CN1207255C - Fixed bed dehydrogenation reactor - Google Patents
Fixed bed dehydrogenation reactor Download PDFInfo
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- CN1207255C CN1207255C CN 02111315 CN02111315A CN1207255C CN 1207255 C CN1207255 C CN 1207255C CN 02111315 CN02111315 CN 02111315 CN 02111315 A CN02111315 A CN 02111315A CN 1207255 C CN1207255 C CN 1207255C
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Abstract
The present invention relates to a fixed bed catalytic dehydrogenation reactor which mainly solves the problem which exists in former literatures that catalyst bed layer temperature changes too much in a reaction medium flow direcrion in a heat insulation bed reactor to influence the performance of catalysts, reaction conversion rates and reaction yields. The fixed bed catalytic dehydrogenation reactor better solves the problem by adopting the technical scheme that at least one reheater is arranged in a reactor bed layer, and the fixed bed catalytic dehydrogenation reactor can be used in an industrial device for preparing styrene from ethylbenzene dehydrogenation.
Description
Technical field
The present invention relates to a kind of fixed bed dehydrogenation reactor, particularly about being used for the dehydrogenation reactor of ethyl benzene dehydrogenation preparation of styrene.
Background technology
Vinylbenzene is widely used as production various kinds of resin, plastics and elastomeric raw material, extensively mainly being easy to polymerization (for example generating polystyrene) owing to vinylbenzene or carrying out the adaptability of copolymerization (for example producing rubber with butadiene copolymer) of its range of application.
Cinnamic production with regard to various catalyzer used in dehydrogenating technology and this technology, is all known.Main goal in research is to improve the benefit of this technology at present.Be known that the dehydrogenating technology method of ethylbenzene especially, wherein dehydrogenation a cover comprise two placed in-line dehydrogenation reactors at least and place between the reactor, reaction effluent and vapor generation heat exchange therein and heated heating unit carries out.According to this technology, steam at first is used for the reacting by heating effluent, mixes with ethylbenzene in the ingress of first reactor then.The operational condition that this technology adopted is that the same 1 mole of ethylbenzene of 3 to 10 moles steam is mixed, and the ingress temperature and pressure of first reactor is respectively 550～680 ℃ and 0.04～0.1MPa (absolute pressure).The temperature and pressure condition at other reactor inlet place is respectively 550～680 ℃ and 0.02～0.08MPa (absolute pressure), and total air speed of ethylbenzene is equal to or greater than 0.15 hour
-1Total air speed of ethylbenzene is meant the ratio of the volumetric flow rate of ethylbenzene with the cumulative volume of catalyzer.By this technology, conversion of ethylbenzene is approximately greater than 65～75%, even higher, and reaches the mole selectivity greater than 94%.But after for some time, the carrying out of this technology can cause the reduction of selectivity of styrene and conversion of ethylbenzene, but this reduction can be limited through improving temperature of reaction.In fact, it is aging gradually to observe catalyzer after for some time, occurs carbon laydown on catalyzer.This is because the focus that exists along production line (especially in middle heating unit) causes thermal degradation reaction, can produce heavy compounds.It is calculated that the ratio of formed heavy product is about 17000PPm in effusive hydrocarbon polymer per ton, even more.As a result, cause that thus loss of material increases, catalyst efficiency reduces, thereby need clean continually.In order to eliminate the shortcoming of this technology, a kind of process for manufacturing styrene is disclosed among the document CN1006061B.Or rather, it is a kind of processing method through producing phenyl ethylene by ethyl benzene catalytic dehydrogenation.By this method, dehydrogenation comprises in three placed in-line fixed bed dehydrogenation reactors at a cover carries out, and settles one or more heating units between reactor.In well heater, reaction effluent and vapor generation heat exchange and be heated, steam is used for the reacting by heating effluent in the fs, mixes with ethylbenzene in the first dehydrogenation reactor ingress in subordinate phase.According to this invention, this processing method is characterised in that:
Ethylbenzene with steam with steam: ethylbenzene is that the molar ratio between 5: 1 and 13: 1 mixes, in the ingress of above-mentioned each reactor with the temperature of mixture heating up to 580 between to 645 ℃.Mean pressure in first reactor is with absolute manometer, and between 0.06～0.1MPa, in the second and the 3rd reactor, pressure remains between 0.04～0.07MPa with absolute manometer, and the total air speed of the liquid ethylbenzene of Cai Yonging was at 0.20 and 0.35 hour simultaneously
-1Between.
