CN105237665B - A kind of on-line cleaning method for being used to produce the gas-phase fluidized-bed reaction system of low density polyethylene (LDPE) - Google Patents
A kind of on-line cleaning method for being used to produce the gas-phase fluidized-bed reaction system of low density polyethylene (LDPE) Download PDFInfo
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- CN105237665B CN105237665B CN201510657016.4A CN201510657016A CN105237665B CN 105237665 B CN105237665 B CN 105237665B CN 201510657016 A CN201510657016 A CN 201510657016A CN 105237665 B CN105237665 B CN 105237665B
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Abstract
The invention discloses a kind of on-line cleaning method for being used to produce the gas-phase fluidized-bed reaction system of low density polyethylene (LDPE).From gas-phase fluidized-bed middle export section gas as circulating current, it is circulated；During on-line cleaning, inert condensable component is added into the circulating current after compression condensation, the solubility parameters of inert condensable component is in 6.5-9cal1/2·cm‑3/2In the range of；Circulating current is compressed, after condensation, forms gas-fluid two-phase mixture, and returns gas-phase fluidized-bed, constitutes circulation loop.The present invention regulates and controls to condensing deep and on-line cleaning time, online effectively cleaning is carried out to reaction system, extension fixture run time, overcome the distribution grid occurred during the gas-phase fluidized-bed reaction system long-term operation of low density polyethylene (LDPE), heat exchanger block, system pressure difference rise, remove the problems such as heat energy power is reduced.
Description
Technical field
The present invention relates to production low density polyethylene (LDPE) gas-phase fluidized-bed reaction system on-line cleaning method, especially by
Consider softening and dissolution of the addition of inert condensable mixture to polyvinyl resin, added in circulating current suitable molten
The inert condensable mixture of parameter is spent, and condensing deep and on-line cleaning time are regulated and controled, reaction system is carried out
Line is effectively cleaned, extension fixture run time.
Background technology
In continuous gas-phase fluidized-bed polyethylene polymerization technique, the difficulty of plant running is to control fluidized state.Fluidisation
State is deteriorated, and hot localised points cause easily sheeting occur in reactor, and sheeting can deteriorate further fluidized status, in fact it could happen that quilt
Compel parking and reactor implode.The presence of fine powder and high activity particle causes gas-phase fluidized-bed polyethylene reaction system inner-walls of duct
Gradually fouling, heat exchanger, distribution grid are gradually blocked.Without cleaning distribution grid can be caused to block seriously for a long time, fluidized state
It is deteriorated, and then triggers parking accident.With the development of national economy, polyvinyl resin demand is continuously increased, but periodically parking
Cleaning distribution grid and reactor can lose a large amount of materials, cause that the gas-phase fluidized-bed polyolefin device cycle of operation is short, and efficiency is low, damage
Lose greatly, while waste gas is set fire, torch can also cause environmental pollution.Therefore, in gas-phase polyolefin production technology reduce scaling,
The influence such as loss of material and environmental pollution is particularly important caused by blocking, the cycle of operation of extension fixture and the non-meter for reducing device
Drawing parking turns into the elementary object that industrial production is pursued.Too high operation temperature can cause polyolefin particles tacky and melt,
Fouling or sheeting can be formed on reactor assembly wall and other process equipments.Reactor condition, except heat and effective catalyst
Influence can be produced on the operation of reactor assembly.
Patent US2008/002311 discloses a kind of system and method for manufacturing alkene, is related to and various is used in oxygen
Method and system in polyolefin polymerization reactor assembly, by first determining to produce polyethylene most in fluidized bed reaction system
Good operation temperature, the chromium oxide-based catalyst for selecting to be reduced according to optimum operating temperature will be in order that fouling minimizes institute
Need the oxygen of effective dose to add into fluidized bed reactor system, reduce the fouling tendency of reaction system.
