CN102068950B - Packed bed microreactor for preparing ethylene by dehydration of bioethanol - Google Patents
Packed bed microreactor for preparing ethylene by dehydration of bioethanol Download PDFInfo
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- CN102068950B CN102068950B CN 200910220045 CN200910220045A CN102068950B CN 102068950 B CN102068950 B CN 102068950B CN 200910220045 CN200910220045 CN 200910220045 CN 200910220045 A CN200910220045 A CN 200910220045A CN 102068950 B CN102068950 B CN 102068950B
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Abstract
The invention discloses a packed bed microreactor for preparing ethylene by the dehydration of bioethanol, which mainly solves the technical problems of a reactor for performing the catalytic dehydration reaction of the ethanol by adopting combustion heat supply, the problems of uniform temperature distribution of a catalyst bed of the reactor in a combustion heat supply way, and the technical problem of how to rapidly and highly-efficiently fill large catalyst particles in the microreactor. In the packed bed microreactor, two microchannel plate cores and three partition plates are sequentially arranged and packaged in a diffusion welding or braze welding way to form catalytic combustion chambers and catalytic hydrogenation reaction chambers which are alternately communicated in series and parallel, and a stratified combustion process is adopted to solve the problems. The catalyst bed of the integrated microreactor has uniform temperature, and ethanol conversion rate and ethylene selectivity which are both higher than 98 percent, and can realize operations at the high space velocity of 10 to 100 h<-1>. After parallel amplification, the microreactor can be used for the large-scale industrial production of the ethylene prepared from the bioethanol.
Description
Technical field
The present invention relates to a kind of packed bed microreactor of Preparation of Ethylene from Biological Ethanol Catalytic Dehydration, particularly the integrated microreactor of methyl alcohol/hydrogen catalytic combustion and ethylene prepared by catalytic dehydration of ethylene course of reaction.
Background technology
Along with the exhaustion day by day of worldwide energy crisis and petroleum resources, can avoid depending on unduly petroleum resources take living beings ethanol as raw materials for ethylene production.And, the biological ethane technological process is short, equipment investment is little, ethene purity is high, especially along with the fast-developing of biotechnology and take large living beings as raw material ethanol technology processed constantly perfect, the production cost of ethanol legal system ethene also will have more the market competitiveness with more rationalization as substitute technology or the additional technology of producing ethene with natural gas or light petroleum fraction.
Be the endothermic reaction because catalytic dehydration of ethanol prepares ethylene process, this process is more responsive to heat transfer condition, require the catalyst reactor axle radially bed near isothermal, to reduce side reaction, improve ethanol conversion and ethylene selectivity.Existing ethanol legal system ethene uses isothermal shell-and-tube reactor or multistage insulation fixed bed reactor more, and with the heat supply of electrically heated rod heating nitrate, its shortcoming is that thermal inertia is large, heating and cooling are slow, catalyst loading and unloading inconvenience.With hydrocarbon or its economy of Hydrogen fuel combustion heat supply is with the obvious advantage, be convenient to reactor integrated.
Board-like microreactor is because its channel characteristics yardstick is little, greatly the heat and mass transfer of strengthening process.Patent CN1629065A has reported a kind of plate-fin steam reforming hydrogen manufacturing reactor, contains 2 combustion chambers, 2 gasification chambers and 1 reformation chamber.The tubular type fluid distributor is set in combustion chamber, makes each cavity temperature distribution uniform, stop up but the distributor micropore is subject to catalytic combustion thermal-flame sintering, cause fluid distribution variation; And when this reactor amplifies, need the more multi-layered combustion chamber of stack, just have the problem of arranging a large amount of microtubule distributors, the distribution of often can not realizing ideal.
Described a kind of board-like microreactor for two phase flow reaction in patent USP7241423, on reactor, integrated heat transfer path, with regulation and control reactant or product temperature, be also a kind of stacked configuration, contains some on flat board and connect dull and stereotyped duct and straight channel.This plate-type reactor adopts micrometer-class yardstick passage, still under jejune condition, can not realize the beaded catalyst filling at catalyst wall carrier technology, therefore is not suitable for the Preparation of Ethylene from Biological Ethanol Catalytic Dehydration reaction.
