CN209597140U - Fluidized bed reaction - Google Patents
Fluidized bed reaction Download PDFInfo
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- CN209597140U CN209597140U CN201822073382.7U CN201822073382U CN209597140U CN 209597140 U CN209597140 U CN 209597140U CN 201822073382 U CN201822073382 U CN 201822073382U CN 209597140 U CN209597140 U CN 209597140U
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Abstract
There is provided one kind can be prepared steadily in the long term, while also be able to maintain that the fluidized bed reaction of reaction achievement.A kind of fluidized bed reaction, it is that have fluidized-bed reactor, with the heat exchanger of the reaction gas export piping connection by the fluidized-bed reactor, the fluidized bed reaction that piping imports the piping of powder is exported with to the reaction gas, the reaction gas export piping has first part and second part, the first part extends along the short transverse of the fluidized-bed reactor from the top of the fluidized-bed reactor and reaches the highest point of the reaction gas export piping, the second part connect with the highest point and extends to the heat exchanger, the importing position of powder is the position in the second part and is the position lower than the highest point.
Description
Technical field
The utility model relates to a kind of fluidized bed reactions.
Background technique
It has industrially been implemented for a long time using the ammoxidation of fluidized-bed reactor.In order to improve α, β-unsaturation
The reaction yield of nitrile, for example, unstrpped gas point has been carried out as the exploitation of catalyst and the improvement of inside reactor device
The improvement of separate tube, dispersion plate.Tight gloomy taste victory hole tail just tough " the reaction engineering of fluidized bed " (Bei Fengguan (1984) distribution) of whip,
Fluidization Engineering (fluidized bed engineering)；DAIZO KUNII·OCTAVE LEVENSPIEL
Very conventional fluidized-bed reaction technology is discussed in (JOHNWILEY&SONS.INC, (1969) distribution).
When preparing monomer by gas phase catalytic reaction using fluidized-bed reactor, especially make ammonia, oxygen (in most cases
Use air) and alkene or the tertiary alcohol reaction when preparing unsaturated nitrile, in order to cool down generation high temperature reaction gas, it will usually
In reactor exit, heat exchanger is set.But it sometimes appear that by generate high boiling point by-products produced of reaction and from fluidized-bed reaction
A small amount of catalyst that device disperses is attached on the heat exchanger, causes to block, and reactor pressure rises, and makes to continue steadily in the long term
The case where operation becomes difficult.
Make technology to solve above-mentioned technical problem, is disclosed in patent document 1 a kind of with for making reaction gas
In the reactor of cooling heat exchanger, by being led in the process of running to the reaction gas between the reactor outlet and heat exchanger
Powder is imported in outlet pipe or imports the fluidized-bed reaction catalyst being piled up in reactor in above-mentioned reaction gas delivery line,
To remove the technology of the blocking substance in heat exchanger.
Existing technical literature
Patent document
[patent document 1] Japanese Laid-Open Patent Publication 5-301040 bulletin
Utility model content
Utility model will solve the problems, such as
According to the cleaning method recorded in patent document 1, although the speed that the pressure loss for being able to suppress heat exchanger rises,
Fluidized-bed reactor can be made to run steadily in the long term with phase ratio is not implemented, but be observed that reaction achievement occurs at any time
Between passage and the tendency of reduction.As it can be seen that from the angle run steadily in the long term without damaging reaction achievement, patent document
There is also rooms for improvement for the technology recorded in 1.
The utility model is based on obtained from above-mentioned the technical problems existing in the prior art, and its purpose is to provide one
Kind can be prepared steadily in the long term, while also be able to maintain that the fluidized bed reaction of reaction achievement.
The solution to the problem
The present inventor is by constantly studying, as a result, it has been found that being able to solve above-mentioned technology by adjusting the importing position of powder
Problem, so as to complete the utility model.
That is, the utility model is as follows.
[1]
A kind of fluidized bed reaction is that have fluidized-bed reactor and the reaction gas by the fluidized-bed reactor
The heat exchanger and export the fluidized bed reaction that piping imports the piping of powder to the reaction gas that body export piping connects,
Reaction gas export piping has first part and a second part, and the first part is from the fluidized-bed reaction
The top of device extends along the short transverse of the fluidized-bed reactor and reaches the highest point of reaction gas export piping, this
Two parts connect with the highest point and extend to the heat exchanger,
The importing position of powder is the position in the second part and is the position lower than the highest point.