This processing method thinks that the various radial reactors of type are preferable described in the employing French Patent FR2365370.Because there is bad adaptability in the radial mode reactor, the easy big area of catalyzer is poisoned, and catalyst life is vulnerable to influence.Simultaneously since catalyst basket generally up to 10 meters, the fluid distribution technical requirements is very high, the outer gap that distributes between tube and the cylindrical shell is difficult to reach design requirements when installing, and promotes the use of and can cause difficulty.In order to solve the defective that the radial reactor reaction process exists, a kind of diameter of axle is disclosed among the document CN86200368U to cold-tube type ammonia synthesis converter catalyst basket, it is that beds is divided into axial direction part and radial section, wherein axial direction part be positioned at radial section above, the top cover that is about to reaction bed is opened or perforate.This reactor process, because an axial direction part is arranged at reactor catalyst bed top, so that when the obnoxious flavour composition is higher, can play a filteration, can avoid the catalyzer big area to poison, it is big to have kept radial reactor throughput simultaneously, the advantage that net value is high.Increase the molecule thermo-negative reaction owing to ethyl benzene dehydrogenation preparation of styrene is one, wish that therefore the beds pressure drop is wanted little and condition of negative pressure is operated down, make reaction carry out and to improve throughput towards purpose product vinylbenzene direction.The characteristics of this reaction wish that more reaction medium streamwise temperature variation is not excessive in the beds on the other hand, the performance of catalyzer can be not fully exerted, improve reaction conversion ratio and reaction yield simultaneously, how not keep changing problem of smaller but above-mentioned document relates to temperature of reaction.
A kind of catalyticreactor of two-stage dehydrogenation reaction has been described in the document U.S. Pat 3918918.This reactor has the catalytic bed of an integral body, by the sealed structure in the catalytic bed catalytic bed is divided into two sections, and this reactor has also comprised an inlet feed mixing tank and an intersegmental reheater.This reactor has characteristics such as thermal expansion reasonable in design, pressure drop are little, but owing to adopt the two-stage adiabatic reaction, has limited the further raising of catalyst reaction performance.
A kind of novel radial reactor that is used for ethyl benzene dehydrogenation preparation of styrene has been described in document European patent EP 0724906A1 and the U.S. Pat 5358698.Be provided with specific plate washer and reduce the ununiformity that reactant flow circumferentially distributes in this Reactor inlet pipe, the center director by optimization design obtains uniform reactor bed flow velocity, thereby optimizes reactivity worth.But still adopt the adiabatic catalytic bed, make reaction effect further improve and be restricted.
Draw after deliberation, in adiabatic heat absorption type reaction process, influence reaction conversion ratio and optionally principal element be temperature.Certainly pressure also has material impact to reaction conversion ratio and selectivity, but in negative dehydrogenation technology commonly used, the variable range of pressure is very little, the restriction of the pressure of machine suction port and system pressure drop by compression, and general reactor exit absolute pressure is 40kPa.0.35～0.5 meter of the liquid air of Ethylbenzene Dehydrogenation Reactor design at present speed
3Ethylbenzene/rice
3Catalyzer. hour condition under, the reactor outlet material composition also has certain distance from the molecular balance composition, limited reactions further carries out and the reason that continues to improve transformation efficiency is that thermo-negative reaction makes temperature of reaction fall too lowly, and make speed of reaction slow excessively, thereby make reaction " being freezed ".
