CN105237665A - On-line cleaning method for low density polyethylene production gas phase fluidized bed reaction system - Google Patents
On-line cleaning method for low density polyethylene production gas phase fluidized bed reaction system Download PDFInfo
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- CN105237665A CN105237665A CN201510657016.4A CN201510657016A CN105237665A CN 105237665 A CN105237665 A CN 105237665A CN 201510657016 A CN201510657016 A CN 201510657016A CN 105237665 A CN105237665 A CN 105237665A
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Abstract
The invention discloses an on-line cleaning method for a low density polyethylene production gas phase fluidized bed reaction system. A part of gas is drawn from a gas phase fluidized bed, is used as a circulation air flow and is circulated, in on-line cleaning, an inert condensable component is added into the circulation air flow subjected to compression and condensation, the inert condensable component has a solubility parameter of 6.5-9cal<1/2>. cm<3/2>, through compression and condensation, the circulation air flow forms a gas-liquid two phase mixture, and the mixture is returned into the gas phase fluidized bed so that a circulation loop is formed. Condensation depth and on-line cleaning time are adjusted and controlled and the reaction system is subjected to on-line effective cleaning so that device running time is prolonged and the problem that a distribution plate and a heat exchanger are blocked, system differential pressure is improved and a heat dissipation capability is reduced in long-time cycle operation of the low density polyethylene production gas phase fluidized bed reaction system is solved.
Description
Technical field
The present invention relates to the on-line cleaning method of the gas-phase fluidized-bed reactive system producing Low Density Polyethylene, add the softening of polyvinyl resin and solvency action especially by what consider inert condensable mixture, the inert condensable mixture of suitable solubility parameters is added in circulating current, and condensing deep and on-line cleaning time are regulated and controled, online effectively cleaning is carried out to reactive system, extension fixture working time.
Background technology
In continuous gas-phase fluidized-bed polyethylene polymerization technique, the difficulty of plant running is to control well fluidized state.Fluidized state is deteriorated, and in reactor, hot localised points causes easily occurring sheeting, and sheeting can make fluidized status worsen further, may occur being forced to stop and reactor implode.The existence of fine powder and high reactivity particle causes the fouling gradually of gas-phase fluidized-bed polyethylene reactive system inner-walls of duct, and interchanger, grid distributor block gradually.Not carrying out cleaning for a long time can cause grid distributor to block seriously, and fluidized state is deteriorated, and then causes parking accident.Along with the development of national economy, polyvinyl resin demand constantly increases, but scheduled shut down cleaning grid distributor and reactor meeting large losses material, cause the gas-phase fluidized-bed polyolefin device cycle of operation short, efficiency is low, and loss is large, and waste gas torch of setting fire also can cause environmental pollution simultaneously.Therefore, in gas-phase polyolefin production technique, reduce scaling, to block the impacts such as the loss of material that causes and environmental pollution particularly important, cycle of operation of extension fixture and the unplanned parking reducing device become the elementary object that industrial production is pursued.Too high service temperature can cause polyolefin particles to be clamminess and melting, and reactor assembly wall and other processing units can form fouling or sheeting.Reactor condition, heat extraction and effective catalyst performance all can have an impact to the operation of reactor assembly.
Patent US2008/002311 discloses a kind of system and method for the manufacture of alkene, relate to the various method and system be used in by oxygen in polyolefin polymerization reactor assembly, by first determining to produce poly optimum operating temperature in fluidized bed reaction system, the chromium oxide-based catalyst be reduced is selected according to optimum operating temperature, oxygen in order to make fouling minimize required significant quantity being added in fluidized bed reactor system, reducing the fouling tendency of reactive system.
Patent US2005/037891 discloses a kind of method preventing in gas-phase polyolefin polymerization process or suppress fouling, the method comprises makes medial temperature pass through processing unit higher than the gaseous mixture of its dew-point temperature, with the dew-point temperature of internal surface temperature lower than this gaseous mixture keeping described equipment, the processing unit internal surface condensed fluid being easy to fouling being soaked with keeping, structure speed can be reduced and long-lasting cleanliness.
