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ACKNOWLEDMENT

We thank to Almighty ALLAH the creator of earth and sky and all the
things in between and WHO has given us a chance to complete this
project. We would like to thank our teachers who helped us by teaching
us the aspects involved in chemical engineering due to which we become
able to design a chemical plant. We would like to thank specially our
supervisor Dr. Umar Manzoor who guided us towards the right path
throughout the project & our co-supervisor Dr. Sikandar Rafiq, who
helped us in the technical section. At end we would like to thank our
friends for their co-operation, which was really helpful.

ABSTRACT

This report includes the work done on a final year project named Production of 10
tons Zinc Stearate using Zinc Dust. Chapter one & two discusses the introduction &
literature reviewed about the project, which includes the current industrial techniques
and past practices and gives a detailed review about the product. Chapter 3 is the
detail of our selected manufacturing process and its process flow diagram. Chapter 4
is about the Material Balance, the balances around individual equipments and overall
balance. Chapter 5 calculates the duty requirements and energy balances for
individual equipments. Chapter 6 covers the design calculation & Selection criteria of
our key equipments which are reactors, centrifuge & dryer. Chapter 7 includes the
selection of construction material for our equipments. Chapter 8 is about
instrumentation and controllers needed for our process. Chapter 9 is giving estimate
cost for the production of zinc stearate on basis of our designing. Chapter 10 contains
the Safety approach. And chapter 11 covers the environmental aspects of zinc
stearate.

TABLE OF CONTENTS
CHAPTER # 1
Introduction......................................................................................................... 7
Chemical composition of zinc stearate ............................................................................................... 8
Physical properties of Zinc Stearate [2] .............................................................................................. 8
Scope ................................................................................................................................................................. 9

CHAPTER # 2
Literature Review ............................................................................................. 10
Stearate ......................................................................................................................................................... 11
Stearic Acid ................................................................................................................................................. 11
Commercial Stearic Acid [3].................................................................................................................. 11
Macro crystalline Stearic Acids [3] ..................................................................................................... 11
High Stearic Acids [3] ............................................................................................................................... 12
Economics and Performance [3] .......................................................................................................... 12
Metallic Stearates [3] ................................................................................................................................. 12
Chemistry of Metallic Stearates [3] .................................................................................................... 13
Melting Point:........................................................................................................................................ 13
Hydrophobic Nature: ......................................................................................................................... 14
Importance of Metallic Stearates [3] .................................................................................................. 14
Characteristics of Metallic Stearates ............................................................................................... 15
Lubricant................................................................................................................................................. 15
Gel .............................................................................................................................................................. 15
Inhibitor ................................................................................................................................................... 15
How Stearates are involved in Rubber Manufacturing [3] ................................................ 16
Dry Process: ........................................................................................................................................... 16
Water-cooled systems......................................................................................................................... 17
Water-Dispersible Forms ................................................................................................................. 18
Metallic Stearates:.................................................................................................................................... 19
Calcium stearate................................................................................................................................... 19
Magnesium stearates .......................................................................................................................... 20
Aluminum stearates ............................................................................................................................ 21
Lithium stearates ................................................................................................................................. 22
Sodium stearates and Sodium OleateS ....................................................................................... 22
Zinc Stearate .......................................................................................................................................... 23
Preparation of Zinc Stearate [1] .......................................................................................................... 24
Precipitation (or double-decomposition) reaction ................................................................. 24

Direct reaction .................................................................................................................................... 25


Fusion process ....................................................................................................................................... 26
AV Process: ............................................................................................................................................ 27
Applications of Zinc Stearate .............................................................................................................. 28
Paint industry ........................................................................................................................................ 28
Concrete manufacturing ................................................................................................................... 28
Lubrication ............................................................................................................................................. 28
Plastics ...................................................................................................................................................... 28
Rubbers .................................................................................................................................................... 28
Cosmetics & Pharmaceuticals: ...................................................................................................... 29
Fields of Application........................................................................................................................... 29
Building Industry................................................................................................................................. 29
Hydrophobic agents............................................................................................................................... 29
Lacquer Industry ................................................................................................................................. 29
Matting agents & abrasives................................................................................................................. 29
Lubricant Industry ............................................................................................................................. 29
Thixotropic agents for the production of lubricants and greases ............................................ 29
Rubber Industry................................................................................................................................... 29
Mold agents-Anti-tack agents ............................................................................................................ 29
Paper Industry ...................................................................................................................................... 29
Coating agents ......................................................................................................................................... 29
Metal Industry ...................................................................................................................................... 29
Lubricants for powder metallurgy .................................................................................................... 29
Pharmaceutical and Cosmetics Industry ................................................................................... 29
Mold release agents ............................................................................................................................... 29
Why we have selected zinc stearate: ................................................................................................. 30

CHAPTER # 3
Process Selection ............................................................................................... 31
Process Selection: ..................................................................................................................................... 32
Precipitation process:......................................................................................................................... 32
Process Flow DiagraM ........................................................................................................................... 35
Process Detail ............................................................................................................................................. 36
Reactor 1.................................................................................................................................................. 36
Settling Tank.......................................................................................................................................... 36
Plate & Frame Filter Press .............................................................................................................. 36
Reactor 2.................................................................................................................................................. 36
Washing Unit ......................................................................................................................................... 36

Centrifuge ............................................................................................................................................... 37
Dryer ......................................................................................................................................................... 37
High Shear Mill .................................................................................................................................... 37

CHAPTER # 4
Material Balance ............................................................................................... 38
Dryer .............................................................................................................................................................. 39
Centrifuge .................................................................................................................................................... 39
Reactor 2 ...................................................................................................................................................... 40
Filter press ................................................................................................................................................... 41
Reactor-1 ...................................................................................................................................................... 41
OVERALL BALANCE .......................................................................................................................... 42

CHAPTER # 5
Energy Balance ................................................................................................. 43
Reactor 1[11] ................................................................................................................................................. 44
Reactor 2 ...................................................................................................................................................... 45
Dryer: ............................................................................................................................................................ 46

CHAPTER # 6
Designing & Selection of Equipments............................................................. 47
Reactors ........................................................................................................................................................ 48
Reactor 1.................................................................................................................................................. 48
Reactor 2.................................................................................................................................................. 52
Centrifuge .................................................................................................................................................... 55
Dryer .............................................................................................................................................................. 58
Designing Specifications ........................................................................................................................ 62

CHAPTER # 7
Material Selection ............................................................................................. 63
CHAPTER # 8
Instrumentation & Process Control ................................................................ 66
Reactor 1 ...................................................................................................................................................... 72
Volume & Level Control .................................................................................................................. 72
Reactor 1 Composition Control ..................................................................................................... 73
Storage of Zinc Sulfate ........................................................................................................................... 74
Reactor 2 ...................................................................................................................................................... 75
Composition ........................................................................................................................................... 75
Level & Temperature......................................................................................................................... 76
Tray Dryer................................................................................................................................................... 77

CHAPTER # 9
Cost Estimation ................................................................................................. 78
CHAPTER # 10
HAZOP .................................................................. Error! Bookmark not defined.
REACTOR 1[21] ............................................................................................................................................ 83
FILTER PRESS[21] ................................................................................................................................... 84
REACTOR 2[21] ......................................................................................................................................... 86
TRAY DRYER[21] ..................................................................................................................................... 88

CHAPTER # 11
Environmental Aspects .................................................................................... 89
Routes of Exposure [9] ............................................................................................................................. 90
Effects on Humans [10] ............................................................................................................................. 90
Methods to control exposure [10] ......................................................................................................... 90

References .......................................................................................................... 91

CHAPTER # 1

INTRODUCTION

CHEMICAL COMPOSITION OF ZINC STEARATE


Zinc stearate is a chemical substance that has a white, fluffy, powdered appearance
and is usually formed from a combination of stearic acid and zinc oxide. It does not
have a strong odor, although traces of a slight fatty acid scent are not uncommon.
Zinc stearate is sometimes referred to as octa-de-canoic acid or zinc salt

SAPOCIFICATION REACTION

PHYSICAL PROPERTIES OF ZINC STEARATE


Appearance

White fine powder

Molten Form

Transparent

Density

1.095g/cm3

Metal Content%

10.0 - 11.5 %

Melting Point

120 - 130C

Boiling Point

Decomposes

Water Solubility

Insoluble

[2]

PROPERTIES OF ZINC STEARATE

ZINC STEARATE

SCOPE
According to our market survey the total demand for year 2012 was 4500 tons;
according to custom report 4000 ton was imported from China, Germany and
Indonesia, which clearly shows us the potential of manufacturing zinc stearate locally.
Our aim is to capitalize this opportunity by erecting a plant of production capacity of
3000 tons per year initially which could be further increased depending upon the
market response. According to our cost analysis report done in the proceeding
chapters per ton cost of production is 200000 PKR and its selling in open market is
285000 PKR this clearly shows us that we have a good profit margin.
Pakistan offers quiet favorable conditions for erection of such plant because of
availability of all the raw materials locally i.e. cheap labor, skilled man power and
high demand of the product. By manufacturing it locally we will sell our product at
lower cost as compared to imported ones because we wont be paying duties and our
transportation cost would be much less.

USES [2]:
The main industries which use zinc stearate as a key component in their
manufacturing processes are:

Plastics and Rubber

Coating/anti block

Paints industry

Food additives & pharmaceuticals

Metal working & powder metallurgy.

Waxes & petroleum products

Lubricant

Mold Release

Acid neutralization

Paper coating

Concrete & cement

Greases & inks.

CHAPTER # 2

LITERATURE
REVIEW

10

STEARATE
Stearates are anionic form of stearic Acid (C17H35COO), It is salt or ester of Stearic
Acid.

STEARIC ACID
Stearic Acid is long chain of hydrocarbons that contains on group of carboxylic & one
group of methyl at their both ends. The hydrocarbon chain can vary from 3 carbons to
24 carbons i.e. propionic acid to lignoceric acid resp. It is a saturated acid having
single bonds between there adjacent carbons, that is why the hydrocarbon chain is
flexible and we can roll it up like a ball or stretch it in zigzag manner.

Stearic acid is mainly found in animal oils or hydrogenated veritable oils are of length
16 20 carbons.

COMMERCIAL STEARIC ACID

[3]

Stearic acid that is used commercially cannot be used in pure state, for making soap
stearic acid used contains 30-60% of palmatic acid. In their pure state, these acids are
solid crystalline, opaque white materials having a waxy feel. The main source of
Stearic acid is animal source; small quantity of it can also be obtained from cotton
seed, corn, soya, coco and palm oils.

