EXP 3 - RTD in Packed Bed

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RTD IN PACKED BED

EXPERIMENT 10: PACKED BED REACTOR 1.0

INTRODUCTION

In the majority of industrial chemical processes, a reactor is the key item of equipment in which raw materials undergo a chemical change to form desired products. The design and operation of chemical reactors is thus crucial to the whole success of the industrial operation. Reactors can take a widely varying form, depending on the nature of the feed materials and the products. Understanding non-steady behaviour of process equipment is necessary for the design and operation of automatic control systems. One particular type of process equipment is the tubular reactor. In this reactor, it is important to determine the system response to a change in concentration. This response of concentration versus time is an indication of the ideality of the system. The RTD in Packed Bed has been designed for students experiment on residence time distribution (RTD) in a tubular reactor. The unit consists of mainly a vertical glass column packed with glass Raschig rings. Sump tanks and circulation pumps are provided as well as instruments to measure concentration of the tracer passing through the column. Students may select either step change input or impulse input to the reactor and will continuously monitor the responses in the reactor at a suitable interval. Objective: The main objective of this laboratory work is to determine the effect of liquid (L) and gas (G) feed rates on the mean residence time and degree (intensity) of liquid-phase axial dispersion. 2.0

SUMMARY OF THEORY

The residence-time distribution (RTD) of a reactor is a characteristic of the mixing that occurs in the chemical reactor. There is no axial mixing in a plug-flow reactor (PFR), and this omission is reflected in RTD which is exhibited by this class of reactors. The CSTR (constant stirred type reactor) is thoroughly mixed and possesses a far different kind of RTD than the plug-flow reactor. The RTD exhibited by a given reactor yields distinctive clues to the type of mixing occurring within it and is one of the most informative characterizations of the reactor. The RTD is determined experimentally by injection an inert chemical, molecule, or atom, called a tracer, into the reactor at some time t = 0 and then measuring the tracer concentration, C, in the effluent stream as a function of time. In addition to being a nonreactive species that is easily detectable, the tracer should have physical properties similar to those of the reacting mixture and be completely soluble in the mixture. It is also should not adsorb on the walls or other surfaces in the reactor. The latter requirements are needed so that the tracer‟s behavior will honestly reflect that of the material flowing through reactor. The two most used methods of injection are pulse input and step input. In a pulse input, an amount of tracer N0 suddenly injected in one shot into the feedstream entering the reactor in as short a time as possible. The outlet concentration is then measured as a function of time. Typical concentration-time curves at the inlet and outlet of an arbitrary reactor are shown in Figure 1. The effluent concentration-time curve is referred to as the C curve in RTD analysis. We

Updated January 2013 by Asnizam Helmy

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RTD IN PACKED BED

shall analyze the injection of a tracer pulse for a single-input and single-output system in which only flow (i.e., no dispersion) carries the tracer material across system boundaries. First, we choose an increment of time t sufficiently small that the concentration of tracer, C(t), exiting between time t and t + t is essentially constant. The amount of tracer material, AN, leaving the reactor between time t and t + t is then N

C (t )v t

(1)

where v is the effluent volumetric flow rate. In other words, N is the amount of material that has spent time between t and t + t in the reactor. If we now divide by the total amount of material that was injected into reactor, N0, we obtain N vC (t ) t (2) N0 N0 which represents the fraction of material that has a residence time in the reactor between time t and t+ t. For pulse injection we define E (t )

vC (t ) N0

(3)

N N0

E (t ) t

(4)

so that

The quantity E(t) is called the residence–time distribution function. It is the function that describes in a quantitative manner how much time different fluid elements have spent in the reactor.

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RTD IN PACKED BED

Figure 2 Concentration-time curves in RTD analysis.

