CA2498763A1 - Process and apparatus for separating diluent from polymer solids - Google Patents

Process and apparatus for separating diluent from polymer solids Download PDF

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Publication number
CA2498763A1
CA2498763A1 CA002498763A CA2498763A CA2498763A1 CA 2498763 A1 CA2498763 A1 CA 2498763A1 CA 002498763 A CA002498763 A CA 002498763A CA 2498763 A CA2498763 A CA 2498763A CA 2498763 A1 CA2498763 A1 CA 2498763A1
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CA
Canada
Prior art keywords
polymer solids
zone
intermediate pressure
diluent
chamber
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Granted
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CA002498763A
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French (fr)
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CA2498763C (en
Inventor
Thomas A. Reid
Scott E. Kufeld
John H. Tait
David H. Burns
Donald W. Verser
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Chevron Phillips Chemical Co LP
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Individual
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Publication of CA2498763A1 publication Critical patent/CA2498763A1/en
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Publication of CA2498763C publication Critical patent/CA2498763C/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00Post-polymerisation treatments
    • C08F6/001Removal of residual monomers by physical means
    • C08F6/003Removal of residual monomers by physical means from polymer solutions, suspensions, dispersions or emulsions without recovery of the polymer therefrom
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • B01J19/1812Tubular reactors
    • B01J19/1837Loop-type reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005Separating solid material from the gas/liquid stream
    • B01J8/007Separating solid material from the gas/liquid stream by sedimentation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/20Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F10/00Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00Post-polymerisation treatments
    • C08F6/24Treatment of polymer suspensions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/0061Controlling the level
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00743Feeding or discharging of solids
    • B01J2208/00761Discharging
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002Chemical plants
    • B01J2219/00004Scale aspects
    • B01J2219/00006Large-scale industrial plants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00245Avoiding undesirable reactions or side-effects
    • B01J2219/00254Formation of unwanted polymer, such as "pop-corn"
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F210/00Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F210/04Monomers containing three or four carbon atoms
    • C08F210/06Propene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F210/00Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F210/16Copolymers of ethene with alpha-alkenes, e.g. EP rubbers

Abstract

Polymer solids are maintained in an intermediate pressure zone for a desired polymer solids residence time and then transferred to a purge zone or other lower pressure zone. An increase in the polymer solids residence time in the intermediate pressure zone allows more diluent to flash or separate, thereby avoiding or reducing the need for a low pressure flash zone. A fluff chamber may be disposed between the intermediate pressure zone and a lower pressure zone. transporter tank may be used to transport polymer solids after the intermediate pressure zone.

Claims (40)

1. A process for slurry polymerization of olefins and for separating polymer solids from diluent, the process comprising:
polymerizing in a reaction zone at least one olefin monomer in a liquid diluent to produce a fluid slurry comprising the liquid diluent and polymer solids;
withdrawing a portion of the slurry from the reaction zone;
heating the withdrawn portion of the slurry;
passing the withdrawn portion of the slurry to an intermediate pressure zone in which a majority of the diluent is separated from the polymer solids, wherein the intermediate pressure zone is at a pressure in the range of from 100 psia to 1500 psia;
withdrawing the polymer solids from the intermediate pressure zone; and transferring the polymer solids to a purge zone without passing through a flash zone.
2. A process according to claim 1 wherein the intermediate pressure zone is at a pressure within the range of from 130 to 190 psia.
3. A process according to claim 1 wherein the intermediate pressure zone is at a temperature in the range of from 100°F to 250°F.
4. A process according to claim 3 wherein the separated diluent is condensed without compression after the intermediate pressure zone.
5. A process according to claim 1 wherein a top valve, a fluff collection zone, and a bottom valve are disposed between the intermediate pressure zone and the purge zone, and the polymer solids are transferred from the intermediate pressure zone to the purge zone by the following steps:

