Final Project On Rosin Production From Pine Tree

CHEMICAL ENGINEERING DEPARTMENT GC 2008 EC
DEPARTMENT OF CHEMICAL ENGINEERING

TITLE: - PRODUCTTION OF ROSIN FROM PINE TREE
IN PARTIAL FULFELIMENT OF REQUIREMENT FOR BACHILOR
OF SCIENCE IN CHEMICAL ENGINEERING
GROUP MEMBERS
NAME ID NO.
1. MILKESA TESFAYE…………………………R/858/04
2. MERGA TAFA………………………………...R/802/04
3. ABDI BIRA...………………….……………….R/005/03
4. DEBELA GEREMU …………………………..R/181/03
5. YADEF DEBELI……………………………….R/746/04
Advisor Name:-HAFTOM.W
DIRE DAWA, ETHIOPIA 2008 E.C
FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 1

ACKNOWLEDGMENT
First and foremost we want to express our sincere gratitude to our advisor Mr. HAFTOM.W for
his genuine and continuous support in advising, encouragement, initiating and guiding us in very
friendly way while doing this paper. His invaluable ideas and help made our work a lot easier.
Not forgetting his excellent supervision which brought us to successfully complete this paper
within the frame time given.
Secondly, we would like to express our gratitude to technicians and laboratory assistants for
their technical support and assistance especially Mr. BELAY.Z.

Abstract
Rosin is one of bio-based polymer obtained from pine trees. The chemical composition is
chiefly composed of 90% rosin acids and 10% non-acidic resinous materials such as turpentine.
It is a solid form of resin obtained from pines and some other plants, mostly conifers, produced
by heating fresh liquid resin to vaporize the volatile liquid terpene components. It is semi-
transparent and varies in color from yellow to black. At room temperature rosin is brittle, but it
melts at stove- top temperatures.
The use of naturally occurring raw materials in surfactant synthesis is expected to provide new
types of surfactants with better biodegradability. Further, in order to achieve long term
sustainable production, it will become necessary to use renewable sources. It has recently been
used as a novel material for sustained applications such as paper sizing, coatings and drug
release. It can be converted to a large number of downstream derivatives that are used in a wide
range of applications. Synthetic rubber, Paint, Foodstuff, Adhesive, Printing oil, Electrical
equipment, Papermaking, Soap, Construction material, linoleum and floor covering, Metal
processing, Bactericide, Fine chemical, Plastic, Oils and greases, Rubber, Printing inks, Shoe
polish and related materials are application areas of rosin.
Ethiopia has a large, as yet, properly unexploited potential to produce natural gums resin
resources in its different regions. Over 60 gum and resin bearing species are found in the
country. The total area of oleo-gum resin bearing wood lands cover about 2.9 million hectares
of land in the country, with over 300,000 metric tons of natural gum production potential.
Therefore, research and development efforts are necessary for the production and
commercialization of rosin from the large amount of raw material resource available.
This paper provides that the pine resin was processed by the processes of mixing, filtration and
two consecutive distillations. The resulting product was rosin which has the properties of brittle,
transparent, glassy solid and insoluble in water but soluble in organic solvents such as ethanol.
The essential oil called turpentine was also produced as a byproduct at the top product of the
final distillation process.

LIST OF FIGURE page
Figure 2.1 Process flow diagram of rosin production ............................................................................. 20

Figure 2.2 grading of rosin types ............................................................................................................ 23
Figure 2.3 Uses of rosin .......................................................................................................................... 19
Figure 3.1 Colecting of raw material ...................................................................................................... 22
Figure 3.2 raw gum resin ........................................................................................................................ 22
Figure 3.3 Block flow diagram of rosin production ................................................................................ 23
Figure 3.4 Mixing process of gum resin & ethanol ................................................................................. 30
Figure 3.5 Filtration process….……………………………………..…………………………24
Figure 3.6 Distillation process of oleoresin and ethanol……………………………………....25
Figure 3.7 Distillation process of turpentine and rosin…………………………... …………...25
Figure 4.1 Rosin from experiment one ................................................................................................... 34
Figure 4.2 Rosin from experiment two…………………………………………………….….28

LIST OF TABLE Page

Table 2.1. Estimated areas covered by natural gum and resin bearing species in the different
regions in Ethiopia……………………………………………………………………………...7
Table 2.2 Natural gums exported from Ethiopia by various enterprises .................................... 7
Table 2.3 standard quality and property determination .......................................................... 16
Table 2.4 Same application area of rosin ................................................................................ 16
Table 4.1 characteristics of rosin .............................................................................................. 29
Table 6.1 purchase equipment cost .......................................................................................... 39
Table 6.2 Total envestment cost ............................................................................................... 40
Table 6.3 Annual requirement of utility and cost ..................................................................... 41
Table 6.4 Man power requirement ........................................................................................... 42
Table 6.5 Total production cost ................................................................................................ 43
Table 6.6 Project profit and loss ............................................................................................... 45

Contents ............................................................................................................................page
Acknowlegement ......................................................................................................................... I
Absract ....................................................................................................................................... II
List of figure ............................................................................................................................... III
List of table ............................................................................................................................... IV
List of acronyms and Abbreviations ............................................................................................ V

CHAPTER ONE
INTRODUCTION
1.1. Background
Rosin, also called colophony, is a solid form of resin obtained from pines and some other plants,
mostly conifers, produced by heating fresh liquid resin to vaporize the volatile liquid turpentine
components. The term "colophony" comes from colophonia resina or “resin from the pine trees
of Colophon,” an ancient Ionic city.
'Naval stores' is the inclusive term used to denote pine oil and their derivatives. Over centuries
pine resin and pitch were so useful to the sailing ships of the navies of the world that even today
the most commonly used term for pine oil products is 'naval stores'. Rosin starting materials are
obtained from the same source gum, wood, and tall oil rosins are similar in composition. [19]
Rosins and oleoresins have an extremely long history of documented use and human exposure.
Retsina, a traditional Greek wine flavored by adding pine resin (oleoresin) during fermentation,
has been made for more than 3,000 years. Human consumption of gum rosin can be traced back
to Neolithic times (approx. 7400 years) from analysis of pottery that contained traces of a
resinated wine product similar to Retsina wine.
Gum rosin was originally added to wine in ancient Rome as a preservative to prevent conversion
in to vinegar as described by Pliny the Elder in the 1st century A.D. Glycerol ester of gum rosin
was the first rosin ester used for protective coatings and this remains an important commercial
use today. Glycerol ester of gum rosin is used in rosin-based printing inks and in adhesive
tackifiers such as for manufacture of adhesive bandages. Glycerol esters of rosin have also been
used in slow-release pharmaceutical preparations to increase digestive transit time.
In the United States, rosin use dates back to native and colonial American times. Uses of rosin
included manufacture of rosin soaps, leather dressings, shoe polishes, and in pharmaceuticals
such as ointments, astringents, a diuretic and laxative, plasters, veterinary internal remedies and
disinfecting compounds. For many years they were used in unprocessed form in the soap, paper
and varnish industries. Today, most rosin is used in various modified forms in a wide range of
products. [19]

1.2. Statement of problem

Currently Ethiopia is collecting and exporting only the crude gum resin resources and again
imports with foreign currencies their various final products from developed countries. Therefore,
devising mechanisms to promote the countries’ potential for value addition and industrialization
of gum resin products should be one of the priority collaboration line in the near future.
Rosin, which is useful in the production of Soap, detergents, chewing gums and many other
valuable products is not yet produced in the country. On the other hand, the availability of large
amount of oleoresin resource reflects researches and development efforts should be made for the
production and commercialization of rosin.
The conventional commercial detergents contain LABSA as active ingredient. It is a petroleum
product and causes environmental problems i.e., the prepared liquid detergent contains
components like phosphate which may cause problem of eutrophication. Hence, surfactants that
are used for the total substitution of LABSA should be produced for the liquid detergent to be
biodegradable and environmentally friendly.

1.3. Objectives
1.3.1. General objective
 Production of rosin from pine tree
1.3.2. Specific objectives
 Extraction of resin by dissolving gum resin with ethanol and separate an insoluble
matters.
 Separation of oleoresin and ethanol at 80 Co
 Separation of rosin and turpentine from oleoresin at 160 Co.
 Characterization of physical and chemical properties of rosin.

 Economic feasibility calculation
 Energy and material balance of selected equipment
 Sizing of selected materials.

1.4. Significance of study

 To replace the total import of rosin by producing domestic rosin with appropriate quality
and quantity.
 It creates the job opportunity for the peoples of the country, since it is the new industry
for the country.
 It may generate foreign exchange through exports.

