물 - 에탄올공비증류공정의최적화 공주대학교화학공학부조정호

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1 물 - 에탄올공비증류공정의최적화 공주대학교화학공학부조정호 1

2 목차 :(1) 공비혼합물을형성하는이성분계의분리공비혼합물의분류올바른열역학모델식의선정원료조건, 제품사양및유틸리티삼성분계액액상평형도상에서의공비증류공정의설계농축기 (Concentrator) 의전산모사기법경사분리기 (Decanter) 의전산모사기법공비증류탑 (Azeotropic Column) 의전산모사기법 2

3 9 10 목차 :(2) Stripper의전산모사기법전제공정에대한공정최적화 3

4 1 공비혼합물을형성하는이성분계의분리 4

5 1. 공비혼합물을형성하는이성분계의분리 1.1 공비혼합물을형성하는이성분계의종류및분리방법개요 : 1.2 공비점분리제를사용하는공비증류공정 1.3 용매를사용하는추출증류공정 1.4 압력변환증류공정 1.5 초임계이산화탄소를이용한초임계추출공정 1.6 진공증류공정 1.7 투과증발공정 5

6 1.1 공비혼합물을형성하는이성분계의종류및분리방법개요 Some azeotropic distillation cases: No. Components to be separated Entrainers 1 Ethanol/water; isopropanol/water; tert-butanol/water Benzene, toluene, hexane, cyclohexane, methanol, normal pentane 2 Acetone/n-heptane Toluene 3 Acetic acid/water N-butyl acetate 4 Isopropanol/toluene Acetone 위의책 ( 책은내가 pdf 파일로전달해줄것임.) 의참고문헌을찾아서박회경박사가모두논문을작성할수있도록준비할것 6

7 1.1 공비혼합물을형성하는이성분계의종류및분리방법개요 Shift the Azeotropic Point by Changing Pressure Pressure Swing Distillation Supercritical Fluid Extraction Using Supercritical CO 2 Solvent Pervaporation Method: Proposed by SKEC Vacuum Distillation Azeotrope between ethanol and water disappears at 11.5kPa. Add the Third Component. Azeotropic Distillation: Entrainer (Benzene, CHX, NC5) Extractive Distillation: Solvent (Ethylene Glycol, DMSO) 7

8 1.2 공비점분리제를사용하는공비증류공정 Vapor Mole Fraction of Ethanol Ethanol / Water System Limit of Azeotropic Distillation Distillation range is restricted by the azeotropic point. Binary azeotropic mixtures, such as ethanol/water and IPA/water, can be separated into their pure components by distillation by the addition of a third component, so called the entrainer, which forms a ternary azeotrope with a lower boiling point than any binary azeotrope Liquid Mole Fraction of Ethanol 8

9 1.2 공비점분리제를사용하는공비증류공정 : 원리 (1) Azeotropic distillation By forming a ternary heterogeneous azeotrope lower than any other binary azeotropic temperatures, nearly pure ethanol can be obtained as a bottom product in an azeotropic distillation column. Ethanol is obtained as a bottom product from an azeotropic distillation column using an entrainer such as benzene or normal pentane. Extractive distillation By adding a solvent which is exclusively familiar with a wanted component in a feed mixture, a desired component can be obtained in an extractive distillation column overhead. Ethanol is obtained as a top product from an extractive distillation with ethylene glycol solvent. 9

10 1.2 공비점분리제를사용하는공비증류공정 : 비교 공비증류공정과추출증류공정의원리비교 RECYCLE UPPER PHASE LOWER PHASE SOLVENT PURE ETHANOL FEED FEED PURE ETHANOL Azeotropic Distillation Extractive Distillation 10

11 1.2 공비점분리제를사용하는공비증류공정 : 원리 (2) Ethanol P II A F A : o C B : o C C : o C D : o C B.4.3 G V R D W Only mixtures in region II will give the desired products of pure ethanol as a bottom product..2.1 I Benzene C III Water Aqueous ethanol can be separated into their pure components by distillation by the addition of a third component, so called the entrainer, which forms a ternary heterogeneous azeotrope with a lower than any other binary azeotropes. 11

