More water is evaporated across evaporators when less condensate is fed to the
stripper. The stripper uses steam to remove methanol and organic sulphur compounds
from the condensates emitted from the evaporators. Less stripper feed means less
consumption of steam in the stripper, leaving a greater amount of steam available for
evaporating water in the black liquor. As a result, more water was evaporated.
2. Steam consumption correlated positively with the steam flow rate and the black
liquor flow rate to the evaporators. It is clear that more steam was used in the system as
the steam flow rate increased. Also, a greater amount of steam was required as the black
Steam consumption was found to be negatively correlated with the WBL % solids
and the WBL temperature. It is desirable to consume less steam for evaporation, in order
to reduce the cost of evaporation. A greater initial solids content of weak black liquor
resulted in less steam consumption. Having WBL with a higher % solids content means
less water available to be evaporated, and in turn less of a steam requirement throughout
the effects. Also, higher WBL temperature resulted in lower ∆T across evaporators,
leading to less heat requirement from steam, i.e. less steam consumption.
74
3. Steam economy, which is an indication of the efficiency of MEE, correlated
positively with the black liquor flow rate to THR, the WBL temperature, and the black
liquor flow rate to and from the concentrator. Steam economy was only calculated across
the evaporator bodies, excluding concentrators. The results showed a higher WBL
black liquor flow rates enhanced the heat transfer and thus increased the efficiency of
MEE.
Steam economy correlated negatively with the steam flow rate, the WBL flow
rate, the product liquor flow rate and the first stage stripper feed. Greater steam flow rate
and steam consumption were expected to have inverse relation with the steam economy
as they are in the denominator of steam economy formula (steam economy = water
explained before, the stripper uses steam to remove methanol and organic sulphur
compounds from condensates coming from evaporators. Less stripper feed means less
75
5. Limitations to Modelling
There were a number of implications for this study. The main one is that there is
scaling correlates with steam consumption, liquor recirculation, liquor flow rate and such
other variables [5]. Therefore, for Mill A, heat transfer coefficient as an indicator of
thermal performance and 3 other variables based on the mill experience were selected as
the primary factors associated with scaling. For Mill B, even less information was
available due to the termination of contribution to the project by the mill. These output
variables can change by causes other than scaling, for example change in the operational
conditions based on the stock. This adds to the complexity of interpreting any changes in
Also, the results of MVDA are mill-specific, and strongly dependent on the data
used. Because of this, the correlations found for the mills under study may not apply to
other mills. It is required to perform a unique MVDA study on each mill to investigate
variables affecting thermal performance and scaling in black liquor evaporators. The
other limitation is that if significant changes are introduced in the process, re-modelling
Moreover, there are also limitations in using the dynamic simulation software,
CADSIM, to model the evaporation system at Mill A. The model could not completely
simulate the evaporator, since it did not allow the user to place control valves after the
flash tank, or to place level indicators on the flash tank. These limitations made the
76
simulation results related to the level in the 58% flash tank unreliable, as it could not
recreate the same control strategies the one employed at Mill A. CADSIM also required
that evaporators pressure be specified, thus the pressure of each effect was fixed to the
average value based on the mill data. Having a fixed pressure in CADSIM’s evaporators
meant that the surface condenser could no longer affect the pressure in evaporators. As a
result, changes in the surface condenser did not carry over to the evaporators’ body in the
CADSIM simulation. This again differed from the situation at the mill, where operational
conditions in the surface condenser affect the vacuum in the fifth effect (which is not a
fixed value as it is in this simulation), and therefore, pressure in all other effects.
77
6. Conclusions
This study showed that it is possible to use multivariate data analysis to find
MEE. MVDA is a suitable tool to find correlation between variables, but it cannot find
cause and effect relations. Further analysis and experimental work, is required to
• The water flow rate to the surface condenser, the weak black liquor % solids, and the
weak black liquor flow rate to the evaporators were the dominant parameters in the
PLS model of the evaporators of this mill based on the loading plot and VIP plot.