1.5. Scope and limitation
1.5.1 Scope
 The scope of our project is from tapping of pine tree up to production of rosin and
characterization of the produced rosin.
1.5.2. Limitation
To achieve our objective there was some sort during the course of this work
 Scarcity of lab equipment’s in our laboratory.

 Some chemical test which is needed for this product is not available in our lab.

CHAPTER TWO
2 LITERATURE REVIEW
Rosin, also known as colophony or Greek pitch, is a solid form of resin obtained from pines and
some other plants, mostly conifers, produced by heating fresh liquid resin to vaporize the volatile
liquid terpene components. It is semi-transparent and varies in color from yellow to black. At
room temperature rosin is brittle, but it melts at stove-top temperatures.
Rosin is the major product obtained from pine. It is in volatile residue. Rosin is a brittle,
transparent, glassy solid insoluble in water but soluble in a number of organic solvents. Most
rosin is used in a chemically modified from rather than in the raw state in which it is obtained. It
consists primarily of a mixture of abietic and pimaric type of acids with smaller amount of
neutral compounds. It can be converted to a large number of downstream derivatives that are
used in a wide range of applications. Synthetic rubber, Paint, Foodstuff, Adhesive, Printing oil,
Electrical equipment, Papermaking, Soap, Construction material, linoleum and floor covering,
Metal processing, Bactericide, Fine chemical, Plastic, Oils and greases, Rubber, Printing inks,
Shoe polish and related materials.[10]
2.1. Source of Rosin

Resin products from pines are commonly called naval stores. There are three classes of resin.
Those are, gum resin, wood resin and tall oil resin. All generated from the pine tree.
 Gum resin - was once the only commercial source of resin. It is obtained by tapping the
trunk of the living pine tree. The harvesting of the resin is simple, involving only periodic
wounding of the tree and collecting of the exudates into cups.
 Wood resin - After harvesting pine trees the stump is allowed to remain in the ground for
about ten years so that its bark and sapwood may decay and slough off to leave the heart
wood rich in resin. Resinous material is extracted from the stump.
 Tall oil resin - is obtained by distillation of crude tall oil (CTO), a by-product of the kraft
sulphate pulping process. CTO contains 70-90% acidic material, which is composed
essentially of fatty acid and tall oil rosin. Tall oil rosin (TOR) has a tendency to
crystallize and usually contains 200-600 ppm sulfur. Highly distilled TOR can produce
esters which are competitive with gum and wood rosin derivatives. [10]
2.2. Chewing Gum

Glycerol ester of gum rosin is approved for use in chewing gum base. According to the National
Association of Chewing Gum Manufacturers and European Association of the Chewing Gum

Industry (NACGM/EACGI 1996), the amount of rosin ester in a chewing gum base may
approach 50 percent. The rosin ester contents of two typical bubble gum bases are 13 and 44
percent, and the rosin ester content of a typical stick gum base is 27 percent. Potential intake of
glycerol ester of gum rosin associated with its approved use in chewing gum was estimated using
data from a Market Facts Consumer Mail Panel survey of chewing gum intake conducted in
1995 that showed that gum users (based on the total surveyed population) chewed a mean
amount of 6.5 grams/day (approximately two sticks of gum). For a heavy (90th percentile) user of
gum, the amount of gum chewed was 13.5 grams.
Based on these use estimates, potential ingested intakes for glycerol ester of gum rosin in
chewing gum were estimated to be 325 mg/day for the mean consumer of chewing gum and 675
mg/day for the 90th percentile consumer if chewing gum was swallowed after chewing and 0.16
mg/day for the average consumer of chewing gum and 0.34 mg/day for the 90th percentile
consumer if the gum was not swallowed. [11]
2.3. World Rosin Production

Total annual production of rosin is about 1.2 million tons world-wide. Of this, it is estimated that
almost 720,000 tons or 60%, is gum rosin; most of the remainder, about 35%, is tall oil rosin and
the rest is wood rosin. The People's Republic of China has been the world's dominant producer
for many years, but a dramatic increase in production, signaled by the installation of an improved
and expanded processing capacity in the early 1980s, has seen Indonesia become the second
biggest producer of gum rosin and turpentine in the world. Chinese production accounts for
430,000 tones (about 60%) of the total annual production of gum rosin and Indonesia accounts
for a further 69,000 tons (almost 10%). [11]
2.4. Production possibility in Ethiopia

Ethiopia is one of the countries well-endowed with various species of Acacia, Boswellia and
Commiphora that are known to produce gum arabic, frankincense and myrrh, respectively.
Available estimates prompt that the total area of oleo-gum resin bearing wood lands cover about
2.9 million hector of land in the country, with over 300,000 metric tons of natural gum
production potential. The trees produce resin in the dry season and provide people with
meaningful economic activities in a period with few other economic activities. [19]

Table: - 2.1. Estimated areas covered by natural gum and resin bearing species in the different
regions in Ethiopia. [19]
National Regional Genus Estimated area (ha)

State
Tigray Boswellia, Sterculia & Commiphora 940,000
Amhara Boswellia, Commiphora & Acacia 680,000
Oromia Boswellia, Acacia & Commiphora 430,000
Gambella Sterculia, Acacia & Commiphora 420,000
Somali Boswellia, Acacia & Sterculia 150,000
Benshangul-Gumuz Boswellia, Acacia & Sterculia 100,000
SNNP* Boswellia, Acacia & Sterculia 70,000
Afar Commiphora & Acacia 65,000
Total 2,855,000
Generally, the availability of large amount of raw material resources reflects that there is a great
opportunity for the production of rosin in Ethiopia. This can be easily conducted by collecting
the crude resin from various regions of the country provided above and then process the raw
material to get the product. The product can easily get the market due to its requirement for many
industries like Paint, Foodstuff, Adhesive, Printing oil, Electrical equipment, Papermaking, Soap,
Construction material, linoleum and floor covering, Metal processing, Bactericide, Fine
chemical, Plastic, Oils and greases, Rubber, Printing inks, Shoe polish and related materials.
Table:-2.2 Natural gums exported from Ethiopia by various enterprises, 1999-2007. [16]
Year Total production Export quantity

(ton) (ton)
1998/1999 4934 1663
1999/2000 4608 1648
2000/2001 4532 2183
2001/2002 4427 2138
2002/2003 4778 1544
2003/2004 7479 3109
2004/2005 4906 3791
2005/2006 2894 3529
2006/2007 1474 3976
Average 4196.36 2383.27

2.5. Raw Material Collections techniques

Resin is obtained from the tree in a manner analogous to rubber tapping except that the exudate
is more viscous and slow-running than rubber latex. Tapping generally involves the following
basic steps:
 Preparation of the face of the tree

 Installation of the resin collection system
 Wounding of the tree to induce resin flow
 Application of a chemical formulation to stimulate and maintain resin flow
 Collection of the resin, re-wounding of the tree, and application of the stimulant at
suitable intervals.
The precise manner in which the above steps are carried out in the various producer countries has
developed in different ways over the course of many years. Nevertheless, it is generally
recognized that tapping should be carried out carefully and in such a way as to avoid permanent
damage to the tree. [19]
2.6. System of tapping

There are two system of tapping. Those are system of using wide face and narrow face. Both
entail the removal of bark and the application of sulphuric acid as a stimulant
1. System of using wide face
2. System of using narrow face
2.6.1. System of using wide face

In order to facilitate installation of the collection system on trees which are to be worked for the
first time, the rough outer bark is first removed from the area at the base of the tree where it is to
be fixed. This rough shaving is usually extended for part of the way up the tree to make the
subsequent tapping easier. Although a two-piece apron and gutter system made of galvanized
iron, this has been dispensed with in Brazil and a specially designed plastic bag is used instead;
this fits across the width of the face and is held flush to the tree by wire which goes round it.
This system is simpler, cheaper and quicker to install than the cup and gutter system, and does
not risk contaminating the resin with dissolved iron (which may result from the corrosive action
of the acid stimulant on the galvanized iron gutter if its application is over-zealous). The risk of
leaving the nails used to fix the apron/gutter system in the tree after tapping has finished, and of
damaging saw blades if the trees are destined for saw timber, is also removed. [19]

