CN101507907B - Temperature control method of fluidized bed reactor - Google Patents
Temperature control method of fluidized bed reactor Download PDFInfo
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- CN101507907B CN101507907B CN2008100061620A CN200810006162A CN101507907B CN 101507907 B CN101507907 B CN 101507907B CN 2008100061620 A CN2008100061620 A CN 2008100061620A CN 200810006162 A CN200810006162 A CN 200810006162A CN 101507907 B CN101507907 B CN 101507907B
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Abstract
The invention provides a temperature control method, which can more precisely control the temperature in a fluidized bed reactor when the fluidized bed reactor is used for implementing gas-phase exothermal reaction. The method for controlling the temperature when the fluidized bed reactor which is provided with a general heat extraction pipe, a heat extraction adjusting pipe and a temperature detector is used for implementing the gas-phase exothermal reaction comprises the following steps: (i) performing heat extraction through the general heat extraction pipe, and simultaneously detecting the temperature of the fluidized bed reactor through the temperature detector; and (ii) converting the heat extraction capacity of the heat extraction adjusting pipe from less than 10 percent of the adjustable range FS to more than 90 percent or from more than 90 percent to less than 10 percent at the average change rate of more than 0.1 FS per minute when the detected temperature deviates from the set temperature so as to adjust the temperature of the fluidized bed reactor to the set temperature.
Description
Technical field
The present invention relates to the temperature-controlled process of fluidized-bed reactor, in more detail, relate to when using fluidized-bed reactor to implement the gas phase exothermic reaction, can control the temperature-controlled process of the temperature in the reactor more accurately.
Background technology
On through gas phase exothermic reaction industry, make when making the useful monomer of various synthetic resin and synthetic fibers widely-used fluidized-bed reactor.As the representation of the gas phase exothermic reaction of implementing in the industry, can enumerate the continuous oxidation reaction of ammoxidation reaction under the coexistence of partial oxidation reaction, ammonia etc.In continuous oxidation reaction,, thereby be accompanied by the carrying out of reaction, promptly be accompanied by the rising of reaction conversion ratio because so not high usually as the oxidation stability of the partial oxidation products of target product, carry out the successive reaction of target product.Its result has the tendency that the complete oxidation product increases, the selection rate of target product reduces.Therefore, the yield with conversion ratio and the long-pending target product that obtains of selection rate has maximum on certain conversion ratio.For example, disclose following content in the non-patent literature 1: about the acrylonitrile manufacturing that the ammoxidation reaction through propylene carries out, be 85～95% o'clock at conversion ratio usually, yield is a peak.Therefore, for economically, manufacturing objective product more advantageously, it is extremely important that the conversion ratio of reaction is controlled at preferable range.Think that certainly this is not limited to oxidation reaction, general gas phase exothermic reaction is also set up.
On the other hand, compare with other reactor types, the reactor of for example fixed-bed type, as one of advantage that fluidized-bed reactor had, can enumerate out heat in the reactor move soon, than being easier to control reaction temperature.When using fluidized-bed reactor to implement the gas phase exothermic reaction, during temperature in the control reactor, use following method usually, that is, control the temperature in the reactor based on the temperature that Temperature Detector detected that is arranged in the reactor.For example, patent documentation 1 discloses following content:, at least one flows through cooling medium in removing heat pipe with variable velocity, and through regulating its flow, thus the temperature control method of the fluidized-bed reactor of temperature controllable and fluidized-bed reactor.In addition, patent documentation 2 discloses following content: at the mixture of feed fluid and steam thereof during as cooling medium, control method of temperature through the flow of the liquid that mixed in the steam of regulating certain flow basically.
Non-patent literature 1: Tanaka Tienan, " acrylonitrile improvement of Manufacturing Technology ", daily use chemicals association monthly magazine, civic organization's Japan Chemical Industry Association, clear and in October, 46 number, p551-561
Patent documentation 1:WO95/21692 brochure
Patent documentation 2: No. 2697334 specification of United States Patent (USP)
Summary of the invention
The problem that invention will solve
Here, the conversion of raw material of gas phase exothermic reaction depends on activity of such catalysts, and conversion ratio also rises when catalyst activity rises.In addition, catalyst activity depends on reaction temperature, and except the such example of enzyme reaction, when reaction temperature rose usually, catalyst activity rose.And then, for example in the situation of oxidation reaction, when partial oxidation products can be compared with the generation of complete oxidation product, can know complete oxidation product (CO for example
2) more stable, if the contribution rate of complete oxidation rises, then all thermal discharges of reaction system increase, this is self-explantory.Can think that this also sets up general gas phase exothermic reaction.
Therefore; In the gas phase exothermic reaction,, trend towards showing below do action if reaction temperature is former thereby when rising because of some: when 1) temperature rises catalyst activity rise, 2) follow catalyst activity to rise and the conversion ratio of reaction rises; Thereby carrying out successive reaction, 3) amount of real reaction increases in the middle of the raw material supplied with; In addition, follow the carrying out of successive reaction, the contribution of more stable product increases; Thereby the thermal discharge of the time per unit that reaction system is all increase, 4) result, reaction temperature further rises.Certainly the situation of reaction temperature reduction too; Be to show reverse do action; In arbitrary situation,, become the reason that produces the reactor temperature distribution because temperature is dispersed at the local location of reactor; And then in extreme situation, all temperature of reactor disperse and might cause the thermal runaway of reactor, reaction to stop.Therefore, in the gas phase exothermic reaction, for economical and more advantageously the manufacturing objective product be needless to say, for sustained response stably, it is extremely important controlling reaction temperature subtly.
Like this, in view of the temperature controlled importance in the gas phase exothermic reaction, according to reaction, temperature control traditionally is also insufficient, requires further precise dose control.In view of the foregoing, when the object of the present invention is to provide, can control the temperature-controlled process of the temperature in the flow reactor more accurately with the exothermic reaction of fluidized-bed reactor enforcement gas phase.
The method of dealing with problems
The inventor has carried out research in depth to the problems referred to above; The result finds a kind of temperature-controlled process; It is conventional temperature-controlled process except that heat pipe, when regulating the fluidized-bed reactor enforcement gas phase exothermic reaction that removes heat pipe and Temperature Detector for use has; This method comprises: when (i) removing the heat pipe heat extraction through aforementioned routine, detect the operation of the temperature in the aforementioned fluidized-bed reactor through the aforementioned temperature detector; During the temperature departure design temperature that (ii) detects; With the mean change speed more than 0.1FS/ minute, make heat-removal capability that aforementioned adjusting removes heat pipe from adjustable extent F S 10% below to change 90% or more, perhaps, from more than 90% to variation below 10%, with the operation of the temperature in the aforementioned fluidized-bed reactor to the design temperature adjusting; Through this method; When implementing the gas phase exothermic reaction, can control the temperature in the reactor more accurately, and accomplish the present invention with fluidized-bed reactor.
