Manufacturing of Pentaerythritol

MANUFACTURING OF PENTAERYTHRITOL
By
Siddharth Maity
B.E., Mumbai University, 2006
An Industrial Engineering Project Report

Submitted to the Faculty of the
Speed Scientific School of the University of Louisville
in Partial Fulfillment of the Requirements
for the Degree of
Master of Engineering
in
Industrial Engineering
Department of Industrial Engineering

University of Louisville
Louisville, Kentucky
December 2009
MANUFACTURING OF PENTAERYTHRITOL
By
Siddharth Maity
B.E., Mumbai University, 2006
An Industrial Engineering Project Report

Approved on
By the Following Faculty Member:
________________________________
Faculty Name
ACKNOWLEDGEMENTS
I take this opportunity to express my sincere gratitude towards Dr. Suraj M. Alexander for his
guidance, help and constant encouragement. This Project Report would not have been possible
without his support.
I also thank Bhageria Dye-Chem for allowing me to visit their plant and providing me with data
required for Material Balance, Energy Balance and Cost Estimation.

ABSTRACT_________________________________________________________________5
INTRODUCTION____________________________________________________________6
Physical and chemical properties_______________________________________________________7
Reactions of Pentaerythritol___________________________________________________________10
Product Applications____________________________________________________________________13
PROCESS SELECTION____________________________________________________17
PROCESS DESCRIPTION_________________________________________________19
THERMODYNAMIC FEASIBILITY_________________________________________20
MATERIAL BALANCE_____________________________________________________21
ENERGY BALANCE________________________________________________________29
DESIGN OF EQUIPMENT_________________________________________________34
Design of Neutralization Tank__________________________________________________________34
Evaporator Design Report______________________________________________________________39
LIST OF MAJOR EQUIPMENTS___________________________________________45
INSTRUMENTAL PROCESS CONTROL & PRECAUTIONS________________50
SELECTION OF LOCATION & PLANT LAYOUT___________________________51
SERVICE AND UTILITIES_________________________________________________53
PROFITABILITY & COST OF PROJECT____________________________________54
CONCLUSION_____________________________________________________________63
REFERENCES_____________________________________________________________64
References
Abstract
Pentaerythritol, an organic compound has found its use in a wide range of industries due to its
multi-functionality and favorable physical & chemical properties. This project studies the various
chemical and industrial aspects involved in the manufacturing of this compound. Process
selection, Material & Energy Balance, Design of Equipments are some the topics from chemical
engineering which are covered during the course of this project. On the other hand, Plant layout
& selection of location, Service and Utilities, Cost estimation are some topics with industrial
engineering background. This project aims at using and analyzing all these ideas and the
available data to come up with a model which can be used for manufacturing of Pentaerythritol.
Introduction
In the year 1882, pentaerythritol was discovered as byproduct of the reaction between barium
hydroxide and impure formaldehyde. Several year later in 1891, Tollens along with his
coworkers found that the impurity was acetaldehyde, which condensed with the formaldehyde
under mildly alkaline conditions. The name pentaerythritol which was assigned to this compound
was derived from erythritol t o indicate the presence of 4 hydroxyl groups and the prefix “penta”
to show that there are 5 carbon atoms in the molecules.
Pentaerythritol is a white crystalline compound. The high melting point, slight solubility in water
and the ready reactivity of its 4 hydroxide groups have been attributed to the compact symmetric
structure of the molecules. It is an optically inactive compound, resembling cane sugar in
appearance and has a sweet taste characteristic of polyols. Pentaerythritol is nonhygroscopic and
stable in air and sublimes slowly on heating. It is moderately soluble in cold water, quite soluble
in hot water, and has only a limited solubility in organic liquids.
Uptil 1930 all pentaerythritol produced was used in manufacturing of pentaerythritol tetranitrate,
an explosive substance. Purified pentaerythritol (P.E) is used as a surface coolant. It is also in
paints, varnishes industry and the production of resins. P.E is increasingly used in resins
manufacturing mainly because of its desirable characteristics and price stability.

Physical and chemical properties
1. Pentaerythritol
CH2OH
|
|
Structure:
HCOH2--------C-------CH2OH
|
|
CH2OH
Physical form White, crystalline and odourless
Molecular weight 136.15
Composition C = 42.2% H = 8.8% O = 49%
Melting point 262oC
Boiling point 276oC at 30m.m pressure.
Specific gravity 1.396
Toxicity Low and nonirritating to skin
Heat of combustion -660 Kcal/Mole
Heat of formation 226.6 Kcal/Mole
Heat of vaporization 22 Kcal/Mole
Heat of sublimation 31.4 Kcal/Mole
Pentaerythritol sublimes on heating under reduced pressure. It is non hygroscopic, nonvolatile,
optically inactive and stable in air. It is slightly soluble in cold water and readily soluble in hot
water.
2. Sodium Hydroxide (NaOH)

Molecular weight 40
Boiling Point 130.04 K
Melting Point 596.04 K
Liquid Molar Volume 2.245 x 10-2 m3/Kg mol
Heat of Formation -4940.27 KJ/Kg
Gibbs Free energy -5008.47 KJ/Kg
Heat of Fusion 165.13 KJ/Kg
Liquid Cp 2.180 KJ/Kg-K
Density 2101.6 Kg/m3
3. Acetaldehyde (CH3CHO)
Molecular weight 44
Liquid Molar Volume 5.652 x 10-2 m3/Kg mol
Gibbs Free energy -2923.81 KJ/Kg
Heat of Fusion 73.07 KJ/Kg
Heat of Combustion -25054.02 KJ/Kg
4. Formaldehyde (HCHO)
Molecular Weight 48
Liquid Molar Volume 5881 x 10-2 m3/Kg mol
Gibbs Free Energy -4387.74 KJ/Kg
Heat of Combustion -23077.02 KJ/Kg
Density 1087 Kg/m3
5. Sodium Formate (HCOONa)
Molecular Weight 68
Gibbs Free Energy -8552 KJ/Kg
Liquid Cp 2.247 KJ/Kg K
Solubility Data
Solvent Temp 0C Solubility Temp 0C Solubility
g/100gms g/100gms solvent
solvent
Water 25 0C 9.23 97 0C 77.2
Methanol(100%) 25 0C 0.75 50 0C 2.10
Ethanol (100%) 25 0C 0.33 50 0C 1.00
Ether 25 0C 0.45 50 0C 5.00
Ethanol amine 25 0C 0.80 100 0C 10.00
Glycerol 25 0C 16.5 100 0C 44.5
Reactions of Pentaerythritol
1. Oxidation: The polyols are readily attacked by a variety of oxidizing agents like
chromic and nitric acid; it degrades the polyols to CO2.
2. Reduction: The polyols can be reduced by conc. HCL in the presence of certain
catalyst. The end product is secondary alkyl iodide and alkenes without alteration of
the carbon chain.
3. Esterification: Esters with organic acids can be produced in the usual manner with
acid anhydrides or acid chlorides. Esters with inorganic acids are nitrates which are
explosive.
4. Etherification: ether of the polyols are readily produced by reaction with methyl or
ethyl sulfate with the appropriate alkyl chloride and alkali.

5. Nitration: Pentaerythritol on nitration with HNO3 gives Pentaerythritol Tetranitrate
which is an explosive substance.
Grades and Analysis
The analysis of technical pentaerythritol generally includes the following determination:
pentaerythritol contents, melting range, hydroxyl content, ash content, acidity, moisture content,
water solubility, color and physical state. The method used for analysis is the Benzal Method.
Technical pentaerythritol contains 85 to 90 % pentaerythritol and 10 to 15% polyhydric alcohol
such as dipentaerythritol.
Byproduct:
• Dipentaerythritol: About 10 to 15 % in the technical grade of pentaerythritol. It is
separated from pentaerythritol by procedure based on differences in solubility in wither
water or alcohol.
• Tripentaerythritol: It is separated from pentaerythritol by fractional crystallization.
• Sodium formate: It is the main byproduct heaving field about 10%. It is separated from
pentaerythritol by the use of different crystallization temperature. It is used in the
manufacture of formic acid.

