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- 1 -

LCD

.

2006 7 21

:

:

:

:

:

:

:

:

- 2 -

032-051-006

2 () / ()

LCD

Combined process development for purification of waste- solvent from LCD process

: 7 : 3 : 4

: 347,000 : 116,000 : 463,000

: 7 : 3 : 4

: 347,000 : 116,000 : 463,000

()

: :

: :

(500 )

88

LCD

, ,

. IT ,

. LCD (IPA)

stripper . IPA

. LCD IPA

.

.

- 3 -

LCD IPA

, .

, IPA

99.99% IPA .

, bench

.

( 5 )

, , , , ,

IPA, adsorbent, combined-process, organic solvent, separation, purification

- 4 -

.

LCD

.

LCD

, ,

. IT

,

. LCD (IPA)

stripper . IPA

.

, 99.99% IPA

. 25KG/day IPA

bench .

.

IPA (25kg IPA/day)

, /

.

,

. bench

pilot

.

- 5 -

.

,

. lab

bench IPA 99.99% IPA LCD

IPA 25kg .

2 /

/.

.

IPA

, pilot LCD

IPA . ,

, ,

,

.

- 6 -

S U M M A R Y

Organic solvent such as methano, ethano and isopropyl alcohol (IPA) which

are used as main cleaning agent in the semiconductor and LCD process, are

one of representative cleaning solvent. Therefore, as the market on the

information technology have been bigger and bigger, the demand on these

organic solvent is being increased and several kinds of technologies for

purifying the waste solvent are suggested. However, azeotropic point of waste

alocohol including water have limited their commercial applications. Among the

suggested ones, the purification method using adsorption and desorption

phenomena are considered as a most efficient alternative for purifying waste

solvent such as methanol, ethanol and IPA.

In this research, we quantitatively measured the water-adsorption capability

of adsorbents having various pore sizes and surface areas, Because adsorption

properties are changed according to the adsorption bed temperature, its effect

was also considered. Ultra high pure IPA (>99.99%) was successfully obtained

from the bench-scale trial apparatus in which the waste IPA from LCD process

was introduced. This apparatus was automatically operated and the long time

operation data will be used for the pilot scale study. In the future, we plan to

test large scale waste-IPA purifucation system including ion-exchange bed and

distillation column for evaluating this approach in economic view.

- 7 -

C O N T E N T S

Chapter 1. Introduction

Chapter 2. Status of Technical Development

Chapter 3. Research Results

Chapter 4. Attainment of Research Goal and the Contribution

Chapter 5. Application of Research Results

Chapter 6. Other Technical Informations

Chapter 7. References

- 8 -

1 1

2

3

2

3 1

2

3 IPA

4 IPA

5 IPA set-up

6 IPA

7

4

5

6

7

- 9 -

1

1

. 2

,

.

.

.

,

. , ,

,

.

,

.

.

.

1 22

1,

21 . ,

, 1990 44%

56%

- 10 -

. , , , ,

.

20

.

,

.

15,

43 .

1 1990 .[1]

1-1. 1990

( : /)

82 19 48 5 10

190 73 69 7 41

302 102 146 11 43

, 394 353 0 2 39

968 547 263 25 133

6,312 2,766 418 2,344 796

15,123 8,880 3 5,104 1,136

21,477 11,646 421 7,448 1,932

22,415 12,193 684 7,473 2,065

- 11 -

2

2

1 .[2] 1

, 70wt%

1-2 3 . IPA

99.99% , ,

100% .

- 12 -

1-2.

INDUSTRY EMISSION SOURCE

Synthetic fiber and films Waste waters, vapors in air

Paper coatings, graphic arts

Vapors in air

Printing

Film coating, photographic & magnetic

Protective coatings, industrial

Architectural coatings

Degreasing, dry cleaning Contaminated liquids

Solvent refining of vegetable oils Waste waters, tank vents

Solvent extraction of pharmaceuticals from natural products Waste waters

Chemical manufacturing

Azeotropic & extractive distillation Waste waters, tank vents

Chemical reaction & crystallization Waste waters, mixed liquids

Chemical drying Vapors in air

Petroleum refining Waste waters, tank vents

Resin manufacturing

Reactor distillate Waste waters

Solvent quench Concentrated vapors

Extractive metallurgy Waste waters

Nuclear-fuel reprocessing Contaminated liquids

- 13 -

1-1.

