2006~2007

Design of an Acetic Acid Aqueous Solution Recovery Process

R123604869


.......................................................................................................................................................... I
................................................................................................................................................... III
................................................................................................................................................... IV
......................................................................................................................................................... V

............................................................................................................................................1

....................................................................................................................................4

2.1 .......................................................................................................................................4
2.2 .......................................................................................................................................4
2.3 ..................................................................................................................... 11
2.3.1 ......................................................................................................................... 11
2.3.2 .............................................................................................................12
2.3.3 (r)(s) .............................................................................................13
2.3.4 (BVDMBoundary Value Design Method) ......................14
2.3.5 ..........................................................................................15
2.4 .............................................................................................................16
2.5 .....................................................................................................................18
2.6 .....................................................................................................................19
2.7 .............................................................................................................20
2.8 .....................................................................................................................................21

..................................................................................................................................22

3.1 .....................................................................................................................................22
3.1.1 .............................................................................................................22
3.1.2 .............................................................................................23
3.1.3 .....................................................................................................24
3.1.4 .....................................................................................................24
3.2 .....................................................................................................................................26
3.2.1 ........................................................................................................................26
3.2.2 ........................................................................................................................26
3.2.3 ............................................................................................................................26
3.2.4 ............................................................................................................................27
3.2.5 .................................................................................................................27
3.2.6 .............................................................................................................................27
3.3 (TOTAL ANNUAL COST, TAC).....................................................................................28
I

3.4 .............................................................................................................................................28
3.4.1 ............................................................................................................................28
3.4.2 ............................................................................................................................28
3.5 ...................................................................................................................................28

......................................................................................................................30

......................................................................................................36

..........................................................................................................................................38

........................................................................................................................................................39
................................................................................................................................................40
....................................................................................................................................................42
........................................................................................................................................................46

............................................................................................................47

(R)(S)..............................................................................................50

(BVDMBOUNDARY VALUE DESIGN METHOD) .60

........................................................................................68

....................................................................................................76

............................................................................................................81

II


- ........................................................................................................1
.........................................................................................................................5
.......................................................................................................12
...............................................................................................14
...................................................................................................17
................................................................................31
....................................................................................32
.......................................................................................................................35
.......................................................................................................................49
FLASH3 .....................................................................................................51
................................................................................54
...................................................................................................56
...........................................................................................59
FLASH3 .................................................................................................61
.......................................................................................................................63
FLASH2 ..........................................................64
FLASH2 ..................................................66
BVDM ..................................................................................................................67
...............................................................................................68

FLG CSB ...................................................................................................................70

...................................................................................................77
VS ........................................................................................................79
...................................................................................................80
....................................................................82
................................................82

III


.....................................................................................................2
.................................................................................................................................7
.....................................................................................................................................8
.....................................................................................................................................9
.......................................................................................................................25
TAC ......................................................................................................................29
.......................................................................................................31
.......................................................................................................32
FLASH3 .....................................................................................................51
....................................................................................54
...................................................................................................56
...........................................................................................59
FLASH3 .................................................................................................61
...................................................................................................64
...................................................................................................66
FLG ...................................................................................................................69
C SB ...................................................................................................................71
FST ....................................................................................................................72
C ......................................................................................................................73
U f Ad At DT .........................................................................................75

IV

(BVDM) Aspen Plus

(RGA)

-
(tangent pinch)
(entrainer)

Othmer (1963)

Chien (2004)
10mol%~90mol%
99.9mol%
Chien
Kuo(2006)

()

(, mol%)

(ethyl acetate)

77.15

31.2

(i-butyl acetate)

117.2

56.1

(n-butyl acetate)

126.2

72.3

100ppm(wt.)
Liu (2005) Ho (2003)


JulkaDoherty(1990)(Boundary Value Design
Method, BVDM)
Aspen Plus (Aspen Technology, Inc.)
Liu(2005)Poly(ether block amide)
(PEBAX2533Arkema)
(RGA)(Control
variable)(Manipulated variable)(Bristol1966)
Douglas(1988)Conceptual Process Design
Seider(1999)Product & Process Design Principles
Aspen Plus

2.1

10
( 0.1)

100ppm
0.999

2.2

(permeate)
(Steam Jet Ejector) 5mmHg
50 o C
4

CW

2
V-100

V=101
E-100
P-100

CW

N-butyl acetate

T-100

Low Pressure Steam

12
3

13
Waste Water

11

P-104
O-100

V-102

P-103

11

Acetic acid + Water

26

10
30
Pure Water
E-101

P-102

7
Acetic acid
P-101

Low Pressure Steam

(Direct contact condenser)

5mmHg

Aspen Plus

( K )

322.1

325.6

325.6

322.1

363.6

( atm )

( kmol hr )
( kg hr )

1
0
0.508
59.067

1
0
238.053
24084.059

1
0
238.561
24143.126

1
0
516.228
10000

1
1
738.139
33143.141

0
0
1

0.0271926
1.40E-05
0.9727933

0.0271261
1.40E-05
0.9728599

0.9
0.1
0

0.2913086
2.27E-05
0.7086687

10

( K )

322.1

391.2

325.6

267.1

325.6

( atm )

( kmol hr )
( kg hr )

1
0
738.139
33143.141

1
0
16.651
1000

1
0
500.087
9059.088

0.00658
0.148
1.828
82.123

1
0
498.258
8976.965

0.2913086
2.27E-05
0.7086687

5.08E-05
0.9995846
3.65E-04

0.9934741
4.58E-05
6.48E-03

0.291061
0
0.708939

0.9999
4.63E-05
5.37E-05

11

12

13

( K )

