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CHAPTER 1

INTRODUCTION

1.1 Background of Research

Nowadays, commercial and institutional buildings have become more complex and
more sophisticated. The traditional methods for building start-up and final acceptance
have proven inadequate and cannot be apply towards modern kind of building. The
increased complexity of building systems is a response to energy conservation
requirements, to the need for safer work environments, to demands for improved
indoor air quality and better comfort control. Distributed digital control systems help to
meet these needs but add so much in term of complexity. Thus, the entire process of
acquiring new facilities must also become more sophisticated in order to keep pace
with the complexity of new technologies and to get the required performance. (Rosaler,
2002)

Demand for commissioning services is increasing as the design and construction


communities require that projects are delivered completely functional, on time, at low
cost, and constructed to run in a highly efficient manner The Commissioning Process
helps to achieve all of these goals through review of design documents and
construction installation. A third party provider, independent of the design and
construction teams, can oversee the quality delivery of the project and provide the
Owner with an advocate that will serve the project through completion. (Lawry & Pons,
2013)

Project commissioning is the process of assuring that all systems and components of
a building or industrial plant are designed, installed, tested, operated, and maintained
according to the operational requirements of the owner or final client. A commissioning
process may be applied not only to new projects but also to existing units and systems
subject to expansion, renovation or revamping. In practice, the commissioning
process comprises the integrated application of a set of engineering techniques and
procedures to check, inspect and test every operational component of the project, from
individual functions, such as instruments and equipment, up to complex
amalgamations such as modules, subsystems and systems. (Rosaler, 2002)

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1.2 Problem Statement

The equipment that needed to be commissioned is Solteq Qvf model BP 121 is


under maintenance and cannot be operated. This is due to some problem occur for
the equipment. For the crystallization unit model BP 121 it cannot be operated due
piping broken and cannot be operated. There are also other problem that occur in the
equipment and the problem need to be troubleshoot. Then, the optimum parameter
for the crystallization unit need to be measured. This is because the parameter of the
production of salt is yet to be tested and being verified. So that the optimum parameter
for the equipment is desirable to achieve the maximum production with less energy
usage.

Plant modifications are an ongoing process throughout the life of any process plant.
Reasons for modification include efforts to improve reliability, production capacity,
quality, or productivity. Seamless incorporation is the key concern associated with the
installation of any new equipment in an operating plant due to the high cost of process
downtime. Several steps can be taken to minimise the risk associated with the
installation of new equipment such as hazard and operability studies, project
management, development of redundancy plans, and commissioning of the new
equipment. Of these, commissioning is an essential activity in many plant-modification
projects and has significant implications for project success. (Lawry & Pons, 2013)

1.3 Objectives of Research

To commission the crystallization equipment at lab pilot plant


To troubleshoot any problem related with crystallizer unit model BP121
To optimize parameter for crystallization of equipment (production of salt)

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1.4 Scope of Research
The equipment that needed to be commission and troubleshoot is the crystallization
unit model BP121. In this research, the main objective is to commission the equipment
and eliminate all the problem regarding the equipment. This is to ensure that the
equipment can be operated as usual and to perform the specific task of the equipment
without any problem. In order to achieve the objectives, the specific equipment which
is the crystallization unit need to be analyse and also research about the fundamental
and also principle of the equipment.
The continuous development of the chemical process industry has been accompanied
by rising demands for product quality. Crystallization is one of the methods to produce
particulate material in the chemical industry. In fact, crystallization is a separation
technique which has been used for centuries. Crystallization is employed in many
cases as an energetically advantageous way to separate an individual compound from
a mixture of substances represented by raw materials or by-products of reaction.
Crystallization may occur as the formation of solid particles from a vapor, as
solidification from a liquid melt or as the formation of dispersed solids from a solution.

