CN105233767A - Catalyst fast dispersion method - Google Patents
Catalyst fast dispersion method Download PDFInfo
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- CN105233767A CN105233767A CN201510657628.3A CN201510657628A CN105233767A CN 105233767 A CN105233767 A CN 105233767A CN 201510657628 A CN201510657628 A CN 201510657628A CN 105233767 A CN105233767 A CN 105233767A
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Abstract
The invention discloses a catalyst fast dispersion method. The method comprises determining a grain flow pattern in a reactor, determining axial height and radial depth of an outlet of a catalyst injection tube based on the grain flow pattern, and carrying out fast and uniform dispersion on the catalyst in the reactor under the condition of smooth catalyst injection. The axial height of the outlet of the catalyst injection tube is in a range of 0-1/4L of the lower part of a particle main cycle zone, the radial depth of the outlet is in a range of 1/4-3/4D in the main cycle zone, L represents the particle main cycle zone length and D represents the reactor diameter. The catalyst fast dispersion method realizes fast and uniform dispersion of the catalyst in a reactor and prevents polymer adhesion to wall and caking caused by nonuniform catalyst dispersion or catalyst adhesion to wall.
Description
Technical field
The present invention relates to catalyst rapid dispersion method, particularly based on the technology of the catalyst rapid dispersion of particle flow pattern detection.
Background technology
Catalytic reaction process is widely used in each industrial circle, in course of reaction, catalyst can dispersedly be in the feed this type of course of reaction can keep stablizing, crucial efficiently.In catalytic cracking reaction process, catalyst distribution inequality will cause local feedstock oil excessive fragmentation, and make catalyst coking and deactivation.In olefin polymerization process, when local catalyst concentrations is too high, local reaction will be too violent, thus produce a large amount of heat of polymerization and cannot remove in time, will form polymer lumps, and affect device stable operation in reactor.
Catalyst cracker is a kind of typical fast fluidized bed reactor, and CN102311758B discloses a kind of method that catalyst mixes with raw material Quick uniform.The method makes catalyst from radial or tangential direction injecting lift pipe reactor by the implant angle changing catalyst.CN101161618B discloses a kind of for adopting the raw material such as acetic acid or acetone through cracking for the method for implanting of catalyst when ketenes and derivative thereof and device.Adopt toroidal expansion tube to utilize shock and the Involving velocity of fluid, make liquid dispersed in short distance.Document 1 improves the uniformity of riser inner catalyst dispersion by layering injecting catalyst.For slurry-phase reactor, CN201372260Y discloses the catalyst injection device that slurry method produces high density polyethylene (HDPE), shortened the incorporation time of catalyst and hexane by the position changing triple valve, and adjust the frequency that catalyst charge angle reduces catalyst blockage.
Analyze existing document patent known, improve the homodisperse method of catalyst at present and mainly contain two kinds: be a kind of by changing catalyst charge tubular construction or the dispersion of charging angle optimization of catalysts; Another kind of realized by layering injecting catalyst that it is dispersed.But change catalyst injection pipe structure and angle only can ensure that catalyst is dispersed in ascending pipe porch, cannot ensure the uniformity that inside reactor catalyst disperses; And catalyst layering injection will make catalyst injection technology more complicated.Meanwhile, existing improvement project does not all consider the impact that reactor endoparticle fluidal texture is disperseed catalyst.For gas-phase polyethylene technique, CN100405027C discloses a kind of detection method of fluidized-bed reactor particle flow pattern, and the particle flow structure during detection discovery is gas-solid fluidized bed exists the large and small circulation Two-way Cycle flow pattern containing stagnant area.In gas-phase polyethylene technique, if catalyst injection pipe exit position is too high, catalyst will reach Bed level after entering reactor very soon, monomer polymerization time in catalyst duct is shorter, the polymer beads particle diameter formed is less, very easily be recycled gas to carry secretly and leave bed and enter in circulating air pipeline, not only cause serious catalyst loss, circulating gas pipe pipeline heat exchanger also can be caused to block.If catalyst injection pipe outlet is positioned at stagnant area, will piles up in this region after catalyst granules enters bed, cannot evenly spread in reactor, thus form caking in catalyst injection pipe exit, blocking catalyst charging, affect reactor stable operation.In addition, if catalyst injection pipe exit distance wall is excessively near, the catalyst spraying into bed forms polymer sheeting by being easily bonded on wall, and then affects reactor stable operation.