416.5944

305.4

323.1

( atm )

( kmol hr )
( kg hr )

0.00658
1
457.6827
8294.473

1
0
17207.615
310000

1
0
17665.298
318294.473

0.9930
0
0.0070

1
0
0

0.9998
0
0.0001

E-100

E-101

P-103

466000
32
1

15000
135
2.04

8212.35
135
2.04

P-100

P-101

P-102

P-104

( kW )

2.95

0.0614

0.675

27.4

( kg hr )
o

( C )
( atm )

(E-100)
(E-101)(O-100)(P-100P-101P-102P-104
(P-103)(T-100)
(V-100)(V-101)(V-102)

E-100

E-101

( m 2 )
( kW )

295
9192

977
9192

32

118

( o C )
( atm )

( o C )
( atm )

90

135

T-100

( C )

118

( atm )

/( m )

29.3

( m )

2.8

30

P-100

P-101

P-102

P-104

Type/Drive

20484
859.31
2.5041

1000
945.31
0.05525

8977
966.64
0.60775

318295
969.11
24.6619

( o C )
( atm )
( atm )

52.5
1
3.54

118.1
1
2.48

52.5
1
2.86

50.0
1
3.13

( kg hr )
2

( kg m )
( kW )

P-103

( kg hr )

82

Type/Drive

( mmHg )
( mmHg )

760
5
O-100

( m )

137

( o C )
( mmHg )

PEBAX2533
52.5
5

( g m 2 hr )

598.5

424.3

174.2

10

2.3

2.3.1

49o C (Antoine equation)

ln P sat = A

B
T +C

(1)

(Raoults law)

i =1

i =1

PT = Pbubble = Pi =

X i Pi sat
Yi

(2)

1atm
1atm 1atm

11

2.3.2
Aspen Plus
(Lever arm
rule)
Aspen Plus
NRTL activity coefficient method Hayden-OConnell
equation of state

12

2.3.3 (r)(s)

0.536
85.966

13

2.3.4 (BVDMBoundary Value Design Method)

Julka Doherty(1990)
(Boundary Value Design Method, BVDM)

stripping section
enriching section

1
0.9

acetic acid mole frac

0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

water mole frac

10 18
30 11

14

2.3.5

30 Eo
0.7432
4629.3

DT

G
4

DT =

Ad

G
(
)

fU

12

(3)

G f U f Ad
(Downcomer area) AT G
DT
2.8m

15

2.4

32 ~ 49o C
9192.0714 kW
466

U C 1.14 kJ K m 2 s
295
(Kettle-type reboiler)
118 o C
5o C ~ 25o C (Nucleate boiling)

122o C ~ 135o C 162o C ~ 186o C

(low pressure steam)

(minimum approach temperature) 17o C 135o C

2.04atm
2736.62 kJ kg 2.04atm 121.3o C
509.14 kJ kg 15

16


U R 1.14 kJ K m 2 s
977

17

2.5

Liu (2005)

Poly(ether block amide) (PEBAX2533Arkema )

6480 ppm 49o C (permeate)

598.5 g m 2 hr 424.3 g m 2 hr

174.2 g m 2 hr
137.2m 2
82.1 kg hr 8976.9 kg hr

46.3 ppm 53.7 ppm

18

2.6

2mmHg
100 psig 100
82.1 kg hr 100 psig
8212.3 kg hr

19

2.7
Aspen Plus 100 psig
1atm 50 o C QS ,C 5860kW

1atm 50 o C QP ,C 18.2kW 1atm

50 o C qU ,C 0.0190kW

m& dc =

QS ,C + QP ,C
qU ,C

310 Ton hr

20

(4)

2.8

(theoretical

power)
Wideal = 1.67 v& P

(5)

Wideal ( kW ) v& ( m 3 min ) P

( bar ) Aspen Plus 2

100 100 2psi
0.1psi
10psi 1.5psi
3psi

Wdrive =

Wideal

sh dr

(6)

Wdrive ( kW ) sh dr
sh dr 0.8 0.9 P-100
2.95 kW P-101 0.0614 kW P-102 0.675 kW

P-104 27.4 kW

21

Douglas Conceptual Process

Design Seider Product & Process Design Principles:

Synthesis, Analysis, and Evaluation

3.1

3.1.1

M &S
0.802
1.066
)(2.18 + Fm Fp )
(101.9 D H T
280
M &S
1.55
4.7 D H t ( Fs ,t + Ft ,t + Fm ,t )
() =
280

() =

(7)
(8)

M & S Marshall & Swift equipment cost INDEX

Chemical Engineering2006 3 M & S 1333.4 D

(ft) H T (ft) H t (ft) Fm
F p Fs ,t Ft ,t Fm,t
22


(SSStainless Steel) 96
86 24

(Sieve Plate) Fm 2.25 F p Fs 1 Ft Fm 0

888940 Fs ,t 1 Ft ,t 0 Fm,t 1.7
161672

3.1.2

M &S
0.65
101.3 AE (2.29 + Fm ,e ( Fd ,e + F p ,e ))
280

() =

(9)

AE 200 ft 2 < AE 5000 ft 2 Fm ,e

Fd ,e Fp ,e

295
(Floating head) 1 Fm,e 1Fd ,e 1
F p ,e 0 299759

977 (Kettle
Reboiler) 1 10516
5000

23

 3 3506 Fm,e 3.75 Fd ,e 1.35 F p ,e

0 2143144

3.1.3

137.22Fontalvo

(2005)2000
36

3.1.4

(f.o.b)

