Mandar Pandit Report

B.
Tech in Oil technology
Index
Sr.No. Name Page No.
1 Introduction 01
-Alkyd resin 01
-Microwave synthesis 10
reactor
2 Aim of present project work 30
3 Experimental work 31
4 Results and conclusions 48
5 References 49
10
Laxminarayan Institute of Technology, Nagpur
B.Tech in Oil technology
Introduction to microwave synthesis
1. MICROWAVE CHEMCAL SYNTHESIS14:-

Microwave synthesis represents a major breakthrough in synthetic chemistry
methodology, a dramatic way in the chemical synthesis is performed & in the way it is perceived
in the scientific community. Conventional heating, long known to be inefficient & time-
consuming, has been recognized to be creatively limiting as well. Microwave synthesis gives
organic chemists more time to expand their scientific creativity, test new theories & develop new
processes. Instead of spending hours or even days synthesizing a single compound, chemist can
now perform that same reaction in minutes. In concert with rapidly expanding application based
microwave synthesis can be effectively applied to any reaction scheme, creating faster reaction,
improving yield, & cleaner chemistries.
In addition, microwave synthesis creates completely new possibilities in performing
chemical transformations. Because microwave can transfer energy directly to the reactive
species, so-called “molecular heating”, they can promote transformation that are currently not
possible using conventional heat. This is creating a new realm in synthetic organic chemistry.
Microwaves also provide chemists with the option to perform “cool reactions”. Energy is
applied directly to the reactants, however. The bulk heating is minimized by use of simultaneous
cooling. This allows for enhanced reactions of larger, more heat sensitive molecules (e.g.
proteins), as the temperatures are low enough to eliminate thermal degradation. This will provide
some new exciting opportunities & an important new tool for proteomics & genomics research.
Recent microwave hardware advancements now provide a range of affordable, flexible
tools for the synthetic chemist. This new technology, coupled with the rapidly expanding
knowledge & applications base, will cause a major shift towards microwave synthesis in next
few years. As Victor Hugo, the famous French novelist and poet wrote, “An invasion of armies
can be resisted, but not an idea whose time has come and whose impact will be truly monumental
on the world of chemistry.
The difference between microwave heating and convective heating:

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1.1 Microwave heating15:-

Microwave energy is a unique source because it creates heat deep within the material
being processed. This property results in much shorter process time, higher yield of finished
product & better quality than conventional processing.
The first successful microwave process on industrial scale was introduced in early 1960.
Microwaves cover a broad spectrum & frequencies range from 300 MHz to 300GHz. The
term microwave denotes technique & concept used as well as range of frequency. Microwave
travels in free space at the speed of light & they are reflected by metallic objects, absorbed by
some dielectric material & transmitted without significant absorption through other dielectric
material for e.g. water, carbon, & food with high water content are good microwave absorbs,
glass, ceramic & most thermoplastic material allow microwave to pass with little or no
absorption. Microwave interacts with dielectric material to generate heat by the agitation of
molecule in a alternating electromagnetic field.
1.2 Reasons for microwave processing:-

The unique property of microwave to penetrate deeply into material of interest reduces
the process time, often by much as 10 to 1 & its reduces the cost of processing. Space saving is
other reason for choosing microwave. Long stretched processing line can be compressed into a
fraction of space. Thus it reduces the cost of construction & substantial economic saving.
The other factors that may consider while using microwave processing are as follows
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1. Geometry i.e. Materials that are thick & therefore difficult & time consuming to
process by conventional heating means.
2. Temperature sensitivity i.e. Material adversely affected by using usual processing
temperature.
3. Cost, costly material generally can tolerate the higher cost of microwave processing.
4. Uniqueness, a unique product or attribute of a product is obtained by the use of
microwave heating.
5. Batch to continuous processing, where batch process can be converted to a
continuous process because of a substantial reduction in a process time.
1.3 Microwave heating mechanism:-
When microwave are intercepted by dielectric material such as food, they interact with
dielectric material, giving of energy which result in a increase in temperature of material. There
are two mechanisms by which microwaves produce heat in the dielectric material.
1) Ionic polarization 2) Dipole rotation
1.3.1 Ionic Polarization:-

Ionic polarization occurs when ions in the solution move in response to an electric field.
Ions carry an electric charge and are accelerated by the electric field. The kinetic energy is given
up by the field to the ions, which collides with the other ions, converting kinetic energy in to heat
more concentration the solution or more dense the solution the greater the frequency of the
solution and more kinetic energy that is released. When the dielectric field is alternating at
microwave frequency, numerous collisions occur and much heat is generated. This increase the
temperature of dielectric material.
1.3.2. Dipole Rotation:-

Water is most common material in food. Under normal conditions, polar molecules are
randomly oriented. In the presence of an electric field, the polar molecule line up with the field.
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As an alternating field is applied. The polarity of the field is varied at the rate of microwave
frequency and the molecules attempt to align themselves with the change in field. Heat is
generated as the result of the rotation of the molecule.
Microwave heating is also dependent on the physical state of the material i.e. ice in which the
movement of the water molecule in microwave field is restricted. The amount of microwave
energy converted to heat in the dielectric material is given by the equation
PD = 55.61 E2 ƒ K’ tanδ* 10-14 watts/cm3
Where PD = Power density

E = Electric field strength in volts/cm
ƒ = Frequency in hertz
K’= Relative dielectric constant
Tanδ = Loss Tangent
The field strength and frequency are properties of the energy source. The relative dielectric
constant and loss tangent are properties of the material being heated.
1.3.3. Penetration depth:-