Patent US2005/037891 discloses a kind of side for being prevented in gas-phase polyolefin polymerization process or suppressing fouling
Method, this method includes making mean temperature higher than the admixture of gas of its dew-point temperature by process equipment, and keeps the equipment
Internal surface temperature be less than the admixture of gas dew-point temperature so that be easy to fouling process equipment inner surface condensed fluid and
Wetting is kept, structure speed and long-lasting cleanliness can be reduced.
Except reducing scaling rate by the operation for adjusting reaction system, also there is patent by adding scale preventative and inhibitor
To reduce scaling degree, the extension fixture cycle of operation.
Polymer beads are sticked in reactor surface and inwall, and polymer beads liquid is intended to adhere to each other, and is formed
Agglomerate.Patent WO96/32420 discloses a kind of method for preventing fouling and sheeting in Gas-phase reactor, and this method is related to multiphase
Polymerization process, including at least one annular-pipe reactor, are connected to Gas-phase reactor.Prevented by addition matching and appropriate scale preventative
Fouling or sheeting in reactor.
Catalyst granules or fine powder resin are easily entrained in loop by recyclegas, and recyclegas can further with its
Further polymerization, aggravates the degree of fouling.Patent CN102627709A is proposed using a kind of gas-phase fluidized-bed production polyolefin
Technique inhibitor injection device, on the reaction cycle loop of existing gas-phase fluidized-bed polyolefin process, by the inhibitor
Injection device is connected in recycle gas compressor upstream, downstream or the dry gas seals system of itself, is prevented or is suppressed to be fluidized
Gas is entrained with the fine powder resin come from gas-phase fluidized-bed reactor and continues polymerisation in circulation loop, so as to prevent knot
Dirt, blocking, the extension cycle of operation.
Prior art has been disclosed many relevant scale formations and causes probing into for this phenomenon reason, and proposes corresponding
Solution.Regardless of scale formation reason, it is all very important progress that fouling, which can be reduced or eliminated,.
It has been found that the inertia condensed components of the gas-phase fluidized-bed reaction system addition high concentration in low density polyethylene (LDPE),
Powder resin feels like jelly, and resin melting index is uprised.High concentration condensable components have emollescence to polymer beads, and polyethylene
Distribution grid, heat exchanger, the material of pipeline are blocked in reaction system and is the powder resin carried secretly in circulating air, can be by by inertia
Condensable components add reaction system, reduce the scaling degree of the process equipments such as reactor.Therefore the invention provides one kind is low
The on-line cleaning method of the gas-phase fluidized-bed reaction system of density polyethylene, by adding suitable solubility parameters in circulating current
Circulating current condensing deep and scavenging period during inert condensable mixture, and Reasonable Regulation And Control on-line cleaning, to reactor
Distribution grid, heat exchanger entrance barrier, suction port of compressor filter screen are effectively washed away and cleaned, and reduce tamper, improve operation steady
It is qualitative, effective extension fixture cycle of operation.
The content of the invention
The present invention is exactly that purpose is exactly to overcome the gas-phase fluidized-bed reaction system long-term operation mistake of low density polyethylene (LDPE)
The distribution grid that occurs in journey, heat exchanger are blocked, system pressure difference rise, remove the problems such as heat energy power is reduced and provide a kind of mitigate anti-
Scaling, blocking are answered, extends the not parking on-line cleaning method of the cycle of operation.
A kind of on-line cleaning method for being used to produce the gas-phase fluidized-bed reaction system of low density polyethylene (LDPE) provided by the present invention,
Methods described includes：
(1) enter during this is gas-phase fluidized-bed at least partially by monomer ethylene, comonomer, inert gas and other components
Row circulation.
(2) during on-line cleaning, inert condensable component is added into circulating current, the solubility parameters of condensable components exists
6.5—9cal1/2·cm-3/2In the range of；
(3) circulating current it is compressed, condensation after, formed gas-fluid two-phase mixture, and return it is gas-phase fluidized-bed, constitute circulation
Loop.
