CN105233767B - A kind of catalyst rapid dispersion method - Google Patents
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- CN105233767B CN105233767B CN201510657628.3A CN201510657628A CN105233767B CN 105233767 B CN105233767 B CN 105233767B CN 201510657628 A CN201510657628 A CN 201510657628A CN 105233767 B CN105233767 B CN 105233767B
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Abstract
The invention discloses a kind of rapid dispersion methods of catalyst.It includes determining reactor endoparticle flow pattern, and the axial height and radial depth of catalyst injection pipe outlet are determined based on particle flow pattern, under conditions of catalyst ejector is unimpeded, realizes that catalyst Quick uniform in reactor disperses.Catalyst injection pipe outlet axial height is located in the range of particle major cycle area 0~1/4L of lower part, and outlet radial depth is located inside major cycle area in the range of 1/4~3/4D, and wherein L is particle major cycle section length, D is reactor diameter.The method of the present invention can be such that catalyst quickly and evenly disperses in inside reactor, prevent reactor from generating polymer due to the uneven or catalyst of catalyst dispersion glues wall and glue wall, caking.
Description
Technical field
The present invention relates to catalyst rapid dispersion methods, more particularly to the catalyst rapid dispersion based on the detection of particle flow pattern
Technology.
Background technology
Catalytic reaction process is widely used in each industrial circle, and during the reaction, catalyst in the feed can be equal
Even dispersion is that can such reaction process keep stable, efficient crucial.During catalytic cracking reaction, catalyst distribution is not
Local feedstock oil excessive fragmentation will be caused, and cause catalyst coking and deactivation.In olefin polymerization process, local catalyst is dense
When spending high, local reaction can not excessively acutely will remove in time so as to generate a large amount of heat of polymerizations, will be formed and polymerize in reactor
Object lumps, and influences device stable operation.
Catalyst cracker is a kind of typical fast fluidized bed reactor, and CN102311758B discloses a kind of catalyst
The method mixed with raw material Quick uniform.This method makes catalyst from radial direction or tangent line by changing the implant angle of catalyst
Direction injecting lift pipe reactor.CN101161618B discloses a kind of be used for using raw materials such as acetic acid or acetone through cracking preparation
The method for implanting and device of catalyst when ketenes and its derivative.Using shock of the toroidal expansion tube using fluid and volume
Suction acts on, and liquid is made to be uniformly dispersed in short distance.Document 1 improves catalyst point in riser by being layered injecting catalyst
Scattered uniformity.For slurry-phase reactor, CN201372260Y discloses the catalysis of slurry method production high density polyethylene (HDPE)
Agent injection device shortens the incorporation time of catalyst and hexane, and adjust catalyst charge angle by the position for changing triple valve
Degree reduces the frequency of catalyst blockage.
Analysis existing literature patent it is found that improve there are mainly two types of the methods that catalyst uniformly disperses at present：One kind passes through
Change catalyst charge pipe structure or the catalyst dispersion of charging orientation optimization；Another kind realizes it by being layered injecting catalyst
Even dispersion.But change catalyst injection pipe structure and angle only can guarantee that catalyst is uniformly dispersed in ascending pipe inlet, nothing
Method ensures the uniformity of inside reactor catalyst dispersion；And catalyst layering injection will be so that catalyst injection technology be more multiple
Hydridization.At the same time, existing improvement project does not consider the influence that reactor endoparticle fluidal texture disperses catalyst.For
For gas-phase polyethylene technique, CN100405027C discloses a kind of detection method of fluidized-bed reactor particle flow pattern, inspection
There is the large and small cycle Two-way Cycle flow pattern containing stagnant area in the particle flow structure during survey discovery is gas-solid fluidized bed.In gas phase
In method polyethylene process, if catalyst injection pipe outlet port is excessively high, catalyst will quickly reach bed material after entering reactor
Face, monomer polymerization time in catalyst duct is shorter, and the polymer beads grain size formed is smaller, is easily carried secretly by circulating air
It leaves bed to enter in circulating air pipeline, not only causes serious catalyst loss, also circulating gas pipe pipeline heat exchanger can be caused to block up
Plug.If catalyst injection pipe outlet is located at stagnant area, catalyst granules will be accumulated in the region after entering bed, can not uniformly be divided
It is scattered in reactor, lumps so as to be formed in catalyst injection pipe exit, blocking catalyst charging, influence reactor stablize fortune
Row.In addition, if catalyst injection pipe exit is excessively near apart from wall surface, spraying into the catalyst of bed will easily be bonded on wall surface
Polymer sheeting is formed, and then influences reactor stable operation.