It is defined as the distance from the surface of the dielectric material at which the
incident power drops to 1/e (about 37%) where e = 2.718282. penetration is also expressed as
half power depth. It is the depth from the surface of the material at which the power has been
reduced to one half of the total incident power.
1.4 Microwaves Are Energy:-
Microwaves are a form of electromagnetic energy. Microwaves, like all electromagnetic

radiation, have an electrical component as well as a magnetic component. The microwave
portion of the electromagnetic spectrum is characterized by wavelengths between 1 mm and 1 m,
and corresponds to frequencies between 100 and 5,000 MHz. Milestone microwave lab stations
use a specific, fixed frequency of 2,450 MHz (2.45 GHz).
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It is useful to consider the quantum energy of microwaves in relation to other forms of

electromagnetic energy. It is important to recognize that the energy delivered by microwaves is
insufficient for breaking covalent chemical bonds. This information can help to narrow
speculation on the mechanisms for enhancement in specific reactions.
1.5 Microwaves Can Interact with Matter:-
One can broadly characterize how bulk materials behave in a microwave field. Materials
can absorb the energy, they can reflect the energy, or they can simply pass the energy. It should
be noted that few materials are either pure absorbers, pure reflectors, or completely transparent to
microwaves. The chemical composition of the material, as well as the physical size and shape,
will affect how it behaves in a microwave field.
Microwave interaction with matter is characterized by a penetration depth. That is,

microwaves can penetrate only a certain distance into a bulk material. Not only is the penetration
depth a function of the material composition, it is a function of the frequency of the microwaves.
It is not true that microwaves "heat" a bulk material "from the inside out."
1.6 Microwave Heating Differs from Conventional Means:-
1.6.1. Conventional Heating Methods:-
In all conventional means for heating reaction mixtures, heating proceeds from a surface,
usually the inside surface of the reaction vessel. Whether one uses a heating mantle, oil bath,
steam bath, or even an immersion heater, the mixture must be in physical contact with a surface
that is at a higher temperature than the rest of the mixture.
In conventional heating, energy is transferred from a surface, to the bulk mixture, and
eventually to the reacting species. The energy can either make the reaction thermodynamically
allowed or it can increase the reaction kinetics.
In conventional heating, spontaneous mixing of the reaction mixture may occur through
convection, or mechanical means (stirring) can be employed to homogeneously distribute the
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reactants and temperature throughout the reaction vessel. Equilibrium temperature conditions can
be established and maintained.
Although it is an obvious point, it should be noted here that in all conventional heating of
open reaction vessels, the highest temperature that can be achieved is limited by the boiling point
of the particular mixture. In order to reach a higher temperature in the open vessel, a higher-
boiling solvent must be used.
1.6.2. Microwave Heating:-
Microwave heating occurs somewhat differently from conventional heating. First, the
reaction vessel must be substantially transparent to the passage of microwaves. The selection of
vessel materials is limited to fluoropolymers and only a few other engineering plastics such as
polypropylene, or glass fiber filled PEEK (poly ether-ether-ketone). Heating of the reaction
mixture does not proceed from the surface of the vessel; the vessel wall is almost always at a
lower temperature than the reaction mixture. In fact, the vessel wall can be an effective route for
heat loss from the reaction mixture.
Second, for microwave heating to occur, there must be some component of the reaction
mixture that absorbs the penetrating microwaves. Microwaves will penetrate the reaction
mixture, and if they are absorbed, the energy will be converted into heat. Just as with
conventional heating, mixing of the reaction mixture may occur through convection, or
mechanical means (stirring) can be employed to homogeneously distribute the reactants and
temperature throughout the reaction vessel.
1.6.3. Single-Mode and Multimode Microwave Cavities:-
The working compartment where materials are exposed to microwaves is variously

called a cavity, a resonator, an applicator, etc. Cavities are available in many sizes and shapes,
depending on the manufacturer and the application.
Despite the variety of cavities available, there are in reality only two basic types: single-
mode (often referred to as monomode), and multimode. It is important to recognize the essential
difference between the two types. Far more important is for synthetic chemists to recognize how
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cavities are the same in every important aspect with regard to chemical reactions. The distinction
between cavity types is determined by the design characteristics, not by the processes that can be
performed inside the cavity. The design characteristics are determined by many factors that have
nothing to do with the reaction chemistry.
(1) Single-Mode Cavities:
The essential characteristic of single-mode cavities is the deliberate creation of a standing

wave pattern inside the cavity. To do this, the dimensions of the cavity must be carefully
controlled to correspond in some systematic way to the characteristic wavelength of the
microwaves. Just as the resonant frequency of a standing wave on a violin string is a function of
the length of the string, so too is the maintenance of that standing wave determined by the
stability of the string dimensions.
For 2.45 GHz microwaves, the length of a single full wave is 12.2 cm. A single-mode
cavity for 2.45 GHz microwaves must be dimensioned such that a whole-number multiple of the
full or half wavelength fits inside the confines of the cavity.
Several consequences of single-mode cavity design must be appreciated. First,

microwave-absorbing materials placed inside such a cavity will, in fact, absorb microwaves and
be heated. Of course, if the intensity of the field is controlled, then the heating rate can be
controlled, some sort of temperature monitoring and feedback control scheme can be
implemented, etc.
The second consequence is far more important. There are specific positions inside the
single-mode cavity where items to be heated must be placed. The intensity of the field is greatest
at the peaks of the standing wave, and actually goes to zero at the nodes of the standing wave.
There are positions in the single-mode cavity (the nodes) where no heating will occur. Only in
the volume of the peak envelopes can transfer of microwave energy to a target absorbing
material occur. This substantially limits the physical dimensions of objects (such as reaction
vessels) that can be placed in a single-mode cavity and be heated effectively.
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The third consequence is probably the most important. Anything placed inside a single-
mode cavity can disrupt the standing wave pattern. For this reason, it is quite uncommon for
single-mode cavities to be designed to accept more than one target object (such as a vessel) to be
heated at a time.
Single-mode cavities do not lend themselves to simultaneous processing of multiple

targets (such as reaction vessels). Also, processing materials in single-mode cavities can result in
inconsistent heating due to variation in the volume, total absorbing mass, or physical shape (in
the cavity) of the material to be heated.
A final consequence of single-mode cavity design is the fact that there is no practical way
to scale up processes. One must recognize from the outset that microwave processes developed
on a small scale may need to be transferred to a larger scale for production. One cannot extend
the dimension of a standing wave cavity indefinitely, nor can one simply purchase components
off the shelf to generate a standing wave of just any delivered power.
(II) Multimode Cavities:-
The essential characteristic of multimode cavities is the deliberate avoidance and/or

disruption of any standing wave pattern inside the cavity. The engineering goal is to produce as
much chaos inside the cavity as possible.
There are two principal approaches to achieving this goal. First, the dimensions of the
cavity must be carefully controlled to avoid whole-number multiples of the microwave full or
half wavelength. Second, some means must be employed to physically disrupt any standing
waves that may form as a consequence of items placed in the cavity. This is best performed with
a mechanical mode stirrer, typically a periodically moving metal vane that continuously changes
the instantaneous field pattern inside the cavity. The shape of the vane and its movement is such
that the microwave field is continually stirred, and therefore the field intensity is homogeneous
in all directions and all locations throughout the entire cavity.
Several consequences of multimode cavity design must be appreciated. First, microwave-

