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Design, fabrication AND testing of

prototype internal 80K helium gas


purification system for helium plant
By:
External Guide:
Mr. A. K. Sahu

Bhavin b. arya
(140280710001)

Internal Guide:
Prof. Dr. S.M.Mehta

Scientist/Engineer SG,

APME, LDCE,

Head LCPC division

Ahmedabad.

IPR, Gandhinagar.

OUTLINE OF PRESENTATION
Indigenous helium plant
Need of purification system
Objective of work
Design of Adsorber bed
1.
2.
3.
4.
5.
6.
7.

Selection of adsorbent
Find mass of Adsorbent required
Calculate the length and diameter of adsorber bed
Calculate MTZ length and breakthrough time
Dimension of vessel
Design of filter
Modelling

References
140280710001

Indigenous helium plant


Different operational system:
1. Compressor Oil removal system
2. Seven Heat exchanger
3. Three turbo expander
4. Two Purification system
5. Two J-T valve
6. Cold circulator
7. Dewar
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Fig.1 Process Flow Diagram for Liquid Helium Production (Courtesy: IPR)

NEED OF PURIFICATION SUYTEM


HRL is operated at purity better than 99.999 % by volume (10 PPM).
Although sufficient precautions impurity level sometimes can go as
high as 100 PPM.
high level of impurity enters cause condensation and choke the pipe
lines and valves leading to large pressure drop and inefficient
liquefaction process.
condensed and frozen impurity can destroy the blades of turbines of
HRL.

140280710001

Objective of project
Design, Fabricate & Testing Of Prototype Adsorber Bed of 80K.
Study of:
Helium plant and its components.
Design and analysis work done for 80 K purifier bed of actual size
Design:
The Adsorber beds,
Filter elements.
Instrumentations for adsorber bed test facility.
Experimental procedure.
Drawings required for manufacturing and assembly of different elements.
Perform the test, collect the data and analyse it. Repeat it for different type of charcoals.
Make a report of above work.
140280710001

Design of adsorber bed


Design of adsorber bed can carryout in following way1.
2.
3.
4.
5.

Selection of adsorbent
Find mass of Adsorbent required
Calculate the length and diameter of adsorber bed
Calculate breakthrough time and mass transfer zone(MTZ)
Optimize the length and diameter of adsorber bed on different parameter like MTZ,
breakthrough time, pressure drop, velocity, mass flow rate etc..
6. Design the filter

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1. Selection of adsorbent
ADSORPTION Adsorption has been defined as operation/process in which the gas molecules (the
adsorbate) stick to the surface of the solid (adsorbent) in one or more layer.
The Gas / liquid particles which are going to adsorb on a surface is called as Adsorbate.
The Material on which that fluid get adsorbed is called as Adsorbent.
Classified as
Physical Adsorption- weak intermolecular forces, called van der waals forces are
brought into play
Chemisorption- strong reaction between the solid and the gas

140280710001

1. Selection of adsorbent
Physical Adsorption

Chemisorption

Low heat of adsorption (<


2 or 3 times latent heat of
evaporation)
Non specific
Monolayer or Multilayer
No
dissociation
of
adsorbed species
Only
significant
at
relatively
low
temperatures
Rapid,
non-activated,
reversible
No
electron
transfer
although polarization of
sorbate may occur

High heat of adsorption (> 2


or 3 times latent heat of
evaporation)
Highly specific
Monolayer only
May involve dissociation.
Possible over a wide range of
temperature
Activated, may be slow and
irreversible
Electron transfer leading to
bond
formation
between
sorbate and surface.

Table: 1
Comparison of Physical Adsorption & Chemisorption (Courtesy: Randall F.
Barron, Cryogenic Systems ) 140280710001

1. Selection of adsorbent
Type of adsorber
Activated Carbons
Carbon Molecular Sieves
Silica gel
Activated Alumina
Zeolites
Fig.2 Schematic
representation
showing
the
frame
work
structure of (a)
zeolite A and (b)
zeolites X and Y
(Courtesy:
Ruthven 1984, p
13)
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Fig.3 Adsorbents (Courtesy: Adsorption


Technology and Design)
9

1. Selection of adsorbent
Required properties of Adsorbent

High adsorption capacity

High surface area per unit mass

Regeneration should be easy

Adsorption energy

Porosity

Availability

Economical

We will go with Coconut Shell based


charcoal

Adsorbent

BPL
(Bitumino
us
Pittsburg
h Lignite)
SC11
(coconut
shell
based)

Character
istic
Adsorptio
Adsorption
adsorptio
n
capacity
n energy
capacity
(mol/g)
Eo(kJ/mol
(kg/kg)
e)

Mass of
Adsorber
required
(kg)