In order to which catalyst is enable to disperse in inside reactor Quick uniform, and consider what particle flow pattern disperseed catalyst
It influences, needs to invent a kind of catalyst rapid dispersion technology detected based on inside reactor particle flow pattern so that catalyst exists
Particle cycle drive under rapid dispersion, and avoid due to catalyst injection pipe outlet port choose it is unreasonable and caused by glue
Wall, caking.
Invention content
The present invention seeks to develop a kind of catalyst rapid dispersion method detected based on particle flow pattern, catalyst can be made
Rapid dispersion is uniform in reactor, the described method comprises the following steps：
A. reactor endoparticle flow pattern is determined；
B. catalyst injection pipe outlet axial height and radial depth are determined based on particle flow pattern；
C. the jet catalyst into reactor regulates and controls catalyst ejector effect by sonic detection.
Sound wave detecting method, ray detection method, Fluid Mechanics Computation can be used in the detection of inside reactor particle flow pattern
The methods of simulation.In one embodiment of the invention, sound wave detecting method is selected to determine particle flow pattern in reactor, it is specific to walk
It is rapid as follows：(1) acoustic emission signal of inside reactor is received by acoustic wave sensing system；(2) the sound emission letter that analysis receives
Number, the frequency f of acoustic signals, amplitude A, ENERGY E, time t are chosen as characteristic value；(3) the axially distinct height of bed is detected
Locate the changes in distribution of the ENERGY E and/or amplitude A under characteristic frequency f, determine the flow pattern of fluid bed endoparticle.Wherein sound wave
Detecting system includes sequentially connected sonic sensor, signal amplifying apparatus, signal pickup assembly, signal processing apparatus, result
Display device, acoustic wave sensing system includes at least one sonic sensor, and sonic sensor uses the installation side of non-intrusion type
Formula.At wall surface of the distribution of sonic sensor for height of materials H in the distribution grid to bed of reactor.
The dynamic acoustic signals of inside reactor pass through the acoustic receiver at the wall surface that is arranged on more than reactor distributing plate
Device enters the amplification that amplifying device carries out signal, to ensure that signal is unattenuated in long range, is acquired subsequently into acoustical signal
Device carries out the A/D conversions of signal, finally enters acoustic signals processing unit (computer) and is handled and analyzed.
Collecting the acoustic signals above fluid bed material position, near material position and below material position, t changes at any time, in material position
Top, the amplitude very little of acoustic signals, and it is more sparse, this is because belonging to fluid bed dilute phase above material position, particle is rare
And grain size is relatively small so that the amplitude that particles collision wall surface generates is smaller.And near material position, when escaping bed surface due to bubble
Ejection effect and entrainment effect, cause the particle from bubble roof and from bubble trailing vortex because bubble breaking is thrown into fluidisation
The free spatial domain of bed, particle movement herein is the most active, i.e., the fluctuation of acoustic energy and acoustic signals that particles collision wall surface generates
Also it is bigger, cause acoustical signal amplitude larger, and size variation is violent.Below material position, the amplitude of acoustic signals is overall relatively to expect
Position is low nearby, and amplitude is more uniform, stablizes, simultaneously because granule density is larger, therefore signal is very intensive, shows that the region belongs to
In the relatively sluggish emulsion zone of particle activity.
In one embodiment of the invention, by sound wave detecting method obtain in fluidized-bed reactor particle flow pattern be containing
There is the large and small cycle Two-way Cycle fluidal texture of stagnant area, wherein particle major cycle length is L.