That is, the present invention is following.
[1]
Temperature-controlled process, it is conventional temperature-controlled process except that heat pipe, when regulating the fluidized-bed reactor enforcement gas phase exothermic reaction that removes heat pipe and Temperature Detector for use has, and this method comprises:
When (i) removing the heat pipe heat extraction, detect the operation of the temperature in the aforementioned fluidized-bed reactor through the aforementioned temperature detector through aforementioned routine;
During the temperature departure design temperature that (ii) detects; With the mean change speed more than 0.1FS/ minute; Make heat-removal capability that aforementioned adjusting removes heat pipe from adjustable extent FS 10% below to change 90% or more, perhaps, from more than 90% to variation below 10%, with the operation of the temperature in the aforementioned fluidized-bed reactor to the design temperature adjusting.
[2]
Above-mentioned [1] described method, in the temperature range of implementing aforementioned gas phase exothermic reaction, total reaction heat is 50～2500kJ/mol (raw material), and the partial differential coefficient to temperature of aforementioned total reaction heat is 0.2～40kJ/mol (raw material) K.
[3]
Above-mentioned [1] or [2] described method, aforementioned gas phase exothermic reaction is for being the gas phase ammonoxidation reaction of raw material with propane and/or propylene, the product of reaction is an acrylonitrile.
[4]
Above-mentioned [1] or [2] described method, aforementioned gas phase exothermic reaction is in the group that normal butane, 1-butylene, 2-butylene, butadiene, benzene formed being the gas phase oxidation of raw material to be selected from more than a kind, the product of reaction is a maleic anhydride.
[5]
Above-mentioned [1] or [2] described method, aforementioned gas phase exothermic reaction is for being the gas phase ammonoxidation reaction of raw material with isobutene and/or iso-butane, the product of reaction is a methacrylonitrile.
[6]
Above-mentioned [1] or [2] described method, aforementioned gas phase exothermic reaction is for being the gas phase oxidation of raw material with ortho-xylene and/or naphthalene, the product of reaction is a phthalic anhydride.
[7]
Above-mentioned [1] or [2] described method, aforementioned gas phase exothermic reaction is for being the vapor phase alkylation of raw material with phenol and methyl alcohol, the product of reaction is 2,6-xylenols and/or orthoresol.
[8]
Above-mentioned [1] or [2] described method, aforementioned gas phase exothermic reaction is for being the gas phase ammonoxidation reaction of raw material with methane and/or methyl alcohol, the product of reaction is hydrogen cyanide (HCN).
[9]
Above-mentioned [1] or [2] described method, aforementioned gas phase exothermic reaction is in the group that ethane, ethene, ethanol formed being the gas phase ammonoxidation reaction of raw material to be selected from more than a kind, the product of reaction is an acetonitrile.
[10]
A kind of manufacturing approach, it has the conventional manufacturing approach of removing heat pipe, regulating the target compound of the fluidized-bed reactor that removes heat pipe and Temperature Detector for using, and this manufacturing approach comprises:
(a) base feed in the aforementioned fluidized-bed reactor that is filled with catalyst, the operation of enforcement gas phase exothermic reaction;
When (b) removing the heat pipe heat extraction, detect the operation of the temperature in the aforementioned fluidized-bed reactor through the aforementioned temperature detector through aforementioned routine;
During the temperature departure design temperature that (c) detects; With the mean change speed more than 0.1FS/ minute; Make heat-removal capability that aforementioned adjusting removes heat pipe from adjustable extent FS 10% below to change 90% or more, perhaps, from more than 90% to variation below 10%, with the operation of the temperature in the aforementioned fluidized-bed reactor to the design temperature adjusting.
The invention effect
According to temperature-controlled process of the present invention, when implementing the gas phase exothermic reaction, can control the temperature in the fluidized-bed reactor more accurately with fluidized-bed reactor.
Description of drawings
Fig. 1 representes an example of the fluidized-bed reactor in this embodiment.
Symbol description
1 fluidized-bed reactor
2 catalyst fluidized beds
3 airways
4 raw material ingress pipes
5 reactions generate gas and extract pipe out
6 use the routine of the cooling medium of liquid to remove heat pipe
The routine of the cooling medium of 7 using gases is removed heat pipe
8 regulate except that heat pipe
9 gas-liquid separation containers
10 cooling medium delivery pumps
11 cooling mediums append pipe
12 superheated vapors are extracted pipe (conventional heat extraction is effective) out
13 cooling medium consumption control valves (regulate and remove heat pipe capacity adjustment valve)
14 superheated vapors are extracted pipe (it is effective to regulate heat extraction) out
15 temperature of reactor detectors
16 attemperators
17 saturated vapors are extracted pipe out
The specific embodiment
Below, the specific embodiment (following is this embodiment) that is used for embodiment of the present invention is elaborated.In addition, the present invention is not limited to following embodiment, in the scope that does not change its purport, can carry out various distortion and implement.
The temperature-controlled process of this embodiment is conventional temperature-controlled process except that heat pipe, when regulating the fluidized-bed reactor enforcement gas phase exothermic reaction that removes heat pipe and Temperature Detector for use has; This method comprises: when (i) removing the heat pipe heat extraction through aforementioned routine, detect the operation of the temperature in the aforementioned fluidized-bed reactor through the aforementioned temperature detector; During the temperature departure design temperature that (ii) detects; With the mean change speed more than 0.1FS/ minute; Make heat-removal capability that aforementioned adjusting removes heat pipe from adjustable extent FS 10% below to change 90% or more, perhaps, from more than 90% to variation below 10%, with the operation of the temperature in the aforementioned fluidized-bed reactor to the design temperature adjusting.
Fluidized-bed reactor in this embodiment has routine to be removed heat pipe, regulates and remove heat pipe and Temperature Detector.Temperature Detector has more than one and gets final product, and can have a plurality of.The position of Temperature Detector is set as long as,, can be arranged at the thin layer of the dense layer of catalyst gas vent etc. according to purpose for the then not special restriction in place of the temperature of assaying reaction device stably.The form of set Temperature Detector is not special to be limited, and can use the detector of normally used form, for example thermocouple, temperature detecting resistance body.
