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02.2 - HDPE Slurry Loop Process Technology
02.2 - HDPE Slurry Loop Process Technology
1935: In the same conditions , but under control this time, production of 8
grams of LDPE,
PE Types
Markets
Pipe Roto-molding Blow molding Other Extrusion Injection Film Coating Other
In WE 7% 1% 16% 6% 12% 52% 4% 2%
Recycle gas
comonomer Flash
Vent
Reactor
Degas
Section
-sing
Nitrogen
Catalyst
cocatalyst
Additives
Purification
Extrusion / Pelletizing
C
2
Hydrogenation-
reactor
H
2
To ethylene dryers
catalyst
Safety aspects:
Heat released at initial saturation with
hydrocarbons Ethylene dryer Ethylene dryer
Hexene
Distillation
Column
Steam
Kettle-accumulator
Degassed hexene
Hexene degassing
Accumulated moisture due to unloading procedures or light
hydrocarbons
Safety aspects : Unloading procedure of utmost importance
Cooling water
To flare
TCV
Hydrogenation reactor
Steam
Storage sphere
1
1
1 Distillation column
1
iC4
1
Fresh hydrogen Cooling water
Steam Reboiler
Cooling water
Degassed isobutane
C4 storage
Safety aspects:
MOC :
(composition, accumulation,…)
Dryer bed
Adsorption on 13X (molecular sieve – To flare To flare
zeolite)
Polar components (H2O, CO, CO2)
Safety aspects:
Isobutane dryer Isobutane dryer
Heat released at initial saturation with
hydrocarbons Nitrogen Dried isobutane
Link between electrical heater and
potential source of hydrocarbons
Safety aspect:
▪Chromium catalyst is
carcinogenic
▪External spills to be
prevented (special
sintered filtering devices)
Risk perception as a function of habit :
“complacency”
CONSIGNES D'ACTIVATION TYPE : TEQ pour grades 38140 - 34150 - Date : 03.03.2005 - REV. 0
Température Débit
CHARGE ( ° C) (Nm³/h)
C25305 1 fût = 50 kg
Terhel 963 175 kg
635 °C [1]
610°C
PROGRAMME
360°C
1. Type 2
300°C
270°C
2. T° palier (°C) 635
47.5
3. Durée palier (h) 6
[3] 41
4. Pente montée 1
(°C/min) 120°C
5. Débit 1 (Nm³/h) 47.5
Temps (h)
6. Débit 2 (Nm³/h) 41
3 7.3 8.3 9.3 15.3 18.5 19.5
7. T° chang. Débit 300
Azote Air Azote
Chargement Déchargement
Catalyst :
▪ Three types of catalysts
▪ Three types of catalyst dosing systems
Activity
Ziegler-Natta
or metallocene
catalyst
Chromium
catalyst
Industrial
Residence
time
Induction time
period
Chromium catalyst
HP FRESH
system:
▪ Good flow-ability
▪ Induction time MS4002
▪ High pressure iC4
▪ Catfeeders 1D 2D 3D
Safety aspects
D1 D2 D3 D4 D5 D6
▪ Chromium carcinogenic
▪ Only 1 manual isolation
valve between atmosphere
and high pressure iC4 of CHROMIUM
mudpot (human error) CATALYST XV4283D XV4285D
▪ Don’t be fooled by induction
TO
time! REACTOR
XV4114B XV4109B
MS441
PICA4118B
FLARE ▪ Nitrogen pressurized
PICB4118B
XV41419B ▪ Catalyst feeding by pumps
N2
XV4123B
M M
FIC4120B
PIC4125B
MS439 MS440A
XV4121B
M PD414I
Safety Aspects
PC405A/B/C/D
FRESH C4
FIC4178B FIC4168B
▪ Catalyst has no induction period
So must prevent too much
PIC4131B
M
catalyst from entering reactor at
PD414J
all times
XV4289E
XV4288E
GF432A/B PD414C/D
NAAR RxA
NAAR REACTOR ▪ So feed tank is at lower
MS442
pressure than reactor, pumps
have limited capacity
MS402O
constant concentration
▪ Catalyst feeding by pumps
GY402B3
▪ Solvent is Olefin free or fresh IC4
GY402B4
M PD414I
M
FIC4178B FIC4168B
FRESH C4
MS439B TIBAL
Safety Aspects
M
▪ Catalyst has no induction period
MS437B
PD414J
XV4281B
XV4282B
MS437
So must prevent too much catalyst
BRANDKAMER
RxB CAT.
