Chemical unit operations 2. lectures 2 hours/week calculation seminars weekly 1 hours laboratory weekly 3 hours

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1 Chemical unit operations 2. lectures 2 hours/week calculation seminars weekl 1 hours laborator weekl 3 hours

2 Requirements Attendance will be checked. Requirements for the signature: Attending on minimum 66% of the lectures and calculation seminars, and on all laborator practices is required. One calculation test will be scheduled during the semester. Eact dates and topics covered will be announced later. The calculation test have to be passed for signature. The grade of the calculation test counts as 25% of the final grade. Nine laborator measurements will be scheduled. Each measurement have to be performed, and reports accepted. Students having valid signature ma take a written eam during the eamination period. Application for the eams is onl possible via the Neptun sstem. Website of the course: Please check it frequentl!

3 Distillation Edit Székel, Béla Simándi

4 Topics to be covered Distillation in the industr (introduction). Basic definitions. apour-liquid equilibria. Measurement and simpl calculation methods. Ideal and non-ideal phase diagrams. Batch distillation. Flash distillation. Distillation columns = rectification.

5 Distillation in the industr Ethanol production Food industr Chemical industr Bioethanol

6 Distillation in the industr Ethanol production Oil industr fractionation (products based on distillation intermediates: fuels, raw material of chemical industr, plastics, solvents, bitumen etc. )

7 Distillation in the industr Ethanol production Oil industr Waste water treatment Mainl waste waters with high solvent contamination Waters from absorption (purification of ehaust gases).

8 Advantages of distillation Major separation process for homogeneous liquids of two or more components. Separation is based on the difference in boiling points (volatilit). No additional chemicals are needed, but energ requirement is relativel high. In a large number of separation task it is the most economical option.

9 Boiling point Depends on: ingredients molar ratios, eact composition pressure A liquid starts to boil if the sum of the partial pressure of its ingredients is equal to the pressure of the environment.

10 apour pressure of a pure component apour pressure is the pressure measured above a neat liquid component in equilibria (no other components in the sstem). It depends on the materials itself, and on temperature. Alwas increases with temperature. Antione equation: lg p 0 A C B T P 0 vapour pressure (Pa; Hgmm), T temperature ( C, K), A,B,C Antoine-constants

11 If its boiling point is lower at a chosen pressure than the other s one, that component is called more volatile. If a liquid miture is boiling, in general, the more voletile component has a higher relative concentration in the vapour phase than in the liquid phase. olatilit is the ratio of the molar fraction of component j in the vapour phase over its molar fraction in the liquid phase. K j j j olatilit

12 aws of Raoult and Dalton Dalton s law Partial pressure is the share of the given vapour of the total pressure. This is proportional with its molar fraction in the vapour phase. p j partial pressure of component j (Pa), j molar fraction of component j in vapour phase (-), P total pressure (Pa). p j j P Raoult s law A miture is ideal from a practical point of view if law of Raoult is valid for an compositions in the eamined range of temperatures. p 0 j vapour pressure of neat component j (Pa) at the given temperature, j molar fraction of component j in the liquid phase. p j p 0 j j

13 Bubble point dew point diagrams These diagrams are constructed based on eperimental data obtained in special equipment.

14 Measurement of vapour- liquid equilibrium data The liquid is heated b electrical heating and kept continuous boiling. Pressure is stricktl kept constant. The vapour phase is circulated. At equilibrium samples are taken from both phases, and composition is analsed.

15 Bubble point dew point diagrams These diagrams are constructed based on eperimental data obtained in special equipment. In case of ideal mitures, phase diagrams can be easil obtained b simple calculations. A miture is ideal if: aw of Raoult is valid, Complete misciblit in liquid phase, The constituents are usuall chemicall similar (e.g. linear chain hdrocarbons).

16 Bubble point dew point curves and the equlibrium curve P=constant miture of benzene and toluene at atmospheric pressure (P=1.013 bar)

17 Bubble point dew point curves and the equlibrium curve P=constant miture of isopropil-ether isopropanol at atmospheric pressure

18 Bubble point dew point curves and the equlibrium curve P=constant miture of acetone-chloroform at atmospheric pressure

19 Bubble point dew point curves and the equlibrium curve P=constant miture of ethl acetate water at atmospheric pressure

20 Batch distillation

21 Batch distillation mathematical description of the unit oparation Deriving the Raleigh-equation Set up the molar balance and component balance equations for an infinitel short dt time. During this dt time, a vapour of molar amount d is produced with a composition (molar increase of distillate is equal, since distillate is formed b condensing the vapour). Molar amount of the boiling liquid in the vessel is meanwhile decreased b d. Thus the molar balance is:

22 Raleigh-equation d ) d )( d ( d d d d d d d d 0 d d d 0 ) ( d d d d d d ln d neglect second-order differential dd and reorder: substitute d=d separate the variables D d d d

23 Batch distillation mathematical description of the unit operation Applications of the Raleigh-equation 0 d ln where and are compositions of vapour and liquid phases in equilibrium; inde 0 refers to initial (at t 0 time) 1 refers to the final (t 1 ) values; is molar amount of the liquid phase (mol). If initial amount of the liquid ( 0 ) and its composition ( 0 ) is known and the desired purit is defined ( 1 ), amount of remaining liquid ( 1 ) can be calculated b the Raleigh-equation.

24 Batch distillation mathematical description of the unit operation Calculation of average composition in distillate 0, 1, 0, 1 are alread known. From molar and composition balances the two unknown can be calculated D D D D D D distillate. the average composition of is where D

25 Applications of batch distillation imits of separation. Subsequent distillations are needed. When relativel smaller amount of feed have to be purified batch distillation is more economic than continuous distillation processes. When composition of feed changes frequentl, but distillation have to be performed in the same unit.

26 Continuous single stage distillation / flash distillation Consists of: vaporizing a definite fraction of the liquid in such a wa, that the evolved vapor is in equilibrium with the residual liquid, separation the vapour and the liquid, condensing the vapour. It is a continuous, stead-state operation. stead-state: temperature, pressure, compositions and flow rates are constant. Separation performed is equivalent to one single theoretical stage.

27 Continuous single stage distillation at constant pressure Molar flow rate of feed is F. Its composition if F (molar fraction of the more volatile component in case of binar mitures). Molar flow rate of the vapour is. Its composition is (molar fraction of the more volatile component in case of binar mitures). The vapour is in equilibrium with the liquid product. Heating steam. Molar flow rate of liquid product is. Its composition is (molar fraction of the more volatile component in case of binar mitures). Condensate of heating steam

28 Flash distillation b reduction of pressure iquid phase feed apour Preheater. The liquid is heated below its boiling point at pressure P1. The final temperature should be sufficientl higher than temperature of boiling at P2. Pressure reducing valve Cclone. apour and drops of liquid are separated b sedimentation. iquid product

29 Flash distillation b partial condensation apour feed apour product Partial condensator Cclone. apour and drops of liquid are separated b sedimentation. iquid product

30 Flash distillation mathematical description Molar balance F Component balance F F Epress as function of and plot the epression in the equilibrium diagram! Since and are equilibrium compositions, intersection of the two curves is the point of operation. F F F F F F F

31 Flash distillation F F if F F F F F

32 Flash distillation range of operation Flash disitillation is one single equilibrium stage.

33 Flash distillation - summar Rarel used as individual separation unit because its limitations in purit. In case of non-ideal mitures like heteroazeotropic mitures it might be an option. Partial reboiler of a rectification column is a flash distillation unit.

34 Distillation columns continuous rectification A separation process performed in stead state operation. As usual for continuous processes, it is mostl applied at constant and high feed rates. Frequentl used in industrial scale. Separation is based on vapour-liquid equlibrium.

35 Rectification = subsequent partial condensations and subsequent partial evaporations P=constant Partial evaporation of liquid Partial condensation of vapor

36 Distillation column

37 Rectification, balance equations Molar balance F DW molar flow rate of feed (F), of distillate (overhead product) (D) and bottoms product (W) (mol/s or kmol/h). Component balance F F D D W W Compositions: molar fraction values of the more volatile component.

38 Simple calculation methods for inital estimations The technique discussed is considered to be the simplest method for analsis of binar distillation. In an ideal stage (plate or tra), the phase leaving the stage is in equilibrium with the phase leaving the same stage. The problem is that of finding the number of ideal stages required in an actual column to achieve a desired separation. If the number of theoretical stages can be determined, and information on the stage efficiencies is available, the number of actual stages can be calculated.

39 Reflu ratio, operating lines Reflu ratio: R=/D Basic assumtion: constant molal overflow.

40 Continuous fractionation column- Constant molal overflow Assumptions: The column is adiabatic (sufficient insulation, neglectable heat loss). Heat effects (heats of solution, heat losses to and from column, etc.) are negligible. Heat of evaporation is the major source of an heat effects in the column. Molal heats of vaporization of the components are roughl the same. For ever mole of vapour is condensed, a mole of liquid vaporized. Results: iquid and vapour molar flow rates are constant in the rectifing and in the stripping sections, separatl.