MACRO CRYSTALLINE STEARIC ACIDS

[3]

Stearic acids whose weight ratio of stearic to palmatic acid is 9:11 are known as
Macro crystalline Stearic acids. Commercially they were firstly produced by pressing
the fatty acids gained from animal tallow. Oleic from crystalline solid acid was
squeezed out by using technique of hydraulic pressure. The greater number of
pressings, the less oleic remained in the solid portion.

11

HIGH STEARIC ACIDS

[3]

Macro crystalline in which the ratio of stearic acid is 50% more than the other acid is
referred as High Stearates. Stearic Acid provides crystalline part a fineness and
softness so when the ratio of stearic acid is less than 50 i.e. 50:50 or 90:10, the acid
that is produces is hard, tough & microcrystalline solid.

ECONOMICS AND PERFORMANCE

[3]

Selection of stearic acid to make metallic crystals is done on the basis of their variety
of applications and cost.
In rubber industry, stearic acid used is made from triple pressed stearic process in
which stearic acid is up to 70 %. It is not possible to make weight ratio of stearic acid
more than 70% so the processes use to create high stearic content are more extensive
an add cost to the end product.

METALLIC STEARATES [3]


Most common metallic stearates are made from zinc, calcium & magnesium metals.
To make metallic stearates the salt of stearates i.e. stearic acid is used to make a soap
by replacing the carboxylic hydrogen with a metal part.
The general structure of metallic stearates is:

GENERAL STRUCTURE OF METALLIC STEARATES

12

CHEMISTRY OF METALLIC STEARATES

[3]

MELTING POINT:
The physical properties are all fairly similar between all three stearates.
The most significant property difference as it relates to the rubber release
agents is their melting points

Melting point defines the usage of product on the surface of uncured rubber.
When the rubber compounder is making stock for compression, transfer molding,
hoses or extruded profiles, the molding or cure temperature and time duration will
limit what can be used on the surface of the compound.
With the low melt point of zinc stearate, this has typically not been a problem. The
zinc stearate will melt during molding and be absorbed into the compound without
leaving discoloration or defects on the surface of the final molded rubber part.

Most stearates have:

Only Zinc stearate:

-Not well defined melt points

- liquefies upon melting.

-wide softening points


-plastic flow at soft point

13

HYDROPHOBIC NATURE
Metallic Stearates consists of long chain stable hydrocarbons. This hydrocarbon chain
structure is water insoluble so it gives hydrophobic nature of metallic stearates. The
solubility parameter values of these stearates are low, and are similar to the common
elastomers. TABLE below compares solubility parameters of these stearates to
elastomers.
Comparison of Solubility Parameters between steartes and elastomers:

IMPORTANCE OF METALLIC STEARATES

[3]

Metallic stearates can be used in different aspects in rubber industry to provide


release.
Properties like lubricity, hydrophobicity, compatibility and melt point are performing
key role to provide required rubber release agent. There variety usage and formulation
is the reason that they are used in several rubber industries.
Among the many interesting properties of metallic stearates, the most important are:
Lubricating properties
Separating properties
Water repellence
Gelling capacity
Stabilizing effect
Foam inhibition

14

CHARACTERISTICS OF METALLIC STEARATES

[3]

LUBRICANT
Main property of metallic stearates as lubricants is that they can bear high
temperature as they have relatively higher meting points as compared to other
release agents & lubricants. So metallic stearates when present in fine dry powder
from can act as dry lubricant also, like graphite. In most cases, the hydrophobic
nature of metallic stearates is highly desirable.
Lubrication and release properties, as well as water repellency, are characteristics
of all metallic stearates. In order to determine that metallic stearate is providing
the lubrication property we need to study the properties related to cations, chain
length and water of crystallization.

GEL
Gelling mainly depends on the type, polarity, viscosity of stearates as well as
solvent properties of the liquid component used. Aluminum stearates are the main
metallic stearates used for gelling property.

INHIBITOR
Calcium stearate, magnesium stearate and zinc stearate have stabilizing and
processing aid effects in a wide range of thermoplastics. Aluminum and
magnesium stearates are used as foam inhibitors for various suspensions.

15

HOW STEARATES ARE INVOLVED IN RUBBER MANUFACTURING [3]


Metallic stearates provide some unique properties that make them ideal rubber release
agents. The presence of lubricity, hydrophobicity and melt point is the reason of using
these materials in several applications. Every rubber industry needs release agent of
specific & unique property, which metallic stearates are providing them.
The most common reasons why metallic stearates are used are listed below:
Uncured rubber needs heat removed quickly, to prevent scorching, thus, the rubber
needs to be water-cooled before stacking or storage
Uncured rubber will be molded with minimal or no post milling or mixing, i.e.
compression and transfer molding.
DRY PROCESS:
Metallic stearates can be applied to rubber several ways and in different forms.

DRY PROCESS

[3]

In dry process, stearates are applied or dusted onto the surface of the rubber by
passing the rubber through a trough or box containing the stearate. This method is
dusty but provides effective dry lubricating properties to the surface of uncured
rubber.

16

WATER-COOLED SYSTEMS
Another way in which the powdered stearates are applied is in water-cooled
systems.
The stearate is mixed on the surface of dip tank on which it starts to float. The
hydrophobic nature of metallic stearates allows the powder to stay on the surface
without getting wet. This process is also effective but cause dust & health issues.
For water-cooled systems, stearates are normally provided in 20-30% active pastes.

WATER COOLED SYSTEM

[3]

The paste is made by combining stearates, water & little quantity of alcohol.
These formulations allow for stearates to be added to the dip tanks directly or can
be premixed in tanks which provide a more thorough dispersion.

FLOATABLE STEARATE DISPERSION

[3]

17

It is advised to premix these all before adding to dip tank. The benefit of using this
method is that stearate is still floating and can be used in water-cooled take-off
units. Figure 2-3 shows how these products would appear in a slab dip tank.
In floatable stearate dispersions dust problem can be minimized.
Here again the hydrophobic nature of metallic stearates is especially important
because this property allows for the cooling of rubber by water. Normal or cold
water is mainly used for heat removal.
This helps prevent scorching of these compounds before they are cured.
WATER-DISPERSIBLE FORMS
The metallic stearates are available in water-dispersible forms. These products
are normally 30-50% active and have surfactant packages that allow for
dispersibility throughout a dip tank

WATER DISPERSAL FORMS

[ 3]

18

METALLIC STEARATES:
CALCIUM STEARATE
Calcium stearates are considered as health friendly stearates so they are becoming
part of life with good speed. They are insoluble in many solvents. We need to
slightly heat them in aromatic compounds, chlorinated hydrocarbons or vegetable
and mineral oils and waxes to make them soluble. Calcium stearates are mainly
used as lubricants, mold release agents and acid scavengers by the plastics
industry. They are used as an anti-caking additive for powder and granules in
pharmaceutical and cosmetics industry and as an excipient for pressing tablets.
The building industry uses it as hydrophobic agent & as inhibitor for moisture
absorption and preservation of building materials and construction. Calcium
stearate when heated dehydrates and softens at temperatures between 120 C and
130 C and takes a viscous consistency at approx. 160 C. This state lasts whilst
the material is heated occurring some slight discoloration.

FIG 2-5 CALCIUM STEARATE

19

MAGNESIUM STEARATES
Magnesium stearates are almost insoluble in normal solvents. They can hold
large quantities of water and take on a creamy consistency. Magnesium stearates
are used to improve the retention power of creams and semi-rigid wax articles as
well as to produce waxes. Since they are also skin & body friendly, they are used
by the cosmetics and pharmaceutical industry.
Magnesium stearates improve the free-flowing properties and are added as anticaking agents to powders. One of the principle uses of magnesium stearate is as a
tablet excipient in pharmaceutical dosage forms. Thermo stable magnesium
stearates are used as lubricants and release agents for the processing of
thermoplastics and thermosets.

FIG 2-6 MAGNESIUM STEARATE

20

ALUMINUM STEARATES
Aluminum stearates are produced by the precipitation process only. There are
three possible combinations of aluminum with fatty acids:
There might be different ratios but the lies between 1:1 and 1:3. That is why there
are many varieties of aluminum stearates, generically known as aluminum mono, di- or tri-stearate, they have different physical properties such as melting point,
free fatty acid and particularly the gelling properties. Aluminum tri- and distearates are used for thickening less viscous oils, whilst very viscous oils form
stiffer gel when combined with aluminum di- or mono-stearates.
The dropping point of aluminum greases usually range from 110 C to 120 C,
but we are in a position to offer special stearates whose dropping point exceed
200 C. All aluminum greases are highly hydrophobic and are characterized by
outstanding transparency and good adhesion to metallic surfaces. Like every
metallic stearate, aluminum stearate is also good water repellent. So we can use
them in coatings and building industry materials as water repellent ingredients.
Aluminum mono-, di- and tri-stearates are insoluble in many solvents like water,
lower alcohols, esters and ketones.
In benzenes, aromatic compounds and halogenated hydrocarbons as well as in
natural and mineral oils, they dissolve to a gel when heated.

FIG 2-7 ALUMINUM STEARATE

21

LITHIUM STEARATES
Lithium stearates are best known for their excellent swelling properties. They
work better than aluminum stearates because properties like dropping point
temperatures of greases containing lithium stearates are much higher than those
of aluminum stearates. Lithium stearates are mostly used to thicken natural as
well as synthetic oils and help to increase the melting point and flexibility of
micro-crystalline waxes and paraffins. They are also used during the production
of light weight metal moldings. The advantage of lithium stearates with long fatty
acid chain lengths is the minimal residue after thermal treatment.

LITHIUM STEARATE

SODIUM STEARATES AND SODIUM OLEATES


We can produce Sodium stearates and oleates by direct reaction according to a
Baerlocher patented process. Possible applications of these products are e.g.
swelling of alcohols, lubrication and nucleating during the processing of
thermoplastics.
Sodium oleates are mainly used as hydrophobic agents for building plasters,
where homogenous dispersion is easily obtained due to its solubility in water.
Due to alkaline components of the plaster and the sodium stearate forms a
calcium stearate which is also finely dispersed, thus imparting high waterrepellency properties to the paste.

SODIUM STEARATE

22

ZINC STEARATE
Zinc stearate is a chemical compound that is white in color, has a fluffy powdered
appearance and is usually formed from a combination of stearic acid and zinc
oxide. It does not have a strong odor, although traces of a slight fatty acid scent
are not uncommon. Zinc stearate is also known as octa-de-canoic acid or zinc
salt.