Chemistry of Pentaerythritol:
The product pentaerythritol is made from acetaldehyde and formaldehyde in the presence of an
alkaline condensing agent. Initial reaction is three successive molecules of formaldehyde added
to one molecule of acetaldehyde by the classic Aldol reaction.
1. CH3CHO + HCHO HOCH2-CH2CHO
2. HOCH2-CH2CHO + HCHO (HOCH2)2CHCHO
3. (HOCH2)2CHCHO + HCHO HOCH2
|
|
HCOH2--------C-------CHO
|
|
CH2OH
These reactions are truly catalytic and consume no base. They are also reversible. The equlibria
of above reactions are displaced continuously to the right by a second possible reaction between
two aldehydes in the presence of base i.e. crossed Cannizaro, and the last reaction is not
reversible which gives pentaerythritol.
4. CH2OH
|
|
HCOH2--------C-------CHO + HCHO + NaOH (CH2OH) + HCOONa + Na FORMATE
|
|
CH2OH
In the last reaction base, which is a reactant rather than a catalyst is consumed stoichiometrically.
Side Reactions:
Most of the side reactions occur due to formaldehyde and acetaldehyde reacting with each other.
Reactions of acetaldehyde with itself are rapid. However these reactions can be minimized by
maintaining formaldehyde concentration at all times.
Formaldehyde can react with itself to form sugar like products which eventually caramelize to
import color and odor to the products. The self canizzaro of formaldehyde to for CO 2 and
methanol can be minimized by avoiding high concentrations of formaldehyde and high
temperature. The desired cannizaro does not progress rapidly below 400C and PH10.
Pentaerythritol is isolated from reaction mixture by successive fractional crystallization.
Product Applications
1. Pentaerythritol is principally used in the surface coating field due to its tetrafunctionality
producing higher viscosity, ability of drying vehicles more rapidly than lower polyols,
hardness, durability, color stability and water resistance. It is usually employed in
combination with polyhydric alcohol such as glycerol to prevent premature gelatin.
2. The resins based on pentaerythritol are used in variety of products such as paints,
varnishes, printing ink and adhesives.
3. Pentaerythritol can be converted to polyether. This compound is characterized by
excellent corrosion resistance and high dimensional stability. It is being used in
manufacturing of molding pipes, gears, valves and metal coating.
4. Pentaerythritol esters of fatty acids are used as plasticizers and also as lubricants.
5. Resins prepared from pentaerythritol such as acrolain is used for electrical insulation,
surface coating, films and fibers.
6. Pentaerythritol is used alone or in combinations with metal salts as heat stabilizers.
7. It is used in the manufacturing of pentaerythritol tetranitrate which is an explosive.
8. It is used in fire retardant surface coatings. When exposed to high temperatures these
coatings froth and swell to produce a solid, non combustible residue which serves to
protect the substrate from fire.
9. Pentaerythritol tetranitrate (PETN) has characteristics similar to those of cyclonite and is
mixed with TNT to form the explosive pentolite. It also forms the core of the explosive
primacord fuses used for detonating demolition charges and the booster charges used on
blasting.
10. Alkyd resin paint is esters of polybasic acids and polyhydric alcohols which have been
modified by oil and fatty acids. Pentaerythritol is used as a polyhydric acid. In particular,
alkyd paint made with pentaerythritol has superior adhersion, weather & water resistance,
color, luster, chemical resistant properties as compared to trihydric alcohols such as
glycerin. They also dry faster than trihydric alcohols.
11. Due to its properties it is also used for many types of varnish enamels.
12. Pentaerythritol and fatty acid esters give plasticity to synthetic resins. Pentaerythritol
tetraacetate, when used as a plasticizer for celluloses, acetates and cellulose esters, gives
them improved plasticity and impact strength.
13. Pentaerythritol and esters of monobasic long chain fatty acids (stearic acid, palmitic
acid), depending on the degree of Esterification, take various physical forms and are used
as emulsifiers in cosmetics, and as abrasives.

14. Monobasic fatty acid esters of pentaerythritol have outstanding characteristics as non-
ionic surface active agents, and are used in softening processes for synthetic fibers and
chemical fibers (acetate, vinylon, nylon). They are also used for smoothing in various
processes of synthetic textile production. Because fatty acid esters of pentaerythritol are
highly stable, have a relatively high boiling point and are low in volatility, they are used
as brake oil as well as lubricating oil and corrosion preventive oil in aircraft engines.
Manufacturers of Pentaerythritol:
➢ Allied Resins and Chemicals Ltd. (India)
➢ Asian Paints (India)
➢ Kanoria Chemicals and Industries Limited. KCIL Group (India)
➢ Perstorp Aegis Chemicals Pvt. Ltd. (India)
➢ Suzhou Fine Chemicals Industrial Group (China)
➢ Shanxi Sanwei Co. Ltd. (China)
➢ AllChem Industries Inc. (USA)
➢ Celanese AG (Germany)
➢ Derivados Forestales SA (Spain)
➢ Polialco SA (Spain)
➢ Dr. Theodor Schuchardt & Company (Germany)
➢ Guizhou Organic Chemical General (China)
➢ Hercules Inc. (USA)
➢ Hubei Yihua Group Limited Liability Company (China)
➢ Mitsubishi Gas Chemical Company Inc. (Japan)

➢ Hunan Zhuzhou Chemical Industry Group Co. Ltd. (China)
➢ JLM Industries Inc. (USA)
➢ Koei Chemical Co. Ltd. (Japan)
➢ Lee Chang Yung Chemical Industry Corporation (Taiwan)
➢ Metafrax JSC (Russia)

Process Selection
Following are the two methods which can be used in the manufacturing of pentaerythritol. These
manufacturing methods are based on the reaction between formaldehyde and acetaldehyde in the
presence of condensing agents.
Method – 1
In this method, pentaerythritol is manufactured by using Soda-ash to remove calcium ion as a
precipitate of CaCO3. Formaldehyde and acetaldehyde are reacted in the presence of Calcium
Hydroxide in S.S. Reactor. The reaction mixture is pumped to precipitator where soda-ash is
added to precipitate CaCO3 leaving formate as sodium formate. After filtration, slurry is
concentrated in a triple effect evaporator. Then crystallization is followed by filtration in the pan
filter. P.E. cake is dissolved and deionised to remove final traces of sodium formate and then the
mixture is again crystallized followed by filtration in second pan filter. The P.E. cake is then
dried and stored.
In this process, recovery of sodium formate and additional P.E. from mother liquor decides the
profit and loss margin. Hence the recovery units are the parts of operation and are not separated
from the main unit in any case. The process requires a large number of equipments made up of
S.S. including two pan filters. This causes a rise in the initial equipment cost, making it
unfeasible for profit making. Another factor which adds to the investment is the requirement of
two separate units for removal calcium carbonate and sodium formate. Considering all these
factors makes this an uneconomical process.