absorbing materials placed anywhere inside the cavity will, in fact, absorb microwaves and be
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heated. Of course, if the intensity of the field is controlled, then the heating rate can be
controlled, some sort of temperature monitoring and feedback control scheme can be
implemented, etc.
The second consequence is far more important. In a properly designed multimode cavity,
there is no specific position inside the cavity where items to be heated must be placed. Because
the field is homogeneous everywhere and in all directions, every position in the cavity is like
every other position.
The third consequence is perhaps the most important. Since the field in a multimode
cavity is continuously re-homogenized (stirred), nothing placed inside the cavity will
permanently affect the distribution of the field intensity. This means that there are no limitations
on the size and shape of the objects placed inside the cavity. If they will physically fit inside the
cavity and if they absorb microwaves, then they will be heated.
This also means that multiple objects (for example, multiple reaction vessels) can be
processed simultaneously, just as effectively as single objects. This is a dominant advantage of
multimode cavity design.
A final consequence of multimode cavity design is the fact that practical scale-up of
processes is easy. Any process that is developed in a bench-top multimode microwave lab station
can be scaled up to production or pilot plant capacities. A multimode cavity can, in theory, be
infinitely extended in every dimension. With a multimode design, additional field intensity to fill
that extended cavity can easily be had by simply adding additional magnetrons to the system.
These facts of cavity design can be important considerations when first exploring the
microwave advantage. The user must carefully assess how the microwave system will be used in
the lab today, and the possible applications and configurations for the future. Only a multimode
cavity provides the opportunity to go beyond a single reaction format to multiple reactions
simultaneously and uniformly. Only a multimode cavity allows you to progress from discovery
through to production, in any form factor, with confidence.
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1.7 MICROWAVE HEATING SYSTEM USED IN PRESENT STUDY:-

Introduction:-
The CEM Focused Microwave™ Synthesis System, Model Discover, is designed to
enhance the ability to perform chemical reactions under controlled conditions on a laboratory
scale. The System facilitates either homogeneous or heterogeneous solution phase chemistry,
solid phase chemistry or chemistry conducted on solid supports. It accommodates vessels
ranging in volume from 5mL to 125mL for reactions performed under atmospheric conditions
and a 10mL vessel with septa for reactions performed at elevated temperatures and pressures.
Primary uses of the Discover are in the discovery and lead optimization phases of the new
product development process.
Microwave energy is applied to the vessel contents (reactants, catalysts, salts, solvents
and/or solid supports) to accelerate the chemical reaction. The microwave absorption properties
of some liquid and solid materials, due to their polar and ionic characteristics, have the capability
to significantly enhance chemical reactions relative to traditional energy application (heating)
techniques. The microwave interaction properties with the reactants, intermediates, catalysts,
solid supports and salts provide unique opportunities for the synthetic chemist.
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The Discover System consists of:

• A continuous microwave power delivery system with operator selectable power output from 0 -
300 watts (+/- 30 watts) programmable in 1-watt increments.
• A self-adjusting, single mode microwave cavity that is manually accessed via multiple
attenuator ports (both ports are included).
• A 4-line x 20-character vacuum fluorescent display with alphanumeric keypad and on-board
computer for programming and operational control of the system. The memory will store and
recall up to 20 methods.
• 3 safety interlocks and an interlock monitoring system to prevent microwave emission when
the attenuator port is not properly installed.
• Two serial ports for computer interface and optional feature connections.
• An ethernet port for network connection (optional configuration).
• An accessory kit.
Optional features include:

• Infrared Temperature Control System –
This temperature control system uses a non-contact, infrared sensor to measure
temperature. It is located below the microwave cavity floor and measures the temperature on the
bottom of the vessel. The sensor is vessel volume independent and is used in a feedback loop
with the on-board computer to control the temperature rise rate and control point of the vessel
contents. Temperature is programmable from 25 - 2500C.
• Fiber Optic Temperature Control System –

This optional temperature control system, for use with large volume, open vessel
applications, uses a fiber optic temperature probe for temperature measurement and control of
the vessel contents. This is an “invasive” measurement technique and thus requires access to the
reaction container from the external environment. It connects to the instrument through the
second serial port at the rear of the instrument. When connected, the Discover system
automatically detects the temperature sensor and defaults to use this sensor for temperature
measurement and control. Temperature is programmable from -80 ºC to 250 ºC.
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• Direct Pressure Control System –

This pressure control system uses a load cell for a direct pressure measurement of the
reaction vessel contents. The load cell is connected to a 10mL vessel via a 22-gauge needle,
which penetrates just below the septum surface (the septum is positioned outside the microwave
field.). The sensor provides very accurate low-end pressure measurements and is used in a
feedback control loop with the on-board controller to control the pressure rise rate and control
point of the vessel contents. Pressure is programmable from 0 – 300 psi (0 – 21 bar).
• IntelliVent Pressure Control System –