Micropore
volume Wo
(m3/g)

Surface
Area
(m2/g)

0.000000
43

434.3
4

19.1

0.00153
7

0.0164

13.176

0.000000
4

547.9
4

23.5

0.00057
2

0.0440

4.909

0.0153

14.079

0.0330

6.541

0.0581

3.722

ACF

2.40E-07

Ajax

4.80E-07

KL3

2.44E-07

140280710001

240.0
0
480.0
0
681.5
6

20.909
21.21
29.7

0.00053
6
0.00115
39
0.00202
82

10

1. Selection of adsorbent
Classification of Pore sizes :
Table shows Pore size (Courtesy: Ruthven
1984, p 8)

Diameter(

Adsorbent
(Carbon)

Adsorbent Physical
Property :
Table
shows
Physical
Property
of
Adsorbents
(Courtesy: Perrys Chemical
Handbook)

Mesopore

Macropore

<2

2-50

>50

nm)

Shape Intern Bulk


of
al
densit
particle porosi
y,
s*
ty %
Kg/L

Sorpti
Surfac
Averag
ve
e
e pore
capaci
area,
diamet
ty,
Km2/k
er, nm
kg/kg
g
(dry)

~55
70-85

0.450.55
0.250.30
0.450.55
0.3-0.5
0.4-0.7

1-4
3

0.8-1.6
0.4-0.7

0.5
0.3

G,P

60-80

0.4-0.6

2-4

0.9-1.2

0.4

35-50

0.5-0.7

0.3-0.6

0.050.20

Shell based

60

Wood-based

~80

G,C

~80

G,C,P
G,P

Petroleumbased
Peat-based
Lignite based
Bituminous
coal-based
Carbon
molecular sieve
*

Micropore

Shapes:140280710001
C, cylindrical pellets;

0.8-1.6

0.4

0.8-1.8

~0.7

0.9-1.3 0.3-0.4

G, granular;

P, powder
11

1. Selection of adsorbent

Nitrogen isotherms at 77K (Courtesy: D. Martins, I. Catarino, D. Three selected adsorption isotherms for the gas nitrogen on the three
Lopes, I. Esteves, J.P. Mota, G. Bonffait, cryocoolers 16, p 568)
charcoal samples (Courtesy: D. Martins, I. Catarino, D. Lopes, I.
Esteves, J.P. Mota, G. Bonffait, cryocoolers 16, p 572).
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2. Mass of adsorbent

ISOTHERMS[2] - If a quantity q of a gas or vapor is adsorbed by a porous solid at constant


temperature and the steady state equilibrium partial pressure is p then the function q(p) is the
adsorption isotherm.
There are mainly six types of Adsorption Isotherms
1.

Microporous materials (e.g. Zeolite and Activated carbon)

2.

Non porous materials (e.g. Nonporous Alumina and Silica)

3.

Non porous materials and materials which have the weak


interaction between the adsorbate and adsorbent (e.g.
Graphite/water)

4.

Mesoporous materials (e.g. Mesoporous Alumina and


Silica)

5.

Porous materials and materials that have the weak


interaction between the adsorbate and adsorbent (e.g.
Activated carbon/water)

6.

Homogeneous surface materials (e.g. Graphite/Kr and


NaCl/Kr)
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2. Mass of adsorbent
Partial
pressure of Impurities

In Indigenous Helium Liquefaction Plant, the helium which is going to use should be pure and
is operated on 14bar pressure. But the helium supply contain the impurities like N2 , O2 & Ar
which is averaging to about 100 PPM.
So, the partial pressure of N2 impurity is given by,
P=*14 = 0.001093 bar.
Now, for the impurity, the saturated pressure at 80K is Po=1.3687bar.
So, Relative Pressure can be given by,
P/P0 = 0.001093/1.3687
=7.99 x 10-4
Same we can do for other impurities.
Partial Pressure of Oxygen = 9.32 x 10-4 bar
Partial Pressure of Argon =1.92 x 10-5 bar.140280710001

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2. Mass of adsorbent
Selection Of Calculation Model From Relative Pressure [3]
Relative

Mechanism

Calculation model

P/Po range
1x10-7 to 0.02

Micropore Filling

DFT, GCMC, HK, SF, DA, DR

0.01 to 0.1

Sub-Monolayer Formation

DR

0.05 to 0.3

Monolayer Complete

BET, Langmuir

> 0.1

Multilayer Formation

t-plot, S

> 0.35

Capillary Condensation

BJH, DH

0.1 to 0.5

Capillary Filling In M41S-Type

DFT, BJH

pressure

Materials

Relative pressure of impurities are in range of 10-04 so -DFT, GCMC, HK, SF, DA, and
DR Micropore Filling Mechanism should be use.
Now, we will go with DR model because for activated carbon DR equation is most
faithful[6].
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2. Mass of adsorbent
Dubinin-Radushkevick
(DR) equation for adsorption of mixture of gases [4]

,
for the mass flow rate of 30 g/s and 3 hour of operation with 100ppm of impurities
by putting the values we will get adsorption capacity around 0.044kg/kg.
0.044 kg of impurities per kg of carbon
Total mass of impurities to be adsorbed 0.21 kg.
So mass of adsorbent required is 4.90 kg
mass of adsorbent is 5 kg.

