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Proceedings of the 2011 4th International Symposium on

Advanced Control of Industrial Processes, Thousand


Islands Lake, Hangzhou, P.R. China, May 23-26, 2011

WePoPo.1

Research on Industrial Modeling of Ethylene Oxide Hydration


Reactor
Fan. Sun, Na. Luo, Rongbin. Qi and Feng. Qian
Abstract Focusing on ethylene oxide (EO) hydration reactor
industrial equipment, the reaction mechanism model is
established. Based on the principle of material balance, energy
balance and kinetics of the reactions of ethylene oxide with water,
partial least squares regression (PLSR) was used in the model to
establish a corresponding relationship between the reaction rate
constant and the reaction temperature. With kinetic parameters
correction by using field data, the results are more tallies with
the actual operation. Influences of water/EO molar ratio and
inlet temperature on product quality, outlet temperature and
energy consumption are analyzed according to the established
model. The results showed that the model can preferably reflect
the performance of EO hydration reactor and have certain
guidance functions to the further advanced control strategies.

I. INTRODUCTION

S the simplest glycol, ethylene glycol (EG) is an


important raw material for industrial applications with
extensive uses. EG is used in the manufacture of polyester
resins, antifreezes, and solvents, etc [1-2]. EG is commonly
produced by the hydration of ethylene oxide (EO) [3-7]. In
this paper, the EG production adopts American SD company
technologies by oxidation in pure oxygen and EO is
synthesized by reaction of ethylene and oxygen under high
temperature and high pressure in the presence of catalyst.
Then EG is produced by the hydration of EO under the
conditions of 22/1 water/EO molar ratio.
Though EO hydration reactor is an important device in EG
production, there are very few articles about mechanism of
hydration of EO and industrial model. Considering the

differences between laboratory results and practical


production conditions, first a kinetic model was put forward
by the laboratory data, and then using field data to correct the
kinetic parameters.
II. MATHEMATICAL MODEL
EO hydration reactor is an adiabatic tubular reactor. During
the reaction, diethylene glycol (DEG), triethylene glycol
(TEG) and polyethylene glycol (PEG) are produced as
byproduct. Both DEG and TEG are also used for the
manufacture of many chemicals, especially in the production
of various polymers.
EO reacts with glycols to make higher order glycols and
polyglycols. It is an exothermic and cascade reaction. The
reactions of EO with glycols occur based on the following
stoichiometry [8-9] :
k1
(1)
C2 H 4O + H 2O
C2 H 6O2
ki
C2 H 4O + C2i 2 H 4i 2Oi
C2i H 4i + 2Oi +1 , i = 2, , 6 (2)
Due to the reactor axial length is far greater than the radial
length, we can assume that there is no temperature gradient
and concentration gradient in radial direction. So it can be
assumed plug flow in the reactor and there is no back mixing.
Axial and radial diffusion can be ignored. According to the
material balance, energy balance and reaction kinetics
equation, model are as follows:

A. Reaction kinetics
The reactions of EO with water and EG can be expressed
as:
k1
EG
EO + H 2O

Manuscript received July 23, 2010. This work was funded by


Distinguished Young Scholars Program of the National Natural Science
k2
(3)
DEG
EO + EG
Foundation of China (NSFC) (Grant Number:60625302), Natural Science
k
3
Foundation of China (60704028), the National High Technology Research
TEG
EO + DEG
and Development Program of China (863 Program, No: 2007AA04Z193).
k4
PEG
EO + TEG
Fan. Sun is with Key Laboratory of Advanced Control and Optimization
for Chemical Processes, Ministry of Education, East China University of
Where k1 , k2 , k3 and k4 are the reaction rate constants.
Science and Technology, Shanghai, 200237 China (e-mail: sun.fan-007@
Each step given in Eqs(3) can be assumed as an irreversible,
163.com).
Na. Luo is with Automatic Institute, Key Laboratory of Advanced Control
bimolecular, and constant density reaction. The rate
and Optimization for Chemical Processes, Ministry of Education, State-Key
expressions, with this assumption, can be given by:
Laboratory of Chemical Engineering, East China University of Science and
dCH 2O
Technology, Shanghai, 200237 China (e-mail: naluo@ecust.edu.cn).
= k1CEO CH 2O
Rongbin.Qi is with Key Laboratory of Advanced Control and
dt
Optimization for Chemical Processes, Ministry of Education, East China
dCEO
University of Science and Technology, Shanghai, 200237 China (e-mail:
=
k1CEO CH 2O k2CEO CEG
rbqi@163.com, qirongbin@ecust.edu.cn).
dt
Feng. Qian is with Automatic Institute, Key Laboratory of Advanced
k3CEO CDEG k4CEO CTEG
Control and Optimization for Chemical Processes, Ministry of Education,
State-Key Laboratory of Chemical Engineering, East China University of
dCEG
Science and Technology, Shanghai, 200237 China (phone: 86-21-64252060; = k1CEO CH 2O k2CEO CEG
dt
fax: 86-21-64252056; e-mail: fqian@ecust.edu.cn).

456

dCDEG
=
k2CEO CEG k3CEO CDEG
dt
dCTEG
=
k3CEO CDEG k4CEO CTEG
dt
dCPEG
= k4CEO CTEG
dt

B. Material balance equation


Taking differential section dl , the mass balance equation of
EG in l to l + dl is as follows:
d ( FCEG )
(4)
FCEG [ FCEG +
dl ] =
rEG R 2 dl
dl
Where F is feed flow, R is reactor radius, CEG is the
concentration of EG in the reaction mixture and rEG is
reaction rate of EG.
Because of the flow is almost constant, Eqs (4) can be
simplified as follows:
dCEG
r R2
(r r ) R 2
=
EG
=
1 2
dl
F
F
Similarly,
dCEO
r R2
( r1 r2 r3 r4 ) R 2
=
EO
=

dl
F
F
dCH 2O
rH 2O R 2 r1 R 2
=

=
dl
F
F
2
( r r ) R 2
dCDEG
r R
=
DEG
=
2 3
dl
F
F
2
dCTEG
r R
(r r ) R 2
=
TEG
3 4
dl
F
F
2
dCPEG
r R
r R2
=
PEG
=
4
dl
F
F
Where r1 ~ r4 are reaction rates of the reactions in Eqs (3).

(PLSR) method to establish the relationship between the


reaction rate constant and the reaction temperature [10-12].
Reaction temperature is the main influencing factor to
determine the reaction rate constants. This process of creating
the regression equation, taking reaction temperature Tx as
the independent variable, and calculating the results to
forecast the dependent variable ki [13]:
ki =
0i + 1iTx + 2iTx 2 + 3iTx 3 , i =
1, 2, 3, 4

(5)

Where Tx is absolute temperature in kelvin, 0i ~ 3i are


factors of correction.
We used the 5 groups of experimental data in literature [9]
to get 5 groups of the reaction rate constants in different
conditions. Then according to the values of Tx , we can get the
square of Tx and the cube of Tx . So there are a
5 3 dimensional nonlinear independent variable matrix
X 1 and a 5 1 dimensional dependent variable matrix Y1 .
After standardization of X 1 and Y1 , we can get the new
matrixes X and Y .The two matrixes are decomposed as:
(6)
X
= TP + E
(7)
=
Y UQ + F
T ( 5 3 dimensional) and U ( 5 3 dimensional) are
latent component matrixes, P ( 3 3 dimensional) and Q
( 3 1 dimensional) represent loading matrixes, E ( 5 3
dimensional) and F ( 5 1 dimensional) are residual matrixes.
Basic idea of extracting component t is finding the max
covariance between the latent component vectors t and u .
(8)
Cov(t , u ) = r (t , u ) Var (t )Var (u )