If N0 is not known directly, it can be obtained from the outlet concentration measurements by summing up all the amounts of materials, N, between time equal to zero and infinity. Writing Eq.(1) in differential form yields dN

vC(t )dt

(5)

and then integrating, we obtain

N0

vC(t )dt 0

the volumetric flow rate is usually constant, so we can define E(t) as

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(6)

RTD IN PACKED BED

C (t )

E (t )

(7)

C (t )dt 0

The integral in the denominator is the area under the C curve. An alternative way of interpreting the residence-time function is in its integral form: Fraction of material leaving the reactor that has resided in the reactor for times between t1 and t2

t2

= E (t )dt

(8)

t1

We know that the fraction of all the material that has resided for a time t in the reactor between t = 0 and t = ∞ is 1; therefore, (9)

E (t )dt 1 0

Let‟s consider the example of constructing the C(t) and E(t) curves. Given: a sample of the tracer hytane at 320 K was injected as a pulse to a reactor and the effluent concentration measured as a function of time, resulting in the following data: Table 1. t (min.) C (g/m3)

0 0

1 1

2 5

3 8

4 10

5 8

6 6

7 4

8 3.0

9 2.2

10 1.5

12 0.6

14 0

Processing original data by cubic spline interpolation, the C(t) curve shown in Figure 3 is obtained. (Here MathCAD package [3] has been used for numerical calculations; alternatively it can be done by any available software). 10

C(t) (g/m3)

8 6 4 2 0

0

2

4

6

8

10

12

14

t (min.)

Figure 3. Points – original data on concentration, line – C(t) spline.

To obtain the E(t) curve, we just divide C(t) by the integral

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RTD IN PACKED BED 14

C (t )dt 0

C (t )dt

(10)

50.55

0

(The integral (10) also can be evaluated directly from the Table 1 by a pencil and paper calculation using Simson‟s rule [4]). C (t ) C (t ) Calculations of E (t ) give the following results: 50.55 C (t )dt 0

Table 2. t (min.) 0 1 2 3 4 5 6 7 8 9 10 12 14 3 C (g/m ) 0 1 5 8 10 8 6 4 3.0 2.2 1.5 0.6 0 E(t)(min 0 0.02 0.099 0.158 0.198 0.158 0.119 0.079 0.059 0.044 0.03 0.012 0 -1) The E(t) curve is plotted in the Figure 4. 0.2

E(t) (1/min)

0.16 0.12 0.08 0.04 0

0

2

4

6

8

10

12

14

t (min.)

Figure 4. RTD curve calculated from experimental data (Table 1).

The principal potential difficulties with the pulse technique lie in the problem connected with obtaining a reasonable pulse at a reactor‟s entrance. The injection must take place over a period which is very short compared with residence times in various segments of the reactor or reactor system, and there must be a negligible amount of dispersion between the point of injection and the entrance to the reactor system. If these conditions can be fulfilled, this technique represents a simple and direct way of obtaining the RTD. There are problems when the concentration-time curve has a long tail because the analysis can be subject to large inaccuracies. This problem principally affects the denominator of the right-hand side of Eq. (7). (i.e. the integration of the C(t) curve). It is desirable to extrapolate the tail and analytically continue the calculation. The tail of the curve may sometimes be approximated as an exponential decay. The inaccuracies introduced by this assumption are very likely to be much less than those resulting from either truncation or numerical imprecision in this region. As a more general relationship between a time varying tracer injection and the corresponding concentration in the effluent we state without development that the output concentration from a

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RTD IN PACKED BED

vessel is related to the input concentration from a vessel is related to the input concentration by the convolution integral (a development can be found in [2]): t

Cout (t )

Cin (t t ) E (t )dt

(11)

0

The inlet concentration of tracer most often takes place the form of either perfect pulse input (Dirac delta function), imperfect pulse injection (see Figure 2), or a step input. Let us analyze a step input in the tracer concentration for a system with a constant volumetric flow rate. Assume a constant rate of tracer addition to a feed that is initiated at time t = 0. Before this time no tracer was added to the feed. Stated symbolically, we have

0 C0 (const )

C0 (t )

t

0

t

0

(12)

The concentration of tracer in the feed to the reactor is kept at this level until the concentration in the effluent is indistinguishable from that in the feed; the test may then be discontinued. A typical outlet concentration curve for this type of input is shown in Figure 2. Because the inlet concentration is a constant with time, C0, we can take it outside the integral (11) sign, that is, t

