CN208287979U - Fluidized bed reaction - Google Patents
Fluidized bed reaction Download PDFInfo
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- CN208287979U CN208287979U CN201820571094.1U CN201820571094U CN208287979U CN 208287979 U CN208287979 U CN 208287979U CN 201820571094 U CN201820571094 U CN 201820571094U CN 208287979 U CN208287979 U CN 208287979U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The utility model provides fluidized bed reaction, which is capable of detecting when the abnormal heating portion of the lower part of the fluidized-bed reactor for manufacturing acrylonitrile, and result can be stablized and safely manufacture acrylonitrile.The fluidized bed reaction has the fluidized-bed reactor comprising catalyst layer and the unstrpped gas feeder for the base feed gas into the fluidized-bed reactor, for the fluidized bed reaction for manufacturing acrylonitrile, which also has the thermometer being disposed near the unstrpped gas feeder.
Description
Technical field
The utility model relates to fluidized bed reactions.
Background technique
Fluidization has been applied to various manufacturing technologies since the second half in 19th century develops.Master as fluidized bed
Want industrial application, can enumerate coal gasifier, FCC (catalytic cracking) device, ammoxidation based on propylene acrylonitrile manufacture dress
It sets, polyethylene gas phase polymerization apparatus and maleic anhydride manufacturing device etc..Fluidized-bed reactor is easily removed or applies reaction heat,
Therefore have many characteristics, such as that uniform temperature, productivity can will be maintained in bed higher.Therefore, it is also contemplated that fluidized-bed reactor from now on
Application, improvement in all respects.
The internal structure of common fluidized bed reaction is for example on the books in non-patent literature 1.This is shown in FIG. 4
The skeleton diagram of the common fluidized bed reaction of kind.In fluidized bed reaction shown in Fig. 4, from fluidized-bed reactor 1
Air (oxygen-containing gas) ingress pipe 2 imports air (oxygen-containing gas), keeps the air (oxygen-containing gas) imported (oxygenous by air
Body) dispersion plate 3 blowout hole, by the air (oxygen-containing gas) of the importing to catalyst layer 6 import.On the other hand, from raw material
Ingress pipe 4 imports unstrpped gas, so that the unstrpped gas imported is passed through the discharge pipe of stock dispersion pipe 5, by the raw material of the importing
Gas is imported to catalyst layer 6.As a result, in catalyst layer 6, flow catalyst using air (oxygen-containing gas) and raw material.
Concomitantly with the generation gas that is generated from catalyst layer 6, it flies out one of catalyst particle from catalyst layer 6
Point.A part of catalyst particle is concomitantly discharged to outside fluidized bed reaction with gas is generated.Therefore, in fluidized bed
In reactor 1, the cyclone separator for preventing catalyst particle to outside discharge is equipped on the top of fluidized-bed reactor 1
8a,8b,8c.It generates gas and is imported into whirlwind point from cyclone inlet 7 with the catalyst particle of the generation gas
From device.In order to improve the arresting efficiency of catalyst particle, such cyclone separator is usually connected in series with 3 grades of cyclone separators
Mode use.In addition, with the sequence that circulates in cyclone separator of gas is generated correspondingly, by 3 grades of cyclone separators point
Also known as make " No.1 cyclone separator ", " No.2 cyclone separator ", " No.3 cyclone separator ".The fluidized bed reaction of Fig. 4
With a serial 3 grade cyclone separator, but fluidized bed reaction also sometimes with generate there are two gas flow correspondingly has
3 grades of more than series cyclone separators.Also, gas is generated by generating gas effuser 10 to outside fluidized-bed reactor 1
Discharge, catalyst particle return to catalyst layer 6 through punishment in advance foot (Japanese: デ ィ プ レ ッ グ) 9a, 9b, 9c.
Describe such method in patent document 1: using have multiple temperature detecting parts and it is multiple series remove
The fluidized-bed reactor that heat pipe and effective sectional area are 20 square metres or more come when implementing gas phase exothermic reaction, for it is each not
Effective sectional area range more than 20 square metres controls temperature.
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2008-80219 bulletin
Non-patent literature
Non-patent literature 1: bridge sheet is strong to be controlled, industrial reaction device, trains wind shop, (1984), page 170
Utility model content
Utility model will solve the problems, such as
The thermometer that fluidized bed reaction is set to described in non-patent literature 1 is from making the yield of target product most
From the perspective of bigization, it is used in the monitoring of reaction temperature.In the fluidized bed reaction of manufacture acrylonitrile, also from same
From the perspective of sample, thermometer is arranged in many places of many places and catalyst layer top in catalyst layer.About this manufacture third
The fluidized bed reaction of alkene nitrile, the utility model inventor discovery there is a situation where it is such: with operating progress or
High-temperature portion when restarting operating after emergent stopping, in fluidized-bed reactor lower part discovery part.