In one embodiment of the invention, the ascending pipe outlet axial height of catalyst is located at particle bodies race way
In the range of 0~1/4L of lower part, it is ensured that catalyst is rapidly and uniformly dispersed in reactor.This is because catalyst injects
When pipe outlet is located at major cycle area lower part, catalyst after entering reactor there is time enough to carry out polymerisation, so as to raw
Into larger polymer beads, and with particle major cycle in reactor rapid dispersion.If catalyst injection pipe goes out to make a slip of the tongue
Height, positioned at particle major cycle area middle and upper part, catalyst reaches bed face quickly after entering reactor, without time enough into
Row polymerisation, the polymer beads grain size generated is smaller, will be easy to be left bed by circulating air entrainment and entered circulating air
Pipeline thereby results in larger catalyst stack less, and blocks circulating gas pipe pipeline heat exchanger.If catalyst injection pipe outlet is located at
Stagnant area, catalyst will be accumulated in stagnant area and can not be disperseed after entering reactor, so as to form caking, influence reactor stabilization
Operation.Equally, if catalyst inlet is located in particle partial circulating, most of catalyst will be small after catalyst enters reactor
As the cycle of particle is disperseed in cycle, catalyst is equally caused to disperse unevenness in reactor.
In one embodiment of the present invention, catalyst injection pipe exports radial depth inside reactor inner circulation zone,
Between about 1/4D-3/4D, D is reactor diameter, and catalyst ejector can be effectively prevent to generate viscous wall, sheeting to wall surface.This is
Because when outlet port is too close to reactor wall surface, catalyst enters the flowing recycled after reactor with particle and easily adheres to
In reactor wall surface, so as to generate viscous wall, sheeting, will fall off when sheeting is excessive influences reactor discharging in reactor, from
And influence reactor stable operation.
In one embodiment of the present invention, in catalyst injection pipe line nitrogen flow rate be 1~20m/s, the stream of catalyst
It measures as 0.03~0.08m3/ s, it is 1~20m/s to inject ethylene gas flow in pipe-in-pipe.
In an embodiment of the invention, sound wave at catalyst ejector tube wall face is received by acoustic wave sensing system and is believed
Number, analysis acoustic signals choose amplitude A as characteristic value, are changed with time by detected amplitude A and detect catalyst ejector and be
It is no unimpeded.In catalyst injection process not be continuously injected into, but by rotating disc type injection device in pipeline is injected nitrogen
It is intermittently injecting in reactor under conveying.In reactor injection process, catalyst granules will with the mutual friction of ascending pipe wall surface phase,
Collision, and generate the acoustic signals of characteristic frequency bands.Produced by being received in catalyst injection process by acoustic wave sensing system
Acoustic signals, when catalyst normally injects reactor, peak value that acoustic signals amplitude A will generate interval；When catalyst is noted
When entering pipeline blocking, acoustic signals amplitude A will be always held at reduced levels, at this moment can make sound wave by increasing nitrogen gas velocity
Signal amplitude A generates the peak value of interval；It can be obtained when catalyst injection amount is excessive by reducing nitrogen gas velocity normal
Acoustic signals.
Catalyst rapid dispersion technology proposed by the present invention can be such that catalyst quickly, uniformly divides in inside reactor
It dissipates, and prevents since catalyst dispersion is uneven or is ejected into wall surface and generates viscous wall, caking.
Description of the drawings
Fig. 1 is fluid bed granulate flow pattern sonic detection result schematic diagram；
Fig. 2 is the catalyst rapid dispersion flow diagram detected based on particle flow pattern；
Fig. 3 is the sound wave on-line checking of catalyst injection process；
Fig. 4 is the device for measuring binary system mixability；
The deployment conditions of catalyst when Fig. 5 is 1 injecting catalyst of decanting point from Fig. 2；
The deployment conditions of catalyst when Fig. 6 is 2 injecting catalyst of decanting point from Fig. 2；
The deployment conditions of catalyst when Fig. 7 is 3 injecting catalyst of decanting point from Fig. 2；
The deployment conditions of catalyst when Fig. 8 is 4 injecting catalyst of decanting point from Fig. 2.