12 1.3 용매를사용하는추출증류공정 : 원리 추출증류공정에적용가능한시스템들 : No. Component 1 Component 2 Solvents 1 Alcohol (ethanol or isopropanol) Water Ethylene glycol, DMSO 2 Acetic acid Water Tributyl amine 3 Acetone Water Water, ethylene glycol 4 Methanol Methanol Water 5 Propylene Propane ACN(Acetonitrile) 6 C4 hydrocarbons C4 hydrocarbons ACN, Acetone, DMF, NMP 7 Tetrahydrofuran Water Ethylene glycol, DMSO 8 C5 hydrocarbons C5 hydrocarbons DMF 9 Aromatics Non-aromatics DMF, NMP, NFM 10 Methanol DMC 2-Ethoxyethanol 4-Methyl-2-pentanone 위의책 ( 책은 pdf 파일로내가전달할것임 ) 의참고문헌들을박회경박사가모두찾아서논문으로작성할수있도록준비할것 12

13 1.3 용매를사용하는추출증류공정 : 원리 IPA Dehydration Using Solvent: Two-columns configuration T02 T03 13

14 1.3 용매를사용하는추출증류공정 : 원리 IPA Dehydration Using Solvent: Three-columns configuration E E T01 4 P02 D T02 D02 P E E05 19 T03 18 P06 D P01 E02 7 P E08 E P05 IPA의농도를공비점직전 P07 어느정도까지농축하느냐가중요함 21 E06 14

15 1.4 압력변환증류공정 : 원리 압력변화에따라서공비조성이민감하게변화하는계에적용할수있다. Vapor Mole Fraction of THF THF / Water System Point B Point C Point A Point D Low pressure High pressure Distillation range is restricted by the azeotropic point. Pressure-sensitive binary azeotropic mixture, such as THF and water system can be separated into their pure components by pressure swing distillation. 낮은압력에서 Point A까지농축함. 높은압력으로변경시키면, Point D까지얻을수있음 Liquid Mole Fraction of THF 15

16 1.4 압력변환증류공정 : 공정의구성 T01 H 2 O Removal Column Pressure Up For Shifting Azeotrope T02 THF Recovery Column 한화건설 실제프로젝트원용덕상무님과제 Low Pressure Column High Pressure Column 16

17 1.4 압력변환증류공정 : 예 압력변환증류공정에적용가능한예 No. Component 1 Component 2 BIP's in P2 BIP's in A+ 1 Carbon dioxide Ethylene X 2 Hydrochloric acid Water X 3 Water Acetonitrile 4 Water Ethanol 5 Water Acrylic acid 6 Water Acetone 7 Water Propylene oxide 8 Water Methyl acetate 9 Water Propionic acid X 10 Water 2-methoxyethanol 11 Water 2-butanone (MEK) 12 Water Tetrahydrofuran (THF) 13 Carbon tetrachloride Ethanol 14 Carbon tetrachloride Ethyl acetate 15 Carbon tetrachloride Ethyl acetate 16 Carbon tetrachloride Benzene 17 Methanol Acetone 18 Methanol 2-butanone (MEK) 19 Methanol Methyl propyl ketone 17

18 1.4 압력변환증류공정 : 예 압력변환증류공정에적용가능한예 No. Component 1 Component 2 BIP's in P2 BIP's in A+ 20 Methanol Methyl acetate 21 Methanol Ethyl acetate 22 Methanol Benzene 23 Methanol Dichloromethane 24 Methylamine Trimethylamine 25 Ethanol Dioxane 26 Ethanol Benzene 27 Ethanol Heptane 28 Dimethylamine Trimethylamine X 29 2-propanol Benzene 30 Propanol Benzene 31 Propanol Cyclohexane X 32 2-butanone (MEK) Benzene 33 2-butanone (MEK) Cyclohexane 34 Isobutyl alcohol Benzene 35 Benzene Cyclohexane 36 Benzene Hexane 37 Phenol Butyl acetate 38 Aniline Octane X X 18