ZINC STEARATE

CHEMISTRY OF ZINC STEARATES

[1]

-It is insoluble in non polar solvents such as alcohol and ether but becomes soluble in
aromatic hydrocarbons (e.g., benzene and chlorinated hydrocarbons) when heated.
-It is the strongest mold release agent among all metal soaps. It contains no electrolyte
and has a hydrophobic effect like other metallic stearates.
-It is mainly applied in the plastics and rubber industry where it is used as a releasing
agent and lubricant which can be easily incorporated.
-Its hydrophobic nature also makes it suitable for many different kinds of
applications.
-In order to make plastics, zinc stearate is combined with a co-stabilizing soap called
Ba-Cd[2] that helps to stabilize the plastic. It does this by mixing with the liquid,
which helps make the material more fluid called a plasticizer.
In paint and coatings industry zinc stearates are used for pigment suspension and to
improve grind ability and matting. The building industry uses powdered, precipitated
zinc stearates as hydrophobic agents for plasters.

23

PREPARATION OF ZINC STEARATE

[1]

PRECIPITATION (OR DOUBLE-DECOMPOSITION) REACTION


The fatty acid i.e. stearic acid is first saponified in large volume of hot water with an
equi-molar to a slight excess quantity of a strong alkali solution (sodium hydroxide,
caustic potash solution, ammonia). The resulting alkali stearate is hydrophilic.
Particle size, surface area and particle morphology or shape is influenced by the
concentration of reactants and precipitation rates. To get smaller particles and the
larger surface area, the dilution of saponified fatty acid should be high. These
properties determine the bulk (apparent) density, which is normally low for
precipitated metallic stearates.
The desired hydrophobic metallic stearate is then produced by adding a metal salt
solution (e.g. calcium chloride solution, aluminum sulfate solution). The hydrophilic
salts are also produced as by products such as sodium chloride or sodium sulfate, they
must be removed from the metallic stearate by filtration and washing. At the end, the
final desired product must be dried and the de-agglomerated or milled.
Double-decomposition reaction generally produces very light, fine powders with a
large surface area and a more platelet morphology. The metallic stearates produced
are used in applications requiring fine particle size and high surface area for the best
lubrication and release properties and where special emphasis is placed on good
hydrophobic properties.

Precipitated stearate characteristics

Smaller average particle size (4 - 10 um)


Limited control of particle size

Higher Purity for Ca and Mg


More impurities washed away

Lower Production Rate


Higher energy usage

24

DIRECT REACTION
In this method, reaction between stearic acid and metal oxide, hydroxide or carbonate
takes place at an elevated temperature in presence of large excess of water. Particle
size, and thus particle surface and bulk weight are influenced by the relation of stearic
acid to water. The higher the dilution, the smaller the particles and the larger the
surface will be. The metallic stearates produced by direct reaction are also relatively
fine powders with a high degree of purity, being free of water-soluble salts.
The reaction takes place at atmospheric pressure, but an advantage of this method is
that it can also be run under pressure and at higher temperatures (> 100 C) to
produce certain types of metallic stearates, which cannot normally be obtained under
atmospheric conditions by the direct reaction process. The product must be filtered
and dried to the final desired moisture content. Direct reaction in water generally
produces a more rounded, agglomerated particle, with higher bulk density than
precipitated stearates.

In this reaction calcium can be replaced by zinc [8]

25

FUSION PROCESS
In this method, metal oxides or hydroxides and stearic acid are heated under pressure
with continual stirring beyond the melting point of the metallic stearate product. As
the melting point of most metallic stearates is higher than 100 C, that is why water
resulting from the reaction escapes as steam and we get a dry product. A variety of
physical forms can be produced from this process, depending on the melting range of
the final product. For relatively low or sharp melting metallic stearates, all forms
(pastilles, prills, flakes and powder) are generally feasible. A very high degree of
purity is achievable with the fusion process.
This method is efficient because no drying is required

Fused stearate characteristics

Larger average particle size


Higher bulk density (up to 48 lb/ft3)
More controllable particle size

May contain metal oxide/hydroxides


More impurities remain

Higher production rate


Lower energy usage

Method for alkali metal salts (Li, Na, K)

Fused products can be made with near precipitation quality

Specific raw materials


Example; synthetic ZnO

Improved processing

Special fused techniques

Complete reaction

Grind to desired particle size

26

AV PROCESS:
This method is the combination of direct reaction and fusion processes. Metal oxides
or hydroxides are heated with a fatty acid and a small quantity of water in a
pressurized reactor, with the final temperature corresponding more or less to the
melting point of the soap. The added water and the water resulting from the reaction
are removed under reduced pressure at the end of the reaction cycle.
The AV process allows the very efficient production of a variety of stoichiometries,
including very pure products. AV technology is generally used to produce metallic
stearates in free-flowing granule or powder forms

In this reaction magnesium can be replaced by zinc [9]

27

APPLICATIONS OF ZINC STEARATE


PAINT INDUSTRY
It has a use in the paint industry where zinc stearate is added to lacquers and paint
coatings for use as a flatting and sanding agent.
CONCRETE MANUFACTURING
For concrete manufacturing, it is mixed as an additive for waterproofing
concrete; this same process is also used to waterproof other products, such as,
rock wools, textiles, and paper products.
LUBRICATION
Even when left in powdered form, it can be used as a drying lubricant or dusting
agent for rubber products.
PLASTICS
Zinc Stearate is one of the most widely used additives in the plastics field. It
serves primarily as a lubricant, but also as a densifying agent and a partitioning
agent. It is used extensively in color concentrates as a dispersion aid. It is used to
improve processing of the styrenics and polyesters, and to a lesser extent with the
olefins. The outstanding clarity and heat stability properties of our crystal clear
zinc stearate grades make them particularly suitable for impact and crystal grade
polystyrene and other clear polymers.
RUBBERS
In rubber applications, it functions as an elastomers processing aid and release
agent. It has been found that formulations can be modified with zinc stearate to
reduce mold sticking without adversely affecting physical properties. External
mold release spray systems can still be used in conjunction with the internal zinc
stearate mold release agent.

28

COSMETICS & PHARMACEUTICALS:


Due to their outstanding lubrication and release properties, their thixotropic effect
and their capacity for gelation, zinc stearates are used by the pharmaceutical and
cosmetics industry. Their lubricating and release properties are utilized during
drage preparation and tablet pressing, whilst their gelation capacities assist in
the production of creams and ointments. The hydrophobic properties of zinc
stearates prevent pharmaceutical and cosmetic products in powder form from
absorbing water and thus from forming agglomerates.
Additionally, metallic stearates are used in shampoos, eyeliners, lipsticks, sun
protective lotions, medicated ointments, body and foot powders, etc. Although
metallic stearates are added to these articles in relatively low dosages ranging
from 0.05 to 1 %, significant volumes of metallic stearates are required for this
application in Europe alone.
Zinc stearate functions as an acid scavenger and processing aid in certain
polyolefin applications.

FIELDS OF APPLICATION

BUILDING INDUSTRY

HYDROPHOBIC AGENTS

LACQUER INDUSTRY

MATTING AGENTS & ABRASIVES

LUBRICANT INDUSTRY

THIXOTROPIC AGENTS FOR THE


PRODUCTION OF LUBRICANTS AND
GREASES

RUBBER INDUSTRY

MOLD AGENTS-ANTI-TACK AGENTS

PAPER INDUSTRY

COATING AGENTS

METAL INDUSTRY

LUBRICANTS FOR POWDER


METALLURGY

PHARMACEUTICAL AND
COSMETICS INDUSTRY

MOLD RELEASE AGENTS

29

WHY WE HAVE SELECTED ZINC STEARATE:

We have selected this project of producing zinc stearate because it is most widely
used stearate in paint, polymers, paper & rubber industry. It gives us a good profit
margin which makes its production feasible and it is required in our local market.
All the raw materials for manufacturing are easily available in local market.
Although all the stearates have their own uses but nowadays our major concern is
environment & safety of the labor, production of some stearates carrying heavy
metals like lead & cadmium is prohibited in many countries due to their cancer
causing tendencies.

30

CHAPTER # 3

PROCESS
SELECTION

31

PROCESS SELECTION:
Several factors affect making a decision for selecting a manufacturing process, the
most important factor is the end to which the metallic soap will be subjected.
For example; in the metallic soap used for making plastics & rubber needs almost
zero moisture & salt content is needed. For these requirements, Fusion process is the
best. On the other hand for the application in cosmetic industry, fine particle size and
fluffy product is needed & these requirements lead to the precipitation process.
Economics is also a major factor in choosing a process.
In our case we are choosing precipitation process, although it is a bit expensive than
the fusion process yet its merits are for more. We can obtain a very high quality
product by this method of we are using quality raw materials & are carefully
following the procedure.
PRECIPITATION PROCESS:
This is a 2 stage process
Sodium salt of fatty acid is prepared by treating caustic soda (at 800C) with stearic
acid that produces sodium salt. The stoichiometric amount of solid stearic acid is
mixed in caustic soda with vigorous stirring.
In other reaction 10-20% metallic salt solution is prepared; this salt is added gradually
in the precipitation tank. When the reaction is finished the resultant is filtered &
washed then can be dried in the tray dryer
The dried cake may be ground to fine powder; the resulting powder is fine, white &
light

C17H35COOH

NaOH

C17H35COONa

Stearic acid

Caustic Soda

Sodium Soap

C17H35COONa

ZnSO4

(C17H35COO)2Zn

Sodium Soap

Zinc Sulfate

H2 O
Na2SO4

Zinc Stearate

32

NUTRALIZATION OF FATTY ACIDS:


When neutralizing liquid acids a final soap concentration of 20-25% is satisfactory,
but for solid acids concentration must be reduced up to 10 %.

After approx half the water needed is run into the reaction vessel then caustic
soda is added

The barrel or drum containing the fatty acid is rolled over the dumping pit and
allowed to be drain

The steam is turned on slightly & the fatty acid is pumped to the reaction
vessel with the pumps throttled so that the fatty acid entering the lye in the
kettle is easily dispersed by swallowing liquid

After all the fatty acid is added steam agitation is continued until a clean liquid
is produced

The bottom valve in the tank is opened & the pump is started again to wash
out the lines still containing fatty acids, the soap in the kettle is tested with
phenolphthalein indicator, a slightly pink color shows neutral soap

The soap is diluted to a proper concentration while agitating. If the solid acid
is used they are added directly to control conc. of caustic soda

HYDROLYSIS:
If the sodium soaps are highly hydrolyzed one would expect to find much metal
hydrate as well as free fatty acid in the precipitated soap. Mc Bain and Hey found that
hydrolysis depends on the molecular mass of the fatty acid. The higher the soap in the
homologous series the higher will be hydrolysis. In conc. Solutions there is less
hydrolysis
PRECIPITATION OF METALLIC SOAP:
There are three different methods of precipitation of metallic soaps:
1- ADDITION OF SOAP TO SALT SOLUTION:
The solution of metallic soap is slowly added to the salt solution while agitating. If the
temperature of the soap is high enough and stirring sufficient, a very finely divided
suspension of metallic soap in the alkali soap slowly forms until much of the latter has
been precipitated at which point the mass coalesces. If salt solution is added too
quickly or if temperature is too low then very viscous, unworkable mass which is
certain to occlude large quantity of soap and alkali salt results. This alkali soap cannot

33

be removed even ob repeated washings. Because of this the finished metallic soap
tends to sludge when dissolved in hydrocarbons
2- ADDITION OF SALT TO SOAP SOLUTION::
The alkali soap solution may be slowly added to the metal salt solution while
agitating. If soap is slowly added and the temperature is high enough then a layer of
molten metallic soap which is quite workable and is not excessively hydrated forms a
precipitation progress. If the soap is added too quickly and temperature is kept low
then unworkable mass will be produced.