This pressure control system uses a load cell for an indirect measurement of the reaction
vessel contents. The load cell is connected to a 10mL vessel and senses changes in the external
deflection of the septa on top of the sealed pressure vessel. The sensor housing incorporates a
capture and release mechanism to secure the reaction in the cavity. Pressure is programmable
from 0 - 300 psi (0 - 21 bar).
• Stirring Option –
The stirring option consists of a rotating magnetic plate located below the floor of the
microwave cavity. “Stirring” occurs when the rotating magnetic field couples with a stir bar in
the vessel. The method setup enables the stirring feature. Standard stir bars or “fleas” are used
(not included).
• Cooling Option –
The cooling option consists of necessary valves and ports to direct a cooling gas (either
nitrogen or “clean” air) onto the vessel in the system cavity. This option will decrease the
temperature of a 2mL solution in a 10mL Pyrex reaction vessel from ~150 ºC to ~40 ºC in less
than 120 seconds. Method setup enables the cooling feature. The gas is user supplied at a
minimum pressure level of 20 psi (~1.5 bar) and a flow rate of 25 liters/min.
Instrument Description:-
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Figure No. 1
• Display –
Displays menus, method parameters and instrument status on a 4 line x 20 character
vacuum fluorescent display.
• Keypad –
Allows the operator to create, edit, store and recall methods start and stop methods and
change programmed parameters during operation.
• Attenuator –
Provides access to the instrument cavity while preventing microwave leakage during
operation. The attenuator can be installed or removed with a “twist-lock” action (no tools
required).
• Interlock Assembly –
Monitors mating of the attenuator to the cavity. If the attenuator is not installed properly,
the instrument will not deliver microwave power nor permit the system to operate.
Discover System - Front View:-
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Figure No.2
• Edit –
Press to access the System Setup options such as sensor configuration and calibration or
system parameters.
• Home –
Press to return to the main screen from any menu in the software. Within the System
Setup portion of the software, press this key to return to the previous menu.
• File –
Press to access the programming options in the software. These options include; Quick
Test, New Method, or a list of methods from the method library.
• C/CE –
Press to clear a key entry or delete a method from the method library when using the
delete method function.
• Enter –
Press to accept entries while editing or creating a method or in System Setup.
• 0-9 –
Press to enter method parameter values such as power, temperature, pressure, ramp time,
run time and hold time.
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• Start/Pause –
Press to start the current method or press during method operation to pause or suspend
operation. Pressing the key again will restart the method from the paused point.
• Stop –
Press to stop any process. Pressing this key when performing a method will stop system
operation and launch the cooling function. Pressing this key during the cooling cycle will abort
the cooling cycle and return the system to the home screen.
• Arrows –
Press these keys to navigate through method programming or System Setup steps.
• Power –
Press this key followed by the appropriate numeric keys to change the maximum applied
microwave power setting. This does not stop or pause a method but updates the setting in real
time. The updated setting is not captured as part of the saved method file in the method library.
• Temperature –
Press this key followed by the appropriate numeric keys to change the temperature set
point before or during a method. This does not stop or pause a method but updates the setting in
real time. The updated setting is not captured as part of the saved method file in the method
library.
• Time –
Press this key followed by the appropriate numeric keys to change the time value during
or after a method. Pressing during the Run Time cycle allows for real time changes to this value.
Pressing during the Hold Time cycle allows for real time changes to this value. This does not
stop or pause a method but updates the setting in real time. The updated setting is not captured as
part of the saved method file in the method library.
• Pressure –
Press this key followed by the appropriate numeric keys to change the pressure set point
during a method. This does not stop or pause a method but updates the setting in real time. The
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updated setting is not captured as part of the saved method file in the method library. This key
can also be pressed when the instrument is idle to open or close the IntelliVent.
• Cooling –
Press this to perform the cooling function during a method. This does not stop or pause a
method but updates the setting in real time. The updated setting is not captured as part of the
saved method file in the method library. The cooling key can also be pressed prior to beginning a
method to turn Power Max “on” or “off.” To cool a vial when a method is not in progress, from
the Main Menu, press the “Home” key; then from the temperature screen, press the cooling key.
• Power Switch –
Turns AC power on and off to the instrument.
• Cooling Gas Line –
Connects cooling gas supply to instrument
Figure
No.3
Temperat ure
Control System
Options
1. Infrared
Temperature Control System:-

The standard temperature control system for the Discover System consists of a non-
contact infrared sensor that monitors and controls the temperature conditions of the reaction
vessel located in the instrument cavity. The temperature sensor is centrally located beneath the
cavity floor and “looks” up at the bottom of the vessel. A lens is positioned between the sensor
and the cavity floor to protect the sensor. The temperature sensor data is set up in a feedback
control loop with the magnetron to regulate the power output to maintain the temperature set-
point through the onboard processor. The instrument software is designed so that the magnetron
provides the lowest power output to maintain the set-point, thus maximizing the “on” time of the
microwave energy input.
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Figure No.4
Bench Mate Option:-
During routine use, the Bench Mate should remain connected to the 7-pin connector
located on the back of the Discover.
1. Plug the Bench Mate into the 7-pin connector located on the back of the Discover instrument.
2. Place the Bench Mate on top of the Bench Mate attenuator, ensuring that the notches on the
Bench Mate are aligned with the slits on the attenuatgor. Lock the Bench Mate onto the
attenuator by pushing down on the sides of the Bench Mate.
3. Tighten the Bench Mate by turning the top of the Bench Mate clockwise until resistance is
felt.
1. Sample Stirrer:-
Based on system design, the sample stirrer is a rotating plate containing either electromagnetic
coils or permanent magnets positioned beneath the instrument cavity floor. It works in
conjunction with stirring bars or “fleas” placed in the reaction vessel to affect stirring and ensure
a homogeneous sample. An initial supply of magnetic stir bars or “fleas” are provided.
Additional stir bars can be purchased from CEM Corporation. Any commercially available
magnetic stir bars or “fleas” are acceptable for use with the Discover system.
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2. Cooling:-
The cooling feature directs a gas source onto the outside wall of the reaction vessel. This
provides the ability to rapidly cool (quench) a reaction after the application of microwave
energy. The cooling feature is either “on or off” and is part of the method.
The feature consists of
• “plumbing” to direct the gas from the inlet point of the Discover to the reaction vessel
in the cavity, a solenoid valve connected to the CPU (controller) board to turn the gas
flow on and off,
• A hose fitting to connect the Discover to the gas source via a hose,
• 8 feet (2.44 meters) of ¼ inch (6.35 mm) inside diameter air hose.
The gas source is user supplied. CEM Corporation recommends either nitrogen or
“clean” air at a minimum pressure of 20 psig (~ 1.5 bar). This will provide a fl ow rate of 25
liters per minute and will cool a 5mL volume of propylene glycol in a 10mL reaction vessel from
150 °C to less than 40 °C in less than 2 minutes.
3. User Interface:-
The user interface consists of the keypad, LCD display, and two serial ports. This
provides the means for the user to input information into and output information from the
Discover System.
The input functions are performed with the keypad and provide the ability to
• create new methods and edit existing methods,
• recall and delete methods,
• change operating parameters during method operation in real time,
• start, pause and stop operation,
• set up a computer, and
• configure the sensor options and system options.
The output functions are obtained from the LCD Display and computer port. The LCD
display provides visual information of the keypad entry and permanently stored instrument
information. The computer port provides the option of using an off-board PC to program the
system and to collect data.
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4. Method Control Options:-