19 1.5 초임계이산화탄소를이용한초임계추출공정 Supercritical CO 2 Ethanol-water mixture SCF: Ethanol-CO 2 Liquid water Ethanol product Water 19

20 1.6 진공증류공정 : Azeotrope between ethanol and water disappears below the pressure, 0.1 bar. STREAM ID S1 S2 S3 NAME PHASE LIQUID LIQUID LIQUID THERMO ID IDEA01 IDEA01 IDEA01 FLUID MOLAR PERCENTS 1 ETHANOL WATER TOTAL RATE, KG-MOL/HR TEMPERATURE, C PRESSURE, BAR ENTHALPY, M*KCAL/HR MOLECULAR WEIGHT MOLE FRAC VAPOR MOLE FRAC LIQUID

21 2 공비혼합물의분류 21

22 2. 공비혼합물의분류 2.1 공비혼합물의정의 2.2 Homogeneous azeotrope 와 heterogeneous azeotrope 2.3 이성분계공비와삼성분계공비혼합물 2.4 실험적인공비온도및조성과계산결과사이의비교 22

23 2.1 공비혼합물의정의 Azeotrope: Boiling at the same temperature and composition both at the vapor and the liquid phases 공비 ( 共沸 ) 일정한온도에서용액의성분비와증기의성분비가같아지는현상을나타내는것을말하며, 이러한상태의조성을공비조성이라고한다. 23

24 2.2 균일공비와불균일공비및이성분계공비와삼성분계공비 Homogeneous azeotrope: 액상이서로다른액상으로상분리가일어나지않는다. 예 : IPA-Water, Benzene-IPA Heterogeneous azeotropes: 액상의서로다른두개의액상으로상분리가일어난다. 종류 : Binary and ternary heterogeneous azeotropes 예 : Water-Benzene, IPA-Water-Benzene 24

25 2.3 실험적인공비온도및조성과계산결과사이의비교 :(1) Binary homogeneous azeotrope: exp vs. P2 Component BP( o C) Azeotropic Temperature ( o C) IPA Water Benzene Ethanol Azeo. Weight % Binary heterogeneous azeotrope: exp vs. P2 Component BP( o C) Azeotropic Temperature ( o C) Azeo. Weight % Upper Layer Lower Layer IPA Water () Ternary heterogeneous azeotrope: exp vs. P2 Component BP( o C) Azeotropic Temperature ( o C) Azeo. Weight % Upper Layer Lower Layer Benzene IPA Water ()

26 2.3 실험적인공비온도및조성과계산결과사이의비교 :(2) Binary homogeneous azeotrope: exp vs. Aspen Plus Component BP( o C) Azeotropic Temperature ( o C) IPA Water Benzene IPA Azeo. Weight % Binary heterogeneous azeotrope: exp vs. Aspen Plus Component BP( o C) Azeotropic Temperature ( o C) Azeo. Weight % Upper Layer Lower Layer Benzene Water () Ternary heterogeneous azeotrope: exp vs. Aspen Plus Component BP( o C) Azeotropic Temperature ( o C) Azeo. Weight % Upper Layer Lower Layer Benzene IPA Water ()

27 3 올바른열역학모델식의선정 27

28 3. 올바른열역학모델식의선정 3.1 기액상평형과액액상평형원리 3.2 활동도계수와퓨개시티계수의정의 3.3 One constant Margules 모델식 3.4 van Laar 모델식 3.5 Wilson 모델식과 Local composition concept 3.6 NRTL 모델식 3.7 UNIQUAC 모델식 3.8 UNIFAC 모델식 28

29 3.1 기액상평형과액액상평형원리 Four criteria for equilibria: v i Situation T T P P l i l1 l 2 i i Thermal Equilibrium Mechanical Equilibrium Condition, Phase Equilibria (VLE, LLE) G T, P 0 Chemical Equilibrium Fugacity (or chemical potential) is defined as an escaping tendency of a component i in a certain phase into another phase. 29

30 3.1 기액상평형과액액상평형원리 Vapor-liquid equilibrium calculations The basic relationship for every component in vapor-liquid equilibrium is: v i T P y f l T P x i where : the fugacity of component i in the vapor phase v fˆi l fˆi f ˆ,, ˆ,, : the fugacity of component i in the liquid phase i i (1) 30