CP ,V = 1330S 0.41

(10)

5mmHg
S 36.2
S=

(lb hr )
(mmHg )

(11)

f.o.b 5793
CE INDEX = 394 2006 8 CE INDEX = 510.0
7499
2.1 f.o.b
23682 Bare-Module
24

 51967
3.1.5
f.o.b

C P , P = exp 9.2951 0.6019[ln(S P )] + 0.0519[ln(S P )]

(12)

S P
S P = Q (H )

0.5

(13)

Q ( gpm ) H ( ft )
f.o.b
CE INDEX = 394 2006 8 CE INDEX = 510.0

Bare-Module

H ( ft )

Q ( gpm )
SP

P-100

P-101

P-102

P-104

3.111947 1.653319 2.024748 2.315506

102.7577 3878.49 34048.6
181.2719 4987.018 48448.98

1204182
1832378

C P , P (UDS)

1936

2787

6920

90094

C P (UDS)

4241

6104

15154

197306

25

3.2

3.2.1

15 / 8.212 /
650 463 /

3.2.2

466 /
1 14.32

3.2.3

310 /
4

38.1 /

26

3.2.4

319 /
4 39.2 /

3.2.5

508.5 /
0.16 81.72 /

3.2.6

31.086 kW 2.5

NTD/kWh 2.39 /

27

3.3 (Total Annual Cost, TAC)

6755787

TAC =

CTBC
+ COW
3

(14)

CTBC (Total Bare module Cost)

COW

3.4

3.4.1

1
500 500 /

3.4.2

8.976
4 1.1 /

3.5

676

28

 400

TAC
()

888940

161672

299759

2143144

1158231

51967

222805

4926517

(/)

463

14.32

38.1

39.2

81.72

2.39

638.73

(/)
TAC

6755787

(/)

4000000

8823

29

(Manipulated variable)
(Control variable)

(inferential control)

(RGA)

0.01%
( QC QR )

30

363.6

364.3

364.8

365.1

365.3

365.4

365.4

TRC
TRC QR

366.4
3.04

367.8
3.77

368.2
3.66

369.4
4.62

373.4
8.71

373.9
9.24

373.7
8.99

TSS
TRC
TRC QR

10

11

12

13

14

365.4
373.6
8.85

365.4
373.6
8.78

365.4
373.5
8.76

365.4
373.5
8.79

365.3
373.5
8.87

362.8
373.5
11.51

369.1
373.5
4.74

TSS
TRC
TRC QR

15

16

17

18

19

20

21

374.0
373.5
-0.53

375.0
373.5
-1.57

375.8
373.5
-2.45

377.3
373.5
-4.05

379.8
373.5
-6.79

383.1
373.5
-10.28

386.1
373.5
-13.50

TSS

22

23

24

25

26

27

28

388.2

389.5

390.3

390.7

390.9

391.0

391.1

TRC
TRC QR

373.6
-15.80

373.6
-17.20

373.6
-17.97

373.7
-18.36

373.8
-18.51

373.9
-18.54

374.0
-18.47

TSS
TRC
TRC QR

29

30

391.1
374.1
-18.34

391.1
374.3
-18.12

TRC/QR

TSS

reboiler

391.2
374.7
-17.76

15
10
5
0
-5
-10
-15
-20
-25
1

9 11 13 15 17 19 21 23 25 27 29 31
stage

31

TSS

363.6

364.3

364.8

365.1

365.3

365.4

365.4

TCC
TCC QC

363.8
-0.28

364.9
-0.65

365.6
-0.86

366.0
-0.93

366.2
-0.94

366.2
-0.93

366.3
-0.91

TSS
TCC
TCC QC

10

11

12

13

14

365.4
366.2
-0.89

365.4
366.2
-0.84

365.4
366.1
-0.77

365.4
366.0
-0.66

365.3
364.1
1.29

362.8
372.2
-10.17

369.1
373.8
-5.03

TSS
TCC
TCC QC

15

16

17

18

19

20

21

374.0
373.8
0.21

375.0
373.8
1.24

375.8
373.8
2.11

377.3
373.8
3.69

379.8
373.9
6.42

383.1
373.9
9.90

386.1
373.9
13.09

TSS

22

23

24

25

26

27

28

388.2

389.5

390.3

390.7

390.9

391.0

391.1

TCC
TCC QC

374.0
15.36

374.1
16.72

374.1
17.43

374.3
17.73

374.5
17.76

374.8
17.56

375.3
17.05

TSS
TCC
TCC QC

29

30

391.1
376.3
15.97

391.1
378.3
13.83

reboiler

391.2
381.4
10.55

20

TCC/QC

15
10
5
0
-5
-10
-15
1

9 11 13 15 17 19 21 23 25 27 29 31
stage

32


13 26 13
5~12
6 26
RGA u1 QC u 2
QR y1 6 T6 y2 26 T26 RGA( )(15)

= 11
21

p11 =

y1

u1 c2 ,OL
y
1
12 u1 c2 ,CL
=
22 y2
u1 c ,OL
1

y2
u
1 c1 ,CL

c2 ,OL

y1

u 2 c ,CL p11 p22

2
=
y2
p12 p21
u 2 c ,OL
1

y2

u 2 c ,CL
1

y1
u2

p12 p21
det( P ) 1
p11 p22

(15)

y1
y
y
y
= 0.93 p 21 = 2 = 17.76 p12 = 1 = 9.24 p 22 = 2 = 18.51
u1
u1
u2
u2

P
0.93 17.76
P=

9.24 18.51

164.10
17.21
0.117 1.117
=
(6.81 10 3 ) =

164.10 17.21
1.117 0.117

33

(inventory control) Chien (2004)

34

CW

LC

V-100

V=101
E-100
PC

P-100

N-butyl acetate

V-103

CW
V-101

T-100

Low Pressure Steam

V-102

Waste Water

6
P-104
O-100

V-102

P-103
11
TC

Acetic acid + Water

TC
26

30
Pure Water

LC
E-101

E-24

V-100

Acetic acid
V-104

P-101

Low Pressure Steam

35

.
16

AO (air-to-open)
36

 AC (air-to-close)

37

1.