Cout

C0 E (t )dt

(13)

0

Dividing by C0 yields Cout C0

t

E (t )dt step

(14)

0

We differentiate this expression to obtain the RTD function E(t): d C (t ) E (t ) dt C0 step

(15)

the positive step is usually easier to carry out experimentally than the pulse test, and it has the additional advantage that the total amount of tracer in the feed over the period of the test does not have to be known as it does in the pulse test. One possible drawback in this technique is that it is sometimes difficult to maintain a constant tracer concentration in the feed. Obtained the RTD from this test also involves differentiation of data and present an additional and probably more serious drawback to the technique, because differentiation of data can, on occasion, lead to large errors. (The relevant available mathematical software, MathCAD for example [3], is recommended to execute the procedure of numerical differentiation of experimental data). A third problem lies with the large amount of tracer required for this test. If the tracer is very expensive, a pulse test is almost always used to minimize the cost. Sometimes E(t) is called the exit-age distribution function. If we regard the “age” of an atom as the time it has resided in the reaction environment, the E(t) concerns the age distributuin of the effluent stream. It is the most used of the distribution functionsconnected with reactor analysis because it characterizes the lengths of time various atoms spend at reaction conditions.

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RTD IN PACKED BED

Figure 5 illustrates typical RTDs resulting from different reactor situations. Figure 5 (a) and (b) correspond to nearly ideal PFRs and CSTRs respectively. In Figure 5 (c) one observes that a V v (i.e., early exit of fluid) and principal peak occurs at a time smaller than the space time also that fluid exits at a time greater than space-time τ. This curve is representative of the RTD for a packed-bed reactor with channeling and dead zones. One scenario by which this situation might occur is shown in Figure 5 (d). Figure 5 (e) shows the RTD for the CSTR in Figure 5 (f), which has dead zones and bypassing. The dead zone serves to reduce the effective reactor volume indicating that the active reactor volume is smaller than expected. The fraction of the exit stream that has resided in the reactor for a period of time shorter than a given value t is equal to the sum over all times less than t of E(t)Δt , or expressed continuously, t

E (t )dt 0

fraction of effluent which has been in reactor for less than time t

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F (t )

(16)

RTD IN PACKED BED

Figure5. (a) RTD for near plug-flow reactor; (b) RTD for near perfectly mixed CSTR; (c) RTD for packed-bed reactor with dead zones and channeling; (e) tank reactor with short-circuiting flow (bypass); (f) CSTR with dead zone.

Analogously, we have t

E (t )dt t

fraction of effluent which has been in reactor 1 F (t ) for longer than time t

(17)

Because t appears in the integration limits of these two expressions, Eq. (16) and (17) are both functions of time. Equation (17) defines a cumulative distribution function F(t). We can calculate F(t) at various times t from the area under the curve of an E(t) versus t plot. The typical shape of the F(t) curve is shown for a tracer response to a step input in Figure 6.

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RTD IN PACKED BED

Figure 6. Cumulative distribution curve, F(t). Here: 80% [F(t)] of the molecules spend 40 min. or less in the reactor, and 20% of the molecules [1 – F(t)] spend longer than 40 min. in the reactor.

The F curve is another function that has been defined as the normalized response to a particular input. Alternatively, Eq.(16) has been used as a definition of F(t), and it has been stated that as a result it can be obtained as the response to a positive-step tracer test. Sometimes the F curve is used in the same manner as the RTD in the modeling of chemical reactors. A parameter frequently used in analysis of ideal reactors is the space-time or average residence time τ, which is defined as being equal to V/v. It can be shown [1] that no matter what RTD exists for a particular reactor, ideal or non-ideal, this nominal holding time, τ, is equal to the mean residence time, tm. As is the case with other variables described by distribution functions, the mean value of the variable is equal to the first moment of the RTD function, E(t). Thus the mean residence time is tE (t )dt tm

tC (t )dt

0

0

tE (t )dt E (t )dt

0

C (t )dt

0

t i Ci t i Ci t i

(18)