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CHAPTER 2
LITERATURE REVIEW
2.1 Introduction
Commissioning and start-up is the final step before production runs in a processing
plant and is uniquely poised to perform commissioning and start-up and the
accompanying trouble-shooting and problem-solving activities, whether as part of a
design/build project or as a final step in an ongoing project.(Lawry & Pons, 2013)

2.2 Plant commissioning

Commissioning verifies that the design meets the needs and functions of the facility,
verifies that the project performs as designed and intended. Commissioning also
prepares the customer/user to effectively and efficiently maintain the facility for its
service life. The commissioning process includes specific tasks that must be done in
a specific order. (Rosaler, 2002)

2.3 Objectives of commissioning

The overall goal of building commissioning is to have a facility that operates as


intended. However, it is important to recognize several subgoals which will be
achieved as a direct result of the commissioning process. The primary goal is to
provide a safe and healthy facility for all occupants: office staff, the public, students,
faculty, researchers, and operations and maintenance staff. Commissioning minimizes
functional and operational deficiencies which have been shown to be responsible for
the majority of indoor air-quality problems and comfort complaints. The second goal is
to improve energy performance. Commissioning is the tune-up that gets the most
efficient performance out of the installed equipment. The third goal is to reduce
operating costs. Equipment operating improperly is operating inefficiently.. The fourth
goal is to improve orientation and training of the operations and maintenance staff.
The sophisticated systems being installed will be disabled if operations and
maintenance staff do not fully understand operation and maintenance requirements.
The final and most important goal is to meet the clients needs. When the design and
construction is subjected to systematic scrutiny and verification, the design intent and
customer satisfaction will be achieved. (Rosaler, 2002)

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2.4 Process of commissioning

Once it is recognized that all building systems must be commissioned, the process for
doing so becomes very specific and disciplined. In order for commissioning to become
an effective program, all participants in the design and construction community must
understand the requirements and willingly accept their responsibilities accordingly.

In brief, the owner must make clear during the programming phases of each project
what the owners commissioning expectations will be, since expectations may vary
with different kinds of projects. Then the design professionals must translate that
program into construction documents. Since commissioning scheduling, procedures,
and activities are currently not well understood throughout the construction industry,
contract documents must be much more comprehensive and specific regarding this
process. New roles may develop, for example, those of commissioning authority (CA)
and testing contractor (TC). As appropriate for each, their roles must be defined and
the working relationships identified. Then, the specifics of each role must be clearly
defined to ensure program continuity and to avoid conflict and redundancy. (Rosaler,
2002)

2.5 Crystallization

Crystallization is a common method for purification of mineral salt to produce standard


food grade sodium chloride. In this method energy consumption is low and impurities
of feed are removed during the process resulting in a product with appropriate mesh.
Salts that are not purified contain components like Lead, Arsenic, Cadmium, Copper
and Mercury which have irreversible adverse effects on human health. Existence of
impurities will deteriorate the size of crystals and may lead to formation of other salts
in the final product. In addition to impurities, other factors including feed concentration,
heating load, residence time, crystallizer form and mixer speed affect the mesh of
sodium chloride which have been investigated. (Ahmadpanah, Shahini, Sadeghzadeh,
& Kakavand, 2007)

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2.6 Batch cooling crystallization model

In industrial batch cooling crystallizers, the crystallizer temperature is often the only
process variable that is controlled. The jacket temperature is the manipulated variable
used to steer the crystallizer temperature. Since accurate on-line temperature
measurements can be readily obtained, the crystallizer temperature is controlled in a
closed-loop setting. In this configuration, the desired cooling profile is given as set-
point to a feedback temperature control loop.(Forgione et al., 2015)

2.7 Seeding

Seeding has been known for a long time as an effective technique to stabilize batch
crystallisation processes. In seeded crystallisation, ideally the supersaturation is
maintained at the desired constant value throughout the entire batch by the application
of properly designed control .Supersaturation, generated by cooling, can be consumed
by the growth of seeds added, and hence, it can be kept relatively low throughout the
batch if enough seeds are loaded. Consequently, secondary nucleation can be
avoided and the process can be stabilized. However, in practice in most of the cases
the suppression of secondary nucleation is achieved by very conservative operation
under the condition of slow cooling. In addition, quantitative information on the quality
and property of seeds is seldom considered in the control of the process, and
variations in seed CSD and property are generally considered as uncertainties rather
than actuators for the control of the final CSD. Seeding seems to be treated as an art
rather than science and generally there is a lack of systematic methodologies related
to the amount and size of seeds that should be added into a crystallizer to obtain a
product with a desired size distribution. (Aamir, Nagy, & Rielly, 2010)

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2.8 Crystal size distribution