• Based on the time series plots, better operational days had less of EA-to-wood and
lower product black liquor % solids. These days had higher tempering water flow rate
to the surface condenser and higher weak black liquor temperature to the 5th effect,
steam pressure resulted in nearly 1.5% increase in the heat transfer coefficient.
• The steam flow, the weak black liquor % solids, and the weak black liquor flow to the
evaporators were the dominant parameters affecting the thermal heat performance of
78
• The steam flow and the weak black liquor % solids were negatively correlated with
the steam economy and scaling. No correlation between the weak black liquor flow to
79
Reference
80
18. Green, R. P. and Hough, G. "Chemical Recovery in the Alkaline Pulping Processes",
3rd ed., Atlanta, GA., TAPPI Press, 1992.
19. Gullichsen, J.; Paulapuro, H. and Fogelholm, C. J. "Chemical Pulping", Paper
Making Science Technology, Finnish Paper Engineers’ Association and TAAPPI, pp. 38-
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20. Shi, B.; Frederick, W. J. and Rousseau, R. W. "Effects of Calcium and other Ionic
Impurities on the Primary Nucleation of Burkeite", American Chemical Society, 2003.
21. Ulmgren, P. and Radestrom, R. "Deposition of Sodium Oxalate in the Black Liquor
Evaporation"
22. Mulligan, C.N.; Yong, R.N. and Gibbs, B.F. "Remediation technologies for metal-
contaminated soils and groundwater: An evaluation", Engineering Geology, vol. 60, pp.
193-207, 2001.
23. Hoeskuldsson, A. "A Combined Theory for PCA and PLS", Journal of
Chemometrics, vol. 98, pp. 91, 1995.
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Sweden, 2005.
26. Wold, S. "Cross-Validatory Estimation of the Number of Components in Factor and
Principal Component Models" Technometrics, vol. 20, pp. 397-405, 1978.
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81
Appendix 1
In Mill A, the problem of scaling was mainly present in the 1st effect and the 58%
flash tank, as well as lines between them and the 58% storage tank. Scaling in the 1st
effect was so severe that 30% to 50% of the evaporator tubes have to be cleaned with
high pressure water during every annual maintenance shutdown in order to remove
accumulated scale. Scaling in the 58% flash tank was mainly observed around the vortex
breaker in the outlet pipe, and has been the cause of occasional emergency shutdowns as
well.
Chemical analysis was performed on a black liquor sample from the second effect
and scale samples from the 1st effect, the flash tank and the HSC heater (Figure 32). The
black liquor analysis indicated that sodium sulfate dicarbonate (2Na2CO3•Na2SO4) is the
first sodium salt to precipitate. The black liquor analysis showed that the residual alkali
was very low, indicating that black liquor viscosity at the higher solids would be
significantly higher than the potential minimum if the hydroxide concentration was
higher. The first effect deposit was found to be 77 % sodium salts (95% dicarbonate and
5% sodium oxalate). The remainder were organics and residual inorganic matter
associated with entrained black liquor that was baked into the scale. The flash tank
deposit was 88 % sodium salts (90 % dicarbonate and 10 % sodium oxalate). The nodules
had essentially the same composition as the bulk scale. The HSC heater deposit was 76 %
82
Figure 32: Scale Samples collected from the 1st Effect, 58% flash tank outlet pipe,
and high solids concentrator tube
The mill’s initiative toward the scaling problem is to clean the evaporators and
flash tanks with water or weak black liquor, a process called “boiling out”. Scaling is
costly due to the price of cleaning and loss of efficiency, i.e. more steam is consumed in
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case of scaling due to loss of heat transfer area. Cleaning the 1st effect during shut down
costs $137,000, with the additional cost of lost efficiency. The effect of lost efficiency
