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Department of Chemical Engineering

Indian Institute of Technology Kanpur

Chemical Engineering Indian Institute of Technology Kanpur Che391-Unit Operations Laboratory - I Experiment no. 12

Che391-Unit Operations Laboratory - I

Experiment no. 12 Vapor-Liquid Equilibrium

Instructors:

Dr. Siddhartha Panda Dr. Raju Kumar Gupta

Name of TA:

Ms. Prasenjit Sadhukhan

Date of experiment: 24/1/2013 Date of submission: 31/1/2013

Group No: 2

Name

Roll No.

Nitin Kumar Singh

10460

Palash Agarwal

10473

Pankaj Kumar

10476

Contents

1. Objective

3

2. Introduction

3

3. Theory

3

4. Experimental apparatus

4

5. Procedure

5

6. Observations

6

7. Calculations

9

8. Discussion

13

9. Causes of deviation

13

10.Nomenclatures

13

11.References

14

2

Objective

To study the operation of plate and frame filter press.

To determine Specific cake resistance (α) and medium resistance (R).

Introduction

Many processes in the food, chemical or pharmaceutical industries make products that are liquid- solid suspensions or slurries. These mixtures are a little like a runny mud or milk-shake. The solids in them do not dissolve in the liquid but are carried along in it. Filter presses separate the solids from the liquids so that the useful part can be processed or packaged.

A filter consists of a series of filter chambers formed between square, rectangular or round filter plates supported on a metal frame. Once the filter chambers are clamped, filter press is loaded with slurry. The plated on the filter press are clamped together with rams that generate pressure.

In addition to the filter plate filtration medium, the growing filter cake enhances removal of fine particles in the slurry. The solution coming through the filter press called filtrate will be pure. The pores of the medium will be larger than the particles which are to be removed, and the filter will work efficiently only after an initial deposit has been trapped in the medium. One of the biggest advantages of this filtration process is that it is a mechanical operation and much less energy demanding than evaporation or drying. The most important factors in the filter selection are the specific resistance of filter cake, the quantity to be filtered and the solid concentration.

Theory

For incompressible cake:

= μ

= 2 +

+ μ

1

2

Where

α 1 = α*μ*c

b 1 = μ*R

Where,

v= volume of filtrate collected, m 3

t = Time, s

A = Total filtration area, m 2

P = Pressure drop, Kg/cm 2

3

μ = Viscosity of the filtrate

α = Specific resistance of the cake, m/Kg

R

= filter medium resistance, m -1

C

– Concentration of slurry, Kg/m 3

Under constant pressure conditions, we can integrate the above equations to yield

= +

Where, =

and =

Plot of t/v vs. v is a straight line by which we can yield a and b and further α and R by the formulae

= and =

Experimental Apparatus

Mixing tank

Agitator

Pump

Filter tank

Filtrate collection tank

Pressure gauge

A pparatus  Mixing tank  Agitator  Pump  Filter tank  Filtrate collection tank

4

Procedure

1. Prepared slurry of CaCO3 in water (5%) in 25 liter water

2. The slurry war fed to the feed tank and Agitator was switched on

3. The pump was also switched on and only by-pass valves were switched on for better mixing

4. The valve connecting the feed tank to the filter press was turned on completely

5. Closed the by-pass valve very slowly so that the pressure drop was observed to be 10 Kg/cm 2

6. The filtrate was collected in the filtrate collection tank and height of the filtrate collected was noted as a function of time till there was appreciable fall in the rate of the filtrate collection.