31 3.1 기액상평형과액액상평형원리 There are two methods for representing liquid fugacities. Equation of state method Liquid activity coefficient method 31

32 3.1 기액상평형과액액상평형원리 The equation of state method defines fugacities as: f ˆ v v ˆ y P (2) i i i f ˆ l l ˆ x P (3) i i i where: i v l i y i x i P is the vapor phase fugacity coefficient is the liquid phase fugacity coefficient is the mole fraction of i in the vapor is the mole fraction of i in the liquid is the system pressure 32

33 3.1 기액상평형과액액상평형원리 We can then rewrite equation 1 as: ˆ y v i i ˆ x l i i (4) This is the standard equation used to represent vaporliquid equilibrium using the equation-of-state method. iv and il are both calculated by the equation-of-state. Note that K-values are defined as: y i Ki (5) xi 33

34 3.1 기액상평형과액액상평형원리 : 활동도계수 (VLE) The activity coefficient method defines liquid fugacities as: fˆ The vapor fugacity is the same as the EOS approach: f ˆ l i v i x f (6) i ˆ v i i y i 0 i P (7) where: i is the liquid activity coefficient of component i 0 fi v ˆi is the standard liquid fugacity of component i is calculated from an equation-of-state model We can then rewrite equation 1 as: ˆv y i i P x i i f 0 i (8) 34

35 3.1 기액상평형과액액상평형원리 : 활동도계수 (LLE) For Liquid-Liquid Equilibrium (LLE) the relationship is: fˆ l1 fˆ l 2 i i (9) where the designators 1 and 2 represent the two separate liquid phases. Using the activity coefficient definition of fugacity, this can be rewritten and simplified as: x l1 l1 x l 2 l 2 i i i i (10) 35

36 3.2 One constant Margules 모델식 The simplest polynomial representation is: Gex Ax 1 x 2 Thus, So that 1 exp and ng ln1 n 1 ex T, P, n Ax 2 2 RT 2 Ann 1 2 n 1 n1 n 2 n2 A n1 n2 2 exp Ax 2 1 RT n 1 n n 1 2 n 2 2 Ax 2 2 The two species activity coefficients are mirror images of each other as a function of composition. 36

37 3.2 One constant Margules: Non-ideal Mixtures A mixture is non-ideal if i are not equal to 1. The value of i indicates the degree of nonideality: If i is less than 1, component interactions are attractive. If i is greater than 1, component interactions are repulsive. If much greater than 1, the formation of 2 liquid phases is possible. For most activity coefficient property methods, non-ideal interactions of components i and j will affect component k. 37

38 3.2 One constant Margules: For a Binary VLE Sub-cooled Liquid Pressure (kpa) Positive: i >1 Negative: i <1 Ideal: i = 1 40 Super-heated Vapor x 1, y 1 38

39 3.2 One constant Margules: For Much Larger Value of i 160 Unstable: Liquid Phase Splitting Pressure (kpa) A = 0.0 A = 0.5 A = 1.0 A = 2.0 A = x 1, y 1 39

40 3.2 One constant Margules: Types of Liquid Mixtures (1) Completely Miscible System Always forms single liquid phase iregardless of mixture composition and temperature Ideal Gas Law (for vapor phase). Double derivative of Gibbs free energy change due to mixing is always positive. (stable) Immiscible System Mutual solubility is nearly zero. Gibbs free energy change due to mixing is always positive. (unstable) Partially Miscible System Liquid mixture forms a stable single liquid phase for some concentration range but splits into the two liquid phases when some more A (or B) is added. 40

41 3.2 One constant Margules: Types of Liquid Mixtures (2) Completely Miscible System (Stable) 2 mix G / RT 0 x Immiscible System (Unstable) 2 2 Partially Miscible System (Conditionally Stable) 2 T, P mix G / RT 0 x 2 T, P mix G / RT 0 x 2 T, P 41

42 3.2 One constant Margules 모델식 Activity Coefficient of each components Liquid Composition, x This model can be applied for chemically not dissimilar systems. 42

