INTRODUCTION

1.1 ETHYL CELLULOSE:

Ethyl cellulose is a derivative of cellulose in which some of the hydroxyl

groups on the repeating glucose units are converted into ethyl ether groups. The number
of ethyl groups can vary depending on the manufacture. Ethyl cellulose is a derivative of
alpha cellulose group.

Ethyl cellulose (EC) is a hydrophobic ethyl ether of cellulose. Ethyl

cellulose is directly extracted from plant fibre (cellulose, cotton) and is then chemically
modified. Ethyl cellulose is a kind of cellulose ether, and it shows good thermo stability
and electric properties. The film made from EC has quite good permeability, it has been
widely used industrial air filter. Ethyl cellulose is prepared from wood pulp or cotton by
treatment with alkali and ethylation of the alkali treated cellulose with ethyl chloride. The
resulting product is then further steamed and dried. Ethyl cellulose is non-bio degradable,
bio-compatible, non-toxic natural polymer and widely used in oral and topical
formulation.

Figure 1.1 Structure of Ethyl cellulose

1.2 BACKGROUND:
In recent years, there has been an increase in the level of research on the
development of new biodegradable materials for use in packaging, agriculture, medicine
and other areas. Generally, biodegradable polymer materials are increasingly important as
environmental contamination and waste disposal problems associated with plastics and

1
related products from synthetic polymers become more severe. Natural polymers have
various advantages over synthetic polymers due to their low-cost, great availability and
biodegradability. Furthermore, oil prices have increased significantly due to the limited
nature of fossil fuels, especially petroleum resources. In response to this situation,
lignocelluloses biomass from plants has become the main focus of the developing bio-
refining industry.
Sugarcane bagasses (SCB) are an abundant agricultural lignocelluloses by-
product on the earth. It is a main product to the sugarcane industry which is generated in
large quantities during the processing of sugarcane in sugar mills. Bagasses offer the
advantages of being a cheap, plentiful and low polluting fuel. Commonly, all plant
biomass consists of cellulose, Hemicellulose, lignin, pectin and protein. Most of the plant
biomass consists of about 33 % of cellulose as the major component of the rigid cell
walls.

Cellulose is a linear and high molecular weight polymer as well as natural,

renewable and biodegradable material. However, due to its high crystallinity and strong
inter- and intra-molecular hydrogen bond, cellulose neither melts nor dissolves in the
most common organic solvents, therefore, reduces its applicability. In order to increase
the cellulose applicability, an alternative pathway is to convert the cellulose to its
derivatives such as Ethyl cellulose (EC) through chemical derivatization reaction. EC is
important for its water-soluble properties where great applications are applied throughout
the food industry, detergents, cosmetics, pharmaceuticals, textiles, paper, adhesives as
well as ceramics.

EC was reported to be synthesized from diverse plant biomasses, which contain

40 50 % cellulose, 25 40 % hemicellulose and 15 35 % lignin on a dry basis. The
synthesis of EC from various agricultural waste cellulose sources such as sugar beet pulp,
cavendish banana pseudo stem, cashew tree gum, sago waste, orange peel, papaya peel
and Mimosa pigra peel have been reported by many researchers.

2
1.3 WHAT IS CELLULOSE?

Cellulose is a long chain of linked sugar molecules that gives wood its remarkable
strength. It is the basic building block for many textiles and for paper. Cellulose is the
back bone structure of plants, and it is the chief constituent of plant cell wall. Cellulose is
the most abundant and widely used organic material in the world, with a worldwide
consumption that is higher than steel, coal, or sugar. Three basic types of cellulose are
available i.e alpha, beta and Gama celluloses. They differ in their solubility behavior in
17.5% w/v of sodium hydroxide .While alpha cellulose is insoluble in 17.5% w/v NaOH
solution, beta cellulose is soluble and can be precipitated out of solution by addition of a
mineral acid; gamma cellulose is soluble in 17.5% w/v of NaOH solution but cannot be
precipitated out of solution. From alpha-cellulose, numerous derivatives of cellulose can
be obtained. Ethyl cellulose is a derivative of alpha cellulose in which some of the
hydroxyl groups on the repeating glucose units are converted into ethyl ether groups.

Figure 1.2 Structure of cellulose

1.4 DERIVATIVES OF CELLULOSE:

Cellulose derivatives which are synthesized from natural waste have diverse
physiochemical properties due to the wide range of substitutions, molecular weight, and
degree of polymerization are valued for their vast application as additives in textile, food,
cosmetic and packaging industries. Through Williamson etherification reaction, several
cellulose derivatives which are soluble in common solvents may be produced, such as

3
carboxy methyl cellulose (CMC), methylcellulose, hydroxy propyl cellulose and
hydroxypropyl methyl cellulose.

Table 1.1 Commercially marketed cellulose Ethers

Cellulose ethers Functional group DS Solubility

Carboxymethyl cellulose -CH2COONa 0.5-2.9 Water

Methyl cellulose -CH3 1.5-2.4 Hot water

Ethyl cellulose -CH2CH3 2.3-2.6 Organic solvent

Hydroxyethyl cellulose -CH2CH2OH 0.5-0.7 Water

Hydroxypropyl cellulose -CH2CH2CH2OH 1.5-1.7 Water

1.5 HISTORY:

Cellulosic plastics are based on cellulose, which is the principal structural

component of plants. The first Cellulosic plastic was invented in 1852 by Alexander
Parkes who developed cellulose nitrate into a mouldable dough he called Parkesine. By
1860 it was being pressed into moulds to make billiard balls, pens, and even artificial
teeth.
Ethyl cellulose is obtained as a white granular solid by treating wood pulp
soaked in sodium hydroxide, with ethyl chloride. During World War II it was a very
versatile material and used in water bottles for the military. It was claimed that even a
heavy person could jump on an ethyl cellulose bottle without breaking it. These particular
samples of ethyl cellulose were donated to the Museum by the Hercules Powder
Company in 1943. The company was established in 1912 and produced nitrocellulose for
photographic films, until cellulose acetate became the preferred material. They recruited
scientists from top universities to research new cellulose acetate products that could allow

4
them to stay ahead in the market. The company's focus changed and its main areas of
business became commercial explosives, such as gun powder and dynamite.

1.6 RAW MATERIALS FOR ETHYL CELLULOSE PRODUCTION:

Chemical functionalization of cellulose is to alter the properties of the
macromolecule for different purposes such as the production of cellulose derivatives for a
variety of applications. The most common sources of cellulose for industrial uses are
from wood pulp (contain 40 50 % cellulose) and cotton linters (contain 90 % cellulose)
which nowadays are discouraged due to the cost of production and increasing
environmental concerns. Besides, renewable materials are gaining importance due to the
limited existing quantities of fossil resources. Thus, biomass rich in cellulose such as
bamboos, weeds, fibers and agriculture waste become an alternative chemical feedstock
as it consists of cellulose, hemicellulose and lignin, which contain various functional
groups suitable for chemical functionalization.

Table 1.2 Different compositions in agricultural waste:

Agricultural waste Cellulose (%) Hemi cellulose (%) Lignin (%)

Corn cobs 45 35 15

Wheat straw 30 50 15

Hardwood stems 45-50 24-40 18-25

Softwood stems 45-50 25-35 25-35

Sugarcane bagasse 40-50 23-35 18-24

1.7 World scenario

During 1920-1930s, the first cellulose ether which gains economic significant was
carboxy methyl cellulose (CMC) followed by methyl cellulose and hydroxyethyl
cellulose. These three types of cellulose ether and their mixed derivatives such as methyl
hydroxyethyl, methyl hydroxyl propyl and hydroxyl propyl methyl cellulose still

5
dominate the market due to their multifunctional properties. The worldwide production of
cellulose ethers to be over 300,000 metric tons annually. Besides, they are kinetically and
thermodynamically more stable and easier to be prepared and characterized
.
The following pie chart shows world consumption of cellulose ethers:

Figure 1.3 World consumption of Ethyl cellulose-2015

The annual production of ethyl cellulose is 4000 tons/annum. The
production of methylcellulose and hydroxyl ethyl cellulose is more concentrated. Three
producers account for 53% of the world market. HEC is the most concentrated market,
with two producersAshland and Dowaccounting for over 75% of the world market.
Ashland produces all three major cellulose ethers, as well as hydroxyl propyl cellulose
and ethyl cellulose.
Although the cellulose ethers market is global, most of the production
capacity is in Europe, as is most of the consumption. Most of the major producers have
facilities in more than one region. An overall average growth rate of 3.5% per year is
expected for all cellulose ether products in 20122018. In Asia, the lowest growth is
expected in Japan, while China and the rest of Asia will lead global growth. The regions
with the largest current consumptionEurope and Chinawill grow at 2.0% and 4.6%
on an average annual basis, respectively. North America will grow faster (4.2%) than
Europe and Japan.