Disperse at inside reactor Quick uniform to enable catalyst, and consider the impact that particle flow pattern is disperseed catalyst, need to invent a kind of catalyst rapid dispersion technology detected based on inside reactor particle flow pattern, make catalyst rapid dispersion under the drive of particles circulating, and avoid because unreasonable and that cause sticky wall, caking are chosen in catalyst injection pipe exit position.
Summary of the invention
The present invention seeks to develop a kind of catalyst rapid dispersion method detected based on particle flow pattern, catalyst rapid dispersion in reactor can be made even, said method comprising the steps of:
A. reactor endoparticle flow pattern is determined;
B. based on particle flow pattern determination catalyst injection pipe outlet axial height and radial depth;
C. to jet catalyst in reactor, by sonic detection regulation and control catalyst ejector effect.
The detection of inside reactor particle flow pattern can adopt the methods such as sound wave detecting method, ray detection method, computational fluid dynamics simulation.In one embodiment of the invention, select particle flow pattern in sound wave detecting method determination reactor, concrete steps are as follows: (1) receives the acoustic emission signal of inside reactor by acoustic wave sensing system; (2) analyze the acoustic emission signal received, choose the frequency f of acoustic signals, amplitude A, ENERGY E, time t as characteristic value; (3) detect the changes in distribution of ENERGY E under the axial differing heights place characteristic frequency f of bed and/or amplitude A, determine the endocorpuscular flow pattern of fluid bed.Wherein acoustic wave sensing system comprises the sonic sensor, signal amplifying apparatus, signal pickup assembly, signal processing apparatus, the device displaying result that connect successively, acoustic wave sensing system comprises at least one sonic sensor, and sonic sensor adopts the mounting means of non-intrusion type.The distribution of sonic sensor is the wall place of distribution grid to height of materials H in bed of reactor.
The dynamic acoustic signals of inside reactor enters by the acoustic receiver device at the wall place being arranged on more than reactor distributing plate the amplification that amplifying device carries out signal, to ensure long unattenuated apart from interior signal, then enter the A/D conversion that acoustical signal harvester carries out signal, finally enter acoustic signals treating apparatus (computer) and carry out processing and analyzing.
Collect above fluid bed material level, acoustic signals t change in time near material level and below material level, above material level, the amplitude of acoustic signals is very little, and it is comparatively sparse, this is because belong to fluid bed dilute phase above material level, particle is rare and particle diameter is relatively little, and the amplitude that particles collision wall is produced is less.And near material level, because launching during bubble effusion bed surface acts on and carry effect secretly, cause and be thrown into the free spatial domain of fluid bed from bubble roof with from the particle of bubble trailing vortex because of bubble breaking, movement of particles is the most active herein, namely the acoustic energy that produces of particles collision wall and the fluctuation of acoustic signals also larger, cause acoustical signal amplitude comparatively large, and size variation is violent.Below material level, low near the overall comparatively material level of amplitude of acoustic signals, and amplitude is comparatively even, stable, simultaneously because granule density is comparatively large, therefore signal is very intensive, shows that this region belongs to the relatively sluggish emulsion zone of particle activity.
In one embodiment of the invention, obtaining particle flow pattern in fluidized-bed reactor by sound wave detecting method is large and small circulation Two-way Cycle fluidal texture containing stagnant area, and wherein particle major cycle length is L.