can be great. For example, in March of 2008, pulp production was reduced by 260 tons
due to 58% flash tank plugging. Valuing $900/ ton of pulp indicates cost due to lost in
efficiency of evaporators. In first quarter of 2007, about 40 tons of pulp was lost due to
plugging. Other impacts include the value of extra steam put in evaporators due to
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Appendix 2
conduct a number of procedures to resolve plugging and or locate it when problems are
seen at the system. An example of locating the pluggage problem is presented here: If the
pump load after the 58% flash tank decreases, the operator can determine the location of
pluggage (whether it is before or after the pump), by closing and opening the butterfly
valve on the 58% storage tank. This is because, typically if the line after the pump is
clean, there should be a noticeable shake in the line by closing and opening the valve, due
to its affect on the pump. In case of pump load decrease, it is possible to close the valve
on the vent line from the 1st effect to the 3rd effect. This will stop the vent from going to
the 3rd effect, thus the 58% flash tank becomes pressurized and pushes through the pump
harder, breaking the plug rather than doing a boil out. These are examples of actions that
can be taken to avoid a boil out, but a boil-out cannot be avoided. The boil-out frequency
varies with time, but averages about once per week and can be as frequent as three times
per week. It is usually higher in the winter months, when the 1st Effect steam pressure
(and hence 1st Effect liquor solids concentration) can widely fluctuate due to inconsistent
Once the tube has been plugged, a boil-out is not enough, necessitating high
pressure cleaning. A high pressure cleaning of the tubes is performed during the annual
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maintenance shutdown. About 30% to 50% of the heat exchange tubes in the 1st effect
of black liquor) and its need due to accumulated scales (mechanical issues). Performing a
boil-out highly depends on inventory. It takes about an hour to reduce the black liquor
flow and steam flow, an hour to perform a boil-out, and another hour to return to normal
operation conditions.
1. The level of the 58% flash tank (a high level of 58% flash tank implies improper
flashing). Also, an increase in the level of the 58% flash tank results in an increase in
level of the 1st effect, since there is free flow between the two, i.e. no pump in between)
2. The pump load, after the 58% flash tank (Low pump load indicates scale/plug
3. The 58% flash tank discharge temperature (If temperature of black liquor in discharge
line is higher than that of the feed line to the flash tank, then flashing did not occur
properly).
4. Vent incidents from the 58% storage tank (the vent indicates pressure build up in the
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- Increased pressure of steam consumed, which can be due to scaling or higher solids and
flow. Primarily, one should investigate pressure and flow from the 1st effect for scaling.
In order to locate the problem, one can look at the pressure and flow of each individual
effect.
Boil-out Procedure:
Effect and the 58% flash tank are periodically taken offline and boiled out. For each boil-
out, the evaporator train must be slowed back to approximately half of normal throughput
for 1 to 3 hours. The following is the procedure taken by operators in the control room at
1. The WBL flow rate to the 5th effect is reduced to 80-90 L/s (compare to 150-160 L/s)
2. The stripper flow rate is reduced to 8 L/s (compare to 15 L/s) to maintain level in strip
feed tank
4. The 400 kPa steam flow rate is reduced to 45 tons/hr (compare to 85 tons/h)
5. Black liquor from the 3rd effect (~50% solids) feeds to HSC instead of the 1st effect.
During boil-out, 35 L/s of WBL is fed to the 1st effect, passing through the 1st effect, the
58% flash tank and pump to the spill tank. Live steam has reduced to 45 tons/h.