Except by regulating the operation of reactive system to reduce scaling rate, also there is patent by adding scale inhibitor and inhibitor reduces scaling degree, the extension fixture cycle of operation.
Polymer beads sticks on reactor surface and inwall, and polymer beads liquid trends towards mutual adhesion, and forms agglomerate.Patent WO96/32420 discloses a kind of method preventing fouling and sheeting in Gas-phase reactor, and the method relates to heterophase polymerization process, comprises at least one annular-pipe reactor, is connected to Gas-phase reactor.By add coupling and appropriate scale inhibitor prevents fouling or sheeting in reactor.
Granules of catalyst or fine powder resin are easily recycled gas entrainment in loop, and recycle gas can be polymerized with it further further, increases the weight of the degree of fouling.Patent CN102627709A proposes and adopts a kind of gas-phase fluidized-bed production polyolefin process inhibitor injection device, on the reaction cycle loop of existing gas-phase fluidized-bed polyolefin process, this inhibitor injection device is connected in recycle gas compressor upstream, downstream or the dry gas seals system of itself, stop or suppress to be fluidized the fine powder resin that gas carries secretly out from gas-phase fluidized-bed reactor and continue polyreaction in circulation loop, thus prevent fouling, blocking, the prolongation cycle of operation.
Prior art has disclosed many relevant scale formations and has caused probing into of this phenomenon reason, and proposes corresponding terms of settlement.Regardless of scale formation reason, fouling can be reduced or eliminate is all very important progress.
Have now found that, add the inertia condensed components of high density at the gas-phase fluidized-bed reactive system of Low Density Polyethylene, powder resin feels like jelly, and resin melting index uprises.High density condensable components has ramollescence to polymer beads, and block in polyethylene reactive system grid distributor, interchanger, pipeline material be the powder resin carried secretly in circulation gas, by inert condensable component is added reactive system, reduce the scaling degree of the processing units such as reactor.Therefore the invention provides the on-line cleaning method of the gas-phase fluidized-bed reactive system of a kind of Low Density Polyethylene, by adding the inert condensable mixture of suitable solubility parameters in circulating current, and circulating current condensing deep and scavenging period in Reasonable Regulation And Control on-line cleaning process, reactor distributing plate, heat exchanger entrance barrier, suction port of compressor filter screen are effectively washed away and cleaned, reduce tamper, improve operational stability, effective extension fixture cycle of operation.
Summary of the invention
To be exactly object be exactly raises to overcome the grid distributor, interchanger blocking, the system pressure difference that occur in Low Density Polyethylene gas-phase fluidized-bed reactive system long-term operation process in the present invention, remove the problems such as heat energy power reduction and the one that provides alleviates reactive system fouling, blocking, extends the on-line cleaning method of not stopping of the cycle of operation.
A kind of on-line cleaning method for the production of the gas-phase fluidized-bed reactive system of Low Density Polyethylene provided by the present invention, described method comprises:
(1) this gas-phase fluidized-bed in circulated by monomer ethylene, comonomer, rare gas element and other components at least partly.
(2) during on-line cleaning, add inert condensable component in circulating current, the solubility parameters of condensable components is at 6.5-9cal
1/2cm
-3/2in scope;
(3) after compressed, the condensation of circulating current, form gas-fluid two-phase mixture, and return gas-phase fluidized-bed, form circulation loop.
In one embodiment of the invention, condensed circulating current transfer line is identical with the phlegma conveying equipment for fluid substances supplemented, circulating current mix with supplementary phlegma laggard enter fluidized-bed reactor bottom.
In one embodiment of the invention, condensed circulating current first passes through gas-liquid separator, condensate tank is connected with after gas-liquid separator, condensed circulating current is after gas-liquid separation, vapor phase stream stock is directly back to fluidized-bed reactor bottom by air-flow straight tube, liquid phase stream stock enters condensate tank as condensed fluid collection under differential pressure action, and liquid phase stream stock is back to fluidized-bed reactor by handling equipment in storage tank subsequently.