FROM

PROCESS

Solvent

vapors

in air

Solvent

vapors

in air

Solvent

vapors

in air

Solvent

vapors

in air

Solvent

vapors

in air

PRETREATMENT

Cooling CoolingCooling

PURIFICATION

Adsorption AbsorptionBurningSimple

distillationCondensing

RECOVERY

Desiccant

drying

Desiccant

drying

Desiccant

drying

Desiccant

drying

Pure

Recovered

solvent

TOPROCESS

- 14 -

(CONTINUED)

VACUUM DRYING

S T I R R I N G

A D D I T I O N

R E F L U X

C O O L I N G

A D D I T I O N

SEPARATION

C D C A

H K C A

MeOH

Water Layer

Na-Metal

To Recovery System

Discard

Water

- 15 -

(CONTINUED)

1-2. Block diagram for the discharge of sec-Butanol & Methanol

Organic Layer

S B AVAC. DIST'N

To Recovery SystemDistillate

U D C A

VAC. DIST'N

Organic Layer

SEPARATION

A D D I T I O NWater

Water Layer

Discard

S B A

To Recovery System

- 16 -

(CONTINUED)

R E A C T O R

S O L U T I O N

Methanol

A D D I T I O NKOH

PHOG A D D I T I O N

IPA A D D I T I O N

To Recovery System

MethanolVAC. DIST'N

R E F L U X

D R Y I N G

- 17 -

(CONTINUED)

1-3. Block diagram for the discharge of Methanol

LCD(Liquid Crystal Display) LCD

(Isopropyl alcohol) . LCD

IPA

. IPA

.

IPA

IPA

IPA . ,

LCD .

A D D I T I O N

R E F L U X

C O O L I N G

FILTRATION

IPA

IPA

W A S H I N G IPAIPA

D R Y I N G

DANNE Salt

- 18 -

LCD IPA ,

.

LCD 1-4 , PR stripper

IPA . IPA

, IPA

(100~500ppm), stripper(BDG/NMP/MEA, 5~15 wt%), photo resist(1%) .

LCD , IPA

. IPA

, IPA 190(LG LCD

) . IPA

.

1-4. LCD

/LCD ,

. (watermark)

,

- 19 -

.

.

LCD

. 2.0

ml 0, 0.5 2.0 ml 0 2, 0.1 0.5

ml 0 30, / ppb ,

10ppm . ,

0.1 100ppm .

, , ,

.

IPA .

IPA , IPA

. ,

,

.

(Pervaporation membrane) . 300

500ppm . ,

100ppm

. ,

.[3]

(molecular sieve)

, .

,

.

, 5,053,563 4,762,616 -

.

. ,

- 20 -

,

,

- 21 -

3

IT 3

.

. TFT-LCD(-

)

(Isopropyl alcohol, IPA). IPA

8

5000 , TFT-LCD

IPA .[4]

IPA TFT-LCD

, 50ppm IPA

. IPA

LG . IPA

, IPA

,

. IPA IPA

.

IPA 70%

, IPA

IPA . ,

IPA /

.

- 22 -

2

.

/ ,

.

, IPA

pervaporation .

10 , .

Pervaporation(PV)

, vapor permeation (VP) ,

. Pervaporation vapor permeation

, .

vapor permeation .[5,6]

. Zeolite A

, , ,

. 65 wt.%

. , OD 12mm, ID 9mm, L

800mm , 1mm 40%.

chromatographic separation. chromatographic

separation .

,

. nanofiltration

, .

.

raw material , ,

pore . 400-1,600 m2/g ,

.

- 23 -

3 .

consumed zone ,

, purification zone .

unconsummated carbon . consumed zone purification zone

unconsummated zone , bed ,

.

IPA, , IPA IPA

,

. IPA

IPA .[Vapor-Liquid Equilibria at 760mmHg Pressure (Louis H. Ballard and

M. Van Winkle-University of Texas, Austin, Texas), Vapor-Liquid Equilibria-2-Propanol

Water System (Abraham Wilson and Edward L. Simons-Rutgers University, New

Brunswick, N.J.)]. , IPA 87wt%

IPA , IPA

IPA .

IPA (Pervaporation Membrane)

300~500ppm IPA . , 100ppm

,

. ,

.[7,8] 1~10mmHg ,

, 0.68 kg/m2hr

(Flux) (50 kg/hr )

.

IPA IPA 3 IPA

3

IPA [9,10] , IPA

3 . ,

,

. IPA 3 ,

,

- 24 -

. , 3 IPA

, .

- 25 -

3

1

1.

. 4

. 100

, Si/Al .

ZSM-5, MFI Si/Al .

.

Si/Al /

, .

.

.

.

FAU Y , 3

.

.