3- ADDITION OF SOAP & SALT TO WATER:


There is another method which will minimize the faults of other two and make it
possible to make a very pure soap. The hot alkali salt and hot soap metal solutions are
added at a constant rate to a bath of clean hot water which is being agitated. During
agitation, slight excess of soap or metal salt is maintained in the tank depending on
whether the traces of alkali soap or metal salt are preferred. The advantage of this
process is obvious that there is very rare possibility of occlusion of alkali soap or
metal salt in the metallic soap. The disadvantage lies in needing the extra tank for
precipitation, thus adding to the cost of the plant
The final selection is based on how high the quality of soap is required.

WASHING & DRYING:


After precipitation, the smooth pasty metallic salt pulp is then pumped in the press of
large capacity and washed until the filtrate is free of sodium salts. Air blowing is
usually used to remove the moisture. The material removed from press is spread on
trays and dried. Because of nature of precipitate most of the product dries quite well
but sintering of particles and discoloration are important factors limiting the use of
high temperature drying. Thus long drying period with resulting decrease in
production capacity is necessary. This is one of the factors that raise the production
cost

34

PROCESS FLOW DIAGRAM

35

PROCESS DETAIL
REACTOR 1
In reactor # 1, Zinc Oxide along with 16% excess sulfuric acid are fed, reaction takes
place between them at room temperature but due to exothermic nature of this reaction
temperature of reactor rises up to (1700C). After 90% completion of reaction product
is formed that is zinc sulfate with water. This zinc sulfate is in form of slurry that
contains impurities & 10% unreacted reactants.
SETTLING TANK
The products are then entered in settling tank where the product cools down to room
temperature and settling occurs for about 3 to 4 hours. Due to density difference the
impurities and unreacted metal oxide settles and the zinc sulfate slurry is pumped to
plate and frame filter press
PLATE & FRAME FILTER PRESS
Zinc sulfate slurry is entered in filter press where the mud and unsettled impurities are
filtered; this feed contains 75% zinc sulfate and 25% of mud. It filters 95% of zinc
sulfate 5% is mud. Mud is separated here, Zinc sulfate is sent to a tank.
REACTOR 2
In reactor 2, two reactions are taking place. In first reaction caustic soda reacts with
17% excess stearic acid this reaction takes place at room temperature and 90% of
reactants converts into sodium stearate and water.
When the reaction is complete then zinc sulfate is added gradually in the reactor that
reacts with sodium stearate, heat is provided for starting the reaction and stirring is
done continuously for proper reaction. This second reaction also completes 90% and
then converts into zinc stearate of mass along with sodium sulfate.
WASHING UNIT
The products are allowed to cool down by adding cold water in the reactor. Sodium
sulfate, water and unreacted masses are dissolved in added water only zinc stearate
slurry is separated from reactor because it is hydrophobic by nature.

36

CENTRIFUGE
In centrifuge zinc stearate is entered that contains 60% moisture and 40% zinc
stearate. Centrifuge works on the principle of centrifugal force and helps to remove
the moisture and the zinc stearate at the end contains only 30% moisture.
DRYER
Zinc stearate containing 30% moisture is entered in tray and shelf dryer at room
temperature and air is used for purpose of drying. Air at 1300C is entered in the dryer,
this is basically batch drying process and drying is taking place by conduction.
Slurry is placed on hot trays at room temperature but due to contact with hot trays the
moisture starts to evaporate and after complete evaporation of moisture from initial
moisture temperature of zinc stearate raises up to 110oC; dried product contains 3%
inherent moisture which was not removed by evaporation.
Now zinc stearate is in form of solid granules which are stored in storage silo to cool
them down at room temperature
HIGH SHEAR MILL
Zinc Stearate in form of granules is entered in high shear mill which simply crush
them in to small size and final product in form of powder is collected.

37

CHAPTER # 4

MATERIAL BALANCE

38

DRYER
Product (F3) containing 70% Zinc Stearate and 30% moisture is entering to give
product (F1) containing 97% Zinc Stearate. Water (F2) is removed separately
F3 = F1 + F2
Applying balance on Zinc Stearate;
F1= 10000 kg
We get

Applying balance on Zinc Stearate;

F3 = 13857 kg product (centrifuge)

From this we get F2 = 3857 kg water

F1
F2
F3

Zinc Stearate(kg)
9700
0
9700

Water(kg)
300
3857.142857
4157.14286

Total (kg)
10000
3857.142857
13857.14286

CENTRIFUGE
Product (F5) containing 40% Zinc Stearate and 60% moisture is entering to give
product of (F3) containing 70% Zinc Stearate. Water (F4) is removed separately

F5 = F3 + F4

We calculated F3 = 13857kg
We get

Applying Balance on Zinc Stearate;

F5 = 24250kg product

From this we get

F3
F4
F5

F4 = 10392.85 kg water.

Zinc Stearate(kg)
9700
0
9700

Water(kg)
4157.142857
10392.85714
14550

Total (kg)
13857.14286
10392.85714
24250

39

REACTOR 2
Stearic Acid (F7) and Caustic soda (F8) reacts to form Sodium stearate which
then reacts with zinc sulfate (F5) to form Zinc Stearate (F9), Sodium Sulfate
(F10) & water (F11)
2 C17H35COOH + 2 NaOH
2 C17H35COONa + ZnSO4
2 C17H35COOH + 2 NaOH + ZnSO4

2 C17H35COONa + 2H20

(C17H35COO) 2 Zn + Na2SO4

(C17H35COO) 2 Zn + Na2SO4 + 2H20

F5 + F7 + F8 F9 + F10 + F11

We get;

We have

F5 =9700 kg Zinc Stearate & Reaction conversion is 90 %

So originally zinc stearate produced

= 9700/0.90

= 10777kg

Moles of zinc stearate

=10777/631

= 17.08kgmoles

Taking Stearaic acid in excess 17% and 17000kg of water is added in the stearic acid
to provide reaction medium
Components

Moles
(kgmole)

Moles in
Reaction
(kgmole)

Molecular
mass
(kg/kgmol)

Mass in
Reaction(kg)

Inlet
F9
F6
F7

ZnSO4
NaOH
C17H35COOH

1
2
2

17.08047191
34.16094383
39.96830428

161
40
284

2749.955978
1366.437753
11350.99842

FM

C17H35COONa

34.16094383

294

9038.985737

945.9165346

18

17026.49762

H2 0
Total
Outlet
S.S

41532.87551
3031.100546
1

17.08047191

631

9700

F10

Reactants
(C17H35COO) 2
Zn
Na2SO4

17.08047191

142

2182.884311

F8

H2 0

34.16094383

18

17579.90491

FM
Total

C17H35COONa

34.16094383

294

9038.985737

F5

41532.87551

40

FILTER PRESS
Product (F12) containing 75% Zinc Sulfate and 25% Mud is entered in a filter
press that gives product (F9) containing 95 % Zinc Sulfate and Mud (F11) which
is separated.
F12 = F9 + F11
Applying balance on Zinc Sulfate;

where F9 = 2749.95kg

By putting in main balance eq. we get


We get F12 = 3483.277 kg
F12
F9
F11

F11 = 733.32 kg mud

Zinc Sulfate (kg)


2612.458179
2612.458179
0

Mud (kg)
870.819393
137.4977989
733.3215942

Total(kg)
3483.277572
2749.955978
733.3215942

REACTOR-1
Zinc Oxide (F14) is reacted with Sulfuric acid (F15) to produce Zinc Sulfate
(F12) and Water (F13)
ZnO + H2SO4 ZnSO4 + H2O
We know F12= ZnSO4 = 2612.45 kg

Reaction conversion is 90 %

Originally Produces Zinc Sulfate =

2612.45/0.90

=2902.722kg

Moles of Zinc Sulfate Produced =

2902.722/161

=18.02kgmoles

Taking 16% excess sulfuric acid =

18.02*1.16

=20.9kgmoles

Inlet
F14
F15

Components

Moles
(kgmole)

Moles in
Reaction
(kgmole)

Molecular
mass
(kg/kgmol)

Mass in
Reaction(kg)

ZnO
H2SO4

1
1

18.02938702
20.91408894

81
98

1460.380349
2049.580716

MUD
Total
Outlet
S.S
F12
F13
Total

1393.311029
4903.272094

Reactants1
ZnSO4
H2O
MUD

18.02938702

161

18.02938702

18

605.4268161
2612.458179
292.0760697
1393.311029
4903.272094

41

OVERALL BALANCE

Components

Molecular
Mass

Mass In Reaction
(kg)

F14

ZnO

81

1460.380349

F15

H2SO4

98

2049.580716

F6

NaOH

40

1366.437753

F7

C17H35COOH

284

11350.99842

in R2
In
washing
unit

H2 0

18

17026.49762

Inlet

H2 0

14550

Mud

1393.311029
49197.20589

Total
Outlet
S.S(R1)
F13
F11
From
settling
Tank
SS(R2)
F10

MUD

522.4916359

Na2SO4

3031.100546
2182.884311

F8

H2 0

18

17579.90491

F4
F1
F2
Total

H2 0
(C17H35COO) 2 Zn
H2 0

18
631
18

10392.85714
10000
3857.142857

H2 0
Mud

18

605.4268161
292.0760697
733.3215942

49197.20589

42

CHAPTER # 5

ENERGY BALANCE

43

REACTOR 1 [11]
Zinc Oxide and Sulfuric acid are reacting, this reaction takes place at 300C but due to
exothermic reaction the reactor temperature rises up to 1700C, the product zinc sulfate
in the form of muddy solution is obtained

Applying Energy Balance: mcpdT

Enthalpy
Tref

T2

Cp

[13]

Mass

Moles

(kg)

(kmol) (OC) (OC) (kJ/kg OC)

Heat (Q)

Enthalpy

of

(kJ)

(kJ/kg)