The crystal size distribution is an important quantity in the production of high quality
product and for determining the efficiency of downstream operations, such as filtration
and washing, reaction with other chemicals, transportation and storage of crystals. If
the crystals are to be marketed as a final product, customers acceptance requires
individual crystals to be strong, non-aggregated, uniform in size and non-caking in the
package. For these reasons, crystal size distribution must be under control and it is
the prime objective in the design and operation of crystallizer. A uniform and narrow
crystal size distribution with a large mean crystal size is often
desired.(Srinivasakannan, Vasanthakumar, Iyappan, & Rao, 2002)

2.9 Salting out crystallization


Manganese sulphate monohydrate is known as an inverse salt because its solubility

decreases as temperature increases, other examples include calcium sulfate, calcium

carbonate, magnesium hydroxide, magnesium sulfate, zinc sulfate, and silicon

dioxide. A supersaturated solution is required for crystallisation to occur. Traditional

approaches for creation of supersaturation use temperature as a control parameter. A

different methodology to obtain crystallisation is by the addition of a second solvent to

the solution, one that is miscible with the original solvent and which also has a very

low solute solubility. In the case of aqueous solutions, low molecular weight alcohols,

such as methanol or ethanol, may serve as the second solvent. This process is often

referred to as salting out or drowning out Salting-out crystallisation of soluble

inorganic salts from an aqueous solution by the addition of an organic second solvent

is now commonly used in many chemical processes. Its advantage as an alternative

to simple heating or cooling crystallisation generally lies in the possibility of increasing

crystal size, form, yield, purity, and conducting the operation at ambient temperature.

(Safaeefar, Ang, Tad, & Reyhani, 2006)

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CHAPTER 3

METHODOLOGY

PRE ACTUAL PLANT TRIAL AND


COMMISSIONING COMMISSIONING RUN

3.1 Material and equipment

3.1.1 Chemicals and raw material

Chemicals that used in this experiment is sodium chloride solution. The sodium
chloride must be added with distilled water to become sodium chloride solution that is
raw material for the experiment

3.1.2 Apparatus

The apparatus that is use in this experiment are beaker, measuring cylinder and
spatula

3.2 Pre commissioning

3.2.1 System Configuration Check

Verify all pipe work and connections within the entire system and perform visual
inspections on equipment and pipe works to ensure they are clean and properly
installed

3.2.2 Cleaning and Flushing of Lines and Vessels

To internally clean up all Pipe Works and Pressure Vessels, ensuring no obstructions,
blockages or any potential contaminants in the process lines or vessels. After flushing,
it is important to ensure all pipelines and equipment are thoroughly dried off

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3.3 Actual Commissioning

3.3.1 Equipment Testing

This involves the test of equipment performances. Equipment such as pumps, heat
exchangers, cooling towers, will be run individually for certain period of time, and its
performances will be checked against design specifications

3.3.2 System Functional Testing

Individual Plant System will be run and all mechanical & electrical items within that
particular system will be checked to ensure the entire system is function as per its
design concept.

3.4 Plant trial and run

3.4.1 The entire plant will be put into operation. All system involves will be run
concurrently to simulate actual Plant Operation condition

3.4.2 Run the experiment design for the crystallization unit which is batch
crystallization experiment (production of salt)

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3.4.3 General procedure for plant trial and run
Prepare about 10 L saturated salt solution & Pour
the saturated salt solution in the crystallizer

Turn on the cooling water flow. Ensure that the


thermostat, T1 contain sufficient heat transfer
fluid

Set the vacuum pressure at 0.3 bar & thermal oil


fluid is set to 110C & Set the crystallization flow
rate, vacuum pressure and temperature of
thermostat T1 to a suitable value.

vessel
Observe the formation of crystal in the
circulation line. Once crystal start to appear,
stop the timer and record the time duration

Observe the formation of crystal in the


circulation line. Once crystal start to appear,
stop the timer and record the time duration

Measure the amount of condensate


accumulated in the condensate vessel and drain
the condensate vessel

Record the total time taken for the


crystallization process

Slowly open vent valve V7 and V8 to release


vacuum, pour the slurry solution through a filter
to obtain the crystallized solid. Dry the solid by
putting it under the sun or in an oven

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3.5 Standard operating procedure of the equipment

It is important that the user read and fully understand all the instruction and precautions
stated in the manufacturers manual supplied with the crystallizer prior to operation.
The following procedures will serve as a quick reference for operating the unit.