In one embodiment of the invention, the ascending pipe outlet axial height of catalyst is positioned at bottom, particle bodies race way 0 ~ 1/4L scope, can ensure that catalyst is dispersed in reactor rapidly and uniformly.This is because when catalyst injection pipe outlet is positioned at bottom, major cycle district, catalyst has time enough and carries out polymerisation after entering reactor, thus generates larger polymer beads, and along with particle major cycle rapid dispersion in reactor.If catalyst injection pipe outlet is too high, be positioned at middle and upper part, particle major cycle district, catalyst arrives bed face after entering reactor very soon, time enough is not had to carry out polymerisation, the polymer beads particle diameter generated is less, to be easy to be recycled gas carry secretly and leave bed and enter circulating air pipeline, and cause larger catalyst stack less thus, and block circulating gas pipe pipeline heat exchanger.If catalyst injection pipe outlet is positioned at stagnant area, will accumulates in stagnant area and cannot disperse after catalyst enters reactor, thus form caking, affect reactor stable operation.Equally, if catalyst inlet is positioned at particle partial circulating, catalyst after entering reactor most of catalyst by partial circulating along with the circulation of particle disperses, cause catalyst in reactor, disperse inequality equally.
In one embodiment of the present invention, catalyst injection pipe outlet radial depth is inner in reactor inner circulation zone, and about between 1/4D-3/4D, D is reactor diameter, can effectively prevent catalyst ejector from producing sticky wall, sheeting to wall.This is because exit position is too when reactor wall, flowing along with particles circulating after catalyst enters reactor very easily adheres to reactor wall, thus produce sticky wall, sheeting, to drop in reactor when sheeting is excessive and affect reactor discharging, thus affect reactor stable operation.
In one embodiment of the present invention, in catalyst injection pipe line, nitrogen flow rate is 1 ~ 20m/s, and the flow of catalyst is 0.03 ~ 0.08m
3/ s, in ascending pipe sleeve pipe, ethylene gas flow is 1 ~ 20m/s.
In an embodiment of the invention, receive catalyst ejector tube wall face place acoustic signals by acoustic wave sensing system, analyze acoustic signals and choose amplitude A as characteristic value, whether unimpededly detect catalyst ejector over time by detected amplitude A.In catalyst injection process and discontinuous injection, but be injected in reactor by rotating disc type injection device interval under the conveying of injecting pipeline nitrogen.In reactor injection process, catalyst granules will with the mutual friction of ascending pipe wall phase, collision, and produce the acoustic signals of characteristic frequency bands.Just can be received the acoustic signals produced in catalyst injection process by acoustic wave sensing system, when the normal injecting reactor of catalyst, acoustic signals amplitude A will produce the peak value of interval; When catalyst injection pipe line blocks, acoustic signals amplitude A will remain on reduced levels always, at this moment acoustic signals amplitude A can be made to produce the peak value of interval by increasing nitrogen gas speed; Normal acoustic signals can be obtained by reducing nitrogen gas speed when catalyst injection amount is excessive.
The catalyst rapid dispersion technology that the present invention proposes can make catalyst disperse at inside reactor fast, uniformly, and prevents because catalyst dispersion is uneven or be ejected into wall and produce sticky wall, caking.
Accompanying drawing explanation
Fig. 1 is fluid bed granulate flow pattern sonic detection result schematic diagram;
Fig. 2 is the catalyst rapid dispersion schematic flow sheet detected based on particle flow pattern;
Fig. 3 is the sound wave on-line checkingi of catalyst injection process;
Fig. 4 is the device for measuring binary system mixability;
The deployment conditions of catalyst when Fig. 5 is decanting point 1 injecting catalyst from Fig. 2;
The deployment conditions of catalyst when Fig. 6 is decanting point 2 injecting catalyst from Fig. 2;
The deployment conditions of catalyst when Fig. 7 is decanting point 3 injecting catalyst from Fig. 2;
The deployment conditions of catalyst when Fig. 8 is decanting point 4 injecting catalyst from Fig. 2.