[2]
The fluidized bed reaction according to [1], wherein have at least part of the second part along described
The middle section that short transverse extends downwardly,
The importing position of the powder is the middle section.
[3]
The fluidized bed reaction according to [1], wherein the first part with connect the highest point and the powder
Angle formed by the line of the importing position at end is 89 ° or less.
[4]
The fluidized bed reaction according to [1], wherein from the importing position of the powder in the second part to changing
The distance of hot device is 10m or more.
[5]
According to described in any item fluidized bed reactions of [1]~[4], it is used to prepare (methyl) acrylonitrile.
The effect of utility model
According to the utility model, being capable of providing one kind can be prepared steadily in the long term, while also be able to maintain that reaction
The fluidized bed reaction of achievement.
Detailed description of the invention
Fig. 1 be exemplify fluidized bed reaction that an example of present embodiment is related to schematically illustrate figure.
Fig. 2 is to exemplify other fluidized bed reactions being related to of present embodiment to schematically illustrate figure.
Fig. 3 is to exemplify the schematic sectional view for the fluidized-bed reactor that can be used in the present embodiment.
Fig. 4 is that fluidized bed reaction used in comparative example 1 schematically illustrates figure.
Description of symbols
1 fluidized bed reaction
2 reactors
3 heat exchangers
The export piping of 4 reaction gas
4A first part
4B second part
The middle section 4C
5 highest points
6 powder import position
7A cooling coil
7B cooling coil
7C cooling coil
8A cyclone separator
8B cyclone separator
8C cyclone separator
9 cyclone inlets
10A dipleg
10B dipleg
10C dipleg
Specific embodiment
Hereinafter, by side as needed referring to attached drawing, while (hereafter, being only called " this to the mode for implementing the utility model
Embodiment ") it is described in detail.Following present embodiments is only for illustrating the example of the utility model, not
Indicate that the utility model is only limitted to following contents.The utility model can carry out reality after various modifications in its main scope
It applies.In addition, using identical appended drawing reference for identical element, repeat description repeats no more in attached drawing.In addition, for
Equal positional relationship indicates positional relationship based on the figure unless otherwise noted up and down.Further, attached drawing
Dimension scale be not limited to diagram ratio.
Fluidized bed reaction of the present embodiment be one kind have fluidized-bed reactor and by the fluidized bed it is anti-
It answers the reaction gas of device to export the heat exchanger of piping connection and exports the fluidisation that piping imports the piping of powder to the reaction gas
Bed reaction device.In addition, the reaction gas export piping has first in fluidized bed reaction of the present embodiment
Part and second part, short transverse of the first part from the top of the fluidized-bed reactor along the fluidized-bed reactor are prolonged
The highest point of the reaction gas export piping is stretched and reaches, which connect with the highest point and prolong to the heat exchanger
It stretches, the importing position of powder is the position in the second part and is the position lower than the highest point.
Since with above-mentioned composition, the fluidized bed reaction being related to according to the present embodiment can be steadily in the long term
It is prepared, while being also able to maintain that reaction achievement.
Fluidized bed reaction of the present embodiment be one kind have fluidized-bed reactor and by the fluidized bed it is anti-
It answers the reaction gas of device to export the heat exchanger of piping connection and exports the fluidisation that piping imports the piping of powder to the reaction gas
Bed reaction device.
Hereinafter, being illustrated to the example of the fluidized bed reaction of present embodiment, but as long as being that can implement this reality
The device for applying each process in mode, then constitute it and be not particularly limited, can be using the fluidisation for having various compositions
Bed reaction device.
Fluidized bed reaction in present embodiment is that one kind has fluidized-bed reactor and by the fluidized-bed reaction
The heat exchanger and export the fluidized bed that piping imports the piping of powder to the reaction gas that the reaction gas export piping of device connects
Reaction unit.
As an example of such fluidized bed reaction, fluidized bed reaction shown in FIG. 1 can be enumerated.Fig. 1
In fluidized bed reaction 1 have reactor 2 and heat exchanger 3 and connect the reaction gas of reactor 2 and heat exchanger 3 and export
Piping 4.
Reaction gas export piping 4 has first part 4A and second part 4B.
First part 4A refers to from the top of reactor 2 and the short transverse of the reactor 2 in extending roughly in parallel, and arrives
Part until the highest point 5 of reaction gas export piping 4.The substantially parallel shape referred within parallel direction ± 10 °
State.
In addition, second part 4B refers to the part for connecting with above-mentioned highest point 5 and extending to heat exchanger 3.