1 Cooling water system Laboratory tap water is used as the cooling media. Hose
connections are such that the cooling water enters both condensers W2 and W3 in
parallel. Adjust each cooling water flow rates using valves V14 and V15 to maximize
cooling and condensation. The temperature of the cooling water leaving condenser
W2 should not exceed 45C.

2 Thermostats (T1 & T2) The thermostat temperature can be adjusted on the
panel located on top of the individual thermostats. The flow rates of the heating/cooling
fluids in both thermostats can also be varied by changing the pump speed setting on
the panel. Press the enter button once and used the up or down button to change
the temperature set point.

3 Circulation pump (P1) Turn the speed control knob on top of the pump to
regulate the propeller pumps speed and consequently the circulation flow rate.

4 Dosing pump (P2) Adjust the frequency inverter on the control panel to change
the mohno pumps speed. The feed flow rate of the pump can be obtained by
monitoring the rate of liquid level drop in the dosing vessel B3.

5 Vacuum pressure control (P3) The vacuum pressure can be controlled by


adjusting the pressure set point of PIC-201 on the control panel. Press the enter
button once and used the up or down button to change the pressure set point.

3.6 General start-up Procedures for Crystallization.

1 Ensure all valve are closed except the ventilation valve V12.

2 Check that the product vessel B2 is empty of liquid.

3 Prepared about 10-L saturated salt solution by dissolving the appropriate amount
of salt in water.

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4 Pour the saturated salt solution into the crystallizer vessel B1 through valve V10
until the liquid overflows at the conical inlet. Close valve V10.

5 Pour the remaining solution into the feed/reaction vessel R1 through the charge
port.

6 Switch on the stirrer M1 and adjust the speed to mid-range.

7 Switch on the crystallizer pump P1 and set the circulation flow rate to 200L/hr.
Observe the liquid solution flowing from the crystallizer vessel B1 through the pump to
the head exchanger and then overflowing at the conical inlet back to the crystallizer
vessel.

8 Turn on the cooling water flow b opening valves V14 and V15.

9 Ensure that the thermostat T1 contain sufficient heat transfer fluid while thermostat
T2 contain sufficient water. Refill as necessary.

10 Switch on both thermostats T1 and T2. Set the temperature of the thermostat T1
(containing thermal-oil fluid) to 110C and thermostat T2 (containing glycol-water) to
80C. Set the pump speed for both thermostats to a value of 8.

11 To operate the crystallization process under vacuum, close valve V12. Switch on
the pump P3 and set vacuum pressure at 0.3 bar on the controller.

12 Observe the temperature rise in the feed/reaction vessel until it has reached a
constant value.

13 Allow the circulation line t heat up until boiling and evaporation occurs, and
condensate starts to appear in the condensate vessel B4.

14 The unit is now ready for experiments.

3.7 General Start-up Procedures for Batch Cooling Crystallization.

1 Ensure all valve are closed except the ventilation valve V7.

2 Prepared about 10-L saturated salt solution by dissolving the appropriate amount
of salt in clean water.

3 Pour the salt solution into the feed/reaction vessel R1 through the charge port.

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4 Switch on the stirrer M1 and adjust the speed to mid-range.

5 Ensure that the thermostat T2 contain glycol-water. Refill as necessary.

6 Switch on thermostat T2. Set the temperature of the thermostat T2 to 60C.

7 Observe the temperature rise in the feed/reaction vessel until it has reached a
constant value.

8 Add the appropriate amount of salt into the feed/reaction vessel R1 through the
charge port and let it dissolve.

9 Allow the circulation line to cool down.

10 The unit is now ready for experiment.

3.8 General Shut-Down Procedures

1 Reduce the temperature set point for both thermostats T1 and T2 to below room
temperature, and allow the liquid in the thermostats to cool down to room temperature.

2 Keep the cooling water running through condensers W2 and W3.

3 Switch off the stirrer M1 and dosing pump P2.

4 Set the circulation flow rates of pump P1 to 200 L/hr and allow the liquid to cool
down to room temperature.

5 Turn off the circulation pump P1.

6 Close valve v14 and V15 to stop the cooling water flow.

7 Carefully open the quick removable connections at product vessel B2 and remove
the vessel. Discard and clean any remaining liquid or solid residue in the vessel.

