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INTRODUCTION
1.1 General
Camphor is a waxy, white or transparent solid with a strong, aromatic odour having the chemical formulaC10H16O. It is found in wood and of the of camphor laurel (Cinnamomumcamphora), a giant of a large evergreen tree found in Asia (particularly in Borneo and Taiwan) also Dryobalanopsaromatica, the Bornean forests. It also occurs in some other related trees in the laurel family, notably Ocoteausambarensis. Dried rosemary leaves (Rosmarinusofficinalis), in the mint family, contain up to 20% camphor. It can also be synthetically produced from oil of turpentine. It is used for its scent, as an ingredient in cooking (mainly in India), as an embalming fluid, for medicinal purposes, and in religious ceremonies. A major source of camphor in Asia is camphor basil. The word camphor derives from the French word camphre, itself from MedievalLatincamfora, from Arabickafur, from Sanskrit, karpuura. Barus was the name of an early port on a city named "Sibolga" (located in the western coast of Sumatra island - North Sumatra Province, Republic of Indonesia]. At that time, this city was initially built prior to the Indian Bataknese trade of camphor and spices. Foreign traders such as; Dravidian - Indian, East Asian and Middle east traders would call "kapurbarus" to buy the extract/dried ooze of camphor tree from the local tribesman (Bataknese), in [Bataknese language "Gorga" It is also known as kapur Barus. Until now, the local tribesman and Indonesian in general refer to naphthalene balls
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and moth balls as kapur Barus. For the local tribesman the use of camphor are ranging from deodorant, wood - cloth finishing veneer coat, traditional ritual and non-edible preservatives as the camphor tree itself natively found on that region. The tree itself in Indonesian language called as "Kamfer" also known for it's resistance. Camphor is readily absorbed through the skin and produces a feeling of cooling similar to that of menthol and act as local anesthetic, however it is poisonous when ingested and can cause seizures, mental confusion, irritability and neuromuscular hyperactivity.
manufacture
"Eucalyptus
chemical
variants
chemotypes) seem dependent upon the country of origin of the tree. The tree is native to China, Japan, and Taiwan. It has been introduced to the other countries where it has been found, and the chemical variants are identifiable by country. i.e., Cinnamomumcamphora grown in Taiwan and Japan, (often commonly called "Ho Wood") is normally very high in Linalool, often between 80 and 85%. In India and Sri Lanka the high camphor variety/chemotype remains dominant. The Cinnamomumcamphora grown in Madagascar, on the other hand, is high in 1,8 Cineole
(averaging
between
40
and
50%.
The
essential
oil
from
the
dihydromyrcenol, applications
other
industries
ranging
flavours&fragrances, pharmaceuticals, soaps & cosmetics, rubber &tyre, paints & varnishes and many more. It is a pioneer in the field of terpene chemistry in India since 1964, having established the first synthetic camphor plant with technology from DuPont of USA. The plant of the company is located finished at Bareilly products in West Uttar and Pradesh, 250 km the from New Delhi. It handles a volume of 20,000 tons of raw materials and annually incorporates latest technology and equipment. The operations company such carries as out all conceivable chemical oxidation,
fractionation,
esterification,
saponification,
hydrogenation,
dehydrogenation,
peroxidation, pyrolysis, etc. in the plant using equipment and technology that is constantly updated with time to keep pace with the latest advancements in chemistry and chemical engineering practices. Its grades), resins vast and product many range pine includes oils, processes
3
synthetic are
camphor by
(all well-
terpineols,
Isobornyl
acetate,
terpene
more. All
monitored
trained
technical
personnel
with
the
help
of
latest
instrumentation and quality control. The company is also having a state-of-the-art manufacturing facility that was set value up at Nandesari, Baroda in 1999, to manufacture high fragrance chemicals and fragrance
chemical intermediates based on in-house technology. Products manufactured at this plant are of international standard and are well accepted in markets abroad and at home. 1.3.1 Product Range 1.3.1.1 Fragrance Chemicals 1. Amberone It is a pale yellow viscous liquid & amber odour. 2.Astromeran It is colourless to pale yellow colour&woody, spicy, floral odour. 3.Astrone It is clear liquid colourless to pale yellow, woody, balsamic, floral, pine odour. 4.Astrolide It is colourless liquid. Clean, powerful, long lasting musk odour (Galaxolide equivalent). 5. Capinone It is colourless woody odour. to pale yellow liquid, rich, sweet and
6.Dihydroterpineol It has piney, woody odour. 7.Dihydroterpinyl Acetate It is citrus fresh & has pine needle odour. 8. Fenchone It is a pale yellow liquid.Strongcamphoraceousodour. 9.Isoborneol It is white crystalline powder.Pineycamphoraceousodour. 10. Isobornyl Acetate It is colourlessliquid.Pine needle camphoraceousodour. 11.Ketone 101 It is pale yellow liquid. Sweet, earthy, woody and slightly camphoraceousodour patchouli oil. 12.Terpineol It is pale yellow to colourlessliquid.Sweet, piney, pleasant, lilac character. 13.Terpinyl Acetate It is colourless liquid - fresh bergamot Lavender odour. 14.Citwanene It is having pleasant citrus 15.Isolongifolene Colourless to pale yellow liquid.Characteristicodour.