Fluidized-bed reactor has the said temperature detector and has the conventional heat pipe that removes and removes heat pipe with regulating." the conventional heat pipe that removes " in this embodiment is meant: control the heat pipe that removes that reactor temperature is the conventional use of purpose to remove reaction heat." adjusting removes heat pipe " is meant: when the temperature departure design temperature that removes the heat pipe heat extraction with routine and detected, be used for the remove heat pipe of reactor temperature to the design temperature adjusting.
As long as the set shape of removing heat pipe can suitably be arranged at then not special restriction in the reactor; From the easy degree and the handling ease degree of having bought material; Be generally the employed material of pipe arrangement, promptly, with steel pipe with the steel pipe combination of interfaces, be processed to the U font that several are connected.Remove the also not special restriction of material of heat pipe; Can be according to employed condition, be the having or not etc. of temperature, pressure, saprophagous character of the such institute's fluid in contact of cooling medium or reacting gas, from the pipe arrangement material, for example be specified in the pipe arrangement material of JIS G-3454, G-3458, G-3459 and be specified in the steel pipe interface of JIS B-2311 etc. and freely select to use.
As fluidized-bed reactor, adopt following form usually, that is, the upwelling of the gas that imports from reactor lower part makes catalyst granules keep the upwelling form of liquidation state.But in this embodiment, having more than and be limited to this form, also can be sinking form or other modes.
[operation (i)]
When operation (i) is removed the heat pipe heat extraction for passing through routine, detect the operation of the temperature in the fluidized-bed reactor through Temperature Detector.
Conventional remove heat pipe be conventional use remove heat pipe, its for according to the feed speed of raw material, or reduce according to the ability of removing heat pipe that causes such as polluting, the purpose of coarse adjustment heat-removal capability and using, it is changeable for use or do not use.Therefore, in order roughly to regulate total heat-removal capability, the pipe that preferably will have certain surplus capacity to the heat of necessity separately is arranged to a plurality of series.Here, series is meant: have can open and close respectively valve that cooling medium flows, can set respectively and use or the obsolete group of removing heat pipe or removing heat pipe.The heat-removal capability of removing heat pipe receives following various factors domination: with the contact area of the dense layer segment of fluid bed, with the kind physical aspect supplying temperature feed speed of the temperature of the contact area of the thin layer of fluid bed, catalyst layer, the cooling medium that fed etc.The decisions such as heat of reaction that produced should be more than the heat (necessary ability) of heat extraction as long as conventional total heat-removal capability of removing heat pipe is served as reasons; Then not special restriction is preferably more than 130% of necessary ability, more preferably more than 150% and then be preferably more than 180%.From the viewpoint that prevents that equipment is excessive, conventional total heat-removal capability of removing heat pipe is preferably below 300% of necessary ability, more preferably below 270%, further be preferably below 240%.Then regulate heat-removal capability more easily owing to trend towards increasing more conventional the serial several of heat pipe of removing, thus preferably be provided with 5 series above, more preferably 8 series above, further be preferably more than 10 series, be preferably more than 16 series especially.Can or not use through the use of suitable these a plurality of series of switching, roughly regulate total heat-removal capability and use.
Can realize the then not special restriction of necessary heat-removal capability as long as feed the conventional cooling medium that removes heat pipe, but be preferably under the operating temperature of reactor evaporated liquid, more preferably water, further be preferably the water that is forced into 0.5～5MPa (gauge pressure).Through with evaporated liquid under the operating temperature of reactor as cooling medium, therefore the heat extraction that evaporation latent heat then capable of using brings, can make this overall heat-transfer coefficient of removing heat pipe become than higher.Therefore, the heat extraction quantitative change of per unit surface area that removes heat pipe is big, can reduce the necessary radical except that heat pipe.In addition, the steam of the cooling medium of gained can be once more as the cooling medium utilization.
In addition; Cooling medium not only uses liquid, and the remove heat pipe of using gases as cooling medium preferably is set simultaneously, and then the following heat pipe that removes more preferably is set simultaneously; Promptly; Cooling medium uses liquid, and the part of the cooling medium of the evaporation gas-liquid multi-phase flow as liquid-steam is reclaimed, and the steam that produces is used as cooling medium again and reclaims the heat pipe that removes of superheated vapor.
In the operation (i), when removing the heat pipe heat extraction, detect the temperature in the fluidized-bed reactor through Temperature Detector through above-mentioned routine.When a plurality of Temperature Detector is set, can use one of them detector in reactor, also can select two above detectors and carry out the equal computing etc. of making even of a plurality of detected temperatures.
[operation (ii)]
Operation (ii) is following operation: during the temperature departure design temperature of detection; With the mean change speed more than 0.1FS/ minute; Make heat-removal capability that regulate to remove heat pipe from adjustable extent FS 10% below to change 90% or more, perhaps, from more than 90% to variation below 10%, with the operation of the temperature in the fluidized-bed reactor to the design temperature adjusting.
Here, " design temperature " is meant: in the gas phase exothermic reaction, the temperature in the such fluidized-bed reactor of the yield of suitable conversion ratio and target product is provided, can comes to set arbitrarily according to the reaction of being implemented.
Adjusting heat extraction pipe in this operation is used for regulating heat according to the temperature that detects with Temperature Detector and the difference of design temperature.Which a plurality of removing in the middle of the heat pipe, conventional actually (removing heat pipe as routine) use, which is used for regulating (removing heat pipe as regulating), and this can be predetermined, and also can wait according to the kind of gas phase exothermic reaction suitably and set.In any case, from making the temperature viewpoint of heat extraction equably in the reactor, a plurality of adjustings remove heat pipe be preferably placed at each other away from the position.
The heat-removal capability of removing heat pipe receives following various factors domination: with the contact area of the dense layer segment of fluid bed, with the kind physical aspect supplying temperature of the temperature of the contact area of the thin layer segment of fluid bed, catalyst layer, the cooling medium that fed. feed speed etc.Therefore, when regulate removing the heat-removal capability of heat pipe, through in the middle of these multiple governing factors, changing more than one of the physical quantity that can set arbitrarily, the for example supplying temperature of cooling medium, feed speed, thereby its ability of scalable.In addition, regulate to remove the use radical of heat pipe through increase and decrease, to change heat transfer area, the whole heat-removal capability of scalable as a result.
Feed to regulate remove heat pipe cooling medium if for the fluid that can realize that necessary heat-removal capability, scalable remove the then not special restriction of heat-removal capability of heat pipe, be preferably under the operating temperature of reactor, not undergoing phase transition, more preferably gas, further be preferably the gas that is forced into 0.2～5MPa (gauge pressure), be preferably the steam that is forced into 0.2～5MPa (gauge pressure) especially.The fluid that does not undergo phase transition under the operating temperature of reactor is owing to have only sensible heat to be used to heat extraction, thereby regulates the heat-removal capability of removing heat pipe and almost change pro rata with the feed speed of cooling medium and change.Therefore, can regulate heat-removal capability more easily except that heat pipe.