The Discover System has four (4) control options for programming a method – Standard Control,
Power-Time Control and SPS Coupling and SPS Deprotection Control. These options permit the
user to control how the system applies the microwave energy to the reaction. In all control
options, the user inputs control parameters to create the method. The user enters more control
information as the level of control increases from the Power-Time Control to the Standard
Control to SPS Control.
.
5. Standard Control:-
The Standard Control option provides more flexibility in how the user programs a
reaction method and makes greater use of the feedback control data from the temperature and
pressure systems. It applies a specified amount of power, defined by the user, to reach the control
point. It modulates this set power automatically, based on the sensor feedback data, to ensure the
control point is reached rapidly, but with limited error (temperature or pressure “overshooting”).
The user programs
1. The maximum amount of microwave power that can be applied to the method,
2. A temperature control point,
3. A pressure control point,
4. A run time (the maximum run time for the method for situations where the control
point is not reached)
5. A hold time (the time the system maintains the control parameters),
6. Optional stirring function, and
7. Optional cooling function.
The Standard Control option can be programmed for five (5) stages for multiple
irradiation steps and is a general control method for maintaining critical control points.
6. Power-Time Control:-
The Power-Time Control option is the simplest programming option. It provides the user
the most direct method to energize reaction systems. This option applies a specified amount of
29
energy for a specified amount of time. Maximum temperature and pressure limits stop instrument
operation if either is reached. The user programs
1. The amount of microwave power applied,
2. A maximum run time (the total time the system applies microwave energy),
3. A maximum temperature (a temperature above which the system will not apply
microwave energy),
4. A maximum pressure (a pressure above which the system will not apply microwave
energy),
5. Optional stirring function, and
6. Optional cooling function.
The Power-Time Control option can be programmed for five (5) stages for multiple
irradiation steps. It does not provide the flexibility to maintain critical control points; thus, it
provides the least amount of control.
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2 AIM OF PRESENT PROJECT WORK

Now a day, there is a global trend of replacing petroleum-based product with
renewable resources like plant extracts in commercial product such as paints, surfactants,
detergents etc.
The petroleum products are sourcing in price and availability, we have to search for
alternatives particularly from vegetable sources. Being of natural origin, these derivatives
are expected to be fairly biodegradable.
Therefore, the present work is aimed at developing novel polymeric material based
mainly on plant extracts like castor oil, Rosin etc.
In this project we are trying to devolve polymeric material from natural origin,
which can be used in the paints or detergents. In this way we are trying to replace the
petroleum based raw materials used in detergents and paints to the maximum extent that
can be possible.
In this project we are also trying to use the different method of manufacturing that
is microwave synthesis reactor method.
We will try to manufacture polymeric material on microwave synthesis reactor that

is a completely new technology.
Regarding microwave, we will prepare polymeric material by this method and we

are going to study the effect of the parameters of microwave synthesis reactor on the
properties of polymeric material.
In this study we are going to compare the properties of polymeric material prepared
on microwave synthesis reactor with that prepared on conventional batch reactor. We are
also going to compare the products prepared from both of these polymeric materials.
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3 EXPERIMENTAL WORK
3.1 PREPARATION OF RESIN

(a) Preparation of rosinated castor-alkyd resin by microwave synthesis equipment:-
The resin is prepared in the microwave synthesis reactor by using following parameters.
Temperature: 2250C
Time: 10 min
Power: 225 W
In the preparation of the resin all the raw materials are mixed properly and that mixed
properly and whole mass is added in to the wire of the microwave synthesis reactor batch wise.
At a time 7 ml resin can be prepared in the one batch of microwave synthesis reactor. In this way
200ml resin is prepared.
(b) Experimental formulations of rosinated Castro-alkyd resin:
Sr.No. Ingredients Formulation I(%) Formulation II(%)

1 Castor Oil 35.00 33.33
2 Rosin 55.00 52.38
3 Maleic anhydride 5.00 5.00
4 Pthalic anhydride 5.00 --
5 Glycerol -- 10.00
3.1.1 ANALYSIS OF RESIN:-

(a) Acid Value5:-
32
Weight about 1.2 gm of resin sample in flat bottom flask. Add 20 ml neutral alcohol in it.
Keep the flask on hot water bath till the solution in the flask homogeneous. Add few drops of
phenolphthalein indicator and titrate the solution of the flask against 0.1 N alcoholic KOH. The
acid value obtained by following formula.
Acid Value = (56.1 × N × V) / W
Where,
N= Normality of KOH.
V= Volume of KOH required.
W= Weight of oil in the flask.
Standardization of KOH:-
Weigh accurately 0.1 to 0.2 gm of oxalic acid and mix it into 20 to 25 ml of distilled
water. Shake and mixed well to dissolve oxalic acid. Add 2 to 3 drops of phenolphthalein
indicator and titrate it against 0.1N KOH till pink color obtained.
(b) Volatile Content6:-

It was determined by weighting out 2 to 3 gm of resin sample in to a Petri dish and
heating for about 3 hours in an oven at 1050C. It was cooled weighted and reheated for a further
half hour to check that the weight was constant. The volatile content is expressed as a percentage
of the original resin.
Solid Content7:-
The percentage of solid in the resin was calculated as follows.
%Solid = (100 – Volatile Content)
3.1.2 PROPERTIES OF ROSINATED CASTOR-ALKYD RESIN:-
33
Sr. Physical Property Observation

No
Formulation I Formulation II
1 Acid value of resin 125 66.98
2 % Solid 91.25 88.56
Conclusions:-
1. As per the formulation and given procedure both resins are prepared and analyzed
according to standard procedure.
2. As per the analysis formulation II is preferred than the formulation I as formulation II has
very high acid value.
3. At the start of project our aim was to use the rosinated castor oil alkyd resin in the paints.
As the acid value of the prepared resin is too high we can use that resin in the formulation
of water based distemper only. Use of the resin prepared from the microwave synthesis in
the formulation of distemper or cement paint will not be cost effective. Hence it is
concluded that the prepared resin cannot be used in the formulation of paints.
4. Above prepared resin has sufficient acid value to use that in the formulation of liquid
detergent.
5. To use the resin in the formulation of liquid detergent it is necessary to neutralize the
resin. Resin is neutralized by using 30% KOH till its PH become 8. After the
neutralization is over 2% tri ethanol amine is added to it.
3.2 PREPARATION OF LIQUID DETERGENT:-
34
Resin prepared by the Formulation II is used in the liquid detergents. This resin is used in
the liquid detergent in various proportions and analyzed for its effect.
Formulation of liquid detergent based on the rosinated castro-alkyd resin (formulation I):-
Sr.No. Ingredients LD1 (%) LD2 (%)