5
with
tobacco
suggestion,
reminiscent
of
16.Longifolene It is colourless to pale yellow liquid. Characteristic terpenic odour. 1.3.1.2 Pharmaceutical Products 1.Camphor EP/USP/BP/DAB/JP It is a white granular powder& it isanti-infective and antipruritic 2.Cerpineolbp It is colourless liquid and has sweet, pleasant, lilac odour, used as anticeptic. 1.3.1.3 Industrial Chemicals 1.AlphaPinene Epoxide It is clear colourlessliquid. 2.AlphaCampholenic Aldehyde It is light pale yellow clear liquid sweet, woody odour. 3.Camphene It is starting material for sandalwood type aroma chemicals. 4.Camphor It is white crystalline material. Characteristic penetrating odour. 5.Camphor oil It has colourless to pale yellowcolour&Camphoraceous 6.Capolene
6
odour.
It is colourless to pale yellow liquid 7.Capolyte CP Resin It is a tackifyingagents. 8.Distilled turpentine It is pale yellow liquid & used as solvent in paint and lacquer industry. 9.Dipentene It is a colourless to pale yellow liquid. 10.Para cymene It is a polymerisation initiator for synthetic rubber 11.Pinenehydroperoxide It is a polymerisation initiator for synthetic rubber 12.Pine tars It is a dark brown viscous liquid, Tackifier. 13.Pine oils It is colourless to pale yellow liquid & have Sweet, pleasant, piney, floral odour. 14.Sodium acetate trihydrate It is a colourless or white crystalline powder. 15.Phenol It is orange coloured liquid.
1.4 Objective
The main objective of the project is to gain knowledge about the manufacturing process of camphor using turpentine oil and to know about the camphor. industrial and pharmaceutical uses of
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in equilibrium with the residual liquid, separating the vapour from liquid and condensing the liquid 2.1.2.2 Steam Distillation Steam distillation generally treated as a simple
evaporation without fractionation and is generally handled as a batch operation. It may be illustrated by the fractionation of crude oil, where the last trace of lighter constituents in the still bottoms are separated by the introduction of steam in the column and all side streams are drawn off the column are stripped with steam to remove same amount of volatile constituents could without the restoring oil. The to high temperature, the which to decompose steam allows column
operate at atmospheric pressure, while at same time gives the effect of a partial vacuum distillation of crude. 2.1.2.3 Vacuum Distillation In vacuum distillation feed is charged into the colum
which is under atmospheric pressure i.e. vacuum, this results in separation into different constituents of the feed. Vacuum distillation is used to separate components of high boiling points, fraction which above could 600 for not degree their be boiled readily are available to heat source or which are unstable at their atm boiling point. Thus celcius subjected because vacuum this distillation separation above
temperature, decomposition and coking occurs in the furnance tubes in which oil is reboiled. Thus it results in loss of valuable plugging. product and destruction of furnance tubes by
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11
2.1.3.
Turpentine
turpentine, and
distillation of resin obtained from live trees, mainly pines. It is composed of terpenes, mainly the monoterpenes alpha-pinene and beta-pinene. It is sometimes colloquially known as turps. 2.1.4. Alpha Pinene -Pinene is an organic compound of the terpene class, one of two isomers of pinene. It is an alkenes and it contains a reactive four-membered ring. It is found in the oils of many species of many coniferous trees, notably the pine. It is also found in the essential oil of rosemary. Both enantiomers are known in nature. The racemic mixture is present in some oils such as eucalyptus oil. 2.1.5. Beta Pinene Beta-Pinene (-pinene) is a colorless liquid, soluble in
alcohol, but not water. It has a woody-green pine-like smell. It occurs naturally in rosemary, parsley, dill, basil, yarrow, and rose. It is also a major constituent of hop aroma and flavor. 2.1.6 Camphene Camphene is bicyclic monoterpene. It is nearly insoluble in water, It is but a very soluble in of It the common many is organic essential produced more solvents. oils such It as by volatilizes readily at room temperature and has a pungent smell. minor and constituent valerian. of turpentine, cypress oil, camphor oil, citronella oil, neroli, ginger oil, industrially catalytic isomerization common alpha-pinene.
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additive for flavoring. Its mid-19th century use as a fuel for lamps was limited by its explosiveness.
ofinsectisides , flysprays,
In medicine it is used as expectorant for cough. In veterinary it is used as expectorant in chronic bronchitis. 2.2.6.Pinetar Orefloatation, tarsoaps preservatives.It roofing is also compositions, general used in paints, of varnishes, rubber and
,asphaltic
compositions,
preservatives,marine
manufacture
rubber gooda as a tackyfyingagent. It is used in manufacture of cordage,insulation varnishes,and quenching oil. 2.2.7.Pine oil Pine oil is an excellent resin solvent,finds use in paints and varnishes.It is used in textile industry as a penitrant, dispersant,detergent, and as bacterial inhibitor in wet processing cotton,silk and rayon. 2.2.8.Caprez resin Caprez resin is an adhesive.It is widely used as a medicinal tape in medicinal industries.Also used in bubble gum industry, 2.2.9.Menthol Used in perfumes, as a flavour in toothpastes, mouthwash, chewinggums, syrups. incosmetics for cooling sensations and in pharmaceutical industries as pain balms,rubs,ointments,and cough
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15
C10H16O 152.23 g mol1 152.120115134 g mol1AppearanceWhite, translucent crystals 0.990 g cm3 175-177 C, 448-450 K, 347-351 F
2. Molar mass
6. Boiling point
7.Physical Appearance
8.Solubility in water 9.Solubility in acetone~ 10.Solubility in acetic acid~
1.2gdm-3 2500 g dm3 2000 g dm 2000gdm-3 1000 g dm3 1000 g dm3 4 mmHg (at 70 C) []D+44.1
11.Solubility in diethyl ether~ 12.Solubility in chloroform~ 13.Solubility in ethanol~log P 14.Vapor pressure 15.Chiral rotation
Source- www.wikipedia.org
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production, and additional steps are taken when large quantities of synthetic camphor are required. 3.2.2 Large scale production For large scale production, synthetic Camphor is produced from -pinene oil which is a main ingredient of turpentine oil. The production of synthetic camphor begin with the distillation of turpentine to yield -pinene. The -pinene is carefully dried and treated dry hydrochloric acid to produce bornyl chloride, also known as Synthetic Camphor.