Summary of the invention
The object of the invention is to provide a kind of bio-ethanol Dehydration ethene packed bed microreactor, it is integrated with fuel catalytic combustion and the reaction of living beings catalytic dehydration of ethanol, improved combustion system, and a large amount of solid particle catalysts of conveniently assemble and disassemble, and avoid using a large amount of distributors.
The present invention is a kind of preparing ethylene from bioethanol packed bed microreactor, its main body is formed by stacking by 〉=2 groups of microchannel plate cores, described plate core is divided into two classes by function, be respectively to realize the heat-absorbing plate core of catalytic and dehydration reaction and the heat liberation board core of catalyst combustion reaction, two class plate cores have many parallel microchannels flat boards by 〉=1 and are formed by stacking, press from both sides dividing plate between every two plate cores, the plate core closely is connected by diffusion welding (DW) or soldering with the dividing plate ordered arrangement, and the dull and stereotyped and described dividing plate of described formation plate core has following architectural feature:
Microchannel on the flat board of described microchannel connects dull and stereotyped, and all there is an open end that is used for catalyst filling in each flat board; It is lateral opening that each dull and stereotyped dual-side has 1-2 the bar shaped that connects flat board, this lateral opening input and/or output channel that is used for medium on the adjacent panel core that formed; Have 2-4 the bar shaped that connects dividing plate on described dividing plate lateral opening, its with plate core flat board on lateral opening or plate core flat board on the microchannel be connected, lateral opening equal in length on its length and plate core;
Overlapping microchannel plate core forms some runners of catalytic and dehydration reaction and catalyst combustion reaction, describedly consists of at least one medium flow process plate groups in order to some runners of realizing same reaction, and every adjacent two plate cores are staggered.
The said flow process of this patent refers to react the quantity of logistics flow direction in reactor; Runner refers to that in each flow process, the reaction logistics is by equidirectional mobile plate core quantity.
In reactor features as mentioned above,
In order to realize that some runners of same reaction consist of the medium flow process plate groups of 2-10 series connection, each flow process plate groups is made of 2-4 runner parallel combination.Realize that the runner series parallel structure is determined by dividing plate perforate rule: be arranged in parallel in order to the lateral opening of the same reaction medium that circulates on dividing plate, in order to the lateral opening adjacent setting of the differential responses medium that circulates; The identical adjacent two plate in-core MEDIA FLOW of function are when opposite, and on each dividing plate and plate core, the lateral opening number in order to this reaction medium that circulates is 1 therebetween; If the identical adjacent two plate in-core MEDIA FLOW of function are to identical, therebetween on each dividing plate and plate core the lateral opening number in order to this reaction medium that circulates be 2.
When the identical arbitrary neighborhood two plate in-core MEDIA FLOW of function on the contrary, i.e. plate core series connection, have on the dividing plate between all plate cores adjacent 2 lateral opening; MEDIA FLOW is to identical in adjacent two heat-absorbing plate cores, and namely the plate core is in parallel, and adjacent two heat liberation board in-core MEDIA FLOW are on the contrary, have on the dividing plate between two heat-absorbing plate cores in parallel 3 lateral opening; And when contain two and in parallel with the upper plate core in order to all flow process plate groups of carrying out two reactions, in and the yoke plate core between the dividing plate of one at least on have 4 lateral opening.Width or the open end width of all parallel microchannels on the lateral opening length of bar shaped on dividing plate 〉=plate core flat board.Parallel microchannels on the flat board of described formation plate core and lateral opening be to form through two-sided the scribing of chemical etching on thickness is the sheet material of 0.1-1mm, or described plate core is made by a slab line cutting processing; Described plate core upper channel has the equivalent diameter of at least 0.5～10mm, the thick 0.3～0.8mm that is generally of described dividing plate.
consisting of as above, the reactor of feature also comprises side seal board: the outside of open end that is fastened on respectively to carry out all plate cores of same reaction, with bolted, during stack, carry out the open end of all plate cores of same reaction towards identical, after packing beaded catalyst into, the open end covers shrouding, wherein a side seal board is provided with a plurality of charging apertures, be used for the input of combustion reaction raw material, fuel advances from the first charging aperture, air advances from each charging aperture respectively, every grade of import comprises the distribution hole count identical with port number in every laminate, material is distributed in each passage in every laminate.