Above-mentioned first part 4A and second part 4B is that reaction gas export piping 4 is divided into 2 areas for boundary with highest point 5
Domain, the component being not offered as in these parts are different.First part 4A and second part 4B i.e. in reaction gas export piping 4
Both it can be formed, can also be formed by connecting different components by identical part integration.
In embodiment shown in FIG. 1, using the line of first part 4A and the importing position 6 for connecting highest point 5 and powder
Formed angle α is less than 90 °, the composition that second part 4B is tilted down towards heat exchanger 3 along the short transverse of reactor 2.
Reaction gas is fed in heat exchanger 3 by reaction gas export piping 4.Further, pass through heat exchanger 3
Reaction gas is fed in flash cold column (not shown), then by recycling such as various well known purification process as product
((methyl) acrylonitrile).
In present embodiment, as described above, the second part in reaction gas export piping uses to have and is lower than highest point
Position composition, can to the position import powder.At this point, even if by the power in the contrary direction of export with reaction gas
It is applied to powder, to keep the powder mobile to reactor side, not only needs the power of the opposite direction, it is also necessary to be equivalent to arrival
The power of position energy until highest point.Therefore, the preparation method of (methyl) acrylonitrile being related to according to the present embodiment, can
Prevent imported powder adverse current to be moved to fluidized-bed reactor side, so as to be effectively prevented the movement due to powder
The catalyst degradation of the catalyst poisoning that may cause etc..
Above, as the typical case of present embodiment, piping (first part is exported to reaction gas shown in FIG. 1
And second part) and the importing position of powder be illustrated, as long as but powder import position second part in position
It sets and is the position lower than highest point, be then not limited to such example.It, can as other typical cases in present embodiment
To enumerate composition shown in Fig. 2.
Embodiment shown in Fig. 2, reaction gas export piping 4 in second part 4B composition with it is shown in FIG. 1
Embodiment is different, other compositions are then identical as the embodiment of Fig. 1.Although in embodiment i.e. shown in Fig. 2, first part
The joint angle of 4A and second part 4B is 90 °, but second part 4B has the centre that the short transverse along reactor 2 extends downwardly
Part 4C, powder are fed in any position of middle section 4C.Therefore, first part 4A with connect highest point 5 and powder
Importing position 6 line formed by angle α in the embodiment shown in figure 2 also for less than 90 °.
Middle section 4C is in extend roughly in parallel relative to the short transverse of reactor 2.It is substantially parallel to refer to that distance is flat
State within line direction ± 10 °.
As described above, having preferably at least part of second part along the height side of reactor in present embodiment
To the middle section extended downwardly, the importing position of powder is the middle section.By using such composition, presentation can be more
Imported powder adverse current is effectively prevented to be moved to the tendency of fluidized-bed reactor side.
Reactor 2 in the fluidized bed reaction 1 of Fig. 1 is equivalent to the reaction system of fluidized-bed reaction and external division
The main part of gas phase reaction device its shape is not particularly limited, can be using various well known shapes.
As shown in figure 3, reactor 2 can use in space inside it, such as possess following composition:
It is set to the lower part of 2 inner space of reactor, the temperature for removing reaction heat and controlling inner space (reacts temperature
Degree) cooling coil 7A, 7B and 7C；
It is configured at cyclone separator 8A, 8B and the 8C on the top of 2 inner space of reactor；
It is equivalent to the cyclone inlet 9 of the entrance of cyclone separator 8A；With
Dipleg 10A, 10B and the 10C being connect with the cyclone separator 8A, 8B and 8C.
In addition, going out although not shown in Fig. 3, but reactor 2 is generally configured with:
It is connect with the bottom of reactor 2, air (oxygen) ingress pipe of air (oxygen) is imported into reaction system；
Be set to the lower part of 2 inner space of reactor, make as reaction raw materials air (oxygen) in the reaction system
Air (oxygen) dispersion plate of dispersion；
It is connect with aftermentioned stock dispersion pipe top, the raw material other than air (oxygen) is imported into the raw material in reaction system
Ingress pipe；
It is set to the lower part of 2 inner space of reactor, the stock dispersion pipe for dispersing raw material in the reaction system；With
The catalyst layer being made of the fluid catalyst filled to the stock dispersion pipe top.