USY(Ultra-Stable-Y) . Si/Al

.

FT-IR . 3-1

(ADS-KRICT-1) / .

(toluene)

3000~3400 cm-1 .

. .

- 26 -

3-2 . 170 . 170

,

. 400 .

3-1. .

- 27 -

90

92

94

96

98

100

102

0 100 200 300 400 500 600 700

-0.05

0.00

0.05

0.10

0.15

0.20

Temperature (oC)

Weight (%

)

Deriv. W

eight (%

/oC)

163.63 oC

471.84 oC

593.43 oC

[ N2 Flow ]

(a)

(b)

90

92

94

96

98

100

102

0 100 200 300 400 500 600 700

-0.05

0.00

0.05

0.10

0.15

0.20

Temperature (oC)W

eight (%

)

Deriv. W

eight (%

/oC)

172.35 oC

412.07 oC

593.96 oC

[ Air Flow ]

(a)

(b)

90

92

94

96

98

100

102

0 100 200 300 400 500 600 700

-0.05

0.00

0.05

0.10

0.15

0.20

Temperature (oC)

Weight (%

)

Deriv. W

eight (%

/oC)

163.63 oC

471.84 oC

593.43 oC

[ N2 Flow ]

(a)

(b)

90

92

94

96

98

100

102

0 100 200 300 400 500 600 700

-0.05

0.00

0.05

0.10

0.15

0.20

Temperature (oC)W

eight (%

)

Deriv. W

eight (%

/oC)

172.35 oC

412.07 oC

593.96 oC

[ Air Flow ]

(a)

(b)

3-2. .

2.

, ,

. Si/Al

,

. Si/Al LTA FAU

, Si/Al

.

.

.

.

.

(T) (T) TO4 .

.

T ,

(zeolite-like material) . AlPO4

- 28 -

, - , , ,

.[11]

(AlO2-) (SiO2)

. +3

1 . .

M2/nO.Al2O3.xSiO2.yH2O

M , n . x , y

.

TO4

.

, .

. -

, . ,

.

. 3-3 FAU, BEA, MOR, MFI .

. ,

. MOR

FAU (supercage)

.

.

.

.

. LTA 8

4 . 10 MFI 6~7 . .

(molecular sieve) .

,

- 29 -

30 .

, , , .

(template, structure directing agent) -

150

, , .

(small-pore),

(medium-pore), (large-pore) .

8 , 10

, 12 .

,

.

Si/Al , 1, 2, 3

.

.

.

,

.

BEA FAU MOR MFI

3-3. .

- 30 -

3.

.

.

.

, ,

Si/Al . , ,

, .

,

. 8, 10 12

.

. MOR BEA

Si/Al . MOR

BEA .

. MOR

BEA

. ,

.

. LTA

K+ 3A . 3 , , . Na+ 4 4A . K+ Na+

, , , . Ca2+

5 5A . Na+ Ca2+ n- , ,

.

. X Ca2+

.

.

- 31 -

Na+

- 32 -

4.

5 .

. .

. .

, , , , corona, acr

.

1 1-15%

90% .

.

4~8 2~4 arm

, .

.

(0.6~40 /). 60 ,

1.5kg /kg , 0~5 mmAq

.

()

, , pH,

.

.

. 2

. ,

() .

- 33 -

, ,

.

(Na, SO4 ) .

,

, , scale up

.

,

.

- 34 -

2

1.

, , .

BEA, FAU, MOR, MFI 4 . 12

BEA [100] 7.6 x 6.4 . [001] 5.5 x 5.5 3 . FAU 12 [111] 7.4

x 7.4 . (supercage) 3 . 1. [100]

12 , [010]

. MFI 10

.

,

.

, , .[15] 3

. , IPA

. Si/Al

. , .

, ,

.

2. IPA

4 ADS-1, ADS-2, ADs-3,

ADS-4 1 , .

700g . 15%

IPA(85% IPA) , 85% IPA

. 1oC EG .

- 35 -

.

3-1. /

170oC

N2 150mL/min

5hrs

IPA 15%

IPA 2mL/min

EG 1oC

1 .

ADS-4

50% .

2 pilot

, .

- 36 -

0 50 100 150 200 250 300 3500

10

20

30

40

50

60

70

Water content in IPA(ppm)

Adsorbed amount of water(g)

Recieved amount of IPA(ml)

0

5000

10000

15000

20000

25000

30000

3-4. ADS-1 IPA

0 50 100 150 200 250 300 3500

10

20

30

40

50

60

70




0

5000

10000

15000

20000

25000

3-5. ADS-2 IPA

- 37 -

0 50 100 150 200 250 300 3500

5

10

15

20

25

30




0

20000

40000

60000

80000

100000

120000

3-6. ADS-3 IPA

0 50 100 150 200 250 3000

5

10

15

20

25

30




0

5000

10000

15000

20000

3-7. ADS-4 IPA

- 38 -

0.3 m/sec .