Detailed description of the invention
A rapid dispersion technology for catalyst, its method comprises the following steps:
A. reactor endoparticle flow pattern is determined;
B. based on axial height and the radial depth of the outlet of particle flow pattern determination catalyst injection pipe;
C. guarantee that the open-flow of catalyst rapid clockwise is mapped in reactor.
First, need to judge the flow pattern of inside reactor, any one method in sonic detection, ray detection, computational fluid dynamics simulation can be utilized.Sonic detection technical monitoring reactor endoparticle flow pattern is adopted in the present invention's specific embodiment, wherein acoustic wave sensing system comprises sonic sensor, amplifying device, signal pickup assembly, signal processing apparatus, and its method comprises the following steps: (1) receives the acoustic emission signal of inside reactor by acoustic wave sensing system; (2) analyze the acoustic emission signal received, choose the frequency f of acoustic signals, amplitude A, ENERGY E, time t as characteristic value; (3) detect the changes in distribution of ENERGY E under the axial differing heights place characteristic frequency f of bed and/or amplitude A, determine the endocorpuscular flow pattern of fluid bed.
Keep fluid bed endoparticle fluidized status and other experiment conditions constant, measure polyethylene particle by some sonic sensors of diverse location on fluid bed whole bed wall and the acoustic signals produced is collided in wall friction, determine fluid bed endoparticle fluidized status thus.
The height of bed when the ENERGY E of acoustical signal or the mean square deviation of amplitude A reach maximum is controlling level.When the ENERGY E of acoustic signals to be less than 80% of the average energy of the signal that all test points obtain along the minimum of a value of fluid bed axis, the height of bed corresponding to this position is the line of demarcation of fluid bed endoparticle motion large and small cycles flow pattern, i.e. position, stagnant area, corresponding movement of particles pattern is Two-way Cycle motion.When the ENERGY E of acoustic signals is more than or equal to 80% of the average energy of the signal that all test points obtain along the minimum of a value of bed axis, then the motion of bed endoparticle is single-cycle flow pattern.In one embodiment of the present of invention, Fig. 1 is the sonic detection result of fluid bed cold model unit particle flow, and wherein bulky grain circulation is particle major cycle district, and its length is L.
In the cold model unit of stabilization fluid, catalyst injection pipe outlet axial height is positioned at bottom, particle major cycle district 0 ~ 1/4L scope, and catalyst injection pipe outlet radial depth is 1/4 ~ 3/4D, D is reactor diameter.Injecting pipeline nitrogen flow rate is 1 ~ 20m/s, and the flow of catalyst is 0.03 ~ 0.08m
3/ s, in ascending pipe sleeve pipe, ethylene gas flow is 1 ~ 20m/s.In injecting catalyst process, adopting sound wave detecting method by receiving the acoustic signals of catalyst injection pipe outer wall, judging whether catalyst injection process keeps unimpeded thus.
During to cold model unit injecting catalyst, in known bed, polyethylene particle quality is Mkg, and when catalyst accounts for bed gross mass 30 ~ 70%, catalyst stops injecting, and runs 20 ~ 40 minutes continually and steadily, then closes air blast rapidly.And then press shown in Fig. 3, by being divided into the part of n 10 cm thicks within the scope of reactor axial height H, with ethene particle, screening being carried out to each partially catalyzed agent particle and is separated, then weighing, determining the mass fraction of catalyst in every part.And the component that reactor head is entrained with is sieved, determine the mass fraction of wherein catalyst.Obtain the axial distribution of catalyst quality mark.Judge that catalyst is uniformly dispersed degree thus.
Embodiment 1
The catalyst rapid dispersion schematic flow sheet that Fig. 2 detects based on particle flow pattern in being.At high 1200mm, internal diameter 150mm, distribution grid is porous flat plate, and aperture is 2.0mm, percent opening be 2.6% lucite build gas-solid fluidized bed in, using air as fluidizing gas, superficial gas velocity is 0.6m/s, adopt particle diameter be 938 μm, density 900kg/m
3polyethylene particle is fluidized particles, and the quiet height of bed is 500mm, and bed granular mass is 3.0kg.Sonic detection technology is adopted to measure recirculating fluidized bed endoparticle flow pattern, wherein acoustic wave sensing system sonic sensor, amplifying device, signal pickup assembly, signal processing apparatus.
When measuring particle flow structure, sonic sensor is affixed on and separates 20mm, 50mm, 100mm, 150mm, 200mm, 250mm, 300mm, 350mm, 400mm, 450mm, 500mm, 550mm, 600mm, 650mm, 700mm, 800mm, 850mm, 900mm, 950mm, 970mm, 1000mm, 1050mm, 1100mm place above fabric swatch, sample frequency is 500kHz, and each sampling time is 10s.