In one embodiment of the invention, condensed circulating current transfer pipeline and the condensate liquid fluid supplemented are defeated
Send equipment identical, circulating current mixes laggard fluidized bed reactor lower part with the condensate liquid supplemented.
In one embodiment of the invention, condensed circulating current first passes through gas-liquid separator, in gas-liquid separation
Condensate tank is connected with after device, condensed circulating current is after gas-liquid separation, and gas phase stream stock is directly returned by air-flow straight tube
Fluidized-bed reactor bottom is back to, liquid phase stream stock is collected into condensate tank under differential pressure action as condensate liquid, subsequent liquid phase
Stock is flowed from fluidized-bed reactor is back to by conveying equipment in storage tank.
In one embodiment of the invention, the inert condensable component solubility parameters is preferably 7-8.5cal1 /2·cm-3/2。
In one embodiment of the invention, the inert condensable component for C4-C7 various paraffinic hydrocarbonses and
Cycloalkane, preferably isopentane, hexene and hexane.
In one embodiment of the invention, the amount of circulating current be 100-90000 ton hours, preferably 2000-
70000 ton hours；Pressure is 0.5-11MPa, preferably 1.8-6MPa；Temperature is 30-140 DEG C, preferably 60-98 DEG C；
It is 5-70wt%, preferably 7-30wt% to add inert condensable constituent content in inert condensable component Posterior circle air-flow.
In one embodiment of the invention, the pressure phase of the pressure and condensed circulating current of the gas phase stream stock
Than pressure drop is 1-500KPa, preferably 10-450KPa.
In one embodiment of the invention, liquid phase stream strand and the quality of gas phase stream stock in the gas-fluid two-phase mixture
The ratio between flow is 0.005-0.6, preferably 0.01-0.4.
In one embodiment of the invention, the amount of the liquid phase stream stock is condensable components total amount in circulating current
10-100wt%, preferably 15-80wt%.
In one embodiment of the invention, the on-line cleaning time of the reaction system is 15h -1000h, preferably
For 30h -500h.
In one embodiment of the invention, during on-line cleaning, gas-phase fluidized-bed reactor pressure be 2.1-
2.4MPa, temperature is 70-110 DEG C.
In one embodiment of the invention, liquid phase stream fluid streams conveying equipment derived from condensate tank may be selected from
Heart pump.
Brief description of the drawings
Fig. 1 is applicable according to a kind of gas-phase fluidized-bed reaction system on-line cleaning of low density polyethylene (LDPE) of the present invention
The first embodiment process chart；
Fig. 2 is fitted according to a kind of gas-phase fluidized-bed lower reaction system on-line cleaning of low density polyethylene (LDPE) of the present invention
Second embodiment process chart；
In figure：
1 represents the fluidized-bed reactor for producing low density polyethylene (LDPE)；
2 represent distribution grid in fluidized-bed reactor；
3 represent the compressor for compressed recycle gas stream；
4 represent the condenser for condensing the circulating current after compression；
4 represent the condenser for condensing the circulating current after compression；
5 represent the storage tank for storing condensate liquid；
The conveying equipment for fluid substances that 6 expressions are connected with storage tank 5；
The valve that 7 expressions are connected with conveying equipment for fluid substances 6 and circulation line.
8 represent the gas-liquid separator for separating condensed circulating current；
9 are shown in the valve that gas-liquid separator liquid stream branch pipe is connected with condensate tank；
The condensate tank that 10 expressions are connected with gas-liquid separator liquid stream branch pipe；
The conveying equipment for fluid substances that 11 expressions are connected with storage tank 10；
The valve that 12 expressions are connected with conveying equipment for fluid substances 11 and fluid bed.
Fig. 3 is with scavenging period pressure difference changing trend diagram.