1.2 sec

4~8 Mesh

35 cm /

150 mmAq

350~950 g/L

3 IPA

1. /

,

.

.

. (fiber)

(cloth)

. .

. ,

. 3-2 .

3-2.

(regeneration)

.

,

.

(reactivation)

- 39 -

(cycle)

.

. kg ,

, . 3-8 -

.

,

.

.

.

3-9 1 2

3 (reactivation) .

- 40 -

steam

adsorvers

adsorvers

blower

condenser

condensate cooler

cooling water

separator

solvent

waste water air filter cooling

water

air cooler

3-8. -

- 41 -

(1)

10 (2)

30 (3)

(1) (2) (3)

C/C

o

0.2

0

0.4

0.6

0.8

1.0

Time

3-9.

2. IPA

IPA .

3-10 ADS-1 IPA .

170oC 150ml/min . 85% IPA 10

ml/min, 1oC . 4 5

.

. .

- 42 -

3-10. IPA

- 43 -

4 IPA

1. IPA

LCD IPA , GC, GC-MS, ICP, Karl

Fisher . LCD IPA photo resist

stripper IPA photo resist stripper

. , IPA .

.

IPA IPA

. photo resist

bolier , . acetone, IPA

, , stripper

.

.

IPA TCD detector GC Karl Fischer

. GC 3-3 , 3-4

. IPA 50% IPA

. IPA

IPA . IPA

87.3% , IPA

IPA .

IPA IPA

Karl Fischer , 3-5 . 3-5

IPA GC ,

. , GC IPA

100% Karl Fischer 96ppm

. TCD GC

Karl Fischer IPA

- 44 -

. , IPA

Karl Fischer .

Detector Column Operating condition

TCD Hysep-Q (6 ft)

Injection temp. = 150Column temp. = 140Det temp. = 160He flow rate = 30 ml/min

* : GOW-MAC 580 (TCD)

3-3. GC (TCD detector)

H2O (wt%) IPA (wt%)

LCD IPA 49.0 51.0

12.7 87.3

- 100.0

3-4. GC (TCD detector)

IPA 13.1 %

IPA 96 ppm

* : Mitsubisi Karl Fisher Moisture Meter CA-100

3-5. Karl Fischer

- 45 -

.

i) GC-MS

IPA .

, GC-MS , 3-6

. , IPA acetone stripper N-methyl

pyrollidone 2-(2-butoxyethoxy) ethanol ( 3-7

). , IPA IPA acetone

N-methyl pyrollidone 2-(2-butoxyethoxy) ethanol

IPA

.

Detector Column Operating condition

Mass

SpectrometerDB-Wax (30m x 0.25)

Oven temp. programming

- Initial = 80oC for 2 min

- Rate = 10oC/min

- Final = 210oC for 15 min

Injection temp. = 180Det temp. = 200

* : HP 5890 series II gas chromatogaph (GC-MS)

3-6. GC-MS

Retention time 1.768 1.981 10.652 11.932

Acetone 2-PropanolN-methyl

Pyrrolidone

2-(2-butoxyethoxy)

-ethanol

3-7. GC-MS

ii) GC

GC-MS IPA HP-Wax

- 46 -

column FID detector GC 3-8 .

, IPA 0.0875% acetone stripper N-methyl pyrollidone

2-(2-butoxyethoxy) ethanol 5.754%, 12.752% ( 3-9

). , IPA , acetone, N-methyl pyrollidone 2-(2-butoxyethoxy)

ethanol

.

N-methyl pyrollidone 2-(2-butoxyethoxy) ethanol stripper

, IPA actone .

, IPA acetone

,

.

IPA .

IPA .

Detector Column Temp()

FID HP-Wax (30m x 0.25)

Oven temp. programming

- Initial = 80oC for 5 min

- Rate = 35oC/min

- Final = 150oC for 15 min

Injection temp. = 180Det temp. = 200

3-8. GC (FID detector)

- 47 -

Acetone

(wt%)

2-Propanol

(wt%)

2-Pyrrolidinone

(wt%)

2-(2-butoxyethox

y)-ethanol (wt%)

LG LCD

IPA0.078 81.415 5.754 12.752

IPA 0.134 99.866 - -

IPA- 100 - -

* : Younglin gas chromatogaph M600D (FID)

3-9. GC (FID detector)

.

