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LABORATORY MANUAL
September 2008
CONTENTS
4. Heat Transfer double tube and shell and tube heat exchangers.
Ensure that you read through each experiment prior to commencement and discuss with
Laboratory reports must be written following the completion of each experiment and
Title
equipment, materials)
Conclusions
References
Safety information
Refer to CRA and MSDS
Hazard identification and risk assessment
Chemical Hazard class Hazard Risk phrases
identification and
risks
Calcium carbonate Xi Xi R 37/38, 41
Precautions
Avoid inhalation of dust
Waste
Calcium carbonate must be dried and reused.
Spillage
Clear up and dispose of as non-hazardous waste
1. Introduction
The integrated form of the filtration equation for constant pressure filtration (assuming an
incompressible filter cake) gives:
V2 + AVL = A2 Pt
2 v rv
where
v= Volume of cake
Volume of filtrate
L= filter cake equivalent thickness to cloth or paper (m)
The terms L and rv are termed the filtration constants and may be determined by
v
Another parameter of interest is the fractional porosity of the cake, e, and this may be
obtained from measuring cake volume and calculating particle volume from specific
gravity. In summary, the objective of the experiment is to operate a laboratory scale
filtration at constant pressure, estimate the filtration constants, calculate r, L and use the
filtration constants to carry out a preliminary design for a filter press.
2. Experimental Procedure
2.1 Equipment
As assembled.
2.2 Method
Make up a suspension of 5%w/w CaCO3 (or CaSO4. 2H2O as available) in water and
place in reservoir. Start the stirrer motor. Start the vacuum pump with stopcock A closed
and using stopcock B obtain a steady pressure reading of between 50 and 60 cm Hg (i.e.
between 67,763 and 78,947 Nm-2) to give a steady filtrate flowrate. Use safety screen
provided. Maintain this pressure at a steady reading. Fill the funnel about half-way, at
the same time opening A fully. Adjust B to obtain a steady pressure reading as before.
Maintain the level in the funnel as constant as possible and take filtrate volume readings
at suitable time intervals i.e. try and include at least five readings for each run. Do not
exceed the capacity of the filtrate vessel. Record final filtrate volume. Repeat the
experiment twice more, for each run changing the P to give sensible filtrate flowrates.
Record P values Dry filter cakes in drying oven to constant weight. Record weight,
diameter and thickness of each filter cake.
Retain filter cakes for further use.
3. Calculations
Use the rv, and L average values obtained to carry out design calculation in 3.2
v
4. Report
The following should be included:
4.1 Comments on control of process, appearance of filter cake etc.
Note: (i) All calculations and units of measurement are to be clearly shown.
(ii) S.I. units are to be used throughout.
Modelling of Chemical Processes Separation Processes (I)
Introduction
This practical is concerned with the use of Aspen Plus as a modeling tool for the
operation of continuous fractional distillation.
Objectives
1. To obtain operating results for a continuous fractional distillation system.
2. To perform a sensitivity analysis for a continuous fractional distillation system.
3. To develop a process flowsheet.
4. To meet a process design specification.
Method
Complete the tutorials in Building and running a process model version 11 as follows:
When the tutorials have been completed build and run a process simulation model using
the following process parameters/system specification:
Feed: 10 kmol h-1 benzene/toluene
Feed composition: 60 mol %toluene/40 mol % benzene (xf = 0.4)
Reflux ratio (R): 4
Feed temperature: 95oC
Theoretical plates: 7 (N)
Distillate flow: 3.75 kmol h-1
Feed stage: 4
Pressure: 1 atm.
Obtain operating results for the above system. Choose Template/Metric units for your
model. Use the RadFrac unit operation model and the UNIFAC activity coefficient
model or IDEAL model. Obtain operating results for a system with 12 stages instead of
7 (N = 12).
Perform a sensitivity analysis on the above system (variation of xd, distillate composition,
with R)
Develop the process flowsheet as described in the tutorial.
Meet a process design specification (say xd = 0.90).
Save results on disc. Print results and include with your report.
Reference
Building and Running a Process Model Version 11.
Modeling of Industrial Chemical Processes Separation Processes (II)
Introduction
This practical is concerned with the use of Aspen Plus as a modeling tool for the
operation of liquid-liquid extraction.
1 3
L2
48 kmol s-1 water
Method
Complete the tutorials in Building and running a process model version 11 as follows:
When the tutorials have been completed build and run a process simulation model using
the following process parameters/system specification:
System specifications.
solvent: 48 kmol s-1 water.
feed: 7.69kmol s-1 benzene/2.31kmol s-1 acetone.