Formation
(kJ)

zinc oxide

1460

18

25

30

0.52

3796

2.6

-348

sulfuric acid

2049

20

25

30

1.704

17457

8.52

-814

Heat IN

21433

zinc sulfate

2612

18

60

170

1.39

399374

152.9

-983

water

292

18

60

170

4.18

134261

459.8

-285.8

Heat OUT

Heat of Reaction [14]

533635

Products

Reactants

(-983-285)

(-348-814)

-1268

-1162

-106kJ

As heat of reaction is negative so reaction is exothermic

44

REACTOR 2
Stearic Acid is solid form it is mixed with hot water to convert in liquid form. Caustic
soda reacts with stearic acid and form sodium stearate, this sodium stearate reacts
with zinc sulfate produced in reactor 1 and gives our main product zinc stearate along
with sodium sulfate and water. The temperature of reactor rises up to 120oC
2 C17H35COOH + 2 NaOH
2 C17H35COONa + ZnSO4

2 C17H35COOH + 2 NaOH + ZnSO4

2 C17H35COONa + 2H20

(C17H35COO) 2 Zn + Na2SO4

(C17H35COO) 2 Zn + Na2SO4 + 2H20

For Reaction 1:
Enthalpy of formation for C17H35COONa = -1978kJ
Hr

=Products Reactants = (-1978-571.6)-(-851.84-1896)=

198.24Kj

So this is endothermic reaction and we have to provide heat to start this reaction
For Reaction 2:
Hr

=Products Reactants = (-1686-1387)-(-1978-983) =

-112kJ

So this is exothermic reaction and heat will be generated during this reaction
For Overall Reaction:
Hr

=Products Reactants = (-1686-1387-571.6)-(-1896-851.84-983) =86.24kJ

Overall the reaction is endothermic


Enthalpy
Mass

Mole

Tref

T2

Cp[13]

Heat

of

(kg)

(kmol)

(OC)

(OC)

(kJ/kg OC)

(kJ)

Formation
(kJ)

water

17026

945

25

120

4.18

6761024

caustic soda

1366

34

25

120

1.3

168701

-851.84

stearic acid

11350

39

25

120

1.8

1940850

-1896

zinc sulfate

2749

17

25

120

0.97

253320

-983

Heat IN

9123895

water

17579

976

25

120

4.18

6980620

-571.6

zinc stearate

9700

17

25

40

2.79

405945

-1686

sodium sulfate

2182

17

25

40

1.29

42221

-1387

Heat OUT

7428786

45

DRYER:
Moist Product is entering in the dryer at room temperature along with hot air
(1300C), dry product is obtained at 1100C along with water, and air is removed at
303K

Mass
(kg/day)

Tref

Cp[13]

(0C) (0C) (KJ/kg0C)

zinc stearate

13857

30

air

8574

130

water

3857

60

zinc stearate

10000

60

air

8574

Heat Required for Drying

T2

50

Enthalpy
(KJ/kg)

Heat (kJ/day)

2.79

55.8

1.01

404

110

3.42

171

806113

110

2.79

139.5

1395000

30

303

3463944kg/day

773220

(From Designing Data)

46

CHAPTER # 6

DESIGNING
&
EQUIPMENT SELECTION

47

REACTORS
We are producing 10 ton zinc stearate per day; it is not a very large quantity so batch
reactor is sufficient for our process. In batch reactor we can achieve high conversion.
Quality of product can be improved in batch reactor as after every batch we can clean
it and remove any impurities, which in case of continuous reactor is difficult to do.
As the reaction time is high (30-45 min) if we choose continuous reactor, its length
would be quite large and would require a large area for it.
Our drying time is high; if we choose a continuous process material will start
accumulating before the dryer.
REACTOR 1
Data:
Comp.

Density

Mass
(kg)

Volume

(kg/m )

Moles
(kgmole)

(m3)

Inlet
F1

ZnO

5606

18.0246914

1460

0.26043525

F2

H2SO4

1800

20.9081633

2049

1.13833333

3509

1.39876858

Total

7406

CAO= moles of ZnO/Total Volume =18.02/1.39

=12.89kmol/m3

Design equation:
d CA/ dt = -rA[15]
We have taken H2SO4 in excess & by assuming first order reaction
dCA/dt = -KCA
dCA/dt = -Kdt
When; t=0, CA = CAO;

integrating & applying limits

We get

t[15]

= (ln(CAO/CA))/k -------- (1)

As we know

CA

=CAO (1-X) [15]

CA

=12.89(1-0.90)

CA

=1.289kmol/m3

assume X

=90%

48

Suppose K=0.05/min;

now by using equation (1)


tr

=(ln(12.89/1.289))/0.05

tr

=45min

Filling Time =

tf

= 120min = 2hr @ 1754.5kg/hr

Reaction time=

tr

=45 min

Cleaning Time =

tc

=120 min

Total time = tf+tr+tc=

TB

=4.75hrs

Total Volume of Reactor [15] = (Mass flow rate * TB)/Density of feed


= (3509*4.75)/ (7406) = 1.129m3
Allowing 30% of volume of fluid as the free space in the reactor
Final Volume =

Vf = 1.129*1.30= 1.468m3

Dimensions:
H/D = 1.5
VF=3.14*L*(D2)/4)
D3= (1.468*4)/(1.5*3.14) =1.24m3
D=1.07m
H=1.5*1.07m
H=1.614m

Height increased up to 30% =1.614*1.30 =2.09m


Total Pressure = Static Pressure + working Pressure
Static Pressure = density * g * H

Working pressure =
Total Pressure=

Ps=

7406*9.8*2.09/1000

Ps=

152.336kPa

Pw=

335kPa

=152+335=

487.46kPa

30% allowance for the pressure =


487*1.30 = 633kPa

Corrosion Allowance for carbon & alloy steel:


C=2mm

49

By Coulson Volume 6; when vessel diameter is 1.60m than maximum thickness is


7mm [16]
Therefore wall thickness =

2mm+7mm =9mm = 0.009m

Outside diameter =

Di + 2(thickness)
= 1.07m+2(0.009) m = 1.09m

Mechanical Design:
Agitator Dimensions: [17]
Impeller Diameter =Da=

Dt/3

= 1.07/3

= 0.35m

Impeller height above vessel floor=E=Da

=0.35m

Length of Impeller blade=L=

Da/4

=1.07/4

=0.26m

Width of impeller blade=W=

Da/5

=0.35/5

=0.07m

As our reactor is not very big so 1 impeller will be enough for proper mixing or
stirring

Designing of Cooling Jacket:


Mass (kg)

Moles
(kmol)

T1 (OC) T2(OC)

Cp

Heat

(kJ/kg OC)

(kJ)

ZnO

1460

60

25

30

0.52

3796

H2SO4

2049

70

25

30

1.704

17457

Total

21253

Zn SO4

2612.5

60

60

170

1.39

399374

H2 O

292.07

60

60

170

4.18

134583
533957

Qout= 148 kj/s = 506093 Btu/hr

50

Pipe Dimensions [18] Table 11:


Nominal pipe size

= 1 in

OD

= 1.05 in

ID

=0.824 in

Flow area

= 0.534 in2

External surface/lin ft

=0.344ft2/ft

Overall heat transfer coefficient [18] Table 8


U=250 btu/hr.ft2.oF it

= 1.4 joule/s.m2.K
Q=UA*delta T[18]
A=Q/U*delta T

A= (heat transfer)

=18.403 ft2

Per turn = pie *0.8 * 0.5

=1.5 ft2

No. of turns = 18/1.5

=12 turns

Dia of reactor =1.07m

=3.5 ft

L= pie*D*no. of turns

=132 ft

Pressure drop

[18]

M= Q/cp(delta T)
M=506093/0.999(104-77)

=18777 lb/hr

V=M/density=18777/62.5

=0.08 ft3/s

Velocity=(V/Flow Area)

=5.71 ft/s

G=M/flow area
G=M/Flow Area

=1341214 lb/hr.ft2

Viscosity=u

=1.96lb/ft.hr

Equivalent diameter

=0.05

Reynolds number = GD/u

=34567

=0.006

=11.95 ft

Pressure Drop

=5 psi

51

REACTOR 2
Data; Reaction 1:
Density

Mass
(kg)

Volume

(kg/m )

Moles
(kgmole)

C17H35COOH

1103

39.9683028

11351

10.2910227

NaOH
water

2130
1000
3233

34.16075
945.888889

Comp.
Inlet
F1
F2
Total
CAO

= moles of NaOH/Total Volume

(m3)

1366.43 0.64151643
17026
17.026
29743.43 27.9585391
=1.22kmol/m3

=34.16/27.958

Design equation:
d CA/ dt = -rA[15]
We have taken C17H35COOH in excess & by assuming first order reaction
dCA/dt = -KCA
dCA/dt = -Kdt
When; t=0, CA = CAO;

integrating & applying limits

We get

t= (ln(CAO/CA))/k -------- (1) [15]

As we know

CA=CAO (1-X)

assume X

=90%
CA=1.22(1-0.90)
CA =0.122kmol/m3
Suppose K=0.05/min;

now by using equation (1)


tr=(ln(3.12/0.312))/0.05
tr= 46.05min

Filling Time =

tf =180min = 3hr @ 9914kg/hr

Reaction time=

tr =46 min

Cleaning Time =

tc =0 min (No Cleaning)

Total time = tf+tr+tc =

TB1=3.76hrs

52

Data; Reaction 2:
Density

Comp.