Summary of the invention
Technical problem to be solved by this invention is to overcome in the past that ethylbenzene dehydrogenation reaction adopts the adiabatic reactor reactor in the document, reaction bed temperature is excessive along reaction medium flow direction temperature variation, influence the problem of catalyst performance performance and reaction conversion ratio and reaction yield, a kind of new fixed bed dehydrogenation reactor is provided.This reactor has reaction bed temperature than homogeneous, and can better eliminate the characteristics of catalyzer local bed high-temperature zone and raising reaction conversion ratio and yield.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of fixed bed dehydrogenation reactor, comprise a housing that can bear pressure, feed-pipe, discharge nozzle, inside distributor, outer tube and first base plate of distributing, its middle shell is by cylindrical tube, upper cover and lower cover are formed, inside distributor and the outer tube that distributes are coaxial and form a catalyst basket with cylindrical tube, inside distributor and the outer tube that distributes have aperture in the catalyst basket corresponding section, first base plate links to each other with the outer bottom that distributes tube with inside distributor respectively, inside distributor is connected with the feed-pipe that gos deep into upper cover, leaving the space between outer distribute tube and the cylindrical tube is connected with the discharging mouth of pipe, wherein reactor also comprises at least one thermal barrier import, at least one heating medium outlet, second base plate and at least one reheater under first base plate, form first enclosed chamber between first base plate and second base plate, form second enclosed chamber between second base plate and the lower cover, two ports of reheater are connected with first enclosed chamber and second enclosed chamber respectively, and go deep into whole catalyst basket, thermal barrier import and heating medium outlet respectively with first enclosed chamber and second enclosed chamber in one be connected, reheater is made up of 2～100 heating tubes, on the same radial section of catalyst basket, be evenly distributed, and coaxial with cylindrical tube.
In the technique scheme, a upper cover being arranged on the reactor catalysis bed or do not have upper cover is the various ways such as upper cover that aperture was opened wide or had at the catalytic bed top fully.If the reactor catalysis bed has upper cover, upper cover links to each other with the outer top that distributes tube with inside distributor respectively, to form radial flow.If reactor does not have upper cover or upper cover has many apertures, and the inseparable aperture of corresponding axial direction part portion of the inside and outside tube that distributes, the length of aperture area is not unequal, distributes that aperture area length is not bigger for tube outward usually, to form the diameter of axle to flowing.If the upper cover perforate, then the size of aperture is not blown to good with the catalyzer in the catalyst basket.The preferable range of thermal barrier import volume is 1, and the preferable range of heating medium outlet quantity is 1.The preferable range of heating tube quantity is 10～40, heating tube pattern preferred version is that inverted-loop tube is or/and two sleeve pipe, heating tube pattern more preferably scheme is that inverted-loop tube is or/and two sleeve pipe, and the outer porous material aerial construction that adopts of its pipe, porous material is selected from wire cloth, porous plate or Johnson's net.