T: 298 K
P: 101325 Pa. (1 atm)
N (stages): 3
Safety information
Precautions
sand is used in this experiment
oven and contents are hot!
Waste
Sand must be dried and reused.
Spillage
Sweep up and dispose of as non-hazardous waste
Oven
Avoid direct contact with any hot item, use tong to manipulate hot apparatus or
use special gloves.
Objectives
Experimental determination of the rate of drying curve for solid, at constant drying
conditions (constant air flow, temperature and humidity).The experiment is carried out in
a batch dryer and heat is supplied by direct contact with heated air at atmospheric
pressure. The drying oven is operated at three temperatures 100, 110 and 120 deg. cent.
Important Definitions
Critical Moisture Content of a solid (Xc): Is the solid moisture content attained,
during the drying process, when the entire surface of the solid is no longer wetted.
The rate of drying R is defined as the mass of liquid evaporated by unit time and by
unit of exposed surface area for drying. It can be mathematically expressed by
S dX
R= (1)
A dt
Where
To experimentally determine the rate of drying for a given material (case study sand), a
sample is placed in a dryer and under constant drying conditions, the loss in weight of
moisture during the drying process is determined at constant time intervals.
With the data obtained from the batch experiment, a plot of the solid moisture content
X versus time can be made (Figure 1). From this plot, the rate of drying curve can be
obtained by measuring the slopes of the tangents drawn to the curve, which give the
values of dX/dt at given values of t. The drying rate R is calculated for each point using
equation (1). The drying rate curve is obtained by plotting R versus the solid moisture
content X as in figure 2.
The plot of the rate of drying curve can presents several shapes but generally the two
major points constant and falling rate period are present. At time zero the initial
moisture content of the solid is shown at point A or A depending on the solid
temperature. At point B the surface temperature as attained its equilibrium value and the
constant rate period starts. This period continues as long as the water is supplied to the
surface as fast as it evaporates. At point C, the solid critical moisture content Xc is
attained. At this point there is no insufficient water on the surface to maintain a
continuous film of water and the first falling rate period starts. The wetted area of the
solid continually decreases until the surface is totally dry at point D. At this point begins
the second falling rate period, that continues until the equilibrium moisture content of the
solid is reached, at point E.
Figure1: solid moisture content X versus time for constant drying conditions
Figure2: drying rate R versus solid moisture content X for constant drying
conditions
Date : /./
Surface area.. m2
Practical Formulas
W Ws
X = I
Ws
Ws dX
R = II
A dt
where
W = weight of total solid (kg)
Ws = weight of dry solid (kg)
References
Geankoplis, Christie, J (1983). Transport Processes and Unit Operations, 2nd ed.
Massachusetts, Allyn and Bacon. Inc., pg 508-552
Spray drying
The aims of this experiment are:
To investigate the performance of the spray drier
To investigate parameters that control the spray drying process
To examine and study spray dried product properties e.g. particle size and shape
See operating manual for experimental details.
Drying of solids fluid bed drying
Operating method:
1- Determine the optimum bed depth
The optimum bed depth is that which can be fluidised at the required temperature by
relative high air velocity. The optimum bed depth will vary appreciably with the
material-an initial bed depth of about 75mm is typical.
1- Remove any excess water from the solid sample by decanting and / or using a
filter pump.
2- Place the sample of material in the tub to an appropriate bed depth. Weigh the tub
alone then with the material.
3- Locating the sealing ring into the groove.
4- Switch on the mains supply and select the drying temperature required (select
three temperatures).
5- Note the wet and dry bulb temperatures of the inlet air to the fan and outlet air
from the fluidised bed.
6- Weigh the tub with material at 2 minutes intervals for about 15 minutes (or as
long as it takes to attain constant weight) recording the wet and dry temperature
before removing the tub for weighing. Then weigh at 5 minutes intervals until
constant weigh is achieved indicating that the equilibrium moisture content has
been reached. Record the drying time and moisture content.
From these results plot drying curves of moisture content vs time and drying rate vs
moisture content.
Calculation of Heat Transfer Coefficient
Heat lost by entering gas = heat transferred to solids to vaporise the liquid
where
dw/ dt = constant drying rate, kg.s -1
L = latent heat of vaporisation, J.kg -1
H = heat transfer coefficient, W.m -2. oC-1
A = surface area, m2
o
Ta = dry bulb air temperature, C
o
Ts = wet bulb air temperature, C
Wo = initial moisture content, kg water/kg dry solid
Wc = critical moisture content at end of constant rate period, kg water/kg dry solid
t = constant rate drying time, s
Heat transfer/Heat exchangers
This aim of this practical is to examine the performance of a double tube heat exchanger
and a shell and tube heat exchanger. Hot and cold water flow rates, hot water temperature
and mode of operation are varied and comparisons are made between the two types of
heat exchanger.