1 S.L.S. 5 5
2 S.L.E.S. 20 10
3 Novel resin 10 15
4 A.O.S. 10 5
3.2.1 ANALYSIS OF POWDER DETERGENT:-

(a) Surface Tension8:-
Surface tension may be defined as the force in dynes acting at right angle to the surface of a
liquid along one centimeter length of the surface. It is generally represented by the symbol “Y”
and expressed in dynes/cm. surface tension of some common liquids.
Some effect of surface tension: -

1) The effect of surface tension is to reduced the area of the surface to a minimum. Hence
drops of a liquid of bubble of a gas are spherical in shape i.e. a sphere has minimum surface are
for a given volume.
2) The rise of liquid in capillary tube (e.g. rise oil in the wick of a lamp, rise of
underground water on the surface of earth, rise of water in plant) is well known phenomenon.
This can be explained in terms of surface tension.
Measurement of Surface Tension:-
35
A number of methods for the measurement of surface tension are known. One of them is
described as follows
The Stalgamometer Method:-

The stalgamometer consist of a pipette like tube having smooth capillary end with sharp
edges. It is filled with the liquid up to the mark M by sucking up at the upper end of the tube.
The liquid is then allowed to come down in the form of drops. Each drop coming out the
capillary end goes on increasing in size to certain point and then falls down. The ultimate size of
the drop depends on the radius of the capillary orifice and the surface tension of the liquid. The
drop is supported by the force of surface tension, 2Лr where r is the radius of the drop at the end
of capillary tube. The drop falls when its weight just exceed the force of surface tension. A
moment before, at equilibrium,
W= mg= 2Лr Y
Where m is the mass of the drop and g is the acceleration due to gravity.
Knowing the surface tension of the one liquid, we can calculate the surface tension of the other
liquid easily by using following formula
Ψ1=(n2 ρ1/n1 ρ2) Ψ2
Where Ψ1= surface tension of the sample
Ψ2= surface tension of water (i.e.71.18 dyne/cm)
ρ1=density of sample
ρ2=density of water
n1=no. of drops of sample
n2=no. of drops of water
These are four method used for determining the surface tension of the samples, among
which we have used stalagmometer.
(b) Foam Height8:-
36
Foam is coarse of dispersion of gas in relatively small amount of liquid or it may be

defined as collection of bubbles. Bubbles vary in size from 50 micrometer to several mm. the
low foaming tendency of surfactant is an important property in some recent application. The
relationship of foaming power to detergency has always been of interest and foaming power has
become associated in many consumer minds with high detersive power. However foam has no
direct relationship to detergency, in ordinary fabric washing system and does not improve
cleaning in a laundry or home washing machine. Indeed excessive foam levels may concentrate
certain surfactant in the foam, reducing their contact with the fabric to be washed. Foam prevents
redeposition and enables the soil to be easily removed by scrapping of or rinsing away the soil
laden foam.
Foam stability in detergency system is an important property in two major surfactant
applications: dishwashing, detergent and hair shampoos. The volume of foam produced is still
very important property of surface active materials. Ability to form at extreme dilution or under
adverse conditions may be important factor in applications.
Many methods for measuring foaming characteristics of the composition have been
devised. Equipment involved may be classified as fallows.
1) Manual manipulation of closed container.
2) Capillary under constant pressure.
3) Mechanical agitation in closed vessel.
4) Ross and Miles method
Procedure
Foam characteristics are measured in terms of volume. The following are carried out for
it
1. Take 1000 ml cylinder provided with stopper. Add to it, 100 ml solution of
particular concentration whose foam characteristic is to be measured.
2. Give it 30 up-down rotation within time period of 30 seconds.
3. Keep that cylinder on table and observe the foam above liquid level and note
down reading at zero minute.
4. The readings were measured after 5, 10, 15 minutes respectively.
37
5. Same procedure is carried out for the solution of different concentration like
0.1 %, 0.25 %, 0.5 % and 1%.
From above experiment we can easily find out the foam stability and change in
foam characteristics with time.
(c) Percentage detergency9: -
This includes the following step

Soil medium:
The soil medium is prepared as following composition
Component %
Carbon black 28.4
Coconut oil 35.8
Lauric acid 17.9
Mineral oil 17.5
The mixture of carbon black and lauric acid along with mineral oil is taken in pastel and
mortar. Coconut oil is added slowly to form thick paste of it. The all component were grinding in
pastel mortar for 1-2 hrs to get fine grinding. Smooth feeling of the mixture can test the fine
grinding.
Soil solution:
This is prepared by adding 2 gm of above paste in 500 ml carbon tetrachloride. Mix it
well and use for further cloth sample preparation.
Methods of application:
The cotton cloth of size 24 × 32 cm was prepared. Take 50 ml of soil solution in beaker.
Dip this cloth sample in it for 5 min. this is kept outside for drying in open atmosphere for 2 hrs.
Than this cloth is cut in to test samples size of 6 × 8 cm2 these samples were used for washing
purposes.
Methods of washing:
38
The solutions of different concentration were prepared. Dip soiled cloth sample in it for
5 min. and given to form 10 hand washes. Washing is carried out in distilled water only. After
rising this sample it is kept for drying purposes.
Percentage detergency:
The samples, which are washed dried and ironed, are used for percentage detergency. The
% detergency is finding out by using Lambert and slandered formula
%Detergency = [(Rw –Rs) × 100] / (Ro- Rs)
Where,
Rw = Reflectance measured on washed cloth.
Rs = Reflectance measured on soiled cloth.
Ro = Reflectance measured on clean cloth.
The reflectance of the cloth samples were measured by using “reflectance meter”
manufactured by Universal Engg. Corporation, Ambala road, Saharanpur (UP). This is digital
instrument. This is first standardizing by using the magnesium oxide or tile, which is provided
along with the instrument. Once this is adjusted, then samples were kept on the instrument and
note down the digital.
(d) Density:-
Density using density bottle

A density bottle is small bottle of 25 cm³ capacity with a capillary stopper fitted its
mouth. Both the stopper and the mouth are ground carefully to perfect fit. The experimental
liquid is filled in the bottle upto the mouth and the stopper is fited tightly. A small amount of
liqud flows out the capillary and liquid fills the bottle and the capillary right up to upper end.
Procedure
1) Thoroughly clean the density bottle with the mixture of nitric or chromic acid
then wash with water. Rinse both stopper and bottle with distill water and finally
39
With little methanol or acetone and dry it in a current of dryer.