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PROPERTIES AND USES OF ETHYLCELLULOSE

2.1 PHYSICAL PROPERTIES:

Ethyl cellulose polymers are inert, high purity powders with no caloric value and
are virtually colorless, odorless, and tasteless. They are derived from and have the
polymeric backbone of cellulose, a naturally occurring polymer

Table 2.1 Properties of Ethyl cellulose

Chemical formula -C6H9O5C2H5

Form Powder
Color White
Smell Odourless

Taste No taste

Melting Point 160O-210Oc

Auto ignition temp. 698F

Hardness 52-61 (Sward, 3-mil. film)
Extent of labelling 48% ethoxyl
2.25-2.58 mol ethyl per mol cellulose
(D.S.)
Water vapour transmission 890g/m2/24hrs, 3-mil. film (ASTM
E96-66,E)
Refractive index n20/D 1.47(lit.)
Viscosity 46 cP, 5 % in toluene/ethanol 80:20(lit.)
Transition temp , Tg 120-124 C
Solubility Esters, aromatics, hydrocarbons,
alcohols, and ketones soluble
Density 1.14 g/mL at 25 C (lit.)
Softening point 140O-170OC

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2.2 APPLICATIONS:

Ethyl cellulose polymers are produced in two ethoxyl types (standard and medium).
Medium polymers are only supplied on a restricted, made-to-order basis. Ethylcellulose
polymers are also produced and marketed in a number of different viscosities. Standard
and medium ethoxyl types are available in premium grades and industrial grades.
Premium grades are designed to meet the requirements of pharmaceutical applications
and are useful in regulated applications. Although designed for pharmaceutical
formulations, these products are useful in other applications, such as personal care or
applications that require high surface area polymers.

Ethyl cellulose polymers have provided excellent functionality in many pharmaceutical

and specialty polymer applications for more than 60 years. They offer an attractive range
of physical properties and can be blended with other materials to achieve intermediate
characteristics.

Pharmaceuticals: Ethyl cellulose polymers are among a very small number of water-
insoluble excipient polymers that are approved and accepted globally for pharmaceutical
applications. They are proven polymers for tablet coatings, controlled-release coatings,
micro encapsulation, granulation, and taste masking

Personal care: Ethyl cellulose polymers are approved for use in cosmetics. Ethyl
cellulose polymers are listed in the International Cosmetic Ingredient Dictionary and
Handbook. It is also listed in the Japanese Standards of Cosmetic Ingredients. These
polymers have been used in lipsticks and nail polishes, as fragrance stabilizers, and as
thickeners for perfumes and body creams (waterproof sunscreens).

Food: In the United States, Ethyl cellulose polymers are used as flavor fixatives in
encapsulation and as vitamin coatings. They are approved for and used in inks for
marking fruits and vegetables, as components of paper and paperboard in contact with
water-based and fatty foods, and for certain uses in animal feed. Ethyl cellulose polymers
have been approved by the EU in food applications since the end of 2006.4 They are also
approved for use in animal feed in Europe.

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Ceramics Ethyl cellulose polymers are used in ceramic applications as a binder and to
change the flow and slip characteristics of wet clay.

Conductive pastes Ethyl cellulose polymers are used in conductive pastes. They
function as binders and stabilizers for pigments and to change the flow characteristics of
the pastes.

Printing inks Ethyl cellulose polymers are used in gravure, flexographic, and screen
printing inks. They are soluble in common solvent systems and are compatible with
plasticizers, waxes, and other commonly used polymers. They contribute to the formation
of tough, abrasion-resistant films.

Specialty coatings Ethyl cellulose polymers bring an unusual combination of

properties to specialty-coating applications such as hot melts, adhesives, paper coatings,
fluorescent lighting, and other applications.

2.3 USES:

It is mainly used as a thin-film coating material.

Ethyl cellulose is used as a food additive as an emulsifier
Ethyl cellulose is used as a flavor fixative in encapsulation and as a vitamin
coating.
It is approved for and used in inks for and making fruits and vegetables ,as a
component of paper and paperboard
Ethyl cellulose is predominantly used in food supplements and flavorings in
capsules.
It functions as a binding and filling agent or serves as protective coating.
Apart from that, Ethyl cellulose can function as an emulsifier to stabilize water-
oil-mixtures.

9
DIFFERENT PROCESSES FOR ETHYL CELLULOSE
MANUFACTURE FROM BAGASSE
Various routes for manufacturing of Ethyl cellulose are:

Two stage digestion process

Steam Explosion process

3.1 Two stage digestion process:

The present invention relates to a process of making alpha-cellulose from fibrous

ligno-cellulose materials particularly from bagasse. Then this alpha cellulose is etherified
to form ethyl cellulose.
According to the process covered by this invention, the bagasse, after being screened to
remove bagasse powder and other impurities, and after being washed with water, is
placed in a digester to be digested in an aqueous solution containing from 3 to 4.5 percent
total sulfur-dioxide, as contained in calcium sulfite, magnesium sulfite and sulfurous acid,
in the following ratio. The ratio of free sulfur dioxide to combined sulfur dioxide should
be 0.95-l.l to 1 calculated by weight and the ratio of magnesium to calcium should be 3~5
to l, calculated as oxides by weight. The bagasse is immersed in the above mentioned
solution in the digester. The bagasse and the solution in that digester are then heated to
reach the maximum temperature of from 145 C. to 150 C. and such maximum
temperature is maintained for a period of from 3 to 4 hours. The solution, which becomes
a black liquor after such digestion, is now drained off.
The fibers produced from the foregoing digestion are then mixed with an aqueous
neutral sodium sulfite solution so as to make a solution of from 5 to 10 per cent
consistency containing from 0.3 to 0.8 per cent total sulfur dioxide. The fibers so mixed
are then placed in a second digester again to be digested, and heated during the second
digestion to reach a maximum temperature of from 145 C. to 150 C. such maximum
temperature to be maintained for a period of from 30 to 60 minutes. Black liquor is
drained off.
These fibers are then treated with a low concentration of a mineral acid
(hydrochloric acid) for hydrolyzing the hemi-cellulose constituents, and then chlorinating

10
the residual lignin in the cellulose and oxidizing the hydrolyzed hemi-cellulose by
chlorine water with very little degradation of the cellulose and dissolving the chlorinated
lignin and degraded hemi-cellulose by means of a diluted caustic soda solution, thereby
obtain alpha cellulose of high quality, whose purity is above 92% and whose degree of
polymerization is above 1000. The product is produced by treating cellulose with an
alkaline solution to produce alkali cellulose, which is then reacted with ethyl chloride,
yielding crude Ethyl cellulose polymers then it is filtered for the removal of salt and
caustic. The product from filtration is treated with steam to remove solvent and
byproducts for recovery. The product is washed and neutralized for the removal of salt
and water then it is dried, densified and sent to storage.

MERITS:

The hydrolyzing effect of the mineral acid employed is only related to the acidity of
the solution. For this reason, it is not necessary to use too much acid and it is
sufficient to use only a small quantity of such acid to maintain the acidity of the
solution.
In this way, any possible degradation of the alpha cellulose during this phase of the
process is kept to an absolute minimum.
A further purpose for applying the mineral acid solution is to have it react on the ash
content of the fibers and thereby render the most portion of such ash soluble in water,
so as to become easily removable.
DEMERITS:

A large fraction of lignin and hemicellulose constituents extracted out from ligno
cellulose plant material (black liquor) are a source of environmental pollution as the
waste liquids as in the form of black liquor are let out into waste streams after
expensive treatments.
The cost of pollution abatement is high.
The valuable industrially useful organic polymeric material such as lignin and
hemicellulose have been lost.

11
Figure 3.1 Flow sheet of Two stage digestion process

12
3.2 Steam explosion process:

The present invention relates to a process for fractionating sugarcane bagasse into
high - cellulose, xylan and lignin. The separated components, are useful in the
production of high value-added commercial products like cellulose ester, pentose sugars
and their derived materials, and lignosulfonates and other lignin derivatives.
The process of the present invention provides a process for an economical, simple
and efficient process for fractionating in high yield and high purity, a wide variety of
renewable lignocellulosic plant material to its major polymeric components cellulose,
lignin and hemicellulose, which can then be used as raw materials for production of
chemicals, plastics, polymers, etc.
Sugarcane bagasse is an agricultural by-product which has the general
composition of 40-45% cellulose, 28-30% hemi cellulose, and 19-21% lignin. Cellulose
from the bagasse fiber is known to have a higher degree of polymerization than the
cellulose obtained from bagasse pith.
Fractionation and isolation of high -cellulose pulp, hemicellulose and lignin
from fibrous organic biomass comprising (a) contacting the biomass with steam at
temperatures in the range 1400 C.-230 C., hydrolyzing and solubilizing the
hemicellulose component to an extent of 70-90% and evaporating the water to get
hemicellulose, (b) separating and washing the undissolved fibrous organic biomass and
treating with 10-24% alkali at temperatures in the range 80 C.-180 C. to solubilize the
lignin component to an extent of 90-95%, as well as solubilizing the residual hemi
cellulose, and precipitating the soluble fraction with mineral acid to get lignin,
(c) separating and washing the undissolved fibrous organic biomass and bleaching with
1-6% by weight of sodium chlorite or chlorine dioxide at a temperature of 30C.-90 C.
(d) separating and washing the fibrous organic residue to get a pulp containing 90-94% -
cellulose. The product is produced by treating cellulose with an alkaline solution to
produce alkali cellulose, which is then reacted with ethyl chloride, yielding crude ethyl
cellulose polymers then it is filtered for the removal of salt and caustic. The product from
filtration is treated with steam to remove solvent and byproducts for recovery. The
product is washed and neutralized for the removal of salt and water then it is dried,
densified and sent to storage.