(see operating manual for details of procedures, observations and calculations)
Reactor experiments
Safety information
Refer to CRA and MSDS sheets
Hazard identification and risk assessment
Chemical Hazard class Hazard Risk phrases
identification and
risks
Sodium hydroxide C Causes severe burns R35
solution
Ethyl acetate F, Xi Highly flammable. R11, 36, 66, 67
Irritating to eyes.
Sodium acetate none none none
Ethanol F Highly flammable R11
Precautions
Avoid contact with sodium hydroxide solution. Wash with water.
Avoid contact with ethyl acetate. Wash with water.
Use sodium hydroxide solution and ethyl acetate solution in sealed containers.
No ignition sources.
Waste
Reactor contents may be diluted with water and washed down the laboratory sink
at the end of the experiment.
Spill
No ignition sources
Wear appropriate PPE
For ethyl acetate solution use spill kit
For sodium hydroxide solution dilute with water and clean up with suitable
absorbent material
Safety Information
Refer to CRA and MSDS sheets
Precautions
Waste
Reactor contents may be diluted with water and washed down the laboratory sink
at the end of the experiment.
Spill
No ignition sources
Wear appropriate PPE
For ethyl acetate solution use spill kit
For sodium hydroxide solution dilute with water and clean up with suitable
absorbent material
The reaction which takes place in the reactor is the alkaline hydrolysis of ethyl acetate.
The following equation shows this reaction:
This reaction is first order with respect to both sodium hydroxide and ethyl acetate, i.e.
the overall reaction order is second order. This reaction is carried out isothermally in a
batch reactor using equal concentrations and volumes of both reactants.
Assuming that the initial concentrations are equal and that the amount of reagent used up
after time (t) is (x) then the concentrations at time (t) are:
at time= 0 a a 0 0
at time=t ax ax x x
From the kinetic analysis of a general second order reaction it can be shown that:
k.t = x / a (a x ) (1)
Where k is the reaction rate constant and t is the time of reaction. Using notation from the
nomenclature at the end of procedure:
x = ao a1
Hence a plot of (ao a1 ) / ao . a1 against t gives straight line of gradient (slope) equal to k.
Both sodium hydroxide and sodium acetate contribute conductance to the reaction
solutions. The conductivity of the reacting solution in the reactor changes with the degree
of conversion and this provides a convenient method for monitoring the progress of the
reaction.
Note: definition of all symbols and units are presented later on page i at the end.
Method
1. Check the actual volume of the reactor, since the reactor volume can be varied.
The reactor volume is now set for 1100 cm3.
2. Set up water circulator if you need to circulate cold or hot water. Adjust the set
point of the temperature controller to 15 oC (or to any other required
temperature(s)). Switch the heat switch on if heating is required. Perform this
experiment at two temperatures (say 15 and 25 oC or other).
3. As the experiment involves the collection and storage of conductivity data, the
data output port in the console must be connected to the CEX-330 IFD (data
logger) interface and the computer as detailed in the instruction leaflet. Ensure
the conductivity probe and temperature sensor have been installed.
4. As the reactor volume is set at 1100 cm 3, carefully add to the reactor 550cm3 (or
other volume - see step 1 above) of 0.025M sodium hydroxide solution (or
other concentration) and 550cm3 0.025M ethyl acetate solution (always same
concentration and volume of sodium hydroxide). Cover the reactor with its cover.
Use 0.025M of both reactants.
6. For collection of conductivity data, it is advisable to set the data collection period
to, say, 45 minutes.
7. All data and results will be presented on the PC directly by the use of Armfield
soft ware supplied for this unit.
NOTE: Sometimes either the PC or the Armfield Data Logger CEX-330 IFD in the
laboratory may not be working; in this case you need to measure the
conductivity directly from the reactor service unit in time intervals of say 1
minute. In this case you need to perform the calculations by yourself to find
the value of k by using the relationships presented above.
It has been determined that the degree of conversion of the reagents affect the
conductivity of the reactor contents so that recording the conductivity with respect to
time using the Armfield Data Logger can be used to calculate the amount of conversion.
Interpretation of results
Having used the Armfield Data Logger CEX-303 IFD to record the conductivity of the
contents of the reactor over a period of the reaction, the conductivity measurements must
now be translated into degree of conversion of the constituents.
