CN101927141B - Method for transferring polymer particles among gas-phase polymerization reactors - Google Patents
Method for transferring polymer particles among gas-phase polymerization reactors Download PDFInfo
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- CN101927141B CN101927141B CN2009100872004A CN200910087200A CN101927141B CN 101927141 B CN101927141 B CN 101927141B CN 2009100872004 A CN2009100872004 A CN 2009100872004A CN 200910087200 A CN200910087200 A CN 200910087200A CN 101927141 B CN101927141 B CN 101927141B
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Abstract
The invention provides a method for transferring polymer particles among gas-phase polymerization reactors, which is used for two or more gas-phase polymerization reactors connected in series, wherein the two or more gas-phase polymerization reactors connected in series continuously polymerize a polymer monomer or a mixture thereof, and each reactor contains a particle-quenching micro-fluidized bed for the polymer monomer. The transferring method shortens the cycle, simplifies the process and can effectively improve the transfer efficiency and the purification efficiency.
Description
Technical field
The present invention relates to a kind of between gas-phase polymerization reactor the method for transfer polymerization composition granule; More specifically, relate to a kind of in the process of the homopolymers of producing alkene or copolymer the transfer method between the gas-phase polymerization reactor of polymer in two or more series connection.
Technical background
Use the gas-phase polymerization reactor of two or more arranged in series, can produce the homopolymers and the copolymer of alkene.Its technological process mainly comprises technique units such as Preparation of Catalyst, polymerisation, reacting gas circulation, the polymer degassing, gas steaming and drying.Existing a lot of patents describe this gas phase polymerization process, comprising US3, and 957,448, US3,965,083, US3,971,768, CN1228096A etc.
Detailed process can comprise: use effective catalyst component and co-catalyst usually; The preferred highly active catalyst component for olefin polymerization of the 4th generation that uses solid based on transition metal; In little still,, be injected into next unit through pump with this catalyst activity component and grease class mixing diluents; In polymerized unit, catalyst activity component and cocatalyst component mixed together join in first Gas-phase reactor.Cocatalyst component generally includes: a kind of is the alkyl aluminum component, like triethyl aluminum; Another kind is typical external modifier component, like silane components.The reactor production period, the internal pressure of about 200-400psig (1400-2800kpa) and about 50-90 ℃ reaction temperature.The quenching particle Micro Fluid bed that contains polymerization single polymerization monomer in each reactor.Gas component is propylene and vinyl monomer normally.The circulating air that the polymerization temperature of each part can get into through agitating device, from reactor bottom and control from the quench liquid of reactor head spray; In order to set up the circulation of gas in still, to reach control temperature and the purpose that improves productive rate, reacting gas will get into the gas circulation unit, and the gas circulation unit comprises evaporator overhead condenser, liquid collecting jar, recycle gas compressor and liquid pump.Gas cools off through evaporator overhead condenser, becomes liquid condition, collect in the liquid collecting jar, again via recycle gas compressor and liquid pump, with the gas circulation of liquid and heating to reactor.The gas of reactor is propylene monomer and vinyl monomer normally, also has the hydrogen of low molar content, with the character of control polymerizate.They can be along with the quenching polymer beads joins in the downstream reactor.The reactor of these series connection has different working conditions and gas composition usually, to form different classes of polymerizate.Arts demand is the transfer polymerization composition granule between the equipment of series connection, and does not bring the gas component in the upstream reactor into downstream, requires this transfer equipment will be simple and easy to use.Possibly be viscose glue because of polymer beads simultaneously, as adhere to, just be not easy from the product letdown tank, to flow out.So requirement can be avoided line clogging effectively in this technology, can be efficiently, operate incessantly, near state stably continuously, can help producing the more polymerizate of homogeneous.
Chinese patent CN1228096A discloses the method that a kind of polymer beads shifts; This method is to come the trasfer of solids particle through a gas-solid separator and a transfer groove; When solid particle when gas one solid separator is transferred to the transfer groove, discontinuously in transfer groove, add Purge gas.This patent utilization purified gas and gas solid separator can be got rid of the gas of the upstream reactor that the quenching solid particle carries.