2.

(BVDM)

3.

(RGA)

4.
676 400

5.

38

Aspen Plus

39

1. Aspen Technology, Inc., Aspen Plus Users Manual 11.1. Aspen

Technology, Inc., Cambridge, 2001.
2. Bristol, E. H., On a new measure of interactions for multivariable
process control, IEEE Trans. Auto. Control, AC-11, 133-134, 1966.
3. Chien, I.L., Kuo, C. L., Investigating the need of a pre-concentrator
column for acetic acid dehydration system via heterogeneous
azeotropic distillation, Chem. Eng. Sci., 61, 569-585, 2006.
4. Chien, I.L., Zeng, K.L., Chao, H.Y., Liu, J.H., Design and control of
acetic acid dehydration system via heterogeneous azeotropic
distillation, Chem. Eng. Sci., 59, 4547-4567, 2004.
5. Douglas, J.M., Conceptual Process Design, McGraw-Hill, New York,
1988.
6. Fontalvo, J., Cuellar, P., Timmer, J. M. K., Vorstman, M. A. G., Wijers,
J. G. and Keurentjes, J. T. F., Comparing pervaporation and vapor
permeation hybrid distillation processes, Ind. Eng. Chem. Res., 44,
5259-5266, 2005.
7. Ho Song Kun, Hoon Song Jee, Rae Lee Kwang, Vapor permeation of
ethyl acetate, propyl acetate, and butyl acetate with hydrophobic
inorganic membrane, Sep. & Pur. Tech., 30, 169-176, 2003.
8. Julka, V., Doherty, M.F., Geometric behavior and minimum flows
for nonideal multicomponent distillation, Chem. Eng. Sci., 45,
1801-1822, 1990.
9. Liu, K., Tong, Z., Liu, L., Feng, X., Separation of organic
compounds from water by pervaporation in the production of n-butyl
acetate via esterification by reactive distillation, J. Mem. Sci., 256,
193-201, 2005.

40

10. McCabe, W. L., Smith, J. C., Harriott, P., Unit operations of chemical
engineering, 6th ed, McGraw-Hill, New York, 2001.
11. Othmer, D.F., Azeotropic separation, Chem. Eng. Prog., 59 (6),
67-78, 1963.
12. Seider, W. D., Seader, J. D., Lewin, D. R., Product & process design
principles, John Wiley & Sons, Inc, 1999.

41

AE

Ad

AT

C P,P

f.o.b

C P ,V

f.o.b

CTBC

COW

DT

Eo

Fd ,e

Fm

42

Fm ,e

Fm ,t

Fp

Fp ,e

Fs ,t

Ft ,t

HT

Ht

m& dc

p11

p12

p21

p22

P sat

Pbubble

43

Pi

Pi sat

PT

QC

QP ,C

QR

QS ,C

qU ,C

SP

T6

T26

26

TCC

0.01%

TRC

0.01%

TSS

u1

u2

2
44

Uf

UC

UR

v&

Wideal

Wdrive

Xi

Yi

y1

y2

dr

sh

45

(r)(s)

(BVDMBoundary Value Design

Method)

46

FEED =

9000 1000
+
= 516.67 kmole / hr
18
60

By lever arm rule

FEED
8.65
=
REFLUX
4.2
REFLUX = 250.87 kmole / hr

By lever arm rule

DIST1 18.75
=
BOTM
0.5
DIST 1 = 37.5 BOTM

By C101 mole balance

FEED + REFLUX = DIST 1 + BOTM
BOTM = 19.94kmole / hr

DIST 1 = 747.60kmole / hr

By D101 mole balance

DIST1 = DIST 2 + REFLUX
DIST 2 = 496.73kmole / hr

FEED
WH 2 O = 0.9

WAA = 0.1

WNBUT = 0

47

X H 2O

0.9
18
=
= 0.968
0.9 0.1
+
18 60

X AA

0.1
60
=
= 0.032
0.9 0.1
+
18 60

X NBUT = 0

REFLUX
X H 2 O = 0.15

WH 2 O =

X AA 0

X NBUT = 0.85

0.15 18
= 0.027
0.15 18 + 0.85 116

WNBUT =

0.85 116
= 0.973
0.15 18 + 0.85 116

WAA = 0

DIST1
X H 2 O = 0.719

WH 2 O =

X AA 0

X NBUT = 0.281

0.719 18
= 0.284
0.719 18 + 0.281 116

WNBUT =

0.281 116
= 0.716
0.719 18 + 0.281 116

WAA = 0

BOTM
X H 2O = 0

X AA 1

X NBUT = 0

48

WH 2 O = 0

WAA 1

WNBUT = 0

WH 2 O 1

WAA = 0

WNBUT = 0

X H 2O 1

X AA = 0

X NBUT = 0

DIST2

STEAM
STEAMJET

CONTCOND
P-CHANGE

MIXER

MAKEUP
CWATER

PERM EATE
ETRANER

REFLUX

COOLER
TOPVAP

DECANTER
WASTE

COND
PERVAP

COLUM N
AQ
FEED

RETENTAT
BOTM

49

(r)(s)