Method – 2
This method uses acids in place soda-ash in the manufacturing of pentaerythritol from
formaldehyde and acetaldehyde. This process is far more economical as compared to the earlier
method. The following main considerations are taken into account for the selection of this
process:
1. The yield in this process is 85 to 90 % which is higher than that in the previous process.
2. Easy removal of sodium ions as they directly combine with formate ions to give sodium
formate.
3. Recent research can help in making the plant operation 99 % automatic.
4. Byproduct sodium formate can be used to produce formic acid which can be reused in the
same plant.
Process Description
Method 2
A solution of formaldehyde (20 to 30% by wt.) is added to 50% NaOH solution. While the
temperature is maintained at 15 to 20 0C with suitable agitation, 99% liquid acetaldehyde is
slowly added under the surface of the formaldehyde alkali solution. Since the reaction is
exothermic, external cooling is used to maintain the reaction temperature around 20 to 30 0C.
The mole ratio of formaldehyde to acetaldehyde generally used is between 4.5:1 and 5:1. A ratio
of 1:15 mole hydroxide ion per m ole of acetaldehyde appears to be the optimum amount of
condensing agent.The crude reaction mixture is transferred to the neutralization tank here formic
acid is added to reduce the PH of the solution to 7.8 to 8 and subsequently to remove the sodium
ions present as sodium formate. The solution is then evaporated to a specific gravity of about
1.270. It is then chilled to crystallize pentaerythritol and the resulting slurry is filtered. The
mother liquor goes to the recovery system, where it is reworked and sodium ions are removed as
sodium formate.
The filter cake contains P.E. and Poly-pentaerythritol. The latter material is formed by the side
reaction and is a mixture of either linked polymers such as Di-pentaerythritol ( (CH2OH)3CCH2-
CH2C(CH2OH)3 ) and Tri-pentaerythritol( (CH2OH)3CCH2-O-CH2C(CH2OH)2CH2-O-
CH2C(CH2OH)3 ) and other byproducts found in the reaction. The yield of pentaerythritol is
about 85 to 90% by weight based on the acetaldehyde charged.
Sodium Formate Recovery Unit:
Mother liquor is concentrated in an evaporator crystallizer to the point where sodium formate
comes out of solution. It is separated from P.E. in solution by centrifugation without cooling.
This phase is batch wise with automatically controlled loading and washing cycle. Formate is
dried in smaller but similar equipment to that used in pentaerythritol.
Filtrate from the centrifuge is cooled and P.E crystallizes. After filtering in a press filter, these
crystals are dissolved in water and activated carbon is added. The solution goes through a plate
frame press and then is recycled back to P.E evaporator feed tank.
Thermodynamic Feasibility
Compound ∆HF (KJ/Kmol) ∆G (KJ/Kmol)
CH3CHO -16580.52 128647.64
HCHO -108415.5 -409702.8
NaOH -197610.8 -136567.6
HCOONa -6480332.2 -340609.96
P.E. -764200.42 -553219.656
∆G = ∑ (∆G) Products - ∑ (∆G) Reactants
= (– 553219.656 – 340609.96) – (– 136567.6 – 409702.8 – 128647.64)
= – 218911.576 KJ/Kmol
∆G = –RT ln Ka at T = 298 K
Material Balance
Annual Output: 600 tons
Operation: 3 shifts (8 hours each), 300 working days/year.
Basis: 2000 Kg of P.E. per day
Required Materials:
 Formaldehyde (37%) – 6350.00 kg
 Acetaldehyde (99%) – 765.00 kg
 Sodium Hydroxide (50%) – 2100.00 kg
 Formic Acid(34.65%) – 1200.00 kg
Reaction:
4HCHO + CH3CHO + NaOH (CH2OH)4C + HCOONa
Input Data:
Pure HCHO input 6350 X 0.37 = 2350 kg

Pure NaOH input 2100 X 0.5 = 1050 kg
Pure CH3CHO input 765 X 0.99 = 757.5 kg
H2O from HCHO 6350 – 2350 = 4000 kg
H2O from CH3CHO 765 – 757.5 = 7.5 kg
H2O from NaOH 2100 – 1050 = 1050 kg
Hence, Total Water Input 757 + 4000 + 1050 = 5057.5 kg
Output Data:
Moles of CH3CHO = 757.5 / 44 = 17.2 kg.mole.
17.2 kg.mole of CH3CHO gives = 17.2 kg.mole of P.E by stoichiometry.
Hence P.E. produced = 17.2 X 136.1 = 2341.23 kg
Moles of CH3CHO = 757.5 / 44 = 17.2 kg.mole.
17.2 kg.mole of CH3CHO gives = 17.2 kg.mole of HCOONa by stoichiometry.
Hence HCOONa produced = 17.21 X 136.1 = 1170 kg
NaOH required = 17.21 X 40 = 688.40 kg
NaOH excess = 1050 – 688.4 = 361.6 kg

HCHO required = 4 X 17.21 X 30 = 2065.33 kg
HCHO excess = 2350 – 2065.33 = 284.67 kg
1. Reactor Material Balance:
Input Output (To Neutralizer)
HCHO 2350 kg
CH3CHO 1050 kg
NaOH 757.5 kg
H2O 5057.5 kg
Total Input 9215 kg

2. Neutralizer Material Balance:
P.E. 2341.23 kg
HCOOH + NaOH
HCOONa 1170 kg
HCOONa + H2O
Excess NaOH 361.6 kg
Formic acid added = 1200 kg. Excess HCHO 284.67 kg
Pure formic acid quantity in input = 1200 X H2O 5057.5 kg
0.346 = 415.84 kg (Since it is 34.6% pure) Total Output 9215 kg
Input Neutralizer Output Neutralizer(To

holding tank)
P.E. 2341.23 kg P.E 2341.23 kg
HCOONa 1170 kg HCOONa 1783.94 kg
Excess NaOH 361.6 kg H2O 6005.16 kg
Excess HCHO 284.67 kg HCHO 284.67 kg
H2O 5057.5 kg Total 10415 kg

Output
HCOOH 1200 kg
(34.6%)
Total Input 10415 kg
3. Holding Tank Material Balance:
Holding Tank Input Holding Tank Output (To evaporator)

P.E 2341.23 kg P.E 2341.23 kg
HCOONa 1783.94 kg HCOONa 1783.94 kg
H2O 6005.16 kg H2O 6005.16 kg
HCHO 284.67 kg HCHO 284.67 kg
Total Intput 10415 kg Total Output 10415 kg

4. Evaporator Material Balance:
From Holding Tank To Atmosphere

3277.22k
P.E 2341.23 kg H2O g
HCOONa 1783.94 kg HCHO 284.67 kg
H2O 6005.16 kg To Holding Tank II
2341.23
HCHO 284.67 kg P.E. kg
2727.94
Total Input 10415 kg H2O kg
1783.94
HCOONa kg
Total
Output 10415 kg
Specific Gravity Volume (Liter) Weight (kg)

P.E 1.396 1677.098 2341.23
HCOONa 1.8 (100%) 991.07 1783.94
H2O 3329 3329
Specific Gravity of Outgoing Slurry = 1.27
1.27 = (wt. of outgoing slurry) / (vol. of outgoing slurry)
= [wt. of (P.E. + HCOONa) + wt. of H2O(x)] / [vol. of (P.E. + HCOONa) + vol. of H2O(x)]
1.27 = [4125.17 + x] / [2668.208 + x]
Hence, x = 2727.94 kg
H2O Evaporated = 6005.94 – 2727.94 = 3277.22kg

5. Holding Tank II Material Balance:
From Evaporator To Vacuum Crystallizer

P.E. 2341.23 kg P.E. 2341.23 kg
H2O 2727.94 kg H2O 2727.94 kg
Total Input 6853.11 kg Total Output 6853.11 kg
6. Vacuum Crystallizer Material Balance: Yield of P.E. is about 85% to 90%.
Assume that 14.8% of P.E. is lost i.e. will not crystallizer in the crystallizer.
P.E. in solution = 2341.23 X 0.148 = 347.23 kg
Hence, P.E. in crystallizer = 2341.23 – 347.23 = 1994 kg ≈ 2000 kg
From Holding Tank To Centrifuge

P.E. 2341.23 kg P.E. Crystal 1994 kg
H2O 2727.94 kg P.E. Liquid 347.23 kg
HCOONa 1783.94 kg H2O 2727.94 kg
Total Input 6853.11 kg HCOONa 1783.94 kg
Total Output 6853.11 kg
7. Centrifuge Material Balance:
From Vacuum Crystallizer To Dryer

P.E. Crystal 1994 kg P.E. 1994 kg
P.E. Liquid 347.23 kg H2O 127.28 kg
H2O 2727.94 kg To Recovery Unit
Total Input 6853.11 kg H2O 2600.66 kg
P.E. 347.23 kg
Moisture loss with P.E. is assumed 6%
WaterP.E+Water= 0.06=x/(1994+x)
Hence, x = 127.28 kg
8. Dryer Material Balance:
From Centrifuge To Bagging

P.E. 1994 kg P.E. 1994 kg
H2O 127.28 kg H2O 6 kg
Total Input 2121.28 kg To Atmosphere
H2O 121.28 kg
SODIUM FORMATE RECOVERY UNIT:
1. Evaporator Crystallizer Material Balance:
Assume specific gravity of outgoing slurry = 1.37
1.37=wt.of HCOONa+wt.of P.E. + wt.of water(x)vol.of HCOONa+vol.of P.E. + vol.of
water(x)
1.37=1783.94+347.23+x991.07+248.73+x
Hence, x = 1185 kg
Input Output
H2O 2600.66 kg P.E. 347.23 kg
P.E. 347.23 kg H2O 1185 kg
HCOONa 1783.94 kg H2O (to atm) 1415.66 kg
2. Centrifuge Material Balance:
From Evaporator Crystallizer To Centrifuge