There is following shortcoming in this method: 1, come the trasfer of solids particle through a series of of gas-solid separator and transfer groove along the control step; Carry out charging, purging respectively, purify, boost, step such as discharge; Make the cycle increase (about 4 minutes; Embodiment 1～3 in the specification), this makes gas-solid separator and transfer groove must use the equipment of larger volume, perhaps many group equipment parallel operations.With respect to 40～50 minutes polymerization time of common reactor, polymer is then longer relatively about 4 minutes transfer time in transfer process, and polymer reaction temperature during this, form and can not control, be disadvantageous for production polymer of high quality product.2, transfer groove adds Purge gas by intermittently adding along control, and the time of purification only accounts for the very little part of transfer process.The time that Purge gas contacts with polymer beads, gentle speed can not be regulated, and can not learn purification effects, can not monitor purification process.When carrying out homopolymerization, can not change along control program control by-pass purification process, make polymer at the transfer process experience polymerizing condition identical with the upstream and downstream reactor.
Summary of the invention
The invention provides a kind of new between gas-phase polymerization reactor the method for transfer polymerization composition granule, this transfer method has been realized from upstream reactor having realized carrying out continuously of gas purification to the carrying out continuously of gas-solid separator discharge.This transfer method shortens the cycle, and the simplification process can improve the transfer efficiency of polymer and the purification efficiency of polymer simultaneously effectively.
The invention provides the transfer method of a kind of polymer beads between gas-phase polymerization reactor; This transfer method is applied in the gas-phase polymerization reactor of two or more series connection; Described two or more series connection a kind of polymerization single polymerization monomer of gas-phase polymerization reactor continuous polymerization or its mixtures; Each polymer reactor contains the quenching particle Micro Fluid bed of polymerization single polymerization monomer; Through this fluid bed, particle at high pressure, be full of between reacting gas, the continuous gas-phase polymerization reactor and shift, this method comprises:
(a) will intermittently or continuous being drained in gas-solid separator from the slurries of the polymer of upstream reactor and reacting gas, keep the low 35kpa at least of operating pressure of the pressure ratio upstream reactor of gas-solid separator;
(b) a kind of Purge gas of adding continuous or intermittence in gas-solid separator bottom; This Purge gas is at least a in the polymerization single polymerization monomer in the upstream reactor, and a part of reacting gas and the Purge gas exhaust outlet that passes through continuous or intermittently is got back to the cycle equipment that comprises gas compressor and continued to participate in reaction in the upstream reactor in gas-solid separator;
(c) solid particle after gas-solid separator is separated, being drained in the transfer groove intermittently;
(d) with carrying gas to boost to transfer groove; This conveying gas is the polymerization single polymerization monomer of described Purge gas, downstream polymer reactor or the inert gas that does not influence the downstream polymerisation; Pressure up to transfer groove is higher than downstream reactor 7kpa at least, and the solid particle in the transfer groove is transported to downstream reactor; Perhaps be lower than upstream reactor pressure 70kpa when above when the downstream reactor pressure, the solid particle in the transfer groove is transported in the downstream reactor.
The polymer of upstream reactor of the present invention can be realized continuous being drained in gas-solid separator, continuable adding Purge gas and discharge tail gas in gas-solid separator.Storage through polymer in control gas-solid separator can be controlled the time that Purge gas contacts with polymer beads; Can control Purge gas through the flow of control Purge gas and contact gas speed with polymer beads.Thereby can well control the degree of purification of polymer, and stop to purify can be readily embodied in homopolymerization the time.Can learn purification effects through analyzing the composition of discharging gas-solid separator gas.
According to the present invention, because upstream reactor is carried out to gas-solid separator transfer polymerization composition granule continuously, the transfer cycle time of polymer beads between two gas-phase polymerization reactors is mainly determined by the responsiveness of transfer groove.Because transfer groove is only carried out single relatively function, make its action step obtain simplifying.
