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VLE

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RE-REFINING OF USED LUBE OIL ,
DISTILLATION COLUMN INTERNALS
COMPANY PROFILE

• Fenix Process Technologies Pvt. Ltd. is a leader in process technologies,
offering a wide range of engineering solutions that serves the refining,
chemicals and petrochemical, Oil & Gas, pharmaceutical, dyes &
intermediates, aromatics & food industries.

• It has a vast industrial experience in the field of Process Design, Equipment
Design, Process Equipment Manufacturing, System integration, Plant Design,
Plant Modifications, Automation, Project Management and Process
Consultancy.
• It manufactures and export a vast range of Mass Transfer Equipment. The
range encompasses Distillation Systems, Absorption Systems and
Liquid-Liquid Extraction Systems.

• The Internals and accessories required for these Mass Transfer
Operations are all designed and manufactured by it: Structured
Packing, Random Packing, Distillation Tray, Tower
Internals , Accessories (condenser, reboiler, reflux drums, flash box
etc.), heat exchangers, mixers, reactors and so on.

• It also provides facilities for Pilot Trails and Case studies.
VAPOUR-LIQUID EQUILIBRIUM

• Vapour-liquid equilibrium is a condition where a liquid and
its vapour are in equilibrium with each other, a condition or a
state where the rate of evaporation equals to rate of
condensation on a molecular level.

• The main purpose of the experiment is to construct the
equilibrium curve at atmospheric pressure for a binary
mixture of Acetone-Water system.
EXPERIMENTAL SETUP
EQUIPMENT:
1.Equilibrium still
2.10 ml volumetric flask
3.2 ml Clip lock tubes OR Sample vials
4.Digital thermometer
5.Beakers
6.Syringe
`7.Gas chromatography instrument

CHEMICALS:
•Acetone
•Water
EXPERIMENTAL PROCEDURE:
•Prepare a mixture of 250 ml acetone and 60 ml water in a 500 ml
beaker.

•Feed the mixture in to the boiling pot.
•Switch on the heater and the digital thermometer & cooling water
supply to the condenser.

•Note down the temperature at which condensation begins.
•Take samples of the vapor distillate and liquid in the clip lock tubes at
different time intervals.
•The remaining distillate obtained is kept separately and add
40 ml of water in to the boiling pot for every sample collected.

•The procedure is repeated until the temperature is reached up
to the boiling point temperature of water, i.e.,100°c.

•The samples taken are analyzed in a gas chromatography
instrument and the compositions of water and acetone in
different sample are noted down.
OBSERVATIONS:

S.NO TIME TEMPERATURE (°C) REMARKS S.NO TIME TEMPERATURE (°C) REMARKS
TOP BOTTOM TOP BOTTOM
1 10:38 34 34 HEATER ON 19 12:42 73 81 CUT 7
2 10:43 35 36   20 12:47 68 80  
3 10:48 49 43   21 12:53 72 81  
4 10:53 53 47 CONDENSATI
22 13:42 80 92  
ON START
23 13:49 78 88 CUT 8
5 10:58 57 50 CUT 1
24 13:54 84 90  
6 11:03 59 56  
7 11:07 61 57 CUT 2 25 14:01 86 94 CUT 9
8 11:12 60 58   26 14:08 84 92  
9 11:17 60 58   27 14:13 87 94 CUT 10
10 11:20 62 59 CUT 3 28 14:20 84 93  
11 11:28 60 61   29 14:25 81 91  
12 11:33 61 62   30 14:31 87 94  
13 11:37 64 63 CUT 4
31 14:39 89 99 CUT 11
14 12:00 64 66 CUT 5
32 14:46 88 94  
15 12:13 64 69  
16 12:23 69 77 CUT 6 33 14:51 89 100  
17 12:27 68 75   34 14:56 90 100 CUT 12
18 12:32 67 73   35 15:02 96 97 CUT 13
Analysis from Gas chromatograph:
S.NO. TEMPEARTURE DISTILLATE COMPOSITION RESIDUE COMPOSITION
(°C) (%) (%)
WATER ACETONE WATER ACETONE