Specific embodiment
A kind of rapid dispersion technology of catalyst, method include the following steps：
A. reactor endoparticle flow pattern is determined；
B. the axial height and radial depth of catalyst injection pipe outlet are determined based on particle flow pattern；
C. ensure that catalyst is quickly smooth to be ejected into reactor.
Firstly, it is necessary to which the flow pattern to inside reactor judges, sonic detection can be utilized, ray detection, calculate stream
Any one of mechanics simulation method.Using in sonic detection technical monitoring reactor in a specific embodiment of the invention
Particle flow pattern, wherein acoustic wave sensing system include sonic sensor, amplifying device, signal pickup assembly, signal processing apparatus,
Method includes the following steps：(1) acoustic emission signal of inside reactor is received by acoustic wave sensing system；(2) analysis receives
Acoustic emission signal, choose the frequency f of acoustic signals, amplitude A, ENERGY E, time t as characteristic value；(3) bed axis is detected
The changes in distribution of ENERGY E and/or amplitude A under characteristic frequency f at different height determines the flowing mould of fluid bed endoparticle
Formula.
It keeps fluid bed endoparticle fluidized status and other experiment conditions constant, passes through positions different on the whole bed wall face of fluid bed
Several sonic sensors put measure polyethylene particle and acoustic signals caused by wall friction collision, thereby determine that fluid bed
Endoparticle fluidized status.
The height of bed when the ENERGY E of acoustical signal or the mean square deviation of amplitude A reach maximum is controlling level.Work as acoustic signals
ENERGY E along fluid bed axial direction minimum value be less than all test points obtain signal average energy 80% when, the position
The corresponding height of bed moves the line of demarcation of large and small cycles flow pattern for fluid bed endoparticle, that is, is detained zone position, corresponding
Grain motor pattern is moved for Two-way Cycle.When the ENERGY E of acoustic signals is more than or equal to all test point institutes along the minimum value of bed axial direction
The 80% of the average energy of the signal of acquisition, then bed endoparticle movement is single-cycle flow pattern.The implementation of the present invention
In example, Fig. 1 is the sonic detection of fluid bed cold model unit particle flow as a result, wherein bulky grain cycle is particle major cycle area,
The length of L.
In the cold model unit of stabilization fluid, catalyst injection pipe outlet axial height is located at particle major cycle area lower part 0
In the range of~1/4L, catalyst injection pipe outlet radial depth is 1/4~3/4D, and D is reactor diameter.Inject nitrogen in pipeline
Flow velocity is 1~20m/s, and the flow of catalyst is 0.03~0.08m3/ s, it is 1~20m/ to inject ethylene gas flow in pipe-in-pipe
s.During injecting catalyst, using sound wave detecting method by receiving the acoustic signals of catalyst injection pipe outer wall, thus
Judge whether catalyst injection process keeps unimpeded.
During to cold model unit injecting catalyst, it is known that polyethylene granular mass is M kg in bed, and when catalyst, to account for bed total
During quality 30~70%, catalyst stops injection, continually and steadily runs 20~40 minutes, then closes air blower rapidly.Immediately
It as shown in Figure 3, the part of n 10 cm thicks will be divided into the range of reactor axial height H, to each section catalyst granules
With ethylene particle detach, then weigh, determine mass fraction of the catalyst in each section.And to reactor top
The component that portion is entrained with is sieved, and determines the mass fraction of wherein catalyst.Obtain the axial distribution of catalyst quality score.
Thus judge that catalyst is uniformly dispersed degree.
Embodiment 1
The catalyst rapid dispersion flow diagram that Fig. 2 is detected in being based on particle flow pattern.In high 1200mm, internal diameter
150mm, distribution grid are porous flat plate, aperture 2.0mm, the organic glass that percent opening is 2.6% build it is gas-solid fluidized bed in,
Using air as fluidizing gas, superficial gas velocity 0.6m/s uses grain size as 938 μm, density 900kg/m3Polyethylene particle is
Fluidized particles, the quiet height of bed are 500mm, and bed granular mass is 3.0kg.Using in sonic detection technology measure recirculating fluidized bed
Grain flow pattern, wherein acoustic wave sensing system sonic sensor, amplifying device, signal pickup assembly, signal processing apparatus.