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Appendix 3
88
Variables Unit Average Min Max STD
#5 EFFECT VAPOUR PRESSURE kPa -62 -66 0 10
SURFACE CONDENSER PRESSURE kPa -76 -87 -10 11
#1 EFF BOILING POINT RISE °C 15 0 18 3
EVAPORATION ACROSS EFFECTS kg/hr 386057 0 469894 73459
STEAM ECONOMY ACROSS EFFECTS 5 0 7 1
COOLING WATER FLOW TO SURFACE CONDENSER L/S 380 0 486 72
TMPERING WATER FLOW TO SURFACE CNDENSER L/S 53 0 162 56
MILL WATER TEMP TO SURFACE CONDENSER °C 14 6 24 3
WARM WATER TEMP FROM SURFACE CONDENSER °C 50 18 57 6
CLEAN CONDENSATE CONDUCTIVITY TO
COLLECTING umhos 4 3 20 2
COMBINED CONDENSATE CONDUCTIVITY umhos 290 4 693 138
FOUL CONDENSATE FROM SEAL TANK umhos 1152 23 2559 440
#2 EFFECT FLASH TANK LEVEL % 45 12 66 8
SBL TEMPERATUR -SOAP SKIMMER TANK °C 97 16 104 12
#2 EFFECT TRANSFER PUMP LOAD % Load 66 0 70 10
SOAP SKIMMER TANK LEVEL % 42 0 110 26
SKIMMED LIQ RETURN PUMP LOAD % Load 49 0 72 30
58% BL STORAGE LEVEL % 63 31 86 14
58% FLASH TANK LEVEL % 50 0 91 14
58% FLASH TANK DISCHARGE TEMPERATUR °C 116 15 127 15
BL FLOW TO HSC L/s 26 0 31 5
SALTCAKE ADDITION L/s 1 0 2 1
SBL % SOLIDS % 59 46 64 2
BL TEMP INLET-N.HSC HEATER °C 135 17 145 18
BL TEMP INLET-S.HSC HEATER °C 135 17 145 18
BL TEMP OUTLT-N.HSC HEATER °C 137 20 148 18
BL TEMP OUTLT-S.HSC HEATER °C 136 20 147 18
HSC PRESSURE kPa 98 1 137 25
HSC BOILING POINT RISE °C 19 -5 23 4
STEAM FLOW TO HSC HEATER kg/hr 17323 778 28335 6547
STEAM TEMP - HSC HEATERS °C 143 21 156 19
STEAM PRESSURE -HSC HEATERS DESUPERHEATER kPa 328 0 452 83
CONTROL VALVE STEAM TO HSC HEATERS % 61 -5 105 22
MANUAL VALVE STEAM-HSC HEATERS % 42 -7 107 36
89
Variables Unit Average Min Max STD
EVAPORATION N. HSC STEAM MASS FLOW kg/hr 8712 3090 13104 2731
EVAPORATION S. HSC STEAM MASS FLOW kg/hr 8538 2847 13479 2830
EVAPORATION ACROSS HSC kg/hr 19215 0 64974 6993
STEAM ECONOMY ACROSS EFFECTS & HSC 4 0 5 1
70% BL STORAGE TEMP °C 114 17 119 14
70% FLASH TANK VAPOUR PRESSURE kPa -3 -20 15 5
70% FLASH TANK LEVEL % 41 11 67 6
PRODUCT BL % SOLIDS % 71 61 230 9
70% BL-STORAGE TANK #1 LEVEL % 69 0 84 18
70% BL STORAGE TANK #2 LEVEL % 70 41 87 10
1100 KPA STEAM FLOW TO EJECTORS kg/hr 1070 0 1154 166
400 KPA STEAM FLOW TO STRIP kg/hr 10695 0 13048 2233
FOUL CONDENSATE FLOW TO STRIPPER PREHEATER L/s 13 0 21 3
FOUL CONDENSATE TEMP TO STRPER PREHTER EX °C 112 18 121 15
CONDENSATE STRIPPER LEVEL % 36 0 101 9
TEMP CONDENSATE STRIPPER UPPER SECTION °C 118 20 123 14