(kg/m )

Moles
(kgmole)

Mass
(kg)

Volume
(m3)

Inlet
F1

C17H35COONa

1103

30.7448299 9038.98

F2

ZnSO4

3540

17.0804658 2749.96 0.77682

4643

11788.9 8.97173

Total
CBO

= moles of ZnSO4 /Total Volume

8.1949

=1.906kmol/m3

=17.08/8.97

Design equation:
d CB/ dt = -rA
We have taken C17H35COOH in excess & by assuming first order reaction
dCB/dt = -KCB
dCB/dt = -Kdt
When; t=0, CB = CBO;

integrating & applying limits

We get

t= (ln(CBO/CB))/k -------- (1)

As we know

CB=CBO (1-X)

assume X

=90%
CA=1.906(1-0.90)
CA =0.1906kmol/m3
Suppose K=0.08/min;

now by using equation (1)


tr=(ln(1.906/0.1906))/0.08
tr= 28.78min

Filling Time =

tf =60min @ 2749kg/hr, as only zinc sulfate is entering

Reaction time=

tr =28 min

Cleaning Time =

tc =90 min
te= 120min

Total time = tf+tr+tc+ te =

TB2=5hrs

Total Volume of Reactor

= (Mass flow rate * TB)/Density of feed


= ((9914+2749)*(3.75+5))/ (1103+1000+2130+3540)
=14.20m3

Allowing 40% of volume of fluid as the free space in the reactor

53

Final Volume =

Vf = 14.20*1.4

Dimensions:

H/D = 1.5

= 19.88m3

VF=

3.14*L*(D2)/4)

D3=

(19.88*4)/(1.5*3.14) = 16.88m3

D=

2.56m

H=

1.5*2.56m

H=

3.84m

Height of dashed bottom is 10% more so H =3.84*1.10 = 4.23m


Total Pressure = Static Pressure + working Pressure
Static Pressure = density * g * H
Ps=

3233*9.8*4.23/1000

Ps=

134kPa

Pw=

295kPa

134+295 =

429kPa

Working pressure =
Total Pressure=

30% allowance for the pressure =


429*1.30 =557.93kPa

Corrosion Allowance for carbon & alloy steel:


C=2mm
when vessel dia is 3.15m than maximum thickness is 12mm[16]
Therefore wall thickness =

2mm+12mm = 14mm = 0.014m

Outside diameter =

Di + 2(thickness)
= 2.56m+2(0.014) m = 2.58m

Mechanical Design:
Agitator Dimensions:
Impeller Diameter =Da=

Dt/3

= 2.56/3

Impeller height above vessel floor=E=Da

= 0.85m
=0.85m

Length of Impeller blade=L=

Da/4

=2.56/4

=0.64m

Width of impeller blade=W=

Da/5

=0.85/5

=0.17m

As our reactor is not very big so 1 impeller will be enough for proper mixing or
stirring

54

CENTRIFUGE

Zinc Stearate(kg)

Water(kg)

Total (kg)

F3

9700

4157.142857

13857.14286

F4

10392.85714

10392.85714

F5

9700

14550

24250

Mass flow rate

24250/24

1010.41kg/hr

Feed entering

1010.41kg/hr

Density of feed

1020kg/m3

Volume of feed

0.99m3/hr

Volume of centrifuge

1.25*0.99 = 1.23 m3

Calculations of Volume of Centrifuge

Calculations of Diameter & height [17]


V

2
D H
4

H/D

0.625

D3

2.52m3

1.36m

&

0.85m

0.68 m

msolid

577.37 kg/hr

solid

1100 kg/m3

Vsolid

0.52 m3/hr

Vsolid

H (R2 IRC2)

IRC

0.52m

Thickness of cake=R IRC

0.68 0.52

.16 m

16 cm

Thickness of Cake
R

D/2

Calculation of Inner Radius of Slurry (IRS)


Volume of slurry

H (R2 IRS2)

IRS

0.30m

55

Relative Centrifugal Force (RCF)


=

0.000142 n2D

0.000142 (1000)2 1.36

190.66 g

1
2 (R 2 IRS 2 )
2

2.205 106N.m2

Diameter of hole

5 mm

Area for one hole

0.0000196m2

Total Area available

DH

3.14 1.36*0.85

3.63 m2

No. of holes

3.63
0.0000196

No. of holes/m2

2500

Moment of inertia of feed

IF =

Where

Radius of Basket

R1

R e (e is thickness of liquid)

R1

0.68 0.16 (0.68)

0.56 m

70.51kg.m2

Moment of inertia of basket

Ib = m2 R2

Where

m2

Mass of Basket

m2

D H S m

49 kg

Ib

22.93m2

IF + Ib

93.45Kg m2

RCF

Centrifugal Pressure
Pc

No. of Holes in Wall of Basket

= 9094

Power Calculations

So

If

m1
(R 2 R 12 )
2

56

d
dt

93.45

161 104.67

16846 Watts

16.846 KW

23H.P

104 .67
= 161 N-m
60

SPECIFICATION SHEET
1.

Equipment

Centrifuge

2.

Type

Top suspended basket

3.

Method of operation

Batch wise

4.

No. Required

5.

Function

To Separate water from


zinc stearate

6.

Basket Diameter

1.36m

7.

Speed

1000 rpm

8.

Maximum centrifugal force

190.66 g.

9.

Typical motor size

23H.P.

10.

Material of construction of basket

Stainless steel 316

11.

No. of holes per sq. meter

2500

57

DRYER
Drying Operation:
Drying of solids means the removal of relatively small amounts of water or other
liquid from the solid material to reduce the content of residual liquid to an acceptably
low value. Drying is usually the final step in a series of operation and the product
from a dryer is often ready for final packaging.
Drying Selection [4]:
Our feed is slurry of zinc stearate containing 60% moisture, and we are producing this
in a batch process do we have the following options:

CLASSIFICATION OF DRYERS

We have selected atmospheric tray dryer because our required temperature is not very
high and also our feed is not heat sensitive, tray dryer works on the principle of
conduction, hot air heats the trays and when the slurry is spread on the trays heat
transfer operation takes place between slurry and trays. Feed takes sufficient time to
get dry so that maximum moisture is removed. Tray dryers have high labor costs but
they are good to handle small amount of feed. We can easily clean the trays by taking
them out of the shelves

58

DATA:
Amount of feed (ms)

13857kg/day

Temperature of Feed (Tf)

30oC
30% of ms 4157.143kg/day

Moisture in Feed (X1)

10000kg/day

Amount of Product (mp)


Solids in Product

97% of mp 9700kg/day

Moisture in Product(X2)

3% of mp

300kg/day

Temperature of Product(Tp)

110oC

Cp of solids

2.79kJ/kgoC

Cp of water

4.18kJ/kgoC

Heating Medium

Air

Inlet Temperature of Air (TA)

130oC

Enthalpy of Air at 130oC

404KJ/kg

Enthalpy of Water at 60oC

251.5KJ/kg

Latent Heat of Vaporization

2270KJ/kg
ms - mp

Total Evaporation

3857.14kg/day

Heating Zone Constant Zone Falling Zone


20

Heat Transfer (KJ/hr m C)

100

700

200

load

100%

80%

60%

59

Zone
1
Operation

Solids temp.
o

Constant-rate

Heating

Steam temp.
o

Falling-rate drying

drying

130

130

130

130

130

30

70

70

70

100

100

60

60

60

30

Tm

LMTD. oC

(T t o ) (T t i ) [18]
ln[(T t o ) / (T t i )]

78

60

43

Heat Loads,
KJ/hr

Solid heat load

(KJ/hr)

Day

kg-mol

24 hr

Day

9700 x(70 30) x 2.79


24

9700 x(100 70 ) x 2.79


24

= 45105 KJ/hr
Liquid heat
load

= 33828 KJ/hr

4157 x(70 30) x 4.18


24

= 23695 KJ/hr

300 (100 70) x 4.18


24

=1282.5 KJ/hr

Evaporation

heat load

251 .5 x3857
24

(KJ/hr)
=40419 KJ/hr
Totals of heat

=68800

load (KJ/hr),
Surface area,
m2

= 40419

Qh
Tmh . h h . L n

= 8.78m2

= 1.20 m2

Qc
Tmc . h c . Lc

=35111
=

Qf
Tm f . h f . Lf

= 6.76 m2

60

Total Drying Area

At

= 8.78+1.20+6.76

=16.74m2

Excess Area

20%

=1.2*16.74

=20.08m2

Total Heat Required =

Qt

=68800+40419+35111

=144331 KJ/hr

Air Flow rate

Qt/HAir =144331/404

Drying Rate

mv

Time for Drying [19]

Total Drying Area

=2586.588kg/hr

h y (T Ti ) * A

=516.50kg/hr

ms
X c
=
X1 X c X c ln
v
m
X 2
At

=12.86hrs
=16.74m2

= .78+1.20+6.76

Assuming that our drying area is square shaped chamber


We can get Length & Width of Drying Area
Length

Width

Assuming Area of Tray

[20]

= (A)^0.5

=4.09m

= (A)^0.5

=4.09m

=Atray

=0.7m2

Assuming Spacing [20]

=0.05m

Spacing Area between Trays

= Aspace

=0.0025m2

Number of Trays along with space

=At/ Atray+ Aspace

=24

Number of Trays

=24/2

=12 Trays of Area

Assuming Height of Tray [20]

=Ht

=0.04m

Height of Drying Chamber= HD

=12(0.04+0.05)

=1.08m

Excess Height of dryer

=15% =1.15*1.08

=1.24.m

0.7m2 each

Length (m) Width (m) Height (m)


Tray

0.83

0.83

0.04

Drying Chamber

4.09

4.09

1.08

Dryer

4.48

4.48

1.24

61

DESIGNING SPECIFICATIONS

Equipment

No. Required

Batch Agitated Reactor 1

With cooling jacket

Batch Agitated Reactor 2

Centrifuge Separator

Tray Dryer

Specifications
Volume

1.46m3

Height

2.09m

Pressure

487KPa

Volume

19.88m3

Height

4.23m

Pressure

429kPa

Basket Diameter

1.36m

Rotations

1000rpm

Centrifugal Force

190.66g

No. of holes/m2

2500

Air Flow Rate

357.25kg/hr

Throughput

516.50kg/hr

Area of Dryer

20.08m2

Height of Dryer

1.24m

Heat Required

144331kJ/hr

62

CHAPTER # 7

MATERIAL
SELECTION

63

Equipment

Material

Options
316 Stainless Steel

Storage Tank

H2SO4

304 Stainless Steel


Carbon Steel

Selection[21]:
316 SS is best material
to store sulfuric acid in
corrosion free
environment
316 SS is the selected
material because as
compared to Glass

Reactor 1

ZnO,

Glass Lined Steel

Lined Steel it is

H2SO4,

316 Stainless Steel

economical & gives

ZnSO4

Carbon Steel

almost same corrosion


resistance in presence
of acidic nature
materials
ZnSO4 is of acidic

Settling Tank

ZnSO4, H2O

316 Stainless Steel

& unreacted

304 Stainless Steel

ZnO, H2SO4

Carbon Steel

nature and 316


Stainless Steel
provides good
atmosphere against
corrosion

CF-8M stainless steel


rubber-covered iron
Filter Press

ZnSO4, H2O

PVC-coated iron

& Mud

Aluminum
Cast iron
Wood

Rubber Covered iron


is good option because
we are dealing with
acidic nature material,
inside the filter press
there will be filter
medium

64

316 Stainless Steel

Storage
Tank

ZnSO4, H2O

C17H35COOH,
Reactor 2

NaOH, ZnSO4

304 Stainless Steel


Carbon Steel

316 SS is best
material to store ZnSO4 in
corrosion free environment

Glass Lined Steel

Atmosphere of reactor will

316 Stainless Steel

be slightly acidic so we are

Carbon Steel

using SS here
We can use 304 SS

Washing
Unit

(C17H35COO)2Zn

316 Stainless Steel

material for construction

Na2SO4

304 Stainless Steel

of this equipment because

H2 0

Carbon Steel

it is cheaper and can resist


corrosion if takes place

Centrifugal

(C17H35COO)2Zn

316 stainless steel


Carbon steel

Filter

We are using SS here


because it is long lasting
and will avoid corrosion
SS can be used here
because it can bear the
temperature up to 15000C