(i) opening the top valve when the bottom valve is closed;
(ii) passing the polymer solids into the fluff collection zone;
(iii) closing the top valve while the bottom valve remains closed after the level of polymer solids in the fluff collection zone reaches a first desired level;
(iv) opening the bottom valve while the top valve remains closed, thereby passing the polymer solids the purge zone; and (v) closing the bottom valve when the level of polymer solids in the fluff collection zone reaches a second desired level.
6. A process according to claim 5 further comprising the steps of decreasing the pressure within the fluff collection zone between steps (iii) and (iv), and increasing the pressure within the fluff collection zone after step (v).
7. A process according to claim 1, further comprising transferring the polymer solids from the intermediate pressure zone to a transporter zone; and transferring the polymer solids from the transporter zone to the purge zone by a force other than gravity.
8. A process according to claim 7, further comprising heating the polymer solids after the transporter zone.
9. A process according to claim 1, further comprising transferring the polymer solids from the intermediate pressure zone to a first transfer zone;
transferring the polymer solids from the intermediate pressure zone to a second transport zone;
when the level of the polymer solids in the first transfer zone reaches a desired level.
10. A process according to claim 1, wherein the polymer solids are transferred to the purge zone primarily by flash gas from the intermediate pressure zone.
11. A process according to claim 1 wherein the polymer solids are substantially free of unentrained diluent after the intermediate pressure zone.
12. A process according to claim 11 wherein the polymer solids are substantially free of entrained diluent after the purge zone.
13. A process for slurry polymerization of olefins and for separating polymer solids from diluent, the process comprising:
polymerizing in a reaction zone at least one olefin monomer in a liquid diluent to produce a fluid slurry comprising the liquid diluent and polymer solids;
withdrawing a portion of the slurry from the reaction zone;
passing the withdrawn portion of the slurry to an intermediate pressure zone in which a majority of the diluent is separated from the polymer solids, wherein the intermediate pressure zone is at a pressure in the range of 100-1500 psia;
withdrawing the polymer solids from the intermediate pressure zone;
monitoring the level of the polymer solids in the intermediate pressure zone;
and adjusting the withdrawal of the polymer solids from the intermediate pressure zone in response to the monitored level.
14. A process according to claim 13 further comprising maintaining a sufficient level of the polymer solids in the intermediate pressure zone to provide a pressure seal for intermediate pressure zone.
15. A process according to claim 13 wherein the polymer solids are held in the intermediate pressure zone for an average polymer solids residence time, and the polymer solids residence time is sufficient to separate substantially all unentrained diluent from the polymer solids.
16. A process according to claim 11 wherein the step for controlling the rate of the withdrawing the polymer solids from the intermediate pressure zone comprises:
establishing a first signal representative of the actual level of the polymer solids in the intermediate pressure zone;
establishing a second signal representative of a desired level of the polymer solids in the intermediate pressure zone;
comparing the first signal and the second signal and establishing a third signal responsive to the difference between the first signal and the second signal;
and manipulating the solids outlet control valve in response to the third signal.
17. A process for slurry polymerization of olefins and for separating polymer solids from diluent, the process comprising:
polymerizing in a reaction zone at least one olefin monomer in a liquid diluent to produce a fluid slurry comprising the liquid diluent and polymer solids;
withdrawing a portion of the slurry from the reaction zone;
introducing the withdrawn portion of the fluid slurry to an intermediate pressure zone in which a majority of the diluent is separated from the polymer solids, wherein the intermediate pressure zone is at a pressure in the range of 100-1500 psia;
holding the polymer solids in the intermediate pressure zone for a polymer solids residence time sufficient to remove substantially all the unentrained diluent;
and withdrawing the polymer solids from the intermediate pressure zone; and transferring the polymer solids to a purge zone to remove substantially all the entrained diluent.
18. A process according to claim 17 wherein the polymer solids residence time is from about 10 seconds to about 30 minutes.
19. A process according to claim 17 wherein the polymer solids residence time is from about 30 to about 120 minutes.
20. A process according to claim 17 wherein a desired level of polymer solids are maintained in the intermediate pressure zone, and the polymer solids are withdrawn from the intermediate pressure zone by uniform flow.
21. A process according to claim 17, further comprising controlling the rate of the withdrawal the polymer solids from the intermediate pressure zone by manipulating a solids outlet control valve.
22. An apparatus for separating diluent from polymer solids, the apparatus comprising:
(a) an intermediate pressure chamber adapted for the separation of diluent vapor from polymer solids, the chamber having an inlet for receiving a fluid slurry comprising diluent and polymer solids from a slurry reactor, a solids outlet for discharging polymer solids, and a gas outlet for discharging vaporized diluent;
(b) a level sensor in contact with the intermediate pressure chamber for sensing the level of polymer solids in the intermediate pressure chamber;
(c) an outlet valve fluidly connected to the solids outlet of the intermediate pressure chamber, wherein the outlet valve is manipulated in response to the sensed level;
(d) a condenser fluidly connected to the gas outlet for receiving and condensing without compression the vaporized diluent; and a purge column fluidly connected to the outlet valve, the purge column receiving the polymer solids from the intermediate pressure chamber.
23. The separating apparatus of claim 22, further comprising:
a fluff chamber downstream of and fluidly connected to the outlet valve;
a fluff chamber valve in fluid connection with the bottom of the fluff chamber;
a purge column in fluid connection with the fluff chamber valve; and means for operating the outlet valve and the fluff chamber valve so that the valves are not open at the same time.
24 24. The separating apparatus of claim 23 wherein the fluff chamber houses a rotating device for avoiding polymer build-up and clogging.
25. The separating apparatus of claim 23 wherein the fluff chamber has an angled bottom and a surface finish that facilities plug flow of the polymer solids.
26. The separating apparatus of claim 23 further comprising a flashline disposed between and fluidly connecting the intermediate pressure chamber and the slurry reactor; and a flashline heater in heat exchange relation with at least a majority of the length of the flashline.
27. The separating apparatus of claim 22, further comprising a first transporter tank downstream of and fluidly connected to the outlet valve.
28. The separating apparatus of claim 27 wherein the first transporter tank is upstream of an fluidly connected to a purge column.
29. The separating apparatus of claim 27, further comprising:
a second transporter tank downstream of and fluidly connected to the outlet valve; and a transporter tank controller operatively connected to the first and second transporter tanks, the controller being adapted to alternate the flow of polymer solids between the first and second transporter tanks.
30. The separating apparatus of claim 22 wherein the intermediate press chamber is also a transporter tank.
31. An apparatus for separating diluent from polymer solids, the apparatus comprising:
(a) an intermediate pressure chamber in which diluent is separated from polymer solids;