IPA 22

ICP , 3-10 . 3-10

0.1 ppm , As, Ga, Ge, Sn,

Pb 1 ppm . , ppb

IPA

.

GC, GC-MS, Karl Fischer, ICP , IPA

, , , ,

IPA

.

- 48 -

(ppm) (ppm)

Ag 0.1 Ga 1

Al 0.1 Ge 1

As 1 Mg 0.1

Au 0.1 Li 0.1

Ba 0.1 Mn 0.1

Ca 0.1 Ni 0.1

Cd 0.1 Pb 1

Co 0.1 Si 0.1

Cr 0.1 Sn 1

Cu 0.1 Sr 0.1

Fe 0.1 Zn 0.1

* : Jobin-Yvon Ultima C ICP-AES

3-10. IPA ICP

- 49 -

Min 1,000 CmSpecific Resistance

Max 8ppbPhosphate(PO4)

Max 4ppbSulfate (SO4)

Max 4ppbNitrate (NO3)

Max 5ppbChloride (Cl)

Max 10ppmN Propanol

Max 5ppmAcetone

Max 5ppmAcidity (as CH3COOH)

To Pass Test~Solubility in Water

Max 50ppmWater (H2O)

Max 1ppmRsidue After Evaporation

0.786~0.787(20/20)Specific Gravity

Max 5APHAColor

Min 99.99Assay (CH3)2CHOH

SpecificationUnitTest Item

Min 1,000 CmSpecific Resistance

Max 8ppbPhosphate(PO4)

Max 4ppbSulfate (SO4)

Max 4ppbNitrate (NO3)

Max 5ppbChloride (Cl)

Max 10ppmN Propanol

Max 5ppmAcetone

Max 5ppmAcidity (as CH3COOH)

To Pass Test~Solubility in Water

Max 50ppmWater (H2O)

Max 1ppmRsidue After Evaporation

0.786~0.787(20/20)Specific Gravity

Max 5APHAColor

Min 99.99Assay (CH3)2CHOH

SpecificationUnitTest Item

2.

IPA 87% .

3

.

LCD IPA specification 3-11 .

3-11. LCD IPA specification

L IPA(IPA 51%, 49%) distillation 87%

IPA GC

. TCD detector(hysep-Q column, 6ft) GC 1% IPA

, coulometric (Karl-Fischer

moisture titrator, MKC-500) . molecular sieve 3A,

700mL . IPA 1~3mL/min

bottom-up flow . IPA ,

IPA . IPA

, -10oC ~

- 50 -

. , 170

. 3-11 0oC

5% IPA 3mL/min IPA

. 300mL 100ppm 500mL

.

.

0 100 200 300 400 500 600 700

2

4

6

8

10

12

14

16

18

20

22

24

Recieved amount of IPA (mL)

Adsorb

ed amount of water (g

)

-1000

0

1000

2000

3000

4000

5000

6000

7000

8000

94 ppm

Tower temp 0oC, IPA (water 5%) flow rate 3mL/min

Water c

ontent in

IPA (p

pm)

3-11. IPA ()

IPA 1%

IPA (3-12 ). 1.5L IPA

100ppm , 1.7L IPA

- 51 -

. IPA

.

0 500 1000 1500 2000 2500 3000

0

20

40

60

80

100

120

Adsorbed amount of water (g)

Recieved amount of IPA (mL)

Tower temp 0oC, IPA (water 1%) flow rate 3mL/min

0

500

1000

1500

2000

2500

3000

3500

4000

Water c

ontent in

IPA (p

pm)

3-12 IPA ()

0oC , 3-13 -5oC

. IPA 1%

3mL/min. 2.6L IPA 100ppm

3.0L . 3-12 3-13

IPA

. bench IPA

/ IPA .

.

- 52 -

0 1000 2000 3000 4000 5000 6000

0

10

20

30

40

Received amount of IPA (mL)

Adsorb

ed amount of water (g

)

0

1000

2000

3000

4000

5000

6000

7000

8000

9000

10000

Tower temp -5oC, IPA (water 1%) flow rate 3mL/min

Water c

ontent in

IPA (p

pm)

3-13. IPA ()

- 53 -

IPA 15% . 15% IPA(5.3mL/min)

-5oC IPA .

3-14 15 150mL/min 300mL/min .

IPA 10,000 ppm(1%) 275 mL 375 mL

. IPA , , ,

.

3-16 1% IPA .