Where t and u are column vectors of T and U ,


Cov(t , u ) is the covariance between t and u , r (t , u ) is the
correlation coefficient, Var is variance operator.
When the correlation coefficient is small, the regression
results
are not satisfactory. So we applied orthogonal
C. Energy balance equation
projection theory to improve PLSR which removes the
The energy balance equation:
irrelevant information in the independent variable matrix.
d ( Fc pT )

(r1H1 + r2 H 2 + r3 H 3 + r4 H 4 ) R 2 =
0
X T YY T X is a 3 3 dimensional symmetric matrix and the
dl
rank of the matrix is l. So there are 2 orthonormal eigenvectors
Where is the density of the reaction mixture, c p is
which eigenvalue equals 0. Take these 2 orthonormal
specific heat capacity of the reaction mixture, H is reaction eigenvectors as column vector, we can get a 3 2
heat.
dimensional matrix B = (b1 , b2 ) . In this way, we get
In general, the flow is relatively stable, F is almost
biT X T YY T Xbi = 0 , so (b1 , b2 , Y T X ) must be a 3 dimensional
constant. The value of c p is dependent upon temperature and
orthonormal basis.
components.
The vector which consists of independent variable matrix
X and is perpendicular to dependent variable matrix Y can
III. THE REACTION RATE CONSTANT REGRESSION
be denoted by H = XA . Then we have Y T XA = 0 . So A
The value of the preexponential factor has an uncertainty consists of orthocomplement space of Y T X . Then A can be
of 10% in the literature [8]. According to the experimental expressed by a linear combination about the columns of
data in the literature [9], the reaction rate constants can be
B that can be denoted by A = BD . Next step we need to find
worked out by regression analysis. And thus the the D that can make the variance of XBD reaches the
macro-kinetics model can be proposed.
maximum, so the useless information between independent
We applied improved partial least squares regression variable and dependent variable can be removed as much as

457

possible. The eigenvector corresponding to the largest


eigenvalue of BT X T XB is just the vector that makes the
variance of XBD reaches the maximum. So we get D and
when X is projected to the orthocomplement space of H , the
new matrix which removes most of the useless information is
obtained: X=
X H ( H T H ) 1 H T X . At last, replacing
0
X with X 0 , we get the improved PLSR model.

The cross validation method is used to validate the results


[14-15]. It is a procedure for accurately assessing the forecast
performance of a model and determining the optimum number
of principal components. The main index in the assessment is
prediction residual error sum of squares (PRESS) that is
defined as follows:
n
(9)
PRESS
=
(h) ( yi yi' (h)) 2
i =1

Where yi is the i-th original value, y (h) is the i-th fitting


value of modeling set up with sample i , PRESS (h) indicates
'
i

the quality of phase h prediction equation.


A model has the best prediction ability when the value of
PRESS (h) reaches minimum, wherein the value of h is the
optimum number of principal components. PRESS (h)
reached its minimum when the number h of principal
components was 4, indicating 4 principal components were
adequate to generalize the information of the original samples.
When the optimum number of principal components is 4,
using nonlinear iterated partial least squares (NIPALS)
algorithm to get the regression coefficient 0i ~ 3i in
Eqs(5):
k=
3.5654 106 1.5114 104 Tx + 0.6733Tx 2 + 0.0385Tx 3
1
k=
8.6762 106 3.6548 104 Tx + 1.4247Tx 2 + 0.0925Tx 3
2
9.7358 106 4.0825 104 Tx + 1.4298Tx 2 + 0.1027Tx 3
k=
3

k=
1.0795 107 4.5102 104 Tx + 1.4350Tx 2 + 0.1129Tx 3
4
Where Tx is absolute temperature in Kelvin, ki is in

Lmol 1 min 1 .
Using the 5 groups of experimental data and another 2
groups of experimental data to verify the reliability of the
model, the absolute value of average relative error between
the predicting data and the experimental data is 5.92%. Using
the same data to calculate the model which established based
on the method in literature, the absolute value of average
relative error is 8.56%. There was a 30.84% decrease. So this
model proved effective.