As the piping for importing powder into reaction gas export piping, it is not particularly limited, as long as in chemical device
Usually used piping.The length of piping, diameter, thickness etc. are also not particularly limited, it can be according to reaction gas
Flow, size of reaction gas export piping etc. are suitably selected.In addition, the adverse current of reaction gas in order to prevent, preferably exists
Some valves are nearby arranged in joint portion between reaction gas export piping and the piping for importing powder.The valve is either hand-operated valve
It is also possible to automatic valve, from the angle that can be controlled together with the metering of imported particle etc., preferably automated valve.
As the method for importing powder, it is not particularly limited.Pass through for example, can enumerate from the dedicated storage tank for saving particle
The method of the conveyings such as air.From the angle for the adverse current for preventing reaction gas, preferably the inside of the piping of importing powder is than anti-
Answer the pressure inside gas export piping high.
Specifically, fluidized-bed reaction may include: the base feed gas into the fluidized-bed reactor containing catalyst layer,
The process for flowing catalyst layer；Unstrpped gas is set to obtain the process that reaction generates gas by catalyst layer；Gas will be generated
After being discharged and import in cyclone separator from catalyst layer, reaction is generated into the process that gas is discharged from fluidized-bed reactor；With
Recycling reaction generates catalyst adjoint when gas is imported into cyclone separator, and the catalyst is made to be back to catalysis by dipleg
The process of oxidant layer.
As the oxygen-containing gas of supply to reactor, it is not particularly limited, such as air can be enumerated, containing the non-of oxygen
Active gases etc. generally uses air.Relative to hydrocarbon or the tertiary alcohol, the supply amount of oxygen-containing gas is preferably 5~15 molar ratios, more excellent
It is selected as 7~14 molar ratios.Relative to hydrocarbon or the tertiary alcohol, the supply amount of ammonia can be preferably 0.5~2 molar ratio, more preferably 1~
The range of 1.5 molar ratios.
As implementation condition, the temperature in catalyst layer is preferably 300~600 DEG C, and more preferably 400~500 DEG C, pressure
Preferably 3kg/cm2- G is hereinafter, more preferably 0.2~1.5kg/cm2-G.For fluid catalyst, can be used the palace of the Qing Dynasty it is rich he
Many texts such as " acrylonitrile " (chemical engineering, vol.48, No. 11,873-881 pages (1984)), tekiaki 51-40391 bulletin
The supported catalyst containing molybdenum offer, discussed in patent can enumerate such as molybdenum-bismuth-Fe-series catalyst.
In present embodiment, during carrying out fluidized-bed reaction, in reactor lower part, there are the dense layers of catalyst, in reactor
There are the sparse layers of catalyst on top.When i.e. fluid catalyst becomes flow regime in reactor, presents closer to top, urges
The smaller tendency of the space density of agent.As described in the big hiding " fluidization process " of state's well (Nikkan Kogyo Shimbun (1962) distribution),
In gas system, the height of fluidized bed may not be able to clearly be determined as liquid level, due to existing by big and small
Therefore protrusion caused by steeping also only approximatively, fifty-fifty determines.
In present embodiment, the range of the bound as the dense layer of catalyst can will be used by being mounted on reactor
On drive nozzle can measure pressure difference, by following formula calculate catalyst layer height as the upper limit, lower limit can determine
For the setting position of oxygen-containing gas dispersion pipe or dispersion plate.
Catalyst layer height Lr=(pressure difference between b-h)/((pressure difference between b-c)/(distance between b-c))+(distance between a-b)
In formula, a indicates the setting height of oxygen-containing gas dispersion pipe or dispersion plate, and b indicates oxygen-containing gas dispersion plate and raw material
The height of the intermediate point of gas dispersion tube, c indicate the height of the top 1m positioned at b, and h indicates cyclone inlet height.
In the upper area of the dense layer of the catalyst, the density of catalyst in fluid is smaller, referred to as the sparse layer of catalyst.In
In reactor, region that the sparse layer region of catalyst usually has layer region denser than catalyst wide.Reaction generates companion in gas
With catalyst inflow be set in the cyclone separator on reactor top.The major part of adjoint catalyst is in herein from reaction
It generates and is separated in gas, by the dipleg being mounted on the cyclone separator, be back to reactor lower part.In addition, from catalyst
Although the reaction isolated in generates to be not shown in gas Fig. 3, can be exported by delivery line to reactor.In addition,
For cyclone separator in Fig. 3, although only giving 1 series (3), the quantity of cyclone separator can be according to reactor
Size, catalyst particle size and reaction generate gas flow and determine, it will usually be arranged multiple.In addition, if being arranged in series 2 or more
Cyclone separator, can present catalyst arresting efficiency improve tendency.