13
Figure 3.2 Block diagram of Steam explosion process

14
4. SELECTION OF THE PROCESS

Among the various processes discussed in the previous chapter, steam

explosion process for extraction of cellulose from bagasse offers considerable advantages
over the other processes. This invention has several advantages over the other process.
We have not found any reference to obtaining all three fractionated products (cellulose,
hemicellulose and lignin) of bagasse and other grasses in such high yields and high
purities. No one has reported the characterization of their pure fractionated cellulose in
terms of residual lignin content and residual hemicellulose content, as this process have
done. Similarly, this process characterized the isolated lignin for residual xylan content.
The lower the xylan content of lignin, the superior its properties. This process also
characterized the hemicellulose to show the extent of hydrolyzed sugars and oligomers
obtained by this method. This is important to design enzymatic or acid hydrolysis of
hemicellulose to sugars for further value-addition. This is crucial information for
designing new products and derivative synthesis from the fractionated cellulose,
hemicellulose and lignin. This process thus gives to us very specific polymers (cellulose,
hemicellulose and lignin) With specific characteristics, not reported elsewhere.
For other process a large fraction of lignin and hemicellulose constituents
extracted out from ligno cellulose plant material (black liquor) are a source of
environmental pollution as the waste liquids as in the form of black liquor are let out into
waste streams after expensive treatments. The valuable industrially useful organic
polymeric material like lignin and hemicellulose being lost. These materials can be used
industrially. Also the cost of pollution abatement is low.
The primary focus of this process appears to be an energy recuperation for
economic viability, and uses only steam, water and oxygen in the process. The main
objective of the present invention is to provide an economical, simple and efficient
process for fractionating a wide variety of renewable lignocellulosic plant material to its
major polymeric components hemicellulose, lignin and cellulose, all in high yields and
high purity, which can then be used as raw materials for production of chemicals, plastics,
polymers, etc. Finally, based on the above considerations steam explosion process for
extraction of cellulose is selected for the manufacture of ethyl cellulose.

15
5. PROCESS DETAILS
This process includes two steps in which first step includes the extraction of
cellulose from bagasse, and the second step includes the etherification of this extracted
cellulose to form Ethyl cellulose. This process is being widely used.
These are the reactions that are taking place in the process:

Cellulose + NAOH Cellulose-Na + H2O

Cellulose-Na + C2H5Cl Ethyl cellulose + NACl

5.1 OPERATING CONDITIONS:

The process variables for the process are:

Process temperature
In solubilizer 1 1400 - 2300 C
In solubilizer 2 -- 800 - 1800 C
In bleaching -- 300 - 900 C
Alkali used in this process is sodium hydroxide.
Mineral acid used in this process is hydrochloric acid.
Bleaching material used in this process is sodium chlorite.
The ratio of the biomass to the Water used is 1:6 to 1:20 by Weight of the
biomass, but preferably in the ratio 1:12.
The ratio of the biomass to the sodium chlorite used is 0.01-0.3 times the
Weight of the biomass material to be bleached.

In this process following steps takes place:

Solubilizing and hydrolysing of Hemi cellulose.
Treating of fibrous organic material with alkali.
Treating undissolved fibrous organic material with sodium chlorite.
Separating and washing to obtain cellulose containing 90-94% alpha cellulose.
Etherifying the cellulose by treating it with sodium hydroxide and ethyl chloride.

16
5.2. PROCESS DESCRIPTION:
Accordingly the present invention provides a process for the fractionation and
isolation of high alpha-cellulose pulp, Hemi cellulose (xylan) and lignin from depithed
fibrous organic biomass and the said process comprising the steps of:
Contacting the biomass with steam at temperatures in the range 1400 C.-230 C.,
hydrolyzing and solubilizing the Hemi cellulose component to an extent of 70-90% and
evaporating the water to get Hemi cellulose.
Xylan + H2O Xylose

Separating and Washing the undissolved fibrous organic bio mass and treating
With 10-24% alkali at temperatures in the range 80 C.-180 C. to solubilize the lignin
component to an
extent of 90-95%, as well as solubilizing the residual Hemi cellulose, and precipitating
the soluble fraction with mineral acid to get lignin as lignose.
Lignin + H2O lignose

Separating and washing the undissolved fibrous organic biomass and bleaching
With 1-6% by weight of sodium chlorite or chlorine dioxide at a temperature of 30C.-
90 C. separating and Washing the fibrous organic residue to get a pulp containing 90-
94% alpha-cellulose.
Then the cellulose content which is free of biomass material is treated with
sodium hydroxide in a mixer and then to reactor where the reaction takes place for four
hours. The mixture is treated with ethyl chloride solution to form ethyl cellulose and un
reacted material.
(C6H10O5)n + n NaOH n(C6H9O5Na) + n(H2O)
n(C6H9O5Na) + n(C2H5Cl) n(C6H9O5C2H5) + n(NaCl)
This is then sent to washing and neautalizing section where it is treated with HCL
and water. The waste is removed and the product is dried and taken out as pure ethyl
cellulose powder.

17
Figure 5.1 Flow sheet of steam explosion process

18
6.1 MATERIAL BALANCE

This chapter includes the detailed study of Material Balance & Energy Balance of
all the streams present in the selected process and details of all the streams are tabulated
accordingly.
Basis: Amount of Ethyl cellulose produced = 2000 tons/year
= 6.4 tons/batch (320 working days per
annum)
Assumptions:
1. It is assumed that the material balance is done for single monomeric compound in
cellulose structure.
2. Let us assume that feed bagasse contains 43% Cellulose, 27% Hemi cellulose,
22% Lignin, 8% Ash & extractives by weight.
3. It is assumed that the conversion of cellulose to ethyl cellulose is 96%.
4. It is assumed that recovery of Hemi cellulose is 92%, lignin is 95% from bagasse.
Reactions taking place:
C6H10O5 + NaOH C6H9O5Na + H2O
C6H9O5Na + C2H5Cl C6H9O5C2H5 + NaCl

Table 6.1: Molecular weights of different components

COMPONENT MOLECULAR WEIGHT

Cellulose 162
C6H9O5Na 184
NaOH 40
H2O 18
C2H5Cl 18
C6H9O5C2H5 190
NaCl 48.5

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 The required amount of raw materials needed to produce the required amount of
ethyl cellulose has been calculated by using the stoichiometry equation of the process.
From the mass balance done by taking into account of conversions and side reactions, the
mass flow rate to produce the required production of ethyl cellulose is 16 tons/batch of
bagasse.

6.1.1 MATERIAL BALANCE AROUND SOLUBILIZER 1:

Amount of water used is in the ratio of 1:12

Water used is 192 tons/ 16 tons of bagasse .

Percentage of separation of hemi cellulose from fibrous material is 92%.

Outlet 1 goes to solubilizer 2, Outlet 2 goes to Evaporator

Water = 92.30%

Cellulose = 3.31%
Cellulose = 24.14%
Hemi cellulose = 2.06%
Hemi cellulose = 1.27%
Lignin = 3.5% Lignin = 12.76%
Ash = 0.625% Ash = 4.77%
H2O = 57.066%

Cellulose = 0.22%
Hemi cellulose = 2.184%
Lignin = 0.035%
Ash = 0.0127%
H2O = 97.54%

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 Table 6.2 Material balance for solubilizer 1

Inlet Stream Outlet 1 Outlet 2

Component
(Tons/batch) (Tons/batch) (Tons/batch)
Cellulose 6.9 6.5 0.4
Hemi cellulose 4.3 0.344 3.956
Lignin 3.5 3.435 0.065
Ash 1.3 1.277 0.023
Water 195 15.36 176.64
26.916 181.084
Total 208
208

6.1.2 MATERIAL BALANCE AROUND EVAPORATOR:

The inlet stream to the evaporator is coming from the solubiliser 1 containing
high amount of water.

H20 = 100%
H2O = 99.73%
Hemi cellulose = 0.2208%
Lignin = 0.035%
Hemi cellulose = 89.01%
Ash = 0.0127%
Cellulose = 9.009%
Lignin = 1.462%
Ash = 0.517%

21
 Table 6.3 Material balance for Evaporator

Inlet Stream Outlet 1 Outlet 2

Component
(Tons/batch) (Tons/batch) (Tons/batch)
Cellulose 0.4 0 0.4
Hemi cellulose 3.956 0 3.956
Lignin 0.065 0 0.065
Ash 0.023 0 0.023
Water 176.64 176.64 0
176.64 4.444
Total 181.084
181.084

6.1.3 MATERIAL BALANCE AROUND PRECIPITATOR:

Table 6.4 Material balance for precipitator

Inlet Stream Outlet 1 Outlet 2
Component
(Tons/batch) (Tons/batch) (Tons/batch)
Cellulose 0.25 0.025 0.23
Hemi cellulose 0.213 0.01 0.203
Lignin 3.325 3.12 0.205
Ash 0.035 0.001 0.035
Water 14.5 12.54 14.45
NaOH 332.4126 20.52 311.89
HCl 33.241 6.32 26.921
32.52 353.959
Total 386.97
386.97

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6.1.4 MATERIAL BALANCE AROUND SOLUBILIZER 2:

Solvent used is 10 - 24 % NaOH solution.

Amount of NaOH used is in the ratio of 1:13

Water used is 349.908 tons/ 27 tons of fibrous material .

Percentage of separation of lignin from fibrous material is 95%.

Outlet 1 goes to precipitator, Outlet 2 goes to bleaching column.