1 57 18.9841 80.6359 26.3796 73.0140
2 61 8.4750 91.4310 26.8845 72.3245
3 62 8.0901 91.8180 25.6440 74.0382
4 63 8.7885 91.0941 27.5207 72.2709
5 66 10..2121 89.7174    
6 69 13.1921 86.6813    
7 74 19.8444 80.0890 34.1312 65.8120
8 76 23.9594 75.9805    
9 86 51.6227 48.3229 55.1580 44.8421
10 87 68.5985 31.3665 62.4705 37.5295
11 89 84.7303 15.2696 66.2088 33.7912
12 91 90.5451 8.3151 72.1778 27.1413
13 95 73.7435 25.5217    

CALCULATIONS:
Antoine parameters:

  A B C
Water 8.07131 1730.63 233.7912
Acetone 7.6313 15566.69 273.419
Total pressure: Ptot = 760 mm of Hg
Partial pressure at saturation temperature T from Antoine equation:
logPsat = A-B/(T+C)
Using Raoult’s law:
Xacetone = Yacetone* Ptot/Psat

The obtained results are tabulated as:

S.NO. TEMPERATURE Pacetone (mm of Yacetone Xacetone
(°C) Hg)
1 57 775.845 0.806359 0.78980
2 61 884.074 0.914310 0.78599
3 62 912.968 0.918180 0.76433
4 63 942.626 0.910941 0.73445
5 66 1036.34 0.897174 0.65794
6 69 1137.47 0.866813 0.57916
7 74 1323.70 0.800890 0.45982
8 76 1404.75 0.759805 0.41107
9 86 1872.18 0.483229 0.19616
10 87 1925.05 0.313665 0.12366
11 89 2034.37 0.152696 0.05700
12 91 2148.60 0.831510 0.02941
13 95 2392.39 0.255217 0.08100
Graphical representation:
T vs. Yacetone , Xacetone :

T-x
T-y

Yacetone vs. Xacetone:

vapor- liquid
equilibrium curve
x=y line
APPLICATIONS

• VLE diagrams are used in the McCabe-Thiele method to
determine the equilibrium stages (or theoretical plates)
needed to distill a given composition binary feed mixture in
to one distillate and one bottom fraction.

• In the determination of activity coefficient for the low
pressure systems containing an ideal gas phase, but a non-
ideal liquid phase.
RE-REFINING OF USED LUBE OIL

LUBE OIL:
Lube oils are a blend of base oil and additives.
Typically lube oil contains 90% base oil (most often
petroleum fractions) and less than 10% additives.

RE-REFINING PROCESS
  The re-refining process restores used lube oil to its original
condition as base oil. The lubricating properties of the oil are
not compromised by use or re-refining.
Re-refining is an energy efficient and environmentally beneficial method
for managing used oil. Instead of burning the used oil, which releases
harmful emission into the atmosphere, re-refining conserves the base oil.
EXPERIMENTAL PROCESS

UTILITIES:
• Chiller
• Cooling Tower
• Vacuum pump
• Vertical thin film evaporator
• Thermic fluid ( Therminol) heater with circulation tank
STAGE 1:
DEHYDRATION ON VERTICAL THIN FILM EVAPORATOR

EXPERIMENTAL CONDITIONS
FEED: Used Oil
Thermic fluid temperature:120°C ,Vacuum:300 mmHg, Shaft rotation: 300 Rpm

Thermic fluid Set point(°C) Time Remarks
temperature(°C)
32 38 11:10 Heating of thermic
fluid is started.
68 70 11:20
90 90 11:30
91 90 11:40
95 98 11:50
100 105 12:00
120 119 12:10 Vacuum is given and
rotation is started.
120 120 12:20 Flow of feed is
started.
120 120 12:25
119 120 13:30 No distillate came
STAGE 2: DIESEL STRIPPING