The ammoxidation reaction of most base feed gas carries out in the dense layer of catalyst, generates reaction heat.This is urged
In the dense layer of agent, since catalyst high density exists, thus heat exchanger effectiveness is high.Equipment in order to reduce control reaction temperature
Burden, remove effectively reaction heat and control temperature the dense layer of catalyst in install at least with 40% or more it is thermally conductive
The cooling coil of area.In order to reduce reaction temperature part it is unbalanced, cooling coil can be by with heat-conducting area size
Different multiple serial groups independent are constituted.
Cooling coil in present embodiment can be used between the various known forms being set in fluidized-bed reactor
Heat exchanger is connect, it is unlimited to its type, size and shape.Flow through cooling coil cryogen be ammoxidation reaction temperature with
Under, preferably 100~300 DEG C of fluid, such as warm water, high pressure warm water, steam, above-mentioned mixture or melting can be used
Salt.
As in present embodiment, unstrpped gas is imported in the fluidized-bed reactor, in the presence of a catalyst
Ammoxidation reaction is carried out, the process for obtaining reaction gas is not particularly limited, can be for for example to the reactor for being filled with catalyst
Such as propane or propylene, ammonia and oxygen of the middle supply as raw material react to obtain acrylonitrile as reaction by gas phase ammonoxidation
The process of gas, or supplied isobutene, the tert-butyl alcohol or iso-butane, ammonia and oxygen as raw material, pass through vapor phase ammonia oxygen
Change reaction and obtains process of the methacrylonitrile as reaction gas.
In fluidized-bed reaction, catalyst granules needs to remain flow regime.As catalyst, or the prior art
It is middle as substance well known to the catalyst used when preparing unsaturated nitrile by ammoxidation reaction according to above-mentioned raw materials gas.Example
It such as, can be that composite oxides as main component are made with molybdenum and/or antimony in the ammoxidation reaction of alkene.In addition, as stone
Catalyst used in the ammoxidation reaction of wax can enumerate and for example make composite oxides as main component with molybdenum or vanadium.
It for the reaction pressure in fluidized-bed reactor, is not particularly limited, can be such as 1.5kg/cm2G or less.As reaction temperature
Degree, is not particularly limited as long as raw material reacts under gas phase state, can be 400~500 DEG C.
In present embodiment, powder is imported into reaction gas export piping, the heat exchanger is cleaned on one side, on one side by institute
Stating reaction gas and exporting to the process of the heat exchanger is to cool down and prevent to react with being originated from for the cooling from reaction gas
The ingredient of gas is attached to the angle inside heat exchanger and sets out progress.I.e. by the process, it is generated by ammoxidation reaction anti-
Gas should be generated to be imported into heat exchanger, it is cooled by refrigerant.As long as heat exchanger has cooling capacity appropriate, to it
Mode, structure are not particularly limited.Wherein, from the angle of the cooling efficiency in heat exchanger, preferably shell/pipe heat exchanger.Make
In pipe side (in pipe) for the conducting-heat elements of the heat exchanger, it is imported into the generation gas for carrying out autoreactor, shell-side (outside pipe) quilt
Refrigerant is imported, by the heat exchange between them, the heat that gas has is generated and is recovered.
The temperature for being imported into the refrigerant in heat exchanger is 110 DEG C or more, using being heated to the substance of the temperature in advance i.e.
It can.By using the refrigerant for being heated to 110 DEG C or more, it is able to maintain that the high boiling point by-products produced temperature for being higher than and generating in gas
Degree, prevents blocking caused by the high boiling point by-products produced condensation in the heat exchanger due to reactor outlet pipeline.
Catalyst used in reaction process is the small particle that such as average grain diameter is 50 μm or so, is generated in gas
Contain the catalyst granules.From the angle for more efficiently preventing from such catalyst granules and being piled up in heat exchanger, use
When shell/pipe heat exchanger, preferably pipe (tube) is straight tube, and generation gas one way is preferably made to pass through the structure in the pipe.