When the present invention adopted the upper cover of not perforate, reactor was a radial reactor.When removing upper cover or upper cover and have many apertures, reactor is an axial-radial flow reactor, more helps making full use of of catalyzer in the beds, is beneficial to improve reactor throughput.Reheater is set in catalyst basket, makes reheater carry out heat exchange, help reacting the reaction mass raising temperature of back cooling, reach the purpose that helps reacting with reactor catalysis bed reactant flow.Heating tube is evenly distributed on the same radial section of catalyst basket, and coaxial with cylindrical tube, make whole beds reach the temperature homogeneous as much as possible.Heating tube is designed to inverted-loop tube or/and two sleeve pipe, makes in the catalyst bed reaction medium and heating tube carry out cross-flow and conduct heat, reach higher heat-transfer effect.The upcast of inverted-loop tube and the fluid temperature (F.T.) of downtake compensate mutually, make that vertically heat exchange effect everywhere is consistent to a great extent, thereby guarantee distribute vertically homogeneity of catalytic bed temperature; In two sleeve pipes, the heat hot carrier at first enters two telescopic pipe cores, and this moment elevated temperature heat carrier and heat exchange of low temperature thermal barrier enters annular space then to keep its thermal barrier temperature, reaches the purpose of heating bed.Because the low temperature thermal barrier complementary heat-exchanging of two sleeve pipe pipe core higher temperature carriers and annular space, thereby can guarantee the homogeneity that the catalytic bed axial temperature distributes; Or/and the built on stilts members of porous material such as two telescopic periphery kalamein silk screen, porous plate or Johnson's net are isolated the heating tube and the catalyzer of high wall temperature, avoided the directly heating tube of the high wall temperature of contact of catalyzer at inverted-loop tube.Though the catalytic amount of heating tube periphery is few, account for 5/10000ths of total amount, can avoid the too high caused side reaction of local temperature thus.Adopt technical scheme of the present invention to be used for ethylbenzene dehydrogenation reaction and compare homogeneous through the evidence reaction bed temperature, can be near waiting hotbed.Use same catalyzer, reaction conversion ratio of the present invention is the highest to be improved approximately 7.6%, and it is nearly 6.7% that purpose product vinylbenzene yield can improve, and obtained better technical effect.
Description of drawings
Fig. 1 is a radial fixed-bed dehydrogenation reactor synoptic diagram of the present invention.
Fig. 2 is that the diameter of axle of the present invention is to the fixed bed dehydrogenation reactor synoptic diagram
Fig. 3 is that reactor radial section reheater is arranged synoptic diagram.
Among Fig. 1, Fig. 2 or Fig. 3,1 is upper cover, and 2 is cylindrical tube, 3 is heating medium outlet, and 4 is the thermal barrier import, and 5 is lower cover, 6 is end socket, and 7 is second base plate, and 8 is first base plate, 9 is beds, 10 is inside distributor, and 11 is reheater, and 12 is the outer tube that distributes, 13 is Reactor inlet, and 14 is reactor outlet.
Reactor has a housing that bears pressure among Fig. 1, and this housing is comprised of cylindrical tube 2, upper cover 1 and low head 5. Respond on the housing device import 13 and reactor outlet 14, housing also has a heat carrier import 4 and a heating medium outlet 3. Have in the housing two with cylindrical tube 2 coaxial, columniform inside distributor 10 and outer distributing barrel 12, they and first base plate 8 are by formation catalyst basket mechanically coupled together, thus catalyst filling formation beds 9 in the catalyst basket. In the appropriate location of catalytic bed, at least one reheater 11 is set, reheater 11 is comprised of heating tube etc. This heating tube can be inverted-loop tube or/and two sleeve pipe is coaxial with reactor cylindrical tube 2 and beds 9. The perforate end original position of inside distributor 10 and the position of opening initiating terminal position of outer distributing barrel 12 can equate also can be unequal, consists of respectively radial bed or axle radial bed.
The flow direction of gas reaction medium in this reactor is such. Reactant enters the central passage that is formed by inside distributor 10 by Reactor inlet 13, and the simultaneously part shunting of flowing in central passage enters beds 9. Enter the gas of beds mainly with radially by bed, contact simultaneously the generation conversion reaction with catalyst. Because the fuel factor of reaction, gas temperature descends after the reaction, and the gas after the cooling continues radially to flow, until conduct heat with reheater generation cross-flow. Reacting gas is heated by high-temperature heat carrier and the temperature rising, so that reaction is carried out at faster speed. Reacted gas flows out beds 9, converges in the confluence passage that is made of outer distributing barrel 12 and cylindrical tube 2, finally by reactor outlet 14 outflow reactors.