TO PRECIPITATOR
Cellulose = 0.071%
Hemi cellulose = 0.0607%
Lignin = 0.948%
NAOH = 92.85 NaOH = 94.775%
H2O = 4.134%
Cellulose = 1.724%
Hemi cellulose = 0.09%
Lignin = 0.911
Ash = 0.33%
H2O = 4.07%
TO BLEACHING
Cellulose = 23.952%
NaOH = 67.02%
H2O = 3.29%
Hemi cellulose = 5.02%
Lignin = 4.77%

23
 Table 6.5 Material balance for Solubilizer 2

Inlet Stream Outlet 1 Outlet 2

Component
(Tons/batch) (Tons/batch) (Tons/batch)
Cellulose 6.5 0.25 6.25
Hemi cellulose 0.344 0.213 0.131
Lignin 3.435 3.325 0.11
Ash 1.277 0.035 1.277
Water 15.36 14.5 0.86
NaOH 349.908 332.4126 17.4954
350.735 26.0934
Total 376.824
376.824

6.1.5 MATERIAL BALANCE AROUND BLEACHING COLUMN:

Bleaching element used in this column is sodium chlorite.
The ratio of NaClO2 to fibrous material is 1:0.3.

NaClO2 = 23.0163%

Cellulose = 18.44%
Lignin = 0.324% Cellulose = 94.51%
Hemi cellulose = 0.386% Hemi cellulose = 0.093%
Ash = 3.66% Lignin = 0.578%
NaOH = 55.03% Ash = 0.124%
NaCO2 = 4.68%

Cellulose = 2.189%
Hemi cellulose = 1.36%
Lignin = 0.799%
Ash = 13.522%
NAClO2 = 82.11%

24
 Table 6.6 Material balance for bleaching column

Inlet Stream Outlet 1 Outlet 2

Component
(Tons/batch) (Tons/batch) (Tons/batch)
Cellulose 6.25 6.05 0.2
Hemi cellulose 0.131 0.006 0.125
Lignin 0.11 0.037 0.073
Ash 1.242 0.008 1.235
Water 0.86 0.45 0.42
NaOH 17.4954 3.426 14.023
NaClO2 7.8 0.3 7.5
10.277 23.576
Total 33.8884
33.884

6.1.6 MATERIAL BALANCE AROUND DRIER:

Cellulose to air ratio taken for drying is 1:1.5.

Humid air = 10.2

Cellulose = 6.453tons/batch Cellulose = 5.953tons/batch

Dry air = 9.7

25
6.1.7 MATERIAL BALANCE AROUND REACTOR:

In reactor the conversion of cellulose is 96%

Celluose entering into the reactor = 5.953 tons/batch

Sodium hydroxide entering the reactor = 1.7638 tons/batch

Cellulose converted in the reactor to celluloseNa = 5.953*0.96

= 5.7148tons/batch

CelluloseNa formed in the reator = 6.49 tons/batch

Ethylchloride entering the reactor = 2.625 tons/batch

Amount of celluloseNa converted into Ethyl cellulose = 6.49*0.96

= 6.2304 tons/batch

Amount of Ethyl cellulose formed In the reactor = 6.430 tons/batch

C2H5Cl = 10.012%

C6H9O5C2H5 = 25.522%
Cellulose = 22.70% NaCl = 8.10%
NaOH+H20 = 67.27% NaOH = 0.3233%
C6H10O5 = 1.1037%
H2O = 62.044%
C6H9O5Na = 1.1108

26
 Table 6.7 Material balance around reactor

Inlet Stream Outlet 1

Component
(Tons/batch) (Tons/batch)
Cellulose 5.953 0.2782
NaOH 17.638 0.0815
C2H5Cl 2.625 0.105
Ethyl cellulose 0 6.433
Water 0 15.6382
NaCl 0 2.042

Rate of mass into the reactor = 26.216

Rate of mass out of the reactor = 26.023
Rate of mass in = Rate of mass out
6.1.8 MATERIAL BALANCE AROUND WATER WASH :
In this unit water wash and neutalisation takes place.
The neutralising element used is hydro choloric acid.
Table 6.8 Material balance around water wash column

Inlet Stream Outlet 1 Outlet 2

Component
(Tons/batch) (Tons/batch) (Tons/batch)
Ethyl Cellulose 6.421 6.405 0.016
NaCl 0.812 0 0.812
Water 143.639 20.218 123.423
C6H9O5Na 0.13 0 0.13
HCL 10 0 10
Total 161.002 161.002

27
6.2 ENERGY BALANCE:
This chapter deals with the energy balance of equipment present in the process
and for streams passing through them. Using energy balance, we can know the flow in
and out of energy around the system and also the total energy required by the system. The
principles that can be related to the energy balance is the law of conservation of energy or
also known as first law of thermodynamics which state that energy neither be created nor
destroyed.

Assumptions:

The system is an open system at steady state.

Steam is used for heating purposes.
Wherever cooling is required, ordinary water is used.

EQUATIONS USED FOR CALCULATION:

General equation

Q Ws = H + Ek + Ep

However, based on the assumption made, the above equation is reduced to the form of:

Q = H = mCpT

Specific heats of the components is taken at standard temperature 250C.

Table 6.9 Specific heats of components
Component Specific heat(250C) KJ/kg K

Cellulose 1.42

Hemi cellulose (Xylan) 1.24

Lignin 1.17

NaOH 3.49

HCl 2.47

H2O 4.18

28
6.2.1 ENERGY BALANCE AROUND SOLUBILIZER 1:

It is the energy used in solubilizer 1

Solubilizer 1 is the steam pre treatment of bagasse.

T=250C T= 2000C

The heat required for steam pre treatment is

Q = m Cp T

Where m = mass of bagasse

Cp = specific heat of baagasse

T = Tf- Ti

Specific heat of bagasse is 0.46 kJ/kg K

Q = m Cp T

= 666.66*0.46*(200-25)

Q = 53666.13kJ/hr

Steam consumption:

Q = Ms cp T

Ms= Q/(Cp T+hlw)

Ms= 22.95kg

29
6.2.2 ENERGY BALANCE AROUND SOLUBILIZER 2:

It is the energy used for hydrolyse Xylan to Xylose

Mf = 15701kg/hr Mp= 1087.225kg/hr

Tin= 2000C Tout= 1600C

Mw=14613kg/hr

CPM = (270.833*1.42+14.33*1.26+143.1*1.17+14579.5*3.49)/(14579.5+427.76)

=3.428kJ/kg.K

The heat released from hydroliser

Q = Mw Cp T +Mp Cp T

= 14613.95*3.46*40+1087.225*3.428*40

= 2171650kJ/hr

Heat in to the solubilizer 2 is

Qin = M Cp T

= 15701*3.42*(200-25)

= 9419029.9kJ/hr

Heat consumed = heat in - heat released

Heat into the solubilizer = Heat out of the solubilizer.

30
6.2.3 ENERGY BALANCE AROUND PRECIPITATOR:

Tin=1600C
Tout=800C
Min=14613kg/hr
M1=1772.5kg/hr

Tout=800C
Mw=1121.708kg/hr

CPM1= (130*1.17+88.33*4.18+263.33*2.47+21.66*3.49)/(503.32)

=2.4782kJ/kg.K

CPMw = (12995.*3.468+602.08*4.18+1121.70*2.47)/(14719.196)

=33.42kJ/kg.K

Heat released during the precipitation is

Q = M1 Cp1T +Mw Cpw T

= 1772.5*2.478*80+1121.708*3.42*80

= 658279.7088kJ/hr

Heat consumed = heat in - heat released

= 1371254.196kJ/hr

Heat in = Heat released + Heat consumed.

31
6.2.4 ENERGY BALANCE AROUND DRIER:

The dryer is dried the sample by 900C from 300C

Tin=300C Tout=900C

Min=268.875kg/hr Mout=248.02kg/hr

The energy required is Q = m Cp T

Mass of cellulose in = 268.875 kg/hr

Cp = C pf *X f + C pf *X w

= 1.42*0.9+4.18*0.1
= 1.696
Q = Min Cp T
= 268.875*1.696*60
Qin = 27360.72kJ/hr

Heat released from drier

Qout = MoutCp T
= 248.04*1.42*60
= 21133.15kJ/hr

Heat absorbed by drier = heat in - heat out

= 6227.57kJ/hr

Heat in = heat released + heat absorbed by drier.

32
SPECIFIC EQUIPMENT DESIGN

In this chapter we have to design thin film evaporator equipment by considering the inlet
and outlet product compositions.

Feed flow rate = 7545.16kg/hr.

Table 7.1 Mass balance for Evaporator

Inlet Stream Outlet 1 Outlet 2

Component
(Tons/batch) (Tons/batch) (Tons/batch)
Cellulose 0.4 0 0.4
Hemi cellulose 3.956 0 3.956
Lignin 0.065 0 0.065
Ash 0.023 0 0.023
Water 176.64 176.64 0
176.64 4.444
Total 181.084
181.084

CALCULATIONS:

Feed Inlet = 7545.16kg/hr

Feed Inlet Temp. = 25C

B P of water = 100C at ATM. Pressure

Specific Heat of feed Solution = 0.2992 kcal/kg C

Latent Heat of steam = 1074.21Btu/lb = 597.594 kcal/kg

Hot fluid Circulation Rate:

m =554.12kg hr

Density of hot Fluid is 54.58 kg/m3 at feed conditions

q = 10.152 m3/hr

33
7.1 Power consumption:

Feed pump:

Feed rate = 7545.16 kg/hr

Density = 1590kg/ m3

Diff. head = 15m

HHP = (m3/hr)* diff. head * S.G/274

= 4.745*15*1.57/274

= 0.407

BHP = HHP/efficiency

= 0.407/0.6 = 0.67HP

Hot fluid circulation pump:

Feed rate = 554.12 m3/hr

Density = 54.58 kg/ m3

Diff. head = 15m

HHP = (m3/hr)* diff. head * S.G/274

= 20.3*15*0.018/274

= 0.02

BHP = 0.02/0.25 = 0.08HP.