From the angle of wall surface that is effective and being prevented securely from the high boiling point by-products produced generation gas flow path for being attached to heat exchanger
It sets out, preferably the temperature of the refrigerant imported in heat exchanger is monitored to carry out temperature control.Closer to downstream, generate
The gas temperature of gas flow path is lower, high boiling point by-products produced more easy to attach.Therefore, using by refrigerant from generate gas flow path
Downstream side import mode, i.e. convection type, the inlet temperature (supplying temperature) that refrigerant enters heat exchanger is controlled
Words are also easier to be managed the temperature in the downstream side for generating gas, thus preferably.In addition, from same angle, it is right
The temperature for generating the heat exchanger exit of gas is monitored, so that its temperature reaches certain temperature with Shangdi in importing heat exchanger
Refrigerant temperature and/or flow to carry out control be also preferred.But, it is not absolutely required to correct measurements to generate gas
The temperature of heat exchanger exit, as long as holding to the refrigerant in the temperature and importing heat exchanger for the heat exchanger exit for generating gas
There are certain relationships between temperature, can also be monitored to the temperature of the refrigerant imported in heat exchanger, so that control should
The temperature and/or flow of refrigerant.
The refrigerant imported in heat exchanger can be liquid, be also possible to gas.As the liquid that refrigerant uses, preferably
For water, such as pure water, industrial water, seawater and the mixture of more than two kinds in them can be enumerated.Such refrigerant
As long as being adjusted by boiler pressurization, heating to 110 DEG C or more of temperature.As the gas that refrigerant uses, can enumerate
Such as vapor, air, nitrogen, carbon dioxide or the mixture of more than two kinds in them out.As long as such refrigerant passes through
The heating such as boiler, adjusts to 110 DEG C or more.From more effective and effectively suppress the higher boiling by-product for generating and containing in gas
The angle that object is attached to the inner wall (such as surface of conducting-heat elements) of heat exchanger is set out, and the temperature of the refrigerant in heat exchanger is imported
Preferably 140~260 DEG C, more preferably 170~240 DEG C.In order to control the temperature of refrigerant to desired temperature, as long as right
Supply the amount and temperature adjustment of the warmed-up refrigerant into heat exchanger.Wherein, the generation due to being flowed out from reactor
The temperature of gas be with the substantially comparable temperature of reaction temperature, therefore generally 400~500 DEG C.Therefore, even if the temperature of refrigerant
Within the above range, the cooling for generating gas can also be carried out unquestionably degree.
Further, from more effective and be prevented securely from the high boiling point by-products produced generation gas flow path for being attached to heat exchanger
The angle of wall surface is set out, in present embodiment, when exporting reaction gas to heat exchanger, by the way that powder is imported reaction gas
In export piping, while carrying out the cleaning of heat exchanger.
It as powder, is not particularly limited, can be used such as sand, waste catalyst, ammonium sulfate, sodium sulphate, from cleaning
The angle of efficiency is set out, preferably sulfuric acid sodium.
In addition, as depicted in figs. 1 and 2, as long as meeting the composition of present embodiment, first part with connect highest point and powder
Angle α formed by the line of the importing position at end is less than 90 °.In present embodiment, first part with connect highest point and powder
Importing angle formed by the line of position is preferably 89 °.When using such composition, presentation can more efficiently prevent from imported powder
Last adverse current is to be moved to the tendency of fluidized-bed reactor side.
In present embodiment, from the angle for further increasing cleaning efficiency, from the importing of the powder in second part
The distance of position to heat exchanger is preferably 10m or more, more preferably 30m or more.Powder described herein from second part
The distance of importing position to heat exchanger can be found out based on the length of the piping in second part, Fig. 1 and mode shown in Fig. 2
In, it is expressed as the aggregate value of L2 and L3.
In present embodiment, the distance of the importing position from highest point to powder is preferably 0.5m or more, more preferably 3m
More than.When using such composition, it is anti-to be moved to fluidized bed that presentation can more efficiently prevent from imported powder adverse current
Answer the tendency of device side.The distance of importing position described herein from highest point to powder can be based on the piping in second part
Length find out, in mode shown in FIG. 1, be expressed as L1, in mode shown in Fig. 2, be expressed as the aggregate value of L1a and L1b.
Embodiment
Next, present embodiment is described in more detail by embodiment and comparative example.But, present embodiment
Without departing from its purport, however it is not limited to following embodiments.
(embodiment 1)
In embodiment 1, the preparation of acrylonitrile is carried out using fluidized bed reaction shown in Fig. 2.From fluidized-bed reactor
Top extend along the short transverse of the fluidized-bed reactor and reach reaction gas export piping highest point first
Part is 89 ° or less with angle formed by the line for the importing position for connecting highest point and the powder.