17
18
The patented
resultant
solid
is
then
converted by
by
several the
chemical
process
into
camphene
removing
hydrochloric acid with phenol, cresol, aniline and alkali. For large scale production of synthetic camphor, the glacial acetic acid. The isobornyl acetate is subsequently separated and treated with alcoholic sodium hydroxide to produce isoborneol. After isoborneol has been purified, it is oxidized by nitric acid and sulphuric acid to finally producing synthetic Camphor.
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85-90% Alpha Pinene 8-10% Carene Turpentine Oil 3-5% Beta Pinene 1-2% Camphene
2.
Alpha
Pinene
oil
obtained
by
fractional
distillation
of
turpentine oil undergo isomerisation reaction in the presence of Titanium dioxide to produce crude camphene tricycle camphene. Isomerisation Alpha Pinene TiO2 Catalyst 3. Crude Tricyclo Camphene is then sent to distillation unit where it undergo fractional distillation to produce Pure camphene along with side products. Fractional distillation Cr camphene Depentene 4. Pure Camphene of is then treated to with acetic acid in the to Pure Camphene + TarpeneD + Cr Tricyclo Camphene
presence
CXC-120
Catalyst
undergo
Esterification
20
21
Esterification Pure camphene IBA + (Acetic Acid + Unreacted Camphene) 5. IBA is further distilled to produce pure IBA.
IBA
6.The next step in camphor manufacture is saponification.Itis done to obtain total conversion. For total conversion the ratio of IBA:NAOH should be 1:0.22 . The reaction is as follows (160-170 C) C10H17COOCH3 +NaOH C10H18O +CH3COONa 7-8 KG/cm2 The product formed is known as isoborneol.After the isoborneol is purified, it is oxidised in presence of nitric acid and sulphuric acid into the final synthetic camphor.
vapours, tank, as
turpentine is much lighter than water. This turpentine is then distilled into "heads" (volatile compounds with no commercial value), and - and -pinene. Of these, -pinene is sold as is and -pinene is further processed to make pine oil by reacting it with phosphoric acid. Pine oil is used as a solvent, disinfectant and deodorant, and -pinene is used to produce camphor and insecticides. A further, less valuable, solvent, dipentene, is produced as a by-product of this process.
smelling sulphurous compounds(e.g. methyl mercaptan and dimethyl sulphide) inorganics associated handling refined turpentine, both because of its volatility and because it has a low flash point. 3.6.1 Operations in camphor manufacture Basically camphor manufacture takes place in three steps. 1.Saponification 2.Washing 3.Dewatering These processes are explained in details now.
23
The processes used in each of the steps include: 1.Charging raw materials For the manufacture of camphor the raw material turpentine oil is charged first.the objective of this is to yield pinene.After that pinene is carefully dried. 1.Reactions 2.Cooling 3.Transfer and flushing 2.Dehydrogenation Dehydrogenation is the process of removal of bulk hydrogen from the raw material. The isoborneol formed is dehydrogenated at a temperature of 220-225 c to form camphor with the elimination of H2.The process include charging the catalyst and then cooling and subsequently filtering it.Inert gas is also purged into it. 3. Camphor refining & distillation Camphor refining takes place in 4 steps.These are as follows: 1.Stripping of hydreogenated benzene. 2.Removal of camphor oil. 3.Distillation of camphor from camphor +hbs mixture. 4.Reclaimingof the camphor from, residue.
4. Camphor reclaiming Camphor reclaiming is a process to obtain the maximum amount of camphor and to minimize the waste. This process is done in following way:
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the
1.Evaporation of camphor through steam distillation. 2.Condensation of water + camphor vapours in benzene. 3.Cooling of water + benzene camphor solution. 4. Removal of water. 5.Draining of pitch. 5.Nutschefilter. IB From R-904a is taken in this filter and it is washed with benzene, vanes of this filter requires the solution and make benzene ( with impurities of IBA ) pass through the filter and get collected. Filter allow the benzene to pass thorough benzene vanes. 5.Isomerisation C10H16 reaction( batch process) C10H16 + Mixed tarpene
The mixed tarpene is a mixture of dipentane and pentane. Camphor is separated from dipentene and pentene D by fractional distillation.