When measuring particle flow structure, by sonic sensor be affixed on from 20mm, 50mm above distribution grid, 100mm, 150mm,
200mm、250mm、300mm、350mm、400mm、450mm、500mm、550mm、600mm、650mm、700mm、800mm、
At 850mm, 900mm, 950mm, 970mm, 1000mm, 1050mm, 1100mm, sample frequency 500kHz, each sampling time
For 10s.
The axial distribution of acoustic feature signal value is analyzed, Fig. 1 is the axial distribution of the mean square deviation of the ENERGY E of acoustical signal, works as E
Height of bed when reaching maximum is controlling level；When the minimum value of E along fluid bed axial direction is less than the signal of all test points acquisition
Average energy 80% when, the height of bed corresponding to the position moves the boundary of large and small cycles flow pattern for fluid bed endoparticle
Line is detained zone position, therefore fluid bed endoparticle fluidal texture is Two-way Cycle fluidal texture, wherein bulky grain in the present embodiment
It recycles as particle major cycle area, length L.
It is stable it is double-circulating fluid bed in, in reactor shown in Fig. 2, catalyst injects everywhere for selection
Point, 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, mean mass flux 0.05m3/ s, it should be noted that during cold work die by
In catalyst growth process can not be simulated, therefore it is 45 μm, density to inject injected catalyst to select grain size at decanting point 3
For 440kg/m3Catalyst；And the catalyst that grain size is 440kg/m3 for 200 μm, density is selected in decanting point 1,2,4, by
The growth course of this catalysts.It is preferably 10m/s to inject nitrogen flow rate in pipeline, injects ethylene gas flow in pipe-in-pipe
Preferably 10m/s.Catalyst injection process is monitored using sound wave detecting method, obtains that the results are shown in Figure 3, from the figure 3, it may be seen that this
When catalyst injection process keep smooth.
In a state that catalyst injection pipe line and reactor are all stable, when catalyst accounts for bed gross mass 50%
When, catalyst stops injection, then continual and steady operation 30 minutes closes rapidly air blower, by as shown in figure 3, by reactor
Be divided into the part of 10 10 cm thicks in the range of axial height 0-1000mm, to each section catalyst granules and ethylene particle into
Row screening separation, then weighs, determines mass fraction of the catalyst in each section.Finally, reactor head is entrained with
Component sieved, and determine catalyst mass fraction.It weighs to obtain at different catalysts decanting point by above-mentioned screening
Catalyst quality score is axially distributed as shown in figures 5-8.When comparison finds that catalyst injects at injection phase 1, catalyst point
Cloth is more uniform, this is because catalyst injection pipe outlet, which is located at particle major cycle bottom and exports radial depth, is located at major cycle
Inside, catalyst into after fluidized bed under the drive of particle major cycle rapid dispersion to each position of bed.When catalyst by
When reactor is injected in position 2, since catalyst injection pipe outlet is excessively near apart from wall surface, catalyst will produce after entering bed with wall surface
Raw severe friction collision is so as to generate electrostatic, and since catalyst particle size is smaller, a large amount of catalyst will under the action of electrostatic effect
Adherency and the wall surface of near exit, so that catalyst distribution is uneven.When catalyst is injected by position 3, below decanting point
Catalyst content it is smaller, containing more catalyst above decanting point and in the particle that is entrained, this is because urging at this time
Agent grain size is smaller, is easy to be fluidized air entrainment and leaves reactor, particle can not be followed to circulate in bed and be uniformly distributed.When
When catalyst is injected by position 4, catalyst is existed only in partial circulating region, is distributed in particle major cycle area less, this is
Because catalyst injection position is too low, into particle partial circulating area after as the movement of particle is in the Regional Dispersion, but due to
Systemic circulation and partial circulating region are there are stagnant area interval, therefore the catalyst in partial circulating area can not be distributed to entire reactor
It is interior.