Tray Dryer

(C17H35COO)2Zn

Stainless steel

which is a way higher than

Carbon steel

our required temperature


so we choose cheaper
material as compared to
stainless steel for dryer

65

CHAPTER # 8

INSTRUMENTATION
&
PROCESS CONTROL

66

Measurement is a fundamental requisite to process control. Either the control can be


affected automatically, semi-automatically or manually. The quality of control
obtainable also bears a relationship to accuracy, re product ability and reliability of
measurement methods, which are employed. Therefore, selection of the most affect
means of measurements is an important first step in design and formulation of any
process control system.
Temperature measurement and control [5]:
Temperature measurement is used to control the temperature of outlet and inlet
streams in heat exchangers, reactors, etc.
Most temperature measurements in the industry are made by means of thermocouple
to facilitate bringing the measurements to centralized location. For local
measurements at the equipment bimetallic or filled system thermometers are used to a
lesser extent. Usually, for high measurement accuracy, resistance thermometers are
used. All these measurements are installed with thermo wells when used locally. This
provides protection against atmosphere and other physical elements.
Thermocouple is an electrical device that responds to a difference in temperature by
producing an electric current. Thermocouples are used as measuring instruments and
as control devices. Thermocouples are simple and rugged, can be used over a wide
range of temperatures (from -200 C. to 1,600 C.), and permit great precision.
Pressure measurement and control [6]:
Like temperature pressure is a value able indication of material state and
composition. In fact, these two measurements considered together are the primary
evaluating devices of industrial materials.
Pumps, compressors and other process equipment associated with pressure changes in
the process material are furnished with pressure measuring devices. Thus pressure
measurement becomes an indication of an energy decrease or increase.
A DP Cell is a type of differential pressure sensor which consists of two oil filled
chambers separated by a single sensing element.
Each oil-filled chamber includes a membrane which allows the oil to be pressurized
externally. If the oil pressure is greater on one side than the other it will cause the
sensing element to flex slightly, which will generate a change in signal output
proportional to the pressure difference.

67

A DP Cell will often include an internal mechanical feature which protects the central
sensing element from damage caused by high overpressure on one side of the DP
Cell. This high overpressure feature is often called a Mechanical Stop because it
limits the travel of the isolation diaphragm on either side of the DP Cell.
Flow measurement and control [7]:
Flow indicators are used to control the amount of liquid. Also all manually set streams
require some flow indication or some easy means for occasional sample measurement.
For accounting purposes, feed and product streams or metered. In addition utilities to
individual and grouped equipment are also metered. Most flow measures in the
industry are/ by Variable Head devices. To a lesser extent variable area is used as are
many types available as special metering situation arise.
Due to simplicity and dependability, the Venturi tube flowmeter is often used in
applications where it's necessary with higher Turn down Rates, or lower pressure
drops, than the orifice plate can provide. In the venturi meter the fluid is accelerated
through a converging cone of angle 15-20o and the pressure difference between the
upstream side of the cone and the throat is measured and provides a signal for the rate
of flow.
The pressure recovery is much better for the venturi meter than for the orifice plate.

The venturi tube is suitable for clean, dirty and viscous liquid and some slurry
services.

The range ability is 4 to 1

Pressure loss is low

Viscosity effect is high

Relative cost is medium

Globe Valve [22]:


The globe valve is used for throttling flow control. Shut off is accomplished by
moving the disc against the flow stream rather than across it as in the case with a gate
valve. The flow pattern through a globe valve involves changes in direction, resulting
in greater resistance to flow, causing high pressure drop. The globe valve is an
excellent valve to use for on-off service, but is highly suited for frequent cycling and
control of fluids anywhere in amount or volume between the open and closed
positions.

68

The globe valve must be installed in the proper relation to the media flow as indicated
by the flow direction arrow marked on the valve body. This valve is considered unidirectional and must be installed with the pressure side or inlet under the seat.

Butterfly valve:
Butterfly valve is used to control flow of material through a circular pipe or tube.
Certain dry materials may also be handled through butterfly valve. Valve body can be
made up of cast iron, ductile iron, aluminum, carbon steel, stainless steel and exotic
metals. They offer an excellent, economically priced, positive shut-off valve for
handling materials; they are easily displaced by valve disc as it closes. When handling
this type of material, butterfly valve provide a reliable, bubble-tight, bi-directional
shut off
Ball Valve [23]:
Ball valves are flow valves that are quarter-turn and straight through apparatuses.
These valves allow for shut-off or purposes of control. They have a round closure
element that contains a matching pair of rounded seats. These seats allow necessary
sealing to take place. The ball valve pressure rating and materials used determines
what kind of seat is required. Not all valve seats are the same. Some are of the single
molded variety while others have higher- pressure ratings, which often include a
design known as a "trunnion." This design means that each ball valve face is sealed
separately, not together.
Ball valves have many good points and are often considered superior to many other
kinds of valves. Ball valves are very easy to use and can both maintain and regulate
three things-high pressure, high volume and high flow of temperature. Other
advantages of ball valves are that they are sturdy devices that can be purchased for a
low price and they have a long service life. An added plus is that the regulating
element's design makes it easy for the ball valve to work without concern about side
loads, which often plague globe or butterfly valves. The ball valve design allows for
the easy ability to fix the seats if a problem arises and also seals without having to
take away the body of the valves from the line.
Ball valves can be found in a number of different styles. Some of these include onepiece, two-piece, three-piece and lastly, what is referred to as flanged body

69

construction. Each form of ball valve has its own good and bad points, all dependent
on what each application calls for. Ball valves are made using an assortment of
materials, some of which include brass, bronze, cast iron, copper ductile iron, metal
alloys, stainless and other steel types, and plastics (including CPVC and PVC). Ball
valves are to be found being used in a number of different industries.
Pressure Relief Valve [24]:
A pressure Relief Valve is a safety device designed to protect a pressurized vessel or
system during an overpressure event.
An overpressure event refers to any condition which would cause pressure in a vessel
or system to increase beyond the specified design pressure or maximum allowable
working pressure (MAWP).
The primary purpose of a pressure Relief Valve is protection of life and property by
venting fluid from an over pressurized vessel.
Many electronic, pneumatic and hydraulic systems exist today to control fluid system
variables, such as pressure, temperature and flow. Each of these systems requires a
power source of some type, such as electricity or compressed air in order to operate.
A pressure Relief Valve must be capable of operating at all times, especially during a
period of power failure when system controls are nonfunctional.
The sole source of power for the pressure Relief Valve, therefore, is the process fluid.
Once a condition occurs that causes the pressure in a system or vessel to increase to a
dangerous level, the pressure Relief Valve may be the only device remaining to
prevent a catastrophic failure. Since reliability is directly related to the complexity of
the device, it is important that the design of the pressure Relief Valve be as simple as
possible.
The pressure Relief Valve must open at a predetermined set pressure, flow a rated
capacity at a specified overpressure, and close when the system pressure has returned
to a safe level. Pressure Relief Valves must be designed with materials compatible
with many process fluids from simple air and water to the most corrosive media. They
must also be designed to operate in a consistently smooth and stable manner on a
variety of fluids and fluid phases.

70

Diaphragm Pump [25]:


A diaphragm pump is a positive displacement pump that uses a combination of
reciprocating action and either a flapper valve or a ball valve to transfer liquids. This
pump is sometimes referred to as a membrane pump. Diaphragm pumps are self
priming and are ideal for viscous liquids.
Diaphragm pumps transfer almost any kind of slurry, debris laden waste, food
processing residual, liquid, stones, sticks, sugar, oil sludge, refinery waste, mud, clay
pharmaceutical, industrial fluids and much more.

Diaphragm pumps have good suction lift characteristics, some are low pressure
pumps with low flow rates; others are capable of higher flow rates, dependent on
the effective working diameter of the diaphragm and its stroke length. They can
handle sludges and slurries with a relatively high amount of grit and solid content.

Diaphragm pumps are suitable for discharge pressure up to 1,200 bar

Diaphragm pumps have good dry running characteristics.

Slurry Pump:
A slurry pump is a type of centrifugal pump, lobe pump or peristaltic hose pump
in physics principle that increases the pressure of liquid and solid particle mixture
(aka slurry), through centrifugal force (a rotating impeller) and converts electrical
energy into slurry potential and kinetic energy.
Slurry pumps are widely used to transport corrosive/abrasive and high concentration
slurry in many industries such as Gold, Silver, Iron ore, Tin, Steel, Coal, Titanium,
Copper, Mineral sands, Lead and Zinc. Various other industries include Molybdenum,
Electric Utilities, Oil Shale, Water & Sewage Utilities, Building areas, Sand &
Gravel, Tobacco and Agriculture (hog, poultry, dairy manure) and are grouped by:

impeller quantity: single stage and multistage slurry pump

shaft position from the horizontal: horizontal and vertical slurry pump

impeller suction way: single suction and double suction slurry pump

pump casing structure: solid casing, horizontal split-case, and vertical split-case
slurry pump

71

REACTOR 1
VOLUME & LEVEL CONTROL

In volume control, level measuring device measures the level in the reactor and then
compares it with the set value and then signal is transferred to the controller which
changes the flow rate with the help of final control element (valve) and maintains the
volume in the reactor.
In temperature control, thermocouple measures the temperature inside the reactor and
then it compares it with the set value and then signal is transferred to the controller,
which changes the flow rate of water to control the temperature inside the reactor.

72

COMPOSITION CONTROL

During filling time of reactor to control the composition in the reactor, composition
analyzer measures the composition of material inside the reactor and changes the flow
rate inside the reactor.

73

STORAGE OF ZINC SULFATE

Level measuring device measures the level inside the storage tank and if the level is
about to exceed the volume of the storage tank, emergency drain will open and
material will go in another small tank to avoid wastage of material.

74

REACTOR 2
COMPOSITION

To control the composition in the reactor, composition analyzer measures the


composition of material inside the reactor and changes the flow rate of feed inside the
reactor; this is during the filling time of reactor.

75

LEVEL & TEMPERATURE

In case of volume control, level measuring device measures the level of material
inside the reactor and then signal is transferred to compare it with the set value and
then controller changes the flow rate with the help of the final control element (valve)
inside the reactor.
In temperature control, thermocouple measures the temperature inside the reactor and
the signal is then transferred to compare it with the set value, in case of any deviation
the controller changes the flow rate of steam with the help of final control element
(valve) to maintain the temperature inside the reactor at the desired value.