Embodiment
Although referential embodiment describes the present invention, it will be understood by those skilled in the art that without departing from the present invention
Spirit and scope in the case of, various changes and modifications can be made.Therefore the invention is not restricted to be used as the implementation present invention's
Particular disclosed in best mode, but the embodiment including falling within the scope of the accompanying claims.
As shown in figure 1, in a preferred embodiment of the invention, under certain polymerization temperature and pressure, circulating air
Body is by fluidized-bed reactor, and vinyl monomer is partially polymerized, recyclegas heat temperature raising.Fresh reactant from fluidized-bed reactor
Circulating current derived from top is first mixed with feed ethylene and hydrogen, is boosted into circulating current compressor, then is total to supplement
Polycondensation monomer and recovery monomer mixing, into the condensation of circulating current condenser portion.Condensate tank passes through conveying equipment for fluid substances
Draw pipeline to communicate with condensed circulating current pipeline, realize that circulating current and the condensate liquid mixed feeding of supplement are delivered to stream
Fluidized bed reactor, is conducive to preventing that fluidisation from wearing reactor and producing hydrops.
As shown in Fig. 2 in a preferred embodiment of the invention, under certain polymerization temperature and pressure, circulating air
Body is by fluidized-bed reactor, and vinyl monomer is partially polymerized, recyclegas heat temperature raising.Fresh reactant from fluidized-bed reactor
Circulating current derived from top is first mixed with feed ethylene and hydrogen, is boosted into circulating current compressor, then is total to supplement
Polycondensation monomer and recovery monomer mixing, into the condensation of circulating current condenser portion.Condensed circulating current enters gas-liquid separation
The gas phase stream stock that device separated in gas-liquid separation, gas-liquid separator returns to fluid bed bottom by airflow manifold.Gas-liquid
The condensate liquid isolated in separator enters storage tank by liquid stream branch pipe, the fairlead that then condensate liquid passes through conveying equipment for fluid substances
Road returns to fluidized-bed reactor.
Embodiment 1
Cleaned using the gas-phase fluidized-bed on-line cleaning technological process of low density polyethylene (LDPE) as shown in Figure 1.
Using Z-N catalyst, gas-phase fluidized-bed reactor reaction pressure 2.3MPa is controlled, reaction temperature is 86 DEG C,.From stream
Changing circulating current derived from bed top includes ethene, butene-1, isopentane, hydrogen, nitrogen, methane, ethane etc., in circulating current
Middle supplement adds isopentane, and condensable isopentane accounts for the 18% of circulating current total amount.Circulating current is compressed, after condensation, shape
Into gas-liquid mixture, wherein density of gas phase is 26kg/m3, liquid phase stream stock is mainly isopentane, and density is 597kg/m3, liquid phase stream
The 89% of the total amount for the condensable materials that the amount of stock is accounted in circulating current, pressure and the condensed circulating current of gas phase stream stock
Pressure is 12KPa compared to pressure drop, and the on-line cleaning time is 45h.It is before contrast reaction system cleaning and clear under equal control condition
Found after washing, reaction system total pressure head have dropped 25KPa, and heat exchanger logarithmic mean temperature difference (LMTD) improves 10.5 DEG C, removes heat energy power bright
It is aobvious to improve, obtain on-line cleaning inside reaction system.After cleaning, reaction load meets operation 17.0T/h requirement, product quality
It is stable, work well.
During to the present embodiment reaction system on-line cleaning, each device is shown in Fig. 3 with scavenging period pressure difference changing trend diagram.
Contrast is carried out to each device pressure difference change before the present embodiment on-line cleaning and after on-line cleaning and is shown in Table 1.
Device pressure difference change numerical value contrast before and after the production butene-1 trade mark on-line cleaning of table 1
Embodiment 2
Cleaned using the gas-phase fluidized-bed on-line cleaning technological process of low density polyethylene (LDPE) as shown in Figure 1.