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4.1 Specification
A process design starts with the development of a process flow sheet for the development of such process flow diagram material balance calculation across each unit is necessary. There material balance follow the law of conservation of mass. According to law of conservation of mass, the total mass of a system whether it undergo unit process or unit operation remain unchanged, it can neither be created nor destroyed. When we deal the material balance, reach and they on pertain and to physical with and chemical reaction or or process and which are often referred to as material balance without chemical that chemical involve respectively. separating Physical process chemical mostly process involve mixing process
process
reaction occurring in the reactor. Now the question comes, why do we need material balance. Although we usually have the idea of the overall process, we immediately face the question of how much product can be produced from the available raw materials or how much the certain raw material need to be processed to meet a particular demand. Thus we are referring to flow of the raw materials and of product or waste materials out of process. A material balance is a careful accounting of this materials flow and is the first and essential step in the analysis of chemical process. It is here that one begin to get a feeling for overall size of the process since one is now dealing with the masses or volumes of material involved. Such considerations are of extremely important because the flow of material involved, to determine size and cost of reactor & number of unit etc.
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balance is
are of
basis the
of
process required
design. and
balance
taken
complete
process
will the
quantities
material
product produced. Balance over individual process unit set the process steam flow and composition. Material balance are also useful for study of plant operation and trouble shooting, it can be used to check performance against design, to check instrument celebration and to locate source of material loss. Assumption made during material balance 1. No material loss is considered 2. No material is accounted for heating the process material that will be calculated in energy balance. 3. Final product is considered as hundred percent pure as per specification 4.2 calculation
Material
Formula
Density
Mol.wt
1. Camphor production initial raw material Raw material are added in following proportion in
manufacturing of Camphor
Material
Weight(in ton)
1 3.493 .053 .5 .1
Since the amount of additive are very small(in kg) hence we neglected 2. Amount it in material balance calculation. of -pinene oil formed from turpentine oil(since
conversion is 90%)
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3 Alpha pinene oil obtained from fractional distillation is kept in a batch reactor for about 2 hour and small amount of titanium dioxide is added as catalyst, this led to isomerization of alpha pinene to crude camphene with no loss of reactant.
TiO2
Alpha pinene(.9ton)
Crude Camphene
4. Pure Camphene Production Yeild of different product from crude camphene are as follows Pure Camphene Dipentine Pine oil 55% 10% 30%
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Other residue
5%
Pure camphene(55%)+
Residue(terpine& hydrate)
Since the yield of pure camphene is 55%, so amount of pure camphene produced = .55*0.9 =.495 tons 5. Isoberneol acetate formation tank Percentage yield of IBA is 70% Acetic acid taken= .33 ton Isoberneol acetate formed = .433 ton Reacted acetic acid = .231 ton Unreacted acetic acid = .33-.231 =.099 ton Unreacted camphene = .1485 ton Unreacted acetic acid
Isoborneol acetate
Unreacted camphene
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6. Saponification reactor( Isoborneol formation) To ensure total conversion IBA: NaOH :: 1:0.22
Since the conversion is 100%, so the amount of Isoberneol formed is same as IBA produced i.e 0.3465 ton Caustic soda (NaOH) taken = .07623 ton 7. Dehydogenation Reactor (Camphor) Isoborneol produced is dehydrogenated to give Camphor
Since
isoborneol
is
totally
convert
into
hydrogen
and
camphor, so the amount of camphor produced is same as that of isoborneol formed. Amount of camphor formed = 0.3465 ton %Conversion of camphor = .3465/1*100 = 34%
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General
design is normally is to divided calculate into the two main of steps, a
tower
process design followed by a mechanical design. The purpose of the process design number required theoretical stages, column diameter and tower height. On the other hand, the mechanical design focuses on the tower internals and heat exchanger arrangements. Many distillation factors column have such to as be the considered safety in and designing a environmental
requirements, column performance, economics of the design and other parameters, which may constrain the work. The determine feed. few design rules for distillation column are as follows: 1) Direct sequences that remove the components one by one in the distillate are generally favored. 2) Sequences that result in a more equal-molar division of the feed between distillate and bottoms products should be favored. 3) Separations where the relative volatility of two adjacent components is close to unity should be performed in the absence of other components; ie, reserve such a separation until the last column in the sequence. first the step in distillation sequences, column which design is on to the separation depends
32
4)
Separations be
should to
reserved the
separation sequence is decided, engineering calculations follow determine theoretical operating parameters and tower dimensions. In general, the steps included in distillation calculations are summarized into the following:
Performing a material balance for the column Determining temperature) Calculating the minimum number of theoretical stages using the Fenske equation Calculating the minimum reflux rate using the Underwood equations the tower operating pressure (and/or
5)
Determining
the
operating
reflux
rate
and
number
of
theoretical stages 6) Selection of column internals (tray or packings) 7) Calculating the tower diameter and height The theoretical explanation and sample calculations of each step above are discussed in detail in later sections. 5.2 Other factors Some general design rules (from Cheresources.com) that should be considered are as follows: 1. Distillation is usually the most economical method of
separating liquids.