A horizontal strip of bark 2-2.5 cm high is removed across the width of the tree, just above the
gutter, to cause the resin to flow and the chemical stimulant, usually acid- is applied along the
top edge of the exposed tissue ('streak'). The combination of bark removal and acid treatment
makes it unnecessary to cut into the wood to open the resin ducts, which was characteristic of
older methods of tapping. Wounding to the tree is therefore only superficial and loss in growth
during tapping is minimal.
The first type of stimulant to be used commercially was a 50% solution of sulphuric acid, applied
as a fine spray from a plastic bottle. This is applied as a thin bead from a plastic bottle and is
now quite widely used, although the precise formulation varies somewhat according to the
availability of local materials. As well as being less wasteful and less hazardous to the person
using it, the paste has the advantage of requiring slightly less frequent applications than the
spray. The greater penetration of the paste requires the removal of a bigger strip of bark than
normal; so in spite of fewer visits to the tree, the total height of the face worked is about the
same as for the spray. [19]
The concentration of the acid used to make the paste may be between 40% and 60% (w/w)
depending on the tapping method used and the climatic conditions under which the paste is
applied. Note: appropriate safety precautions should be taken when preparing, handling and
using strongly acidic materials and their formulations.
During the course of its flow some resin solidifies on the face of the tree before reaching the
receiver. The extent to which this happens depends on the species of pine being tapped. The
solid may be scraped off periodically during the season, or it may be left to the end and collected
and processed separately from the bulk of the resin as it will yield a slightly lower grade of rosin.
2.6.2. System of using narrow face

Procedures using a narrow face are also based on the removal of bark with acid treatment. It is
usually 10 cm wide, brings with it several advantages, the most important being the simpler
system of guttering. A small, flat, arc-shaped piece of galvanized iron is inserted edgewise into
the shaved part of the tree with a special tool; it requires no nails to hold it in place. A clay or
plastic pot is supported under it by a single nail or wooden splint; in appropriate circumstances, a
bamboo cup or coconut shell can be used as the resin receiver.
The height of bark removed at each visit to the tree is similar to that for a wide face, about 2-2.5
cm; the tapping schedule (using spray or paste-based stimulant) is also similar. After working on
one vertical face for four years, another may be started about 10 cm to one side of the first. In
this way, four or five faces, each lasting for four years, may be worked on large trees. If the trees

are large enough, two or more faces may be worked simultaneously; however, although they will
be higher, resin yields for two faces are not twice that for a single face. [19]
The tools and accessories required for tapping are relatively few and simple and include the
following:
 Bark shaving tool, Cup or other form of receiver

 Guttering and Nail(s) (to support cup and/or to fix guttering)
 Hammer, Bark hack
 File or whetting stone (for sharpening bark hack)
 Sulphuric acid-based stimulant (liquid or paste)
 Bottle (plastic, for application of acid)
 Bucket (into which resin from cup is emptied)
 Funnel (for transfer of resin from bucket to drum) , Drum or barrel
 Protective clothing and accessories (for tapper, including visor or goggles, acid-proof
gloves, plastic apron or other garment, and rubber boots).
2.7. Properties of Rosin

Rosin is brittle and friable, with a faint piny odor and it is typically a glassy solid, through some
rosin will form crystals. Especially when brought into solution. The practical melting point
varies with different specimens, it is semi-fluid at low temperature and that is melting at
temperature of 70-150 OC. It is very flammable, burning with smoky flame and therefore the care
should be taken when melting it. [3]
A. Solubility
Insoluble in water; freely soluble in alcohol, benzene, ether, chloroform, glacial acetic acid, oils,
carbon disulfide, and dilute solutions of fixed alkali hydroxides, low toxicity, hard and friable at
room temperature.
B Melting and Flammability

The practical melting point varies with different specimens, some being semi-fluid at low
temperature and melting at the temperature of 70°C to 150°C. It is very flammable (Flashpoint
187°C), burning with a smoky flame, so care should be taken when melting it.

C. Rosin Salts
Rosin combines with caustic alkalis to form salts (rosinates or pinates) that are known as rosin soaps.
D. Deterioration of Rosin
Rosin, particularly when in a powdered form deteriorates rapidly on exposure to air. Oxidized
rosin is insoluble in petroleum ether and can thus be readily detected. It has been stated that
exposure of rosin to air leads to the formation of unstable peroxides which are insoluble in
aliphatic hydrocarbons.
2.8. Chemistry of Rosin

Approximately 80 percent of rosin consists of unsaturated isomeric acids, the most important of
which are abietic and pimaric acids. They belong to the terpene family and their structure can be
divided into isoprene units.
Rosin on refluxing with acetic acid yields abietic acid which can also be obtained by dissolving
rosin in alcohol containing a little hydrochloric acid. Ruzicka has suggested that abietic acid,
C20H3002, has the structure shown in the diagram below. [7]
2.9 Chemical Modifications of Rosin

Due to its high acidity, rosin is seldom used alone or without further processing. Most of the
rosin-derivatives are obtained by neutralization or esterification of the carboxyl group but more
recently new modification has been obtained by reacting the unsaturated linkages. [4]
a. Rosin Soaps
The earliest modifications of rosin were intended to increase its hardness and also to improve the
tackiness of varnishes by reducing its acidity. The carboxyl group of rosin can readily be reacted
with alkalis or metallic oxides to form soaps. The first modification was limed-rosin which may
be considered as the first synthetic resin. Liming of rosin results in a hardened product;
depending upon the amount of lime used. In the case of wood rosin, slightly more lime is
required than with gum rosin in order to obtain a product with the same melting point.

Generally, 5-6 percent hydrated lime (with low carbonate and magnesia content) is used with
larger quantities of lime, a neutral soap is obtained which is insoluble in drying oils and solvents.
b. Rosin ester
Rosin esters have received considerable attention, the glycerol ester, commonly known as "ester
gum," being the most important ester. The preparation of ester gum was described in 1886 by
Schaal'" and the expanding use of tung oil in the paint industry gave the product a merited
impetus. The advantages of using ester gum instead of rosin in drying oil varnishes are mainly
better durability and resistance to water and alkalis, and the possibility of pigmentation with
basic pigments without levering.
Ester gum is obtained by reacting rosin with glycerol at 280-290 °C. The quantity of glycerol
used is 11-12 percent, on the weight of rosin, i.e. about 30-33 per cent, more than the
theoretically required weight. It is not necessary to use an esterifying catalyst although
Aluminium, zinc, and succinic acid have been suggested. A harder resin than ester gum is
obtained when polyglycerol is used.
Rosin has also been esterified with mono-, di-, and tri-ethylene glycol, the melting point of the
ester decreasing with the increasing molecular weight of the glycol. These esters have high
refractive index and are neutral, sticky, adhesive, non-hygroscopic and water insensitive. They
are compatible with most film forming materials, and are miscible with both hydrophilic and
hydrophobic colloids.
c. Polymerized Rosin
Improved properties such as higher melting point, increased solubility and improved colour
retention are obtained when rosin is polymerized. The polymerization can be effected by treating
a solution of rosin with boron triflouride or sulphuric acid. The acid value of the product is
unaffected by polymerization, but the degree of unsaturation is reduced and the melting point is
considerably increased.
d. Oxidized Rosin
In this an unstable peroxide is first formed which helps to oxidize more abietic acid. Rosin can
be oxidized by blowing air or ozone through molten rosin. Metal resinates catalyze the reaction
while phenols retard it. Oxidation changes the properties of rosin and darkens its colour. The
acid value and saponification values are reduced and the oxidized rosins are dark reddish-brown
in colour, have higher melting point and can be incorporated in tung oil.

They exhibit strong anti-oxidizing properties so that when used with drying oils, a larger amount
of drier must be employed. They are brittle but can be plasticized with castor oil. They are used
as shellac-substitutes for air-drying insulating spirit-varnishes and have also found an outlet in
petrol resisting lacquers, nitrocellulose lacquers, spirit varnish stains, spirit chassis blacks,
asphalt emulsions, cement roads, etc.
e. Hydrogenated Rosin
The tendency of yellowing and discoloration of rosin which is associated with the presence of
unsaturated linkages is reduced by hydrogenation. Hydrogenation is carried out by passing
hydrogen under pressure at elevated temperatures in the presence of catalysts. Temperatures
employed range from 125°C to 250°C the pressures may vary from 200 to 15,000 lbs. per sq.
Inch and the catalysts usually used are nickel or copper chromites. Hydrogenation can also be
carried out at room temperature when palladium is used as a catalyst and has been recommended
as an analytical method. Under these conditions, only one double bond is hydrogenated.
Hydrogenation at higher temperatures, for example at 450°C leads to the removal of the carboxyl
group and formation of tetra hydro naphthalene. Various grades of hydrogenated rosins are now
available. An almost colorless grade is obtained by vacuum distillation.
f. Esters of Hydrogenated, Oxidized and Polymerized Rosins
Like rosin, the modified rosins can also be esterified with various alcohols to yield
corresponding esters. Methyl, glycol and glycerol esters of hydrogenated rosin have shown
promise as softeners and tackifiers for rubber, as modifiers and transparentizing agents for
tracing papers, as plasticizers for ethyl cellulose and polyvinyl acetate chloride and as binders for
wool, glass and cellulose fibrous insulation materials. Their use in asphalt laminating adhesives
has also been suggested. These ethers differs from rosin ester in being essentially non-oxidizing.
g. Rosin Oil
When rosin is distilled, rosin oil is obtained which is a mixture of rosin acids and hydrocarbons.
The crude oil distilling up to 250°C is known as kidney oil. On fractionating, a pale yellow to
reddish-brown viscous liquid is obtained. It is used in printing inks, in greases and as a softener
in milling of rubber. Rosin oil has excellent penetrating properties. On beating at temperatures
above 250°C, rosin decomposes and undergoes partial decarboxylation.
2.10. Production process

The separation of rosin in its component parts, rosin and turpentine involve two basic steps:-
1. Cleaning- Cleaning is necessary to remove all extraneous material from the resin, both
solid and soluble. This includes forest debris such as bark, pine needles and insects, which may
have fallen into the cup during its period on the tree, and which require removal by filtration.