, -5oC, 5 hrs,

300mL/min . 1 IPA ( 300ppm,)

IPA (5.4mL/min) 5 .

.

- 54 -

0 50 100 150 200 250 300 350 400 4500

20

40

60

80




0

10000

20000

30000

40000

50000

60000

70000

3-14. 150mL/min IPA

0 50 100 150 200 250 300 350 400 450 5000

20

40

60

80

100Water content in IPA(ppm)



0

5000

10000

15000

20000

25000

30000

35000

40000

45000

50000

3-15. 300mL/min IPA

- 55 -

0 1000 2000 3000 4000 5000 6000 7000 8000 90000

10

20

30

40

50

60

70

80

90

100

100 ppm




0

500

1000

1500

2000

2500

3000

3500

4000

4500

5000

3-16. 1% IPA IPA

- 56 -

5 IPA set-up

1.

IPA IPA

, - 3 kg/day IPA

3-17 . ,

, -

switching 4-way valve timer

. ,

jacket chiller .

heating jacket , programming

.

IPA RI detector , computer

logging . , -

, 3-18

3-12 .

3-19 1 / IPA

. IPA , ,

. IPA( 1%)

, / 1

. 20 4320 mL IPA (3.6mL/min)

, IPA 60 ppm .

- 57 -

IPA In

ADSORBENTADSORBENT

CONTINEOUS ADSORPTION COLUMN

Dry N2

Relief

Valve

Relief

Valve

CHILLER

VENT

PRODUCT

3-17. IPA

- 58 -

3-18. IPA

- 59 -

3 Liter/day Product

-

800 ml x 2 2

-15 ~

0 - 300oC

0.5 ~ 10

Swiping gas 0 - 3 L/min

Control Automatic

RI detector

3-12. IPA

- 60 -

0 200 400 600 800 1000 12000

20

40

60

80

100

120

140

160

180

200Water Content in IPA

Operation Time(min)

3-19. IPA

- 61 -

Adsorbent 3A (, 1.5 x 3 mm)

Experimental

condition

Water cont. (ppm) 54351

Temperature (oC) -5

Flow rate (ml/min) 2~4

Regeneration

condition

Temperature (oC) 170

Time (hr) 10

N2 flow rate (ml/min) 350

2.

IPA

.

IPA , .

3A (, 1.5 x 3 mm) .

3-13 . 170, 10 350cc/min

, 5.4% IPA -5oC 2~4cc/min

. 3-20 .

3-13. IPA .

- 62 -

0 100 200 300 400 500 600 700 800 900

0

2000

4000

6000

8000

10000

12000

14000

Weight(g)

Water Content in IPA(ppm)

Tower temp -5oC, IPA (water 5%) flow rate 2~4cc/min

2cc/min

3cc/min

4cc/min

3-20. IPA .

- 63 -

(85 ~ 87wt%)

(Option)

(Option)

WWT

3.

LCD IPA /

.

. 3-21 .

3-21. IPA

A. IPA

1.

2. 85~87wt%

3.

4.

5.

6.

7. Option Unit

B. IPA

- 64 -

1. (85~87 wt%)

2. (TAT System)

3. TAT System N2

4. Option , 99.99%

C. /

1.

2. 0.1 ~ 0.3ppb

3. 0.3 50 ea/ml

4. Filtering System

D. /

,

option unit

IPA spec() .

1. Assay: min. 99.99 wt%

2. Color: APHA: max. 5

3. S.G: 0.786 ~ 0.787

4. Residue After Evaporation: max.1 ppm

5. Water: max. 50 ppm

6. Acetone: max. 5 ppm

7. N-Propanol: max. 10 ppm

3-22 25kg/day IPA P&ID .

- 65 -

SEOUL, KOREASUNJINSEOUL, KOREA

DEAJEON, KOREA

3-22. 2 IPA (25kG/day) PFD

- 66 -

6 IPA

1. Bench IPA

LCD IPA IPA

, 24 kg/day IPA 3-23 .

, (50kg) (vol. 70L)

, -

switching 4-way valve

timer . ,

jacket chiller

. staem heating

jacket , programming

. IPA Carl

Fischer titrator , 6-2 .

- 67 -

3-23. Bench IPA .

