M.

Tech Project Final Presentation

Dept. of Chemical Engineering IIT Delhi

TOPIC: CATALYTIC WET AIR OXIDATION

Supervisor-Dr A.K Saroha

Amit Gupta 2007ch50101

To perform catalytic wet air oxidation of a multicomponent reactant. To go through literature and find suitable catalyst and conditions for the reaction. To find temperature and other conditions optimum for the reaction To understand the Deactivation rate and methods to regenerate the catalyst

Involves the liquid phase oxidation of organic or oxidizable inorganic components . Complex organic compounds are mostly oxidized into carbon dioxide and water along with simpler forms .
Useful when concentration of organic pollutant are too low or when organic pollutant are toxic

Schematic Diagram of the Experimental Set-up

1- Compressor 2- Rotameter 3 Condenser 4 Heating mantle 5-Agitation controller 6- Thermometer 7 Cooling water out 8 Cooling water in 9- Pipette to withdraw sample 10 Magnetic bar 11- Air flow 7

2 11 1 4 10 5

Based on oxidation of carbon of organic matter to carbon dioxide Carbon dioxide is swept into a non dispersive infrared analyzer Steam is condensed and removed Includes both organic and inorganic carbon in the sample Sample Injected : 100 microlitres Temperature : 8000C T.O.C. for the sample : 133.2 mg/ltr

Sample : Organic Raffinate Temperature : 100C Air flow rate : 2 ltr/min Initial T.O.C : 133.2 mg/ltr
Time (hr)
1 2 3 4 5

T.O.C (mg/ltr)
118.67 108.43 96.27 87.48 78.09

Experiment 1: Temperature 10 0C
140

120

T.O.C (mg/ltr)

100

80

60

Experiment 3: Temp 10C

40

20

0 0 1 2 3 4 5 6

Time (hr)

Sample : Organic Raffinate Temperature : 300C Air flow rate : 2 ltr/min Initial T.O.C : 133.2 mg/ltr
Time (hr)
1 2 3 4 5

T.O.C (mg/ltr)
109.67 102.45 91.42 81.28 69.32

Experiment 2: Temperature 30 0C
140

120

100

T.O.C (mg/ltr)

80

60

40

20

0 0 1 2 3 4 5 6

Time (hr)

Sample : Organic Raffinate Temperature : 700C Air flow rate : 2 ltr/min Initial T.O.C : 133.2 mg/ltr
Time (hr)
1 2 3 4 5

T.O.C (mg/ltr)
105.9 93.11 82.55 74.25 52.63

Experiment 3 : Temperature 70 0C
140

120

100

T.O.C (mg/ltr)

80

60

Experiment 1 :Temp 70C

40

20

0 0 1 2 3 4 5 6

time (hr)

Comparison at different Temperature

140 120

100

T.O.C (mg/ltr)

80

60

T.O.C 70 degree T.O.C 30 Degree T.O.C 10 degree

40

20

0 0 1 2 3 4 5

Time (hr)

Sample : Organic Raffinate Temperature : 300C Catalyst : Alumina ( 2 g/ltr) Air flow rate : 2 ltr/min Initial T.O.C : 133.2 mg/ltr
Time (hr)
1 2 3 4 5

T.O.C (mg/ltr)
107.63 101.08 87.49 77.28 66.32

Experiment 4 : Reaction using Alumina at 30C

140

120

100

T.O.C (mg/L)

80

60

Using Alumina

40

20

0 0 1 2 3 4 5

time (hr)

Preparation of Platinum/Alumina Catalyst Wetness Incipient Method

Commonly used technique for synthesis of heterogeneous catalyst Active metal precursor is dissolved in an aqueous or organic solution Then the metal containing solution is added to a catalyst support Then the mixture is stirred in a magnetic stirrer for around 5 hours It is then left for overnight drying to convert the catalyst in powder form and remove excess moisture

Calculations
Total Alumina taken - 10 gram

Platinum weight % in the catalyst 0.58 %

Total Platinum that has to be taken 0.0583 g Molecular weight of Platinum chloride 409.82 Molecular Weight of Platinum 195.078 Total salt that has to be taken - 0.1218 gram

Thermo gravimetric Analysis

T.G.A. of Pt/Alumina catalyst

Temperature Programmed Reduction

T.P.R. of Pt/Alumina Catalyst

Sample : Organic Raffinate Temperature : 300C Catalyst : Pt/Alumina ( 2 g/ltr) Air flow rate : 2 ltr/min Initial T.O.C : 133.2 mg/ltr
Time (hr)
1 2 3 4 5

T.O.C (mg/ltr)
102.32 90.58 79.44 68.79 59.26

Experiment 5
Experiment : Using Pt/alumina
140
120 100 80 60 40 20 0 0 1 2 3 4 5 With Pt/alumina

T.O.C (mg/ltr)

Time (hr)

Comparison at 30C
Comparison :
140

120

100 T.O.C (mg/ltr)

80

T.O.C with Alumina T.O.C. without catalyst T.O.C with pt/Alumina catalyst

60

40

20

0 0 1 2 3 4 5

 1.

2.

Catalytic Wet Air Oxidation Catalytic wet air oxidation at different temperature using Pt/Alumina catalyst Wet air oxidation of the sample using catalyst like ceria with platinum

1.

Characterization
Physical properties like EDX, Metal dispersion, surface area, pore area

 1.

2.

Deactivation Deactivation of supported metals by carbon or coke may occur chemically owing to chemisorptions or carbide formation or physically and mechanically Blocking of surface sites, metal crystallite encapsulation, plugging of pores, and destruction of catalyst pellets by carbon laments Regeneration Carbon and coke formation is relatively easily reversed through gasication with hydrogen, water, or oxygen

1.

Compared to conventional wet oxidation, catalytic wet oxidation offers lower energy requirements and much higher oxidation efficiencies Literature only shows catalytic wet air oxidation of single component reactant Result would be compared on the basis of T.O.C. rather than conversion; leading to better results

LITERATURE REVIEW
Presently reading the following manuscripts:
Mishra et al. (1995) Wet Air Oxidation.

Luck(1996) A review of industrial catalytic wet air oxidation process J. Levec and A. Pintar. Catal. Today 24 (1995) M. J. Dietrich et al. (1996) Wet Air Oxidation of Hazardous Oraanics in Wastewater. F. Luck (1994) Wet air oxidation: past, present and future.