1. Flash3 (r)

(reflux ratio) Aspen plus

Flash3 (Decanter)

r=

L REFLUX 254.704
=
=
= 0.536
D
AQ
475.519

FEED
Pressure = 1atm

VaporFrac = 1
TotalFlow = 33000kg / hr
X H 2O = 0.7231

X AA = 0

X NBUT = 0.2769

Flash3
Pressure = 1atm

VaporFrac = 0

50

(16)

VAPOR

FLASH3

FEED

REFLUX

AQ

Flash3

Flash3

Heat and M aterial Balance Table

Stream ID

FEED

Temperature

Pressure

atm

Vapor Frac

VAPOR

REFLUX

363.7
1.00

364.1
1.00

1.000

AQ
364.1

1.00
0.000

1.00
0.000

M ole Flow

kmol/hr

730.225

0.000

254.706

475.519

M ass Flow

kg/hr

33000.000

0.000

24375.920

8624.080

Volume Flow

l/min

354534.719

0.000

Enthalpy

M M Btu/hr

M ass Flow

kg/hr

WATER

495.200

155.194

-211.152

-112.161

-126.804

9512.526

956.469

8556.056

23487.474

23419.451

68.023

0.288

0.039

0.992

0.712

0.961

0.008

528.025

53.092

474.933

202.199

201.614

0.586

0.723

0.208

0.999

0.277

0.792

0.001

ACETI-01
N-BUT-01
M ass Frac
WATER
ACETI-01
N-BUT-01
M ole Flow
WATER

kmol/hr

ACETI-01
N-BUT-01
M ole Frac
WATER
ACETI-01
N-BUT-01

51

2.

(Separator)(Heater)(Cooler)