Water-soluble impurities carried into the cup by rain water are removed by washing the filtered
resin with water. The approximate composition of crude resin, as it is received at the plant for
processing, is 70% rosin, 15% turpentine and 15% debris and water. . Small amounts of iron
produced by the corrosive action of excess sulphuric acid on galvanized iron guttering and cups
may also contaminate the resin. As the presence of iron would lead to darker, lower-grade rosin,
it is removed by adding oxalic acid prior to filtration. Iron contamination has become less of a
problem as the use of acid paste rather than spray has become more widely adopted. The use of
cups made of plastic or other non-ferrous material eliminates the risk of iron contamination from
this source. [8]
2. Distillation- The cleaned resin is then ready to be distilled, or, to be precise, steam-
distilled, the older type of direct-fired still has given way, almost universally, to a still in which
steam is used both to heat the resin and to facilitate the distillation by co-distilling with the
turpentine vapors. [19]
2.11. Olustee process for the production of turpentine and rosin

Barrels of resin arriving at the plant are immediately weighed and upturned over an iron grill
covering a large concrete or mild steel dump vat. The barrels are placed over steam outlets to
remove the last of the adhering semisolid resin. 'Scrape', the solidified resin which is taken off
the face of the tree at the end of the season and which yields poorer quality rosin, is emptied into
a separate compartment for separate processing.
Figure: -2.1 Process flow diagram of rosin production

The resin is transferred first from the dump vat to a blow-case, and then from the blow-case to a
melter, by the use of steam pressure. Filter aid ( 0.5-0.6 kg/tone of resin) and oxalic acid (0.6-1.2
kg/tone) are added at either of the two units. Turpentine (from a previous distillation) is added to

bring the turpentine content of the resin to between 30% and 40% the precise amount added
depends on whether good quality resin or 'scrape' is being processed. The temperature inside the
melter is raised to 85-100°C by steam, the exact temperature again being dependent on the
quality of the resin. Steam pressure is then used to force the hot resin first through a metal screen
at the bottom of the melter to remove the larger sized solid matter, and then through a filter to
remove all remaining solids.
The filter is of the horizontal or vertical plate type and consists of about 12 plates backed with
filter paper or cloth. The resin passes directly from the filter to the bottom of a wash tank
containing hot water. Each tank holds 1500-2000 liters of water which is sufficient for washing
up to 20000 litres of resin. After washing, the mixture is allowed to settle for at least 4 hours and
preferably overnight. The bottom aqueous layer is then run off to waste, an intermediate layer of
unbroken emulsion ('muck') is run off to be returned to the low grade dump vat for reprocessing,
and the top layer, which consists of washed resin, is drained and pumped to a charge tank in
preparation for distillation.
The still is filled with resin from the charge tank. The temperature is then raised by means of
steam coils to about 110°C at which point live steam is gradually introduced through sparger
valves. As the temperature continues to rise, distillation proceeds and the sparger steam inflow is
increased until, at the end of the distillation, the temperature has reached 160-170°C. The rate of
increase in temperature, and therefore the time taken for the distillation, is dependent on the
steam pressure used; the higher the pressure within the range 8.8-10.5kg/cm (125-150 psi), the
faster the distillation. For still capacities of about 4-5 tones, distillation times vary between 90
and 150 minutes. If the steam pressure is too low, it will be more difficult to remove the last of
the turpentine and there will be an inordinately long residence time for the hot rosin in the still;
both these factors have an adverse effect on the quality of the rosin.
The turpentine and steam vapours pass through an entrainment trap to remove any entrained
resin and then condense in a water-cooled condenser. Completion of distillation is indicated by a
minimal level of turpentine in the distillate. A small proportion of the turpentine coming over at
the beginning and end of the distillation may be collected separately as slightly lower-quality
turpentine, and used for diluting the next batch of resin at the melter.
The water-turpentine distillate is led immediately to a separating tank; the upper turpentine layer
overflows and passes first down to the base of the dehydrator and then upwards through a bed of
rock salt to remove all traces of water. The dry turpentine is then fed to holding tanks for
subsequent storage in bulk or in galvanized steel drums. The hot rosin from the body of the still
is discharged from the bottom into suitable containers which are set aside for the rosin to cool

and solidify. [19]
2.12. Standard quality and property determination of rosin product

The standard quality and property determination of rosin depend on the following factors:-
Table:-2.3 standard quality and property determination

No. Property Standard
1 Mechanical strength Brittle
2 Solubility(in organic solvent) Soluble
3 Color Yellow(yellow-brown) transparent

4 Odor Faint piny odor
5 Melting point 70-150 OC
2.13. Application area of rosin

Rosin are plays a great role in the following some application area include;
Table 2.4 Same application area of rosin

Application area Uses
In soap industry As raw material & for emulsifying
In paints & varnish industry For gelatin & stabilizer
In paper industry For paper sizing
In chewing gum Glazing agent
2.14. Grading of rosin

After the processing of resin, the grading should be done so as to check the quality. The grading
should be done on the basis of color and transparency. There are nine grade of rosin, which are
having their difference properties color and quality. The highly transparency shows the high
quality of the rosin. The low transparency shows that this form of rosin is low grade. Those are
showing in the following figure:

Figure:-2.2 grading of rosin types
2.15. Uses of Rosin

Rosin is a versatile material and plays an important part in a number of industries. Its main
outlet is in the paint and varnish, the paper and the soap industries. Appreciable quantities are
also used in adhesives and cements, plastics, linoleum, printing inks, rubber, asphalt emulsions,
belt dressings and sealing waxes. [18]
1. Rosin in varnishes and paints

Rosin probably enters more different types of finishes and compositions than any other raw
material. Rosin retards gelation of wood oil and when properly cooked, varnishes having
satisfactory durability and water-resistance are obtained. Varnish produced with softer oil like
linseed oil are not so satisfactory, the films are soft, easily affected by water and have poor
durability.
The solubility of fossil resins is improved by the addition of rosin; substantial quantities of rosin
are used in conjunction with Manila and Pontianak resins in spirit varnishes. Rosin exerts
excellent solvent power on gelled oils and is used as a peptizing agent for reclamation of wood
oil gels. It is also used as a stabilizer for varnishes of poor stability and as a flux in solubilizing
difficulty soluble resins.
Large quantities of limed rosin are employed for gloss oils which are often used as media for
quick-drying cheap paints. Zinc resinate and zinc-lime resinates in conjunction with drying oils
are well established as is the use of ester gums. Quite satisfactory varnishes are thereby obtained.

Appreciable quantities of ester gum are also used in cellulose lacquers. Substantial quantities of
rosin are also used in the production of cobalt, lead and manganese resinates which are used as
driers.
2. Use of Rosin in Soap
The sodium salt of rosin has excellent wetting and emulsifying properties and is an essential
component of all kinds of soaps, particularly laundry soaps in which it is incorporated in
appreciable proportions. Somewhat smaller quantities of sodium salt of rosin are incorporated in
toilet soaps.
3. Rosin in Paper Industry
Sodium soap of rosin is employed as a size for paper. Usually an aqueous solution of the soap is
employed although a dry rosin size is also available.
4. Other Uses of rosin
Rosin soaps are much more soluble in water than are the ordinary fatty acid soaps. Soaps with
fairly high rosin content, therefore, are particularly useful in liquid soap. Laundry soaps and soap
powders may be prepared from blends of fatty acids, rosin, and other components in minor
amounts. Rosin improves the sudsing, the detergency, and the wetting rate of the soap. Rosin
soaps also have germicidal activity. Soaps composed entirely of sodium or potassium resinate
find specialized uses.
Stabilized rosin soap, for example, serves as an emulsifying agent in the emulsion
polymerization of butadiene and styrene for the manufacture of synthetic rubber. In fact, this
type of rosin soap is used as the emulsifying agent in about one-third of all synthetic rubber now
being produced. Because of its good solubility in water, this soap is especially effective in the
low-temperature polymerization of butadiene and styrene. Rosin used for this soap should
contain less than 1% abietic -type acids and should be free of inhibitors which retard the rate of
polymerization.
Another advantage of using rosin soap in the emulsion-polymerization step in the preparation of
synthetic rubber is that the rosin serves' a dual purpose. The polymer is coagulated by the
addition of salt and acid, the acid decomposes the soap, and practically all of the rosin used
remains in the rubber to act as a softener. Rosin soap is used in the polymerization of synthetic
rubber. Rosin is used as a softening agent or plasticizer in both natural and synthetic rubber.
Rosin is used frequently as a bonding agent to strengthen the sand cores of molds in preparing
steel castings.