Using Z-N catalyst, gas-phase fluidized-bed reactor reaction pressure 2.35MPa is controlled, reaction temperature is 87 DEG C,.From
Circulating current derived from fluid bed top includes ethene, hexene -1, hydrogen, nitrogen, methane, ethane etc., is mended in circulating current
Addition hexene is filled, wherein condensable hexene accounts for the 23% of circulating current total amount.Circulating current is compressed, after condensation, forms gas
Liquid mixture, wherein density of gas phase are 29kg/m3, liquid phase stream stock is hexene, and density is 650kg/m3, the amount of liquid phase stream stock, which is accounted for, to be followed
The 60% of the total amount of condensable materials in ring air-flow, the pressure of gas phase stream stock is pressed compared with the pressure of condensed circulating current
6KPa is reduced to, the on-line cleaning time is 86h.Under equal control condition, before contrast reaction system cleaning and after cleaning, reaction system
System total pressure head have dropped 20KPa, and the logarithmic mean temperature difference (LMTD) of heat exchanger improves 9.7 DEG C, removes heat energy power and significantly improves, reaction system
Inside obtains on-line cleaning.After cleaning, reaction load meets operation 17.0T/h requirement, and product quality is stable, works well.
Contrast is carried out to each device pressure difference change before the present embodiment on-line cleaning and after on-line cleaning and is shown in Table 2.
Device pressure difference change numerical value contrast before and after the production trade mark on-line cleaning of hexene -1 of table 2
Embodiment 3
On-line cleaning is carried out using the gas-phase fluidized-bed reaction system of low density polyethylene (LDPE) as shown in Figure 2.
Using Z-N catalyst, gas-phase fluidized-bed reactor reaction pressure 2.3MPa is controlled, reaction temperature is 86 DEG C,.From stream
Changing circulating current derived from bed top includes ethene, butene-1, isopentane, hydrogen, nitrogen, methane, ethane etc., wherein condensable
Isopentane account for the 20% of circulating current total amount.Circulating current is compressed, after condensation, is separated into gas-liquid separator.Point
It is 27kg/m from obtained density of gas phase3, liquid phase stream stock is isopentane, and density is 600kg/m3, liquid phase stream stock amount account for circulating air
The 87% of the total amount of condensable materials in stream, the pressure drop compared with the pressure of condensed circulating current of the pressure of gas phase stream stock is
11KPa, the on-line cleaning time is 40h.Under equal control condition, before contrast reaction system cleaning and after cleaning, reaction system
Total pressure head have dropped 29KPa, and heat exchanger logarithmic mean temperature difference (LMTD) improves 11.3 DEG C, heat energy power of removing significantly improve, reaction system
Inside obtains on-line cleaning.After cleaning, reaction load meets operation 17.0T/h requirement, and product quality is stable, works well.
Contrast is carried out to each device pressure difference change before the present embodiment on-line cleaning and after on-line cleaning and is shown in Table 3.
Device pressure difference change numerical value contrast before and after the production butene-1 trade mark on-line cleaning of table 3
Embodiment 4
On-line cleaning is carried out using the gas-phase fluidized-bed reaction system of low density polyethylene (LDPE) as shown in Figure 2.
Using Z-N catalyst, gas-phase fluidized-bed reactor reaction pressure 2.3MPa is controlled, reaction temperature is 86 DEG C,.From stream
Changing circulating current derived from bed top includes ethene, hexene -1, isopentane, hydrogen, nitrogen, methane, ethane etc., wherein condensable
Hexene and isopentane account for the 25% of circulating current total amount.Circulating current is compressed, after condensation, is divided into gas-liquid separator
From.Isolated density of gas phase is 28kg/m3, liquid phase stream stock is isopentane, and density is 632kg/m3, liquid phase stream stock amount account for
The 67% of the total amount of condensable materials in circulating current, the pressure of gas phase stream stock is compared with the pressure of condensed circulating current
Pressure drop is 6KPa, and the on-line cleaning time is 53h.Under equal control condition, before contrast reaction system cleaning and after cleaning, reaction
Overall system pressure drop have dropped 24KPa, and the logarithmic mean temperature difference (LMTD) of heat exchanger improves 10.1 DEG C, removes heat energy power and significantly improves, reaction
Internal system obtains on-line cleaning.After cleaning, reaction load meets operation 17.0T/h requirement, and product quality is stable, and effect is good
It is good.
