University Azzawiya

Faculty of oil and gas

Department of Chemical Engineering

Experiment name:

plug flow reactor, Tubular reactor

Name of article:-

Laboratory standardized processes "II"

Preparation:-

Basim al arif Saeed Al Zawiley 61212234

Bashir Arab Mahdi 61212238

Mohammed Juma Munis 61212456

Supervised by:

D. Ibrahim Howeidi. D Riad Mahfouz.

Date of procedure:

2016\6\10

spring 2016
 ‫‪Contents‬‬

‫‪1.0‬ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪INTRODUCTION‬‬

‫‪ 1.1.0‬ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ‪PLUG FLOW REACTOR‬‬

‫‪1.1.1‬ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪Object‬‬

‫‪ 1.1.2‬ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪Theory‬‬

‫‪ 1.1.3‬ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪Apparatus‬‬

‫‪ 2.0‬ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪EQUIPMENT DESCRIPTION‬‬

‫‪ 2.1‬ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪The Reactor Vessel‬‬

‫‪ 2.2‬ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ــــــــــــــــــــــــــ‪Flow of materials‬‬

‫‪ 3.0‬ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪Operating the CET MkII‬‬

‫‪ 4.1‬ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪Reactor dimensions‬‬

‫‪ 5.0‬ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪EXPERIMENTAL PROCEDURES‬‬

‫‪ 6.0‬ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪Equations‬‬

‫‪ 7.0‬ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪Calculation‬‬

‫‪ 8.0‬ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪The diagram‬‬

‫‪ 9.0‬ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪Conclusion‬‬

‫‪ 10.0‬ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ ‪References‬‬
1.0 INTRODUCTION

Tubular reactors are often used when continuous operation is required

but without backmixing
of products and reactants.
The Armfield CET MkII Tubular Reactor is specially designed to allow
detailed study
of this important process. It is one of three reactor types which are
interchangeable on
the Reactor Service Unit (CEX MkII), the others being CEM MkII -
Continuous Stirred
Tank Reactor and CEB MkII - Batch Reactor.
Reactions are monitored by conductivity probe as the conductivity of the
solution
changes with conversion of the reactants to product. This means that
the inaccurate and
inconvenient process of titration, which was formally used to monitor
the reaction
progress, is no longer necessary.
CEX fitted

1.1.0 PLUG FLOW REACTOR

Keywords: Tubular reactor, plug flow reactor, saponification, integral
method, differential method.

1.1.1 Object
The object of this experiment is to study the behaviour of a plug-flow
reactor by performing a series of experiments on the saponification of
ethyl acetate.

1.1.2 Theory
In a tubular reactor, the feed enters at one end of a cylindrical tube and
the product stream leaves at the other end. The long tube and the lack
of provision for stirring prevents complete mixing of the fluid in the
tube. Hence the properties of the flowing stream will vary from one
point to another, namely in both radial and axial directions.
In the ideal tubular reactor, which is called the “plug flow” reactor,
specific assumptions are made about the extent of mixing:
1. no mixing in the axial direction, i.e., the direction of flow
2. complete mixing in the radial direction
3. a uniform velocity profile across the radius.

The absence of longitudinal mixing is the special characteristics of this

type of reactor. It is an assumption at the opposite extreme from the
complete mixing assumption of the ideal stirred tank reactor.
The validity of the assumptions will depend on the geometry of the
reactor and the flow conditions. Deviations, which are frequent but not
always important, are of two kinds:
1. mixing in longitudinal direction due to vortices and turbulence
2. incomplete mixing in radial direction in laminar flow conditions

1.1.3 Apparatus
The apparatus used in this experiment is shown in Figures (A)and Figures
(B):

Figures (B) Figures (A)

2.0 EQUIPMENT DESCRIPTION

2.1 The Reactor Vessel

The reactor vessel (1) is set on a baseplate (14) which is designed to be
located on the
four studs of the CEX service unit and then secured by thumbnuts (15).
The positioning
of the reactor on the service unit is illustrated. The reactor is positioned
on the service
unit with the non-return valve sited on the left and towards the
rear.
The tubular reactor in which the chemical reaction takes place is a
flexible coil (4)
wound around an acrylic former. Total volume of the reactor coil is 0.4 L.
In order to maintain a constant temperature throughout the reactor coil,
the coil bundle
is submerged in circulating water which is automatically maintained at a
pre-selected
CET TUBULAR REACTOR
8
temperature by the temperature controller (TIC) in the console. The
actual temperature
of the circulating water and therefore the reactants is relayed to the
controller by a
sensing probe (TS) which is held in gland (8) in the lid. Water enters from
the circulator
at the non-return valve (11) - this prevents water draining back through
the priming
vessel of the circulator when the pump is stopped. Water leaves the
reactor at overflow
(12) and returns to the circulator.

A filling plug (17) is provided on the top of the reactor vessel to allow the
vessel to be
filled with clean water. This plug (with sealing washer) must be fitted
when the hot
water circulator on the CEX service unit is in operation.
Sockets in the side of the console pod of the service unit are provided to
connect the
conductivity probe and temperature sensor to the instrumentation in
the console. These
are of a different size so that the probes cannot be wrongly connected.
When not in use, the reactor can be drained using valve (13) in the
base

2.2 Flow of materials

Reactants are pumped from the two feed tanks by the peristaltic pumps
and enter the
reactor through connectors (6) and (7) in the lid of the vessel. Each
reactant is preheated
by heat transfer coils (2) and (3) before being blended together in “T”
fitting (5).
The reactants pass up through the reactor coil and leave the reactor
vessel through the
conductivity probe housing (16). This housing allows the
conductivity probe (CP) to be

held in the stream of reactants emerging from the reactor. Flexible

tubing from the hose
nozzle (10) is used to guide the reactants to drain.