(b) a fluid passage connected at one end to a bottom portion of the intermediate pressure chamber;
(c) a purge column connected at an opposite end of the fluid passage;
(d) a condenser fluidly connected to the flash gas outlet for receiving and condensing without compression the vaporized diluent; and (e) a recycle line for transferring the condensed diluent to the slurry reactor; wherein the separating apparatus does not comprise a low pressure flash chamber.
32. The separating apparatus of claim 31, further comprising:
an outlet valve disposed along the fluid passage;
a fluff chamber downstream of and fluidly connected to the outlet valve;
a fluff chamber valve disposed along the fluid passage and in fluid connection with the bottom of the fluff chamber; and means for operating the outlet valve and the fluff chamber valve so that the valves are not open at the same time.
33. The separating apparatus of claim 32 wherein the fluff chamber houses a rotating device for avoiding polymer build-up and clogging.
34. The separating apparatus of claim 31 wherein the fluff chamber has an angled bottom and a surface finish that facilities plug flow of the polymer solids.
35. The separating apparatus of claim 31 further comprising a flashline fluidly connected with and upstream of the intermediate pressure chamber; and a flashline heater in heat exchange relation with at least a majority of the length of the flashline.
36. The separating apparatus of claim 31 further comprising a timer connected to the outlet valve, wherein the timer determines the opening and closing of the outlet valve.
37. The separating apparatus of claim 31, further comprising a first transporter tank downstream of and fluidly connected to the outlet valve.
38. The separating apparatus of claim 37 wherein the first transporter tank is upstream of an fluidly connected to a purge column.
39. The separating apparatus of claim 37, further comprising:
a second transporter tank downstream of and fluidly connected to the outlet valve; and a transporter tank controller operatively connected to the first and second transporter tanks, the controller being adapted to alternate the flow of polymer solids between the first and second transporter tanks.
40. The separating apparatus of claim 31 wherein the intermediate press chamber is also a transporter tank.
CA002498763A 2002-09-16 2003-09-15 Process and apparatus for separating diluent from polymer solids Expired - Lifetime CA2498763C (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US41125502P 2002-09-16 2002-09-16
US60/411,255 2002-09-16
US10/662,260 2003-09-15
US10/662,260 US6838531B2 (en) 2002-09-16 2003-09-15 Process and apparatus for separating diluent from polymer solids
PCT/US2003/029331 WO2004026914A1 (en) 2002-09-16 2003-09-15 Process and apparatus for separating diluent from polymer solids