7.2 LMTD calculation:

Thi = 200C

Tci = 25C

mh =554.12 kg/hr =0.153 kg/sec

mc = 0.405kg/sec

34
Cpc = 0.2992 kcal/kg0C

Figure 7.1 Thin film Evaporator

Cph = 0.5494kcal/kg0C

Ch = mh * Cph = 0.087kcal/s C

Cc = mc * Cpc = 0.12117 kcal/s C

Cmin = 0.087

Cmax = 0.12117

C* = Cmin/ Cmax <=1

= 0.717 <= 1

Thi = Hot Fluid Temperature (Inlet Temperature)

Tci = Cold Fluid Temperature (Inlet Temperature)

Cmin = Smaller of the two magnitudes of Ch & Cc

Cmax = Smaller of the two magnitudes of Ch & Cc

Ch = Hot fluid flow steam heat capacity rate, kcal/kg C

CC = Cold Fluid Flow Steam heat capacity rate, kcal/kg C

35
TLM =( T1-T2)/ln(T1/T2)

T1= Thi - Tci = 400-25 =175C

T2 = Tco - Tho = 130-120 = 10C

TLM = 57.647C

Assume fouling factor F=0.5;

Overall heat transfer coefficient as U =150 kcal/hr m2 C

Total Heat Load = Sensible Heat + Latent Heat

Q = (m x cp x T) + (xm)

= (554.12* 0.549*(80+273.15)) + 416.57

= 107803.36kcal/kg

Q = UAFTLM

Area A = Q/ (U*TLM)

= 24.93m2

Depending on the velocity criterion ID of WFE shall be calculated as under:

Maximum allowable vapour velocity is 3 m/s and min velocity is 1 m/s. For Design
assumed minimum possible velocity i.e. 1 m/s.

Vol. flow rate = ( rate of evaporation/density)

= 20.3/54.58 =0.371m3/hr

Velocity v = (vol. flow rate /Area)

1 = 0.371/((/4)*Di2)

Di = 688mm

36
7.3 Number of blade calculations:

Blade Size: 250 mm H 70 mm W 12 mm Thk

Effective Heat Transfer Height: 4300-500 (Required for distribution Plate) =3800 mm
Number of Blades in each row: 3800/250 =15 Nos.

Blades are welded 90 apart to the inner rotating cylinder.

Hence the required blades are as under: Total Blades: 15 4 = 60 Nos.

7.4 Power calculation:

Considering Gland losses, transmission losses and gear box losses to 50%. Hence the
agitator power consumption will reduced to 50% efficiency.

Total Power Required HP = 20.06 HP

Jacket thickness calculations:

Total Length: 7000 mm

Jacket ID: 700 mm

Design Temp : 300 C

Design Pressure: 5 bar (g)

MOC of Material is SS304 and properties are as under

Composition as : Cr: 18% and Ni: 8%

Design Stress: 113.2 N/mm2 at 300 C

Joint Efficiency : 0.85

Thickness is calculated as under: ts = 19 mm

Hence the diameter of the evaporator is 688mm

And the height of the thin film evaporator is 3.8m.

Thus the design of evaporator is completed.

37
8.1 MATERIALS OF CONSTRUCTION:

This chapter gives an insight to the of type of materials used and methods of the
construction of various equipment used in this process like reactors,evaporators, drier,
water wash columns, precipitators etc

The selection of materials of construction for chemical engineering equipment is

not a trivial matter. The choice of material influences the safety, reliability, lifetime, and
cost of the equipment. Many criteria must be considered, and many types of materials
exist.The used material for the equipment should some following properties like
temperature, pressure etc.

8.2 Types of materials:

There are many classes of materials

Metals: The most common class of materials for chemical engineering equipment
because they generally are easy to fabricate, have high strength, and are resistance to
fracture. Pure metals and metallic alloys are included under this classification. Some
commonly used metals are Iron and steel.

Although many materials have greater corrosion resistance than iron and steel,
cost aspects favor the use of iron and steel. As a result, they are often used as materials of
construction when it is known that some corrosion will occur. In general, cast iron and
carbon steel exhibit about the same corrosion resistance. They are not suitable with dilute
acids, but can be used with strong acids, since a protective coating composed of corrosion
products forms on the metal surface. Carbon steel plates for reactor vessels are a good
example. This application generally requires a minimum level of mechanical properties,
weld ability, formability, and toughness as well as some assurance that these properties
will be uniform throughout.

Stainless steel: There are more than 100 different types of stainless steels. These
materials are high chromium or high nickel-chromium alloys of iron containing small

38
amounts of other essential constituents. They have excellent corrosion-resistance and heat
resistance properties. The addition of molybdenum to the alloy increases the corrosion
resistance and high temperature strength. If nickel is not included, the low temperature
brittleness of the material is increased and the ductility and pit type corrosion resistance
are reduced. The presence of chromium in the alloy gives resistance to oxidizing agents.

Polymers: Use in piping, valves and equipment is increasing, particularly as strength and
temperature stability are increased.

IMPORTANT MATERIALS AVAILABLE:

1. Iron and Steel:

Although many materials have greater corrosion resistance than iron and steel, cost
aspects favor the use of iron and steel. As a result they are often used as a material of
construction when it is known that some corrosion will occur. They are not suitable
for use with dilute acids, but can be used with many strong acids, since a protective
coating composed of corrosion products forms on the metal surface.

2. Stainless Steel:

There are more than 100 different types of stainless steels. The main reason for the
existence of stainless steels is in their resistance to corrosion. Chromium is the main
alloying element, and the steel should contain at least 11%. Chromium is a reactive
element but it and its alloys passivity exhibit excellent resistance to many
environments. So stainless steel contains chromium, nickel, iron, and also containing
small amount of other essentials properties. They have excellent corrosion resistance
and heat-resistance properties.

3. Nickel and its Alloy:

Nickel exhibits high corrosion resistance to most alkalies. The strength and hardness
of nickel is almost as great as carbon steel. In general, oxidizing conditions promote
the corrosion of nickel, and reducing conditions retard it. Monel, an alloy of nickel
containing 67% nickel and 30% copper is often used in food industry. This alloy is

39
stronger than nickel and has better corrosion resistance properties than nickel or
copper.

4. Copper:

Copper and Copper base alloys are used in the formation of heat exchanger tubing,
piping, fittings, etc. although corrosion rates are comparatively small.

5. Aluminum:

The lightness and relative ease of fabrication of Aluminum and its alloys are factors
favoring the use of these materials.

8.3 Criteria for selection:

Following are the primary criteria for materials selection. The weighting of these
is somewhat flexible, although those influencing safety trump all others.

Strength
Ease of fabrication
Tendency to form sparks
Corrosion and chemical resistance
Resistance to mechanical and thermal shock
Oxygen resistance
cost
Temperature stability

40
SAFETY, HEALTH AND ENVIRONMENTAL ASPECTS
This chapter includes the study of various safety, health and environmental factors
along with the material safety data sheets (MSDS) of ethyl cellulose and ethyl chloride.
The goal of chemical plant is not only to produce the chemicals, but to produce them
safely. In the plants chain of processes and operations, loss of control anywhere can lead
to accidents and then losses of life and property from hazards. Attempts should be made
to prevent troubles from the inspection while designing, fabricating and operating.

9.1. HUMAN HEALTH AND ENVIRONMENT:

Several studies of cellulose and its derivatives in different species following oral and
non-oral routes have been published. The toxicological data on modified celluloses
include acute toxicity, subchronic and chronic toxicity and genotoxicity as well as
reproductive and developmental toxicity and can be found in a number of reviews. The
safety assessment of ethyl cellulose is based on the totality of available evidence
including metabolic, mutagenicity, and toxicological data in general, and on the resulting
exposure to ethyl cellulose from its proposed uses. As indicated earlier, ethyl cellulose
has been approved as a multipurpose additive for its use as a binder and filler, protective
coating for tablets, and as a fixative in flavoring compounds. Ethyl cellulose has been
assessed for safety-in-use by national and international regulatory and other agencies. In
these comprehensive safety evaluations as part of regulations, cellulose and its
derivatives, including ethyl cellulose has been extensively reviewed and demonstrated to
be safe for use as a food ingredient or dietary supplement at the levels described in those
assessments

Safety generally involves:

1. Identification and assessments of the hazards
2. Control of hazards
3. Control of the process by provision of automatic control system, interlocks, alarms, etc.
4. Limitation of the loss, by press relief, plant layout, etc.

41
9.2 PLANT MAINTENANCE:

Plant maintenance is another critical phase in plant safety. It is vital that plant
maintenance and repairs be conducted in a manner to preserve the integrity of the plant
and equipment. How often do we see machinery guards removed to affect a repair and
then left lying or worse yet, discarded? Every time this is done a trap to set for the
unwary or unthinking man who follow.

Maintenance practices in themselves offer many opportunities to improve safety

performance. Emphasis should be placed on the use of the correct tools, and those should
be kept in good condition.