2. For Ideal mixtures (low pressure, medium temperature, and non-
3. Tower
operating
pressure
is
determined
most
often
by
the
temperature of the available cooling medium in the condenser or by the maximum allowable reboiler temperature. 4. Tower Sequencing Easiest separation first least trays and reflux When neither relative volatility nor feed concentrations vary
widely, remove components one by one as overhead products. When the adjacent ordered components in the feed vary widely
in relative volatility, sequence the splits in order of decreasing volatility. When the concentration in the feed varies widely but the
relative volatilities do not, remove the components in the order of decreasing concentration in the feed. 5. Economically optimum reflux ratio is about 120% to 150% of the minimum reflux ratio. 6. The economically optimum number of stages is about 200% of the minimum value. 7) A safety factor of at least 10% above the number of stages by the best method is advisable.
8) A safety factor of at least 25% about the reflux should be utilized for the reflux pumps. 9) Reflux drums are almost always horizontally mounted and designed for a 5 min holdup at half of the drum's capacity. 10) For towers that are at least 3 ft (0.9 m) in diameter, 4 ft (1.2 m) should be added to the top for vapor release and 6 ft (1.8 m) should be added to the bottom to account for the liquid level and reboiler return. 11) Limit tower heights to 175 ft (53 m) due to wind load and foundation considerations. 12) The Length/Diameter ratio of a tower should be no more than 30 and preferably below 20.
34
13) A rough estimate of reboiler duty as a function of tower diameter is given by: Q = 0.5 D2 for pressure distillation Q = 0.3 D2 for atmospheric distillation Q = 0.15 D2 for vacuum distillation Where, Q : Energy in Million Btu/hr D : Tower diameter in feet.
35
On
the
other
hand,
packing
divisions
include
grid
random
packing,
conventional
structured
packing,
capacity structured packing. The rules of thumb for selecting packing are: 1) The compounds are temperature sensitive 2) Pressure drop is important (vacuum service) 3) Liquid loads are low 4) Towers are small in diameter 5) Highly corrosive service (use plastic or carbon) 6) The system is foaming 7) The ratio of tower diameter to random packing is greater than 10 Some design guidelines should be considered when designing a tray tower, such as follows: 1) Constriction factor The constriction factor should not be less than 0.6. This parameter shall be checked only for the side downcomer. 2) Tray spacing Overall column heights depend on tray spacing. Tray spacing should common be from 18 to is 24 inches, inches with to accessibility allow easy in mind for (Generally, for a tower diameter of 4 feet and above, the most tray spacing 24 access maintenance. However, for a tower diameter below 4 feet, a tray spacing of 18 inches is adequate as the column wall can be reached from the man way.) 3) Peak tray efficiencies Iy usually occur at linear vapor velocities of 2 ft/s (0.6 m/s) at moderate pressures, or 6 ft/s (1.8 m/s) under vacuum conditions.
36
4) A typical pressure drop : Pressure drop per tray is 0.1 psi (0.007 bar). Max Dry pressure drop in height of hot liquid less than 16% of tray spacing. 5) Tray efficiencies: For aqueous solutions these are usually in the range of 60-90% while gas absorption and stripping typically have efficiencies closer to 10-20% 6) Sieve tray holes The generally vary are 0.25 to 0.50 in. diameter with the total hole area being about 10% of the total active tray area. Maximum efficiency is 0.5 in and 8%. That large holes are recommended for fouling and corrosive services and a spray regime. 7) Valve trays Valve tray typically has 1.5 in and 2 in. diameter holes each with a lifting cap. 12- 14 caps/square foot of tray is a good benchmark. The disk typically rises 3/16 to 7/16 in above the tray deck and 10 % open area of fully open valves. 8) Weir height The most common weir heights are 2 to 3 in and the weir length is typically 75% of the tray diameter. For vacuum operation is recommended 0.25 to 0.5 in to reduce the pressure drop. 9) Weir loading The maximum recommended weir loading is 13 gpm/inch. At high weir loadings, trays will have high pressure drop, high froth height and potential downcomer limitations. At lower weir loading, picket fencing may be required.
37
10) Downcomer clearance It is recommended 1.5 in. At low liquid loading the clearance can be reduced to secure a proper distribution of the liquid on the active area, but lower than 1 in are not recommended. At high liquid loading the clearance can be increased up to the weir height to minimize the head loss and the jetting. 11) Downcomer velocity: and residence time velocities is range from 0.1-0.7 ft/s, the maximum velocity needs to be lowenough to prevent downcomer flooding. The minimum residence time is 3 s and the best residence time is 5 s. the residence time needs to be long enough to allow adequate vapor-liquid disengagement. 12)Flow path length The flow path length is measured from the downcomer exit to the outlet weir. Minimum size is typically 16 to 18 inches. High flow path length will enhance the efficiency while the low flow path length will increase weir load. 13) Open area Open area typically 0.04 to 0.15. lower values may result hydraulic limitation and mass transfer efficiency reduced while higher value result less the tray efficiency. The packed tower design concepts are listed below: 1) Packed towers almost always have lower pressure drop compared to tray towers. 2) Packing is often retrofitted into existing tray towers to increase capacity or separation.