In one embodiment of the invention, described inert condensable component solubility parameters is preferably 7-8.5cal
1/2cm
-3/2.
In one embodiment of the invention, described inert condensable component is various paraffinic hydrocarbons and the naphthenic hydrocarbon of C4-C7, preferred iso-pentane, hexene and hexane.
In one embodiment of the invention, the amount of circulating current be 100-90000 ton/hour, be preferably 2000-70000 tons/hours; Pressure is 0.5-11MPa, is preferably 1.8-6MPa; Temperature is 30-140 DEG C, is preferably 60-98 DEG C; Adding inert condensable component concentration in inert condensable component Posterior circle air-flow is 5-70wt%, is preferably 7-30wt%.
In one embodiment of the invention, the pressure of described vapor phase stream stock is compared with the pressure of condensed circulating current, and pressure drop is 1-500KPa, is preferably 10-450KPa.
In one embodiment of the invention, in described gas-fluid two-phase mixture, liquid phase stream stock is 0.005-0.6 with the ratio of the mass rate of vapor phase stream stock, is preferably 0.01-0.4.
In one embodiment of the invention, the amount of described liquid phase stream stock is 10-100wt% of condensable components total amount in circulating current, is preferably 15-80wt%.
In one embodiment of the invention, the on-line cleaning time of described reactive system is 15h-1000h, is preferably 30h-500h.
In one embodiment of the invention, in on-line cleaning process, gas-phase fluidized-bed reactor pressure is 2.1-2.4MPa, and temperature is 70-110 DEG C.
In one embodiment of the invention, the liquid phase stream fluid streams handling equipment that condensate tank is derived can select impeller pump.
Accompanying drawing explanation
Fig. 1 be according to the gas-phase fluidized-bed reactive system on-line cleaning of a kind of Low Density Polyethylene of the present invention the first embodiment process flow sheet of being suitable for;
Fig. 2 be according to the gas-phase fluidized-bed lower reactive system on-line cleaning of a kind of Low Density Polyethylene of the present invention the second embodiment process flow sheet of being suitable for;
In figure:
1 represents the fluidized-bed reactor for the production of Low Density Polyethylene;
2 represent grid distributor in fluidized-bed reactor;
3 represent the compressor being used for compression cycle air-flow;
4 expressions are used for the condenser of the circulating current after condensation compression;
4 expressions are used for the condenser of the circulating current after condensation compression;
5 represent the storage tank for storing phlegma;
6 represent the conveying equipment for fluid substances be connected with storage tank 5;
7 represent the valve be connected with circulation line with conveying equipment for fluid substances 6.
8 represent the gas-liquid separator for separating of condensed circulating current;
9 are shown in the valve that gas-liquid separator liquid stream arm is connected with condensate tank;
10 represent the condensate tank be connected with gas-liquid separator liquid stream arm;
11 represent the conveying equipment for fluid substances be connected with storage tank 10;
12 represent the valve be connected with fluidized-bed with conveying equipment for fluid substances 11.
Fig. 3 is with scavenging period pressure reduction changing trend diagram.
Embodiment
Although referential embodiment describes the present invention, it will be understood by those skilled in the art that when without departing from the spirit and scope of the present invention, various change and amendment can be made.Therefore the invention is not restricted to as implementing particular disclosed in best mode of the present invention, but comprise the embodiment fallen within the scope of appended claims.
As shown in Figure 1, in a preferred embodiment of the invention, under certain polymerization temperature and pressure, recycle gas is by fluidized-bed reactor, and vinyl monomer is partially polymerized, recycle gas heat temperature raising.The circulating current of deriving from fluidized-bed reactor top of fresh reactant first mix with feed ethylene and hydrogen, enters the boosting of circulating current compressor, then with supplementary comonomer with reclaim monomer and mix, enter the condensation of circulating current condenser portion.Condensate tank is communicated with condensed circulating current pipeline by the extraction pipeline of conveying equipment for fluid substances, realizes circulating current and is delivered to fluidized-bed reactor with the phlegma parallel feeding supplemented, and is conducive to preventing fluidisation from wearing reactor and produces hydrops.