Publications (2)

Publication Number Publication Date
CA2498763A1 true CA2498763A1 (en) 2004-04-01
CA2498763C CA2498763C (en) 2009-11-10

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CA002498763A Expired - Lifetime CA2498763C (en) 2002-09-16 2003-09-15 Process and apparatus for separating diluent from polymer solids

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US (2) US6838531B2 (en)
EP (1) EP1551881B1 (en)
AT (1) ATE457321T1 (en)
AU (1) AU2003272518A1 (en)
BR (1) BR0314384B1 (en)
CA (1) CA2498763C (en)
DE (1) DE60331233D1 (en)
DK (1) DK1551881T3 (en)
ES (1) ES2340993T3 (en)
MX (1) MXPA05002956A (en)
WO (1) WO2004026914A1 (en)

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US7629421B2 (en) * 2005-12-21 2009-12-08 Chevron Phillips Chemical Company Lp Monomer recovery by returning column overhead liquid to the reactor
US7957947B2 (en) * 2006-08-25 2011-06-07 Chevron Phillips Chemical Company Lp Method and apparatus for managing volatile organic content in polyolefin
EP1918308A1 (en) * 2006-10-30 2008-05-07 Total Petrochemicals Research Feluy Process for improving the devolatilization of polymer slurry produced in a polymerization reactor
US7381777B1 (en) 2007-02-26 2008-06-03 Exxonmobil Chemical Patents Inc. Method for controlling fouling in slurry-type polymerization reactors
US9637570B2 (en) * 2009-06-11 2017-05-02 Exxonmobil Chemical Patents Inc. Method and apparatus for reducing fouling
MX2012006794A (en) * 2009-12-18 2012-10-05 Total Petrochemicals Res Feluy Method for monitoring the level of an ethylene polymerization catalyst slurry.
US9211523B2 (en) 2010-07-01 2015-12-15 Chevron Phillips Chemical Company Lp Polyolefin manufacturing system including a membrane fractionation system for diluent recovery
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US8440772B2 (en) 2011-04-28 2013-05-14 Chevron Phillips Chemical Company Lp Methods for terminating olefin polymerizations
US8597582B2 (en) 2011-06-30 2013-12-03 Chevron Phillips Chemical Company Lp Flashline heater system and method
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WO2022108803A1 (en) * 2020-11-17 2022-05-27 Ineos Usa Llc Process
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Also Published As

Publication number Publication date
EP1551881B1 (en) 2010-02-10
DE60331233D1 (en) 2010-03-25
CA2498763C (en) 2009-11-10
AU2003272518A1 (en) 2004-04-08
BR0314384B1 (en) 2014-10-21
WO2004026914A1 (en) 2004-04-01
BR0314384A (en) 2005-07-26
US6953553B2 (en) 2005-10-11
US20040116597A1 (en) 2004-06-17
ES2340993T3 (en) 2010-06-14
US6838531B2 (en) 2005-01-04
EP1551881A1 (en) 2005-07-13
DK1551881T3 (en) 2010-05-25
ATE457321T1 (en) 2010-02-15
MXPA05002956A (en) 2005-10-19
EP1551881A4 (en) 2007-05-02
US20050034968A1 (en) 2005-02-17

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