It, can in order to which the yield of target product is maintained a high position in the temprature control method described in patent document 1
It is finely controlled reaction temperature, but temperature measurement can not be carried out at the position other than the position for being provided with thermometer, it can not
High-temperature portion that do not know wherein to occur, local is effectively detected.
Thus, project to be solved in the utility model is to provide the manufacturing method of fluidized bed reaction and acrylonitrile,
The manufacturing method of the fluidized bed reaction and acrylonitrile is capable of detecting when under the fluidized-bed reactor for manufacturing acrylonitrile
The abnormal heating portion in portion, result can be stablized and safely manufacture acrylonitrile.
The solution to the problem
The inventor of the utility model is inferred to, the reason of previous fluidized-bed reactor lower part is abnormal fever
In the accumulation of the catalyst of fluidized-bed reactor lower part etc. and the delay of gas.Also, the inventor of the utility model is further
Discussion with keen determination has been carried out, as a result, it has been found that, if having temperature near the unstrpped gas feeder for base feed gas
Degree meter, then be able to solve the above subject, so as to complete the utility model.
That is, the utility model is as follows.
(1)
A kind of fluidized bed reaction, the fluidized bed reaction have fluidized-bed reactor and use comprising catalyst layer
In the unstrpped gas feeder of the base feed gas into the fluidized-bed reactor, the fluidized bed reaction is for manufacturing third
Alkene nitrile, the fluidized bed reaction be characterized in that,
The fluidized bed reaction also has the thermometer being disposed near the unstrpped gas feeder.
(2)
According to the fluidized bed reaction of (1), which is characterized in that the fluidized-bed reactor includes unstrpped gas dispersion
Pipe, is disposed in the lower section of the catalyst layer, and make using unstrpped gas feeder supply come unstrpped gas to institute
State dispersion in catalyst layer；And oxygen-containing gas dispersion plate, with the unstrpped gas dispersion pipe it is spaced a predetermined distance from be arranged
In the lower section of the unstrpped gas dispersion pipe, and make the oxygen-containing gas being supplied in the fluidized-bed reactor to the fluidized bed
Interior dispersion,
The thermometer is disposed in the oxygen-containing gas dispersion plate and along upper direction away from the unstrpped gas dispersion pipe 1m's
Between height and position.
(3)
According to the fluidized bed reaction of (2), which is characterized in that the oxygen-containing gas dispersion plate has multiple holes, so that
The oxygen-containing gas is uniformly dispersed into the catalyst layer,
The thermometer has the 1st thermometer configured in a manner of not covering the multiple hole when looking down.
(4)
The fluidized bed reaction according to any one of (1)~(3), which is characterized in that the thermometer has edge
The 2nd arranged circumferentially thermometer of the inner wall of the side wall of the fluidized-bed reactor.
The effect of utility model
According to the utility model, it is capable of providing the manufacturing method of fluidized bed reaction and acrylonitrile, the fluidized-bed reaction
The manufacturing method of device and acrylonitrile is capable of detecting when the abnormal heating of the lower part of the fluidized-bed reactor for manufacturing acrylonitrile
Portion, result can be stablized and safely manufacture acrylonitrile.
Detailed description of the invention
Fig. 1 is the schematic sectional view for indicating an example of fluidized bed reaction of the utility model.
Fig. 2 is the local summary section obtained when observing the fluidized bed reaction of Fig. 1 along the direction A-A.
Fig. 3 is the local summary section obtained when observing the fluidized bed reaction of Fig. 1 along the direction A-A.
Fig. 4 is the schematic sectional view for indicating an example of common fluidized bed reaction.
Description of symbols
1, fluidized-bed reactor；2, airway；3, oxygen-containing gas dispersion plate；4, unstrpped gas ingress pipe；5, raw material
Gas dispersion tube；6, catalyst layer；7, cyclone inlet；8c, the 1st grade of cyclone separator；8b, the 2nd grade of cyclone separator；
8a, 3rd level cyclone separator；9c, the 1st grade of material foot；9b, the 2nd grade of material foot；9a, 3rd level material foot；10, gas effuser is generated；
11, cooling coil；12, the 1st thermometer (oxygen-containing gas dispersion plate use)；13, the 2nd thermometer (sidewall of reactor use).
Specific embodiment
Come referring to attached drawing below according to needs to mode (hereinafter referred to only " this embodiment party for implementing the utility model
Formula ") it is described in detail.Present embodiment below is the illustration for illustrating the utility model, and there is no will be originally practical new
Type is limited to the meaning of content below.The utility model can implement various deformation within its scope.In addition, attached
Same appended drawing reference is marked for same element in figure, and the repetitive description thereof will be omitted.If in addition, the positional relationships such as up and down
It is not particularly illustrated, is then set as positional relationship based on the figure.Also, the dimension scale of attached drawing is not limited to diagram
Ratio.