38
3) For gas flow rates of 500 ft3/min (14.2 m3/min), use 1 in (2.5 cm) packing, for gas flows of 2000 ft3/min (56.6 m3/min) or more, use 2 in (5 cm) packing. 4) Ratio of tower diameter to packing diameter should usually be at least 15 5) Due to the possibility of deformation, plastic packing should be limited to an unsupported depth of 10-15 ft (3-4 m) while metal packing can withstand 20-25 ft (6-7.6 m). 6) Liquid distributor should be placed every 5-10 tower
diameters (along the length) for pall rings and every 20 ft (6.5 m) for other types of random packing. 7) For redistribution, there should be 8-12 streams per sq. foot of tower area for towers larger than three feet in diameter. They should be even more numerous in smaller towers. 8) Packed columns should operate near 70% flooding. 9) Height Equivalent to Theoretical Stage (HETS) for vaporliquid contacting is 1.3- 1.8 ft (0.4-0.56 m) for 1 in pall rings and 2.5-3.0 ft (0.76-0.90 m) for 2 in pall rings. 10) Packing support is used to carry the weight of the wet packing while allowing free passage of the gas and liquid. Gas inlets are provided above the level where the liquid flows from the bed. 11) Liquid distributor is used to maintaining a uniform flow of liquid throughout the column. For small diameter columns, a
39
central open feed pipe or one fitted with a spray nozzle may well be adequate. 12)Liquid redistributors Redistributors are used to collect liquid that has migrated to the column walls and redistribute it evenly over the packing and also out any maldistribution.
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40
While designing a chemical plants material of construction of various units must be properly selected.Once the type of equipment is selected,the materialsfor construction have to be established.The process engineer should have a general idea of the materials that are compatible with the process.The selection of materials for specific application depends upon the process requirement,purity of product,mechanical properties of materials such as knowledge brittleness, creep, ductility , fatigue,hardness,impact strength,malleability,toughness strength characteristic etc.The permits the of material strength,tensile
process engineer to select the proper material efficiency for process equipment and its supporting structure.While selecting the material economic consideration also play a major role.The cost of materials,its availability,fabrication technique,cost & strength or properties has to be specifically considered. The most economically materials that satisfies both process & mechanical requirement should be selected. This will be the materials that gives the lowest cost over the working life of the plant allowing for maintenance and replacement.Other factors such as product contamination & process safety must also be considered.All these factors mostly varies with materials and its properties.The different properties of materials are classified as.
6.1. Properties
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6.1.1Mechanical properties 1.Strength- Tensile strength 2.Stillness-Elastic modulus 3.Toughness- Fracture resistance 4. Fatigue resistance 5. Creep resistance 6. Ductility-brittleness 6.1.2 Thermal properties These includes thermal conductivity,heat capacity, melting point etc. The mechanical properties vary with thermal properties. 6.1.3 Corrosion resistance This is the most important aspects that plays prominent role in the selection of materials of construction.Corrosion resistance depends & upon may precise greatly corrosive influence environment the resistance where of a concentration,purity level,aeration flow velocity,heat transfer temperature particular material.Usually corrosion rate is measured in terms of thickness reduction or weight loss.As in meter stream is passed through jacket therefore care it cause be high corrosion during stresses.Therefore selection. 6.1.4 Temperature This is an important as the aspect may while be selecting or low material which of will respective should taken
construction
temp
high
defiantlyshows its influence on the mechanical properties of the materials. In the Camphor plant the maximum temperature attained
42
is 150-250 C. The materials of construction for these equipment should be proportionally chosen taking into accounts the mechanical properties at such a high temperature. 6.1.5 Special properties Special properties required are thermal conductivities,
electrical resistance, magnetic resistance etc. 6.1.6 Fabrication These properties govern the case of fabrication
i.e.,forming,welding, casing. 6.1.7 Availability Materials of construction should be available in standard sizes and may be in the form plate section or tube. 6.1.8 Machinability The ease with which material may be machined or fabricated plays an important role upon the cost of the equipment.
6.2 Cost
This is the most important criteria which has to be looked. It itself depends upon number of factor,which is shown in cost estimation.The more cost rating compares the relative cost of various materials as given by. CR = C/Fs C = Cost per unit mass(Rs/kg) = Density
Fs = Design stress(N/mm2)
43
The
appropriate
values
of
relative
cost(CR)
for
the
following materials are:Carbon Steel Aluminum Stainless Steel Copper 01 18 06 27 Seeing all these factor we can say the for selection of materials,it really requires the large experience.So referring literature it is found that no special materials of construction are necessary & stainless steel is used only in those parts which are in contact with the product. For the manufacturing of Camphor,the reactor are made
from stainless steel. Stainless steel can be considered as: i. ii. Feritic stainless steel Martensitic stainless steel
1.Feritic
stainless
steel-It
has
carbon
content
less
than
0.2%,chromium contents are between 11-18%,its tensile and impact strength is poor.It cannot be heat treated,it has good corrosion resistance.It is useful for handling strong oxidizing acids i.e. nitric acid, sulphuric acid etc. 2. Martensitic stainless contents is issued steel-It are as has carbon to content has steel upto good for
1.2%,chromium
between cladding
12-18%.It carbon
hardenability,it chemicals.