Remove heat that the heat pipe routine removes and remove heat pipe and regulate the heat of the heat of removing and distribute not special restriction with conventional with regulating; Design arbitrarily, setting get final product for reactor temperature is stablized; Can not bring in the dysgenic scope the control of the temperature in the reactor, expectation removes heat pipe with the conventional routine of using and removes heat as much as possible.With the conventional heat that removes the heat pipe heat extraction be preferably should heat extraction more than 80% of heat (all heat), more preferably more than 85%, further be preferably more than 90%.
The operation of this embodiment (ii) in; When the detected temperatures that detects through Temperature Detector departs from design temperature; Importantly with the mean change speed more than 0.1FS/ minute, make regulate the heat-removal capability of removing heat pipe from adjustable extent FS 10% below to variation 90% or more, perhaps, from more than 90% to variation below 10%.Promptly; Be not to control as follows, promptly the mean change speed of heat-removal capability is increased, hour mean change speed is reduced with the difference of design temperature; But when there are difference in the temperature that is detected and design temperature; All the time with the mean change speed more than 0.1FS/ minute, from adjustable extent FS below 10% to change more than 90%, perhaps, from 90% or more to variation below 10%.
Deducibility: through with the mean change speed more than 0.1FS/ minute; Make heat-removal capability that regulate to remove heat pipe from adjustable extent FS 10% below to variation 90% or more, perhaps, from more than 90% to variation below 10%; Can prevent that the further temperature that temperature rising (decline) causes from rising (decline), also can prevent dispersing of temperature; Therefore, can control the interior temperature of reactor more accurately.When the situation of temperature rising is explained as an example; Through change heat-removal capability like this; Thereby before through the chain reaction that makes reaction carry out and make temperature further rise of rising at Yin Wendu, improve heat-removal capability, easily the temperature in the reactor is remained near design temperature thus by the reaction heat that produces.Therefore, in the situation of the big reaction of the partial differential coefficient to temperature of total reaction heat and total reaction heat, especially preferably control temperature through the method for this embodiment.
In addition, also can set for use temperature that Temperature Detector detects and design temperature difference as setting change heat-removal capability when above.Certainly; Also be as long as difference is more than the setting under this situation; All the time with the mean change speed more than 0.1FS/ minute, make regulate the heat-removal capability of removing heat pipe from adjustable extent FS 10% below to variation 90% or more, perhaps, from more than 90% to variation below 10%.Setting can be the detection boundary value of Temperature Detector, also can wait according to the characteristic of gas phase exothermic reaction and set.
The control method that the heat-removal capability of regulating the heat extraction pipe is carried out ON-OFF control is described when setting is above for the difference of detected temperatures and design temperature.Setting according to after the size to the partial differential coefficient of temperature of the reaction heat stated come suitably to set to get final product, for example, under the situation of the ammoxidation reaction of propane, be preferably 0.30～2.0 ℃, under the situation of the ammoxidation reaction of propylene, be preferably 0.50～3.0 ℃.As long as detected temperatures exceeds more than the setting than design temperature; Then with the mean change speed more than 0.1FS/ minute from adjustable extent FS below 10% to changing more than 90%; As long as hang down more than the setting than design temperature, then with the mean change speed more than 0.1FS/ minute from adjustable extent FS 90% or more to variation below 10%.
Adjustable extent FS can be by whole adjustable ranges of regulating the specification of equipment decision that removes heat pipe, also can be with wherein limited scope as adjustable extent FS.That is, adjustable extent FS is not limited to represent from not using the extremely whole states that use of the state that removes heat pipe of regulating fully.Except that in the middle of the heat pipe, as long as the conventional part of using, then routine uses its a part of state to be 0FS in a plurality of adjustings.On the other hand, a part that regulate to remove heat pipe for for example non-common, promptly be not used for common temperature control, the state that then removes the ability of heat pipe except the adjusting that is not used is 1.0FS.The method of adjustable range about the restriction heat-removal capability does not have special provision; For example; When regulating heat-removal capability according to changes in flow rate; Through adjusting be arranged at stream valve, insert restricting orifice limit maximum stream flow, in control valve, be provided with suitable bypass with the restriction minimum flow, or limit the method etc. of the movable range of self-regulating control valve, thereby can the adjustable range of heat-removal capability be restricted to narrower range.
It is certain that governing speed (pace of change) that regulate to remove the heat-removal capability of heat pipe there is no need, and can change according to the response characteristic of employed operation result, system in regulating.In this embodiment, with the mean change speed more than 0.1FS/ minute, make heat-removal capability from adjustable extent FS below 10% to change more than 90%, perhaps, from 90% or more to variation below 10%.The mean change speed of heat-removal capability is more than 0.1FS/ minute, more preferably more than 0.2FS/ minute, further is preferably more than 0.25FS/ minute.The upper limit as mean change speed; Not special restriction has aspect considerations such as boundary from the stability of automatic adjusting computing, the responsiveness of control valve, is preferably below 6.0FS/ minute; More preferably below 5.0FS/ minute, further be preferably below 4.0FS/ minute.The value of employed algorithm when the mean change speed of heat-removal capability can be through regulating power, the control variables in the algorithm that adopts, used, the responsiveness of employed control valve wait and regulate.
In addition, the control that regulate to remove the heat-removal capability of heat pipe can be set at automatically to be carried out.Employed algorithm when regulating the ability of removing heat pipe automatically; As long as through selecting the scope of suitable control variables so that the mean change speed controlling of heat-removal capability is being stipulated; Then not special restriction; For example, can use ON-OFF control, PID s operation control, fuzzy operation control, neural network computing control, but the common ON-OFF of use control or PID computing are gone up in industry.For example, when using ON-OFF control, through regulating the mean change speed that the speed that drives control valve can obtain stipulating.In addition, when using the PID s operation control, according to the response characteristic of system, suitable selection percentage band (P), the time of integration (I), derivative time (D), the mean change speed that can obtain stipulating.