Other food-related uses of rosin esters include coatings on fruits, can linings and in flexible films
such as cellophane and paper. Rosin esters are also used in fragrances (perfumes) to retard rapid
evaporation and in cosmetics such as mascara, other eye make-up and depilatories
Figure:-2.3 Uses of rosin
 Current FAD regulatory status of rosin glycerol esters

Currently, glycerol ester of gum rosin has two approved uses in food, as direct additives in
chewing gum base and as an indirect food additive. Glycerol ester of wood rosin is also approved
for these two uses, and in addition, glycerol ester of wood rosin is approved for use as a direct
food additive as an agent in citrus-based beverages.
 Approval for Use in Chewing Gum
Both glycerol ester of gum rosin and wood rosin are approved as plasticizing agents in chewing
gum base. As stated previously, glycerol esters of gum or wood rosin are widely used in chewing
gums, and especially in bubble gum, whose gum base may contain up to 44 percent (by weight)
of rosin ester.
 Approval for Use as an Indirect Food Additive
Glycerol ester of gum rosin, purified by steam stripping to have an acid number of 3 to 9, a drop-
softening point of 79 to 88°C, and a color is approved for use as an indirect food additive. It may

safely be used in the manufacture of articles or components of articles intended for use in
producing, manufacturing, processing, preparing, treating, packaging, transporting or holding
food.
 Approval of Glycerol Ester of Wood Rosin as a Direct Food Additive
Glycerol ester of wood rosin has been approved by the FDA since 1963 as a food additive for
use as a direct agent to adjust the density of citrus oils used in the preparation of beverages. The
additive must also be purified by countercurrent steam distillation for use in foods.

CHAPTER THREE
3. METHODOLOGY
3.1. Equipments and Chemicals Used
 1000 ml beaker
 Mixer
 Vacuum filter
 Distillation column
 Heater
 Oil bath
 Oven
 Flask
 Measuring cylinder
 Analytical balance
 Water chiller
 Filter paper
 Gum resin
 Ethanol
3.2. Extraction of rosin

Method selection
Rosin is a product derived from pine trees and consists of a complex mixture of mutually soluble
organic compounds. Because, gum, tall oil and wood rosins are obtained from pine trees, they
are similar in composition. All rosins consist of free organic acids, called resin acids, as well as
non-acidic saponifiable and unsaponifiable substances (neutrals). Rosins are produced
commercially by one of the following three methods:
1. extraction of crude tall oil as a byproduct of the Kraft pulping process for making paper
followed by acidification and fractional distillation (tall oil rosin)
2. Solvent extraction of aged and ground pine stumps (wood rosin) and,

3. Tapping the living tree to collect crude resin followed by distillation to yield turpentine
and a resinous substance (gum rosin)
Due to the reality of pine tree found in our country and availability of the raw material found we
select the tapping the living tree to collect oleoresin followed by distillation to yield turpentine
and gum rosin.
3.3. Raw material collection

The raw material (pine resin) will be collected from pine tree where it found (collected from
Harar beer and Hararge area). The pine gum will be collected into small beaker or plastic in safe
way in order to keep the purity of resin gum.
Figure:-3.1 Collecting of raw material
Figure: - 3.2 Raw Gum Resin

Extracted Gum Resin Mixing Mixture Filtration waste

Ethanol
Pure mixture
First
Ethanol
distillation
@ 80 OC
Oleoresin
Second
distillation
@ 160 OC
Turpentine
Rosin
Figure:-3.3 Block flow diagram of rosin production

Process description
1. Mixing process: - mixing the two raw material ethanol and gum resin is conduct to form
uniform mixture. Some insoluble matters i.e. forest debris such as bark, pine needles and
insects are found suspended in the solution. The uniform solution is obtain because of gum
resin is soluble in organic solvents like ethanol. At his stage ethanol is used to extract soluble
matter in the gum resin from insoluble matters.

Figure 3.4 Mixing process of gum resin & ethanol

2. Filtration processes: - At this stage the mixture of ethanol and resin, pure filtrate will
obtain. The insoluble matters i.e. forest debris such as bark, pine needles and insects, which may
has fall into the cup during resin collection are form as a cake. Waste and insoluble
material are removed.
Figure 3.5 Filtration process of resin

4. Distillation process 1: - Taking the clean mixture into distillation to separate ethanol
from oleoresin. Ethanol is formed at the top product and oleoresin is at the bottom
product. This is because of ethanol is more volatile than oleoresin.
Figure 3.6 Distillation processes of oleoresin & ethanol

5. Distillation process 2:- At this stage the oleoresin processed into second distillation to
separate turpentine from the rosin. Turpentine is formed in the top product and rosin was
at the bottom product.
Figure 3.7 Distillation process of turpentine and rosin

Lab procedure for production of rosin
Step 1:- Preparing raw materials. Those are ethanol and pine resin (resin gum).
Step 2:- Adjusting all equipments those are needed for our process.
Step 3:- mixing: - Adjusting the mixer in constant speed (at 250 rpm).measuring appropriate
raw material in weight. Take sample of pine resin and ethanol and add the two raw materials in
beaker to form mixture and put the beaker under the mixer. The mixture is stay for 30 -60 min to
form uniform mixture.
Step 4:- Filtration: - The mixture will take in to vacuum filtration or using filter paper. Then the
insoluble matter is separated from the mixture.
Step 5:- Distillation 1:- Taking the clean mixture in to distillation to separate ethanol and
oleoresin at temperature = 80 0C.
Step 6: - Distillation 2:- Taking the oleoresin in to distillation to separate turpentine from rosin
at temperature = 160 0c.
Step 7: - Taking the final product rosin into oven to solidify it.

CHAPTER FOUR
4. RESULT AND DISCUSSION
The raw material oleoresin which was obtained from pine tree was processed in the laboratory
to produce rosin by passing through the processes of mixing (resin and ethanol), filtration and
two consecutive distillation, the former for the separation of ethanol and oleoresin and the later
for the separation of turpentine and rosin. The processes and results obtained are described as
follows:-
• The mixing process: - The mixing of ethanol 625 ml and resin 222.22 gram was
conducted for 30 minutes, uniform mixture of ethanol and resin was obtained. Some
insoluble matters i.e., forest debris such as bark, pine needles and insects were found
suspended in the solution. The uniform solution was obtained because of gum resin is
soluble in organic solvents like ethanol, hexane and so on.
• Filtration processes: - after filtration of the mixture of ethanol and resin, pure filtrate
was obtained. The insoluble matters like forest debris such as bark, pine needles and
insects, which may have fallen into the cup during resin collection were formed as a
cake. The mass of insoluble (waste) material removed was 20.9g and that of the filtrate
was 694.47 gram.
• The first distillation process: - Ethanol was produced at the top product and resin was at
the bottom product. This is because of ethanol is more volatile than resin. The mass of
ethanol recovered was 443.75g and that of oleoresin was 250.72 gram
• The second distillation process: - Turpentine was obtained as the top product which has
a mass of 111.83gram. The bottom product of 138.89gram was rosin.
• The product obtained, rosin was brittle, yellow-brown transparent and friable with a
faint piny odor. It was a glassy solid material which meets the properties of
conventional rosin.
Experiment one
We performed the separation by distillation, by taking simple distillation within time operation.
This simple distillation has taken long time to us to separate turpentine from rosin, because of
this simple distillation has less steam temperature. During this work we used oil bath and it takes
long time to separate turpentine from rosin. This is also due to the increasing separation of time.
From this experiment we concluded that, the large increment of time affected the product quality.
At this stage the color obtained was red-brown color which has less quality (low grade rosin).