44
3. its
Austenitic austenitic
stainless
steel-In at
to
carbon
&
chromium,it contains 3.5-22% nickel.Nickel allows it to retain microstructure high strength,good containing ductility & corrosion resistance. It is also good for handling sulphuricacids,organicacids.Austenitic moly denum upto temperature of 3 0 C not good enough for has good resist to pitting corrosion.high above and in alkaline solution,it is reducing toxic environment & severe
susceptible to stress corrosion cracking.All these steels are corroding media. Some of the stainless steel used application are as follows: Type Application
of
the
liquid
being
processed adopting
specially the
in
food
&
pharmaceutical advantage
industries. of strength
In of
composite
structure,
cheaper material and corrosion resistant properties of material which may either lack in strength or may be costly beneficially utilized. Mild steel lined with lead, titanium, rubber, plastic,
glass are well known in chemical process industries. In Camphor units, camphor should be stored in epoxy lined silos
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46
The success
proper as the
of of
plant a up
is of
as
to of
its an
process. any
appropriate
location
setting
is
quite
necessary so as to run the plant under profitable condition. It is necessary that overall outlook s taken into account and all selection factor while selecting a suitable location of the proposed plant. In this chapter a brief discussion regarding the principle factor leading to selection of location are summarized as follows.
1.
2. Sufficient raw material supply. 3. Uninterrupted supply of utilities like water, power & fuel. 4. Location with respect to market for products. 5. Good transport facilities. 6. Availability of labour. 7. Effluent disposal facilities. 8. Suitable topography and weather condition. 9. Soil condition and bearing quality of site. 10.Local community consideration. 11.Political atmosphere.
47
For the safe and economic working of a plant it is of great importance to take into account selecting the site. Camphor & Allied product limited are pioneers in the field of turpentine chemistry in India, having established the first synthetic camphor plant with technology from Dupontof USA in 1964. There Gujarat with from tons are and two plant operating Uttar in Indiai.e The The just in Vadodara, plant and away is raw so and all the above factors while
Bareilly,
Pradesh.
located in West Uttar Pradesh, 250 km from New Delhi on NH-24 coordinate here, of 2823'46"N railway and 7922'57"E. station is materials can be easily transported by road and rail network Bareilly transportation can be easily done. It handles a volume of 20,000 raw materials finished products annually incorporates the latest technology and equipment. It carry out all conceivable chemical operations such as
fractionation,
esterification,
saponification,
hydrogenation,
dehydrogenation, oxidation, peroxidation, pyrolysis, etc. in the plant using equipment and technology that is constantly updated with time to keep pace with the latest advancements in chemistry and chemical engineering practices. Their grades), resins vast product range Pine includes is synthetic free Camphor of air (all and
Terpineols, many
Oils, plant
Isobornyl totally
acetate,
Terpene
and
more. The
liquid pollution and maintains strict vigil all the time to protect environment and people.
possible ease of
output
of
high is
quality performed
at at
lowest the
possible point of
cost
of
manufacturing. It aims at discovering an optimum plan by which operation greatest convenience. Maximum productivity from plant building and equipments can be obtained only when these facilities are so integrated to provide smooth flow of materials, parts and products. Smooth flow is a result of a good plant layout. Management can obtain the desired objectives through an efficient follows. 1. Economics in material and product handling. 2. Minimizing of useful areas. 3. Avoidance bottlenecks. 4. Avoidance of unnecessary and costly charges once a layout is made. 5. Improvements in production process & methods. 6. Incorporation of safety into the physical plant as part of the layout & organization. 7. Better product control & supervision. 8. Safety. Plant layouts ideally involve the allocation of space and the arrangement of the equipment in such a way that overall operating costs are minimized. A complete layout project represents the master plan for physically integrating the factor of production which are required on the premises. Poor layout
49
plant
layout.
The
objectives
to
be
attained
as
results
in
high to
materials mention
handling only a
cost few
& of
excessive the
space
requirements
consequent
inefficiencies.
and
they
can
be
manufactured
in
stock.
The
equipments
and
machines us in such factor are therefore generally arranged in a straight line or in sequence in which they are used. The functional layout is more suitable for those which
carry out for job order production. In such factories no two job are similar and so line layout is out of questions. Machines in such factories are generally arranged according to functions. The machines performing the same process are grouped together in department. In this way a number of departments are set up each of which is responsible for a specific process and not a product as in the line layout.
different equipment in a certain typical sequence. Hence the product layout process suitable manufacture of camphor. One important factor to kept in is adequate space for future expansion to meet the changing demands. Again not only the processing block like boiler house, dumping yard section, canteen should be given due importance. More room should be provided near the raw material and product storage to allow easy loading and unloading operations. The general need which must considered while laying out a plant are: 1. Ensuring smooth production flow. 2. Absence of back traffic and congestion. 3. Easy control and supervision. 4. Maximum productivity.
51
5. Flexibility in operation. 6. Should consider expansion and growth potential of enterprise. The cost of construction can be minimized by adopting a layout that gives the shortest run of construction pipe between equipments. Adequate space must be provided for man, machines, raw
materials and products. Due consideration must also be given to technical requirements, waste disposal, antipollution and other legal provision. The given figure the complete plant layout for manufacture of camphor in which all above aspects have been considered. The not on layout danger should the be such that of the man movement and of man and and
materials should be in minimum possible time. The layout should security equipments consideration should be given to waste disposal arrangement and waste effect treatment.