43 3.2 One constant Margules 모델식 References 1. Margules, 1895, Sitzber., Akad. Wiss. Wien, Math. Naturw., (2A). 104,

44 3.3 van Laar 모델식 van Laar was one of the students of van der Waals. Mixing pure A and B gases Condensation of gaseous mixture into liquid solution Vaporization of liquid A and B into gases Direct Mixing Process Liquid Solution A + B Pure A Pure B 44

45 3.3 van Laar 모델식 Another old correlation which is still frequently used is the van Laar equation. The resulting expression for the activity coefficient is: where: ln i Z N a Z N a Z Z il l ij i j i1 j1 2 l j xl a x j a il li Two parameters, a ij and a ji, are required for each binary. 1 N j1 j, k1 a j, k a a ij ji Z j Z k 45

46 3.3 van Laar 모델식 46 The van Laar equations for the activity coefficients: and With relation to the van der Waals parameter a and b and Since we know the van der Waals equation is not very accurate, it is not surprising that the correlative value of the van Laar equations is different from the regressed values ln x x ln x x b a b a RT b b a b a RT b

47 3.3 van Laar 모델식 Comparison of the van Laar constants between parameters obtained from regressed data and parameters calculated from van der Waals equation Obtained from regression Obtained from vdw EOS System acetaldehyde-water Acetone-methanol Acetone-water

48 3.3 van Laar 모델식 Table: Application guideline of van Laar equation Required Pure-component Properties Application Guidelines Vapor Pressure Components Use for chemically not dissimilar components References 1. van Laar, J. J., 1910, The vapor pressure of binary mixtures, Z. Phys. Chem., 72,

49 3.4 Wilson 모델식 Basis Derived from the Flory-Huggins model, by assuming that the local composition is not equal to the overall composition to account for non-randomness of mixture composition. The activity coefficient model to use local composition concept. Cannot predict two liquid phases regardless of binary parameter values - Will never predict two liquid phases. - Not recommended it process has two liquid phases such as decanters. 49

50 3.4 Wilson 모델식 The Wilson equation was the first to incorporate the concept of local Composition. The basic idea is that, because of differences in intermolecular forces, the composition in the neighborhood of a specific molecule in solution will differ from that of the bulk liquid. The two parameters per binary are, at least in principle, associated with the degree to which each molecule can produce a change in the composition of the local environment. 50

51 3.4 Wilson 모델식 The expression for the activity coefficient is: ln 1ln i N j1 x N k1 L v a where: i ij Aij exp L (when unit of a ij is K) vj T j A ij N x j1 k x A j ki A kj L v i = the liquid molar volume of component i 51

52 3.4 Wilson 모델식 The Wilson equation cannot describe local maxima or minima in the activity coefficient. Its single significant shortcoming, however, is that it is mathematically unable to predict the splitting of a liquid into two partially miscible phases. It is therefore completely unsuitable for problems involving liquid-liquid equilibria. References 1. Wilson, G. M., 1964, Vapor-Liquid Equilibrium XI. A New Expression for the Excess Free Energy of Mixing, J. Amer. Chem. Soc., 86,

53 3.4 Wilson 모델식 Fatal weakness of Wilson model: 53

54 3.4 Wilson 모델식 Fatal weakness of Wilson model: 54

55 3.4 Wilson 모델식 It does not return to ideal Raoult s law when the BIP s are not available in DB. 55

56 3.4 Wilson 모델식 How about Aspen Plus? 56

57 3.4 Wilson 모델식 Fatal weakness of Wilson model: 57

58 3.4 Wilson 모델식 Fatal weakness of Wilson model: 58

59 3.4 Wilson 모델식 : Stability Criteria for Liquid Mixtures If the second derivative of total Gibbs free energy change vs. composition is bigger than zero for any composition, the system satisfies the stability criteria so, liquid mixture forms a single stable liquid mixture. (a) Ideal (b) Slightly Non-ideal (c) Critical Miscibility (d) Liquid Phase Splitting Activity of Component (d) (c) (b) (a) Mole Fraction of Component 1 59