As reactor 2, the reactor of composition shown in Fig. 3 is used.It is constituted using following: being had in the lower part of reactor 2
There are the dispersion pipe and dispersion plate (not shown) of the gas as reaction raw materials, in addition, configuring in the lower part of fluidized-bed reactor
Cooling coil 7A~7C is mixed into the catalysis generated in gas flowed out from reactor in the configuration trapping of the top of fluidized-bed reactor
Catalyst is returned to lower part by dipleg 10A~10C by cyclone separator 8A~8C of agent.
In addition, it is linked to be 3 sections 1 series of conduct using series connection as shown in Figure 3 as cyclone separator, it is same total
Configure 8 series.Metrical instrument, auxiliary device are usually used metrical instrument, auxiliary device.
Propylene, ammonia and air are supplied into the reactor 2 of the diameter 7.8m for the catalyst for being 50 μm filled with average grain diameter,
Carry out ammoxidation reaction.In order to confirm the state of catalyst, the catalyst before being started by atom light absorption method to reaction carries out group
At analysis, as a result, it has been found that, the Na concentration in catalyst is 1500ppm.The reaction gas generated in reactor 2 is via reaction gas
Export piping 4, is cooled down by heat exchanger 3.Heat exchanger 3 uses the multitube drum type brake of the single tube journey of diameter 1.8m, length 2.2m
Heat exchanger, refrigerant use water.
1700mmH is risen in the pressure loss of heat exchanger 32When O, to the middle section 4C of reaction gas export piping 4
In position 6 import average grain diameter be 0.1mm sodium sulphate (powder).It is the position lower than highest point 5 that powder, which imports position 6,.
Before and after powder importing, the reduction of the significant pressure loss has been confirmed.In this way, reaction continues 2 years after starting.
After reaction, filling to the catalyst in reactor 2 is extracted out, in order to confirm the state of catalyst, passes through atom light absorption method
The composition of catalyst is analyzed, as a result, it has been found that, the Na concentration in catalyst is 1500ppm.Catalysis i.e. after reaction
Agent does not observe the variation of Na concentration compared with the catalyst before reaction starts.
Further, (pressure loss of above-mentioned heat exchanger 3 rises to the reaction achievement after finding out equipment starting
1700mmH2Reaction achievement when O) with continue 2 years achievement reacted shortly before arrestment by the sandblasting of powder.That is,
Gas sample to reactor outlet analyzes reaction gas by gas chromatograph, calculates the acrylonitrile phase of generation
For supplying to the ratio of the propylene of reactor, as a result respectively 81.5%, 81.3%, continue not observe after 2 years powder import
To the variation of reaction achievement.
According to the above results it is found that method according to the present embodiment, can prepare acrylonitrile, and also can steadily in the long term
It is enough to maintain reaction achievement.
(comparative example 1)
In comparative example 1, other than using fluidized bed reaction shown in Fig. 4, propylene is carried out similarly to Example 1
The preparation of nitrile.Fluidized bed reaction shown in Fig. 4 is that have and Fig. 2 institute other than the shape of reaction gas export piping
The device of the identical composition of the fluidized bed reaction shown.That is, in fluidized bed reaction shown in Fig. 4, first part 4A and
Two part 4B are at right angles connected, the middle section 4C in not formed Fig. 2.
1700mmH is risen in the pressure loss of heat exchanger 32When O, to the first part 4A of reaction gas export piping 4
In position 6 in import average grain diameter be 0.1mm sodium sulphate (powder).Although it is lower than highest point 5 that powder, which imports position 6,
Position, but it is the position in first part 4A.After the powder imports, compared with before importing, subtracting for the pressure loss has been confirmed
It is few.In this way, reaction continues to react for 2 years after starting.After reaction, filling to the catalyst in reactor 2 is extracted out,
In order to confirm the state of catalyst, analyzed similarly to Example 1, as a result, it has been found that, the Na concentration in catalyst is
4900ppm.As it can be seen that having confirmed the poisoning of catalyst sodium.From this result, a part of the powder of importing is countercurrently to reactor
Side.
Further, the reaction achievement after equipment starts is found out similarly to Example 1 and continues the spray by powder in 2 years
Reaction achievement of the sand shortly before arrestment, as a result respectively 81.5%, 79.2%, continue to observe after 2 years powder import
To the deterioration of reaction achievement.From this result, since the powder of importing causes catalyst poisoning, reaction achievement is had occurred
Deteriorate.
Industrial availability
When the utility model implements fluidized-bed reaction using fluidized bed reaction, it can effectively utilize.