Analyze the axial distribution of acoustic feature signal value, Fig. 1 is the axial distribution of the mean square deviation of the ENERGY E of acoustical signal, and the height of bed when E reaches maximum is controlling level; When E to be less than 80% of the average energy of the signal that all test points obtain along the minimum of a value of fluid bed axis, the height of bed corresponding to this position is the line of demarcation of fluid bed endoparticle motion large and small cycles flow pattern, i.e. position, stagnant area, therefore in the present embodiment, fluid bed endoparticle fluidal texture is Two-way Cycle fluidal texture, wherein bulky grain circulation is particle major cycle district, and length is L.
Stable double-circulating fluid bed in, in the reactor shown in Fig. 2, select injection catalyst point everywhere, be respectively decanting point 1 (1/8L, 1/4D), decanting point 2 (1/8L, 4/5D), decanting point 3 (3/4L, 1/4D) and decanting point 4 (-1/8L, 1/4D) injecting catalyst, its mean mass flux is 0.05m
3/ s, it should be noted that owing to cannot simulate catalyst growth process in cold work die process, and the catalyst therefore injected at decanting point 3 place selects that particle diameter is 45 μm, density is 440kg/m
3catalyst; Then select at decanting point 1,2,4 that particle diameter is 200 μm, density is the catalyst of 440kg/m3, the growth course of catalysts thus.Inject pipeline nitrogen flow rate and be preferably 10m/s, in ascending pipe sleeve pipe, ethylene gas flow is preferably 10m/s.Adopt sound wave detecting method monitoring catalyst injection process, obtain result as shown in Figure 3, as shown in Figure 3, now catalyst injection process keeps smooth and easy.
Under catalyst injection pipe line and all stable state of reactor, when catalyst accounts for bed gross mass 50%, catalyst stops injecting, continual and steady operation 30 minutes, then closes air blast rapidly, presses as shown in Figure 3, the part of 10 10 cm thicks will be divided within the scope of reactor axial height 0-1000mm, carry out screening to each partially catalyzed agent particle with ethene particle to be separated, then weigh, determine the mass fraction of catalyst in every part.Finally, the component that reactor head is entrained with is sieved, and determine the mass fraction of catalyst.Weigh through above-mentioned screening and obtain different catalysts decanting point place catalyst quality mark axial distribution as shown in figures 5-8.When contrast finds that catalyst injects at injection phase 1 place, catalyst distribution is more even, this is because catalyst injection pipe outlet to be positioned at bottom particle major cycle and to export radial depth be positioned at major cycle inside, catalyst to enter after fluid bed under the drive of particle major cycle rapid dispersion to each position of bed.When catalyst is by position 2 injecting reactor, because catalyst injection pipe outlet distance wall is excessively near, severe friction will be produced with wall after catalyst enters bed collide thus produce electrostatic, because catalyst particle size is less, the wall that a large amount of catalyst will adhere to and near outlet under the effect of electrostatic effect, makes catalyst distribution uneven thus.When catalyst is injected by position 3, catalyst content below decanting point is less, above decanting point and by the particle carried secretly containing more catalyst, this is because now catalyst particle size is less, the as easy as rolling off a log air that is fluidized is carried secretly and is left reactor, cannot follow particles circulating and be uniformly distributed at bed.When catalyst is injected by position 4, catalyst exists only in partial circulating region, distribute in particle major cycle district less, this is because catalyst injection position is too low, enter behind particle partial circulating district along with the motion of particle is at this Regional Dispersion, but because systemic circulation and partial circulating region exist interval, stagnant area, the catalyst therefore in partial circulating district cannot be distributed in whole reactor.
To sum up, in the present embodiment, on the basis adopting acoustic wave methodogy monitoring fluid bed granulate Two-way Cycle fluidal texture, when catalyst injection pipe outlet axial height be positioned at bottom, particle major cycle district, radial depth be positioned at particle major cycle district inner time, catalyst can be made to be distributed to quickly and evenly in reactor.