7. The process was repeated for the concentration 10% in 15 liter water and 20% in 10 liter water.

filtrate collection. 7. The process was repeated for the concentration 10% in 15 liter water and

5

Observation

Data:-

N F = 6

A c = 16 x 16 cm 2 = 256 cm 2 = .0256 m 2

A Fl = 8 x 8 cm 2 = 64 cm 2 = .0064 m 2

μ = .001 Ns/m 2

g = 9.81 m/sec 2

Wt. of plate 1 = 42.63 g Wt. of plate 2 = 39.39 g Wt. of plate 3 = 42.93 g Wt. of plate 4 = 41.15 g Wt. of plate 5 = 44.76 g Wt. of plate 6 = 42.15 g Wt. of plate 7 = 42.99 g Table# 1 For CaCO 3 concentration 5% in 25 litre water

Time(s)

Height(cm)

P in (mm-Hg)

P out (mm-hg)

0

16

10

0

30

18.8

10

0

60

21.5

10

0

90

24.1

10

0

120

26.6

10

0

150

29.2

10

0

180

31.5

10

0

210

33.8

10

0

240

35.9

10

0

270

38.4

10

0

300

45.5

10

0

330

47.5

10

0

360

49

10

0

390

50.8

12

0

420

52.4

12

0

450

54

12

0

480

55.6

12

0

510

57.2

12

0

540

58.7

12

0

570

60.2

12

0

600

61.7

12

0

630

63.4

12

0

690

64.7

12

0

720

66

12

0

750

67.4

14

0

6

780

68.8

14

0

810

70.1

14

0

840

71.2

14

0

870

72.4

14

0

900

73.5

14

0

930

74.4

14

0

960

75.3

14

0

990

76.2

14

0

1020

77.1

14

0

1050

78

14

0

1080

78.7

14

0

Table #2 For CaCO 3 concentration 10% in 15 litre water

Time(s)

Height(cm)

P in (mm-Hg)

P out (mm-hg)

0

4

10

0

30

6.5

10

0

60

8.7

10

0

90

10.8

10

0

120

12.8

10

0

150

14.5

10

0

180

16.4

10

0

210

18.1

10

0

240

19.8

10

0

270

21.4

10

0

300

22.7

10

0

330

23.8

10

0

360

25.9

12

0

390

26.5

12

0

420

27.3

12

0

450

27.5

12

0

480

27.8

12

0

510

28

12

0

540

28.2

12

0

570

28.4

12

0

600

28.5

12

0

630

28.6

12

0

7

Table #3 For CaCO 3 concentration 20% in 10 litre water

Time(s)

Height(cm)

P in (mm-Hg)

P out (mm-hg)

0

4

10

0

30

6

10

0

60

8.8

10

0

90

9.3

10

0

120

10.1

10

0

150

10.5

12

0

180

10.7

12

0

210

10.8

12

0

240

10.8

12

0

Table#4 Weight of the cake formed for 5% concentration

Plate Number

Wt. of cake with plate(g)

Wt. of cake without plate(g)

1

249.42

206.79

2

235.18

195.79

3

254.65

211.72

4

248.00

203.85

5

255.72

210.96

7

252.64

209.65

Table#5 Weight of the cake formed for 10% concentration

Plate Number

Wt. of cake with plate(g)

Wt. of cake without plate(g)

1

249.21

206.58

2

249.63

210.24

3

253.93

210.62

4

252.42

211.27

5

254.51

209.75

6

249.40

203.25

Table#6 Weight of the cake formed for 20% concentration

Plate Number

Wt. of cake with plate(g)

Wt. of cake without plate(g)

1

250.05

207.42

2

242.32

202.93

3

246.93

204

4

247.92

206.77

5

248.91

204.15

6

248.08

205.93

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Calculations

Table#7 Ref. Height, volume and t/v for 5% concentration

Time(s)

Height, h (cm)

Ref. Height, h`(cm)

Volume(m 3 )

t/v(s/m 3 )