Be used for the conveying gas that transfer groove boosts and only bear conveying function, the Purge gas that this conveying gas can use for gas-solid separator, the polymerization single polymerization monomer of downstream reactor or do not influence the inert gas of downstream polymerisation.When using Purge gas, tail gas was drained in the cycle equipment that comprises gas compressor when transfer groove reduced pressure, got back to then and continued to participate in reaction in the upstream reactor.When the polymerization single polymerization monomer that uses downstream reactor or the inert gas that do not influence polymerisation when boosting gas, tail gas was drained into the cycle equipment that comprises gas compressor and gets back to and continue to participate in reaction in the downstream reactor when transfer groove reduced pressure.
Disclosing in the described transfer method of Chinese patent CN1228096A, describing action one-period needs 4 minutes according to it.This patent needs moving along control more than ten steps in practice, wherein only upstream reactor just needs the multistep pulse action to gas-solid separator and transfer groove charging.Only needed for four steps and obtain simplification according to transfer groove action of the present invention, the action one-period needs 0.5～2 minute.Therefore use the present invention's action cycle under reach, improve transfer efficiency effectively.
The gas-phase polymerization reactor that transfer method of the present invention preferably is used for two series connection carries out.In polymer reactor; The quenching particle Micro Fluid bed of polymerization single polymerization monomer is contained in the cylindrical portions may of each reactor; This reactor at least a portion polymerization reaction heat is to remove through the evaporation of volatile quench liquid; This reactor is a horizontal reactor, on its circular cross section the center have one run through reactor central shaft, through the blade on this polymer beads that is in the Micro Fluid state in reactor is stirred.The reactor that contains quenching particle Micro Fluid bed is disclosed among Chinese patent CN1281380A, the CN1081683A.Its disclosed related content is all introduced the present invention as a reference.
In the gas-phase polymerization reactor of two series connection, polymer beads can shift through single transfer groove
A kind of polymerization single polymerization monomer of gas-phase polymerization reactor continuous polymerization of the present invention or its mixture, described polymerization single polymerization monomer comprises in ethene, propylene and the butylene at least a, preferred especially polymerization single polymerization monomer is a propylene.When comprising two or more polymerisable monomer in the upstream reactor, Purge gas is an at least a monomer wherein.
Transfer method of the present invention also comprises, measures the control valve that exhaust forms to come adjustments of gas-solid separator bottom-purge gas air inlet place through a chromatograph of gas-solid separator exhaust ports, controls the addition of Purge gas.Measure exhaust through the chromatograph of gas-solid separator exhaust ports and form, control the addition of Purge gas, thereby realize using less Purge gas to meet the requirements of degree of purification through the control valve of adjustments of gas-solid separator bottom-purge gas.
The present invention has save independent purifying step in the prior art polymer beads transfer process, and gas solid separation process and purification process are carried out simultaneously.Gas-solid separator and transfer groove are born single work, have simplified the step that shifts.Because transfer valve is carried out the cancellation of displacement step between unlatching gas-solid separator and transfer groove, and upstream reactor discharging ability is promoted greatly, polymer transfer efficiency between reactor increases, and is beneficial to raising output.
In transfer method of the present invention; Carry gas only to be used for boosting to transfer groove, its air inlet position places between separator and transfer groove after the transfer valve, and can effectively remove the buildup in the pipeline between separator and the transfer groove this moment; Avoid stopping up, improve transfer efficiency and production efficiency.
Description of drawings
Fig. 1 is the process chart of an embodiment of the transfer method of polymer beads of the present invention between gas-phase polymerization reactor.
It comprises the gas-phase polymerization reactor of two series connection, and wherein each reactor contains particulate polymers Micro Fluid bed.Polymer beads shifts between gas-phase polymerization reactor; 101 and 102 is respectively the reactor of upstream and downstream; Purification and buanch unit have comprised gas-solid separator 110,111,112,113 and gas-chromatographies of transfer groove (GC); The reaction gas cycling element has comprised tail-gas compressor 121, condenser 122, condensate drum 123, recycle gas compressor 124 and quenching liquid pump 125, and downstream reactor 102 reaction gas cycling elements have comprised tail-gas compressor 221, condenser 222, condensate drum 223, recycle gas compressor 224 and quenching liquid pump 225.