The fluidized bed reaction of present embodiment has the fluidized-bed reactor comprising catalyst layer and is used for fluidisation
The unstrpped gas feeder of base feed gas in bed reactor, the fluidized bed reaction is for manufacturing acrylonitrile.Fluidized bed
Reaction unit also have and be disposed near unstrpped gas feeder (such as unstrpped gas feeder into fluidized-bed reactor
Be discharged unstrpped gas outlet) thermometer.There is thermometer by fluidized bed reaction, fluidized bed reaction can
High-temperature portion caused by detecting because of abnormal fever, can stablize and safely manufacture acrylonitrile.
[fluidized bed reaction]
Fig. 1 is the schematic sectional view for indicating an example of fluidized bed reaction of present embodiment.Fluidized bed shown in FIG. 1
Reaction unit has fluidized-bed reactor 1 and the unstrpped gas feeder for the base feed gas into fluidized-bed reactor 1
4.Fluidized-bed reactor 1 shown in FIG. 1 is equivalent to the main body of the reaction system for dividing gas phase reaction and external gas phase reaction device
Part.The shape of fluidized-bed reactor 1 is not particularly limited, and is also possible to well known shape.As unstrpped gas feeder 4,
As long as can supply unstrpped gas into fluidized-bed reactor 1, it is not particularly limited.The shape of unstrpped gas feeder 4
It is not particularly limited, such as also can have the form of tubulose.As unstrpped gas, can enumerate for manufacturing the logical of acrylonitrile
The unstrpped gas being often used more specifically can enumerate propylene and/or propane and ammonia.
(fluidized-bed reactor 1)
Fluidized-bed reactor 1 for example includes catalyst layer 6, is formed in the lower part of the inside of the fluidized-bed reactor 1；
Unstrpped gas dispersion pipe 5, is disposed in the lower section of catalyst layer 6, and makes the unstrpped gas supplied using unstrpped gas feeder 4
Disperse into catalyst layer 6；Airway 2 is disposed in the bottom of fluidized-bed reactor 1, and into fluidized-bed reactor 1
Portion imports oxygen-containing gas；Oxygen-containing gas dispersion plate 3, with unstrpped gas dispersion pipe 5 it is spaced a predetermined distance from be disposed in unstripped gas
The lower section of body dispersion pipe, and make the oxygen-containing gas being supplied in fluidized-bed reactor 1 using airway 2 to catalyst layer 6
Interior dispersion；This 3 grades of cyclone separators of cyclone separator 8a, cyclone separator 8b and cyclone separator 8c, they are disposed in stream
Top in fluidized bed reactor 1；Cyclone inlet 7 is equivalent to the entrance of cyclone separator 8a；Expect foot 9a, material foot 9b
And material this 3 grades material feet of foot 9c, they are connected with cyclone separator 8a, cyclone separator 8b and cyclone separator 8c respectively
It connects；Gas effuser 10 is generated, the top of tower of fluidized-bed reactor 1 is disposed in；Cooling coil 11；And the 1st thermometer 12
With the 2nd thermometer 13, they are disposed between oxygen-containing gas dispersion plate 3 and unstrpped gas dispersion pipe 5.
(catalyst layer 6)
Catalyst layer 6 is formed in the lower part of the inside of fluidized-bed reactor 1.Catalyst layer 6 is filled with and the type reacted
Corresponding fluid catalyst.Fluid catalyst is not particularly limited, such as can be enumerated and be carried on silica etc.
Metal oxide catalyst.In the case where reaction is the ammoxidation reaction of propylene and/or propane, as fluid catalyst,
The oxide of Mo-V- (Sb and/or Ti) system, Mo-V-Fe system and Mo-Bi-Fe system can be enumerated, and 90 matter are preferably used
Measure % or more catalyst particle partial size be 10 μm~197 μm, the fluid catalyst that compression strength is 10MPa or more.
(unstrpped gas dispersion pipe 5)
Unstrpped gas dispersion pipe 5 is disposed in the lower section of catalyst layer 6, and makes the original supplied using unstrpped gas feeder 4
Material gas disperses into catalyst layer 6.As long as unstrpped gas dispersion pipe 5 can be such that unstrpped gas disperses simultaneously into catalyst layer 6
Form with tubulose, is not particularly limited.
(oxygen-containing gas ingress pipe 2)
Oxygen-containing gas ingress pipe 2 is disposed in the bottom of fluidized-bed reactor 1, and for importing into fluidized-bed reactor 1
Oxygen-containing gas.As long as oxygen-containing gas can be imported 1 inside of fluidized-bed reactor and with the shape of tubulose by oxygen-containing gas ingress pipe 2
State is not particularly limited.As oxygen-containing gas, such as oxygen and air can be enumerated.