H2O 1185 kg H2O. 1113.9 kg
P.E. 347.23 kg M.L.P.E. 347.23 kg
Total Input 3316.17 kg To Atmosphere
HCOONa 1694.743 kg
H2O. 71.1 kg
3. Chiller Material Balance:
From Centrifuge To Filter Press

H2O 1113.9 kg H2O 1113.9 kg
P.E. 347.23 kg P.E. Crystals 318.86 kg
HCOONa 89.197 kg Liquid P.E. 28.37 kg
4. Filter Press Material Balance:
From Chiller Output

P.E. Crystals 318.86 kg P.E. Crystals 318.86 kg
Liquid P.E. 28.37 kg Liquid P.E. 28.37 kg
H2O 1113.9 kg H2O 1083.9 kg
Total Input 1550.327 kg H2O (to atm) 30 kg
For Recovery Unit:
1. P.E. from dryer having 0.3% moisture = 0.003 X 318.8 = 0.957 ≈ 1
Total P.E from Recovery Unit = 318.8 + 1 = 319.8 ≈ 320 kg
2. Sodium formate from dryer having 0.3% moisture = 0.03 X 1694.7 = 5.08 kg
Total HCOONa = 1694.7 + 5.08 ≈ 1700 kg
3. Total P.E. produced per day = 2000 + 320 = 2320 kg

Energy Balance
1. Energy Balance of Reactor
Reaction: 4CH2O + CH3CHO + NaOH C(CH2OH)4 + HCOONa
Compounds Specific Heat CP (cal/gm0C) Heat of Formation HF (Kcal/gm-mole)

CH2O 0.526 -30.29
CH3CHO 0.54 -41.72
NaOH 0.3125 -112.193
C(CH2OH)4 [P.E.] 0.386 -226.6
HCOONa 0.269 -100
H298 = (HF) products – (HF) reactants = -326 – (-275.11) = -51.49 Kcal/gm-mole
H298 = -51.49 X (2341.23 X 1000) / 136 = -886396.564 Kcal/day
H reactant = ∑ m.Cp.dt = (2350 X 0.526 + 1050 X 0.54 + 757.5 X 0.3125) X (298 – 303)
= -10199.1 Kcal/day
H product = ∑ m.Cp.dt = [(2341.23 X .386) + (1170 X .269)] X 5 = 6092.2 cal/day
Q = H reactant + H product + H298 = -10199.1 + 6092.2 – 886396.564 = -890503.464 kcal/day
Heat loss by radiation 10% = -89050.3464 kcal/day
Heat to be removed = 890903.464 - 89050.3464 = 801453.1176 kcal/day
Q = m.CP.dt = m X 1 X (303-293)
m = 801453.1176 / (10 X 3.78) = 21202.46 gallons

2. Energy Balance of Holding Tank
Temp of Holding Tank = 90 0C
Heat to be supplied = ∑ m.Cp.dt
= (2341.23 X 0.386 + 1783.4 X .269 + 6005.16 X 1 + 284.67 X .576) X (90 – 30)
= 453154.758 kcal/day
Now, considering heat loss due to radiation 10%
Heat required = Heat supplied = 1.1 X 453154.758 = 498470.2338 kcal/day
Heat lost by radiation = 498470.2338 – 453154.758 = 45315.47 kcal/day
Steam Required at 2.1125 atm, Ms = (498470.2338 / 525.6475) = 948.3 kg/day
Heat loss by condensation = 121.27 X 948.3 = 115000 kcal/day
Heat to be supplied by steam = (525.6475 – 121.27) X 948.3
= 383471.19 kcal/day
3. Energy Balance for Dryer
Amount of P.E. to be dried = 1994 kg, Water to be removed = 121.28 kg
Sensible heat required to heat material from 25 0C to 100 0C = ∑ m.Cp.dt
= 1994 X (100 – 75) X .386 + 121.28 X (100 – 75) X 1 = 66822.3 kcal/day
Heat required for vaporization of 121.28 kg of water = 121.28 X 540 = 65491.2 kcal
Hence, Total heat required = 66822.3 + 65491.2 = 132313.5 kcal
Assuming 10% heat loss due to radiation, Hence Heat required = 1.1 X 1323 = 145544.85 kcal
Steam Required = 145544.85 / 525.6475 = 276.88 kg
Enthalpy of Feed = ∑ m.Cp.dt = (1994 X 0.386 + 127.28 X 1) X 5 = 4454.82 kcal
4. Energy Balance of Evaporator
Basis: 2 tons per day
Amount of P.E. present in feed = 2341.23 kg/day
The same amount is to be present in the liquor coming out of the evaporator.
Flow rate:
Total Flow rate (kg/hr) P.E Flow rate (kg/hr) Liquid Flow Rate (kg/hr)
Feed Solution 433.958 97.55 336.40
Thick Liquor 285.54 97.55 167.90
Water + CH2O 148.418 168.5
evaporated
Pressure in atm Temperature in 0F

Inlet stream 2 248
Outlet stream 1 221
Total Temp Drop:
∆T = Th – Tc
Th = 248 0F
Tc = (212 + 192) / 2 = 46 0F
Assume B.P.R. = 1 0F
Effective Temp Drop = 46 – 1 = 45 0F
mf = 10415 kg/day = 433.958 kg/hr
Hf= 298(298+90)m.Cp.dt
= (2341.23 X 0.36 + 1783 X .26 + 284.67 X .5760) X (90) = 679708.053 kcal/day
= 28321.17 kg/hr
Hproduct= 298398m.Cp.dt
Hproduct = (2341.23 X 0.38 + 2727.94 X 1 + 1783.94 X 0.269) X 100 = 411152.4 kcal/day
= 17131.39 kcal/hr
V = 3561.89 kg/day = 148.41 kg/hr
Latent heat of water at 1000C = 1150.4 Btu/hr
Hs = 1162.5 Btu/lb = 645.26 Kcal/kg
(Sensible heat + latent heat at 248 0F from Mc Cabe Appendix 6)
Let, mc = X kg/hr
Hc = 188.17 Btu/lb = 105.64 Kcal/kg (sensible heat for condensate at 221 0F)
The Enthalpy Balance Equation is given by: mf.Hf + ms.Hs = (mf – m)Hv + mc.Hc + ms.Hc
28321.17 + X.(645.26) = 17131.35 + 94768.24 + X.(105.64)
Hence, X = 154.8 kg/hr = 3717.20 kg/hr
Steam Economy = (kg water evaporated) / ( kg of steam required) = 3561.89/3717.2 = 0.95

Design of Equipment
Design of Neutralization Tank

(ref: Unit operations of chemical engineering: Mc Cabe)
In the neutralization tank formic acid is added to neutralize the excess alkali and to effect
removal of the metallic ion of the condensing agent. Formic cid maybe added to reduce pH of
solution to 7.8 to 8 and subsequently to remove the sodium ion present as sodium formate.
Selection of Equipment: The reaction is carried out in a cylindrical vessel provided with the
drain value at the bottom for the gravity flow. To achieve the good mixing of the reactants, a 6
bladed turbine agitator is provided.
Selection of MOC: In the selection of material of construction for any vessel, the factors to be
considered are initial lost, corrosive action of the reactants, cost of replacement, maintenance and
probable life. Taking the corrosive action of NaOH into account, the best choice to use is
Stainless Steel.
Mechanical Design Calculation: Since the kinetic data is not available, we have to design the
neutralization tank on the basis on reactants mass.
Material in Neutralization Tank Weight in kgs Density at 25 0C (g/cc)