The present invention has the bio-ethanol legal system ethene packed bed microreactor of above-mentioned feature, is in fact the consersion unit of the reinforcement of a kind of endothermic reaction and exothermal reaction process and process integration.
Exothermic reaction in this integrated reactor is catalyst combustion reaction, and as the catalytic combustion of hydrogen-oxygen, the catalytic combustion of liquid methanol, hydrogen can be that pure hydrogen or hydrogen containing tail gas such as anode of fuel cell tail gas, natural gas hydrogen preparation pressure-variable adsorption are carried hydrogen tail gas etc.In course of reaction, fuel all enters all runners in the 1st flow process plate groups of combustion side, and with fuel entering part air; Surplus air enters respectively the 3rd, the 5th all runners of flow process plate groups, also can the several flow processs in interval add the classification air, in the 1st flow process plate groups, complete oxidation is transformed into partial oxidation reaction at this moment, this place's bed temperature rise reduces, in reactor, focus is eliminated, and then produces desirable Temperature Distribution.The classification air is controlled respectively by some mass-flow gas meters, or utilizes classification charging Fine distributions few in number on combustion chamber shrouding ducts allocation proportion.
The integrated microreactor original intention of the present invention is that to be exclusively used in Ethanol Method ethylene reaction produced, this reaction is the endothermic reaction, in actual use, can carry out other the endothermic reaction in endothermic reaction passage, as: the steam reformation of methanol to produce hydrogen reaction, CO water gas shift reactions etc. are just filled the catalyst corresponding with each reacting phase in heat recipient passage.When not adding catalyst in the heat-absorbing plate core internal channel, by suitably dwindling its channel size, or directly replace it with the Thermal Performance of Micro Channels sheet, reactor changes a kind of catalytic combustion-vaporizer into.
When microreactor amplified, the passage of suitable filler particles catalyst generally should be greater than the 0.5mm equivalent diameter, and was suitable with the popular response device greater than its mass-and heat-transfer characteristic of passage of 10mm equivalent diameter, can not the high-speed conditional operation.But the present invention realizes the microchannel of catalyst filling by dual mode: the one, and the two-sided perforation etching of chemical etching generally to be no more than the thick thin metal blank processing of 1mm, is then taked some thin plates to overlap into one deck without dividing plate; The 2nd, directly to require the metal printed line cutting of the degree of depth.The passageway machining method has been known in this field, is the necessary means that realizes structure of reactor of the present invention.
The present invention uses dividing plate that catalytic and dehydration reaction logistics and catalyst combustion reaction logistics in accordance with regulations direction between the little packed bed reactor plate of described integrated multi-channel core is flowed, thereby coutroi velocity, obtain mass-and heat-transfer effect and reactor pressure decrease preferably, satisfy technological requirement.Therefore, the present invention is in fact again the performance of a flow process and runner combining form.Two kinds of anti-logistics need on all plate core space bars 2 of lateral opening adjacent at least layouts; When a flow process existed multiple flow passages in parallel, between multiple flow passages in parallel, the parallel edges of at least one dividing plate was established lateral openingly, adds input and/or the output channel of reaction logistics on another reaction runner between multiple flow passages in parallel, need have on dividing plate 3 or 4 lateral opening.Because dividing plate plays heat transfer effect simultaneously, its thinner thickness, the present invention selects 0.3～0.8mm, and the plate of other thickness is also optional certainly.
Consist of two sides on all microchannel plates of each plate core establish at least 1 lateral opening must be by lateral opening connection the on this interlayer because burn the adjacent two-layer dehydration runner of reaction runner with arbitrary grate firing.Before address, as long as have the adjacent two plate cores structure that is communicated with in parallel, its space bar need establish 3 lateral opening, in the case and between the yoke plate core sandwich plate core need have 2 lateral opening to realize this combination.These are lateral opening is long and narrow bar shaped, and its length equals plate core open end extended distance at least, so that all reaction channels are communicated with it, avoid becoming the high-drag stream near place, both sides passage, even short circuit when ordered arrangement plate core, dividing plate and end pressure strip, needs all plates of alignment.