H F H D H B = 142.1 - (-7.451 - 134.517) = 0.132MMBtu/hr

= 38.7968 KW

FEED
Pressure = 1atm

Temperature = 49 o C

TotalFlow = 10000kg / hr
WH 2O = 0.9

W AA = 0.1

X NBUT = 0

Sep
Outletstream = DIST 1

Water : AA : NBUT = 1 : 0 : 0

52

COOLER
Pressure = 1atm

Temperature = 49o C

ValidPhases = Vapor Liquid

HEATER
Pressure = 1atm

VaporFrac = 1
ValidPhases = Vapor Liquid

53

COOLER
DIST1

DIST

SEP
FEED

HEATER
BOTM

BOTM1

Heat and Material Balance Table

Stream ID

BOTM

Temperature

Pres sure

atm

Vapor Frac

BOTM1

DIST

DIST1

FEED

391.2

322.1

322.1

322.1

1.00

1.00

1.00

1.00

322.1
1.00

0.000

0.000

0.000

0.000

0.000

Mole Flow

kmol/hr

16.652

16.652

499.576

499.576

516.228

Mas s Flow

kg/hr

1000.000

1000.000

9000.000

9000.000

10000.000

Volume Flow

l/min

17.630

16.004

154.629

154.629

172.824

Enthalpy

MMBtu/hr

-7.451

-7.575

-134.517

-134.517

-142.100

Mas s Flow

kg/hr
9000.000

9000.000

9000.000

1000.000

1000.000

1.000

1.000

16.652

16.652

W ATER
ACETI-01

1000.000

N-BUT-01
Mas s Frac
W ATER

1.000

ACETI-01

1.000

0.900
0.100

N-BUT-01
Mole Flow

kmol/hr

W ATER
ACETI-01

499.576

499.576

499.576
16.652

N-BUT-01
Mole Frac
W ATER
ACETI-01

1.000
1.000

1.000

N-BUT-01

54

1.000

0.968
0.032

3. QC

QC (Heater)
49

Q C = 9561.227 KW

TOP,IN
Pressure = 1atm

VaporFrac = 1
TotalFlow = ( R + 1) 500kmole / hr = 1.536 500
= 768kmole / hr

X H 2O = 0.7231

X AA = 0

X NBUT = 0.2769

HEATER
Pressure = 1atm

Temperature = 49 o C
ValidPhases = Liquid Only

55

HEATER

TOP,IN

TOP,OUT

Heat and M aterial Balance Table

Stream ID

TOP,IN

Temp erature

Pressure

atm

Vapor Frac

TOP,OUT

363.7

322.1

1.00

1.00

1.000

0.000

768.000

768.000

kg/hr

34707.130

34707.130

l/min

372875.226

640.843

-222.075

-254.699

10004.620

10004.620

24702.510

24702.510

0.288

0.288

0.712

0.712

555.341

555.341

212.659

212.659

0.723

0.723

0.277

0.277

M ole Flow

kmol/hr

M ass Flow
Volume Flow
Enthalpy

M M Btu/hr

M ass Flow

kg/hr

WATER
ACETI-01
N-BUT-01
M ass Frac
WATER
ACETI-01
N-BUT-01
M ole Flow

kmol/hr

WATER
ACETI-01
N-BUT-01
M ole Frac
WATER
ACETI-01
N-BUT-01

56

4. Q R

H F H D H B = QR QC
Q R = H F H D H B + QC = 38.7968 + 9561.227 = 9522.4302 KW

5. q R

(reboiler) 1 /

qR = 6.64486 KW

VB =

Q R 9522.4302
=
= 1433.052kmole / hr
qr
6.64486

B = 16.67 kmole / hr

s=

V B 1433.052
=
= 85.966
B
16.67

57


1. BOTM,IN
Pressure = 1atm

VaporFrac = 0
TotalFlow = 1kmole / hr

X H 2O = 0

X NBUT = 0

X AA = 1

2. HEATER
Pressure = 1atm

VaporFrac = 1

ValidPhases = Vapor Liquid

58

HEATER

BOTM ,IN

BOTM ,OUT

Heat and M aterial Balance Table

Stream ID

BOTM ,IN

Temp erature

Pressure

atm

391.2

Vapor Frac
M ole Flow

kmol/hr

M ass Flow

kg/hr

Volume Flow

l/min

Enthalpy

M M Btu/hr

M ass Flow

kg/hr

BOTM ,OUT
391.2

1.00

1.00

0.000

1.000

1.000

1.000

60.053

60.053

1.059

337.098

-0.447

-0.425

60.053

60.053

1.000

1.000

1.000

1.000

1.000

1.000

WATER
ACETI-01
N-BUT-01
M ass Frac
WATER
ACETI-01
N-BUT-01
M ole Flow

kmol/hr

WATER
ACETI-01
N-BUT-01
M ole Frac
WATER
ACETI-01
N-BUT-01

59

(BVDMBoundary Value Design

Method)

1. Flash3 (Decanter)

Aspen plus Flash3

(Decanter)

FEED
Pressure = 1atm

VaporFrac = 1
TotalFlow = 33000kg / hr
X H 2O = 0.723

X NBUT = 0.2769

X AA = 0.0001

Flash3 unit
Pressure = 1atm

VaporFrac = 0

60

VAPOR

FLASH3

FEED

REFLUX

AQ

Flash3

Flash3

Heat and M aterial Balance Table

Stream ID

FEED

Temp erature

Pressure

atm

Vapor Frac

VAPOR

REFLUX

363.8
1.00

364.1
1.00

1.000

AQ
364.1

1.00

1.00

0.000

0.000

M ole Flow

kmol/hr

730.157

0.000

254.770

475.387

M ass Flow

kg/hr

33000.000

0.000

24376.681

8623.319

Volume Flow

l/min

355113.519

0.000

Enthalpy

M M Btu/hr

M ass Flow

kg/hr

WATER

495.211

155.187

-211.118

-112.180

-126.775

8553.023

9510.325

957.303

ACETI-01

4.385

2.267

2.117

N-BUT-01

23485.290

23417.111

68.179

M ass Frac
WATER
ACETI-01
N-BUT-01
M ole Flow
WATER

0.288

0.039

0.992

133 PPM

93 PPM

246 PPM

0.712

0.961

0.008

kmol/hr
527.903

53.138

474.765

ACETI-01

0.073

0.038

0.035

N-BUT-01

202.180

201.593

0.587

M ole Frac
WATER

0.723

0.209

0.999

ACETI-01

100 PPM

148 PPM

74 PPM

N-BUT-01

0.277

0.791

0.001

61

2. Flash2

(Boundary Value Design Method, BVDM)

Flash2

y N +1 =

x
r
xN + D
r +1
r +1

(17)

Flash2

Flash2

62

VAPOR
Pressure = 1atm

VaporFrac = 1
TotalFlow = 1kg / hr
X H 2O = 0.0005

X NBUT = 0.0005

X AA = 0.999

Flash2
VaporFrac = 0.999
Pressure = 1atm

63

EQVAPOR

FLASH2

VAPOR

EQLIQUID

Flash2

D
x water

0.99873

0.208483

0.217926

0.224644

0.229993

0.23502

x Acetic acid

3.66E-05

7.32E-05

0.000254

0.00059

0.001223

0.002421

x N ba

0.001233

0.791444

0.78182

0.774766

0.768785

0.762558

10

x water

0.240952

0.249834

0.266063

0.302198

0.439265

0.948637

x Acetic acid

0.004703

0.009065

0.017497

0.034467

0.076448

0.048765

x N ba

0.754345

0.741101

0.71644

0.663335

0.484287

2.60E-03

64

3. Flash2

Flash2

x M +1 =

x
s
yM + W
s +1
s +1

VAPOR
Pressure = 1atm

VaporFrac = 0
TotalFlow = 1kg / hr

Flash2 unit
VaporFrac = 0.001
Pressure = 1atm

65

(18)

EQVAPOR

FLASH2

LIQUID

EQLIQUID

Flash2

x water
x Acetic acid
x N ba

0.0005

0.0005

0.000976

0.001898

0.003685

0.007138

0.013785

0.999

0.999

0.99858

0.997706

0.995962

0.992546

0.98593

0.0005

0.0005

0.000444

0.000396

0.000353

0.000316

0.000284

10

11

12

13

x water

0.026489

0.050412

0.094193

0.169997

0.287951

0.440295

0.591046

x Acetic acid

0.973254

0.949352

0.905587

0.82979

0.711829

0.559442

0.408537

x N ba

0.000257

0.000236

0.00022

0.000212

0.00022

0.000263

0.000418

14
x water

15

16

17

18

0.70529

0.778805

0.809625

0.710045

0.722733

x Acetic acid

0.293655

0.216526

0.156847

0.07366

0.020264

x N ba

0.001055

0.004669

0.033528

0.216295

0.257003

66

10 18 (
) 30 () 11

stripping section
enriching section

1
0.9

acetic acid mole frac

0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

water mole frac

BVDM

67

0.9

( H actual )
Eo L = 0.328cP Eo
0.7

N equilibrum = 30 (
)
N actual =

N equilibrum
Eo

30
= 43
0.7

(19)