9.3. TRANSPORTATION AND SAFETY CONCERNS:

The proper training of plant personnel in safety procedures is not only important, it is
required by OSHA. The ethyl cellulose industry has an enviable safety record, even
though there are numerous safety hazards that can pose significant risk. While state and
federal laws set certain requirements, it is important for management to go beyond these
base regulations by placing a strong company emphasis on plant safety. No matter what
the size of the plant, a Safety Director, responsible for encouraging and enforcing safety
procedures, needs to be appointed. An important first step is to either develop a safety
manual internally or hire an experienced safety consultant to develop one. This manual
will serve as the guide to implementing an effective safety program that will minimize
on-the-job injuries. In addition, a well-developed safety manual will also reduce the
number of OSHA violations by pointing out problem areas in advance. It is important to
establish an environment of safety first right from the start.

9.4 SAFETY RECOMMENDATIONS:

The plant safety manual should cover basic safety expectations, enforcement provisions
and other critical operational procedures, including:

Lockout/Tagout

Confined space entry

42
 Use of personal protective equipment

Emergency response

Hazard communication (employee right-to-know)

Hot works

Respiratory protection

Fall protection

Other related management issues affecting the facility

Train employees at the time of initial employment about the safety program, safety
expectations and how employees will be held accountable for the implementation of the
plants safety program.

All personnel should have an understanding of hazardous materials present in the plant.
This includes training them on how to work with those hazardous materials safely (prior
to use) and the use of any appropriate personal protective equipment.

9.5 MSDS SHEET FOR ETHYL CELLULOSE:

Chemical Product and Company Identification

Product Name : Ethylcellulose
CAS# : 9004-57-3
Chemical Name : Ethyl Cellulose Ethoxyl Content 48%
Chemical Formula : C6H9O5C2H5

1. HAZARD IDENTIFICATION
EMERGENCY OVERVIEW:
Appearance: white to liqht tan
Cautionl: This is expected to be a low hazard for usualindustrial handling May cause eye
and skin irritation. May cause respiratory and digestive tract irritation.
Target Organs: None

43
POTENTIAL HEALTH EFFECTS: Effects
Eyes: May cause irritation Low hazard for nomnal insustrial handling.
Skin: May cause skin irritation Low hazard for usual industrial handling Ingestion
Inhalation: May cause respiratory tract irritation .Low hazard for usual induatrial
handling.
Ingestion:.May cause gastreintestingal initation with nausea vomiting and diarrhea .Low
hazard for usual industrial handling.

2.FIRST AID MEASURES

Eye Contact: Flush eyes with pienty of water for at least 15 minutes. Occasionaliy lifting
the upper and lower eyelids .If irritation develops .get medical aid.

Skin Contact: Flush skin with plenty of soap and water for at least 15 minutes.while
removing contaminated clothing and shoes. Get medical aid if irritation develops or
persists.

Inhalation: Remove from exposure to fresh air immediately.If not breathing

giveartificial respiration .If breathing is difficult .give oxygen.Get medical aid if
cough or other symptoms appear.

Ingestion: .If victim is conseious and alert,give 2-4cuptuls or milk or water.Never

give andything by mouth to an unconscious person.Get medical aid if irritation of
symptoms occur..

3. FIRE FIGHTING MEASURES:

General information:

As in any fire wear a self-contained breathing apparatus in pressure-demand.

MSHA/NIOSH(approved or equivalent),and full protective gear During a fire
irritating and highly toxic gases.may be generated by thermal decomposition or
combustion.

Extinguishing Media:.

Use water fog dry chemical carbon dioxide .or regular foam.

44
4. ACCIDENTAL RELEASE MEASURES:

General information: Use proper personal protective equipment as indicated in

Section 8
Spills/Leaks: Clean up spills immediately,observing precautions in the Protective
Equipment section:Sweep up or absorb material ,then place into a suitable clean
dry.closed container for disposal .Avoid generating dusty conditions ,Provide
ventilation

5. HANDLING AND STORAGE :

Handling: Wash thorougnly after handling ..Use only in a well-ventilated area.

Minimize dust generation and accumulation Avoid contact with eyes.skin,and
clothing ,Avoid ingestion and inhatation.
Storage: Keep container closed when not in use Store in a cool dry. Well-ventilated
area away from incompatible
substances
6. OSHA VACATED PELS:
Ethyl Cellulose Ethoxyl CONTENT 48%
No OSHA Vacated PELS are listed for this chemical.
Personal Protective Equipment.
Eyes:
Wear appropriate prctective eyeglasses or chemical safety goggles as desoribed by
OSHA`S eye and face protection regulations in 29OFR 1910.133 European Standard
EN166.
Skin: Wear appropriate prctective gloves to prevent skin exposure.
Clothing: Wear appropriatel protectiv closthing to prevent skin exposure.
Respirators:
Follow the OSHA Respirator regulations found in 29CFR 1910.134 or European
Standard EN 149.Always use
a NIOSH or European Standard EN 149 approved respirator when necessary.

45
7.STABILITY AND REACTIVITY:
Chemical stability: stable under normal temperatures and pressures.
Conditions to avoid: incompatible materials,strong oxidants
Incompatiblities with other materials: strong-oxidizing agents
Hazardous decomposition products: carbon monoxide carbon dioxide
Hazardous polymerization: will not occur
8. ADDITIONAL INFORMATION
MSDS Croation Date:5/04/1008 Revision #2 Date:8/02/2000
The information above is believed to be accurate and represents the best information
currently available to us.However,we make no warranty of merchantability or any other
warranty,express or implied with respect to such information,and we assume no liability
resulting from its use.Users should make their own investigations to determine the
suitability of the information for their partioular purposes.In no way shall the company
beliable for any claims,losses or damages of any third party or for lost profits or any
special. Indirect,incidental,consequential or exemplary damages howsoever arising,even
if the company has been advised of the possibility of such damages.

46
INSTRUMENTATION AND PROCESS CONTROL

This chapter gives an insight to the of type of instrumentation used and process
control of various equipment. The modern industrial plant relies on instrumentation as a
regular part of its production equipment. In a few, industrial instrumentation is simple. In
the vast majority, instrumentation is more elaborate, and, in an increasing number of
processes, complete instrumentation is a necessity without which the plant cannot operate
efficiently. A whole new field is gradually taking shape, and the instrumentation
engineers becoming an important factor in the engineering of newly designed
manufacturing processes.

Process instrumentation, whether it is the temperature control of a milk cooler, the

operation control means for a distillery, or the control means for a large steel plant, is still
accomplished largely by experience. As instrumentation analysis adopts more of the
analytical approach, pure study will become more useful.

10.1 INSTRUMENTATION AND CONTROL OBJECTIVES:

The primary objective of the designer when specifying instrumentation and control
schemes are:

1. Safer Plant Operation:

a) To keep the process variables within known safe operating limits.

b) To detect dangerous situations and to provide alarms & automatic shut-

down systems.

c) To provide inter locks and alarms to prevent dangerous operating

procedures.

2. Production rate: To achieve the design product output.

3. Product Quality: To maintain the product composition within specific quality

standards.

4. Cost: To operate at the lowest production cost, commensurate with other objects.

47
10.2 COMPONENTS OF THE CONTROL SYSTEM

Process: Any operation or series of operations that produces a desired final result is a
process.

Measuring Means: Measuring means of all the parts of the control system, the
measuring element is perhaps the most important. If measurements are not made
properly the remainder of the system cannot operate satisfactorily.

Analysis of Measurement:

Variables to be Measured:

a) Pressure Measurements

b) Temperature Measurements

c) Flow Rate Measurements

d) Level Measurements

Variables to be Recorded:

e) Indicated temperature

f) Composition

g) Pressure

Controller:

The controller is the mechanism that responds to any error indicated by the error
detecting mechanism. The output of the controller is some predetermined function of
the error. In the controller there is also an error-detecting mechanism which
compares the measured variables with the desired value of the measured variable, the
difference being the error.

48
Final Control Element:

The final control element receives the signal from the controller and by some
predetermined relationships changes the energy input to the process.

10.3 ALARMS AND SAFETY TRIPS:

Alarms are used to alert operators of serious, and potentially hazardous, deviations in
process conditions. Key instruments are fitted with switches and relays to operate
audible and visual alarms on the control panels.

The basic components of automatic trip systems are:

1. A sensor to monitor the control variable and provide an output signal when a
preset valve is exceeded (the instrument).

2. A link to transfer the signal to the actuator usually consisting of a system of

pneumatic or electric relays.

3. An actuator to carry out the required action, close or open a valve, switch off a
motor.

10.4 FLOW CONTROLLERS:

These are used to control feed rate into a process unit. Orifice plates are by far the most
common type of flow rate sensor. Normally, orifice plates are designed to give pressure
drops in the range of 20 to 200 inch of water. Venture tubes and turbine meters are also
used.

10.5 TEMPERATURE CONTROLLER:

Thermocouples are the most commonly used temperature sensing devices. The two
dissimilar wires produce a milli volt emf that varies with the hot junction
temperature. Iron constricted thermocouples are commonly used over the 0 to
13000F temperature range.

49
10.6 PRESSURE CONTROLLER:

Bourdon tubes, bellows, and diaphragms are used to sense pressure and differential
pressure. For example, in a mechanical system the process pressure force is balanced
by the movement of a spring. The spring position can be related to process pressure.