2) Fill the bottles with air free distill water and insert the stopper into its mouth so that a
small amount of water flows out of capillary. Suspend a bottle in thermostat at the
required temperature (room temperature). With the upper end of the stopper 1 cm above
the surface of the water bath. Weight the bottle and the content after allowing them to
stand for a short time to take the temperature of the balance.
Empty the bottle and dry it repeat the determination with liquid under investigation.
Observation
1) Weight of density bottle = W1 gm
2) Weight of the bottle + water = W2 gm
3) Weight of the bottle + liquid = W3 gm
4) Temperature of Expt. = t0 C
Calculation
wt of the liquid
ρ= × Density of water at t 0 C
wt of equal volume of water
W3 − W1
= × Density of water at t 0 C
W2 − W1
Where ρ is density of liquid
Results of the analysis of liquid detergent samples: -
Name Conc. Foam Height (cm3) Density Surface

liquid (cm3) Tension
Time in minute
40
detergent 0 5 10 15 (Dynes/c
sample m)
LD1
0.25% 440 415 400 375 0.982 29.57
0.5% 585 565 550 525 0.984 28.02
1% 720 695 675 655 0.988 26.05
LD2
0.25% 460 425 410 385 0.980 30.01
0.5% 610 585 570 550 0.982 28.29
1% 740 715 700 670 0.985 26.93
Results of percentage detergency by soil: -
Name of liquid Concentration % detergency

detergent samples Cotton Polyester
LD1 0.25% 80% 82%
0.50% 84% 86%
1.00% 88% 90%
LD2 0.25% 82% 84%
0.50% 85% 88%
1.00% 89% 91%
3.3 STUDY THE EFFECT OF THE POWER ON THE ACID VALUE OF RESIN IN
THE MICROWAVE SYNTHESIS REACTOR.
41
While studying the effect of various parameters of the microwave synthesis reactor we
have studied the effect of power on the various properties of resin. We have observed that the
change in the power of the microwave synthesis reactor greatly affect the acid value of the resin.
Hence we compare the acid value of resin by continuously increasing the power of the
microwave synthesis reactor. All other parameters are remained same.
Procedure: -
1. All the raw materials of resin formulations are mixed in the one container.
2. Then resin of the same formulation is subjected to continuously increasing power of

microwave synthesis reactor. Resin is prepared in six different batch and each batch is subjected
to different power starting from 100 to 225.
3. Prepared resin is analyzed for its acid value.
Results: -
Power Time Temperature Acid value

100 W 10 min 2250C 59.46
125 W 10 min 2250C 57.2
150 W 10 min 2250C 56.28
175 W 10 min 2250C 53.21
200 W 10 min 2250C 51.82
225 W 10 min 2250C 49.36
42
Graph 1 – effect of power on the acid value of resin.
Conclusions: -
From above experiments we can conclude that by increasing the power of the microwave
synthesis reactor acid value of the decreases. As the power goes on increasing the required
temperature is attained in lesser time so resin is exposed to maximum temperature for more time
and hence acid value goes on reducing.
43
3.4 COMPARISON BETWEEN RESIN PREPARED BY MICROWAVE SYNTHESIS

AND RESIN PREPARED BY BATCH OPERATION: -
Aim: -
In this our aim is to compare the properties of resin having the same formulation but
prepared with different methods. In this comparison is made of a resin prepared by microwave
synthesis with the resin prepared by batch i.e. by using normal reactor.
Outline of the experiment: -
1. In this first we prepared resin using microwave synthesis reactor with a parameters,
which are mentioned earlier.
2. Then we prepared a resin with a same formulation as above but in the normal batch
reactor.
3. We analyzed both the resin prepared above.
4. Both the resins are then use in the same type of application. Here we prepare liquid
detergent with both these resins.
5. Analysis of above liquid detergent is carried out. By comparing the properties of liquid
detergents prepared from resin manufactured by different method, the effect of
manufacturing technique of resin on the liquid detergent is observed.
6. In this way comparison is carried out.
Formulation of resin used for the comparison: -
Sr.No Ingredients Quantity

1 Castor Oil 33.33
2 Rosin 52.38
3 Maleic Anhydride 5.00
4 Glycerol 10.00
Resin of above formulation is prepared on microwave synthesis reactor as well as on

conventional batch reactor.
44
Analysis of resin: -
Sr. Physical Property Observation

No
Microwave reactor Batch reactor
1 Acid value of resin 66.98 63.17
2 % Solid 91.02 92.17
Formulation of liquid detergent: -
Sr.No. Ingredients LD (a) (%) LD (b) (%)

1 S.L.S. 10 10
2 S.L.E.S. 20 20
3 Novel resin 20 10
4 A.O.S. 10 20
Analysis of liquid detergents: -
1. Analysis of LD (a): -
Resin used Conc. Foam Height (cm3) Density Surface

(cm3) Tension
Time in minute (Dynes/
cm)
0 5 10 15
Microwave
Reactor 0.25% 475 450 430 415 0.981 29.95
0.5% 630 610 585 570 0.983 28.02
1% Foam
750 Heig
725ht v/s
710 Time
695 (B.R.)
0.986 26.04
Batch
reactor
800 0.25% 460 425 410 385 0.980 30.01
700 0.5% 610 585 570 550 0.982 28.29
m
1% 740 715 700 670 0.985 26.93
600
m
n
i 500
t
h
g
i 400 0.25
e
H 300 0.5
m
a 200
o
F 1
100
45
0
0 5 10 15
Time in min
Graph 2 – Foam height of LD (a) from resin prepared on batch reactor.
Graph 3 – Foam height of LD (a) from resin prepared on microwave synthesis reactor.
46
Graph 4 – Comparison of foam height of LD (a) using resin prepared by microwave

synthesis reactor with that prepared on the batch reactor.
2. Analysis of LD (b): -
Resin used Conc. Foam Height (cm3) Density Surface

(cm3) Tension
Time in minute (Dynes/
cm)
0 5 10 15
Microwave
Reactor 0.25% 500 475 450 420 0.9744 30.12
0.5% 650 630 600 580 0.978 28.45
1% 800 770 750 725 0.981 26.21
Batch
reactor 0.25% 480 465 450 425 0.976 29.81
0.5% 625 610 585 575 0.979 28.16
1% 780 765 745 725 0.982 26.34
47
3. Comparison of detergency of liquid detergent from resin prepared from microwave

reactor and batch reactor: -
Resin used Concentration % Detergency

Cotton Polyester
M.R. 0.25% 82% 83%
0.50% 84% 86%
1.00% 87% 91%
B.R 0.25% 75% 77%
0.50% 78% 80%
1.00% 82% 83%
Graph 5-Comparison of detergency.
48
4 RESULTS AND CONCLUSIONS