IV. PARAMETER CALIBRATION OF INDUSTRIAL MODEL


Due to various reasons (such as heat loss, etc), the
laboratory results are different with the actual industrial
conditions. On account of kinetic parameters correction by
using field data, the results are more tallies with the actual
operation. Correction factors a1 , a2 , a3 , a4 are introduced to
correct the changes of reaction rate constants.

k1 ' = a1k1
k2 ' = a2 k2

(10)

k3 ' = a3 k3
k4 ' = a4 k4
1) Input the real-time operation conditions, including the
inlet temperature, pressure, flow and components of the
reactor. According to the input conditions, we can calculate
the outlet components of the reactor when taking the value
of k1 , k2 , k3 , k4 as initial value.

2) According to the calculating values and the actual values


in the factory, we used the sequential quadratic programming
(SQP) algorithm to get the correction coefficients
a1 , a2 , a3 , a4 . The SQP algorithm has been one of the most
successful general methods for solving nonlinear constrained
optimization problems [16-22]. The objective function is:
2
2

n ( y
EG ,i z EG ,i ) + ( y DEG ,i z DEG ,i )
(11)
min
2
2

i =1 + y
( TEG ,i zTEG ,i ) + ( yPEG ,i z PEG ,i )
Boundary conditions: ki > 0, i =
1, 2, 3, 4 , C j 0
Initial value: a=
1,=
i 1, 2, 3, 4
i
Where C j is the concentration of the components in the
reaction mixture, yEG ,i is the calculating value of EG, z EG ,i is
the actual value of EG.
3) Using the correcting reaction rate constants to calculate
the model, we can get the simulation results which are more
suitable for the operation conditions.
V. THE CALCULATED RESULTS AND RESULTS ANALYSIS
A. The calculated results of the model
The reactions of ethylene oxide with water are irreversible
and exothermic. The conversion rate of EO can reach to 100%
in industry control. The model can preferably reflect the
performance of EO hydration reactor after the parameter
calibration. Using 10 groups of field data to verify the
reliability of the model, the absolute value of average relative
error is 4.82%. The model calculating components are
compared with the designed conditions in Table I.
TABLE I

SIMULATION RESULTS OF ETHYLENE OXIDE HYDRATION REACTOR

Mass Fraction

Reactor
Inlet
(designed)

EO
H2O
EG
DEG
TEG
PEG
Total Flow(Kg/hr)

0.0999
0.8985
0.0016
0.0000
0.0000
0.0000
260377.5

Reactor
Outlet
(designed)

Reactor
Outlet
(calculated)

0.0000
0.8600
0.1269
0.0123
0.0007
0.0001
260377.5

0.0000
0.8595
0.1281
0.0117
0.0006
0.0001
260377.5

Axial temperature distribution of the reactor is shown in


Fig.1. EOs conversion rate is shown in Fig.2. The flow rates
of the components along the reactor length are shown in Fig.3.

458

changes of DEG, TEG and PEG are shown in Fig.4.

460

B. Effect of water/EO molar ratio on the product


In the process of EG production, different water/EO molar
ratios can lead to different product distributions. When the
flow rate of EO is unchanged, adjusting the flow rate of water
can get different water/EO molar ratios. Taking the flow rate
of EO for constant, the flow rate of water for variable, and
then different product distributions at different water/EO
molar ratios are shown in Table II.

450

T(K)

440
430
420
410
400

20

40

60

80 100 120
l(m)

140 160

xEO

Fig. 1. Axial temperature distribution


1

20

32992.4

3305.6

188.9

33.7

179.8

0.8

21
22

33174.9
33345.5

3174.5
3051.4

172.9
157.8

30.8
28.1

177.7
175.7

23

33502.5

2936.4

145.1

25.8

173.8

24

33649.2

2829.6

133.1

23.7

172.2

25

33777.1

2730.8

122.4

21.8

170.9

0.6
0.4
0.2
0

20

40

60

80 100
l(m)