Pentaerythritol 2341.3 1.396
HCOONa 1783.94 1.274
H2O 6005.16 1
HCHO 284.67 1.029
1g/cc = 1 kg/ltr
Average density of reaction mass at 300C = 1.1747 g/cc
Total volume of reaction mass = 10415/1.1747 = 8866.09 ltr/day
Assume residence time in neutralization tank as 2 hours.
Residence time, T = V/ vo
vo = 8866.09 / 24 = 369.42 ltr/hr = 369420 c.c/hr
V = ( ∏ D2 H ) / 4 { D = Diameter of Tank, H = Height of Tank}
Assume H/D = 1.25
Hence, V = [ ∏ D2 (1.25D) ] / 4
D3 = (4V) / ( 3.14 X 1.25) = (4 X 369420) / (3.14 X 1.25) = 376478.98.09 c.c/hr
D = 71.89 cm = 72 cm
H = 1.25D = 1.25 X 72 = 90cm
Shell Thickness: In the tank the pressure is atmospheric, hence the maximum pressure will at the
bottom due to the hydraulic pressure. Taking maximum design pressure to be 20 psi.
Shell Thickness ts = (Pd/2fE) + C
Where, ts = Shell Thickness
f = Allowable stress in psi
E = Joint efficiency
C = Corrosion Allowance
ts = [((20 X 72) / (2 X 20000 X 0.8))+ 0.005] X 2.54
ts = 0.127 cm = 1.27mm
Take shell thickness as 5mm.
We can take thickness of bottom and head equal to shaft i.e. 5mm. Select the elliptical head and
bottom with major to minor axis ratio to be 2. i.e. a = 2b
Inside depth, b = a/2 = I.D/4 = 72/4 = 18cm
Hence, V = ( ∏ / 4 ) X 722 X 90 + ( ∏ X 723 ) / 12 = 464.151 ltr
Space allowance
= [ ( 464.151 – 369.4) / 369.4 ] X 100 = 25 %
Volume of incoming feed – Volume of Head
= ( ∏ / 4 ) X D2 ( h1 – b )
= 369420 – (∏ D3) / 24 = ( ∏ / 4 ) X D2 ( h1 – b )
Hence, h1 = 96.72 cm
This is the height of the liquid level from bottom of elliptical head.
Design of Agitator: (ref: Unit operations of chemical engineering: Mc Cabe)
Calculations are done in order to obtain Power in HP.
In order to provide better mixing, 6 blade turbine agitator is the best choice.
Let diameter of agitator = 0.6 ( Diameter of Tank)
Da = 0.6 X 72 = 43.2 cm
Speed of Agitator = 75rpm
n = 75/60 = 1.25
Assume viscosity of slurry = 5cp
A.V density of slurry = 1.1747 kg/ltr
Nre = (Da X n X ρ) / μ = (43.2)2 X 1.25 X 1.174 / 60 = 54774.144
Nfr = (n2 X Da) / a = 1.252 X 43.2 / 980 = 0.068
From table, a = 1, b = 40
m = ( a - log Nre ) / b = ( 1 – log54774.144) / 40 = -0.0935
P = ((Nfr)m n3Da5) / gc = (0.068)-0.0935 X 1.253 X (43.2/30.48)5 X 1.17 X 62 / 32.17
43.2 cm = 43.2 / 30.8 ft
1.17 kg/ltr = 1.17 X 62 (lb/ft2)
9.81 m/s2 = 32.17 (ft/s2)

Hence, P = 31.95 ft.lbf = 0.05 HP ̴ 1HP
Taking frictional losses into account, P = 2 HP
Shaft diameter = (53.3 X 2/75)0.33 = 1.123cm ̴ 2cm
Torque in shaft = (2 X 550) / (2πn) = (2 X 550) / ( 2 X 3.14 X 1.25 ) = 140 ft.lb
Standard Dimensions for Nozzle requirement:
Charging Hole 125 cm diameter

Man Hole 200 X 250 mm diameter
Stuffing Box 100 mm diameter
Drain Value 150 mm diameter
Specification sheet for neutralization tank:
Number Required 1
Type Cylindrical, closed tank with turbine type
agitator
Normal Capacity 370 ltr
Critical Dimension Overall height = 90cm
Inside diameter = 72 cm
Shell thickness = 5cm

Material of construction Stainless steel
Baffles No
Agitator Turbine type
Number of blades = 6
Diameter = 44cm
Rpm = 75
Shaft diameter = 2cm
Material of Construction = Carbon steel

Nozzles Feed charge nozzle = 125 m diameter
Man hole = 200 X 50 mm
Stuffing box stump = 100 mm diameter
Drain value = 150 mm diameter

Supports 4 lug supports, supported at a height of 3m for
gravity flow
Cost Rs 2,00,00 (Approx)
To evaporate 1 lb of water, steam required is about 1 to 1.3 lb or 1000 to 1200 Btu heat is
required.
Evaporator Design Report
Circulation and heat transfer in this type of evaporator is strongly affected by the liquid level as
indicated by an external gauge glass, which is only about half way of the tube. Slight reduction
in level below the optimum results in incomplete wetting of the tube walls with a consequent
increase in tendency to foul and causes rapid reduction in capacity. When this type of evaporator
is used with a liquid that can deposit scale, it is customary to operate with the liquid level
appreciably higher than the optimum level which is above the top tube sheet.
Advantages of Short Tube Vertical Evaporator:
• High heat transfer coefficient
• Low head room
• Easy mechanical descaling
• Relatively inexpensive
• Mild scaling solution can be used for mechanical cleaning as the tubes are short and large
in diameter
• Crystalline products can be removed using the agitator
Procedure followed in design of evaporator assembly: (ref: Unit operations of chemical
engineering: Mc Cabe)
The liquid Flowrate coming out of the evaporator is calculated using material balance. Since the
inlet steam pressure is known, a certain volume is assumed in the evaporator to find the
corresponding temperature for saturated steam. Using this value the total temperature difference
in the evaporator system can be calculated.
The energy balance equations for the evaporator are used in order to calculate the heat duty.
Taking the ud values from Mc Cabe, the total heat transfer area for the evaporator is calculated.
By manipulating the temperature drop appropriate area is calculated. For this calculated area,
tubes requirement for required heat duty is calculated.
Ref: Unit operations of chemical engineering, McCabe.

Q = U.A.∆T
Q = 1316857.143 Kcal/hr
Q = 1316857.143 X 0.252 = 331848 Btu/hr
U = 160 Btu/hr.ft2.0F Ref: Unit operations of chemical engineering, McCabe.
∆T = 45 0F
Hence, A = (331848) / (45 X 160) = 46.09 ft2
For Sheet Diameter: C/S Area of one tube = (π/4).d2.l = (3.14/4) X (2.2)2 X (48) = 182.463 in2
From McCabe, 30% of A is the area of downcomer = 182.463 X 0.3 = 54.4 in2
(π/4).d2.= 54.4 in2
Hence, d ≈ 8 inches
Length & Number of tubes: in standard short tube evaporators the length varies from 4 to 8 ft
and the diameter is around 2 to 4 inches. In this case, the length is assumed as 4ft and diameter as
2 inches.
Outer area of each tube = π.do.l = 3.14 X (2.2/12) X 4 = 2.1 ft2
Number of tubes required = 46.09/2.1 = 22.2 tubes
Hence we can take 22 to 24 tubes.
A staggered arrangement is used as it permits higher tube accommodation, for a given distance
between the tubes. From the approximate calculations, the shell inside diameter is taken as 21.2
inches.
Thickness of Shell = [(P.d) / (2.f.E) ] + Corrosion Allowance
= (30 X 21.2)/(2 X 0.8 X 3312.5) + 0.08 = 0.2 inches ̴ minimum
Hence Outer Diameter = 21.2 + 0.2 + 0.2 = 21.6 inches
Length of the evaporator is proportioned with respect to the length of tubes.
Design of evaporator and its accessories: The standard evaporator consists of a vertical
cylinder with calendria across which the heat exchange takes place. The cylindrical body
terminates at the top in a “save all”, the objective of which is to separate the liquid droplets
which maybe entrained with the vapor from the solution. Previously the evaporator body was
fabricated with cast iron; however more recently fabrication using steel plate is becoming more
common.
Height of the Vessel: The space above the tubular calendria represents the greater part of the
volume taken up by the equipment. The objective is to diminish the risk of entrainment of
droplets of solution projected by boiling. Various MOC used are as follows:
Part Old Modern Special

Shell Steel Bronze Mild Steel Stainless Steel
Tubes Brass, Cast Iron Mild Steel -
The height of the cylindrical portion above the steel plates is 1.5 to 2 times the length of the tube.
Calendria: It is the continuation of the shell or body of the evaporator. It is often fixed to the
shell. The bore of the holes provided in the tube plate is about 1/32 inch greater than the outer
diameter of the tubes. Vertical baffles are often placed in the calendria with the object of
compelling the steam to follow a certain path.