10.7 LEVEL CONTROLLER:

Liquid levels are detected in a variety of ways. The three most common are:

1) Following the position of a float that is lighter than the fluid.

2) Measuring the apparent weight of a heavy cylinder as it buoyed up more or less by

the liquid.
3) Measuring the difference in static pressure between two fixed elevations, one in
the vapor above the liquid and the other under the liquid surface. The differential
pressure between the two liquid level taps is directly related to the liquid level in
the vessel.
10.8 CONTROL VALVES:

The interface with the process at the other end of the control loop is made by the final
control element is an automatic control valve with throttles the flow of a stem that
open or closes an orifice opening as the stem is raised or lowered. The stem is
attached to a diaphragm that is driven by changing air pressure above the diaphragm.
The force of the air pressure is opposed by a spring.

50
PLANT LOCATION

This chapter includes the place where the plant is decided to setup and also checking
the availability of all the facilities required for the plant. The location of the plant has
a crucial effect on the profitability of a project and scope of future expansion. Many
factors must be considered while selecting a suitable site and of the plant on studying
many factors Samarlakota in Andhra Pradesh is selected as the best place.
The principal factors to be considered are:

Marketing area.

Raw material supply.

Transport facilities.

Availability of labor.

Availability of utilities: water, fuel, power.

Availability of suitable land.

Environmental impact and effluent disposal.

Local community considerations.

Climate.

Political strategic considerations.

11.1.1. Marketing Area: For materials that are produced in bulk quantities: such as
cement, mineral acids and fertilizers, where the cost of the product per ton is
relatively low and the cost of transport a significant fraction of the sales price, the
plant should be located close to the primary market. In an international market, there
may be an advantage to be gained by locating the plant within an area with
preferential tariff.

51
11.1.2. Raw Materials: The availability and price of suitable raw materials will often
determine the site location. Plants producing bulk chemicals are best located close to
the source of the major raw material; where this is also close to the marketing area.

11.1.3. Transport: The transport of materials and products to and from plant will be
an overriding consideration in site selection. If practicable, a site should be selected
that is close at least two major forms of transport: road, rail, waterway or a seaport.
Road transport is being increasingly used, and is suitable for local distribution from a
central warehouse. Rail transport will be cheaper for the long-distance transport of
bulk chemicals. Air transport is convenient and efficient for the movement of
personnel and essential equipment and supplies, and the proximity of the site to a
major airport should be considered.
11.1.4. Availability of Labor: Labor will be needed for construction of the plant and
its operation. Skilled construction workers will usually be brought in from outside
the site, but there should be an adequate pool of unskilled labor available locally and
labor suitable for training to operate the plant. Skilled tradesmen will be needed for
plant maintenance. Local trade union customs and restrictive practices will have to
be considered when assessing the availability and suitability of the labor for
recruitment and training.
11.1.5. Utilities (services): The word utilities is now generally used for the
auxiliary services needed in the operation of any production process. These services
will normally be supplied from a central facility and will include:
Electricity - Power required for electrochemical processes, motors, lightings and
general use.
Steam for process heating - The steams required for the process are generated in the
tube boilers using most economic fuel.
Cooling water - Natural and forced draft cooling towers are generally used to provide
the cooling water required on site.

52
 Water for general use - The water required for the general purpose will be taken from
local water supplies like rivers, lakes and seas. Because of this reason all the plants
located on the banks of river.
Dematerialized water - Dematerialized water, from which all the minerals have been
removed by ion-exchange is used where pure water is needed for the process use, in
boiler feed water.
Refrigeration - Refrigeration is needed for the processes, which require temperatures
below that are provided by the cooling water.
Inert-gas supplies.

Effluent disposal facilities - Facilities must be provided for the effective disposal of
the effluent without any public nuisance.
11.1.6. Environmental Impact and Effluent Disposal: All industrial processes
produce waste products, and full consideration must be given to the difficulties and
coat of their disposal. The disposal of toxic and harmful effluents will be covered by
local regulations, and the appropriate authorities must be consulted during the initial
site survey to determine the standards that must be met.
11.1.7. Local Community Considerations: The proposed plant must fit in with and
be acceptable to the local community. Full consideration must be given to the safe
location of the plant so that it does not impose a significant additional risk to the
community. Land (site considerations) sufficient suitable land must be available for
the proposed plant and future expansion. The land should be ideally flat, well
drained and have loadbearing characteristics. A full site evaluation should be made
to determine the need for piling or other foundations.
11.1.8. Climate: Adverse climatic conditions at site will increase costs. Abnormally
low temperatures will require the provision of additional insulation and special
heating for equipment and piping. Stronger locations will be needed at locations
subject to high wind loads or earthquakes.

53
11.1.9. Political and Strategic Considerations: Capital grants, tax concessions, and
other inducements are often given by governments to direct new investment to
preferred locations; such as areas of high unemployment.
The present plant may be locate in samarlakota near kakinada because of its
favorable conditions cited below:

Raw materials- one of the key raw materials, bagasse is available from the sugar
factory in smarlakota . Water will be available from river Godavari.

Markets-New market opportunities will be developed as the project on Industrial

Corridor is implemented. Otherwise also ethyl cellulose can be marketed to China as
it is going to be a single largest consumer in Asia.

Energy availability- GVK Power Station is located nearby and one more thermal
power station is available in vemagiri near rajhamundry.

Transportation facilities- It is well connected by Rail and Road to all states in India.
The sea port facilities are excellent as it is near to kakinada.

Climate- No severe climatic conditions exist in this part of India

Water supply- Godavari waters is being used. Most of the water requirement for
process cooling purposes sea water can be used.

Labor supply- Skilled, semiskilled and unskilled labor are available in samarlakota
and kakinada.

Taxation and legal restrictions- The tax rules and legalities are favorable to promote
industries.

Site characteristics- these are good for setting up an industry. The costs are moderate
in and around samarlakota area.

Flood and Fire protection-No flood prone area. It is near to the industrial belt and the
plant will be constructed taking preventive measures to fire hazards and fail safe
methods in any eventuality

54
PLANT LAYOUT

This chapter includes the layout of the whole plant which gives brief idea for
understanding the overall process in the plant.

The economic construction and efficient operation of a process unit will depend
on how well the plant and equipment specified on the process flow sheet is laid out. The
principal factors considered are:
Economic considerations: construction and operating costs.
The process requirements.
Convenience of operation.
Convenience of maintenance.
Safety.
Future expansion.
Modular construction.

12.1 Economic considerations:

The cost of construction can be minimized by adopting a layout that gives the
shortest run of connecting pipe between equipment, and at least amount of structural steel
work. However, this will not necessarily be the best arrangement for operation and
maintenance.

12.2 Process requirements:

An example of the need to take into account process consideration is the need to
elevate the base of columns to provide the necessary net positive suction head to a pump
or the operating head for a thermosiphon reboiler.

12.3 Convenience of operation:

Equipment that needs to have frequent attention should be located convenient to
the control room. Valves, sample points, and instruments should be located at convenient
positions and heights. Sufficient working space and headroom must be provided to allow
easy access to equipment.

55
12.4 Maintenance:
Heat exchangers need to be sited so that the tube bundles can be easily with
drawn for cleaning and tube replacement. Vessels that require frequent replacement of
catalyst or packing should be located on the outside of buildings. Equipment that requires
dismantling for maintenance, such as compressors and large pumps, should be places
under cover.
12.5 Safety:
Blast walls may be needed to isolate potentially hazardous equipment, and
confine the effects of an explosion. At least two escape routes for operators must be
provided from each level in process buildings.
12.6 Future expansion:
Equipment should be located so that it can be conveniently tied in with any future
expansion of the process. Space should be left on pipe alleys for future needs, and service
pipes over-sized to allow for future requirements.
12.7 Modular construction:
In recent years there has been a move to assemble sections of plant at the plant
Manufacturers site. These modules will include the equipment, structural steel, piping
and instrumentation. The modules are then transported to the plant site, by road or sea.
The advantages of modular construction are:
Improved quality control
Reduced construction cost
Less need for skilled labor on site
Some of the disadvantages are:
Higher design costs & more structural steel work
More flanged constructions & possible problems with assembly, on site.

Typical plant layout of 2-butanol production plant is shown in the figure below.
In this figure
N- North
G- Gate

56
12.8 Plant layout:

Figure 12.1 Plant layout

57
13. COST ESTIMATION

This chapter includes the detailed study of cost calculations done for the whole
plant and find the rate of return per annum based on Ethyl cellulose sales.

13.1 ESTIMATION OF PRESENT PLANT COST:

The cost estimate of the Ethyl cellulose plant for the production capacity of 2000 TPA
according to the rates and data available is Rs. 30*107 in the year.

Cost estimate of the plant = Rs. 20, 00, 00,000

The chemical engineering Ethyl cellulose plant cost index corresponding to year 1970 =
120

The chemical engineering Ethyl cellulose plant cost index corresponding to year 2015 =
720

The present value of the Ethyl cellulose plant can be estimated from both the indices as

Present value of plant = 20, 00, 00, 000 *(720/120) = Rs. 120*107

13.2 DETAILED COST ANALYSIS:

All the percentage ranges of calculation are obtained from the standard data book:

Plant design and economics of chemical engineering by Timmerhaus.