(oxygen-containing gas dispersion plate 3)
Oxygen-containing gas dispersion plate 3 and unstrpped gas dispersion pipe 5 it is spaced a predetermined distance from be disposed in unstrpped gas dispersion pipe 5
Lower section, and disperse the oxygen-containing gas being supplied in fluidized-bed reactor 1 using airway 2 into catalyst layer 6.It is oxygen-containing
As long as gas dispersion plate 3 can be such that oxygen-containing gas disperses into catalyst layer 6 and have the form of plate, do not limit especially
It is fixed.The concrete example of oxygen-containing gas dispersion plate 3 is shown in FIG. 3.Fig. 3 is the fluidized-bed reaction dress for indicating to observe Fig. 1 along the direction A-A
The local summary section of an example when setting.Oxygen-containing gas dispersion plate 3 shown in Fig. 3 has multiple holes, so that oxygen-containing gas is equal
Disperse evenly into catalyst layer.Fig. 2 or shown in Fig. 3 equably matches in multiple holes at a predetermined interval on file direction
It sets.But in the present embodiment, it's not limited to that for the configuration mode in multiple holes.
(cyclone separator 8a~cyclone separator 8c)
Cyclone separator 8a~cyclone separator 8c is disposed in the top in fluidized-bed reactor 1.Fluidized bed shown in FIG. 1
Reactor 1 has a serial cyclone separator, but the series of the cyclone separator of the fluidized-bed reactor of present embodiment
Quantity is also possible to multiple either one.
(material foot 9a~material foot 9c)
Each material foot 9a~material foot 9c is connected with each cyclone separator 8a~cyclone separator 8c.Fluidized bed shown in FIG. 1
Reactor 1 have a serial material foot, but the fluidized-bed reactor of present embodiment material foot number of series either
One, it is also possible to multiple.
(generating gas effuser 10)
The top of tower that gas effuser 10 is disposed in fluidized-bed reactor 1 is generated, for making to generate gas to outside outflow.
As long as generating gas effuser 10 can make to generate gas to the external form flowed out and have tubulose, it is not particularly limited.
(cooling coil 11)
As long as cooling coil 11 has spiral helicine form and can control the temperature in fluidized-bed reactor, without spy
It does not limit.In this example embodiment, cooling coil is constituted more by eradicating heat pipe etc..In the case where gas phase reaction is exothermic reaction, make
Reaction heat is removed with the cooling coil 11 being set in fluidized-bed reactor 1, to control reaction temperature.Reaction temperature passes through use
It is measured in the reaction temperature measurement of measurement reaction temperature with thermometer, but as long as being usually used temperature in chemical devices
Meter, form etc. are not particularly limited.Preferably in the Temperature Distribution that can hold catalyst layer in fluidized bed reaction
Position multiple reaction temperature measurement thermometers are set.
(the 1st thermometer 12 and the 2nd thermometer 13)
1st thermometer 12 and the 2nd thermometer 13 be separately equipped in oxygen-containing gas dispersion plate 3 and unstrpped gas dispersion pipe 5 it
Between.As shown in Fig. 2, thermometer 12 is not in a manner of covering multiple holes when looking down configured with multiple.Fluidized-bed reaction fills as a result,
The abnormal heating that can be effectively detected out on oxygen-containing gas dispersion plate 3 is set, and oxygen-containing gas will not be hindered to catalyst layer 6
Interior dispersion.As shown in figure 3, thermometer 13 has one along the arranged circumferentially of inner wall of the side wall of fluidized-bed reactor 1.Thus, it is possible to
The abnormal heating of the side wall of fluidized-bed reactor 1 is enough effectively detected out.In addition, the 2nd thermometer 13 not shown in Fig. 2,
1st thermometer 12 not shown in Fig. 3, but fluidized-bed reactor shown in FIG. 11 has the 1st thermometer 12 shown in Fig. 2 and Fig. 3
Shown in the 2nd thermometer 13.
1st thermometer 12 and the 2nd thermometer 13 shown in FIG. 1 to FIG. 3 are separately equipped in oxygen-containing gas dispersion plate 3 and raw material
Between gas dispersion tube 5, but in the fluidized bed reaction of present embodiment, as long as thermometer is disposed in unstrpped gas supply
Near device, it is not particularly limited." near unstrpped gas feeder " described herein is, for example, to refer to suitably examine
The position for measuring the abnormal heating of fluidized-bed reactor lower part, from can further detect that its result of abnormal heating can in advance
From the perspective of further suppressing catalyst degradation, further increasing stability and safety, it is preferred that thermometer configuration exists
Oxygen-containing gas dispersion plate and between height and position of the upper direction away from unstrpped gas dispersion pipe 1m, it is further preferred that thermometer is matched
It sets in oxygen-containing gas dispersion plate and between height and position of the upper direction away from unstrpped gas dispersion pipe 0.5m, further preferred
It is that thermometer configuration is in oxygen-containing gas dispersion plate between unstrpped gas dispersion pipe.Furthermore, it is therefore particularly preferred that thermometer is set
It sets at the position of worry Mo piece (molybdenum sheet) accumulation, obstruction catalyst flowing.