The polymer beads transfer step is: the material level according to 101 is opened 101 bleeder valve 1101 and 1102 with pulse mode, and polymer beads and admixture of gas are discharged in gas-solid separator 110 and 111.In this process, gas-solid separator bottom purified gas adds continuously, purifies polymer.Give gas-solid separator step-down through 1201 valves simultaneously, get rid of the reacting gas that Purge gas and polymer beads bring.Through the pressure in opening degree control gas-solid separator of regulating 1201 valves a little less than 101 pressure (low approximately 50kpa).
The material level of gas-solid separator reach the control material level in limited time, open 1103 and 1104 valves, the quenching polymer beads after the purification is discharged into transfer groove 112 and 113.Reach the following of control material level at the material level of gas-solid separator and close 1103 and 1104 valves in limited time, gas-solid separator stops to the transfer groove discharging.Then through carrying gas to boost to transfer groove.When the pressure of transfer groove 112 and 113 is higher than downstream reactor 7kpa at least, open the charging valve 1105 and 1106 of downstream reactor, mass transport is to downstream reactor 102.After finishing, conveying closes blow-off valve 1105 and 1106.The valve of opening exhaust emissions is reduced to the pressure of transfer groove 112 and 113 and is lower than gas-solid separator 35kpa at least, waits for gas-solid separator discharging next time.According to the difference of carrying gas, tail gas is discharged to the tail-gas compressor of upstream reactor 101 or the tail-gas compressor inlet of downstream reactor 102.
The specific embodiment
Provide following examples so that the present invention is described better, be not used for limiting scope of the present invention.
Embodiment 1
In the gas-phase polymerization reactor of two arranged in series, propylene monomer is carried out continuous gas-phase polymerization, prepare solid homopolymer normally, in the upstream and downstream reactor, there is the hydrogen of low molar content.According to the present invention, only use the polyacrylic particle of a column jump in the two row equipment, be 1 minute the circulation timei of use.Use propylene monomer as Purge gas, use propylene monomer as carrying gas.The tail gas of transfer groove is discharged to the inlet of tail-gas compressor 121.
Embodiment 2
In the gas-phase polymerization reactor of two arranged in series, propylene monomer is carried out continuous gas-phase polymerization, prepare solid homopolymer normally, in the upstream and downstream reactor, there is the hydrogen of low molar content.According to the present invention; The bleeder valve 1101 of 101 reactors and 1102 uses the adjustable continuous discharging of valve of separating aperture, does not adopt pulse mode, and the adding of Purge gas and tail gas recycle are also carried out continuously; Only use the polyacrylic particle of a column jump in the two row equipment, be 1 minute the circulation timei of use.Use propylene monomer as Purge gas, use propylene monomer as carrying gas.The tail gas of transfer groove is discharged to the inlet of tail-gas compressor 121.
Embodiment 3
In the gas-phase polymerization reactor of two arranged in series, propylene monomer is carried out continuous gas-phase polymerization, prepare solid homopolymer normally, in the upstream and downstream reactor, there is the hydrogen of low molar content.According to the present invention, use two row equipment to shift polyacrylic particle simultaneously, be 1 minute the circulation timei of use.Use propylene monomer as Purge gas, use propylene monomer as carrying gas.The tail gas of transfer groove is discharged to the inlet of tail-gas compressor 121.
Embodiment 4
In the gas-phase polymerization reactor of two arranged in series, propylene monomer is carried out continuous gas-phase polymerization, prepare solid homopolymer normally, in the upstream and downstream reactor, there is the hydrogen of low molar content.According to the present invention, only use the polyacrylic particle of a column jump in the two row equipment, be 1 minute the circulation timei of use.Use propylene monomer as Purge gas, use reacting gas behind the second reactor cycles air compressor 224 as carrying gas.The tail gas of transfer groove is discharged to the inlet of the tail-gas compressor 221 of second reactor.