Contrast is carried out to each device pressure difference change before the present embodiment on-line cleaning and after on-line cleaning and is shown in Table 4.
Device pressure difference change numerical value contrast before and after the production butene-1 trade mark on-line cleaning of table 4
As can be seen that utilizing the gas-phase fluidized-bed reaction of low density polyethylene (LDPE) according to the present invention in four embodiments more than
The on-line cleaning method of system, can effectively be washed away to reactor distributing plate, heat exchanger entrance barrier, suction port of compressor filter screen
And cleaning, tamper is reduced, reaction system overall presure drop declines, and on-line cleaning is obtained inside reaction system, improves operational stability,
Effectively extend the cycle of operation.
Claims (10)
1. a kind of on-line cleaning method for being used to produce the gas-phase fluidized-bed reaction system of low density polyethylene (LDPE), it is characterised in that institute
The method of stating includes：
（1）From gas-phase fluidized-bed middle export section gas as circulating current, it is circulated；
（2）During on-line cleaning, inert condensable component is added into the circulating current after compression condensation, inert condensable component
Solubility parameters is in 6.5-9 cal1/2·cm-3/2In the range of；
（3）Circulating current is compressed, after condensation, forms gas-fluid two-phase mixture, and returns gas-phase fluidized-bed, and composition is recycled back to
Road.
2. according to the method described in claim 1, it is characterised in that the inert condensable component solubility parameters is 7-8.5
cal1/2·cm-3/2。
3. according to the method described in claim 1, it is characterised in that the inert condensable component is C4-C7 various saturations
Alkane and cycloalkane.
4. according to the method described in claim 1, it is characterised in that the inert condensable component is isopentane or hexane.
5. according to the method described in claim 1, it is characterised in that the circulating current component includes monomer ethylene, copolymerization list
Body and inert gas, the amount of circulating current is 50-90000 ton hours, and pressure is 0.5-10 MPa, and temperature is 30-120
DEG C, it is 2-70 wt% to add inert condensable constituent content in inert condensable component Posterior circle air-flow.
6. according to the method described in claim 1, it is characterised in that the pressure of the gas phase stream stock in the gas-fluid two-phase mixture
Compared with the pressure of the circulating current before condensation, pressure drop is 1-500 KPa.
7. according to the method described in claim 1, it is characterised in that liquid phase stream stock and gas phase stream in the gas-fluid two-phase mixture
The ratio between mass flow of stock is 0.005-0.6.
8. method according to claim 7, it is characterised in that the amount of the liquid phase stream stock can be cold for inertia in circulating current
10-100 wt% of solidifying component total amount.
9. it is according to the method described in claim 1, it is characterised in that the on-line cleaning time is the h of 20h -1000, online clear
During washing, gas-phase fluidized-bed reactor pressure is 2.1-2.4 MPa, and temperature is 70-110 DEG C.
10. according to the method described in claim 1, in the circulating current gas phase stream stock from distributing plate of fluidized-bed reactor bottom
Into reactor, liquid phase enters reactor into reactor from distributing plate of fluidized-bed reactor bottom and/or distribution grid top.
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| US7696289B2 (en) * | 2006-05-12 | 2010-04-13 | Exxonmobil Chemical Patents Inc. | Low molecular weight induced condensing agents |
| CN100590136C (en) * | 2008-06-03 | 2010-02-17 | 中国石油化工集团公司 | Improvement of manner for introducing condensation agent into fluidised bed polymerisation reactor and device |
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