60 3.4 Wilson 모델식 Table: Application guideline of Wilson equation Required Pure-component Application Guidelines Properties Vapor Pressure Components Useful for polar or associating Liquid molar volume component in nonpolar solvents. Cannot be used if liquid-liquid immiscibility exists. 60

61 3.5 NRTL 모델식 The NRTL (non-random-two-liquid) equation was developed by Renon and Prausnitz to make use of the local composition concept, while avoiding the Wilson equation s inability to predict liquid-liquid phase separation. The resulting equation has been quite successful in correlating a wide variety of systems. References 1. Renon, H. and Prausnitz, J. M., 1968, Local Composition in Thermodynamic Excess Functions for Liquid Mixtures, AIChE J., 14,

62 3.5 NRTL 모델식 NRTL. This model has up to 8 adjustable binary parameters that can be fitted to data. ln i j G k ji G ki ij ji x x k j a ij j b ij T k x j G G c T kj ij ij 2 x k ij l k x G l G lj kj x k lj G ij exp T ij ij ij 62

63 3.5 NRTL 모델식 Three parameters, ij, ji, and ij = ji, are e NRTL (nonrandom-two-liquid) equation was developed by Renon and Prausnitz to make use of the local composition concept, while avoiding the Wilson equation s inability to predict liquid-liquid phase separation. The resulting equation has been quite successful in correlating a wide variety of systems. Table: Application guideline of NRTL equation Required Pure-component Application Guidelines Properties Vapor Pressure Components Use for strongly nonideal mixtures and for partially miscible systems 63

64 3.5 NRTL 모델식 ij 0.3 For mixtures of non-polar substances; mixtures for which deviation from ideality is small; for VLE ij 0.2 For systems that exhibit liquid-liquid immiscibility ij 0.47 For mixtures of strongly self-associated substances with Non-polar substances, but not recommended since alternative equations are available, Hayden- O'Connell model for dimers and hexamer model for hexamers. 64

65 3.6 UNIQUAC 모델식 Basis Derived from Derived from on ideas of Guggenheim quasichemical theory to introduce local area fraction in a similar way to local fraction in Wilson model and local mole fraction in Renon model. Takes into account differences in molecular size and shape by introducing area parameter q and volume parameter r. It is superior to Wilson model since it can predict liquid phase splitting phase behavior. Can be used to multi-component phase equilibria with pure and binary parameters only. It is superior to NRTL since it has only two adjustable parameters. (NRTL has 3 parameter for each binary pair.) 65

66 3.6 UNIQUAC 모델식 The excess Gibbs energy (and therefore the logarithm of the activity coefficient) is divided into a combinatorial and a residual part. The combinatorial part depends on the sizes and shapes of the individual molecules; it contains no binary parameters. The residual part, which accounts for the energetic interactions, has two adjustable parameters. The UNIQUAC equation has, like the NRTL equation, been quite successful in correlating a wide variety of systems involving highly nonideal systems or partially miscible systems. 66

67 3.6 UNIQUAC 모델식 67 The expression for the activity coefficient is: R i C i i ln ln ln N j j j i i i i i i i i C i l x x l q z x 1 ln 2 ln ln M j M k kj k ij j M j ji j i R i q ln 1 ln

68 3.6 UNIQUAC 모델식 References 1. Abrams, D. S. and Prausnitz, J. M., 1975, Statistical Thermodynamics of Mixtures: A New Expression for the Excess Gibbs Free Energy of Partly or Completely Miscible Systems, AIChE J., 21,

69 3.7 UNIFAC 모델식 The UNIFAC (UNIQUAC functional activity coefficient) method was developed in 1975 by Fredenslud, Jones, and Prausnitz. This method estimates activity coefficients based on the group contribution concept following the ASOG model. Interactions between two molecules are assumed to be a function of group-group interactions. Whereas there are thousands of chemical compounds of interest in chemical processing, the number of functional groups is much smaller. 69