Embodiment 5
In the gas-phase polymerization reactor of two arranged in series, propylene monomer is carried out continuous gas-phase polymerization, prepare solid homopolymer normally, in the upstream and downstream reactor, there is the hydrogen of low molar content.According to the present invention, the Purge gas of gas-solid separator adds in 101 reactor pulse dischargings, stops to add Purge gas after the stop pulse discharging, opens 1201 and reclaims tail gas.Make discharging, add the Purge gas action and reclaim the tail gas intermittently operated and hocket.Only use the polyacrylic particle of a column jump in the two row equipment, be 1 minute the circulation timei of use.Use propylene monomer as Purge gas, use propylene monomer as carrying gas.The tail gas of transfer groove is discharged to the inlet of tail-gas compressor 121.
Embodiment 6
In the gas-phase polymerization reactor of two arranged in series, propylene monomer is carried out continuous gas-phase polymerization, prepare solid homopolymer normally, in the upstream and downstream reactor, there is the hydrogen of low molar content.According to the present invention, the Purge gas of gas-solid separator adds in 101 reactor pulse dischargings, stops to add Purge gas after the stop pulse discharging, opens 1201 and reclaims tail gas.Reclaim tail gas to requiring to open 1103 or 1104 to the transfer groove discharging behind the pressure.Make gas-solid separator charging, add the Purge gas action and reclaim the tail gas action and go on foot and carry out intermittently operated successively with gas-solid separator discharging action three.Only use the polyacrylic particle of a column jump in the two row equipment, be 2 minutes the circulation timei of use.Use propylene monomer as Purge gas, use propylene monomer as carrying gas.The tail gas of transfer groove is discharged to the inlet of tail-gas compressor 121.
Embodiment 7
In the gas-phase polymerization reactor of two arranged in series, propylene monomer is carried out continuous gas-phase polymerization, prepare solid homopolymer normally, in the upstream and downstream reactor, there is the hydrogen of low molar content.Wherein the pressure of first reactor 101 is higher than second reactor, 102 pressure 200kpa.According to the present invention, only use the polyacrylic particle of a column jump in the two row equipment, propylene monomer does not use conveying gas as Purge gas.Be 0.8 minute the circulation timei of operation.
Embodiment 8
In the gas-phase polymerization reactor of two arranged in series, propylene monomer and vinyl monomer are carried out continuous gas-phase polymerization, prepare solid atactic copolymer normally, in the upstream and downstream reactor, there is the hydrogen of low molar content.According to the present invention, only use the polyacrylic particle of a column jump in the two row equipment, be 1 minute the circulation timei of use.Use propylene monomer as Purge gas, use propylene monomer as carrying gas.The tail gas of transfer groove is discharged to the inlet of tail-gas compressor 121.
Embodiment 9
In the gas-phase polymerization reactor of two arranged in series, propylene monomer and vinyl monomer are carried out continuous gas-phase polymerization, prepare the solid impact copolymer normally.In upstream reactor, carry out the propylene homopolymerization, have the hydrogen of low molar content.Add ethene at downstream reactor and carry out copolymerization, and contain the hydrogen that is less than upstream reactor.There is not oxygen with control output in the oxygen that in downstream reactor, contains low content in upstream reactor basically.According to the present invention, only use the polyacrylic particle of a column jump in the two row equipment, be 1 minute the circulation timei of use.Use propylene monomer as Purge gas, use propylene monomer as carrying gas.The tail gas of transfer groove is discharged to the inlet of tail-gas compressor 121.
Embodiment 10
In the gas-phase polymerization reactor of two arranged in series, propylene monomer and vinyl monomer are carried out continuous gas-phase polymerization, prepare the solid impact copolymer normally.In upstream reactor, carry out the propylene homopolymerization, have the hydrogen of low molar content.Add ethene at downstream reactor and carry out copolymerization, and contain the hydrogen that is less than upstream reactor.There is not oxygen with control output in the oxygen that in downstream reactor, contains low content in upstream reactor basically.According to the present invention, only use the polyacrylic particle of a column jump in the two row equipment, be 1 minute the circulation timei of use.Use propylene monomer as Purge gas, use reacting gas behind the second reactor cycles air compressor 224 as carrying gas.The tail gas of transfer groove is discharged to the inlet of the tail-gas compressor 221 of second reactor.