As shown in Figure 2, in a preferred embodiment of the invention, under certain polymerization temperature and pressure, recycle gas is by fluidized-bed reactor, and vinyl monomer is partially polymerized, recycle gas heat temperature raising.The circulating current of deriving from fluidized-bed reactor top of fresh reactant first mix with feed ethylene and hydrogen, enters the boosting of circulating current compressor, then with supplementary comonomer with reclaim monomer and mix, enter the condensation of circulating current condenser portion.Condensed circulating current enters gas-liquid separator and carries out gas-liquid separation, and the vapor phase stream stock be separated in gas-liquid separator returns to fluidized-bed bottom by airflow manifold.In gas-liquid separator, isolated phlegma enters storage tank by liquid stream arm, and then phlegma returns fluidized-bed reactor by the extraction pipeline of conveying equipment for fluid substances.
Embodiment 1
The gas-phase fluidized-bed on-line cleaning technical process of Low Density Polyethylene is as shown in Figure 1 adopted to clean.Adopt Z-N catalyzer, control gas-phase fluidized-bed reactor reaction pressure 2.3MPa, temperature of reaction is 86 DEG C.The circulating current of deriving from fluidized-bed top comprises ethene, butene-1, iso-pentane, hydrogen, nitrogen, methane, ethane etc., and supplement in circulating current and add iso-pentane, condensable iso-pentane accounts for 18% of circulating current total amount.Circulating current is compressed, after condensation, form gas-liquid mixture, wherein density of gas phase is 26kg/m
3, liquid phase stream stock is mainly iso-pentane, and density is 597kg/m
3, the amount of liquid phase stream stock accounts for 89% of the total amount of the condensable materials in circulating current, and the pressure of vapor phase stream stock is 12KPa with the pressure phase specific pressure drop of condensed circulating current, and the on-line cleaning time is 45h.Under equal control condition, find before the cleaning of contrast reactive system with after cleaning, reactive system total pressure head have dropped 25KPa, and interchanger log-mean temperature difference improves 10.5 DEG C, and remove heat energy power and significantly improve, reactive system inside obtains on-line cleaning.After cleaning, reaction load meets the requirement running 17.0T/h, constant product quality, respond well.
During to the present embodiment reactive system on-line cleaning, each device is shown in Fig. 3 with scavenging period pressure reduction changing trend diagram.
Contrast is carried out in table 1 to device pressure reduction change each before the present embodiment on-line cleaning and after on-line cleaning.
Device pressure reduction change numerical value contrast before and after butene-1 trade mark on-line cleaning produced by table 1
Embodiment 2
The gas-phase fluidized-bed on-line cleaning technical process of Low Density Polyethylene is as shown in Figure 1 adopted to clean.
Adopt Z-N catalyzer, control gas-phase fluidized-bed reactor reaction pressure 2.35MPa, temperature of reaction is 87 DEG C.The circulating current of deriving from fluidized-bed top comprises ethene, hexene-1, hydrogen, nitrogen, methane, ethane etc., and supplement in circulating current and add hexene, wherein condensable hexene accounts for 23% of circulating current total amount.Circulating current is compressed, after condensation, form gas-liquid mixture, wherein density of gas phase is 29kg/m
3, liquid phase stream stock is hexene, and density is 650kg/m
3, the amount of liquid phase stream stock accounts for 60% of the total amount of the condensable materials in circulating current, and the pressure of vapor phase stream stock is 6KPa with the pressure phase specific pressure drop of condensed circulating current, and the on-line cleaning time is 86h.Under equal control condition, the cleaning of contrast reactive system is front and after cleaning, reactive system total pressure head have dropped 20KPa, and the log-mean temperature difference of interchanger improves 9.7 DEG C, and remove heat energy power and significantly improve, reactive system inside obtains on-line cleaning.After cleaning, reaction load meets the requirement running 17.0T/h, constant product quality, respond well.