0

It is very common to compare RTDs by using their moments instead of trying to compare their entire distributions. For this purpose, three moments are normally used. The first is the mean residence time. The second moment commonly used is taken about the mean and is called the variance, or square of the standard deviation. It is defined by 2

(t t m ) 2 E (t )dt 0

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(19)

RTD IN PACKED BED

alternatively (t t m ) 2 C (t )dt 2

(ti

0

t m ) 2 Ci t i

(20)

Ci t i

C (t )dt 0

The magnitude of this moment is an indication of the „spread‟ of the distribution; the greater the value of this moment, the greater a distribution‟s spread. The third moment is also taken about the mean and is related to the skewness. The skewness is defined by 1 (21) s3 (t t m ) 3 E (t )dt 3/ 2 0

The magnitude of this moment measures the extent that a distribution is skewed in one direction or another in reference to the mean. Rigorously, for complete description of a distribution, all moments must be determined. Practically, these three (tm, σ2, s3) are usually sufficient for a reasonable characterization of an RTD. Calculations of mean residence time and variance for experimental data from above example (Table 1) give the following: 14

tm

14

tE (t )dt

5.13 min . ,

0

2

(t t m ) 2 E (t )dt

6.06 min 2 ,

2.46 min .

0

(MathCAD package has been used for numerical integration; E(t) being expressed by cubic spline interpolation). Frequently, a normalized RTD E(Θ) is used instead of E(t). Here time is measured in terms of mean residence time Θ=t/τ, then (22) E( ) E(t ) 2 Correspondently, the dispersion coefficient is introduced as 2 2 2

(23)

Models are useful for representing flow in real vessel, for scale up, and for diagnosing poor flow. There are different kinds of models depending on whether flow is close to plug, mixed, or somewhere in between. The chart from Figure 7 points out which model should be used to represent a given setup if it is uncertain.

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RTD IN PACKED BED

Figure 7 Map showing which flow models should be used in any situation.

Figure 8. The spreading of tracer according to the dispersion model.

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RTD IN PACKED BED

Suppose an ideal pulse of tracer is introduced into the fluid entering a reactor. The pulse spreads as it passes through the vessel, and to characterize the spreading according to dispersion model Figure 8), we assume a diffusion-like process superimposed on plug flow. We call this dispersion or longitudinal dispersion to distinguish it from molecular diffusion. The dispersion coefficient D (m2/s) represent this spreading process. Thus large D means rapid spreading of the tracer curve small D means slow spreading D = 0 means no spreading, hence plug flow Also

D uL

is the dimensionless group characterizing the spread in the whole vessel. Levenspiel

[2} suggested calling

D as a vessel dispersion number and uL

D as an intensity (degree) of ud

axial dispersion. (Note it is not recommended to call the reciprocal of this group

uL as the Peclet number defined D

uL . The difference rests in the use of D in place of D (molecular diffusion coefficient) hence, D these group have completely different meanings.) In dimensionless form where z = (ut + x )/L and Θ = t/τ = tu/L, the basic differential equation representing this dispersion model is 2 C D C C (24) 2 uL z z where the vessel dispersion number is the parameter that measures the extent of axial dispersion. Thus D 0 negligible dispersion, hence plug flow uL D large dispersion, hence mixed flow uL The dispersion model usually represents quite satisfactory flow that deviates not too greatly from plug flow, thus real packed bed and tubes.

as

Case D/uL < 0.01. When an idealized pulse is imposed fitting the dispersion model for small extents of dispersion, D/uL < 0.01, results in the following family of equations: E E

1

E

4 (D / uL)

u3 exp 4 DL

tm

Updated January 2013 by Asnizam Helmy

exp

( L ut ) 2 4DL / u

V v

L u

12

(1 )2 4(D / uL)

(25) (26) (27)

RTD IN PACKED BED 2 2

D uL

2

2

or

2

2

DL U3

(28)