41 Continuous fractionation column reflu ratio, operating lines Plates are numbered seriall from the top down. Flows leaving the plates are numberred accordingl. Assumption: liquid and molar flows leaving a theoretical (ideal) plate have equilibrium compositions. Based on constant molal overflow: n n

42 Consider the part of the column enclosed b control line, a component balance of rectifing section can be written as: Rectifing operating line D n n D 1 Molar balance of the rectifing section (similar to the balance equation of the condenser): D Epressing n+1 from the component balance and substituting into molar balance equation we obtain: D n D n n D D D D 1

43 Rectifing operating line D n D n n D D D D 1 Divide b D and substitute the reflu ratio (R=/D): R R R D n n Generalized form is an equation of a straight line: 1 1 R R R D

44 Operation line of the stripping section Balance equations can be set analogousl to the lower part of the column. Control line includes the still and all plates below plate m. and are the molar flow rates of vapor and liquid in the stripping section: ' ' W 'm m1 W W

45 Operation line of the stripping section W ' ' W m m W ' 1 W m m W ' ' ' 1 W W ' ' '

46 Continuous fractionation column reflu ratio and operating lines With known reflu ratio operating line of the rectifing section can be draw in the E (equlibrium) diagram. The condition of the feed can be deduced b the slope of the feed line or q-line. The q-line is that drawn between the intersection of the operating lines, and where the feed composition lies on the diagonal line. ' ' W ' W

47 Continuous fractionation column feed q H F h F F line/ q-line, where H F is the enthalp of the saturated vapour with the composition of F (J/mol), h F is the enthalp of the feed (J/mol), λ F is molar heat of vaporization of a miture with F composition (J/mol). Consistence and properties of feed h F q Cold liquid (below its boiling point) h F < H F -λ F 1 < q known as subcooled liquid Boiling liquid known as saturated liquid h F = H F -λ F q = 1 Miture of liquid and vapour, q is equal h F = H F q λ F 0 < q < 1 to liquid mole fraction Saturated vapour h F = H F q = 0 Overheated (superheated) vapour h F > H F q < 0

48 q Continuous fractionation column effect of feed condition on molar flow rates H F h F F Molar balance of the feed plate: F When feed is miture of vapour and liquid, (q) liquid fraction is added to the liquid and (1-q) fraction to the vapour flow. qf (1 q) F

49 Continuous fractionation column condition of feed F q q q Knowing q the q-line can be drawn. Deduct equation of rectifing operating line from equation of stripping operation line: W W D D ) ( ) ( W W W W ' ' ' ' ' D D n D D F F F q F q ) ( 1 F q q ) ( 1 F q F q ) 1 ( (-)

50 1 D = D 0,8 0,6 0,4 0,2 w = w 0 saturated miture subcooled saturated overheated liquid of liquid Effect of feed condition and vapour vapour Rectifing q>1 operation line R q=1 tg R 1 0<q<1 q line q q=0 tg q 1 D R q<0 1 Given: R, q, w, D, F Stripping operation line 0 0, , ,6 0,8 1 w F D

51 Minimal reflu ratio 1 D = D 0,8 Upper operating line R min can be calculated Rmin tg from the read Rvalue 1 min N= 0,6 R min D 1 q line tg q q 1 0,4 Given: 0,2 q, w, D, F R min =? w = w 0 0 0,2 0,4 0,6 0,8 1 w F D

52 1 Minimal number of theoretical plates D = D 0.8 Equilibrium curve Given: 0.4 w, D N min =? line: = N min =4 w = w w D

53 Simple calculation methods for inital estimations Calculation of the minimal number of theoretical plates. gives us information about the difficultness of the desired separation, needed: desired compositions of overhead and bottoms products. Minimal reflu ratio: to achive the desired separation, reflu ratio has a minimal value. Number of theoretical plates is determined: with McCabe Thiele method.

54 1 McCabe-Thiele method (1925) D = D 1 0,8 0,6 0,4 D R 1 tg 6 R R q line tg 3 2 q q 1 R, q, w, D, F 7 N theoretical =? 0,2 N theoretical =7 w = w 0 0 0,2 0,4 0,6 0,8 1 w F D

55 cooling water in cooling water out 1 D = D 1 D Distillate (overhead product) D 0,8 0,6 Feed , , w = w 0 0 0,2 0,4 0,6 0,8 1 w F D Heating steam in Bottoms product w Condensate out

56 Simple calculation methods for inital estimations Calculation of the minimal number of theoretical plates. gives us information about the difficultness of the desired separation, needed: desired compositions of overhead and bottoms products. Minimal reflu ratio: to achive the desired separation, reflu ratio has a minimal value. Number of theoretical plates: with McCabe Thiele method. Calculation of column diameter.