Figure 4.1 Rosin from experiment one
Experiment 2
From the error of experiment one we changed the time wastage and its effect on our product, by
generating the more steam of oil bath in order to facilitate the rate of separation time of
turpentine and rosin. Therefore, the increment of steam formed the separation faster than the first
experiment.
Depending on the experiment two we can characterize our product rosin as follows: the best
quality determination properties of rosin are yellow-brown color, glassy solid, semi-transparent,
brittle, insoluble in water but soluble in organic solvent and low melting point. It is summarized
in the following table.
Figure 4.2 Rosin from experiment two

Table:-4.1 characteristics of rosin

Property Characteristics
Mechanical strength Brittle
Odor Faint piny odor
Color Yellow-brown transparent
Solubility in water Insoluble
Solubility in organic solvent like ethanol Soluble
Melting point 96 OC

CHAPTER FIVE
5. MATERIAL AND ENERGY BALANCE
5.1. MATERIAL BALANCE
Material balance is the basis of process design. It will determine the quantities of raw material
required and products produced, balance over individual process units set the process stream
flow and composition and tools for the study of plant operation.
 Operating with 24 hour and working day 300day/year
 Our Plant capacity is 1000 ton/year
 Open system and steady state
From the lab the ratio of pine resin to ethanol is 222.22gram to 625ml. Depending on this mass
of pine resin is 1600 ton /yrs.
About 625ml/hrs of solvent (98% ethanol) was used to mix the 222.22gram/hrs of Pine gum.
Since ethanol has a density (0.789g/ml) at T = 20oC. Then the volume of ethanol needed is
4500000ml/yrs to mix resin.
Mass of ethanol= density*volume
= 0.789g/mol*4500000l/yrs=3550500 kg/yrs
Mass of mixture =16000000+ 35505500= 5150500 kg/yrs
Mass balance on filtration
Filtration
Mixture=5150500 pure mixture (Pm)
Waste
Mass of waste (W) = 150963kg/yrs
Mass of pure mixture (P M ) = 51505000-150963
= 4999537 kg/yrs

Mass balance on first distillation
First
Pure mixture (Pm) Oleoresin (O)
distillation
Ethanol (E)
Mass of ethanol removed=3195450kg/yrs
Pure Mixture (P m ) =ethanol + oleoresin
Mass of Oleoresin =4999537kg/yrs - 3195450kg/yrs = 1804087 kg/yrs
Mass balance on second distillation
Oleoresin Second Turpentine

distillatio
n
Rosin
Mass of turpentine=mass of oleoresin-mass of rosin
=1804081 kg/yrs-1000008kg/yrs
=804079kg/yrs

5.2. Energy Balance

Energy balances are to determine the energy requirement of the process, the heating cooling and
power require in plant, operation an energy balance on the plant will show the pattern of energy
usage and suggest areas for conservation and saving.
Ein = Eout
Energy balance on first distillation
Ethanol (T E2 ,Cp E ,M E)
Mixture (M) (T E1 ,Cp E,M E ) First

M O , Cp O , T o , distillation Oleoresin (T o2 ,Cp o , M o )
M – Extract that contains extracted matter (oleoresin and solvent)
ME, and Mo ethanol and oleoresin; respectively
CPE, and Cpo – specific heat capacities of ethanol and oleoresin; respectively
TE1, and To1 – inlet temperatures of ethanol and oleoresin; respectively
TE2, and To2 – outlet temperatures of ethanol and oleoresin; respectively
Data required:
 Boiling point of ethanol = 78.5 0C Latent heat of vaporization (λe) of ethanol at 78.5 0C =
855kJ/kg
 Specific heat of ethanol (CPE) = 2.845kJ/kg
 Specific heat of oleoresin (CPo) = 12.5kJ/kg
 Inlet temperatures of extract (TW1, TE1, and To1) = 20 0C and
 Distillation process is controlled at temperature of 80 0C, so that the final temperature of

ethanol and oleoresin ( TE2=800C, and To2=800C; respectively)
From material balance on distillation:-

Mass of oleoresin=1804081 kg/yrs
Mass of ethanol=3195450 kg/yrs
Heat load calculation during first distillation
Heat living with ethanol
QE= ME+ +M e*Cp*∆Te
= 855 + 3550500kg/yrs∗ 0.00246 ∗ (80-20)
= 3036201554kj/ rs
Heat leaving with the oleoresin:
= ∗ ∗∆
=1804087 g/y ∗ 2.5 ∗ (80-20)
= 270613050 kj/ yrs
Total heat load during first distillation
QT = Qe + Qo = 270613050 kj/ yrs + 3036201554kj/ rs
= 4389266804 kj/yrs
Energy balance on second distillation
Turpentine (Tt=160,Mt=804081)
Second
Oleoresin (To,Mo) Rosin (Tr=160,Mr=1000000)
distillation
Data required
✓ Boiling point of ethanol = 78.5 0C
✓ Latent heat of vaporization (Xe) of ethanol at 78.5 0C = 855kJ/kg

✓ Specific heat of rosin (Cp r) = 4.2kJ/kg
✓ Specific heat of ethanol (CPE) = 2.845kJ/kg

✓ Specific heat of oleoresin (Cp o) = 12.5kJ/kg
Inlet temperatures of extract (TE1, and To1) = 20 0C and Distillation process is controlled at
temperature of 80 0C so that the final temperature of, ethanol and oleoresin ( TE2=800C, and
T o2=80°C; respectively)
Heat leave with turpentine (Qt)
= M t * Cp t * ∆T t =804081kg/yrs *4.2kj/kg*(160-25)
= 455917329 kj/yrs
Heat leave with oleoresin
= Mo*CPo*∆To
= 1804081 kg/yrs*2.5kj/kg (160-20)
= 270613050 kj/yrs
Heat leave with rosin(Qr) = 1000008*4.2*140
=58800470.4 kg/hr
So, Total heat load during distillation 2 is

QT = Q r + Q t -Q ol
= 455913927 Kj/yrs +58800470.4-270613050 kj/yrs
= 244101347.4 kj/yrs
5.3. Equipment Sizing

Sizing of filtration
The purpose of filtration in this paper is to remove all unwanted solid particle. Cleaning is
necessary to remove all extraneous material from the resin, both solid and soluble. This includes
forest debris such as bark, pine needles and insects, which may have fallen into the cup during
its period on the tree, and which require removal by filtration.
Assumption: filtrate at constant pressure and rate
Number of Filters
We can estimate the number of filters required using the following formula:
Number of filter = 2.7 √Q
Where:
Q = Flow rate

Q=1.2 MGD=0.0526m3/s
So, for filters with a flow of 1.2 MGD, then the approximate number of filters would be:
Number of filter = 2.7√1.2 = 2.95 ≈ 3
Flow
Next, the flow through one filter is calculated just as it was for one tank of the sedimentation
basin:
Qc = Q / n
Qc = (1.2 MGD) / 3 = 0.5 MGD = 0.0175 m3/s
Surface Area
The required filter surface area is calculated using the formula below:
A = Qc / F.R.
Where
A = filter surface area, ft2
QC = flow into one filter, gpm
F.R. = filtration rate, gal/min-ft
We will use a filtration rate of 0.271m/s.
A=0.0175/0.0646 =0.0646 m2
Tank Length
Since the filter tank is a square, the length of the tank can be calculated with the following
simple formula:
L= √A
L = Length, m
A = Surface area, m
L=√0.0645
=0.25 m
Sizing of First Distillation
The distillation column contains one feed stream and two product streams. The feed contains a mole
percent of the light component, ZF. The product stream exiting the top has a composition of XD of
the light component. The product stream leaving the bottom contains a composition of XB of the
heavy component. The column is broken in two sections. The top section is referred to as the
rectifying section. The bottom section is known as the stripping section. The top product stream
passes through a total condenser. This effectively condenses all of the vapor distillate to liquid. The
bottom product stream uses a partial reboiler. This allows for the input of energy into our column
and calculated by using analytical method.