13.2.1 Direct costs:

Direct costs included all the below costs such as:

1. Purchased cost

2. Installation cost

3. Instrumentation and controls installation

4. Piping

5. Electrical installation

6. Building process and auxiliaries

58
7. Service facilities

8. Yard improvement

9. Land

Purchased cost: It contains the equipment cost-15-40% of fixed capital investment

Assume 30% of the fixed capital investment = 0.3 * 120 * 107 = Rs. 36*107

Installation cost: It include insulation and painting costs-25-55% of purchased cost.

Considering 40% of purchased cost = 0.4 * 36*107= Rs. 14.4*107

Instrumentation and controls cost: 6-30% of purchased cost

Considering 13% of purchased cost = 0.13 * 36*107= Rs. 4.68*107

Piping installation cost: 10-80% of purchased cost

Assume 45% of purchased cost = 0.45 * 36*107= Rs. 16.2*107

Electrical cost: 10-40% of purchased cost

Assume 15% of purchased cost = 0.15 * 36*107 = Rs. 5.4*107

Building process and auxiliaries: 10-70% of purchased cost

Assume 40% of purchased cost = 0.40 * 36*107 = Rs. 14.4*107

Service facilities: 30-80% of purchased cost

Assume 45% of purchased cost = 0.45 * 36*107 = Rs. 16.2*107

Yard improvement: 10-15% of purchased cost

Assume 12% of the purchased cost = 0.12 * 36*107 = Rs. 4.32*107

Land: 4-8% of purchased cost

Assume 6% of purchased cost = 0.06 * 36*107 = Rs. 2.16*107

All the costs calculated are tabulated in the Table 13.1. and the summation of all
the costs give the Total direct costs = Rs. 113.76*107

59
 Table 13.1 Various direct costs

Type of cost Amount(Rs.107)

Purchased cost 36
Installation Cost 14.4
Instrumentation and controls 4.68
installation
Piping 16.2
Electrical installation 5.4
Building Process and 14.4

auxiliaries
Services facilities 16.2
Yard improvement 4.32
Land 2.16
Total Direct costs 113.76

13.2.2 Indirect costs:

Indirect costs include the following costs such as:

1. Engineering supervision

2. Construction expenses

3. Contractor fee

4. Contingency plan

Engineering supervision: 5-30% of direct cost

Assume 15% of direct costs = 0.15 *113.76*107 = Rs. 17.064*107

Construction expenses: 6-30% of direct cost

Assume 10% of direct costs = 0.1 *113.76*107 = Rs. 11.376*107

60
Contractor fee: 2-7% of direct cost
Assume 4% of direct cost = 0.04* 113.76*107 = Rs. 4.55*107
Contingency costs: 5-15% of present cost
Assume 10% of present cost = 0.1 * 113.76*107 = Rs.11.376*107

Table 13.2 Various indirect costs

Type of cost Amount(Rs.107)

Engineering supervision 17.064
Construction expenses 11.376
Contractor fee 4.5504
Contingency costs 11.376
Total indirect costs 44.36

Total indirect costs are calculated by the summation of all the costs present in Table.14.2.
which is = Rs.44.36*107

13.2.3. Fixed capital investments:

Fixed capital investments = Direct + Indirect costs = Rs.158.32*107

13.2.4. Working capital:

Working capital = 10-20% of fixed capital investment

Assume 15% of fixed capital investment = 0.15 * 158.32*107 = Rs. 23.71*107

13.2.5. Total capital investment:

Total capital investment = total fixed capital + working capital = Rs. 181.83*107

13.3. ESTIMATION OF MANUFACTURING COST:

13.3.1. Fixed costs: There are mainly four types of fixed costs. They are:

Depreciation

Local taxes

61
 Insurances
Rent

Depreciation: 10% of fixed capital investment for machinery and 3% of

building value for building = Rs. 20.213*107
Local taxes: 3-4% of fixed capital investment

Assume 4% of fixed capital investment = Rs. 6.13*107

Insurances: 0.4-1% of fixed capital investment

Assume 0.6% of fixed capital investment = Rs. 0.97*107

Rent: 8-12% of the rented land and buildings
Assume 10% of building value = Rs. 1.44*107

Fixed charges = 18% of product cost = Total fixed costs = Rs. 28.64*107
which is summation of costs present in Table13.3.

Total product cost = Rs. 159.11*107

13.3.2. Direct production costs:

These direct production costs are mainly divided into following categories. They are:

1. Raw materials

2. Operating labor

3. Direct supervisory and electrical labor

4. Utilities

5. Maintenance and repairs

6. Operating supplies

7. Laboratory charges

8. Patents and royalties

62
Raw materials: 10-50% of total product cost

Assumed value, 30% of the total product cost = 0.3*159.11*107 = Rs. 47.733*107

Operating Labor: 10-20% of the total product cost

Assume 15% of total product cost = 0.15*159.11*107 = Rs. 23.866*107

Direct supervisory and electrical labor: 10-25% of operating labor

Assume 12% of operating labor = 0.12*23.866*107 = Rs. 2.86*107

Utilities: 10-20% of total production cost

Assume 13% of total production cost = 0.13*159.11*107 = Rs. 20.68*107

Maintenance and repairs: 2-10% of fixed capital investment

Assume 8% of fixed capital investment = 0.08*158.32*107 = Rs. 8.69*107

Operating supplies: 10-20% of cost of maintenance and repairs

Assume 15% of maintenance and repairs = 0.15*8.69*107 = Rs. 1.30*107

Laboratory charges: 0-20% of operating labor

Assume 15% of operating labor = 0.15*23.866*107 = Rs. 3.57*107

Patents and royalties: 2-6% of total product cost

Assume 5% of total product cost = 0.05*159.11*107 = Rs. 7.955*107

Direct production cost = Total direct production costs = Rs. 116.66*107 is given by the
summation of various costs present in table 13.3

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 Table 13.3 Various direct product cost

Type of cost Amount (Rs. 107)

Raw materials 47.733
Operating labor 23.866
Direct supervisory and 2.86
electrical labor
Utilities 20.68
Maintenance and repairs 8.69
Operating supplies 1.30

Laboratory charges 43.579

Patents and royalties 7.955
Total direct product costs 116.66

13.3.3. Plant overhead costs:

Plant overhead costs-50-70% of operating labor+ direct supervisory + Maintenance cost

Assume 55% of total costs = Rs. 18.195*107

Total manufacturing cost = Fixed costs + Direct production costs + plant overhead costs

= 158.32*107 + 116.66*107 + 18.195*107

= Rs.293.58 *107

13.4. GENERAL EXPENSES:

General expenses include various costs in it. They are:

1. Administration costs

2. Distribution costs

3. Research and development costs

64
Administration costs: 40-60% of the operating labor cost

Assume 50% of the operating labor cost = 0.5*23.866*107 =11.93*107

Distribution cost: 2-20% of total product costs

Assume 10% of the total product cost = 0.1*159.11*107 = Rs. 15.91*107

Research and development cost: 0-5% of total direct product cost

Assume 3% of the total direct product cost = 0.03*116.66*107 = Rs. 2.49*107

Total general expenses = Rs. 30.33*107 is given by the summation of various costs
present in Table 13.4

Table 13.4 various general expenses

Type of cost Amount (Rs. 107)
Administration costs 11.9
Distribution costs 15.9
Research and 2.49
development
Total general expenses 30.33

13.5. TOTAL PRODUCT COST:

Total product cost = Manufacturing cost + general expenses
= 293.58*107 + 30.33*107 = Rs. 323.92*107
13.5.1. Current selling price:

Cost of methanol = Rs. 1840 per kg

Total selling price per annum = (2000*103) * 1840

= Rs. 368*107 per annum

13.5.2. Gross earnings:
Gross earnings = Total selling price Total product rate
= 368*107 323.92*107 = Rs. 44.08*107 per annum

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13.5.3. Tax:
Assume the local tax rate as 25%
Tax on the gross earnings = 0.25*44.08*107
= Rs. 11.02*107
13.5.4. Net profits:
Net profits = Gross earnings Tax
= (44.08 - 11.02) *107
= Rs. 33.06*107
13.5.5. Rate of return:
Rate of return = Net profit/Fixed capital investments
= 33.06*107 /159.11*107
= 20.77%
Payback period = FCI/Net profit
= 4.81years.

66
14. BIBLIOGRAPHY

1. A Guide to Chemical Engineering Process Design & Economics, Gael D.Ulrich,

Process Publishing, 1984.
2. Applied Process Design For Chemical & Petro Chemical Plants, E.E Ludwig,
Gulf Professional Publishing, Vol-1,2&3, 3rdEdition, Elsevier,2001.
3. Chemical engineering design, Principles, Practice and Economics of Plant and
Process Design by Gavin Towler & Ray Sinnott, 2008.
4. Chemical Process Safety: Fundamentals with Applications, , Daniel A.Crowl,
Joseph F. Louvar, Prentice Hall,3rd Edition 2011.
5. Handbook of Pharmaceutical Excipients, Ainley Wade & Paul J. Weller, 2nd
edition, The Pharmaceutical Press, London, 1994
6. Polymer data handbook - Kingdware.
7. Petroleum Refining: Materials and Equipment, P. Trambouze, Editions Technip,
2000.
8. Perrys Chemical Engineers Hand Book, 7th edition, 2004.

9. Process Heat Transfer, Donald Q. Kern, International edition, 1965.

10. Unit Operations of chemical engineering, McCabe, Smith, Peter Harriot,

McGraw-Hill Publications, 5th edition,, 2009.

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