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3. Calculate the length and diameter of adsorber


bed
There is a pressure drop in the helium flow across the bad because of the adsorbent
material, carbon SC11 in this case. First thing we keep in mind while designing the bed is
that the pressure drop across the bed should not be more than 30 mbar.
The graph for pressure drop across the bed with various

Pressure drop vs Diameter


bed diameter is shown
So the diameter of bed should be more than 6 inch for
f(x) = 271.89 x^-2
pressure drop less than 30 mbar.
So initially taking diameter of bed 6 inch ( 0.1524 m)
Length can be calculated as follow,

Now, and taking D = 0.1524 m


L = 0.50 m
L/D = 3.27
Which we will be optimized further.
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4. Calculate MTZ length and breakthrough time

Fig -Mass transfer zone

Fig -Break through curve

Breakthrough time, tb is the time when the C/Co value becomes 0.01 (proposed outlet
impurity/ Inlet impurity) & saturated time, ts is the time when C/Co value becomes (1- proposed
outlet impurity/ Inlet impurity).
There are two model for prediction on MTZ length and breakthrough time
1. Rosen model
2. Axial dispersion model
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4. Calculate MTZ length and breakthrough time

Rosen model

The Rosen Model, developed by Rosen


Assistances in finding analytical results to adsorption
difficulties.
The basic assumptions for this model are as below
1. No Axial dispersion
2. Isothermal conditions and linear isotherm
3.Constant flow velocity & Constant effective
diffusivity

Axial dispersion model

The axial dispersion model is based on the concept


that the concentration front is dispersed by both
hydrodynamic and kinetic (finite transport rates) factors.
The equation for the axial dispersion model is given
by

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4. Calculate MTZ length and breakthrough time


DR theory

Adsorption capacity & Mass of Adsorbent (N2)


N2 adsorption capacity of coconut shell at 80K

f(x) = 0.02 ln(x) + 0.11

Nitrogen Isotherm at 80K for Coconut Shell Based Activated Charcoal


f(x) = 0.02 ln(x) + 0.38

henry constant

Characteristic Curve

f(x) = 0.45 ln(x) + 8.18

140280710001

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4. Calculate MTZ length and breakthrough time


DR theory

Adsorption capacity & Mass of Adsorbent (O2)

Oxygen Isotherm at 80K for Coconut Shell Based Activated Charcoal

O2 adsorption capacity of coconut shell at 80K


f(x) = 0.04 ln(x) + 0.14

f(x) = 0.04 ln(x) + 0.56

Characteristic curve

Henry constant
f(x) = 0.63 ln(x) + 11.6

140280710001

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4. Calculate MTZ length and breakthrough time


Rosen - Time vs C/Co
NITROGEN Rosen -Time Vs C/Co

From Breakthrough
curve

tb

ts

2901 s
0.4984 m
LMTZ = 0.167

MTZ

NITROGEN Axial Dispersion - C/Co vs. Time

From Break through


curve

@C/Co
0.99

tb

26501s

@C/Co 0.01

@C/Co
0.01

ts

39801s
0.167m

@C/Co 0.99

MTZ

m
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4. Calculate MTZ length and breakthrough time


OXYGEN Axial Dispersion - Time vs C/Co

OXYGEN Rosen - Time Vs C/Co

From Breakthrough
curve

ts
tb
MTZ

From Break through


curve

C/Co
0.99
C/Co
0.01

80601 s
1s
0.498 m

0.167 m
LMTZ =

tb

29001s

ts
MTZ

43701s
0.167m

C/Co
0.01
C/Co
0.99

Length of bed = 0.667


m

140280710001

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4. Calculate MTZ length and breakthrough time


We will consider axial dispersion model for our calculation. We are not getting required
result in a Rosen model because Rosen model is based on a basic assumption that there
will no axial dispersion in flow, which in not correct in this case because of the large
diameter.
MTZ length in both the case for nitrogen and oxygen is same as 0.167 m. The
breakthrough time for nitrogen and oxygen are around 7.3 hour and 8.0 hour, which are
far more than our time of operation. We can use that length and diameter bed for our test
facility.