Center Well (Downcomer): The calendria is generally designed with a wide tube or center wall.
Solution which has been projected over the top tube plate is returned to the bottom by the
downcomer. This center well is often used to collect the concentrated solution in order to transfer
it from vessel to the other.
Air source for condenser: Air introduced into the condensers comes from various sources such
as air contained in the heating system, air introduced in the cold rejection water, air entering by
leakage.
Specification sheet of evaporator:
Number Required 1
Type Short tube, vertical calendria type evaporator
Normal Capacity 328.25 ltr/hr
Working Pressure 2 atm
Critical Dimension Overall height = 220 inches
Inside diameter of Shell = 21.2 inches
Inside diameter of tube = 2 inches
Thickness of shell = 0.2 inches
Thickness of tube = 0.1 inches
Diameter of downcomer = 3 inches
Length of tube = 48 inches
Number of tubes = 22 to 24
Material of construction Stainless steel
Baffles As per requirement
Nozzles or jet stream At steam inlet to increase velocity
Cost Rs 6,00,000(Approx)
List of Major Equipments
1. Reactor
Number Required 1
Type S.S. jacketed cylindrical type reaction vessel
with anchor type agitator.

Capacity of Jacket 890 gallon/hr
Operating conditions P = 1atm, T = 30 0C
Overall dimensions D = 90cm, H = 110cm
Material Of Construction Stainless Steel
Accessories and fittings Thermometer pocket, safety valve,
observation glass assembly, pressure gauge,
manhole etc.
Heat transmitting surface 4 square meter.
Agitator type Anchor type with explosion proof motor
Method of drive: 50 RPM
Electrical Motor Voltage: 415 V
H.P = 7.5, Croft Ratio = 30:1

Cost Rs. 4,00,000 (Approx)
2. Neutralizing Tank
Number Required 1
Type Vertical Cylindrical round bottom tank
Dimensions D = 72cm, H = 90cm, Thickness = 5mm
MOC Stainless Steel
Agitator Turbine type, 6 bladed
Motor speed: 75 RPM, H.P = 3,Voltage = 415 V

Supports Supported at 3m from bottom with 4 legs
3. Centrifuge
Number Required 5
Type Basket Type
Cake Capacity 400 kg/ltr
Overall Dimensions Basket = 60cm I.D , Depth = 30cm,
Outer Case = 61cm I.D.

MOC Basket of S.S plate outer cage lined with S.S
sheet filer of asbestos

Drive Motor H.P = 3, Speed = 1400 RPM, Voltage = 460 V
4. Dryer
Number Required 1
Type Counter current rotary dryer
Normal capacity 150 kg/hr
Dimensions & other details L = 12.5 ft, D = 2.5 ft, Speed = 5 RPM, H.P = 10
Entering Feed Temp = 30 0C
Outgoing Temp = 90 0C
Temp of entering steam = 120 0C

MOC Stainless Steel
5. Evaporator
Number Required 1
Type Short tube calendria type
Normal capacity 1600 ltr
Dimensions & other details D = 55cm, Ht = 550 cm, Shell thickness = 5cm
No of tubes = 24, Ht of tube = 120cm,
D of tube = 50cm, D of Downcomer = 15cm,
thickness of downcomer wall = 5mm, H.P = 10

MOC Stainless Steel
6. Evaporator Crystallizer
Duty To evaporate water from the filtrate and hence

to produce super-saturation with respect to
sodium formate and finally to produce crystals
of HCOONa
No. Required 1
Type Single effect evaporator crystallizer with pump
motor assembly. Heat exchanger vacuum pump
crystallizer with screen.

Capacity 200 ltr/hr
Temperature 100 0C
Pump To handle 200 ltr/hr centrifugal pump
7. Holding Tank
Number Required 2
Type Cylindrical type
Dimensions D = 60cm , H = 75 cm
MOC Stainless Steel
Cost Rs 50,000 (Approx)
8. Pumps
Number Required 8
Type Centrifugal
Normal Capacity 15 Gallons per minute
Drive Motor 3 H.P
MOC Stainless Steel
Cost Rs 50,000 (Approx)
9. Boiler
Duty To produce the steam required in holding tank
to keep the reaction mixture in liquid form.

Number Required 1
Type Vaporax boiler forced circulation coil
Capacity 500 kg/hr
Maximum Pressure 30 p.s.i
Water inlet temperature 30 0C
Firing Liquid Furnace oil
Accessories and mountings Water level indicator, Feed check valve,
Safety valve to control allowable pressure,
Pressure gauge, fusible plug, blow off valve,
Feed pump.
Instrumental process control & precautions
Controllers are gaining utmost importance in industries due to their efficiency, compactness,
response and hazard control capability. These advantages of automatic systems outweigh their
disadvantage of high cost.

Instruments are used for monitoring key process variables during plant operations. Process
variables depend on physical and chemical conditions, which vary with time. To control the
product quality it is necessary that different process variables like temperature and pressure are
maintained to prefix values. Fully automatic plant gives uniform products, avoids accidents and
minimizes the cost of labor; however it causes an increase in the initial cost of the project. the
present project is operated on batch basis and requires moderate capital investment.
Process control and automation together with their instrumentation can be considered as the
mechanical brain and nerves of modern chemical processes. However automatic control is highly
expensive. As far as the current plant is concerned no automation is recommended except for a
temperature controller. The temperature controller is used to control and stop the reaction. Also
the pH in neutralizer is maintained using a controller.
For temperature measurements of the reactor, thermo couples type measuring services are used.
One pressure gauge is also used for the reactor for safety purposes. Various values are provided
in pipe lines for manually controlling the quantity and flow rates of liquids. As the process is
continuous, precise control is needed.

Selection of location & plant layout
One of the most important parts of the final planning is the site location. Careful selection and
engineering research is necessary for attaining the advantage of the process and development
work. Factors contributing towards final site location are as follows:
• Raw material supply: Raw material should be cheaply and regularly available. Plant site
near to the raw material source permits considerable reduction in transportation and
storage charges.
• Market: Plant location near to the market reduces the cost of product distribution and
shipping time. If the plant is not situated near to the market for its final product, quick
and cheap transportation facilities should be available.
• Power and fuel supply: Electricity and fuel should be available regularly otherwise the
production may cease.
• Water supply: Process industries require water for processing, cooling, steam generation.
When an industry requires large amounts of water it should be located at areas with
constant water supply.
• Climate: Weather has a serious effect on the economic operation of a plant. The
temperature and humidity should be favorable for human body. Pentaerythritol reacts
with oxidizing agents on heating; hence oxidizing atmosphere should be avoided.
• Transportation: Waterways, railways and highways are the common means of
transportation. These services should be available near the plant for cheap and quick
transportation.
• Labor supply: Availability of labor at stable pay rates should be considered. The other
factors that need to be considered are the intelligence, stability, efficiency of the labor for
economic planning.
• Taxes and regulation laws: State and local tax rates on property, income, building codes,
restrictions on transportation are some of the factors which need to considered while
zeroing on the plant location.
• Site characteristics: Soil structure, availability of excess space for future expansions and
cost of the site should also be considered.
• Layout of the plant: The advantage of gravity flow should be taken if possible in order to
reduce the pumping cost. Water, steam and power should be available for cheap. Safety
of the site location should be considered in order to avoid hazards such as fire explosions.
The site should have a proper waste disposal system. Proper usage of the floor and
elevation space should be planned.
• Storage layout: Storage facilities should be provided in isolated or adjoining areas.
Arranging the storage of material so as to facilitate the easy handling is an important
factor which needs to be considered in storage layout.
• Equipment layout: While designing the plant layout ample of space should be provided to
all the equipments as they may need replacement, repairs and maintenance at regular time
intervals. If the equipments are placed very close to each other in a plant it raises the risk
of hazards due to interactions of processes. Gravity flow is preferable for viscous
material. In this case reaction mass and also the mass form evaporator.
Service and utilities
The main services required for the manufacturing of Pentaerythritol from formaldehyde and
acetaldehyde are water, steam and electricity.
• Process Water: It is required to prepare the solution as per requirements for:
I. Neutralization Reaction
II. Washing the Pentaerythritol cake
III. General services
The requirement can be served by municipal water supply or the industries own water supply is
recommended.
• Cooling Water: It is required to extract the exothermic heat of reaction to maintain the
required reaction temperature.
• Process Air: The heated air or steam is required in the plant as a heating medium in the
rotary dryer. It is a minor cost item for the process.
• Steam: Steam is required in the plant for heating and for evaporation of water in the
evaporator. It is also used in holding tanks to keep the reaction mixture in solution form.
• Electricity: When power requirement is high, industries should have their own power
stations. However in small scale industries, power is supplied by the state government
electricity board.
• Chilling Water: It is necessary to maintain the temperature at which Pentaerythritol is
crystallized in recovery plant.