1st thermometer 12 and the 2nd thermometer 13 are respectively preferably armoured thermocouple (Japanese: シ ー ス thermoelectricity to).Armouring
Thermocouple refers to such thermometer: interior to high-density in the superfine pipe of made of metal (sheath) using the inorganic insulating material of high-purity
Filled with thermocouple core wire, there is high-insulativity and high voltage.Sheath is not particularly limited, but preferably outer diameter 0.25mm~
The made of metal of 8.0mm, and preferably SUS316, SUS310S, SUS347, SUS316L, NCF600, Ni alloy.The type of thermocouple
It is not particularly limited, but preferably nichrome alumino-nickel couple (CA thermocouple), chromel-constantan thermocouple (CRC thermocouple), iron-
Copper-constantan thermocouple (IC thermocouple), copper-constantan thermocouple (CC thermocouple).
In the case where the 1st thermometer 12 and the 2nd thermometer 13 are armoured thermocouple, armoured thermocouple has on its top
Thermometric contact, and measure the temperature of the position of the contact.The discussion of inventor according to the present utility model is continuing to catalysis
Position that the flowing of agent stopped supply propylene and/or propane in the case where ammonia and oxygen-containing gas, can not utilize cooling sometimes
Coil pipe removes reaction heat, causes abnormal heating to 2000 DEG C or more.Thermoelectricity of the thermometer before reaching 2000 DEG C, inside sheath
Even fusing, or also fuse comprising protecting pipe.In the case where producing these fusing, thermometer has been unable to measure temperature
Degree, becomes so-called malfunction.It is redefined for, is indicated when thermometer breaks down in high-temperature side.It is as a result,
The position except the temperature measurement end of thermometer is set also can effectively further to detect abnormal heating.As prevention by non-
The method of error detection caused by broken string caused by the non-fusing such as mechanical broken string, bad connection caused by abnormal heating, it is excellent
It is selected in same position and multiple armoured thermocouples is set to improve reliability.By the way that multiple armoured thermocouples are arranged, two can be constructed
The detection architectures such as two (2out of 2), two from three (2out of 3) are taken, can exclude useless caused by error detection promptly to stop
Only.
[manufacturing method of acrylonitrile]
The manufacturing method of the acrylonitrile of present embodiment includes: process (1), in this process, to including catalyst layer
Fluidized-bed reactor supplies the unstrpped gas containing ammonia and propylene and/or propane, air or oxygen；And process (2), at this
In process, make unstrpped gas by catalyst layer acrylonitrile is made, fluidized-bed reactor is at the position of base feed gas
Thermometer is nearby arranged.
Hereinafter, the case where to use fluidized bed reaction shown in FIG. 1, illustrates the third of present embodiment as an example
Alkene nitrile generation method.
[process (1)]
Process (1) is to supply the original containing ammonia and propylene and/or propane to the fluidized-bed reactor comprising catalyst layer
Expect the process of gas, oxygen-containing gas.Unstrpped gas is for example supplied using unstrpped gas feeder 4 to fluidized-bed reactor 1.It is oxygen-containing
Gas is for example supplied using oxygen-containing gas ingress pipe 2 to fluidized-bed reactor 1.It sets out from a security point, oxygen-containing gas is not
It can be mixed in piping with unstrpped gas in advance, but pass through oxygen-containing gas ingress pipe 2 from the lower part for being set to fluidized-bed reactor 1
Oxygen-containing gas dispersion plate 3 to reactor import.
The unstrpped gas that supply comes pass through the unstrpped gas feeder 4 that is connected with the downside of fluidized-bed reactor 1 and with
The unstrpped gas dispersion pipe 5 that unstrpped gas feeder 4 is connected is anti-to the fluidized bed filled with the desired amount of fluid catalyst
Answer supply in device.Oxygen-containing gas passes through the oxygen-containing gas ingress pipe 2 being connected with the bottom (downside) of fluidized-bed reactor 1 and contains
Carrier of oxygen dispersion plate 3 is imported into the fluidized-bed reactor filled with the desired amount of fluid catalyst.Reaction raw materials and reaction
Product generally circulates in reactor from bottom to top.
Catalyst layer, fluid catalyst flowing are imported by unstrpped gas.In addition, recording flowing catalysis in Fig. 1
The interface of oxidant layer 6.The interface is static when unstrpped gas does not import.After unstrpped gas importing, due to the gap of catalyst layer
The increase of rate and the bubble for generating size cause the protrusion at interface, therefore layer height becomes uneven.Thus, the position at interface is after all
The position only approximatively, fifty-fifty illustrated.