Claims (10)
1. a catalyst rapid dispersion method, is characterized in that said method comprising the steps of:
A. reactor endoparticle flow pattern is determined;
B. based on axial height and the radial depth of the outlet of particle flow pattern determination catalyst injection pipe;
C. to jet catalyst in reactor, by sonic detection regulation and control catalyst ejector effect.
2. rapid dispersion method according to claim 1, is characterized in that: described reactor endoparticle flow pattern is determined by sonic detection, ray detection or Fluid Mechanics Computation.
3. rapid dispersion method according to claim 1, is characterized in that: described catalyst injection pipe outlet axial height is positioned at 0 ~ 1/4L scope bottom reactor endoparticle major cycle district, and L is the length in particle major cycle district.
4. rapid dispersion method according to claim 1, is characterized in that: described catalyst injection pipe outlet radial depth is positioned at inside 1/4 ~ 3/4D scope of reactor endoparticle major cycle, and D is reactor diameter.
5. rapid dispersion method according to claim 1, is characterized in that: described in reactor during jet catalyst, injecting pipeline nitrogen flow rate is 1 ~ 20m/s.
6. rapid dispersion technology according to claim 1, is characterized in that: described in reactor during jet catalyst, in ascending pipe sleeve pipe, ethylene gas flow is 1 ~ 20m/s.
7. rapid dispersion technology according to claim 1, is characterized in that: described in reactor during jet catalyst, the flow injecting pipeline catalyst is 0.03 ~ 0.08m
3/ s.
8. rapid dispersion method according to claim 1, is characterized in that described determination reactor endoparticle flow pattern is specially: (1) receives the acoustic signals of inside reactor by acoustic wave sensing system; (2) analyze the acoustic signals received, choose the frequency f of acoustic signals, amplitude A, ENERGY E, time t as characteristic value; (3) distribution of reactor wall place acoustic feature signal value with bed axial height is detected; (4) pass through along the axial endocorpuscular flow pattern of difference determination reactor detecting the ENERGY E under the frequency f in above-mentioned characteristic value and/or amplitude A of bed.
9. described rapid dispersion method according to claim 1, is characterized in that described being specially by sonic detection regulation and control catalyst ejector effect:
(1) acoustic signals at catalyst ejector tube wall face place is received by acoustic wave sensing system;
(2) analyze the acoustic signals received, choose the amplitude A of acoustic signals as characteristic value;
(3) when the normal injecting reactor of catalyst, acoustic signals amplitude A produces the peak signal of interval; When the jitter that amplitude A produces, regulated and controled the jeting effect of catalyst by the flow velocity changing nitrogen in catalyst injection pipe line.
10. acoustic wave sensing system according to claim 9, is characterized in that: comprise with lower device: sonic sensor, catalyst jet pipe sonic sensor, amplifying device, signal pickup assembly and signal processing apparatus,
Described amplifying device comprises preamplifier and main amplifier, described sonic sensor is evenly arranged along bed axial height, described catalyst jet pipe sonic sensor is arranged on catalyst and injects on jet pipe, described sonic sensor, catalyst jet pipe sonic sensor are connected with preamplifier respectively, and preamplifier, main amplifier, signal pickup assembly are connected in turn with signal processing apparatus.
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| CN102311758A (en) * | 2010-07-05 | 2012-01-11 | 中国石油化工股份有限公司 | Catalyst injection method and catalyst injection device |
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2015
- 2015-11-26 CN CN201510657628.3A patent/CN105233767B/en active Active
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| JPH07246326A (en) * | 1994-03-09 | 1995-09-26 | Hosokawa Micron Corp | Granulation control method using fluidized bed and device therefor |
| US20020189358A1 (en) * | 2001-03-08 | 2002-12-19 | Novozymes A/S | Method of analyzing granular composition by acoustic emission |
| CN1831494A (en) * | 2006-02-24 | 2006-09-13 | 中国石油化工股份有限公司 | Detection method for reactor of fluid-bed |
| CN102311758A (en) * | 2010-07-05 | 2012-01-11 | 中国石油化工股份有限公司 | Catalyst injection method and catalyst injection device |
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