In addition, for the temperature control of the fluidized-bed reactor of implementing the gas phase exothermic reaction more accurately, heat that expectation stably keeps being produced as far as possible and the heat in the fluid bed move rapidly carries out.In order stably to keep producing heat, expectation is tried one's best and is remained necessarily, makes stable reaction ground to carry out reaction conditions such as the feed speed of raw material, reaction pressure.In addition, for the heat of carrying out in the fluid bed rapidly moves, be necessary to keep well the flow regime of fluid bed.Known, the flow regime of fluid bed receives the dominations such as particle diameter of gas flow rate (superficial linear velocity in a column), catalyst usually.For gas flow rate, so long as can keep the then not special restriction of scope of the flow regime of fluid bed well.In addition, but catalyst if for the employed catalyst of fluidized-bed reactor then former state use, but weight average particle diameter is preferably 20～100 μ m, more preferably 30～80 μ m further are preferably 40～60 μ m.In addition, the content of the micropowder (so-called good component) below the particle diameter 44 μ m is preferably 10～70 weight %, further in Geldart powder category map, is categorized as the A particle.
As the gas phase exothermic reaction in this embodiment; Not special the qualification; For example can enumerate; With propane and/or propylene as raw material make acrylonitrile the gas phase ammonoxidation reaction, be selected from the group that normal butane, 1-butylene, 2-butylene, butadiene, benzene formed more than a kind as raw material make maleic anhydride gas phase oxidation, with isobutene and/or iso-butane as raw material make methacrylonitrile the gas phase ammonoxidation reaction, with ortho-xylene and/or naphthalene as raw material make phthalic anhydride gas phase oxidation, make 2 with phenol and methyl alcohol as raw material, the vapor phase alkylation of 6-xylenols and/or orthoresol, make the gas phase ammonoxidation reaction of hydrogen cyanide (HCN) etc. as raw material with methane and/or methyl alcohol.
The reaction heat of gas phase exothermic reaction is different because of reaction, and the reaction heat that for example generates the reaction of acrylonitrile by propylene and ammonia is 520kJ/mol (propylene), be 637kJ/mol (propane) by the reaction heat of the reaction of propane and ammonia generation acrylonitrile.But actual reaction is concurrent, successive reaction, produces CO
2, CO, other accessory substance.Connect side reaction and be also included within interior total reaction heat, can consider that the contribution rate (yield of each product) of the reaction that each is concurrent is tried to achieve.
For example, the propane burning generates CO
2With water, or the reaction heat that generates the reaction of CO and water be do for oneself 2043kJ/mol (propane) and 1194kJ/mol (propane) of every 1mol propane; Therefore; When under certain condition, making 100mol propane and ammonia and oxygen reaction; The propane reaction (reactivity 80%) of 80mol generates the acrylonitrile (yield 50%) of 50mol, the CO of 60mol
2During the CO of (yield 20%), 30mol (yield 10%), the total reaction heat under this condition can be tried to achieve through 637 * 0.5+2043 * 0.2+1194 * 0.1=846.5 (kJ/mol).Can know from computational process,, thereby depend on reaction condition owing to total reaction heat changes because of the reactivity of raw material, the contribution rate of each concurrent reaction (distribution of product) etc.The not special restriction of total reaction heat; If excessive, then, make control become difficulty because heat that should heat extraction increases; Become the reason of the Temperature Distribution in the reactor and then also can cause the thermal runaway of reactor in opposite extreme situations; Therefore, when the choice reaction condition, total reaction heat is reduced as far as possible.Specifically, can the choice reaction condition, the raw material that makes every 1mol supply be preferably 50～2500kJ/mol (raw material), more preferably 70～2000kJ/mol (raw material), further be preferably 100～1500kJ/mol (raw material).
On the other hand, so not big as the stability of the product of target in the gas phase exothermic reaction, therefore, follow reaction carrying out, be the rising of reaction conversion ratio, carry out the successive reaction of target product, the selection rate of target product trends towards reducing.Conversion ratio also rose when here, reaction conversion ratio depended on activity of such catalysts and active the rising.In addition, activity of such catalysts depend on reaction temperature and when usually reaction temperature rises activity also rise, therefore, if reaction temperature is former thereby when rising because of some, reacting dose increases and successive reaction is carried out, and therefore increases as overall reaction heat.
For example, from the preceding paragraph condition, have only temperature to rise 5 ℃ and when not changing other condition fully, in the middle of the 100mol propane of supply, the propane of 82.5mol reaction (reactivity 82.5%) generates the acrylonitrile (yield 50.3%) of 50.3mol, the CO of 64.5mol
2The CO of (yield 21.5%), 32.1mol (yield 10.7%), when so changing, the total reaction heat under this condition is 637 * 0.503+2043 * 0.215+1194 * 0.107=887.4 (kJ/mol).The rate of change of total reaction heat can represent that do near linear this moment around this temperature, thereby try to achieve with (887.4-846.5) ÷ 5=8.2 (kJ/molK) through the partial differential coefficient to temperature of total reaction heat.As judging from computational process, the partial differential coefficient to temperature of total reaction heat changes because of the reactivity of reaction temperature, raw material, the contribution rate of each concurrent reaction (yield of each product) etc., thereby depends on reaction condition.When the rate of change of total reaction heat is excessive; On the thermal balance, it is unstable that the control of reaction temperature becomes, and causes the reason of the Temperature Distribution in the reactor and then under opposite extreme situations, also can cause the thermal runaway of reactor; Therefore; From this aspect, during the choice reaction condition, the rate of change of total reaction heat is reduced as far as possible.Specifically, can the choice reaction condition, make that the partial differential coefficient to temperature of total reaction heat is 0.2～40kJ/mol (raw material) K, be preferably 0.5～30kJ/mol (raw material) K, further be preferably 1～10kJ/mol (raw material) K.
[manufacturing approach of target compound]
In addition; The manufacturing approach of the target compound of this embodiment has the conventional manufacturing approach of removing heat pipe, regulating the target compound of the fluidized-bed reactor that removes heat pipe and Temperature Detector for using; This method comprises: (a) base feed in the aforementioned fluidized-bed reactor that is filled with catalyst; Implement the operation of gas phase exothermic reaction, when (b) removes the heat pipe heat extraction through aforementioned routine, detect the operation of the temperature in the aforementioned fluidized-bed reactor through the aforementioned temperature detector; During the temperature departure design temperature that (c) detects; With the mean change speed more than 0.1FS/ minute; Make heat-removal capability that aforementioned adjusting removes heat pipe from adjustable extent FS 10% below to change 90% or more, perhaps, from more than 90% to variation below 10%, with the operation of the temperature in the aforementioned fluidized-bed reactor to the design temperature adjusting.
Operation (a) is base feed in the fluidized-bed reactor that is filled with catalyst, implements the operation of gas phase exothermic reaction.Here,, can enumerate and the identical reaction of above-mentioned gas phase exothermic reaction as the gas phase exothermic reaction, as its raw material, can enumerate with as the raw material of this gas phase exothermic reaction the identical raw material of illustrative raw material.In addition, as catalyst, not special restriction can be enumerated normally used catalyst in the gas phase exothermic reaction such as composite oxide catalysts.