To sum up, in the present embodiment, on the basis of using acoustic wave methodogy monitoring fluid bed granulate Two-way Cycle fluidal texture,
When catalyst injection pipe outlet, axial height is located at particle major cycle area lower part, radial depth is located inside particle major cycle area
When, catalyst is enabled to quickly and evenly to be distributed in reactor.
Claims (7)
- A kind of 1. catalyst rapid dispersion method, it is characterised in that the described method comprises the following steps：A. reactor endoparticle flow pattern is determined；B. the axial height and radial depth of catalyst injection pipe outlet are determined based on particle flow pattern；The catalyst injection pipe Outlet axial height is located in the range of reactor endoparticle major cycle area 0 ~ 1/4L of bottom, and L is the length in particle major cycle area；Institute The catalyst injection pipe outlet radial depth stated is located in the range of 1/4 ~ 3/4D of inside of reactor endoparticle major cycle, and D is anti- Answer device diameter；C. the jet catalyst into reactor regulates and controls catalyst ejector effect by sonic detection；The judgement of catalyst ejector effect is：When catalyst accounts for bed 30 ~ 70 % of gross mass, catalyst stops injection, continues Then air blower is closed rapidly in stable operation 20 ~ 40 minutes, a 10 cm thicks of n will be divided into the range of reactor axial height H Part with ethylene particle detach, then weighs, determine catalyst in each section to each section catalyst granules In mass fraction, and the component that reactor head is entrained with is sieved, determines the mass fraction of wherein catalyst, obtain The axial distribution of catalyst quality score.
- 2. catalyst rapid dispersion method according to claim 1, it is characterised in that：The reactor endoparticle flow pattern It is determined by sonic detection, ray detection or Fluid Mechanics Computation.
- 3. catalyst rapid dispersion method according to claim 1, it is characterised in that：Described being sprayed into reactor is urged During agent, it is 1 ~ 20m/s to inject nitrogen flow rate in pipeline.
- 4. catalyst rapid dispersion method according to claim 1, it is characterised in that：Described being sprayed into reactor is urged During agent, it is 1 ~ 20m/s to inject ethylene gas flow in pipe-in-pipe.
- 5. catalyst rapid dispersion method according to claim 1, it is characterised in that：Described being sprayed into reactor is urged During agent, the flow for injecting catalyst in pipeline is 0.03 ~ 0.08m3/s。
- 6. catalyst rapid dispersion method according to claim 1, it is characterised in that the determining reactor endoparticle Flow pattern is specially：（1）The acoustic signals of inside reactor are received by acoustic wave sensing system；（2）Analyze the sound wave letter received Number, the frequency f of acoustic signals, amplitude A, ENERGY E, time t are chosen as characteristic value；（3）Detect sound wave at reactor wall surface Signal characteristic value with bed axial height distribution；（4）By axially being detected along bed under the frequency f in features described above value ENERGY E and/or the difference of amplitude A determine the flow pattern of reactor endoparticle.
- 7. catalyst rapid dispersion method according to claim 1, it is characterised in that described to be regulated and controled by sonic detection Catalyst ejector effect is specially：（1）Acoustic signals at catalyst ejector tube wall face are received by acoustic wave sensing system；（2）The acoustic signals received are analyzed, choose the amplitude A of acoustic signals as characteristic value；（3）When catalyst normally injects reactor, acoustic signals amplitude A generates the peak signal of interval；It is generated when amplitude A Jitter regulates and controls the jeting effect of catalyst by changing the flow velocity of nitrogen in catalyst injection pipe line.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3056939B2 (en) * | 1994-03-09 | 2000-06-26 | ホソカワミクロン株式会社 | Granulation control method and apparatus using fluidized bed |
| US7114392B2 (en) * | 2001-03-08 | 2006-10-03 | Novozymes A/S | Method of analyzing granular composition by acoustic emission |
| CN100405027C (en) * | 2006-02-24 | 2008-07-23 | 中国石油化工股份有限公司 | Detection method for reactor of fluid-bed |
| CN102311758B (en) * | 2010-07-05 | 2014-03-26 | 中国石油化工股份有限公司 | Catalyst injection method and catalyst injection device |
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