120

140

160

Fig. 2. The conversion rate of EO


5

yEO, ,yH2O, yEG, yDEG, yTEG, yPEG (kg/h)

x 10

2
yEO
yH2O
yEG
yDEG
yTEG
yPEG

1.5

0.5

20

40

60

80
l(m)

100

120

140

160

Fig. 3. The flow rates of every component


3500
3000

yDEG, yTEG, yPEG (kg/h)

TABLE II
PRODUCT DISTRIBUTIONS AT DIFFERENT WATER/EO MOLAR RATIOS
Outlet
Water/E
DEG
TEG
PEG
EG
Temperat
O Molar
(kg/h)
(kg/h)
(kg/h)
(kg/h)
ure (C)
Ratios

TABLE III

2500

OUTLET COMPONENTS AND TEMPERATURES AT DIFFERENT INLET


TEMPERATURES

yDEG
yTEG
yPEG

2000

Inlet
Temperat
ure (C)

1500
1000
500
0

From the data above, analysis is as follows:


1) Water/EO molar ratio has great influence on EG
production. Increasing water/EO molar ratio can increase the
output of EG and decrease by-products DEG, TEG and PEG.
But at the same time, the outlet temperature falls sharply
which will cause more consumption of subsequent
high-pressure steam. And also when the water/EO molar ratio
increases, purification of the product needs removing a lot of
water by evaporation which will increase the energy
consumption.
2) How to adjust the water/EO molar ratio depends on the
market price of the product. If the benefits of increasing the
output of EG are lower than the costs of increasing the energy
consumption, smaller water/EO molar ratio should be taken.
On the other hand, if the benefits of increasing the output of
EG are higher than the costs of increasing the energy
consumption, bigger water/EO molar ratio should be taken. In
general, adjusting the water/EO molar ratio bases on
comprehensive consideration of product benefit, energy
consumption and the market price changes of EO, EG and
TEG.

20

40

60

80
l(m)

100

120

140

160

Fig. 4. The flow rates of the by-products

The contents of by-products DEG, TEG and PEG are


relatively less. They are not obvious in Fig.3. So the specific

EG
(kg/h)

DEG
(kg/h)

TEG
(kg/h)

PEG
(kg/h)

Outlet
Temperat
ure (C)

127

33352.3

3041.2

157.3

28.0

172.9

128
129

33350.2
33347.8

3044.6
3078.0

157.5
157.7

28.0
28.0

173.8
174.8

130

33345.5

3051.4

157.8

28.1

175.7

131

33343.2

3054.7

158.0

28.1

176.6

132

33340.8

3057.9

158.2

28.1

177.7

133

33338.5

3061.3

158.3

28.1

178.6

459

C. Effect of the inlet temperature on the product


Under the designed conditions, the inlet temperature of the
reactor is 130. In order to analyze the effect of the inlet
temperature fluctuations on the reaction, taking 3 of
fluctuating range simulated and analyzed. When the inlet
temperature ranges from 127 to 133, the outlet
components and temperatures are shown in Table .
Increasing inlet temperature had little influence on product
distributions. Increasing reaction temperature can slightly
promote the reaction degree and it will lead to the outlet
temperature increasing which will cause less consumption of
subsequent high-pressure steam. So increasing inlet
temperature is one of the methods that expand the capacity of
EO hydration reactor.
VI. CONCLUSION
PLSR was used to establish the EO hydration reactor model.
Utilizing the PLSR method decreased the error for the
reaction rate constants fitting. By using SQP algorithm for
dynamic equation calibration, the results are more tallies with
the industrial equipment. According to the established model,
we analyzed influences of water/EO molar ratio and inlet
temperature on product quality. Increasing water/EO molar
ratio can increase the output of EG but will increase the energy
consumption. Adjusting water/EO molar ratio bases on
comprehensive consideration of product benefit, energy
consumption and the market price changes of EO, EG and
TEG. Appropriately increase of the inlet temperature can
reduce energy consumption.

[9]

[10]
[11]

[12]

[13]

[14]

[15]

[16]

[17]
[18]
[19]

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