Profitability & Cost of Project
A computation of all data relative to the cost of raw materials, land, buildings, labor and
supervision, equipment cost, taxes, insurance, interest etc. should be obtained by the designer on
an approximate pre-construction cost estimation basis. This data can be used for the actual
operation cost accounting if the project goes commercial. It gives the investors a rough estimate
of the total cost of the project and the payback period.
All the costs taken into account may vary according to the market demand and supply.
Basis: 2000kg/day and 300 workings days in a year.
COST ESTIMATION:
(A) Plant Equipment Cost:
Equipment Approximate Cost (Rs. In Lakhs)

Reactor 4
Neutralizer 3
Holding Tank (Quantity: 2) 2 (1 Lakh each)
Evaporator 6
Crystallizer 3
Dryer 8
Centrifuge (Quantity: 5) 15 (3 Lakhs each)
Conveyor 3
Pumps (Quantity: 10) 5 ( 0.5 Lakh each)
Total Cost (A) 49
(B) Recovery Equipment Cost:
Equipment Approximate Cost (Rs. In Lakhs)
Evaporator Crystallizer 6
Chiller 2
Press Filter 3
Centrifuge 3
Total Cost (B) 14
Total Equipment Cost (P.E.C) = Total Cost (A) + Total Cost (B)
= Rs. 49,00,000 +14,00,000 = Rs.63,00,000
Installation Equipment Cost (I.E.C) Rs 6,30,000 (10% of P.E.C)

Piping Cost (P.C) Rs 6,30,000 (10% of P.E.C)
Installation Cost (I.C) Rs 6,30,000 (10% of P.E.C)
Land Cost (2 Acres) Rs 40,00,000 (20000 ft2 X 500 Rs/ft2)
Building Rs. 1,00,00,000
Installation and Electric Fitting (I.E.F) Rs. 9,45,000 (15% of P.E.C)
Total Direct Cost (T.D.C) = I.E.C + P.C + I.C + L.C + Building + I.E.F
T.D.C = Rs. 1,68,35,000

Foundation cost Rs. 5,04,000 (8% of P.E.C)
Platform and support cost Rs. 4,41,000 (7% of P.E.C)
Erection of equipment cost Rs. 9,45,000 ( 15% of P.E.C)
Total cost Rs. 18,90,000
Total Installed Equipment cost (T.E.C) = 18,90,000 + P.E.C + T.D.C = 2,50,25,000
Instrumentation cost Rs. 9,45,000 (15% of P.E.C)

Electrical Insulation cost Rs. 6,30,000 (10% of P.E.C)
Land cost (1 acre) Rs. 20,00,000
Building yard improvement cost & utilities Rs. 2,52,000
Total cost of auxiliary items Rs. 38,27,000
Total physical plant cost (P.P.C) = Total cost of auxiliary items + T.E.C
= Rs. 2,88,52,000
Engineering and construction cost (E.C.C) 1 Rs. 14,42,600 (5% of P.P.C)

Direct Plant Cost (D.P.C) = P.P.C + E.C.C 3,02,98,000
Construction Fee 2 Rs. 6,05,960 (2% of P.P.C)
Contingencies 3 Rs. 30,29,800 (10% of D.P.C)
Total Fixed Investment (F.C.I) = 1+2+3+P.P.C Rs. 3,39,30,360
Working Capital Margin Money 4 Rs. 27,14,428 (8% of F.C.I)
Total Capital Investment (T.C.I) = F.C.I + 4 Rs. 3,66,44,788
Estimation of Product and Raw Material Cost
Formaldehyde = Rs.11/kg X 2350 kg/day X 300 days/yr = Rs. 77,55,000

Acetaldehyde = Rs. 36/kg X 757.7 kg/day X 300 days/yr = Rs. 81,81,000
NaOH (50%) = Rs. 9/kg X 1050 kg/day X 300 days/yr = Rs. 28,35,000
Formic Acid = Rs 9/kg X 415.84 kg/day X 300 days/yr = Rs. 11,22,768
Hence, Total Product and Raw Material Cost is
= 77,55,000 + 81,81,000 + 28,35,000 + 11,22,768 = Rs.1,98,93,768
Labor and Supervision Cost:
General Manager Rs 5 lakhs/annum 1

Engineers Rs. 6 lakhs/annum 2
Chemists Rs. 6 lakhs/annum 3
Clerks Rs. 3 lakhs/annum 3
Skilled Workers Rs. 10.8 lakhs/annum 18 (Rs. 5000/month each)
Semi-skilled Workers Rs. 10.08 lakhs/annum 21 (Rs. 4000/month each)
Unskilled Workers Rs. 10.08 lakhs/annum 30 (Rs. 3000/month each)
Watchmen Rs. 1.44 lakhs/annum 3 (Rs. 4000/month each)
Total Direct Labor Cost Rs. 52.4 lakhs/annum
Utilities:
Cost of Power:
Equipments Power in H.P Quantity

Reactor 7.5 1
Neutralizer 3
Centrifuge 15 (3 H.P each)
Dryer 10
Evaporator 10
Crystallizer 5
Pumps 30 (3 H.P each)
Boilers 10
Lightings, Blowers, 40
Air compressor, vacuum system

Chiller (Recovery equipment) 20
Crystallizer (Recovery equipment) 10
Elevator (Recovery equipment) 3
Filter Press (Recovery equipment) 10
Conveyor (Recovery equipment) 3
Centrifuge (Recovery equipment) 3
Total Power Required 179.6 ≈180
Calculation:
Load 180 KVA

Power Factor 180 KVA X 0.9 162 KVA
Maximum Demand 162 X 0.8 129.6 KVA
(80% of operating load)

Diversity Factor for batch 129.6 KVA X 0.4 51.84 KVA
Total Cost of Power = 51.84 X 0.9 KWHR x 300 days X 24 hrs X 5 Rs/Unit KWHR
= 16.796 lakhs/yr ≈ 16.8 lakhs/yr
Cost of Steam:
Equipment Steam required in kg/day

Evaporator 3800
Dryer 290
Total steam required 4090
Steam required per year = 4090 kg/day X 300 days/yr = 12,27,000 kg/yr
Amount of furnace oil required = 12,27,000 / 13 = 94384.615 kg/yr
Cost of furnace oil to produce steam required
= 94384.615 kg/yr X 16 rs/kg furnace oil = 15.10 lakhs/yr
Cost of water: Water required = 40 m3/day X 300 days/yr = 1200m3/year

Total cost of water = 1200m3/year X 20 rs/m3 = 2.4 lakhs/year
Cost of effluent treatment operation plant = Rs 1.69 lakhs/yr
Utility Cost
Total cost of Power required Rs. 16.8 Lakhs/year

Cost of furnace oil to produce steam required Rs. 15.10 Lakhs/year
Total cost of water Rs. 2.4 Lakhs/year
Cost of effluent treatment operation plant Rs. 1.70 Lakhs/year
Total utility cost Rs. 36 Lakhs/year
Fix charges
Maintenance a Rs. 3 Lakhs/year