0

16

0

0

0

30

18.8

2.8

0.000717

41852.68

60

21.5

5.5

0.001408

42613.64

90

24.1

8.1

0.002074

43402.78

120

26.6

10.6

0.002714

44221.7

150

29.2

13.2

0.003379

44389.2

180

31.5

15.5

0.003968

45362.9

210

33.8

17.8

0.004557

46084.97

240

35.9

19.9

0.005094

47110.55

270

38.4

22.4

0.005734

47084.26

300

45.5

29.5

0.007552

39724.58

330

47.5

31.5

0.008064

40922.62

360

49

33

0.008448

42613.64

390

50.8

34.8

0.008909

43776.94

420

52.4

36.4

0.009318

45072.12

450

54

38

0.009728

46258.22

480

55.6

39.6

0.010138

47348.48

510

57.2

41.2

0.010547

48354.07

540

58.7

42.7

0.010931

49399.88

570

60.2

44.2

0.011315

50374.72

600

61.7

45.7

0.011699

51285.56

630

63.4

47.4

0.012134

51918.51

690

64.7

48.7

0.012467

55345.23

720

66

50

0.0128

56250

750

67.4

51.4

0.013158

56997.81

780

68.8

52.8

0.013517

57705.97

810

70.1

54.1

0.01385

58485.44

840

71.2

55.2

0.014131

59442.93

870

72.4

56.4

0.014438

60255.98

900

73.5

57.5

0.01472

61141.3

930

74.4

58.4

0.01495

62205.69

960

75.3

59.3

0.015181

63237.77

990

76.2

60.2

0.015411

64239

1020

77.1

61.1

0.015642

65210.72

1050

78

62

0.015872

66154.23

1080

78.7

62.7

0.016051

67284.69

9

Table#8 Ref. Height, volume and t/v for 10% concentration

Time(s)

Height, h (cm)

Ref. Height, h`(cm)

Volume(m 3 )

t/v(s/m 3 )

0

4

0

0

0

30

6.5

2.5

0.00064

46875

60

8.7

4.7

0.001203

49867.02

90

10.8

6.8

0.001741

51700.37

120

12.8

8.8

0.002253

53267.05

150

14.5

10.5

0.002688

55803.57

180

16.4

12.4

0.003174

56703.63

210

18.1

14.1

0.00361

58178.19

240

19.8

15.8

0.004045

59335.44

270

21.4

17.4

0.004454

60614.22

300

22.7

18.7

0.004787

62667.11

330

23.8

19.8

0.005069

65104.17

360

25.9

21.9

0.005606

64212.33

390

26.5

22.5

0.00576

67708.33

420

27.3

23.3

0.005965

70413.09

450

27.5

23.5

0.006016

74800.53

480

27.8

23.8

0.006093

78781.51

510

28

24

0.006144

83007.81

540

28.2

24.2

0.006195

87164.26

570

28.4

24.4

0.006246

91252.56

600

28.5

24.5

0.006272

95663.27

630

28.6

24.6

0.006298

100038.1

Table#9 Ref. Height, volume and t/v for 20% concentration

 

Time(s)

Height, h (cm)

Ref. Height, h`(cm)

Volume(m 3 )

t/v(s/m 3 )

0

4

0

0

0

30

6

2

0.000512

58593.75

60

8.8

4.8

0.001229

63828.56

90

9.3

5.3

0.001357

66332.55

120

10.1

6.1

0.001562

76844.26

150

10.5

6.5

0.001664

90144.23

180

10.7

6.7

0.001715

104944

210

10.8

6.8

0.001741

120634.2

240

10.8

6.8

0.001741

137867.6

10

Sample calculations:-

For CaCO3 concentration of 5% P = 11.94*1333.22 Pa = 15918.64 pa A = 2 * N f * A fl m 2 = 2 * 6 * (64 * 10-4) = 0.0768 m 2 a(slope) = 2 x 10 6 m -3 b(intercept) = 36270 s/m 3 α = 2 * A 2 * ΔP * a / (μ * c) m/kg = 7.51*10 10 m/Kg R = A * ΔP * b / μ m -1 = 4.43* 10 12 m -1

Concentration

50

100

200

a(slope)( m -3 )

2 x 10 6

7 x 10 6

5 x 10 7

b(intercept)( s/m 3 )

36270

36211

16637

P(Pa)

15918.64

14532.09

14517.43

α(m/Kg)