24
6
H actual = N actual 2 + 4 + 6 = 96 ft = 29.26m

68

(20)

2.3.5.2 ( DT )
(flow ratio parameter) FLG

FLG

L
= G
G L

0.5

(21)

L G L G

L(kg/hr)
G (kg/hr)

L (kg/cum)
G (kg/cum)
FLG

L(kg/hr)
G (kg/hr)

L (kg/cum)
G (kg/cum)
FLG

L(kg/hr)
G (kg/hr)

L (kg/cum)
G (kg/cum)
FLG

FLG

27157.24
36157.24
27.32199
821.9479
0.032837

27702.98
36702.98
26.44603
819.9183
0.033261

28029.67
37029.67
25.92473
818.6666
0.033513

28204.89
37204.89
25.64188
817.9901
0.033647

28284.71
37284.71
25.50385
817.6928
0.033706

10

11

12

28302.56 28272.4
37302.56 37272.4
25.45403 25.46557
817.6535 817.8272
0.033718 0.033691
13

14

28193.09 28050.15 27813.98 27431.82 27168.36 32836.22 23261.71

37193.09
25.53318
818.2337
0.033625

37050.15 36813.98 36431.82 36168.36 31836.22

25.66961 25.90813 26.31434 27.02153 49.26367
818.9567 820.1576 822.1149 825.3286 868.926
0.033506 0.03331 0.03299 0.032773 0.040068

22261.71
51.74033
893.0165
0.033318

15

16

17

18

19

20

21

23936.32
22936.32
49.88414
894.519
0.033537

26843.78
25843.78
47.40931
895.1748
0.035283

31980.93
30980.93
43.5964
898.8269
0.038084

40284.01
39284.01
38.13641
907.6292
0.041996

51278.55
50278.55
31.90872
919.8982
0.0464

62392.41
61392.41
26.53311
930.6678
0.050247

71212.47
70212.47
22.82094
937.5749
0.052976

69


L(kg/hr)
G (kg/hr)

L (kg/cum)
G (kg/cum)
FLG

L(kg/hr)
G (kg/hr)

L (kg/cum)
G (kg/cum)
FLG

22

23

24

25

26

27

28

77092.1 80596.79 82551.69 83602.32 84155.76 84444.26 84593.86

76092.1
20.58929
941.3537
0.054662

79596.79
19.34504
943.3044
0.055619

81551.69 82602.32 83155.76 83444.26 83593.86

18.67767 18.3267 18.14395 18.04927 18.00034
944.2981 944.8042 945.0619 945.1926 945.2579
0.056139 0.056414 0.056558 0.056633 0.056672

29

30

reboiler

84671.27
83671.27
17.97506
945.2893
0.056692

84711.33
83711.33
17.96199
945.3031
0.056702

1000
83711.33
17.95522
945.3074
0.000669

C SB FLG 24

FLG CSB

70

C SB ( ft / s )
C SB (m / s )

C SB ( ft / s )
C SB (m / s )

C SB ( ft / s )
C SB (m / s )

C SB ( ft / s )
C SB (m / s )

C SB ( ft / s )
C SB (m / s )

C SB

0.39

0.39

0.39

0.39

0.39

0.39

0.39

0.118872 0.118872 0.118872 0.118872 0.118872 0.118872 0.118872

8

10

11

12

13

14

0.39
0.39
0.39
0.39
0.39
0.39
0.39
0.118872 0.118872 0.118872 0.118872 0.118872 0.118872 0.118872
15

16

17

18

19

20

21

0.39
0.39
0.39
0.39
0.39
0.39
0.39
0.118872 0.118872 0.118872 0.118872 0.118872 0.118872 0.118872
22

23

24

25

26

27

28

0.39

0.39

0.38

0.38

0.38

0.38

0.38

0.118872 0.118872 0.115824 0.115824 0.115824 0.115824 0.115824

29

30

reboiler

0.37
0.37
0.37
0.112776 0.112776 0.112776

71

 FST

FST

=
20

0.20

(22)

(dyne/cm)
FST

(dyne/cm)
FST

(dyne/cm)
FST

(dyne/cm)
FST

(dyne/cm)
FST

FST
3

1.571045 1.592218 1.604711 1.611321 1.614255 1.614789 1.613424

1.064379 1.057465 1.053263 1.050955 1.049821 1.04941 1.049505
8

10

11

12

13

14

1.610062 1.604071 1.594187 1.578171 1.571093 1.311312 0.907935

1.050062 1.051182 1.053128
15

16

17

18

0.923767 1.032905 1.223423

1.200567 1.188411 1.168649
22

23

1.05641 1.062028 1.197566 1.209372

24

19

20

21

1.52227 1.90398 2.274981 2.557922

1.13779 1.097933 1.058161 1.026741
25

26

27

28

2.740168 2.846163 2.904392 2.935415 2.951681 2.96014 2.964523

1.005825 0.993363 0.986412 0.982677 0.98071 0.979684 0.979152
29

30

reboiler

2.96679 2.967965 2.967965

0.978877 0.978735 0.978661

72

 FF = 1

Ah Aa

0.1 FHA

FHA

Ah
1.0
0.06

Aa

1,

=
5 Ah + 0.5 ,

Aa

Ah
0.1
Aa

(23)

FHA = 1

empirical capacity parameter C

C = C SB FST FF FHA

C (m / s)

C (m / s)

C (m / s)

C (m / s)

C (m / s)

(24)