The flow direction of heat carrier in reheater is such: the heat carrier of high temperature enters the second sealing chamber that is made of second base plate 7 and end socket 6 by reheater import 4, evenly distributes, enters in the pipe of each reheater 11 by the second sealing chamber high-temperature heat carrier. This heating tube 11 be inverted-loop tube or/and two sleeve pipe is coaxial with reactor cylindrical tube 2 and beds 9, thereby guaranteed the circumferential uniformity of bed temperature after the heating. The heat carrier that flows out from the pipe of each reheater 11 is pooled to the first sealing chamber that the not perforate section by second base plate 7, first base plate 8 and outer distributing barrel 12 consists of, and by heating medium outlet 3 outflow reactors.
Heating tube adopts inverted-loop tube or/and two sleeve pipe. Adopt inverted-loop tube or/and two sleeve pipe mainly is in order to eliminate the axial temperature difference of catalytic bed. Heat carrier temperature in inverted-loop tube in the down-comer of tedge compensates mutually, and both mean temperatures are little along the variation of pipe range, thereby guarantees the vertically uniformity of temperature of heating rear catalyst bed. High-temperature heat carrier at first enters central tube in two sleeve pipes, then flows out two sleeve pipes through annular space. Because the heat carrier of higher temperature will heat the lower heat carrier of annular space temperature in the central tube, keeping annular space heat carrier temperature, thus the assurance catalytic bed uniformity of temperature vertically.
Heating tube adopts inverted-loop tube or/and two sleeve pipe, for avoiding high wall temperature on the impact of catalytic reaction, adopt porous material aerial construction outside pipe, avoid catalyst directly to contact tube wall, this porous material can adopt the materials such as woven wire, porous plate or Johnson Net.
This type of reactor especially is suitable for ethyl benzene dehydrogenation preparation of styrene technology, can be used for new device former many thermal insulation, intersegmental reheat-type reactor are improved to the fixed-bed reactor that have heat-exchanging tube bundle in the separate unit catalytic bed, strengthens and produces, and saves facility investment; Can be used for the transformation of expanding production of existing apparatus, can in original radial reactor or axial-radial flow reactor catalytic bed, increase reheater.
The present invention is further elaborated below by embodiment.
Specific implementation method
[embodiment 1]
The catalytic dehydrogenation of ethylbenzene/vapour mixture is carried out in the reactor of accompanying drawing 1 or accompanying drawing 2, and the catalyzer of use adopts iron-potassium-cerium-molybdenum system.Reactor inside distributor diameter is 1150 millimeters, and the bed radial thickness is 600 millimeters, and static total height is 5500 millimeters.Reactor adopts upper cover to have the axial-radial flow reactor form of many apertures, and heating tube adopts inverted-loop tube, gos deep into whole beds.Heating tube quantity is 28, is uniformly distributed on the radial section logical thermal barrier in the inverted-loop tube.The temperature that reaction mass advances first reactor is 620 ℃, and whole reaction bed temperature is 547.6 ℃ of homogeneous, and pressure is 58KPa, and flow is 32257.2 kilograms/hour, and reaction result sees Table 1.
[comparative example 1]
The reactor geometrical dimension is with embodiment 1, and catalyzer and reaction process condition be with embodiment 1, just among Fig. 1 in the reactor not according to the dress reheater.After reaction for some time, reaction result sees Table 1.
[embodiment 2]
Press condition and the step of embodiment 1, just change the reheater pattern and be two sleeve pipes, two sleeve pipe quantity are 40, whole reaction bed temperature is 550.9 ℃ of homogeneous, reaction result is: conversion of ethylbenzene is 48.11%, and selectivity of styrene is 96.0%, and the vinylbenzene yield is 46.2%.
[embodiment 3]
Press condition and the step of embodiment 1, just changing the reheater pattern is inverted-loop tube and each 10 of two sleeve pipes, and whole reaction bed temperature is 545.3 ℃ near homogeneous, and reaction result is: conversion of ethylbenzene is 44.15%, selectivity of styrene is 97.2%, and the vinylbenzene yield is 42.9%.