Assume that
The feed will contain 80% w/w rosin
Rosin of at least 95% purity wanted
Effluent must no contain more than 50ppm
Molecular weight of rosin (C19H29COOH) =302, ethanol =46
Mole fraction of rosin in feed = 80/ 302 =0.378(XF)

80/ 302 +20/46
Top product = 50 ∗ 10−6 ∗46 /302
= 7.62 ∗ 10−6
Bottom product= 95/302 =0.115(XB)
95/302+5+46
Feed Stream, Rosin………………………………… = 0.93 /ℎ
Light-Key Mole Fraction………………………….. = 0.378
Percentage of Light in Distillate…………………… = 7.62 ∗ 10−6
Percentage of Light in Bottoms…………………... = 0.115
Quality of Feed
F ∗ XF = XD ∗ D + XB ∗ B………….... (1)
F = D + B…………………...................... (2)
To obtain the amount of distillate and bottoms:

0.94*.378=.9*D+.1*B
0.94=D+B
B = 0.34 /ℎ .
D= 3.9 /ℎ .
The minimum reflux ratio can be calculated through a variation of the Underwood equation.
When the quality is equal to one and in a binary mixture, equation reduces to:
= (1/( − 1)) ∗ (( / )− ∗ (1 − )/(1 − ))
Where: α=(yi/xi)/(yj+xj)=ki/kj, α=4.0
Rmin = (1/(4.0 − 1)) ∗ ((7.62 ∗ 10−6/0.378) − 4.0 ∗ 1.61)
= 0.78
The theoretical minimum reflux ratio is derived from equation,
ℎ = 1.2 ∗ :
=1.2*0.78= 0.936
From the Fenske equation we can determine the number of trays:
= / ( /(√1 + 1/ ∗ )/ 1)
= ∗ /(1 – )∗ (1 − ) = 81
Where,
− Fractional recovery of light in the distillate
− Fractional recovery of light in the bottom
Reflux ratio
Relative volatility and zF Mole ratio of light component in feed.
Then, Nmin = (81)/ (4.36/ (1 + 1/(0.81 ∗ 0.3))
=6
Determine Actual Number of Trays:
This is determined by taking the quotient of the number of theoretical trays to the tray efficiency.
Typical values for tray efficiency range from 0.5 to 0.7. These values depend on the type of trays
being used, as well as the internal liquid and vapor flow rates. Take efficiency 0.65
Nactual =N/e
= 6/0.65 = 9
The tower height can be related to the number of trays in the column
H = 2.3Nactual
= 2.3 * 9 =20.7ft
Height-to-diameter ratio should be less than 20 to 30. Let take 25
/ = 25 = 20.7 /D= 25 = =20.7/25 = 0.83

CHAPTER SIX
6. ECONOMIC ANALYSIS
6.1. PLANT CAPACITY AND PRODUCTION PROGRAMING
The plant has an installed capacity of producing 1000 ton of rosin from 1600ton of crude resin.
The factory will initially operate at 85% capacity in the first year and then continues producing at
its full capacity. The plant is planned to work for 300 days per annum and 24h per day. Assume
plant capacity and production programming is Capacity utilization 85% for first year, 100% for
second year and resin production rate 850 ton/yr for first year, 1000 ton/yr for second year

6.1.1. Project cost estimation

A. Purchased equipment cost
Table: - 6.1 Purchased equipment cost
NO. Equipment Quantity Unit Total

price(Birr) price(Birr
)
1 Dam vat 1 1000000 1000000
2 Blow case 1 100000 100000
3 Melter 1 300000 300000
4 Filter 1 140000 140000
5 Washing 2 250000 500000
Tank
6 Charge tank 1 420000 420000
7 Distillation 1 340000 340000
Tower
8 Condenser 1 40000 40000
9 Separator 1 50000 50000
10 Muck Tank 1 30000 30000
11 Pump 1 60000 60000
12 Dehydrator 1 200000 200000
13 Sump 1 25000 25000
14 Product Silo 1 300000 300000
15 Packaging 1 120000 120000
Machine
TOTAL 3425000
B. Total capital investment cost

Total capital investment is estimated based on delivered equipment cost of solid-fluid processing
plant; according to Peters & Timmerhaus (1991). The capital investment is calculated as a factor
of the ratios of equipment purchase cost.
 Purchased equipment cost = 3,425,000 Birr

 Assuming delivery cost = 10% of purchased equipment cost

 Purchased-Delivered equipment cost = 3,767,500 birr
Table: - 6.2 Total investment cost
Item Percentage (%)of PEC Price( birr)
Direct cost
Purchased & delivered 100% 3767500
equipment cost(PEC)
Purchased equipment 33% 1243275
installation
Instrumentation & control 9% 339075
Piping installation 16% 602800
Electrical installation 10% 376750
Buildings 25% 941875
Yard improvement 8% 301400
Services facility 40% 1507000
Land 6% 226050
TOTAL DIRECT COST (A) 9305725
Indirect cost
Engineering & super vision 26% 979550
Constriction expense 28% 1054900
TOTAL IN DIRECT COST(B) 2034450
Total direct & Indirect cost(A+B) 11340175
Contractors free cost=5%(A+B) 567008.75
Contingency/(D)=10%(A+B) 1134017.5
Fixed capital Investment(FCI)=A+B+C+D 13041201.25
Working capital(WC)=15%FCI 1556180.188
Total capital investment(TCI)=FCI+WC 14997381.44

C. Total product cost

1. Raw material cost
The major raw material used in the production of rosin is pine resin. The annual raw pine resin
required in full plant capacity utilization is 1600 tonnes per year to produce 1,000 tonnes of
rosin. Taking raw material cost is estimated about 5birr/Kg in Ethiopia. Therefore, the total raw
material cost is 8,000,000 birr
2. Auxiliary material cost
Cost auxiliary materials per year are 60,000 birr.
3. Cost of utilities
Electricity and water are the two utilities required by the plant. Table below shows annual
requirement of utilities at full production capacity.
Table: - 6.3 Annual requirements of utilities and cost
No. Description Quantity Unit cost Cost(birr)
1 Electricity(kwh) 66600 0.474 31568
2 Water(M3) 4500 10 45000
Total 76570

4. Man power requirement and labor cost

Table: - 6.4 Man power requirement
NO. Description Requirement Monthly(birr) Annual
no. salary(birr)
1 General 1 4500 54000
manager
2 Accountant 1 2200 26400
3 Sales person 1 1300 15600
4 Store man 1 1300 15600
5 Clerk 1 750 9000
6 Secretary 1 1200 14400
7 Quality 1 2200 26400
control expert
8 Chemist 1 2000 24000
9 Operator 10 900 108000
10 Mechanic 1 2000 24000
11 Electrician 1 2000 24000
12 Unskilled 8 700 67200
labor
13 Guard 4 800 38400
14 Driver 2 1000 24000
TOTAL 34 471000
Workers 117750
Benefit=25%
of basic salary
TOTAL 588750
5. Total production cost estimation

Table:-6.5 Total production cost

Components Percentages Cost(birr/yrs)
A. Direct
production cost
1.Raw material 8000000
cost
2.Auxialary 60000
material cost
3.Operating 588750
1.Manufacturing labor(OL)
cost 4.Direct super 10%OL 58875
vision
5.Utilities 76570
6.Maintence and 3%FCI 391236.04
repair
7.Labratoy 10%OL 588750
charges
TOTAL DIRECT PRODUCTION 9764181.04
COST
B. Fixed charges
1.Depreciation 10%FCI 1304120.125
2.Capital charge 1%FCI 130412.0125
3.Insurance 0.5%FCI 65206.01
Total fixed charge 1499738.15
C. Plant over 50%OL 294375
head
Total manufacturing cost(A+B+C) 11558294.19
1.Administrative 3%TPC 385276.5
2. General cost
expenses 2. Distribution 4%TPC 513701.96
and selling cost
3. R & D 3%TPC 385276.5
Total production cost(TPC)=Manufacturing cost + 16743519.8
General expenses

Total production cost=manufacturing cost + General expense
TPC=1155829.19 + 10%TPC
TPC=12842549.1 Birr
6.2. Financial evaluation and project appraisal
6.2.1 Financial analysis
A. Unit product cost determination
Unit product cost=TPC/annual production
Annual production =138.89*24*300* 1000tonn=1000008 kg/yrs
12842549.1
= 1000008
=12.84birr/kg
Selling price of rosin =unit product cost+80% profit margin
=12.84(1+0.8) = 23.112 birr/kg
B. Project profit and loss

Total annual revenue = selling prices * annual production
= 23.112 * 1000008 =23112184.89 birr
Total annual product cost = 12842549.1 birr
 Profit before tax=total revenue-total production cost
 Business tax=30% of profit before tax
 Net profit after tax=profit before tax-business tax

Table: - 6.6 project profit and loss
Description Year 1 Year 2 Average

85% 100%
Total 19645,200 23112000 21378600
revenue
Total 10916166.74 12842549.1 11879357.92
product cost
Profit before 8729033.3 10269450.9 9499242.1
tax
Business tax 2618709.99 3080835.27 2849772.63
(30%)
NPA Tax 6110323.31 7188615.63 6649469.47
6.2.2. Project appraisal

A. The Return on Total Capital Invested (ROI)
Annual net profit
RIO = Total capital requirement
*100%
6649469.47
= 14997381.44
*100%
= 44.34%
B. Pay-back period analysis
Payback period =Initial Investment/Annual net profit (average)