[process (2)]
Process (2) makes unstrpped gas by catalyst layer acrylonitrile is made.Unstrpped gas passes through catalyst layer one on one side
Side reaction, obtains the generation gas containing acrylonitrile, acetonitrile, hydrogen cyanide etc..
The manufacturing method of the acrylonitrile of present embodiment preferably contains detection process (3), in this process, uses the
Near (such as near raw material supply device) position of 1 thermometer 12 and the 2nd thermometer 13 to detect base feed gas
The presence or absence of abnormal heating.Detecting process (3) can both carry out before process (2), can also carry out after process (2).
The manufacturing method of the acrylonitrile of present embodiment can also have process (4) and/or process (5), in process (4)
In, after it will generate gas and be discharged and import cyclone separator from catalyst layer, gas will be generated and arranged from fluidized-bed reactor
Out, in process (5), the catalyst adjoint when generating gas and importing to cyclone separator is recycled, and return the catalyst
Return the catalyst layer.
[process (4)]
Process (4) will be discharged and is imported the generation gas after cyclone separator from catalyst layer will generate gas
The process being discharged from fluidized-bed reactor 1.The generation gas obtained in the process (2) is discharged from catalyst layer and from cyclonic separation
Device entrance 7 imports after cyclone separator 8c, cyclone separator 8b and/or cyclone separator 8a, from 1 row of fluidized-bed reactor
Out.
[process (5)]
Process (5) is to recycle the catalyst adjoint when generating gas and importing to cyclone separator and return the catalyst
The process for returning the catalyst layer.When generating gas from catalyst layer discharge, generates gas and be accompanied by catalyst, therefore be catalyzed
Agent is dispersed.In order to trap and generate catalyst that gas concomitantly disperses and separate the catalyst with gas is generated, such as
Use 3rd level cyclone separator 8a, the 2nd grade of cyclone separator 8b and/or the 1st grade of cyclone separator 8c as shown in Figure 1.Companion
With there is the generation gas of catalyst to flow into the cyclone inlet 7 of Fig. 1, and successively by the 1st grade of cyclone separator 8a, the
2 grades of cyclone separator 8b, 3rd level cyclone separator 8c generate gas and separate with catalyst.The catalyst separated is recovered
Into the 1st grade of material foot 9c, the 2nd grade of material foot 9b and the 3rd level material foot 9a for being respectively arranged in each cyclone separator, and return to catalysis
Oxidant layer 6.
It is narrow to the distance between stock dispersion pipe 5 from air (oxygen) dispersion plate 3 in fluidized-bed reactor,
Usually 50mm~450mm, and the same space exist for by unstrpped gas, air (oxygen) into fluid catalyst
The multiple nozzles sprayed.In addition to this, there is also the supporting member of the stock dispersion pipe, thermometer, various nozzles etc..In propylene
In the manufacture of nitrile, a part of the molybdenum (Mo) that the fluid catalyst in fluidized-bed reactor is included is from fluid catalyst liter
China, into reaction gas.Cooling coil, reactor are vaporized on as Mo oxide mostly in the sublimed Mo compound
The low temperature portion surface of wall, nozzle, cyclone separator etc..Fluid catalyst is involved in etc. on the surface by these Mo oxides
Solidification.The inventor of the utility model has found, with the progress of operating, the layer of Mo oxide increases, and surprising
It is that thickness is sometimes up to 5mm~20mm.Thermal shock caused by conversion of the Mo oxide skin(coating) because of the cooling coil in operating etc.,
It is normal stop and temperature history when emergent stopping etc. and peel off, and fall on reactor lower part.Mo oxide is broken due to falling
It is broken, become the Mo piece for the plate that surface area is several square centimeters~several dozen square centimeters.The Mo piece is mostly and fluidized bed catalytic
Agent is flowed together, is repeated sectionalization, is become having a size of several mm~micron-sized small pieces.On the other hand, with immobilising matter
The equipment of the obstructions flowings such as the large-scale Mo piece of amount, the peripheral part for dropping to reactor lower part, such as thermometer, nozzle, bearing
The Mo piece etc. of the poor position of mobility will not be segmented as aforementioned near part etc., and Mo piece is accumulated sometimes.The accumulation
Mo piece hinder the flowing of good catalyst, therefore the catalyst at the position becomes bad catalyst, is easy to generate abnormal heating.
In order to solve the above problems, inventor's discovery of the utility model, having near the position of base feed gas can be
The mechanism that early detection goes out abnormal heating is effective.
Embodiment
Then, present embodiment is illustrated by embodiment and comparative example in further detail.But present embodiment is only
Its purport is not departed from, then is not limited to following embodiments.
In addition, the fluidized bed reaction used in embodiment is identical as fluidized bed reaction shown in FIG. 1.Measurement
Device and auxiliary device are usually used equipment, and error is in usual range.
The yield and unreacted rate of reaction product are according to generating, gas sample and utilization gas-chromatography (GC) is surveyed
The analysis data measured are calculated using following formula.