3.0 Operating the CET MkII

Temperature in the reactor is controlled by circulating heating or cooling

liquid through
the interior of the reactor (13).
The volumetric ratio in which the reactants are mixed is defined by the
relative flow
rates of the two pumps. If the pumps are operated at the same flow rate
then the
reactants are mixed in equal volumes.
The residence time in the reactor is defined by the total flow rates of the
two feed
pumps. The total volume of the reactor coil is approximately 400 mL.
Dividing this
volume by the combined flow rates of the feed pumps in mL/s will yield
the residence
time in seconds.
The extent of conversion of the reactants is determined from the
conductivity, which is
measured by the conductivity probe sited in the housing (16) where the
liquid stream
exits the reactor. It is important that the probe is inserted into the
housing with the
electrode access holes in the glass surround in line with the flow.
4.0 SPECIFICATIONS

4.1 Reactor dimensions:

Pre-heat coils (each):
Total length: 1.2m
Internal diam: 4.9mm
Total vol of coil: 0.02L
Reactor coil:
Total length: 20.9m
Internal diam: 5.0mm
Total vol of coil: 0.41L

5.0 EXPERIMENTAL PROCEDURES

1:The Armfield Continuous Tubular Flow Reactor is designed to

demonstrate the mechanism of a chemical reaction in such a reactor as
well as the effects of varying the process conditions such as reaction
temperature, reactant concentration, feed rate etc.
2: The reaction chosen is the saponification of ethyl acetate by sodium
hydroxide as it can be carried out under safe conditions of temperature
and pressure and is well documented.
3: Although it may be possible to carry out demonstrations using other
chemicals it is not advisable as the materials of construction of the
reactor may not be compatible.
4: Before carrying out reactions involving any other reagents please
refer to Armfield Ltd. for advice.
5: DILUTION OF ETHYL ACETATE FOR USE WITH CET MKII REACTOR
Armfield recommends the use of a 0.1M solution of Ethyl Acetate in the
CET MkII
reactor. This should be made by diluting concentrated Ethyl Acetate as
follows:

Therefore add 9.79 ml of concentrated Ethyl Acetate to 900 ml of

deionised or distilled water.

Shake the mixture vigorously until the two liquids have mixed. Add
further water to make up the final volume to 1000 ml.
Note: The practice of making a strong solution (e.g. 1M) then further
diluting this to the required concentration (e.g. 0.1M) cannot be applied
when using Ethyl Acetate. The required dilution should be made directly
as stated above.

DILUTION OF SODIUM HYDROXIDE FOR USE WITH CET MKII

REACTOR

Armfield recommends the use of a 0.1M solution of Sodium Hydroxide in

the CET MkII reactor. This may be made by adding 4.0g of NaOH to

960ml of deionised water then making up the solution to 1000ml.

6.0 Equations:-

For a tubular reactor, the mass balance for a reactant a is represented by

For the reaction between ethyl acetate and sodium hydroxide, it is equi-
molar and is second order in nature, thus

r = k × a ×b

where k is the kinetic rate constant.

Arranging for initial concentrations of a and b to be equal r = k × a2

Integrating,
Fractional conversion,

Therefore,

𝑋𝑎
Thus the conversion factor is directly proportional to tR the
1−𝑋𝑎
residence time for constant reaction temperatures (T).

7.0 Calculation:-

𝐶𝑎 =19.56K– 0.1015
𝐴𝑐 ∗𝐿
𝑡𝑅= 𝐹𝐴
 K(s) 𝐶𝑎 (mol) 𝐹𝐴 (ml/min) 𝑡𝑅
0.148 2.79338 27 1.51719E-05
0.151 2.85206 37 1.10714E-05
0.156 2.94986 68 6.02412E-06

1 1 1 𝐴𝑐 ∗𝐿
[ - ]=
𝑘 𝐶 𝐶
𝐴 𝐴0 𝐹𝐴
𝑋𝐴
K* 𝑡𝑅 *𝐶𝐴0 =
1−𝑋𝐴

𝑡𝑅 K (𝑋𝐴 /1-𝑋𝐴 )
1.51719E-05 24471.67948 1.037128
1.10714E-05 32820.21854 1.036336
6.02412E-06 58248.26978 1.035089

8.0 The diagram:-

The diagram between 𝑡𝑅 and (𝑋𝐴 /1-𝑋𝐴 ):-

9.0 Conclusion:-

plug flow reactor, Tubular reactor In a plug ow reactor reactants are fed
to the reactor at the inlet and the products are removed from the
reactor at the outlet. The reaction takes place within the reactor as the
reacting mixture moves through the pipe. In an ideal plug ow reactor,
the reacting mixture is assumed to move as a plug and its properties are
assumed to be uniformly distributed across the cross-section of the
reactor.

Minimal pilot-scale data are available to use to evaluate tubular

reactors. However, bench-
scale data raise doubt about their performance treating most DOE mixed
wastes because of
corrosion and deposition that would lead to operational problems and
high costs.
At present there does not appear to be an economic means of
controlling corrosion in
tubular reactors for wastes with high levels of acid precursors. The high
chloride content of some
DOE wastes makes feed dilution economically infeasible as a means of
corrosion control.
10.0 References:-

1. Denbihh, K. G., and J. C. R. Turner, Chemical Reactor Theory, 2nd

edition, Cambridge University, 1971.

2. Levenspiel, O., Chemical Reaction Engineering, 2nd edition, John Wiley

and Sons, 1972.

3. Perry, R. H., and D. Green, Perry’s Chemical Engineer’s Handbook, 6th

edition, McGraw-Hill, 1984.

4. Smith, J. M., Chemical Engineering Kinetics, 3rd edition, McGraw-Hill,

1981.