70 3.7 UNIFAC 모델식 70

71 3.7 UNIFAC 모델식 The UNIFAC method is based on the UNIQIAC model, which represents the excess Gibbs energy (and logarithm of activity coefficient) as a combination of two effects. ln i ln C i ln R i The combinatorial term is computed from the UNIQUAC equation using the van der Waals are and volume parameter calculated from the individual structural groups. A large number of interaction parameters between structural groups for the calculation of residual term, as well as group size and shape parameters habe been incorporated into Aspen Plus. 71

72 3.7 UNIFAC 모델식 72

73 3.7 UNIFAC 모델식 73

74 3.7 UNIFAC 모델식 74

75 3.7 UNIFAC 모델식 75

76 3.7 UNIFAC 모델식 References 1. Fredenslund, Aa., Jones, R. L., and Prausnitz, J. M., 1975, Group Contribution Estimation of Activity Coefficients in Nonideal Liquid Mixtures, AIChE J., 18,

77 4 원료조건, 제품사양및유틸리티조건 77

78 4. 원료조건, 제품사양및유틸리티 4.1 원료조건 4.2 제품사양 4.3 사용하는유틸리티종류및공급및회수온도 78

79 4.1 원료조건 Feedstock Conditions: Component Mole% Ethanol 10.0 Water 90.0 Flow (kmol/h) Temperature ( o C) 45.0 Pressure (bar)

80 4.2 제품사양 Product Specifications: Ethanol purity: Not less than 99.9% by mole Ethanol recovery: Not less than 99.9% Ethanol content in waste water: Not more than 500 ppm by mole Entrainer Selection: Benzene 80

81 4.3 사용하는유틸리티종류및공급및회수온도 Utility Conditions: Steam: 180 o C saturated steam Cooling water 32 o C supply and 40 o C return 81

82 5 삼성분계상평형도상에서의 공비증류공정의설계 82

83 5. 삼성분계상평형도상에서의공비증류공정의설계 5.1 액 - 액상분리선 (Binodal curve) 의도시 5.2 이성분계및삼성분계공비점의추산및공비온도계산 5.3 Residual curve 의도시및영역 I, II 및 III 의특징 5.4 영역 I, II 및 III 에서의공비증류탑의전산모사 83

84 Binodal Curve and Plait Point: P: , IPA P Benzene Water 84

85 Homogeneous & Heterogeneous Azeotropes: P: (0.0500, , ) A: (0.325, 0.675, 0.000), o C B: (0.000, 0.420, 0.580), o C C: (0.299, 0.000, 0.701), o C D: (0.328, 0.244, 0.518), o C IPA A B P D Benzene C Water 85

86 Residual Curve for IPA and Water: Trial Water IPA Benzene

87 Residual Curve for IPA and Water: IPA Benzene Water 87

88 Residual Curve for IPA and Benzene: Trial Water IPA Benzene

89 Residual Curve for IPA and Benzene: IPA Benzene Water 89

90 Residual Curve for Water and Benzene: Trial Water IPA Benzene

91 Residual Curve for Water and Benzene: IPA B II 0.7 A I P D III Benzene C Water 91

92 Composition at Region II can produce pure IPA. IPA B II 0.7 A I P D III Benzene C Water 92

93 Feedstock in Region I. Component S1 S2 S3 Water E-13 IPA Benzene Flow (kmol/h)

94 Feedstock in Region II. Component S1 S2 S3 Water IPA Benzene E-6 Flow (kmol/h)

95 Feedstock in Region III. Component S1 S2 S3 Water IPA Benzene E-8 Flow (kmol/h)

96 6 농축기 (Concentrator) 의전산모사기법 96

97 Concentrator Simulation: Basis: Feed = 100 Kg-mole/hr x F = 0.10 Feed Concentrated ethanol Ethanol Mole Balance F x F = D x D (Nearly Pure Water at Column Bottom) Concentrator Waste water D F x x D F F x x F azeo

98 PRO/II Flow Sheet for a Concentrator: 98

99 Column Summary for a Concentrator: COLUMN SUMMARY NET FLOW RATES HEATER TRAY TEMP PRESSURE LIQUID VAPOR FEED PRODUCT DUTIES DEG C BAR KG/HR M*KCAL/HR C L L R L