(yield (%) of reaction product)=(the carbonaceous amount (g) in product)/(reaction raw materials supplied are i.e. organic
Carbonaceous amount (g) in compound) × 100
(unreacted rate (%))=and (unreacted reaction raw materials, that is, the carbonaceous amount (g) in organic compound)/it (is supplied
Carbonaceous amount (g) in reaction raw materials, that is, organic compound) × 100
In addition, the measuring device and measuring condition of GC are as follows.
Gas-chromatography: Shimadzu GC-14B
Column: Porapack-QS (50~80Mesh)
Detector: FID
Carrier gas: nitrogen
[embodiment 1]
Unstrpped gas, that is, propylene, ammonia and the air of reaction are supplied to fluidized-bed reactor 1 shown in FIG. 1, as following
The ammoxidation reaction of propylene has been carried out in this way.
Fluidized-bed reactor 1 is the vertical cylinder type of internal diameter 8m, length 20m, is had in the position away from lower part 2m oxygenous
Body dispersion plate 3 has unstrpped gas dispersion pipe 5 in the top of oxygen-containing gas dispersion plate 3.For measuring the temperature of catalyst layer
Thermometer is equipped with 20 between 1.5m~4.5m above away from oxygen-containing gas dispersion plate 3.For measuring reactor upper temp
Thermometer be equipped with two in cyclone separator 8a~top cyclone separator 8c space.As shown in Fig. 2, in oxygen-containing gas
Armoured thermocouple (the 1st thermometer) 12 is provided on dispersion plate 3.Inside the protecting pipe of armoured thermocouple (the 1st thermometer) 12
There are two the CA thermocouples of series for receiving.The material of protecting pipe is SUS316.Also, in oxygen-containing gas dispersion plate 3 and unstripped gas
The wall of reactor between body dispersion pipe 5 is provided with two armoured thermocouples (the 2nd thermometer) 13, and two armouring heat
Galvanic couple (the 2nd thermometer) 13 is as shown in figure 3, be arranged in the position away from wall 10mm~15mm along wall.In armoured thermocouple (
2 thermometers) 13 protecting pipe inside contain a serial CA thermocouple.The material of protecting pipe is SUS316.Catalyst makes
Molybdenum-bismuth-iron series the load for being 1.4wt.% with 24 μm of 10 μm~100 μm of partial size, 55 μm of average grain diameter, partial size containing ratios below
Catalyst, and it is filled into a height of 2.7m of quiescent layer.From oxygen-containing gas dispersion plate 3 with 56000Nm3/ h supplies air, from unstripped gas
Body feeder 4 is with 6200Nm3/ h supplies propylene and with 6600Nm3/ h supplies ammonia.Reaction temperature is 440 DEG C, the pressure on reactor top
Power is 0.70kg/cm2G, the pressure of the lower part (near unstrpped gas dispersion pipe 5) of fluidized-bed reactor 1 are 0.73kg/cm2G。
Reactor starts running, and stablizes post analysis reaction achievement, and the yield of acrylonitrile is 81.5%, the unreacted of propylene
Rate is 1.1%.During starting the operating to after 01 months 1 year, the yield of acrylonitrile becomes 80.9%~81.7%
Dynamic, the unreacted rate of propylene is changed 0.80%~1.3%.Then, since production adjusts, reactor is made to stopped two stars
Phase.During the stopping of fortnight, the catalyst in reactor is remained unchanged.In order to restart, by unstrpped gas and sky
Conductance has entered reactor.Stablize post analysis reaction achievement, the yield of acrylonitrile is 81.4%, and the unreacted rate of propylene is
1.0%.The yield of the acrylonitrile for the next day restarted is 79.9%, and the unreacted rate of propylene is 2.3%.On the same day at dusk,
Armoured thermocouple (the 2nd thermometer) 13 breaks down in temperature high side.Make reactor emergent stopping.The inside of reactor is carried out
It checks, 280 ° of position has found the block (about 40cm square) of catalyst in Fig. 4.With armoured thermocouple (the 2nd temperature at position
Meter) it 13 has fused, but it is sound with several stock dispersion pipe nozzles and air dispersion plate of near sites.To the block of above-mentioned catalyst
Catalyst performance is sampled and is observed, which has inactivated.There is no problem in performance for other catalyst, can be again
It uses.
[embodiment 2]
Using device same as Example 1, the propylene in unstrpped gas is become into propane, by unstrpped gas to fluidized bed
Reactor supply, has carried out the ammoxidation reaction of propane as so following.