Claims (6)
1. the transfer method of polymer beads between gas-phase polymerization reactor; This transfer method is applied in the gas-phase polymerization reactor of two or more series connection; Described two or more series connection a kind of polymerization single polymerization monomer of gas-phase polymerization reactor continuous polymerization or its mixtures, each polymer reactor contains the quenching particle Micro Fluid bed of polymerization single polymerization monomer, through this fluid bed; Particle shifts between continuous gas-phase polymerization reactor, and this method comprises:
(a) will intermittently or continuous being drained in gas one solid separator from the slurries of the polymer of upstream reactor and reacting gas, keep the low 35kPa at least of operating pressure of the pressure ratio upstream reactor of gas one solid separator;
(b) a kind of Purge gas of adding continuous or intermittence in gas one solid separator bottom; This Purge gas is at least a in the polymerization single polymerization monomer in the upstream reactor, and a part of reacting gas and the Purge gas exhaust outlet that passes through continuous or intermittently is got back to the cycle equipment that comprises gas compressor and continued to participate in reaction in the upstream reactor in gas one solid separator;
(c) solid particle after gas one solid separator is separated, being drained in the transfer groove intermittently;
(d) with carrying gas to boost to transfer groove; This conveying gas is the polymerization single polymerization monomer of described Purge gas, downstream polymer reactor or the inert gas that does not influence the downstream polymerisation; Pressure up to transfer groove is higher than downstream reactor 7kPa at least, and the solid particle in the transfer groove is transported to downstream reactor; Perhaps be lower than upstream reactor pressure 70kPa when above when the downstream reactor pressure, the solid particle in the transfer groove is transported in the downstream reactor.
2. the transfer method of polymer beads according to claim 1 between gas-phase polymerization reactor; Wherein in the step (a); When from the polymer of upstream reactor and reacting gas slurries by intermittently be drained in gas one solid separator time, gas one solid separator when the upstream reactor blow-off valve cuts out to the transfer groove discharge.
3. the transfer method of polymer beads according to claim 1 between gas-phase polymerization reactor, wherein this transfer method is applied in two series connection Gas-phase reactor.
4. the transfer method of polymer beads according to claim 1 between gas-phase polymerization reactor, wherein said gas-phase polymerization reactor continuous polymerization monomer comprises following a kind of at least: ethene, propylene and butylene.
5. the transfer method of polymer beads according to claim 1 between gas-phase polymerization reactor, wherein said polymerization single polymerization monomer is a propylene.
6. the transfer method of polymer beads according to claim 1 between gas-phase polymerization reactor; This method also comprises; A chromatograph through gas one solid separator exhaust ports is measured the control valve that exhaust forms to come adjustments of gas one solid separator bottom-purge gas air inlet place, controls the addition of Purge gas.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1081683A (en) * | 1992-05-29 | 1994-02-09 | 阿莫科公司 | The polymerization of alpha-olefin |
| CN1124029A (en) * | 1993-05-20 | 1996-06-05 | 英国石油化学品有限公司 | Polymerisation process |
| CN1228096A (en) * | 1996-08-20 | 1999-09-08 | 阿莫科公司 | Transfer of polymer particles between vapor phase polymerization reactors |
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- 2009-06-19 CN CN2009100872004A patent/CN101927141B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1081683A (en) * | 1992-05-29 | 1994-02-09 | 阿莫科公司 | The polymerization of alpha-olefin |
| CN1124029A (en) * | 1993-05-20 | 1996-06-05 | 英国石油化学品有限公司 | Polymerisation process |
| CN1228096A (en) * | 1996-08-20 | 1999-09-08 | 阿莫科公司 | Transfer of polymer particles between vapor phase polymerization reactors |
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