140280710001

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4. Calculate MTZ length and breakthrough time


breakthrough curve for different mass flow rate

breakthrough curve for different charcoal Particle diameter

35 g/s
30 g/s
25 g/s
20 g/s
15 g/s

D=
0.0001
D=
0.0002

Breakthrough curve for different void fraction

Figure shows the breakthrough curve for different mass


flow rate, different particle diameter and different void fraction.
v=
0.48
v=
0.3
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5. DIMENSION OF VESSEL
Since the pressurized helium gas has to be passed through the adsorber vessel, it can be designed

considering a pressure vessel. According to the ASME Section VIII, the minimum thickness of the
cylindrical shell can be given by;
The minimum thickness for spherical shells,
hemispherical heads is given by;
Where
=design internal pressure,
Where
=inside diameter of shell,
= constant=
=allowable stress,
=weld efficiency.
The internal design pressure is 20 bar =2.0 MPa,

We have, hemispherical head thickness

Considering the material to be SS304L, so, Sa =120.6 0.74 mm < 0.280 inch
MPa,
Head thickness th = 0.280 inch
Taking weld efficiency ew =0.85
= 1.50 mm. For the safe side and market availability
we take pipe of NSP-6 with outer diameter 6.625
inch
Inner diameter 6.065 inch and,
140280710001
Thickness of vessel is 0.280 inch

26

6. Design of filter
Consider that Dp is the particle diameter and w is the aperture of the mesh. Now from

Pythagoras theorem we have,

Mesh opening
For the present work, the charcoal dust that is carried with helium has particle size ranging from 30 microns.

So by using equation,

Particle dia. vs. mesh size

;
We have,
In 1 we have 25400 microns, so
Mesh = 25400/51 = 498~500.

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6. Design of filter
Filter
Operating Pressure
Operating Temperature
Density of He
Mass flow rate, m
Vol.Flow rate, Q
Operation time
Charcoal particle Dia,Dp
Aperture Size,Width, Opening, w
~
Diameter of wire, d
Pitch of the Mesh, P

14
80
8.2196
30
0.003649
3
10800
30
21
21
30
51

Mesh

498

~Mesh

550

Void

0.16

bar
K
Kg/m3
g/s
m3/s
Hr
Sec
microns
microns
microns
microns
microns

P Across Wire Screen


Viscosity of He
He flow rate,Q
Length, L
Diameter of Screen,Di
Pressure Drop, P

8.69E-6
0.003649
0.08
0.06
1514

Ns/m2
m3/s
m
m
Pa

15.14 mbar
Across Inlet Pipe
D
Pre. Drop mbar
Across Outlet Pipe
D
A
Pre. Drop mbar
Across Annular Space Area
Do
Aannular
Uannular
Pre.Drop
Pre.Drop mbar
Total P Drop

140280710001

0.0254 m
2.1344 mbar
0.0254 m
0.000506451 m2
2.1344 mbar
0.0765
0.00172
2.1141
18.36
0.1836
17.4670

m
m2
m/s
Pa
mbar
mbar

28

6. Design of filter
Cartridge Diameter Optimization

Length Optimization of Cartridge

Wire Diameter Optimization

Pipe Diameter Optimization

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29

6. modelling

F
ilter

Adsorber bed

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30

Design Data Prototype Adsorber Beds


Mass flow rate
Impurity
Design Pr.
Time of Operation
Mass of He supplied, mHe
Volume of He Supplied
Volume of Impurity Supplied

30
100
14
3
324
1839.34
0.1839

Aligibility for DR Eq.

DR Theory

Model Selected

Axial dispersion

tb

26501

ts

39801

MTZ Length=
Adsorber bed Dia
Total Length of bed

0.167
6.065
0.667

m
Inch
m

140280710001

g/s
PPM
bar
hr
Kg
m3
m3

31

Work will be carried out

Fabrication & Purchasing of Instruments for adsorber bed test facility.


Experimental procedure.
Perform the test, collect the data and analyse it.
Repeat it for different type of charcoals.
Documentation.

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References
1.

Douglas M. Ruthven, Principles of Adsorption and Adsorption Processes, John Wiley


& Sons, 1984.

2.

Roop Chand Bansal & Meenakshi Goyal, Activated Carbon Adsorption, CRC Press,
2005.

3.

S. Lowell, Joan E. Shields, Martin A. Thomas and Matthias Thommes,


Characterization of Porous Solids and Powders: Surface Area, Pore Size and Density,
by Kluwer Academic Publishers,
20048

4.

Quantachrome Instruments, Physisorption Methods and Techniques, Seminar JSD


II.ppt

5.

Ralph. T. Yang, Gas Separation by Adsorption Process, Imperial college Publication.

6.

Activated charcoal adsorption by r bansal and minaxi.

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Thank You

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