Overhead b 10.5 Lakhs/year (20% of D.LC)
Quality control lab & technical assistance c Rs. 5.2 Lakhs/year (10% of D.L.C)
Depreciation cost of 1st year d1 Rs. 40.716 Lakhs/year (12% of F.C.I)
Depreciation cost of each additional year d2 Rs.33.9036 Lakhs/year (10% of F.C.I)
Interest on total investment e Rs. 16.965 Lakhs/year (5% of F.C.I)
Insurance f Rs. 6.786 Lakhs/year (2% of F.C.I)
Total fix charges for 1st year a+b+c+d1+e+f Rs. 83.167 Lakhs/year
Total fix charges for additional year a+b+c+d1+e+f Rs. 76.35 Lakhs/year
Product sales value, Penterythritol = 72 Rs/kg X 2000 kg/day X 300 days/yr= 432 lakhs/year
General expenses, sales, research and development = 2% of 432lakhs = 8.64 lakhs/year

g General expenses, sales, r and d Rs. 8.64 lakhs/year
x Total raw material cost Rs. 198.93768 lakhs/year
y Total direct labor cost (D.L.C) Rs. 52.4 lakhs/year
z Utilities Rs. 36 lakhs/year
F1 Total fix charges for 1st year Rs. 83.167 Lakhs/year
F2 Total fix charges for additional year Rs. 76.35 Lakhs/year
Total manufacturing cost for 1st year (g+x+y+z+F1) 379.14 lakhs
Total manufacturing cost for additional year (g+x+y+z+F2) 372.32 lakhs
Sodium formate recovery (Bypdt) = 15 rs/kg X 1700 kg/day X 300 days/year = Rs. 76.5 lakhs
Total sales of P.E. + sodium formate = 432 + 76.5 = 508.5 lakhs
Sales, Profit & Year
1st year Additional year

x Total sales of P.E. + sodium formate 508.5 lakhs 508.5 lakhs
y Total manufacturing cost 379.14 lakhs 372.32 lakhs
z Gross Profit (x – y) 129.36 lakhs 136.18 lakhs
IT Income tax (35% of Gross Profit) 45.27 lakhs 47.66 lakhs
Net Profit (z – IT) 84.08 lakhs 88.52 lakhs
Payout Period=1+TC.I-Net Profit for 1st YearNet Profit for additional Year
Payout Period=1+366.4478-84.0888.52
Payout Period = 4.1898 ≈4.2 years

Conclusion
Pentaerythritol is produced using formaldehyde and acetaldehyde using acids instead of soda-ash
as it is more economical.
Annual Output: 600 tons
Operation: 3 shifts (8 hours each), 300 working days/year.
Basic: 2000 Kg of P.E. per day
Required Materials:
 Formaldehyde (37%) – 6350.00 kg
 Acetaldehyde (99%) – 765.00 kg
 Sodium Hydroxide (50%) – 2100.00 kg
 Formic Acid(34.65%) – 1200.00 kg
Based on the production requirements, Material Balance for the entire process and Material
balance for individual equipments is carried out. Sodium Formate is separated from P.E in the
Sodium Formate recovery unit, where it is converted into Formic acid. Energy Balance and
Design of Equipments is studied based on which the requirements and cost of the equipments is
approximated. Cost Analysis helps in determining the pay-back period for the project which
works out to 4.2 years. For the Cost Analysis all the factors which contribute towards the total
expenditure of the project are considered.

References
Mc Ketta J.J., “Encyclopedia Of Chemical Processing and Design. Volume 5”
Perry R.H., “Chemical Engineering Hand Book”
Kirk, Othmer, “Concise Encyclopedia of Chemical Technology”
B.I. Bhatt, S.M. Vora, “Stoichiometry. 4th Edition”
McCabe W.L., Smith J.C., Harriot P., “Unit Operations of Chemical Engineering 5th Edition”
Treybal R.E., “Mass Transfer Operations”
Joshi M.V., “Process Equipment Design”
Peters M.S., Timmerhaus K.D., “Plant Design and Economics for Chemical Engineering 3rd
Edition”
Richardson, Coulson “Chemical Engineering Volume 6”
Bhageria Dye Chem Ltd, Vapi, Gujrat
Websites:
www.chemicalland.com
www.chemicalregister.com
www.pentaprocess.com
www.chemicalweekly.com
www.kanoriachem.com

Manufacturing of Pentaerythritol

Transféré par

Informations du document

Description originale:

Copyright

Formats disponibles

Partager ce document

Partager ou intégrer le document

Options de partage

Avez-vous trouvé ce document utile ?

Ce contenu est-il inapproprié ?

Droits d'auteur :

Formats disponibles

Manufacturing of Pentaerythritol

Transféré par

Droits d'auteur :

Formats disponibles

MANUFACTURING OF PENTAERYTHRITOL

An Industrial Engineering Project Report

Department of Industrial Engineering

An Industrial Engineering Project Report

By the Following Faculty Member:

without his support.

required for Material Balance, Energy Balance and Cost Estimation.

Physical and chemical properties_______________________________________________________7

Design of Neutralization Tank__________________________________________________________34

Evaporator Design Report______________________________________________________________39

LIST OF MAJOR EQUIPMENTS___________________________________________45

INSTRUMENTAL PROCESS CONTROL & PRECAUTIONS________________50

SELECTION OF LOCATION & PLANT LAYOUT___________________________51

SERVICE AND UTILITIES_________________________________________________53

PROFITABILITY & COST OF PROJECT____________________________________54

to show that there are 5 carbon atoms in the molecules.

structure of the molecules. It is an optically inactive compound, resembling cane sugar in

in hot water, and has only a limited solubility in organic liquids.

an explosive substance. Purified pentaerythritol (P.E) is used as a surface coolant. It is also in

manufacturing mainly because of its desirable characteristics and price stability.

Pentaerythritol sublimes on heating under reduced pressure. It is non hygroscopic, nonvolatile,

2. Sodium Hydroxide (NaOH)

5. Sodium Formate (HCOONa)

Solvent Temp 0C Solubility Temp 0C Solubility

g/100gms g/100gms solvent

chromic and nitric acid; it degrades the polyols to CO2.

the carbon chain.

ethyl sulfate with the appropriate alkyl chloride and alkali.

which is an explosive substance.

Grades and Analysis

The analysis of technical pentaerythritol generally includes the following determination:

Technical pentaerythritol contains 85 to 90 % pentaerythritol and 10 to 15% polyhydric alcohol

• Dipentaerythritol: About 10 to 15 % in the technical grade of pentaerythritol. It is

separated from pentaerythritol by procedure based on differences in solubility in wither

• Tripentaerythritol: It is separated from pentaerythritol by fractional crystallization.

pentaerythritol by the use of different crystallization temperature. It is used in the

manufacture of formic acid.

to one molecule of acetaldehyde by the classic Aldol reaction.

1. CH3CHO + HCHO HOCH2-CH2CHO

2. HOCH2-CH2CHO + HCHO (HOCH2)2CHCHO

3. (HOCH2)2CHCHO + HCHO HOCH2

maintaining formaldehyde concentration at all times.

methanol can be minimized by avoiding high concentrations of formaldehyde and high

Pentaerythritol is isolated from reaction mixture by successive fractional crystallization.

hardness, durability, color stability and water resistance. It is usually employed in

combination with polyhydric alcohol such as glycerol to prevent premature gelatin.

varnishes, printing ink and adhesives.

3. Pentaerythritol can be converted to polyether. This compound is characterized by

excellent corrosion resistance and high dimensional stability. It is being used in

manufacturing of molding pipes, gears, valves and metal coating.

surface coating, films and fibers.

6. Pentaerythritol is used alone or in combinations with metal salts as heat stabilizers.

7. It is used in the manufacturing of pentaerythritol tetranitrate which is an explosive.

protect the substrate from fire.

9. Pentaerythritol tetranitrate (PETN) has characteristics similar to those of cyclonite and is

color, luster, chemical resistant properties as compared to trihydric alcohols such as

glycerin. They also dry faster than trihydric alcohols.

them improved plasticity and impact strength.

as emulsifiers in cosmetics, and as abrasives.

➢ Allied Resins and Chemicals Ltd. (India)

➢ Asian Paints (India)

➢ Kanoria Chemicals and Industries Limited. KCIL Group (India)

➢ Perstorp Aegis Chemicals Pvt. Ltd. (India)