FEED: Residue fraction from dehydration process
Thermic fluid temperature: 220°C, Vacuum: 3-4 torr, Shaft rotation: 300
Rpm
Thermic Set Time Remarks 171 179 11:50
fluid point(
temperatu °C) 181 185 12:00
re(°C)
46 49 10:30 Heating of thermic 191 199 12:10
fluid is started.
65 63 10:40 200 205 12:20

84 84 10:50 217 220 12:30

220 220 12:40 Vacuum is given and
99 97 11:00 rotation is started

115 118 11:10
220 220 13:30 Flow of feed is started.
131 134 11:20

220 220 14:15 200ml of distillate was
141 146 11:30
out
STAGE 3: ASPHALT REMOVAL
FEED: Residue fraction from Diesel stripping process
Thermic fluid temperature: 265°C, Vacuum: 3-4 torr, Shaft rotation: 300 Rpm

Thermic fluid Set point Time Remarks 237 238 14:00
temperature (°C) (°C)
34 35 10:45 Heating of thermic 241 245 14:10
fluid is started.
246 250 14:20
44 41 10:55
252 256 14:30
60 60 11:00
256 260 14:40

66 66 11:05 258 260 14:50

72 72 11:10 261 265 15:00 Vacuum is given
and rotation is
started.
86 86 11:15
263 265 15:10 Flow of feed is
started.
95 95 11:20 265 265 15:20

265 265 16:05 Feed off
105 105 11:30 150 ml of
distillate was out
STAGE 4: SOLVENT EXTRACTION

• FEED: The distillate from Asphalt removal process which
contains lube oil fractions.
• N-methyl pyrolidine (NMP) is added to the distillate obtained
from Asphalt removal process in 3:1 ratio.
• The NMP is an aromatic selective solvent which, in addition to
removing some colour and odour, is able to extract all unwanted
aromatic contaminants present in the paraffinic lubricating oil
fraction.
• The upper layer contains NMP and aromatics and lower layer
contains lubricating oil fraction.
• After solvent extraction using NMP as a solvent about 30 ml of
lube base oil has been recovered.
BENEFITS OF RE-REFININIG

•Reduce dependence on base oil imports saving foreign exchange.

•Prevent ground water contamination and pollution of surface
water.

•Preserve natural resources like coal and crude oil.

•Reduce sewage treatment costs.

•Eliminate improper burning of waste oil as fuel, which generate
toxic fumes and air pollution.
DISTILLATION COLUMN
INTERNALS
DISTILLATION:
A process in which a liquid or vapour mixture of two or
more substances is separated into its component fractions of
desired purity, by the application and removal of heat.

Distillation columns are made up of several components,
each of which is used either to transfer heat energy or
enhance mass transfer. A typical distillation contains several
major components.
 
TYPES OF VAPOUR-LIQUID CONTACT EQUIPMENT

Typical internal accessories include trays, packing, liquid distributors, redistributors, collectors, bed limiters, mist eliminators.

I.TRAYS
II.PACKINGS

Trays and packing are installed in the column for efficient vapour liquid contact.
TYPES OF VAPOUR-LIQUID CONTACT
EQUIPMENT

TRAYS PACKINGS

Tray columns can handle wide range Packed are more suitable for low
of gas and liquid flow rates. capacity operations
Trays are used for fouling liquid and For separating heat sensitive
for liquids with solid deposition, materials packed columns are useful.
even the tray is blocked up, it is
easier to clean it and manholes can
be provided over the plate.

The tray columns provide stage-wise Continuous counter current contact
contact. of vapor and liquid phases take
place.
Tray columns are more expensive. Packed columns are less expensive.
SIEVE TRAY FIXED VALVE TRAY

FLOATING VALVE TRAY BUBBLE CAP TRAY
I.TRAYS

The function of a Tray is
to felicitate contact
between the vapour
phase and liquid phase,
so that mass transfer
between the two phases
can take place.