76

TRAY DRYER

In dryer, thermocouple measures the temperature inside the dryer and then signal is
transferred to compare it with the set value , in case of any deviation controller
changes the flow rate of air to maintain the temperature inside the dryer at the
required value.

77

CHAPTER # 9

COST
ESTIMATION

78

Equipment

Equipment
Specifications

[26]

Cost
2012

Materials of
Construction

Equipment
Cost in $, Jan
2013
CE index =
564.2
1*4000

Hopper for ZnO


Storage Tank for
H2SO4

4m3

32357

316 Stainless
Steel

1*46761

Reactor
Turbine single
impeller Agitator

2 m3
8 kW

30615
28862

Stainless steel
316 Stainless
Steel

1*44244
1*41710

Storage Tank for


ZnSO4

4m3

32357

316 Stainless
Steel

1*32357

Horizontal
Centrifugal pump

6m3/s

8716

Cast Steel
Casing

1*12598

Plate-and-frame
filter

2.5 m2

7361

Rubber Covered
Iron

1*10638

Horizontal
Centrifugal pump

6m3/s

8716

Cast Steel
Casing

1*12598

Storage Tank for


ZnSO4

4m3

32357

316 Stainless
Steel

1*46761

Hopper for
C17H35COOH

1*4000

Hopper for NaOH

1*4000

Reactor
Single Impeller
Agitator

20 m3
8 kW

118541
28862

Stainless Steel
Stainless Steel

1*1717313
1*41710

Washing Unit

30m2

321373

1*464443

Centrifuge

Bowl dia =
1.36m
20m2

266831
36312

304 Stainless
Steel
316 Stainless
Steel
Stainless Steel

200 kW

10019

Carbon steel

1kg/s

157843

1*14479
1*4000
1*228112
3140820

Atmospheric
Tray dryer
Heater
Storage
Shear Mill
Total

1*358619
1*52477

79

Purchased equipment cost

=E

= $3140820

Installation cost

= 40%E

=$1256328

Instrumentation and control cost

=13%E

=$408306

Piping cost

=10% E

=$314082

Electric cost

=10%E

=$314082

Building (including services)

=29%E

=$910837.8

Yard improvement

=10%E

=$314082

Land cost

=6%E

=$188449

Total Direct Cost [21]

= $6846988

Indirect cost:
Engineering and Supervision Cost

=32%E

=$1005062

Construction Expenses

=30%E

=$942246

Contractor fee

=18%E

=$565347

Contingency Cost

=30%E

=$942246

Total Indirect Cost [21]


Fixed Capital Investment [21]
F.C.I

= $3454902

= Direct cost + Indirect cost


= D.C

I.C

= $10301890
Working Capital

=18%F.C.I

= $1854340

Total Capital Investment [21]


T.C.I

W.C

F.C.I

=$12156230

80

CHAPTER # 10

SAFETY ANALAYIS

81

PROCESS FLOW DIAGRAM

82

REACTOR 1 [21]
Study Node:

Reactor-1

Material:

H2SO4

Study Parameter:

Volume of H2SO4

Source:

H2SO4 Tank

No

Guide
Word

Deviation

Possible
Causes

Consequences

-No Level
sensor.

-Tank overflow.
-Greater Conc. of

More

More

-Operators

H2SO4 can lead to

mistake.

runaway reaction as it

volume

is an exothermic
-Malfunction

reaction.

of pump.

-Overflow valve
provided on tanks
jacket.
-Pump shutdown.

provided on the

Less

-Malfunction

volume

of pump.

-Less H2SO4 in tank.


-Increased conc. Of
ZnO.
-Improper Reaction.

pipe.

remove choking.
-Operator
Re-establish H2SO4

provided on the

-Operator
mistake.

-No H2SO4 in tank.

-Malfunction

-ZnO being the only

No

of pump.

reactant leads to no

Volume

-Power failure.

reaction.

jammed.

-Blow pipe to

-Level sensor

sensor.

-Inlet vale

tanks jacket.

supply in tank.

-No level

No

tanks jacket.

sensor.

-Choking of

provided on the

-Level sensor

mistake.
Less

-Level sensor

-No Level

-Operator

Action Required

tanks jacket.
-Operator reestablishes H2SO4
supply in tank.
-Backup-generator.
Alternate inlet.

83

FILTER PRESS

Study Node:

Filter Press

Study Parameter:

No

Pressure

Guide

Possible

Word

Causes

1
More

[21]

Material:

ZnSO4

Source:

Settling Tank

Consequences

Actions Required

-Pump capacity

-Increased pressure of

-Control valve provided

is greater than

ZnSO4 leads to cloth

on ZnSO4 inlet.

required

rupture or damage.

-Impurities tend to pass

-Automatic ZnSO4

-Operator

through the cloth.

injection system.

mistake
-Pump to be of exact
-No automatic

specification to provide

system.

optimum pressure.

-Pipe leakage.
2

-Slow rate of filtration.

-Remove blockage of
pipe.

Less
-Partial
blockage in

-Alternate ZnSO4

pipe.

injection.

-Pump capacity
less than
required.

84

-Pipe block.

-No filtration

-Remove blockage.

-Pump

-ZnSO4 not suitable for

-Re-establish supply of

malfunction

further use.

ZnSO4.

-Impurities in

-Filter cloth blockage.

-Replace the raw

No

Other

pump casing.

material source
-Filter cloth damage due

-Impurities in

to reaction with

-Clean pump for

raw material

impurities.

removal of impurities.

85

REACTOR 2 [21]
Study Node:

Reactor-2

Material:

ZnSO4

Study Parameter:

Volume of ZnSO4

Source:

H2SO4 Tank

Guide
No.

Word

Less

No

Possible Causes

Consequences

Actions Required

-Malfunction of high

-Increased

-Re-establish

service pump.

concentration of

required zinc sulfate

-Leakage of pipe.

sodium stearate in

supply.

-Partial Pipe

product rather

-Remove blockage.

Blockage

than that of zinc

-Pipe repair.

stearate.

-Alternate pipe.

-Pipe blocked.

-Product only

-Remove blockage.

-Power failure.

containing sodium -Re-establish power

-No ZnSO4 in-take

stearate.

by pump from tank.

supply.
-Backup pump

86

Other

-Impurities from

-ZnSO4 not

-Re-filter if required

storage vessel

suitable for

-Clean storage tank

-Impurities from

reaction.

to remove

filter press.

-Low Product

impurities

-Impurities from

purity.

-Clean pump casing

pump casing.

to remove
impurities

More

-No Level sensor.

-Greater conc. Of

-Level sensor

-Malfunction of

zinc sulfate in the

provided on the

pump

reactor.

tanks jacket.

-Operator mistake

-Un-reacted zinc

-Overflow valve

sulfate in product

provided on tanks

line

jacket.

-Low product

-Pump shutdown

quality

87

TRAY DRYER

Study Node:

Tray & Shelf Dryer

Study Parameter:

No Guide

Flow Rate

Possible Causes

[21]

Material:

Air

Source:

Heat Exchanger

Consequences

Actions Required

Word

1
More

-Blower capacity

-Increased rate of

-Replace with blower

greater than required.

drying may cause

of required capacity.

-Operator mistakes no damage to the

-Install a flow meter

automatic system.

material.

on the pipe to control

-Material might be

the flow.

blown away from the -Automatic system


tray

Less

-Pipe leakage.

-Less rate of drying.

-Remove blockage of

-Partial blockage in

-Product containing

pipe.

pipe.

more than

-Alternate blower or

-Blower capacity less

appropriate quantity

air inlet.

than required.

of water.

-Install a blower of
the appropriate
capacity.

Other -Absence of air filter.


than

-Impurities in

-Blow pipe to

-Impurities in blower

product can disturb

remove impurities.

casing.

quality of product.

-Clean pipe and

-Impurities in pipe.

-It can decrease the

blower on regular

-Impurities due to

rate of drying in the

basis.

some leakage.

dryer.

-Install air filter.

88

CHAPTER # 11

ENVIRONMENTAL
ASPECTS

89

ROUTES OF EXPOSURE

[9]

Exposure to zinc stearate can occur through inhalation, ingestion, and eye or skin
contact.

EFFECTS ON HUMANS

[10]

Zinc stearate is a physical irritant in humans. A worker in a rubber factory in Italy


exposed to zinc stearate for 29 years, developed extensive fibrosis of the lungs
and died from that condition [Clayton and Clayton 1981]. Although no specific
information is available on the concentration of the exposure leading to the
condition, it is believed that it was very high because no adverse effects have
been noted in workers at a large U.S. rubber factory following many years of
exposure to zinc stearate. Aspiration of zinc stearate by infants is associated with
respiratory distress and acute pneumonitis [ACGIH 1991].

METHODS TO CONTROL EXPOSURE

[10]

Methods that are effective in controlling worker exposures to zinc stearate,


depending on the feasibility of implementation, are as follows:
Process enclosure

Personal protective equipment

Local exhaust ventilation

General dilution ventilation

STORAGE:
Zinc stearate should be stored in a cool, dry, well-ventilated area in tightly sealed
containers that are labeled in accordance with OSHA's Hazard Communication
Standard [29 CFR 1910.1200]. Containers of zinc stearate should be protected from
physical damage and should be stored separately from strong oxidizers or dilute acids
may cause reactions to occur.

90

REFERENCES
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http://www.baerlocher.com/fileadmin/media/0.5_Service/0.5.1_brochures/0.5.1.3_pro
duct_brochures/metallic_stearates.pdf
[2]-Zinc Stearate, Properties of Zinc Stearate [Online]. Available:
http://en.wikipedia.org/wiki/Zinc_stearate
[3]- Richard H. Morris and Stephen E. ORourke, Metallic Stearates [Online]:
http://www.hallstar.com/techdocs/metallic.pdf
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Calculations in Chemical Engineering (pp 104-148)

91

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Calculations in Chemical Engineering (pp 362-480)
[13]- Sinnott R. K., Volume 6, (Fourth edition), Coulsons and Richardsons
Chemical Engineering Design (pp 322)
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http://chemwiki.ucdavis.edu/Physical_Chemistry/Thermodynamics/State_Functions/E
nthalpy/Heat_of_Reaction
[15]- Fogler H.S (Fourth Edition), Elements of Chemical Reaction Engineering
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Chemical Engineering Design (pp 814)
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[22]-Globe Valves [Online] Available at:
http://www.ladishvalves.com/globe-valves-corrosion-resistant/
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http://www.thomasnet.com/about/ball-valves-90370206.html
[24]-Relief Valve [Online] Available at:
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92

[25]-Diaphragm Pump [Online] Available at:


http://www.wastecorp.com/mudsucker/ms-faqs.html
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93

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