TEMP CONDENSATE STRIPPER LOWER SECTION °C 133 20 147 19
STRIPPED CONDENSATE TO RECAUST umhos 272 0 738 248
MILL WATER TO TRIM CONDENSER TEMP °C 18 8 48 6
WARM WATER TO TRIM CONDENSER TEMP °C 64 24 86 14
NCG PRESSURE FROM TRIM CONDENSER kPa 124 16 295 19
%CAUSTICITY (CE) % 81 73 88 2
GREEN LIQUOR REDUCTION % 94 89 98 2
TOTAL TITRATABL ALKALI g/L 117 106 122 2
CAUSTIC FLOW TO WHITE LIQUOR STORAGE TANK L/s 0 0 3 1
TOTAL EA TO WOOD % 13 0 20 2
SPECIES INTO CHIPMETER 1 0 1 0.4
EXTRACTION RESIDUAL FROM DIGESTER -EA g/L 8 3 20 3
MCC EA TREND DATA g/L 9 5 17 2
WASH RESIDUAL EA g/L 9 6 17 1
58% BL STORAGE TANK VENT TEMP °C 26 12 48 5
ANALYZER BLOW KAPPA # KAPPA# 19 11 32 6
Notes: WBL=Weak Black Liquor, Temp=Temperature,BL=Black Liquor, SBL=Strong Black Liquor, HSC=High Solids
Concentrator, N=North, S=South, MCC=Modified Continuous Cooking
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Appendix 4
91
Variables Unit Average Min Max STD
5TH EFFECT TEMPERATURE F 175.6 48.3 192.5 16.1
4TH EFFECT TEMPERATURE F 200.8 57.6 216.7 18.6
3RD EFFECT TEMPERATURE F 227 51.4 242.9 22.2
2ND EFFECT TEMPERATURE F 260.8 54.2 282.1 27.1
1 ST EFFECT TEMPERATURE F 311.2 49.6 338.4 33.8
1ST EFFECT VAPOUR HEAD TEMPERATURE F 270.4 60 290.7 27.6
CONCENTRATOR STEAM FLOW PPH 8140 157.5 27780.6 5857.6
CONCENTRATOR STEAM PRESSURE psi 22.8 -2 51.1 13.9
WHITE LIQUOR EA g/L 18.6 -1.4 52.7 5.8
WHITE LIQUOR TTA g/L 18.6 -1.4 52.7 5.8
WHITE LIQUOR SULPHIDITY % on AA 27.5 0 34.9 6.5
WHITE LIQUOR CE % 74.7 0 83.5 16.9
DIGESTER PRODUCTION ADMT/D 928.6 0 1152.4 238.2
EA TO WOOD RATIO % 14.7 0.1 19.3 3.3
BLOW KAPPA NUMBER 18.6 9.6 48.1 8.6
DIGESTER WOOD SPECIES
0 = SOFT WOOD, 1 = HARD WOOD 0.65 0 1 0.44
FIRST STAGE STRIPPER FEED USGPM 497 3.1 695.3 118.2
CONDENSATE TEMPERATURE TO 1ST STAGE F 231.6 96 250.7 21.5
BROWNSTOCK FILTRATE TO WBL STORAGE 462.8 -997.5 1099.8 246.9
O2 to THR 19244.8 0 32897.8 12028.9
6TH EFFECT BOILING POINT RISE F 0.8 0 30.3 3.3
5TH EFFCT BOILING POINT RISE F 3.2 0 45.7 9.9
4TH EFFECT BOILING POINT RISE F 32.7 0 100 42.8
3RD EFFECT BOILING POINT RISE F 5.7 0 9 1.1
2ND EFFECT BOILING POINT RISE F 0.05 0 4.8 0.3
1ST EFFECT BOILING POINT RISE F 10.4 0 14 1.9
CONCENTRATOR #2 DOME PRESSURE psi -2.9 -20.8 19.1 5.9
WATER EVAPORATED PPH 377927 -10159.4 527867 69702.3
STEAM USED PPH 90093.9 0 122128 18993.4
STEAM ECONOMY 5.9 -0.5 1657.7 50.8
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