In addition, when operation (b) is removed the heat pipe heat extraction for passing through routine, detect the operation of the temperature in the fluidized-bed reactor through Temperature Detector; Operation (c) is when the temperature departure design temperature that detects; With the mean change speed more than 0.1FS/ minute; Make heat-removal capability that regulate to remove heat pipe from adjustable extent FS 10% below to change 90% or more, perhaps, from more than 90% to variation below 10%, with the operation of the temperature in the fluidized-bed reactor to the design temperature adjusting.Here, operation (b) and operation (c) are (ii) corresponding respectively with the operation (i) and the operation of front narration respectively, carry out through using the same method, but the manufacturing objective compound.As target compound, can enumerate with as the product of above-mentioned gas phase exothermic reaction the identical compound of illustrative compound.
Fig. 1 representes an example of the fluidized-bed reactor in this embodiment.Reactor (1) inside is formed with the fluid bed (2) that is formed by catalyst.When using fluidized-bed reactor oxidation raw material, comprise the gas (being generally air) of oxygen, supply with the gas that comprises raw material from raw material supplying pipe (4) from airway (3) supply of being located at reactor lower part.The gas that comprises product is extracted to outside the reactor (1) through extracting pipe (5) out.
Be arranged in the cooling medium that removes the heat pipe feed fluid of fluid bed (2) or the cooling medium of gas.The heat pipe that removes of the cooling medium of feed fluid is used, on the other hand, the cooling medium of supply gas remove the pipe that heat pipe has the pipe that is used by routine and is conditioned usefulness.Below, liquid is used for cooling medium and is called and conventionally removes heat pipe (6), gas is used for cooling medium and is called and conventionally removes heat pipe (7), the heat pipe that removes of remainder is called to regulate and removes heat pipe (8) by the conventional heat pipe that removes that uses by the conventional heat pipe that removes that uses.In addition, each only shows each 1 series except that heat pipe among Fig. 1, but usually a plurality of series separately is set.
Remove heat pipe (6) supply cooling medium from gas-liquid separation container (9) to the routine of using liquid through pump (10).The part of cooling medium is evaporated through fluid bed (2) and the conventional heat exchange that removes heat pipe (6), and turns back in the gas-liquid separation container (9) with gas-liquid two-phase flow, and gas-liquid is separated.The cooling medium of liquid appends pipe (11) by additional services through the part that evaporation reduces through cooling medium.
A conventional part of removing the cooling medium steam that produces in the heat pipe (6) is fed into conventional removing in the heat pipe (7).The cooling medium steam becomes superheated vapor through fluid bed (2) and the conventional heat exchange that removes heat pipe (7), extracts pipe (12) out through superheated vapor and is fed into outside the system.
Conventional other part of removing the cooling medium steam that produces in the heat pipe (6) is fed into to regulate and removes in the heat pipe (8).The flow that is supplied to can pass through the meticulous control of flow control valve (13).The cooling medium steam becomes superheated vapor through fluid bed (2) and the heat exchange of regulating except that heat pipe (8), extracts pipe (14) out through superheated vapor and is fed into outside the system.
In addition, in fluid bed (2), be provided with Temperature Detector (15).Only show a detector among Fig. 1, but along continuous straight runs, vertical direction change position are waited a plurality of test sections are set usually.The temperature information that detects with Temperature Detector (15) is communicated to attemperator (16), and is to be detected as the temperature of fluid bed.When a plurality of detector is set, after the suitable computing of selecting suitable detector to average etc., use as the temperature of fluid bed.
In the accommodometer (16); The computing of stipulating based on the difference of the temperature of the fluid bed of such detection and design temperature; Based on the flow control valve (13) of operation result operation cooling medium, regulate feeding the flow of regulating the cooling medium that removes heat pipe (8), thereby regulate the ability of removing heat pipe (8).
Conventional removing in the middle of the cooling medium steam that produces in the heat pipe (6) removed heat pipe (7) and regulated the remainder that except that heat pipe (8) in, there is not use and manage (17) through the saturated vapor extraction and be fed into the system in routine.
Embodiment
Below, use embodiment that the present invention is more specified, but the present invention is not limited to following embodiment.
[embodiment 1]
In fluidized-bed reactor form as shown in Figure 1, diameter 6.82m (1), fill 80 tons of composite oxide catalysts, wherein, this catalyst is made up of molybdenum, vanadium, antimony, niobium, and average grain diameter is 50 μ m, contain 12% particle diameter is the following micropowders of 44 μ m.From oxygen supply pipe (3) air supply 45000Nm
3/ Hr supplies with mixing propane 3000Nm from raw material supplying pipe (4)
3/ Hr and ammonia 2700Nm
3The gas of/Hr is mainly made acrylonitrile.
Conventional heat pipe (6) 30 series (straight sections add up to 1250m) of removing are set in the fluid bed (2), and this pipe uses 180 ° of long radius bend pipes of butt welding formula of the corresponding diameter that steel pipe and the JIS B-2311 of the external diameter 114.3mm of JIS G-3458 regulation stipulate to make.Supply with 235 ℃ 800 tons/Hr of water from gas-liquid separation container (9) the heat pipe (6) to these conventional removing, and its part is evaporated, flow back to receipts mutually with the gas-liquid 2 of 236 ℃ of temperature, pressure 3MPa (gauge pressure).Evaporation rate under the normal condition is 5.8%.
In addition, be provided with to use and remove routine that heat pipe (6) identical materials makes and remove heat pipe (7) 8 series (straight sections add up to 225m) with conventional.Supply with 236 ℃ of the temperature of from the gas-liquid two-phase flow of routine, separating with gas-liquid separation container (9), the 17 tons/Hr of saturated steam of pressure 3MPa (gauge pressure), the superheated vapor that recovered temperature is 370～372 ℃ in the heat pipe (7) to these conventional removing except that generation the heat pipe (6).
And then, be provided with to use and remove adjusting that heat pipe (6) identical materials makes and remove heat pipe (8) 12 series (straight sections add up to 370m) with conventional.Flow control valve (13) through regulating flow removes the temperature 236 ℃ in the gas-liquid two-phase flow that heat pipe (6) produce separated, the saturated steam of pressure 3MPa (gauge pressure) except that supplying with gas-liquid separation container (9) in the heat pipe (8) from routine to these adjustings, reclaims 370～438 ℃ superheated vapor.