Claims (5)
1. a kind of fluidized bed reaction is that have fluidized-bed reactor and the reaction gas by the fluidized-bed reactor
The heat exchanger and export the fluidized bed reaction that piping imports the piping of powder to the reaction gas that export piping connects,
It is characterized in that,
Reaction gas export piping has first part and a second part, and the first part is from the fluidized-bed reactor
Top extends along the short transverse of the fluidized-bed reactor and reaches the highest point of reaction gas export piping, and this second
Divide and connect with the highest point and extend to the heat exchanger,
The importing position of powder is the position in the second part and is the position lower than the highest point.
2. fluidized bed reaction according to claim 1, which is characterized in that at least part of the second part
With along the middle section that the short transverse extends downwardly,
The importing position of the powder is the middle section.
3. fluidized bed reaction according to claim 1, which is characterized in that the first part with connect the highest
Angle formed by the line of the importing position of point and the powder is 89 ° or less.
4. fluidized bed reaction according to claim 1, which is characterized in that from leading for the powder in the second part
The distance for entering position to heat exchanger is 10m or more.
5. fluidized bed reaction according to any one of claims 1 to 4, which is characterized in that it is used to prepare (first
Base) acrylonitrile.
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| JP2017-236864 | 2017-12-11 | ||
| JP2017236864A JP7012523B2 (en) | 2017-12-11 | 2017-12-11 | Method for producing (meth) acrylonitrile |
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| CN201822073382.7U Active CN209597140U (en) | 2017-12-11 | 2018-12-11 | Fluidized bed reaction |
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| CN110947342A (en) * | 2019-12-29 | 2020-04-03 | 安徽瑞邦生物科技有限公司 | Ammonia oxidation reaction heat energy recycling device and method |
| CN114192077B (en) * | 2021-12-16 | 2023-05-26 | 万华化学集团股份有限公司 | Fluidized bed reactor and system device for preparing isophthalonitrile |
Family Cites Families (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4366855A (en) * | 1981-02-27 | 1983-01-04 | Milpat Corporation | Self-cleaning recuperator |
| JPS5855352Y2 (en) * | 1981-05-11 | 1983-12-17 | 志津男 佐川 | Heat exchanger pipe cleaning equipment |
| JPS6026959B2 (en) * | 1981-08-11 | 1985-06-26 | 日本施設保全株式会社 | Method for removing carbon scale from heating piping for crude oil refining |
| DK0425633T3 (en) * | 1989-04-14 | 1994-11-28 | Procedes Petroliers Petrochim | Process for steam phase cracking of hydrocarbons |
| FR2670479B1 (en) * | 1990-12-17 | 1993-05-28 | Electricite De France | PROCESS FOR TREATING SILICA FUMES WITH A VIEW TO THEIR BLEACHING, AND DEVICE FOR CARRYING OUT SAID METHOD. |
| JPH05301040A (en) * | 1992-04-24 | 1993-11-16 | Asahi Chem Ind Co Ltd | Method for washing heat exchanger for reactor |
| JPH07275686A (en) * | 1994-04-05 | 1995-10-24 | Nippon Steel Corp | Circulation fluidized reaction apparatus |
| CN1055916C (en) * | 1997-06-06 | 2000-08-30 | 中国石油化工总公司 | fluid bed reactor for ammoxidation of hydrocarbons |
| JP3906174B2 (en) * | 2003-03-24 | 2007-04-18 | 三井造船株式会社 | High temperature corrosion countermeasure and cleaning system of convection heat transfer section in circulating fluidized bed boiler. |
| CN102010350B (en) * | 2009-09-07 | 2013-12-18 | 中国石油化工集团公司 | Method for increasing production capacity of acrylonitrile or methacrylonitrile |
| CN102049315B (en) * | 2009-10-30 | 2013-01-09 | 中国石油化工股份有限公司 | Method for preparing catalytic cracking catalyst |
| JP2011236995A (en) | 2010-05-12 | 2011-11-24 | Daiyanitorikkusu Kk | Method for preventing liquid retention in pipe and preventive structure |
| CN104279914A (en) * | 2013-07-09 | 2015-01-14 | 中国石油化工股份有限公司 | Online decoking device and decoking method |
| CN103968689A (en) | 2014-05-26 | 2014-08-06 | 英尼奥斯欧洲股份公司 | Waste water cooler used in acrylonitrile manufacture |
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| JP7012523B2 (en) | 2022-02-14 |
| CN109894059B (en) | 2021-08-20 |
| CN109894059A (en) | 2019-06-18 |
| JP2019104693A (en) | 2019-06-27 |
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