Table 1
| Component | | Embodiment | 1 | Comparative example 1 | ||||
| The flow kilogram/hour | Form % weight | The flow kilogram/hour | Form % weight | The flow kilogram/hour | Form % weight | |||
| Ethylbenzene | 13138 | 40.73 | 7854.1 | 24.34 | 7924.6 | 24.56 | ||
| Vinylbenzene | 98.7 | 0.31 | 5157.4 | 15.98 | 5089.9 | 15.77 | ||
| Temperature, ℃ | 620 | 547.6 | 542.0 | |||||
| Pressure, kPaA | 58 | 52 | 52 | |||||
| Conversion of ethylbenzene, % | 46.7 | 40.52 | ||||||
| Selectivity of styrene, % | 97.0 | 97.5 | ||||||
| The vinylbenzene yield, % | 45.3 | 39.5 | ||||||
Claims (7)
1, a kind of fixed bed dehydrogenation reactor, comprise a housing that can bear pressure, feed-pipe, discharge nozzle, inside distributor, outer tube and first base plate of distributing, its middle shell is by cylindrical tube, upper cover and lower cover are formed, inside distributor and the outer tube that distributes are coaxial and form a catalyst basket with cylindrical tube, inside distributor and the outer tube that distributes have aperture in the catalyst basket corresponding section, first base plate links to each other with the outer bottom that distributes tube with inside distributor respectively, leaving the space between outer distribute tube and the cylindrical tube is connected with the discharging mouth of pipe, it is characterized in that reactor also comprises at least one thermal barrier import, at least one heating medium outlet, second base plate and at least one reheater under first base plate, form first enclosed chamber between first base plate and second base plate, form second enclosed chamber between second base plate and the lower cover, two ports of reheater are connected with first enclosed chamber and second enclosed chamber respectively, and go deep into whole catalyst basket, thermal barrier import and heating medium outlet respectively with first enclosed chamber and second enclosed chamber in one be connected, reheater is made up of 2～100 heating tubes, on the same radial section of catalyst basket, be evenly distributed, and coaxial with cylindrical tube.
2, according to the described fixed bed dehydrogenation reactor of claim 1, it is characterized in that also comprising on the catalytic bed upper cover, upper cover links to each other with the outer top that distributes tube with inside distributor respectively, and upper cover is not perforate, and inside distributor communicates with the feed-pipe that gos deep into upper cover.
3, according to the described fixed bed dehydrogenation reactor of claim 1, the top that it is characterized in that catalytic bed is to open wide fully; Or have a capping that has many apertures.
4,, it is characterized in that the thermal barrier import is 1 according to the described fixed bed dehydrogenation reactor of claim 1.
5,, it is characterized in that heating medium outlet is 1 according to the described fixed bed dehydrogenation reactor of claim 1.
6,, it is characterized in that heating tube is 10～40 according to the described fixed bed dehydrogenation reactor of claim 1.
7,, it is characterized in that heating tube is that inverted-loop tube is or/and two sleeve pipe according to the described fixed bed dehydrogenation reactor of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02111315 CN1207255C (en) | 2002-04-10 | 2002-04-10 | Fixed bed dehydrogenation reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02111315 CN1207255C (en) | 2002-04-10 | 2002-04-10 | Fixed bed dehydrogenation reactor |
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| CN1450039A CN1450039A (en) | 2003-10-22 |
| CN1207255C true CN1207255C (en) | 2005-06-22 |
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| CN 02111315 Expired - Fee Related CN1207255C (en) | 2002-04-10 | 2002-04-10 | Fixed bed dehydrogenation reactor |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106478351B (en) * | 2015-08-28 | 2019-02-19 | 中国石油化工股份有限公司 | The method of iso-butane and/or dehydrogenating propane |
| CN105413592B (en) * | 2015-12-17 | 2018-03-23 | 北京烨晶科技有限公司 | A kind of combined type fixed bed reactors and the device formed by it |
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