Central part at fluid bed is provided with K type thermocouple as Temperature Detector (15), with attemperator (16) thermo-electromotive force is transformed to temperature signal and detects.In the attemperator (16); Poor based on the temperature of the reactor that detects and design temperature uses the DCS device CS3000 of Yokogawa electronics (strain) manufacturing to carry out the sequence computing, corresponding to this result; Flow control valve (13) is carried out opening and closing operations, regulate the ability of removing heat pipe (8).
At first; The design temperature that will offer attemperator (16) is made as 445.0 ℃, setting is made as ± 0.3 ℃ (444.7 ℃, 445.3 ℃ of control temperature); The set speed regulator of drive air (instrument air) pipe arrangement to the drive unit that offers control valve is regulated; Set control valve; So that with 3.0FS/ minute mean change speed, make heat-removal capability that regulate to remove heat pipe (8) from adjustable extent FS 100% to 0% changing, perhaps, change from 0% to 100%, control running automatically.At this moment, the mobility scale of temperature of reactor is 444.5～445.5 ℃, can control automatically in respect to the scope of design temperature ± 0.5 ℃.
[embodiment 2]
Among the embodiment 1; Do not change design temperature and setting, set control valve, so that with 0.2FS/ minute mean change speed; Make heat-removal capability that regulate to remove heat pipe (8) from adjustable extent FS 100% to 0% changing, perhaps, change from 0% to 100%, control running automatically.At this moment, the mobility scale of temperature of reactor is 444～446 ℃, can control automatically in respect to the scope of design temperature ± 1 ℃.
In the present embodiment, the thermocouple that the K type is set at the central part of fluid bed is transformed to temperature signal with attemperator (16) with thermo-electromotive force and detects as Temperature Detector (15).In the attemperator (16); Poor based on the temperature of the reactor that detects and design temperature; The DCS device CS3000 that uses Yokogawa electronics (strain) to make carries out the PID computing, corresponding to the aperture that this result regulates flow control valve (13), regulates the ability of removing heat pipe (8).
[embodiment 3]
Carry out the PID computing through the DCS device; Set control variables (P: proportional band, I: the time of integration, D: derivative time); So that with 3.0FS/ minute mean change speed, make except that the heat-removal capability of heat pipe (8) from adjustable extent FS 100% to 0% changing, perhaps, change from 0% to 100%, control running automatically; In addition, likewise carry out the ammoxidation reaction of propane with embodiment 1.At this moment, the mobility scale of temperature of reactor is 444.5～445.5 ℃, can control automatically in respect to the scope of design temperature ± 0.5 ℃.
[embodiment 4]
Set control variables; So that mean change speed with 0.2FS/ minute; Make heat-removal capability that regulate to remove heat pipe (8) from adjustable extent FS 100% to 0% changing, perhaps, change from 0% to 100%; In addition, likewise control running automatically, carry out the ammoxidation reaction of propane with embodiment 3.At this moment, the mobility scale of temperature of reactor is 444～446 ℃, can be in the scope inner control with respect to design temperature ± 1 ℃.
[embodiment 5]
With the same fluidized-bed reactor of embodiment 1 in fill 105 tons of composite oxide catalysts, wherein, this catalyst end is made up of vanadium, phosphorus, average grain diameter is 60 μ m, contain 40% particle diameter is the following micropowders of 44 μ m.From oxygen supply pipe (3) air supply 70000Nm
3/ Hr, supply with normal butane 2950Nm from raw material supplying pipe (4)
3/ Hr mainly makes maleic anhydride.
The design temperature that will offer attemperator (16) is made as 452.5 ℃, setting is made as ± 0.2 ℃ (452.3 ℃, 452.7 ℃ of control temperature); The set speed regulator of drive air (instrument air) pipe arrangement to the drive unit that offers control valve is regulated; Set control valve; So that with 3.0FS/ minute mean change speed, make heat-removal capability that regulate to remove heat pipe from adjustable extent FS 100% to 0% changing, perhaps, change from 0% to 100%, control running automatically.At this moment, the mobility scale of temperature of reactor is 452.1～452.9 ℃, can control automatically in respect to the scope of design temperature ± 0.4 ℃.
[embodiment 6]
With the same fluidized-bed reactor of embodiment 1 in fill 300 tons of composite oxide catalysts, wherein, this catalyst is made up of iron, vanadium, average grain diameter is 50 μ m, contain 40% particle diameter is the following micropowders of 44 μ m.Supply with the mist 50000Nm of methyl alcohol, phenol from raw material supplying pipe (4)
3/ Hr mainly makes orthoresol, 2, the 6-xylenols.
The design temperature that will offer attemperator (16) is made as 333.0 ℃, setting is made as ± 0.2 ℃ (332.8 ℃, 333.2 ℃ of control temperature); The set speed regulator of drive air (instrument air) pipe arrangement to the drive unit that offers control valve is regulated; Set control valve; So that with 3.0FS/ minute mean change speed, make heat-removal capability that regulate to remove heat pipe from adjustable extent FS 100% to 0% changing, perhaps, change from 0% to 100%, control running automatically.At this moment, the mobility scale of temperature of reactor is 332.6～333.4 ℃, can control automatically in respect to the scope of design temperature ± 0.4 ℃.
[comparative example 1]
(1) reaction example 1
Among the embodiment 1; Do not change design temperature, set control valve, so that with 0.05FS/ minute mean change speed; Make heat-removal capability that regulate to remove heat pipe (8) from regulate possible range FS 100% to 0% changing, perhaps, change from 0% to 100%, control running automatically.At this moment, temperature of reactor continues to rise, disperse, can't A.T.C.
(2) reaction example 2
Under the condition identical with reaction example 1, implement the gas phase exothermic reaction, temperature of reactor continues to descend, disperse, can't A.T.C.
As react shown in the example 1 and 2, repeatedly implement the ammoxidation reaction of propane under the same conditions, the temperature in the fluid bed is dispersed to any direction that rises or descend, and all can not control temperature at every turn.
[comparative example 2]
(1) reaction example 1
Do not change design temperature; Set the speed regulator of control valve; So that mean change speed with 0.05FS/ minute; Make heat-removal capability that regulate to remove heat pipe (8) from adjustable extent FS 100% to 0% changing, perhaps, change from 0% to 100%, in addition, with the embodiment 5 same maleic anhydrides of making.At this moment, temperature of reactor continues to rise, disperse, can't A.T.C.
(2) reaction example 2
Under the condition identical with reaction example 1, implement the gas phase exothermic reaction, temperature of reactor continues to descend, disperse, can't A.T.C.