8 Remove the sampling bottle B5 and open valve V5 to drain all liquid from the
circulation line.

9 To clean the solid residue in the circulation line, attach a hose to valve V9 and
flush the pipelines with tap water. Drain the water through valves V5 and V6.

10 Drain the condensate vessel B4 by opening valve V13.

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11 If required, drain the liquid in the feed/reaction vessel by opening valves V1, V2
and V3.

12 Place the product vessel B2 and sampling bottle B5 back into the unit. Close
valves V5 and V6.

3.9 Product Collection

1 Make sure the product vessel B2 is empty.

2 If the unit is operating at atmospheric pressure, simply open valve V6 and let the
slurry solution flow from the circulation line into the product vessel.

3 If the unit is operating under vacuum, slowly open vent valve V7 and V8 to release
the vacuum.

4 Open valve V6 to collect the required amount of slurry solution and close valve V6.

5 Clean the product vessel before placing it back into the unit.

6 From the collection bottle, pour the slurry solution through a filter to obtain the
crystallized solid. Dry the solid by putting it under the sun or in an oven.

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RESULT

PRELIMINARY RESULT

4.0 Introduction

Under this chapter, the preliminary and expected result obtained after the experiment is to be
discussed

4.1 Equipment checklist

Commissioning Description Condition


item
Ok Not

Glassware Some of the piping glassware is broken


and need to be replace

Crystallization The stirrer in the crystallization pump is


pump broken and need to be replace

Vacuum pump The vacuum pump is easily clogged


with salt particles and need to be
equipped with filtration medium

Electrical There is no wire broken and electrical


supply and wire supply function well

Thermostat Thermostat reading is fluctuated and


need replacement

Condenser The condenser can be operated at


designated specification

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4.2 Expected result

Experiments data

As previously mentioned, the goal of the experiments is to study the effects of four
parameters, i.e. heating load, mixer speed, residence time and primary solution
concentration to yield larger crystals of sodium chloride. To do this, a base point has
to be considered for comparison purposes. Therefore, one of the best pure crystalline
salt in the market was selected as a base material for this research. The selected
crystalline salt was sorted out by means of a shaker-sieve system. As shown in Table
3, mass percentage of mesh 60 crystals is has the highest value and those of the
mesh 40 and mesh 80 are approximately equal. This indicates that the crystalline salt
distribution is quite good. According to the results denoted in Table 3, the higher mass
percentage of the crystalline salt with mesh 60 was selected as a criterion for
identifying of a suitable salt. The results of experiments 1 to 9 were classified based
on this criterion. Table 4 presents the results of the experiments.

Table 1: Results of Sizing of the Crystals (Base Point)

Mesh Weight Wt (%)

40 10.8 12.76

60 62.74 74.12

80 10.134 11.97

100 0.6 0.7

200 0.37 0.44

Sum 86.64 100

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Table 2 Results of the Experiments

No Solubility Mixture Residence Heating Percentage


speed (rpm) time load (watt) of Sizing on
(minute) Sieve Mesh
60

1 0.342 500 30 300 0

2 0.342 700 45 800 59.83

3 0.342 900 60 500 79.34

4 0.315 500 45 500 44.63

5 0.315 700 60 300 0

6 0.315 900 30 800 15.4

7 0.370 500 60 800 60

8 0.370 700 30 500 56.22

9 0.370 900 45 300 31.52

Discussion and Results

Considering Table 1, mesh 60 is selected as a criterion based on which the Taguchi


Analysis shall be carried out. As illustrated in Table 4 effective parameters on crystal
sizes will be classified as heating load, feed concentration, residence time and mixer
speed respectively.

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Mixer speed has no important effect on crystal sizing and hence its effect is ignored.
Table 6 shows all the parameters with their respective effect percentage. Experiments
show that increase of heating load enhances the rate of evaporation, which will
subsequently lead to increase of super-saturation and occurrence of nucleation, but
this does not imply production of large crystals. Heating load must have a proper value
to result in suitable growth of crystals. If heating load is considerably increased, it will
cause disturbance in the crystallizer, which will subsequently result in crash of the
crystals, which had already started growing up. On the other hand, decrease of heating
load extends the production time duration. Analysis of experiments shows a specific
amount for heating load, which will lead to production of appropriate crystals in the
shortest possible time interval.