Case D/uL > 0.01, closed vessel/open vessel. For the large deviations from plug flow, D/uL > 0.01, here the pulse response is broad and it passes the measurement point slowly enough that it changes shape – it spreads – as it being measured. This gives a nonsymmetrical E curve. An additional complication enters the picture for large D/uL : what happens right at the entrance and exit of the vessel strongly affects the shape of the tracer curve as well as the relationship between the parameters of the curve and D/uL . Let us consider two types of boundary conditions: either the flow is undisturbed as it passes the entrance and exit boundaries (we call it open boundary conditions), or you have plug flow outside the vessel up to the boundaries we call this the closed boundary conditions). In all cases D/uL is evaluated from the parameters of the trace curves; however each curve has its own mathematics. Closed vessel. For the closed vessel situation an analytical expression for the E curve is not available. However the curve can be constructed by numerical methods, or its mean and variance can be evaluated exactly as tm

2

V , v

2 2

2

D uL

2

D uL

2

1 e

uL / D

(29)

Open vessel (00). This represents a convenient and commonly used experimental device, a section of long pipe, a fixed-bed tubular reactor, etc. It also happens to be the only physical situation (besides small D/uL ) where the analytical expression for the E curve is not too complex:

E

, 00

1 exp 4 (D / uL)

u ( L ut ) 2 exp 4Dt 4 Dt V D t m,00 1 2 v uL

E00

2

t

Updated January 2013 by Asnizam Helmy

(1 )2 4 (D / uL)

2 00 2 m

2

D D 8 uL uL

13

(30) (31) (32)

2

(33)

RTD IN PACKED BED

3.0

METHODOLOGY The unit consists of the followings: a)

Reactor A column made of borosilicate glass packed with 8 x 8mm Raschig rings. Column OD: 100 mm; ID: 82 mm; Height: 1,500 mm. Top and bottom caps made of stainless steel fitted with appropriate inlet and outlet ports. A differential pressure tapping is also provided on both caps.

b)

Feed Tank 20-L cylindrical tank made of stainless steel comes with a circulation pump. The tank is fitted with a level switch to protect the pump from dry run.

c)

Dosing Tank 20-L cylindrical tank made of stainless steels a metering pump.

d)

Waste Tank 50-L rectangular tank made of stainless steel.

e)

Instrumentations Air Flowmeters: Range : 0 to 50 LPM; 0 to 200 LPM Output : 0 to 5 VDC Display : LCD digital display Liquid Flowmeter: Range : Output : Display : Conductivity Meter: Sensor Range : No. of Sensors : Output : Display :

g)

0 to 5 LPM 0 to 5 VDC LCD digital display 0 to 200 mS/cm 2 (CT1, CT2) 4 to 20 mA conductivity controller with digital display for each sensor mounted on the control panel

Data Acquisition System The Data Acquisition System consists of a personal computer, ADC modules and instrumentations for measuring the process parameters. A flowmeter with 0 to 5 VDC output signal is supplied for feed flowrate measurement. Conductivity sensors with controller are provided for monitoring the tracer concentration in each reactor. All analog signals from the sensors will be converted by the ADC modules into digital signals before being sent to the personal computer for display and manipulation.

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RTD IN PACKED BED

Figure 1. Process Diagram for RTD Studies in Tubular Reactor (BP 112).

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RTD IN PACKED BED

EXPERIMENTAL PROCEDURES GENERAL START-UP PROCEDURE 1.

Perform a quick inspection to make sure that the equipment is in proper working condition.

2.

Check that all valves are initially closed.

3.

Open valve V13 to fill up the feed tank T1 with de-ionized water.

4.

Prepare 10 liter of 0.2M NaCl solution in dosing tank T2. Record the conductivity reading for this solution.

5.

Flush the system with de-ionized water until no traces of salt is detected.

6.

Switch on the main power on the control panel. Note: For operations with SOLDAS Data Acquisition System, switch on the computer and run the Data Acquisitions System (DAS) software. Refer to DAS operating procedure.

7.

Ensure the compressed air supply is on. Set the pressure regulator to about 2 bar.

8.

The equipment is now ready to be run.

OPERATING MODES: There are two modes of operations: 1.