- 68 -

25kg/day

-

70L(50kg) x 2 2

-5oC ~

0 - 190oC

~ 48

Swiping gas ~ 2 L/min

Control Automatic

Carl Fischer titrator

3-14. Bench IPA

- 69 -

2. Bench IPA (1)

( 3-24)

: 95% IPA, 5% H2O (simulated)

Feeding rate: 0.91kg/hr

: 61

200ppm IPA 15.3kg (production rate 0.25kg/hr)

3. Bench IPA (2)

( 3-24)

: 94% IPA, 6% H2O (simulated)


: 67


- 70 -

-2 0 2 4 6 8 10 12 14 16

100

200

300

400

500

600

Concentration(ppm)

W eight(kg)

1 (le ft) 2 (righ t)

3-24. Bench IPA .

- 71 -

3. Bench IPA (3)

( 3-25)

: 92% IPA, 8% H2O (() )

Feeding rate: 1.7 kg/hr

: 60


4. Bench IPA (4)

( 3-25)

: 91% IPA, 9% H2O (() )

Feeding rate: 1.0 kg/hr

: 100


- 72 -

0 10 20 30 40 50

0

500

1000

1500

2000

2500

Concentration(ppm)

Weight(kg)

3 (le ft) 4 (righ t)

3-25. Bench IPA .

- 73 -

7

. 1 LCD

IPA . IPA

, IPA ,

. IPA

.

.[16] ,

2009 . ,

, .

99.5% .

IPA ,

.

E100( 100%), E10( 90% + 10%)

. .

.

.

35,000

.

.

,

. 2008

.

. 90 E10(

90% + 10%) . 70 ,

. EU 5%(E5)

.

- 74 -

93~95% 7~5% .

infra , 99.5%

,

.

1. Bench (1)

( 3-26)

: 92.6% , 7.4% H2O ( )


: 7

10,000ppm 43.7kg (production rate 6.2kg/hr)

2. Bench (2)

( 3-26)

: 92.6% , 7.4% H2O ( )


: 5


- 75 -

0 10 20 30 40 50

0

5000

10000

15000

20000

Concentration(ppm)

Weight(kg)

1 Left 2 R ight

3-26. Bench .

- 76 -

3. Bench (3)

: 92.5% , 7.5% H2O ( )


: 5


4. Bench (4)

: 92.5% , 7.5% H2O ( )


: 5


- 77 -

4

1.

(1)

LCD IPA -

-. LCD IPA( 30% )

-. IPA ( 50ppm ) (

50%)

-. 25KG/day IPA bench

(2)

LCD IPA

100% IPA > 99.99%

100%

90% 25kg/day IPA

(3)

99.99% IPA LCD IPA

, / / .

- 78 -

. bench

IPA / , IPA (99.99%)

. IPA LCD

, 25kg/day

, ??kg/day . LCD

IPA 30% ,

1 IPA . LCD 99.99%

IPA , , , 99.9% IPA

IPA .

data , IPA

.

2 IPA

, . ,

, ,

. ,

IPA stripper ,

package , LCD

IPA data .

- 79 -

2.

(1) LCD IPA

--> LCD IPA .

IPA stripper , 40%

. IPA

84% , 99.99% IPA

. / IPA IPA

. .

IPA 3

IPA .

(2)

--> 2 / IPA

-5oC , 150oC

. /

, IPA .

.

IPA full package .

(3)

--> 1 lab IPA (2kg/day, )

. , IPA ,

, IPA data .

2 25kg/day /

- 80 -

. 70L , 50kg 5A ( 2~3mm)

. IPA

. 1 LCD IPA (92%) 99.95% IPA

, 21kg/day . IPA

.

- 81 -

5

1. LCD IPA

IPA

25kg/day , .

pilot (, /, ...)

. LCD IPA LCD

, IPA

. 99.9% B

.

/ .

2.

, 5-1 .

IPA

.

5-1, ( TFT-LCD ).[17]

2006 2007

() 150 220

() 10 15

IPA , .

pilot

. , ,

, LCD

- 82 -

.

, ,

pilot ,

2, 3 ( 5-2 ),

SWOT . ( 5-3 )

5-2. .

(2007) (2009)

LCD IPA

LCD IPA

5 8

5 8

1 2

() 500 1000

()

8 16

2 4

10 20

- 83 -

5-3 SWOT .

()

-. TFT-LCD

IPA

-. IPA

-.

-.

-.

()

-.

.

()

-. grade

IPA (

)

-. chemical reprocess system

IPA

-. MEK

()

-. IPA

-. VOC

-. TFT-LCD

(IPA)

- 84 -

6

1. DuPont [18]

.

(biorefinery)

18.3 , 18.9

. 200

, ' (Integrated Corn-Based

Bioproducts Refinery)'

.

(Diversa) ,

.

3GT(Sorona 3GT) 1,3-(PDO) .

(Genencor) PDO

. DNA

500 .

PDO .