Each tray is considered
as being made up of 3
sections:
•Weir
•Bubbling area
•Downcomer
II.PACKINGS:
• STRUCTURED PACKING (also called as stacked or arranged)
• RANDOM PACKING (also called dumped).

• A good packing material is one that provides a high surface area per volume
• The material of construction must provide a high liquid flow capacity through
it to ensure a uniform liquid layer (good wettability) as well as good
resistance to pressure .
STRUCTURED PACKING:

Structured Packings are of three types:
•Structured packing made of wire mesh
•Structured packing made of sheet metal
• Structured grid Packing
•RANDOM PACKING :
Random packings are small objects made from metals,
polymers, ceramics are dumped into the column.

Random packings have low pressure drop when compared to tray
columns.
Random packings are made of
•Metal
•Ceramic
•Plastic
Cylindrical rings P-Rings C-Rings

Saddle-Rings N-Rings
STRUCTURED PACKING RANDOM PACKING

More expensive but very efficient. Cheap and relatively efficient.

Useful for times when we don’t have Used if the packing is a consumable/
a lot of pressure drop to play with wearable packing that needs
.e.g ; vacuum service. replacing regularly.

For fouling liquid, it is impossible to Can be used for fouling liquids.
clean and often difficult to even get
out of the column.

It has more number of stages per It is cheaper, but will contain voids
packed height, which reduces the which may reduce structural
total height of the column required, performance. Also it has less number
thus reducing the cost of material in of stages per packed height, thus
construction. increasing the height of the column.
LIQUID DISTRIBUTORS AND REDISTRIBUTORS
Packing whether random or structured, serves the basic purpose of
providing intimate contact between vapor and liquid in mass
transfer operations. But for effective and efficient performance of
packing some peripherals are needed.

Liquid distributors serve the purpose of distributing liquid evenly
over the packing

CLASSIFICATION OF LIQUID DISTRIBUTORS:
Distributors are basically classified as

1.Pressure distributors
2.Gravity Distributors: a) Weir Type b)Orifice Plate Type
CHANNEL TYPE DISTRIBUTOR BAFFLE TYPE DISTRIBUTOR SPIRAL TYPE DISTRIBUTOR

CHIMNEY TYPE DISTRIBUTOR PAN TYPE DISTRIBUTOR PIPE TYPE DISTRIBUTOR

TROUGH TYPE DISTRIBUTOR SPRAY NOZZLE DISTRIBUTOR SPIDER TYPE DISTRIBUTOR
PACKING SUPPORTS

For large columns and heavy duty distillation columns, the static
weight of packed bed combined with liquid column is quite high.
Strong construction of packing support is needed.
BED LIMITERS

Bed limiters are installed directly above a packed bed in a
distillation column to prevent shifting of packing elements under
turbulent conditions of vapour and liquid.
MIST ELIMINATORS
Mist eliminator which helps in separation of liquid droplets from gas
stream which provide suitable foaming system with higher liquid
loading.

WIRE TYPE MIST ELIMINATORS
(Knitted mesh type, High efficiency mesh type)

VANE TYPE

Plain vane type Pocketed vane type Hook vane type
CONCLUSIONS:
An experiment on Vapor-Liquid equilibrium for a binary mixture of
acetone-water is conducted and T-xy diagram is generated. The xy data
obtained from vapor-liquid equilibrium condition can be correlated for the
generation of equilibrium curve in distillation .
 
Re-refining of used lube oil is done on a thin-film evaporator and used lube
oil is restored as base oil. After the entire five step operation is completed 30 ml
of lube base oil is recovered.

Column internals which include several internal accessories
like trays, packings, liquid distributors, bed limiters, mist
eliminators are used to enhance heat and mass transfer.
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