Results of the experiments show that increase of feed concentration will cause
increase of mesh 60 crystals, on the other hand experiments show that increase of
feed concentration is more effective on crystals growth than nucleation rate. Increase
of the residence time, at presence of nucleuses and suitable operating conditions will
result in a better growth process and yield of larger crystals. If the residence time in
crystallizer is long, the grown crystals break and are divided into new nucleuses. In
other words, growth of crystals is limitedly increasable based on system conditions.
As an example if the mixer is of blade type and its speed is high, increase of residence
time will have no effects on growth of crystals because when the crystals are a bit
grown, they will face collisions with each other, the blade of the mixer and the body of
the crystallizer which will cause them to be broken to smaller ones.
Increase of mixer speed enhances the rate of nucleation and as a result more
nucleuses will be produced in the process environment. Therefore, high mixer speed
causes production of crystals with small sizes as in this case the crystals experience
more collisions and dont find the opportunity to have growth. This matter is obviously
observed when the mixer is of blade type. When the mixer is of impeller type, there
are less collisions between crystals and the mixer because of its shape and hence the
crystals are less broken. As a result, in identical operating conditions, the product of a
crystallizer with impeller mixer has larger size than that with a blade type mixer. Of
course in both cases increase of the mixer speed causes production of smaller size
product. The result of experiments confirms this matter (increase of crystals with 60
mesh).

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Table 3 The Optimum Operating Condition Obtained from Software

Operating parameter type Optimum condition

Solubility 0.37

Mixer speed (rpm) 900

Residence time (minutes) 60

Heating load (watt) 50

Obtain from journal Ahmadpanah, S. J., Shahini, M., Sadeghzadeh, J., & Kakavand,
M. (2007). Study of parameters affecting the crystal size distribution of sodium chloride
in bench scale crystallizers

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CHAPTER 6

6.0 ESTIMATED BUDGET

Chemical and Actual price Expected usage Price (RM)


equipment

Sodium chloride RM 20.11 per 10L RM 402.20


500g

Glass piping RM161.75 1 unit RM 161.75

Thermostat RM 75.00 1 unit RM 75.00

Stirrer RM 281.00 1 unit RM 281.00

Total RM 919.95

obtained from https://www.flinnsci.com, http://jinan-tyk.en.made-in-china.com/,


http://www.ika.com/.

6.0 RESEARCH PLAN ACTIVITY

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CHAPTER 7

7.0 REFERENCE

Aamir, E., Nagy, Z. K., & Rielly, C. D. (2010). Optimal seed recipe design for crystal
size distribution control for batch cooling crystallisation processes. Chemical
Engineering Science, 65(11), 36023614.
https://doi.org/10.1016/j.ces.2010.02.051

Ahmadpanah, S. J., Shahini, M., Sadeghzadeh, J., & Kakavand, M. (2007). Study of
parameters affecting the crystal size distribution of sodium chloride in bench
scale crystallizers. Petroleum & Coal, 49(1), 5460.

Forgione, M., Birpoutsoukis, G., Bombois, X., Mesbah, A., Daudey, P. J., & Van den
Hof, P. M. J. (2015). Batch-to-batch model improvement for cooling
crystallization. Control Engineering Practice, 41, 7282.
https://doi.org/10.1016/j.conengprac.2015.04.011

Lawry, K., & Pons, D. J. (2013). Integrative Approach to the Plant Commissioning
Process. Journal of Industrial Engineering, 2013, 112.
https://doi.org/10.1155/2013/572072

Rosaler, R. C. (2002). Standard Handbook of Plant Engineering. Plant McGraw Hill


Professional, 1019.

Safaeefar, P., Ang, H. M., Tad, M. O., & Reyhani, M. (2006). Growth Kinetics of
Manganese Sulphate from Heating and Salting-out Batch Cry s t allisation, 14,
303312.

Srinivasakannan, C., Vasanthakumar, R., Iyappan, K., & Rao, P. G. (2002). A Study
on Crystallization of Oxalic Acid in Batch Cooling Crystallizer, 16(3), 125129.

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