Contrast is carried out in table 2 to device pressure reduction change each before the present embodiment on-line cleaning and after on-line cleaning.
Device pressure reduction change numerical value contrast before and after hexene-1 trade mark on-line cleaning produced by table 2
Embodiment 3
The gas-phase fluidized-bed reactive system of Low Density Polyethylene is as shown in Figure 2 adopted to carry out on-line cleaning.
Adopt Z-N catalyzer, control gas-phase fluidized-bed reactor reaction pressure 2.3MPa, temperature of reaction is 86 DEG C.The circulating current of deriving from fluidized-bed top comprises ethene, butene-1, iso-pentane, hydrogen, nitrogen, methane, ethane etc., and wherein condensable iso-pentane accounts for 20% of circulating current total amount.Circulating current is compressed, after condensation, enter gas-liquid separator and be separated.Being separated the density of gas phase obtained is 27kg/m
3, liquid phase stream stock is iso-pentane, and density is 600kg/m
3, the amount of liquid phase stream stock accounts for 87% of the total amount of the condensable materials in circulating current, and the pressure of vapor phase stream stock is 11KPa with the pressure phase specific pressure drop of condensed circulating current, and the on-line cleaning time is 40h.Under equal control condition, contrast reactive system cleaning before with cleaning after, reactive system total pressure head have dropped 29KPa, and interchanger log-mean temperature difference improves 11.3 DEG C, heat energy power of removing significantly improve, reactive system inside obtains on-line cleaning.After cleaning, reaction load meets the requirement running 17.0T/h, constant product quality, respond well.
Contrast is carried out in table 3 to device pressure reduction change each before the present embodiment on-line cleaning and after on-line cleaning.
Device pressure reduction change numerical value contrast before and after butene-1 trade mark on-line cleaning produced by table 3
Embodiment 4
The gas-phase fluidized-bed reactive system of Low Density Polyethylene is as shown in Figure 2 adopted to carry out on-line cleaning.
Adopt Z-N catalyzer, control gas-phase fluidized-bed reactor reaction pressure 2.3MPa, temperature of reaction is 86 DEG C.The circulating current of deriving from fluidized-bed top comprises ethene, hexene-1, iso-pentane, hydrogen, nitrogen, methane, ethane etc., and wherein condensable hexene and iso-pentane account for 25% of circulating current total amount.Circulating current is compressed, after condensation, enter gas-liquid separator and be separated.Being separated the density of gas phase obtained is 28kg/m
3, liquid phase stream stock is iso-pentane, and density is 632kg/m
3, the amount of liquid phase stream stock accounts for 67% of the total amount of the condensable materials in circulating current, and the pressure of vapor phase stream stock is 6KPa with the pressure phase specific pressure drop of condensed circulating current, and the on-line cleaning time is 53h.Under equal control condition, the cleaning of contrast reactive system is front and after cleaning, reactive system total pressure head have dropped 24KPa, and the log-mean temperature difference of interchanger improves 10.1 DEG C, and remove heat energy power and significantly improve, reactive system inside obtains on-line cleaning.After cleaning, reaction load meets the requirement running 17.0T/h, constant product quality, respond well.
Contrast is carried out in table 4 to device pressure reduction change each before the present embodiment on-line cleaning and after on-line cleaning.
Device pressure reduction change numerical value contrast before and after butene-1 trade mark on-line cleaning produced by table 4
As can be seen from above four embodiments, utilize the on-line cleaning method of the gas-phase fluidized-bed reactive system of Low Density Polyethylene according to the present invention, can reactor distributing plate, heat exchanger entrance barrier, suction port of compressor filter screen effectively be washed away and be cleaned, reduce tamper, reactive system total pressure drop declines, reactive system inside obtains on-line cleaning, improves operational stability, effectively extends the cycle of operation.