100 Distillation Algorithm Selection: (1) Inside Out (I/O) Relatively Ideal Thermodynamics including Hydrocarbon with Water Decant Incorporates sidestrippers into column: No recycle! Thermosiphon Reboilers Flash Zone Model Very forgiving of bad initial estimates Fast! No VLLE 100

101 Distillation Algorithm Selection: (2) CHEMDIST Mechanically simple columns, complex thermo True VLLE Azeotropic and Reactive distillation Sidestrippers solved by recycle No Pumparounds or Thermosiphons More sensitive to bad initial estimates 101

102 Distillation Algorithm Selection: (3) SURE Very general: Complex column and thermo Use when I/O and Chemdist do not apply Newton Method Very sensitive to bad initial estimates 102

103 Distillation Algorithm Selection: (4) Inside/Out (I/O) CHEMDIST SURE Unique Features Strengths Limitations Side & main columns solved simultaneously Very fast Insensitive to initial estimates Thermo non-ideality NO VLLE capability (VLWE at condenser) Reactive Distillation VLLE on any tray Highly Non-Ideal Systems No Pumparounds Side columns solved as recycles Total Pumparounds VLWE on any tray Water draw any tray Generality Slow Sensitive to initial guesses Applicability Hydrocarbons EOS & Slightly nonideal LACT Thermo Interlinked columns Non-Ideal Systems Mechanically simple columns VLLE within column Free water or water draw on trays other than condenser Total pumparounds or vapor bypass 103

104 7 경사분리기 (Decanter) 의전산모사기법 104

105 Decanter Simulation: V R W Assume OVHD Vapor Composition, V around ternary azeotrope Mole % Benzene IPA Water

106 Decanter Simulation: TITLE PROJ=AZEOTROPE, PROB=FLASH,USER=J.H.CHO PRINT INPUT=ALL, RATE=M, FRACTION=M, PERCENT=M DIMENSION METRIC COMPONENT DATA LIBID 1,BENZENE/2,ETHANOL/3,WATER THERMODYNAMIC DATA METHOD SYSTEM(VLLE)=NRTL, SET=NRTL01 STREAM DATA PROP STRM=V, TEMP=70, PRES=1.033, RATE(M)=100, & COMPOSITION(M)=1,53/2,31/3,16 UNIT OPERATIONS FLASH UID=COND, NAME=Condenser, KPRINT FEED V PRODUCT L=R, W=W ISO TEMPERATURE=45, PRESSURE=1.033 END V (Mole %) R (Mole %) W (Mole %) Benzene Ethanol Water Flow Rate 100 % % % 106

107 8 공비증류탑 (Azeotropic Column) 의 전산모사기법 107

108 Azeotropic Column Simulation: V F 2 R Composition of Stream F Component Mole % F W IPA Water Azeo Column Flow Rate 14.8 K-mol/hr P 108

109 Azeotropic Column Simulation: Water balance around Azeotropic Column F Azeo _ feed F W V F 2 F V R W V Azeo Column V F -(1) Ethanol balance around Azeotropic Column F2 V F V -(2) Combining Eq. (1) & (2): V 127.4K-mol/hr, F K-mol/hr 2 Benzene flow from the decanter P K-mol/hr 109

110 Azeotropic Column Simulation: V F F 2 R W Bz Controller P 110

111 9 Stripper 의전산모사기법 111

112 Azeotropic Distillation Process: Scheme 1 Decanter Concentrator Azeotropic Tower Feed Water Dry Ethanol 112

113 Azeotropic Distillation Process: Scheme 2 Decanter Concentrator Azeotropic Tower Stripper Feed Water Dry Ethanol Water 113

114 Azeotropic Distillation Process: Scheme 3 Azeotropic Tower Decanter Concentrator Feed Stripper Water Dry Ethanol Water 114

115 10 전체공정에대한공정최적화 115

116 전제공정에대한 PRO/II Flow Sheet 116

117 전체공정에대한공정최적화 : Concentrator Azeotropic Column Stripper 117

118 Conclusion: 약 * 10 6 Kcal/hr 약 77.38% 118

119 THANK YOU 119

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