PD414C/D
NAAR REACTOR B
from entering reactor at all times
FLARE
NAAR REACTOR A
So mixing vessel is at lower pressure
MS437B
STOOM
than reactor, pumps have limited
N2
COND
capacity
▪ Prevent reaction by residual ethylene
or hexene
▪ Catalyst is pyrophoric and water
reactive
HDPE slurry loop process 17
Catalyst and cocatalyst
N2 TIBAL 60%
PIC4037E
Co-catalyst:
MIN. OIL
▪ TIBAL & DEZ (organometallic compounds)
XV4000E
XV4077E
XV4004E
XV4005E
▪ Different concentrations 10,20,60% MS428E
XV4068E
HV4070E
▪ +/-25% pyrophoric limit
XV4047E XV4049E
XV4076E
XV4006E
XV4002E
XV4048E
Safety precautions:
GW425A GW425B
▪ Burning pit
XV4091E
▪ Firewalls separating vessels and pumps NAAR
MS428E
▪ Sloped floors
▪ Well ventilated area MS425C
XV4093E
▪ Welding procedures with fuse tube and M PD425E
Cooling Jacket
Steam
Recycle isobutane
Ethylene
Hexene
Hydrogen
Anti-fouling Cooler
Coolant
Drum
Killing gas Gas recovery
Flash
Tank
Settling Legs Flash
Circulation pump
Fresh isobutane PTO valves Line(s)
Catalyst
Finishing
▪ Closed loop
▪ Surge vessel Pressurized by nitrogen (only DP by pump)
feeds cata
cata
feeds
feeds cata
1400
1200
1000
800
600
400
1
10
19
28
37
46
55
64
73
82
91
100
109
118
127
136
145
154
163
172
181
190
199
208
HDPE slurry loop process 24
The reactor section: Cooling/Fouling
The reactor wall can be prone to fouling
Model
Measured
Safety aspects:
▪ Typically, the seal of a centrifugal pump is a weak part and is likely to leak
eventually
▪ Double or triple seal design
▪ Flushing fluids
Reactor homogeneity
10
34150
9
38140 42170
0% H2
% C2 OG
47100
8 0.15% H2
49090 53080
ER2245 0.3% H2
3802
46110 5203 0.6% H2
7
53140
6
5702
52021
5
85 90 95 100 105 110
RX temperature
Flash lines:
▪ Objective to flash all liquid while
maintaining the polymer
temperature at best degassing
temperature
▪ Consist in steam-jacketed pipes
▪ Low pressure steam
▪ Dynamics of the flashing
phenomenon, linked to the settling
legs, makes design difficult with
PTO valves
Safety aspects
▪ Prevent presence of liquid
isobutane after flash
▪ Very dangerous when liquid is
conveyed to extruder
Sam is the solubility in the amorphous fraction of the polymer, (mol/liter PEamorphous)
kam is the Henry’s law constant, (bar / l amorph. polymer / mol)
pi is the partial pressure of the gas around the polymer, (bar )
Arrhenius law
Sam = S0,am exp (-Ea / RT)
Ea Activation energy,(J.mol-1)
R Ideal Gas constant: 8.314 (J.mol-1.K-1)
T Temperature, (K)
Pigments (colour)
POWDER
+ additives
+ additives
(+ pigments)
PELLETS POWDER
(COMMERCIAL FLUFF)
Reaction
30% of plot space
Degassing
Extrusion
Blenders+Silos 70% of plot space
Conditioning
& Pallets storage
Gate
section
Discharge
section
Start-up
diverter Pelletizer
Gear
Pump Motor
(Option)
(KNT)
Diverting
Valve
Die Plate
Low-Pressure-Design structure
allows both low extrusion
pressure and high throughput.