Claims (10)
1. for the production of an on-line cleaning method for the gas-phase fluidized-bed reactive system of Low Density Polyethylene, it is characterized in that, described method comprises:
(1) from gas-phase fluidized-bed middle export section gas as circulating current, circulate;
(2), during on-line cleaning, in the circulating current after compression condensation, add inert condensable component, the solubility parameters of inert condensable component is at 6.5-9cal
1/2cm
-3/2in scope;
(3) after compressed, the condensation of circulating current, form gas-fluid two-phase mixture, and return gas-phase fluidized-bed, form circulation loop.
2. method according to claim 1, is characterized in that, described inert condensable component solubility parameters is preferably 7-8.5cal
1/2cm
-3/2.
3. method according to claim 1, is characterized in that, described inert condensable component is various paraffinic hydrocarbons and the naphthenic hydrocarbon of C4-C7,
4. method according to claim 1, is characterized in that, described inert condensable component is preferred iso-pentane, hexene and hexane.
5. method according to claim 1, it is characterized in that, described circulating current component comprises monomer ethylene, comonomer and rare gas element, the amount of the circulating current of circulating current be 50-90000 ton/hour, pressure is 0.5-10MPa, temperature is 30-120 DEG C, and adding inert condensable component concentration in inert condensable component Posterior circle air-flow is 2-70wt%.
6. method according to claim 1, is characterized in that, the pressure of vapor phase stream stock in described gas-fluid two-phase mixture is compared with the pressure of the circulating current before condensation, and pressure drop is 1-500KPa.
7. method according to claim 1, is characterized in that, in described gas-fluid two-phase mixture, liquid phase stream stock is 0.005-0.6 with the ratio of the mass rate of vapor phase stream stock.
8. method according to claim 7, is characterized in that, the amount of described liquid phase stream stock is 10-100wt% of inert condensable component total amount in circulating current.
9. method according to claim 1, is characterized in that, the described on-line cleaning time is 20h-1000h, and in on-line cleaning process, gas-phase fluidized-bed reactor pressure is 2.1-2.4MPa, and temperature is 70-110 DEG C.
10. method according to claim 1, in described circulating current, vapor phase stream stock enters reactor from distributing plate of fluidized-bed reactor bottom, and liquid phase enters reactor and enters reactor from distributing plate of fluidized-bed reactor bottom and/or grid distributor top.
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|---|---|---|---|
| CN201510657016.4A CN105237665B (en) | 2015-10-12 | 2015-10-12 | A kind of on-line cleaning method for being used to produce the gas-phase fluidized-bed reaction system of low density polyethylene (LDPE) |
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|---|---|---|---|
| CN201510657016.4A CN105237665B (en) | 2015-10-12 | 2015-10-12 | A kind of on-line cleaning method for being used to produce the gas-phase fluidized-bed reaction system of low density polyethylene (LDPE) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108218661A (en) * | 2016-12-22 | 2018-06-29 | 阿克森斯公司 | Use the alkene oligomerization process of cleaning device |
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| CN1438250A (en) * | 2002-12-17 | 2003-08-27 | 中国石油化工股份有限公司 | Condensation and cooling combined gas-phase fluidized-bed polymerization method and apparatus |
| CN101284889A (en) * | 2008-06-03 | 2008-10-15 | 中国石油化工集团公司 | Improvement of manner for introducing condensation agent into fluidised bed polymerisation reactor and device |
| CN101432320A (en) * | 2006-05-12 | 2009-05-13 | 尤尼威蒂恩技术有限责任公司 | Low molecular weight induced condensing agents |
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| US6096837A (en) * | 1995-04-12 | 2000-08-01 | Borealis Polymers Oy | Method for preventing fouling and sheeting in gas phase reactors |
| CN1438250A (en) * | 2002-12-17 | 2003-08-27 | 中国石油化工股份有限公司 | Condensation and cooling combined gas-phase fluidized-bed polymerization method and apparatus |
| CN101432320A (en) * | 2006-05-12 | 2009-05-13 | 尤尼威蒂恩技术有限责任公司 | Low molecular weight induced condensing agents |
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