2. IPA - [19]

(isopropyl alcohol ;IPA) -

(silicone-urea copolymers)

Koc Iskender Yilgor . -

.

2 .

.

.

(N,N-Dimethylformamide, DMF)

. Yilgor

- 85 -

DMF IPA

.

Polymer 2003 -

(4-

)[bis(4-isocyanatocyclohexyl)methane ; HMDI] 23 C

(infrared spectroscopy, IR) .

IPA HMDI 23 C .

- (aminopropyl) N-

(N-methylaminopropyl) (polydimethylsiloxane ;

PDMS) (oligomers) HMDI . PDMS

(Number average molecular weights) 900~7000 g/mol

. IPA , -

urea 10~42% .

(Thermal properties)

(microphase-separated systems) .

3. [20]

Royal Dutch/Shell

Iogen Energy 2,900 . Shell

Mark Gainborough Shell ,

Shell ,

. Gainborough

, Shell Iogen

.

Shell Global Solutions .

.

. Shell

90% .

- 86 -

,

. , Shell Iogen

.

4. [21]

2- (2-methoxyphenol: = 478.15 K) 1,2- 1,2-dimethoxy

benzene: = 479.15 K) (methoxyphenol)

.

. Lee 323.15-423.15 K

20 MPa

- (VLE) .

. Hwang

2- (2-methoxyphenol)+ 1,2- (1,2-dimethoxybenzene)

, (diphenylmethane)

(entrainer) .

,

. Hwang 433.15K 463.15K 2-

(2-methoxyphenol), 1,2- (1,2-dimethoxybenzene), (diphenylmethane)

VLE ,

. (entrainer)

(diphenylmethane) .

2- (2-methoxyphenol), 1,2- (1,2-dimethoxy

benzene), (diphenylmethane) - (SLE) .

SLE

. , SLE 3 ,

.

Wilson NRTL 2 SLE .

2 -

- 87 -

, , 2 .

.

, (diphenylmethane)

2- (2-methoxyphenol), 1,2- (1,2-dimethoxybenzene) 2

3 - .

, 2 , ,

(diphenylmethane) + 2- (2-methoxyphenol) + 1,2-

(1,2-dimethoxybenzene) , 3

- .

2- (2-methoxyphenol) 1,2-

(1,2-dimethoxybenzene)

(diphenylmethane) . , 2

,

Wilson NRTL 0.42% 3

- .

- 88 -

7

1. , 1990.

2. P.A. Schweitzer, "Handbook of separation techniques for chemical engineer", 2nd

Ed., McGraw-Hill, 1988.

3. The 2nd Asian Textile Conference Technological Innovations in Asian Textile

Industry, 1, p134.

4. www.mykrolis.com/publication.nsf.

5. , 13, 3, 328.

6. The 2nd Asian Textile Conference Technological Innovations in Asian Textile

Industry, 1, p129.

7. US Pat. 5,868,906, Consider Membrane Pervaporation.

8. Hurbert L. Flewing, Zenon Environmental, Inc. Chemical Engineering Progress

Jul. 1992.

9. U.S. Pat. No. 5,053,563.

10. U.S. Pat. No. 4,762,616.

11. Meier, W. M., Proc. 7th Intern,. Zeolite Conf., 13 (1986).

12. , , , 23 51 (1985)

13. Minachev, Kh.M. and Isakov, Ya. I., ACS Monograph, 171, 552 (1974)

14. Kaeding, W., J. Phys. Chem., 80, 262 (1976).

15. , 88-10-0407-00-00

16. Bio Industry, 2002, 19(8), 58.

17. WWW.CISCHEM.COM ( IPA ).

18. http://pubs.acs.org/cen/topstory/8042/8042notw2.html .

19. http://www.chemweb.com/alchem/articles/1066208136238.html.

20. http://www.gnet.org.

21. Ind. Eng. Chem. Res., 42, 3434 (2003).

1 1 2 3

2 3 1 1. 2. 3. 4.

2 1. 2. IPA

3 IPA 1. / 2. IPA

4 IPA 1. IPA 2.

5 IPA set- up 1. 2. 3.

6 IPA 1. Bench IPA 2. Bench IPA ( 1) 3. Bench IPA ( 2) 3. Bench IPA ( 3) 4. Bench IPA ( 4)

7 1. Bench ( 1) 2. Bench ( 2) 3. Bench ( 3) 4. Bench ( 4)

4 1. 2.

5 1. LCD IPA 2.

6 1. DuPont [ 18] 2. IPA - [ 19] 3. [ 20] 4. [ 21]

7

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