Catalyst is 1.3wt.% using 24 μm of 10 μm~100 μm of partial size, 55 μm of average grain diameter, partial size containing ratios below
Molybdenum-vanadium system supported catalyst, and be filled into a height of 2.2m of quiescent layer.From oxygen-containing gas dispersion plate 3 with 64500Nm3/ h supply
Air, from unstrpped gas dispersion pipe with 4300Nm3/ h supplying propane and with 4300Nm3/ h supplies ammonia.Reaction temperature is 440 DEG C, stream
The pressure on 1 top of fluidized bed reactor is 0.75kg/cm2G, the pressure of 1 lower part of fluidized-bed reactor (near unstrpped gas dispersion pipe 5)
Power is 0.77kg/cm2G。
Analyze reaction achievement soon after reactor starts running, the yield of acrylonitrile is 52.1%, and propane is not
Reactivity is 10.8%.During the operating of a year and a half, the yield of acrylonitrile is changed 51.7%~52.5%, and propane is not
Reactivity is changed 9.9%~11.3%.After a year and a half, armoured thermocouple (the 1st thermometer) 12 occurs in temperature high side
Failure.Make reactor emergent stopping.The internal check for having carried out fluidized-bed reactor 1, the armoured thermocouple of the rightmost side in Fig. 2
(the 1st thermometer) 12, which is nearby accumulated, Mo piece, and armoured thermocouple (the 1st thermometer) 12 has fused.Catalyst, reactor be not different
Often.
[comparative example 1]
Other than being not provided with armoured thermocouple (the 1st thermometer) 12 and armoured thermocouple (the 2nd thermometer) 13 with
In the identical fluidized bed reaction of embodiment 1, with the propylene of catalyst and same traffic same as Example 1, ammonia and
Air operates fluidized bed reaction.
Analyze reaction achievement soon after reactor starts running, the yield of acrylonitrile is 81.5%, and propylene is not
Reactivity is 1.1%.During operating in 2 years, the yield of acrylonitrile is changed 79.9%~81.7%, propylene it is not anti-
Should rate 0.75%~1.3% change.After 2 years, it stopped reactor since reaction.The internal check of reactor is implemented,
Nearby there is the block of catalyst 170 ° of periphery, a unstrpped gas dispersion pipe nozzle near the block of the catalyst and contains
Carrier of oxygen dispersion plate melting loss.Confirmation can be carried out to catalyst performance, shown that the conversion performance of propylene has dropped 10%.
Industrial availability
The utility model can effectively utilize when using fluidized bed reaction to implement gas phase reaction.
Claims (4)
1. a kind of fluidized bed reaction, which has the fluidized-bed reactor comprising catalyst layer and is used for
The unstrpped gas feeder of base feed gas into the fluidized-bed reactor, the fluidized bed reaction is for manufacturing propylene
Nitrile, the fluidized bed reaction be characterized in that,
The fluidized bed reaction also has the thermometer being disposed near the unstrpped gas feeder.
2. fluidized bed reaction according to claim 1, which is characterized in that
The fluidized-bed reactor includes unstrpped gas dispersion pipe, is disposed in the lower section of the catalyst layer, and makes to utilize institute
The unstrpped gas that the supply of unstrpped gas feeder comes is stated to disperse into the catalyst layer；And oxygen-containing gas dispersion plate, with
The unstrpped gas dispersion pipe is disposed in the lower section of the unstrpped gas dispersion pipe spaced a predetermined distance fromly, and makes to be supplied to described
Oxygen-containing gas in fluidized-bed reactor disperses into the catalyst layer,
The thermometer is disposed in the oxygen-containing gas dispersion plate and the height along upper direction away from the unstrpped gas dispersion pipe 1m
Between position.
3. fluidized bed reaction according to claim 2, which is characterized in that
The oxygen-containing gas dispersion plate has multiple holes, so that the oxygen-containing gas is uniformly dispersed into the catalyst layer,
The thermometer has the 1st thermometer configured in a manner of not covering the multiple hole when looking down.
4. fluidized bed reaction described in any one of claim 1 to 3, which is characterized in that
The thermometer has the 2nd arranged circumferentially thermometer of the inner wall of the side wall along the fluidized-bed reactor.
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| CN114828995A (en) * | 2019-09-24 | 2022-07-29 | 株式会社Lg化学 | Fluidized bed reactor |
| CN115337871A (en) * | 2021-04-09 | 2022-11-15 | 中国石油化工股份有限公司 | Heat removal water pipe, fluidized bed reactor and application of fluidized bed reactor in acrylonitrile manufacture |
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| JP5770195B2 (en) * | 2010-09-14 | 2015-08-26 | 旭化成ケミカルズ株式会社 | Vapor phase exothermic reaction method and vapor phase exothermic reactor |
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| CN114828995B (en) * | 2019-09-24 | 2024-04-12 | 株式会社Lg化学 | Fluidized bed reactor |
| CN115337871A (en) * | 2021-04-09 | 2022-11-15 | 中国石油化工股份有限公司 | Heat removal water pipe, fluidized bed reactor and application of fluidized bed reactor in acrylonitrile manufacture |
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