1. The polymeric surfactant rosinated castor oil alkyd resin prepared on microwave
synthesis reactor can be effectively used in the liquid detergents.
2. First we try to use the resin prepared on microwave synthesis in the paint. Due to
high acid value of the resin it can be only utilized in the preparation of distemper
paint. But using the resin prepared on microwave synthesis in the distemper paint
will not be cost effective. Hence we prepared liquid detergent by neutralized the
resin.
3. Rosinated castor oil alkyd resin prepared on microwave synthesis reactor will be
effectively used as polymeric surfactant in the liquid detergent.
4. Liquid detergent prepared by the above resin is giving excellent foam height and
detergency.
5. By using this polymeric surfactant we can achieve our aim of replacing petroleum
product with the vegetable product.
6. Novel alkyd resin mainly based on castor oil and rosin has been prepared .The other
ingredients used are in a small quantities such as anhydrides (maleic anhyride ) and
glycerol.
7. In this project we have also compare the resin prepared by microwave synthesis
reactor and that prepared with conventional batch reactor process. In this
comparison the resin prepared on microwave synthesis reactor shows good
properties when used in the liquid detergent. Though the foam height of liquid
detergent prepared from both these resin is same but the liquid detergent prepared
by resin made by microwave synthesis reactor show better detergency than other
one.
8. The only problem with using this alkyd resin in the liquid detergent is that it gives
very undesirable colour to the liquid detergent.
49
5 REFERENCES
1. Taylor, C.J.A and S. Marks, Paint technology manual- part III Convertible
coatings. Chapman and Hall publications, London (1972).
2. Payne, I.I.F, Organic coating technology, Vol II, John Wiley Sons, New York (1961).
3. Taylor, C.J and Marks, O.C.C.A. Part III, Page 88-90, London (1972).
4. Taylor, C.J and Marks, O.C.C.A. Part III, Page 92-94, London (1972).
5. Zini P, “ Polymeric additives for high performing detergents” Technomic

publication Co inc Lancaster BASEL ; 1995, pp: 15-18.
6. “Detergent Additives” INFORM Vol-9, No-10 Oct.1998 pp.928.
7. Bayuy A. D. “Polymeric surfactant and their use in industrial product,” Paint India
(March 1993) pp.45-52.
8. Marcel Dekkar “Polymeric surfactant” Surfactant Science series, Vol-42, Inc

pp.165-176,203-205.
9. Annul book of ASTM Standard American society for testing and material, Vol-
6.01d, 1639-81. (1981), ASTM standard Method for acid value of organic coating
materials.
50
10. Annul book of ASTM Standard American society for testing and material, Vol-
6.01d, 1639-61. (1981) ASTM standard Method for non volatile contains of resin
solutions.
11. Annul book of ASTM standard American society for testing and material 6.01 D
1259-61 (For non volatile contains of resin), 1980.
12. Haries, “Detergency Evaluation and Testing,” Wiley-interscience Publisher 1954

pp.92-103.
13. P. S. Kalsi, “Spectroscopy of organic compound” Text book, pp: 103-104, 114, 125.
14. Brittany L. Hayes, “Microwave Synthesis Chemistry”, CEM Publication, 2002, pp:
11-25.
15. www.milestone.com
51

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Tech in Oil technology

4 Results and conclusions 48

Introduction to microwave synthesis

1. MICROWAVE CHEMCAL SYNTHESIS14:-

The difference between microwave heating and convective heating:

1.1 Microwave heating15:-

1.2 Reasons for microwave processing:-

1.3 Microwave heating mechanism:-

1.3.1 Ionic Polarization:-

1.3.2. Dipole Rotation:-

PD = 55.61 E2 ƒ K’ tanδ* 10-14 watts/cm3

Where PD = Power density

1.3.3. Penetration depth:-

1.4 Microwaves Are Energy:-

Microwaves are a form of electromagnetic energy. Microwaves, like all electromagnetic

It is useful to consider the quantum energy of microwaves in relation to other forms of

1.5 Microwaves Can Interact with Matter:-

Microwave interaction with matter is characterized by a penetration depth. That is,

1.6 Microwave Heating Differs from Conventional Means:-

1.6.1. Conventional Heating Methods:-

1.6.2. Microwave Heating:-

1.6.3. Single-Mode and Multimode Microwave Cavities:-

The working compartment where materials are exposed to microwaves is variously

(1) Single-Mode Cavities:

The essential characteristic of single-mode cavities is the deliberate creation of a standing

Several consequences of single-mode cavity design must be appreciated. First,

Single-mode cavities do not lend themselves to simultaneous processing of multiple

(II) Multimode Cavities:-

The essential characteristic of multimode cavities is the deliberate avoidance and/or

Several consequences of multimode cavity design must be appreciated. First, microwave-

1.7 MICROWAVE HEATING SYSTEM USED IN PRESENT STUDY:-

The Discover System consists of:

Optional features include:

• Fiber Optic Temperature Control System –

• Direct Pressure Control System –

• IntelliVent Pressure Control System –

Temperature Control System:-

4. Method Control Options:-

2 AIM OF PRESENT PROJECT WORK

We will try to manufacture polymeric material on microwave synthesis reactor that

Regarding microwave, we will prepare polymeric material by this method and we

3.1 PREPARATION OF RESIN

(b) Experimental formulations of rosinated Castro-alkyd resin:

Sr.No. Ingredients Formulation I(%) Formulation II(%)

3.1.1 ANALYSIS OF RESIN:-

(b) Volatile Content6:-

3.1.2 PROPERTIES OF ROSINATED CASTOR-ALKYD RESIN:-

Sr. Physical Property Observation

2 % Solid 91.25 88.56

3.2 PREPARATION OF LIQUID DETERGENT:-

Sr.No. Ingredients LD1 (%) LD2 (%)

3.2.1 ANALYSIS OF POWDER DETERGENT:-

Some effect of surface tension: -

Measurement of Surface Tension:-

The Stalgamometer Method:-

(b) Foam Height8:-

Foam is coarse of dispersion of gas in relatively small amount of liquid or it may be

(c) Percentage detergency9: -

This includes the following step

Density using density bottle

With little methanol or acetone and dry it in a current of dryer.

Where ρ is density of liquid