C
3

0.126525 0.125703 0.125203 0.124929 0.124794 0.124745 0.124757

8

10

11

12

13

0.124823 0.124956 0.125187 0.125578 0.126245 0.142357

15

16

0.142714 0.141269
22

23

0.119564 0.118083
29

30

17

18

19

20

14

0.14376
21

0.13892 0.135251 0.130513 0.125786 0.122051

24

25

0.11425 0.113818
reboiler

0.110394 0.110378 0.110369

73

26

27

28

0.11359 0.113471 0.113409

 U f

G
U f = C L
G

12

(25)

DT

4G

DT =

Ad
G
( fU f ) 1
A

12

(26)

Ad
FLG
AT
FLG 0.1

0.1,
(F 0.1) ,
Ad
= 0.1 + LG
AT
9
0.2,

0.1 FLG 1.0

FLG 1.0

74

(27)

U f (m / s)

Ad / AT
DT (m)

U f (m / s)

Ad / AT
DT (m)

U f (m / s)

Ad / AT
DT (m)

U f (m / s)

Ad / AT

2.81202 2.805915 2.804286 2.806028

10

11

12

13

14

2.811151 2.820658 2.836726 2.863414 2.890775 3.661756 4.506309

0.1
0.1
0.1
0.1
0.1
0.1
0.1
2.075007 2.071381 2.065285 2.055291 2.042717 1.863867 1.68847
15

16

17

18

19

20

21

4.438696 4.156418 3.762856 3.299783 2.865789 2.541021 2.333492

0.1
0.1
0.1
0.1
0.1
0.1
0.1
1.712005 1.775988 1.877811 2.024283 2.197303 2.358937 2.482631
22

23

2.212874 2.146482

29

DT (m)

0.1
0.1
0.1
0.1
0.1
0.1
0.1
2.04226 2.058721 2.068739 2.074205 2.076796 2.077553 2.076947

DT (m)

Ad / AT

2.891268 2.849756 2.825176

0.1
2.564217

U f (m / s)

U f Ad At DT

24

25

27

28

2.05691 2.038778 2.029341 2.024451 2.021922

0.1
0.1
0.1
2.6128 2.674442 2.689233
30

26

0.1
0.1
0.1
2.69703 2.701098 2.703209

reboiler

1.967438 1.966776 1.966632

0.1
0.1
0.1
2.740603 2.741178 2.741278

DT 2.8m

75

(Condenser)

Aspen plus Q C = 9192.0714kW

32 ~ 49o C

& cCP ,c Tc
QC = m

(28)

CP ,C
C P ,C = 4.18 kJ kg K

(29)

&c =
m

&c =
m

QC
CP , c Tc

9192.0714
= 129.356kg/sec = 465683kg/hr
4.18 (49 - 32)

76

(30)

U C
U C = 200 Btu o F ft 2 hr = 1.13545 kJ K m 2 s

(Log Mean Temperature Difference, LMTD)

TLM ,C =

TLM ,C =

Th Tc (Th ,in Tc ,out ) (Th ,out Tc ,in )

=
Th
(T T )
ln
ln h,in c , out
Tc
(Th, out Tc ,in )

(31)

(363.6 322.1) (322.1 305.1)

= 27.45 K
(363.6 322.1)
ln
(322.1 305.1)

AC
QC = U C AC TLM ,C

AC =

QC
9192.0714
=
= 295m 2
U C TLM ,C
1.13545 27.45

77

(32)

(33)

(reboiler)

(Kettle-type reboiler) Aspen

plus 118 o C

5o C ~ 25o C
(Nucleate boiling)
122o C ~ 135o C 162o C ~ 186o C
(low pressure steam)

(minimum approach temperature) 17o C 135o C

2.04atm
2736.62 kJ kg 2.04atm 121.3o C
509.14 kJ kg
&h =
m

&h =
m

QR
Q

9192.0714
= 4.13kg s = 14856 kg hr 15 ton hr
2736.62 509.14

78

(34)

VS

79

U R

U R = 200 Btu o F ft 2 hr = 1.13545 kJ K m 2 s

AR
QR = U R AR TLM , R

TLM , R =

AR =

(135 118) (121.3 118)

= 8.357 K
(135 118)
ln
(121.3 118)

QR
9267.12803
=
= 977 m 2
U R TLM , R 1.13545 8.357

80

(35)

(36)

(37)

Arkema

Poly(ether block amide) (PEBAX2533) Liu (2005)

xF , N BA = 6480ppm

49o C (permeation)
J total = 598.5 g m 2 hr

J N BA = 424.3 g m 2 hr

J WATER = J total J N BA = 174.2 g m 2 hr

81

(38)

82


F = 9059.088 kg hr

WF ,WATER = 0.99347 WF , AA = 0.00005 WF , N BA = 0.00648

V = J total A
WV ,WATER =

(39)

J WATER A
J
A
= 0.291 WV , AA = 0 WV , N BA = N BA
= 0.709
J total A
J total A

(retentate)
WL ,WATER = 0.9999

F = V + L = J total A + L

(40)

F WF ,WATER = V WV ,WATER + L WL ,WATER = ( J total A) WV ,WATER + L WL ,WATER

(41)

F WF , AA = V WV , AA + L WL , AA = ( J total A) WV , AA + L WL ,, AA

(42)

F WF , N BA = V WV , N BA + L WL , N BA = ( J total A) WV , N BA + L WL, N BA

(43)

L WL , AA
WL , N BA
83

 Apervaporation = 137.2155m 2
V = 82.1235 kg hr L = 8976.96454 kg hr

xL , AA = 46.3 ppm xL , N BA = 53.7 ppm

84