Counter-current mode: The liquid stream is flowing downward from top of the column while the gas stream is flowing upward from bottom of the column. The pulse or step input tracer is injected at the top of the column.

2.

Co-current mode: Both the liquid and gas streams are flowing upward from bottom of the column. The pulse or step input tracer is injected at the bottom of the column.

Note: Refer to the notes at the end of the experimental procedure for the TASK list.

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RTD IN PACKED BED

Experiment A: The effect of step change input In this experiment a step change input would be introduced and the progression of the tracer will be monitored via the conductivity measurements. a) Counter-current Mode Procedures: 1.

Perform the general start-up procedure.

2.

Set the valves appropriately for counter-current mode: Valves V3, V5 and V10 remain closed.

3.

Open valve V1 and switch on pump P1. Fill up the column with de-ionized water to packing height. Note: The water level must be maintained throughout the experiment. Use valve V4 to adjust the level if necessary.

4.

Adjust valve V1 to obtain a liquid flowrate of 500 ml/min.

5.

Open valve V6. Open valve V8 to obtain a gas flow rate of 1.0 L min-1.

6.

Observe the conductivity reading of CT1 and let it stabilizes at low value.

7.

Switch on dosing pump P2. Open valve V14 and bleed off any air trapped in the tubing.

8.

Close valve V14. Open valve V9 and start timer simultaneously. Record conductivity reading CT1 at 1 min interval.

9.

Continue recording until conductivity reading is constant.

10.

Repeat the experiment with gas flow rate of 2.0 L min -1. Ensure that the system is flushed with de-ionized water until no traces of salt is detected.

11.

Stop the experiment and drain out all liquid from the system.

Note: For operations with SOLDAS Data Acquisition System, refer to the DAS operating procedure. In step 8, click the START button. Conductivity values will be recorded automatically and a table will be generated. b) Co-current Mode Procedures: 1.

Perform the general start-up procedure.

2.

Set the valves appropriately for co-current mode: Valves V2, V4 and V9 remain closed. Open valves V3 and V5.

3.

Switch on pump P1. Open and adjust valve V1 to obtain a liquid flowrate of 500 ml/min.

4.

Open valve V6. Open valve V8 to obtain a gas flowrate of 1 Lmin-1.

5.

Observe the conductivity reading of CT2 and let it stabilizes at low value.

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RTD IN PACKED BED

6.

Switch on dosing pump P2. Open valve V15 and bleed off any air trapped in the tubing.

7.

Close valve V15. Open valve V10 and start timer simultaneously. Record conductivity reading CT2 at 1 min interval.

8.

Continue recording until conductivity reading is constant.

9.

Repeat the experiment with gas flow rate of 2.0 L min-1. Ensure that the system is flushed with de-ionized water until no traces of salt is detected.

10.

Stop the experiment and drain out all liquid from the system.

Note: For operations with SOLDAS Data Acquisition System, refer to the DAS operating procedure. In step 7, click the START button. Conductivity values will be recorded automatically and a table will be generated. Results: COUNTER-CURRENT MODE

CO-CURRENT MODE

Liquid Flowrate:

L min-1

Liquid Flowrate:

L min-1

Air Flowrate:

L min-1

Air Flowrate:

L min-1

Time [min]

CT1 [ s/cm]

Time [min]

0

0

1

1

2

2

3

3

4

4

.

.

.

.

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CT2 [ s/cm]

RTD IN PACKED BED

Experiment B: The effect of pulse input. In this experiment a pulse input would be introduced and the progression of the tracer will be monitored via the conductivity measurements. a) Counter-current Mode Procedures: 1.

Perform the general start-up procedure.

2.

Set the valves appropriately for counter-current mode: Valves V3, V5 and V10 remain closed.

3.

Open valve V1 and switch on pump P1. Fill up the column with de-ionized water to packing height. Note: The water level must be maintained throughout the experiment. Use valve V4 to adjust the level if necessary.

4.

Adjust valve V1 to obtain a liquid flowrate of 500 ml/min.

5.