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52
Inspite of all skill of operation, all the precision in design inspection & equipment reviews, the process has to operate under component failure, utility imperfection & human error. In consequence each item may cause damage to the equipment, plants, public lives and to the environment. Modern some technology has been since quite successful & in developing are
failure mode chemicals. However this effort has also introduced additional problems manufacturing handling frequently found to be inadequate to deal with the question of hazards. Various types of hazard are either due to the nature and properties of the materials or due to side reactions. During processing the materials are likely to undergo fire hazards, mechanical hazards, chemical hazards, electrical hazards etc. All manufacturing processes are to some extent hazardous but in chemical process there are addition hazard associated with the process. The designer must be aware of those hazards & ensure the application of sound engineering practices so that the risk are reduced a to acceptable plant levels. Attempt must be made to provide design having maximum protection for plant
personal and minimum chance of occurring of any accident. All operating personnel in the plant should study and get themselves well acquainted and well versed in various hazardous situations. In every process industry a wide variety of preventive & protective safety measure must be provided, such measure are of two type.
53
2.
Measure
which
will
limit
the
extent
of
damage,
if
the
8.1 Hazards
8.1.1 Fire Hazard Fire can be due to inflammable fuel like petroleum product, oils, lubricants, wood etc. The objective is to minimize the chance of personnel injury, loss of life and property, damage and production discontinuity, so we must require necessary means to control fire. The properties of flammable materials must be studied &no where in process the temperature should be allowed to reach 30% auto ignition temperature or above flash point. So allied air, so flammable product, these substance camphor can must be handled with care. at to These normal dissent
catches crawl
fire along
temperature. The vapour of flammable substance is heavier than vapour flames & spark and then flashed back to the source. All drums, container and tanks are connected to ground
electricity whenever flammable material is being transferred, this prevents build up of static electricity and the possibility of starting of spark. All flammable container are kept closed when not in operation. Fire alarm system are must to control fire, necessary and equipment like heater, supply furnances should be should there be to protected against accidental explosion. Hot surface should be insulated uninterrupted water control fire in case of emergency. 8.1.2 Mechanical Hazards All the machinery & tools must be well protected in
accordance with the instruction laid down in Indian factory act for safeguarding against mechanical hazards. Automatic control
54
systems, alarms should be provided correct structural design of the vessels, piping & steel work should be done. Some of the safety measure are: 1. Guarding or avoiding sharp ends. 2. Insulation of electrical tools. 3. Process relief jets in steam jackets or chambers. 4. Use anti spark tools in explosive and inflammable areas. 8.1.3. Electrical Hazards All the electrical appliance should be installed accordingly to Indian electricity act for safeguarding against electrical hazards. Proper insulation of valves is of utmost importance Preventive measure should be taken against shock and burns. High voltage equipment should be properly covered. There should be proper wiring and insulation, safety switches and capacitor should be used. Periodic checking should be done be maintenance department. 8.1.4 Chemical Hazards These may be due to persons coming in the contact with the corrosive chemical directly or indirectly. Inhalation of harmful fumes should be checked. These may be due to process leaks or through vents. Storing of chemicals should be as minimum as possible, it should be stored to safe places and arrangement should be made to ensure 100% safety. During handling of hazardous chemicals, normal safety equipment such as gloves & chemical splash goggles should be worn. In case of exposure to eyes, it should be
55
flushed
with
water
and
physician
should
be
contacted
immediately. Prolong contact with solution should be avoided. Some of basic preventive and protective measure that should be taken in in from consideration process spill and areadequate and supply of water for of and & protection over pressure relief device, segregation of reactive materials drainage plant lines fire all equipment, water from grounding nozzles electrical equipment, safe location of auxiliary electrical gear fighting adequate sprinkler head, insulation of hot surface, proper building and layout above advanced instruments control facilities.
2. Side reaction 3. Stability 4. Temperature 5. Pressure Control 8.2.3 Control system 1. Fail safe 2. Back up system 3. Automatic operation of valves 4. Alarms 5. Inert purging blanketing 6. Mechanical control system ( in case of failure) If fire takes place one of following should be onsite 1. DCP-Dry chemical cylinder 2. Water extinguisher 3. Foam extinguisher 4. CO2 extinguisher 5. Dry sand
57
7. Fire extinguisher are placed at various locations & fire hydrant fighting. is available throughout the plant for fire
regulations and to maintain ecological balance, zero effluent technology for camphor and allied products plants have been selected discharge Pradesh at the outset. The is quality of liquid effluent and is at from the factory control by monitored The high continuously air quality samplers
remains much lower than the norms prescribed by the Uttar pollution board. constantly monitored providing volume
different locations around the factory campus. Eighty meter wide green belt has been developed around the factory and the township to keep the environment clean. A number of trees have been planted in the plant area to check the pollution level inside plant and to control its adverse effect. 8.4.1 Methodology for environment protection Environment protection starts with identification of all the activities, which have a substantial environmental impact. These are: i) Air emission quality and quantity ii) Effluent quality and quantity iii) Hazardous waste generation iv)Non hazardous waste generation v) Consumption & conservation of Natural resources. vi) Ensure compliances with National Environmental Quality vii)Standards, Rules & Regulations covered under Environmental Protection Act, 1986. viii) Recycle and reuse of the wastes generated
58
ix) Ammonia odor in the plant x) Noise 8.4.2. Environment management system at Camphor & allied product ltd, Bareilly Camphor & allied product ltd. has sound environmental management system comprising of following features:i) Afforestation ii)Zero Effluent Technology iii)Social Forestry iv) Monitoring of ambient air and stack emissions v)Development of all-round awareness regarding environmental issues vi) ISO-14001:2004 (EMS) Accreditation
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59