Both sodium hydroxide and sodium acetate contribute conductance to the reaction
solution whilst ethyl acetate and ethyl alcohol do not. The conductivity of a sodium
Page i
Exercises
2. Find the conversion that maximizes the output from the reactor and determine
what this is per annum assuming plant availability is 8,000h per annum.
Vapour liquid equilibrium curve and its application
Safety information
For further information refer to CRA and MSDS sheets
Hazard identification and risk assessment
Chemical Hazard Hazard identification and risks Risk
class phrases
methanol F, T Highly flammable. Toxic by inhalation, in contact R11, 23,
with skin and if swallowed. Toxic: danger of very 24, 25, 39
serious irreversible effects through inhalation, in
contact with skin and if swallowed.
isopropanol F, Xi Highly flammable. Irritating to eyes. Vapours may R11, 36,
cause drowsiness and diziness. 37
Precautions
Handling of methanol is carried out in the fume cupboard. All glassware, sample
bottles and other containers containing methanol must be sealed.
No ignition sources
Handling of isopropanol is carried out in the fume cupboard. All glassware,
sample bottles and other containers containing isopropanol must be sealed.
Avoid contact of methanol with skin. Use gloves if necessary.
All glassware contaminated with traces of methanol and isopropanol must be
washed in the fume cupboard.
Any skin contact with methanol or isopropanol should be washed with water.
Waste
Methanol and isopropanol waste must be put into the solvent waste container in
the fume cupboard.
Spills
Use spill kit and appropriate PPE to deal with large spillages.
Small spillages may be dealt with using gloves and a suitable absorbent material
which must then sealed in a suitable container and disposed of as hazardous
waste.
Further information: see MSDSs and chemical risk assessment.
INJ/DET 120
Initial 80
Final 80
Prograte 4
Range 102
Attenuation 24
Primary 2 kg cm-2
Carrier gas 1 0
Carrier gas 2 2
Hydrogen 1 0
Hydrogen 2 0.5
Air 0.5
Parameters (Para/enter)
WIDTH 5
DRIFT 0
T.DBL 0
ATTEN. 10
METHOD 2421
SPL.WT. 100
SLOPE 1000
MIN.AREA 1000
STOP.TM 655
SPEED 5
FORMAT 0
IS.WT 1
Fluid flow experiments
The aims of this experiment are: (1) to investigate the performance of various flow
measuring devices and (2) to investigate the flow through a pipe at high and low flow
rates.
(see operating manual for details)
Continuous column extraction (UOP 5)
Safety information
Refer to CRA and MSDS sheets
Hazard identification and risk assessment
Chemical Hazard Hazard identification and Risk
class risks phrases
111 - trichloroethane Xn, N Harmful by inhalation. R20, R59
propanoic acid C Causes burns R34
Leksol (n-propyl Xn Harmful by inhalation R20
bromide)
Precautions
Avoid skin contact with propanoic acid. Wash with water if contact.
111-trichloroethane must only be handled in a fume cupboard. Sample bottles and
other containers must be sealed. No open glassware containing 111-
trichloroethane must be left in the laboratory.
Avoid contact with Leksol. Do not breathe in vapours. Handle in a fume
cupboard.
Seal all containers containing Leksol.
Waste procedure
All 111-trichloroethane waste must be separated from water (lower layer) and
collected in the 111-trichloroethane waste container in the fume cupboard for
recovery.
Propanoic acid solutions may be diluted with water and washed down a laboratory
sink.
Leksol waste should be collected in a separate waste container, separated from
water and recovered.
Spill procedure
Spills of propanoic acid solutions may be neutralised with soda ash and
diluted with water and wiped up with absorbent paper or cloth. Rubber gloves
must be worn.
Spills of 111-trichloroethane must be dealt with by the laboratory technician
using a spill kit and respiratory protection. The laboratory should be
evacuated. Any solid waste resulting from the spill clean-up procedure must
be put in a sealed container and disposed of as hazardous waste.
Spills of Leksol must be dealt with by the laboratory technician using a spill
kit and respiratory protection. The laboratory should be evacuated. Any solid
waste resulting from the spill clean-up procedure must be put in a sealed
container and disposed of as hazardous waste.
Further information: MSDSs and chemical risk assessment available in the laboratory.
Precautions
No ignition sources
Avoid contact with skin. Wash off with water.
Waste procedures
Waste ethanol should be put into the solvent waste container in the laboratory
Ethanol/water mixtures should be diluted with water and washed down the
laboratory sink
Spills
Large spillages should be dealt with using a spill kit and appropriate PPE