Open valve V6. Open valve V8 to obtain a gas flowrate of 1.0 L min-1.

6.

Observe the conductivity reading of CT1 and let it stabilizes at low value.

7.

Switch on dosing pump P2. Open valve V14 and bleed off any air trapped in the tubing.

8.

Close valve V14. Open valve V9 and start timer simultaneously. Record conductivity reading CT1 at 1 min interval.

9.

Let dosing pump P2 run for 2 minutes. Close valve V9 and stop pump P2.

10.

Continue recording until conductivity reading is constant.

11.

Repeat the experiment with gas flow rate of 2.0 L min-1. Ensure that the system is flushed with de-ionized water until no traces of salt is detected.

12.

Stop the experiment and drain out all liquid from the system.

Note: For operations with SOLDAS Data Acquisition System, refer to the DAS operating procedure. In step 8, click the START button. Conductivity values will be recorded automatically and a table will be generated. b)

Co-current Mode

Procedures: 1.

Perform the general start-up procedure.

2.

Set the valves appropriately for co-current mode: Valves V2, V4 and V9 remain closed. Open valves V3 and V5.

3.

Switch on pump P1. Open and adjust valve V1 to obtain a liquid flowrate of 500 ml/min.

4.

Open valve V6. Open valve V8 to obtain a gas flowrate of 10

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RTD IN PACKED BED

5.

Observe the conductivity reading of CT2 and let it stabilizes at low value.

6.

Switch on dosing pump P2. Open valve V15 and bleed off any air trapped in the tubing.

7.

Close valve V15. Open valve V10 and start timer simultaneously. Record conductivity reading CT1 at 1 min interval.

8.

Let dosing pump P2 run for 2 minutes. Close valve V10 and stop pump P2.

9.

Continue recording until conductivity reading is constant.

10.

Stop the experiment and drain out all liquid from the system.

Note: For operations with SOLDAS Data Acquisition System, refer to the DAS operating procedure. In step 7, click the START button. Conductivity values will be recorded automatically and a table will be generated. Results: COUNTER-CURRENT MODE

CO-CURRENT MODE

Liquid Flowrate:

L min-1

Liquid Flowrate:

L min-1

Air Flowrate:

L min-1

Air Flowrate:

L min-1

Time [min]

CT1 [ s/cm]

Time [min]

0

0

1

1

2

2

3

3

4

4

.

.

.

.

CT2 [ s/cm]

Task: 1. For all experiment above, carry out the following task: a. Obtain the E(t) curve b. Determine the mean residence time, tm, of the system. c. Determine the variance, 2, and the skewness, s3, of the system. d. Does your system has negligible dispersion or large dispersion? (Hint: Give your comment based on the value of the dimensionless group, D/uL)

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RTD IN PACKED BED

4.

REFERENCES 1.0 2.0 3.0 4.0

5.

6.

Levenspiel, O., Chemical Reaction Engineering, John Wiley, 1972. Fogler, H.S., Elements of Chemical Reaction Engineering, 3rd Edition, Prentice Hall PTR, 1999. Smith, J.M., Chemical Engineering Kinetics, McGraw Hill, 1981. Astarita, G., Mass Transfer with Chemical Reaction, Elsevier, 1967.

MAINTENANCE 1.

After each experiment, drain off any liquids from the reactor and make sure that the reactor and tubings are cleaned properly. Flush the system with de-ionized water until no traces of salt are detected.

2.

Dispose all liquids immediately after each experiment. Do not leave any solution or waste in the tanks over a long period of time.

3.

Wipe off any spillage from the unit immediately.

SAFETY PRECAUTIONS 1.

Always observe all safety precautions in laboratory.

2.

Always wear protective clothing, shoes, helmet and goggles throughout the laboratory session.

3.

Always run the experiment after fully understand the equipment and procedures.

4.

Always plug in all cables into appropriate sockets before switching on the main power on the control panel. Inspect all cables for any damage to avoid electrical shock. Replace if necessary.

5.

Inspect the unit, including tubings and fittings, periodically for leakage and worn out.

Updated January 2013 by Asnizam Helmy

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