14997381.44
= 6649469.4
=2.25 years

CHAPTER SEVEN
7. ENVIMENTAL EMPACT
For potential human health effects, the totality of the SIDS data demonstrates that rosin is non-
toxic. Accordingly, based on the category approach, it can be inferred that all of the substances
in this group are also non-toxic.
Rosin has no acute oral toxicity (i.e., LD50 > 5,000 mg/kg), and repeat dose toxicity data
demonstrate a no observed effect level (NOEL) of approximately 105 - 200 mg/kg/day and a
NOEL of approximately 275 mg/kg/day for reproductive/developmental effects. The lack of
acute oral toxicity (i.e., LD50 > 5,000 mg/kg) for rosin, hydrogenated, is confirmatory of the
lack of acute toxicity of the substances in this category. The lack of carcinogenic effects in two-
year feeding studies for rosin and rosin, hydrogenated suggests that neither substance is
genotoxic. [9]
Consequently, no adverse health consequences would be associated with any exposures to any
of the rosins or rosin salts. For potential eco-toxicological effects, the data on rosin demonstrate
that all of the substances in this category are non-toxic to aquatic organisms with the NOELr for
fish and algae.
With respect to potential exposure to the substances in this category, a ll are consumed almost
entirely in the production of other chemical intermediates. Rosin is reacted in a variety of ways
to form salts, adducts, esters, dimers and other reaction products which find application in the
production of printing inks, adhesives (primarily hot melt packaging adhesives), paper size, and
coatings. These uses would be considered non-dispersive in that the rosin derived chemical is
reacted or otherwise contained within the article in which it is being used.
It is estimated that greater than 80% of the various rosin derivatives are used in the type of
applications described above. As such inhalation exposure or volatization to air is minimal due
to a lack of vapor pressure for these substances. Exposure in the listed applications is generally
limited to dermal contact during the processing, finishing and shipping of the products of which
they become a part. Approximately 3% of rosin is reacted to form specific rosin esters which are
marketed to the chewing gum industry. [9]

CHAPTER EIGHT
8. SITE SELLECTION
Site selection means to discover place where an industrial experience can be started more
profitable & a plant is a place where men power, material, money, equipment, machinery etc. are
brought together for manufacturing products. Site selection plays a major role in the design or
production as it determines the cost of
 Getting suitable raw material.

 Processing raw material to finished products.
 Finished products distribution to customers.
The final site selection of the plant location has a strong influence on the success of any
industrial venture. So, we considering the following reason and possible any where the area of
this is available:-
 Availability of raw materials
 Large market
 Very nice attitude of the local people
 Good transportation facility like, road
 Availability of adequate supply of labor force
 High proportion of skilled employees
 Good communication facility
 Rapid contact with customers and supply
 Low land cost, waste disposal and pollution
In general we can select the location area of this plant is around Harar area, since the
availability of raw material and other necessities for this plant are available.

CHAPTER NINE
9. CONCLUSION AND RECOMMENDATION
9.1. Conclusion
The study was conducted with the objective of producing rosin from resins of pine tree. The pine
resin of 222.23g was processed and Rosin of 138.89g was obtained after the raw material was
passed through the stages of mixing, filtration and two consecutive distillations. The essential oil
called turpentine was obtained as a byproduct. The rosin obtained was brittle, transparent, glassy
solid. It is insoluble in water but soluble in organic solvent such as hexane, ethanol. Finally we
conclude that rosin processing is profitable due to the law cost of the gum resin in our country.
So the project is feasible, by checking the techno economic estimation with pay back 2.25 years
and rate of return with 44.34%.

9.2. Recommendation
 The raw material tapping mechanism should be employed appropriately and handled
safely with the time needed it reaches the plant. The quality of rosin, turpentine oil and
other products manufactured from it will also be much better and fetch higher prices.
 Turpentine cannot be separated from pine gum by simple distillation because of its low
volatility, unless excessive heat or heating time was used. Our experiment demonstrated
the separation of pine gum into turpentine and rosin by means of co distillation with
steam at temperature above 100Oc.
 The country is collecting and exporting only the crude gum resources and again import
with foreign currencies their final products from developed countries. Therefore devising
mechanisms to promote the country potential for value addition and industrialization of
gum resin products should be one of the priority collaboration lines in the near future.
 Resin gum is widely found from different areas in our country. So, if any entrepreneur
who is interested to invest in the production of rosin will become profitable. Since the
present demand of this product is increased day to day and create job opportunities.

CHAPTER TEN
References
1. Adefires W., Mulugeta L., Masresha F. & Demel T., 2011, socio-economic importance
of gum and resin resources in the dry woodlands of borana, southern Ethiopia, Forests,
Trees and Livelihoods, Taylor & Francis
2. Antonio Rumero Luresa, OCTOBRE 2012, "la colophane et son avenir dans le domaine
du sudoe" bordeaux (France)
3. Amelia P. and Anamaria A. (2012).Pine resin sector in Portugal-weakness and
challenges volume 18.
4. Coppen, J.J.W 12 Devon Close, Rainham Kent ME8 7LG, U.K., Overview of
International Trade and Markets
5. Coulson and Richardson (2003). Chemical Engineering Design, Butterworth-
Heinemann,
6. Coulson and Richardson (1993).Chemical Engineering Design, Butterworth-Heinemann,
volume 2.
7. Chretien Donker, The Chemistry of Tackifying Resins
8. Douglas J. (1988) Conceptual design of chemical process. McGraw-Hill Inc.
9. Generally Recognized As Safe (GRAS) notification for glycerol ester of gum rosin, by
Environ International Corporation Arlington, VA June 24, 2002
10. Ibrahim Jantan and Abu Said Ahmad, Oleoresins of Three Pinus Species from
Malaysian Pine Plantations
11. J.J.W. Coppen and G.A. Hone, 1995, Gum naval stores: turpentine and rosin from pine
resin, Natural Resources Institute, Food and Agriculture Organization of the United
Nations
12. Lemenih, M. and Kassa, H. (2011). Opportunities and challenges for sustainable
production and marketing of gums and resins in Ethiopia. CIFOR, Bogor, Indonesia
13. Max S. Peter D.Timmerhaus (1991). Plant design and Economics for chemical
engineering: McGraw-Hill
14. Max S. Peters, Klaus D. Timmerhaus, The plant design and economic for chemical
engineering
15. McCabe W. (1993).Unit operation of Chemical Engineering, fifth edition. McGraw-
Hill, Inc.
16. Mulugeta L. and Habtemariam K., February 2011, Gums and resins of Ethiopia, No. 3,
17. Ray V. Lawrence, The industrial utilization of rosin

18. Williams, Don-Gidvanil, Natural_Resin part 2

19. W. Tadesse, G. Dessalegn and R. Alia (2007).Natural gum and resin bearing species of
Ethiopia Institute of Agriculture Research. Forestry Research center

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CHEMICAL ENGINEERING DEPARTMENT GC 2008 EC

DEPARTMENT OF CHEMICAL ENGINEERING

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 1

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 2

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 3

LIST OF FIGURE page

Figure 2.1 Process flow diagram of rosin production ............................................................................. 20

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 4

LIST OF TABLE Page

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 5

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 6

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 7

1.2. Statement of problem

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 8

 Separation of oleoresin and ethanol at 80 Co

 Separation of rosin and turpentine from oleoresin at 160 Co.

 Characterization of physical and chemical properties of rosin.

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 9

1.4. Significance of study

 It may generate foreign exchange through exports.

 Scarcity of lab equipment’s in our laboratory.

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 10

2.1. Source of Rosin

2.2. Chewing Gum

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 11

2.3. World Rosin Production

2.4. Production possibility in Ethiopia

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 12

National Regional Genus Estimated area (ha)

Year Total production Export quantity

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 13

2.5. Raw Material Collections techniques

 Preparation of the face of the tree

2.6. System of tapping

2.6.1. System of using wide face

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 14

2.6.2. System of using narrow face

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 15

 Bark shaving tool, Cup or other form of receiver

 Hammer, Bark hack

 File or whetting stone (for sharpening bark hack)

 Sulphuric acid-based stimulant (liquid or paste)

 Bottle (plastic, for application of acid)

 Bucket (into which resin from cup is emptied)

 Funnel (for transfer of resin from bucket to drum) , Drum or barrel

2.7. Properties of Rosin

B Melting and Flammability

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 16

2.8. Chemistry of Rosin

2.9 Chemical Modifications of Rosin

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 17

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 18

2.10. Production process

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 19

2.11. Olustee process for the production of turpentine and rosin

Figure: -2.1 Process flow diagram of rosin production

FINAL PROJECT ON ROSIN PRODUCTION FROM PINE TREE Page 20