As react shown in the example 1 and 2, repeatedly implement the oxidation reaction of normal butane under the same conditions, the temperature in the fluid bed is dispersed along any direction that rises or descend, and all can not control temperature at every turn.
[comparative example 3]
(1) reaction example 1
Among the embodiment 6; Do not change design temperature, set the speed regulator of control valve, so that with 0.05FS/ minute mean change speed; Make heat-removal capability that regulate to remove heat pipe (8) from adjustable extent FS 100% to 0% changing, perhaps, change from 0% to 100%, control running automatically.At this moment, temperature of reactor continues to rise, disperse, can't A.T.C.
(2) reaction example 2
Under the condition identical with reaction example 1, implement the gas phase exothermic reaction, temperature of reactor continues to descend, disperse, can't A.T.C.
As react shown in the example 1 and 2, repeatedly implement the alkylated reaction of phenol under the same conditions, the temperature in the fluid bed is dispersed to any direction that rises or descend, and all can not control temperature at every turn.
Can know that from above result use in the gas phase exothermic reaction of embodiment 1～6 of temperature-controlled process of this embodiment, the temperature in the reactor rises or descends and all do not disperse, and can accurately be controlled at certain certain scope.
Relative therewith; The gas phase exothermic reaction of comparative example 1～3 is owing to the mean change speed of regulating the heat-removal capability of removing heat pipe is not more than 0.1FS/ minute; Thereby follow the carrying out of reaction, the temperature in the reactor to rise or descend and all disperse, the temperature control difficulty in the reactor.
Utilizability in the industry
According to the present invention; Can accurately control the temperature of fluidized-bed reactor; This fluidized-bed reactor is widely used when in industry, making the useful monomer of the manufacturing of various synthetic resin synthetic fibers, in the temperature province of catalyst for the highest yield, can turn round steadily in the long term.
Claims (10)
1. temperature-controlled process, its for use have conventionally remove heat pipe, temperature-controlled process when regulating the fluidized-bed reactor that removes heat pipe and Temperature Detector and implementing the gas phase exothermic reaction, this method comprises:
When (i) removing the heat pipe heat extraction, detect the operation of the temperature in the aforementioned fluidized-bed reactor through the aforementioned temperature detector through aforementioned routine;
During the temperature departure design temperature that (ii) detects; With the mean change speed more than 0.1FS/ minute; Make heat-removal capability that aforementioned adjusting removes heat pipe from adjustable extent FS 10% below to change 90% or more, perhaps, from more than 90% to variation below 10%, with the operation of the temperature in the aforementioned fluidized-bed reactor to the design temperature adjusting.
2. method according to claim 1, in the temperature range of implementing aforementioned gas phase exothermic reaction, the total reaction heat of raw material is 50～2500kJ/mol, and the partial differential coefficient to temperature of the total reaction heat of aforementioned base materials is 0.2～40kJ/molK.
3. method according to claim 1 and 2, aforementioned gas phase exothermic reaction is for being the gas phase ammonoxidation reaction of raw material with propane and/or propylene, the product of reaction is an acrylonitrile.
4. method according to claim 1 and 2, aforementioned gas phase exothermic reaction is in the group that normal butane, 1-butylene, 2-butylene, butadiene, benzene formed being the gas phase oxidation of raw material to be selected from more than a kind, the product of reaction is a maleic anhydride.
5. method according to claim 1 and 2, aforementioned gas phase exothermic reaction is for being the gas phase ammonoxidation reaction of raw material with isobutene and/or iso-butane, the product of reaction is a methacrylonitrile.
6. method according to claim 1 and 2, aforementioned gas phase exothermic reaction is for being the gas phase oxidation of raw material with ortho-xylene and/or naphthalene, the product of reaction is a phthalic anhydride.
7. method according to claim 1 and 2, aforementioned gas phase exothermic reaction is for being the vapor phase alkylation of raw material with phenol and methyl alcohol, the product of reaction is 2,6-xylenols and/or orthoresol.
8. method according to claim 1 and 2, aforementioned gas phase exothermic reaction is for being the gas phase ammonoxidation reaction of raw material with methane and/or methyl alcohol, the product of reaction is hydrogen cyanide (HCN).
9. method according to claim 1 and 2, aforementioned gas phase exothermic reaction is in the group that ethane, ethene, ethanol formed being the gas phase ammonoxidation reaction of raw material to be selected from more than a kind, the product of reaction is an acetonitrile.
10. manufacturing approach, it has the conventional manufacturing approach of removing heat pipe, regulating the target compound of the fluidized-bed reactor that removes heat pipe and Temperature Detector for using, and this manufacturing approach comprises:
(a) base feed in the aforementioned fluidized-bed reactor that is filled with catalyst, the operation of enforcement gas phase exothermic reaction;
When (b) removing the heat pipe heat extraction, detect the operation of the temperature in the aforementioned fluidized-bed reactor through the aforementioned temperature detector through aforementioned routine;
During the temperature departure design temperature that (c) detects; With the mean change speed more than 0.1FS/ minute; Make heat-removal capability that aforementioned adjusting removes heat pipe from adjustable extent F S 10% below to change 90% or more, perhaps, from more than 90% to variation below 10%, with the operation of the temperature in the aforementioned fluidized-bed reactor to the design temperature adjusting.
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| CN105388939B (en) * | 2015-12-18 | 2017-12-08 | 重庆科技学院 | The temprature control method and system of pharmacy fluid bed |
| CN107765730A (en) * | 2016-08-18 | 2018-03-06 | 蓝星（北京）技术中心有限公司 | A kind of fluidized-bed temperature control method and control device |
| CN110045764B (en) * | 2019-04-10 | 2021-04-20 | 万华化学集团股份有限公司 | Reactor temperature automatic control method based on feedforward-reaction mechanism model |
| KR20230165912A (en) * | 2021-04-09 | 2023-12-05 | 차이나 페트로리움 앤드 케미컬 코포레이션 | Heat removal tube set, method for controlling reaction temperature, and method for producing unsaturated nitrile |
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| JP2001294859A (en) * | 2000-04-13 | 2001-10-23 | Kawasaki Heavy Ind Ltd | Method for producing ground improving material and apparatus therefor |
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| JP2001294859A (en) * | 2000-04-13 | 2001-10-23 | Kawasaki Heavy Ind Ltd | Method for producing ground improving material and apparatus therefor |
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Effective date of registration: 20160511 Address after: Tokyo, Japan, Japan Patentee after: Asahi Kasei Kogyo K. K. Address before: Tokyo, Japan, Japan Patentee before: Asahi Kasei Chemical K. K. |