57 oad factor m s G F load v kg Pa 3 m P P P M R T 1 2 P G 0 N real oad factor (F load ) : Depends on: linear velocit of vapour in the empt column (v) densit of vapour (ρ G ). Densit of vapour is influenced b: average molar mass (composition!), temperature (P, ), pressure. Pressure is lowest at top, highest at bottom of column.

58 Plate efficienc valve plate bubble plate sieve plate Operation range: horizontal part

59

60 Calculation of column diameter v F load volumetric flow rate at top and bottom R T const t P 0 R P 4 v 2 2 A D D o 4 v G o D o 4 const T a Selection of load factor value, caluclate diameter at top and bottom (D 0 ), select a suitable value in between. R const is the ideal gas constant J/(mol*K)

61 Simple calculation methods for inital estimations Calculation of the minimal number of theoretical plates. gives us information about the difficultness of the desired separation, needed: desired compositions of overhead and bottoms products. Minimal reflu ratio: to achive the desired separation, reflu ratio has a minimal value. Number of theoretical plates: with McCabe Thiele method. Calculation of column diameter. Calculation the height of the column.

62 Determine (N theoretical ). Height of column Read average plate efficeinc (η plate ) and calculate the number of real plate. Round up. Multipl with plate height. N real N theoretical plate H N real H

63 Plate columns topics covered Theoretical and real plates Operation Calculation of N min, R min McCabe Thiele method, plate efficienc oad factor Construction. 63

64 Bubble-cap plate 64

65 sieve plate weir downcomer 65

66

67 alve plate 67

68 Operation of valve tras G ő z G ő z G ő z 68

69 Packed columns Random or structured packing. Random packing is cheaper, but less efficient (same height less separation efficienc). Modern structured packing can be applied from laborator scale to large industrial scales.

70 Determination of the heights of the column 1. H N HETP HETP= Height Equivalent to a Theoretical Plate Sulzer Mellapak packing 70

71 Determination of the heights of the column 2. Instead of theoretical plates the term transfer units migh be also applied. NTU (Number of Transfer Units) HTU (Height of a Transfer Unit) To be calculated separatl for the upper and lower sections of the column. Onl the active height is calculated. H HTU l NTU l HTU u NTU u 71

72 Theoretical background d K a A( ) d H K a A m molar flow rate of vapour at top of column (mol/s), mass tranfer coefficient (mol/(m 2 s)), relative surface area of packing (m 2 /m 3 ), wetting coefficient(-), cross section of column (m 2 ), virtual vapour concentration which would be in equilibrium with the liquid concentration (-). 72

73 Theoretical background the two film theor m K 1 1 Ai m Ai ) ( Ai A A J ( A) Ai A J Ai A A m J A Ai A J ( A) A A K J ) ( ) ( Ai A Ai A m m m A Ai Ai A A m J 1 73

74 Calculation of the heights of the column H A a K d ) ( d D F f H A a K H H d d 0 A a K H d d A a K HTU u D F u NTU d A a K HTU l ' F W l NTU d 74

75 Calculation of HTU known: F, R, q, F, D, W D W F D w F D W F D w D w F W F W D W F D W D F F W W F D D R 1 A a K HTU u F q 1 ' A a K HTU l ' 75

76 Calculation of NTU 76

77 Random packing 77

78 Random packing / rings Raschig-ring Pall-ring 78 Cascade ring

79 Random packing / saddles Berl-saddle Intalo-saddle 79 Super intalo-saddle

80 Further random packing elements Snowflakes Konjugated rings 80 essing-ring

81 Further random packing elements balls Envipack spheres 81 Spiral packing

82

83 Structured packing 83

84 Structured packing tpes of distillation 84

85 iquid distributors 85

86 Grids 86

87 ocating grids 87

88 Assembl The column sleeve is lowered into the column with two cranes. Weight: 100 tons Installation of the liquid distributor photos: Sulzer 88

89 Economical optimum 89

90 Economical optimum Cooling and heating W W W F q D R F q Q 1 1 1) reb D D D R Q 1 cond 90

91 Thank ou for our attention!

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