7.51

x10 10

1.2 x 10 11

4.3

x10 10

R(m -1 )

4.43

x 10 12

4.04 x 10 10

1.9

x10 10

Graph#1 t/v vs. v for 5% concentration of CaCO 3 t/v vs v 80000 70000
Graph#1 t/v vs. v for 5% concentration of CaCO 3
t/v vs v
80000
70000
y = 2E+06x + 36270
60000
R² = 0.7509
50000
40000
30000
20000
10000
0
0
0.002
0.004
0.006
0.008
0.01
0.012
0.014
0.016
0.018
V (cu. m)

11

Graph#2 t/v vs. v for 10% concentration of CaCO 3

t/v vs v 120000 100000 y = 7E+06x + 36211 80000 R² = 0.7237 60000
t/v vs v
120000
100000
y = 7E+06x + 36211
80000
R² = 0.7237
60000
40000
20000
0
0
0.001
0.002
0.003
0.004
0.005
0.006
0.007
V (cu. m)
Graph#3 t/v vs. v for 20% concentration of CaCO 3 t/v vs v 160000 140000
Graph#3 t/v vs. v for 20% concentration of CaCO 3
t/v vs v
160000
140000
120000
y = 5E+07x + 16637
100000
R² = 0.5455
80000
60000
40000
20000
0
0 0.0002
0.0004
0.0006
0.0008
0.001
0.0012
0.0014
0.0016
0.0018
0.002
V (cu. m)

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Discussion

Surface filtration works largely through direct interception. This means that the pore size of the medium are stopped at the upstream surface of the filter. The particle size prevents them from entering or passing the pores. Surface type media are not perfectly smooth on their surfaces, nor are their pores perfectly in their shape or direction.

Typically, when surface type filters are exposed to the flow of contaminated fluid, two effects- the gradual reduction in effective pores size and the building of a cake bed- start to take place almost immediately.

Gradual reduction in effective pore size- The effective pore size of the medium is gradually reduced, as some of the pores become partially blocked by the particles, this reduction makes the filter become more effective in removing fine particles. Pore size reduction can be caused by the retention of extremely small particles within the pores by absorptive forces.

Building of cake filter- A cake or bed filter aid particles start to build on the surface of the filter cloth. This build-up of filter cake actually does the filtering. As time continues this cake becomes progressively finer.

Causes of Deviations:

1. The deposition of filtrate inside the plate and frame filter press led to deviated results filtrate

volume.

2. Pressure drop could not be maintained constant as all the slurry made was exhausted and some

air had entered the pump.

3. The readings on the scale were not clear and only after a certain time the readings became visible;

Also error due to parallax.

4. Some filtrate was lost when additional slurry was prepared and mixed in the agitator.

Nomenclature

A = Slope of the graph

A Fl = Area of one frame, m 2

A C = filtration area, m 2

B = Intercept of the graph

V = Volume of filtrate collected in time t, m 3

t = time, s

C = Concentration of the slurry, Kg/m 3

g = Acceleration due to gravity, m/sec 2

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N f = Number of frames

ΔP = pressure drop, mm-Hg

μ = viscosity of the filtrate Ns/m 2

α = specific resistance of the cake, m/Kg

R = filter medium resistance, m -1

V = volume of filtrate collected in time t, m 3

Pi = Inlet Pressure, mm-Hg

Po = Outlet Pressure, mm-Hg

h = height of filtrate collected in time t, cm

Reference

1. Lab Manual ChE 391, 2012-13

2. McCabe, W.L. and J.C. Smith, Unit Operations of Chemical Engineering, 3rdEdition, McGraw-Hill,

1976 pp. 932-942

3. Coulson, J.M. and J.F. Richardson, Chemical Engineering, Vol. 2, Pergamon Press, 1960, pp. 414-

421

4. Walas, S.M, Chemical Process Equipment Selection and Design, Butterworth- Heinemann, 1990,

pp. 305-334

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