When the integrated microreactor of the present invention is used for preparing ethylene from bioethanol, the bio-ethanol raw material can enter the reaction runner with any state in principle, preferably use the bio-ethanol raw material of vaporized state, reactant is preferentially in integrated microreactor dehydration outlet heat exchange, then further with the combustion tail gas heat exchange, and be vaporized and be warming up to 150-250 ℃, after enter reactor so that material and uniformity of temperature profile, Fuel Consumption is few.The vaporization of reactant is preferably in the known efficient micro-channel heat exchanger in this area (little reaction technology) to be carried out, to reduce heat loss.
Due in order to carrying out all runner interphase distributions of two reactions, and the several millimeters only of each the catalytic reaction passage equivalent diameter on runner, in reactor, the catalytic dehydration of ethanol reaction can be at 10-100h
-1High-speed under operate, the reaction bed temperature is controlled at 380-500 ℃, reactor performance is good.
Characteristics of the present invention: simple in structure, be convenient to processing, can any integrated amplification; Be easy to realize a large amount of beaded catalysts of filling in micro passage reaction; But be used for operating under bio-ethanol Dehydration ethene high-speed, and bed temperature is even, ethylene selectivity and yield are higher than 98%.
Description of drawings
Fig. 1, the integrated microreactor agent structure of the present invention schematic diagram; In figure, the 1-heat-absorbing plate core, 2-heat liberation board core, the 3-dividing plate, 4-is lateral opening.
Temperature Distribution under Fig. 2, each measurement point of microreactor dehydration side of the present invention.
The specific embodiment
Fig. 1 has disclosed a kind of part of complicated enforcement the most of packed bed microreactor of the present invention.Comprise a plurality of heat-absorbing plate cores 1 and heat liberation board core 2, and dividing plate 3, have lateral opening 4 on each heat-absorbing plate core 1 and heat liberation board core 2 and dividing plate 3.be used for carrying out 1 folder one deck of adjacent two layers plate core of catalytic and dehydration reaction (heat absorption) for the plate core 2 that carries out catalyst combustion reaction (heat release), and become the serial or parallel connection runner plate by lateral opening 4 connections on a sidewall on plate core 2, plate core 1 and 2 is staggered, all plate cores fit tightly and form in order to carry out the multipaths plate groups of two catalytic reactions (catalytic combustion and catalytic dehydration), in this enforcement, often flow through in some runner plates separately two plate cores of each catalytic reaction logistics change once and flow to, be that each flow process plate groups is made of two runner plate parallel combinations.Dividing plate 3 top hole counts be respectively 2,3,4 and by 2,3,4,3,2,3,4... is arranged sequentially, lateral opening 4 its length on dividing plate equate with runner plate top edge two passes spacing, open on the first laminate core 11 lateral opening, open on the first laminate core 22 lateral opening, also open 2 lateral opening so that the first laminate cores 2 on the second laminate core 1 and second laminate core 2 is in parallel is communicated with.
At the alternate plate core 1 channel opener end that is used for carrying out the catalytic dehydration of ethanol reaction dehydration catalyst (alumina system or molecular sieve system) of packing into, at the alternate plate core 2 channel opener ends combustion catalyst (as: Pt/Al system) of packing into, the catalyst grain size of loading and passage equivalent diameter adapt, and passage of the present invention is 4 * 4mm
2, every plate core contains 8 passages, and catalyst grain size is the 20-40 order.
At the channel opener end of the packed bed microreactor that is consisted of by cross-flow passage and dividing plate, after populated catalyst, sealed by side seal board.wherein, establish stratified combustion air feed mouth on the catalytic combustion side seal board, the first charging aperture is located on the upper of plate core or lower shrouding, fuel (as hydrogen or methyl alcohol etc.) all enters burning zone by the first charging aperture, and in company with the entering part combustion air, surplus air the 2nd grade of the 3rd flow process plate groups that the air feed mouth enters combustion side from the side seal board, charging aperture is a narrow bar-shaped trough, and in the groove open interior, hole count equates with individual layer runner plate upper channel number, each hole can contain a plurality of micropores again, the 1st grade of air capacity accounts for total amount 40-50%, the 2nd grade accounts for total amount 50-60%, because the static pressure that reaction produces at the reactor front end is always greater than tail end, the front end that causes burning easily accumulates heat, so should make as far as possible the exothermic heat of reaction amount of reaction front end low, being conducive to bed temperature distributes.
Overall volume by the bio-ethanol legal system ethene packed bed microreactor of previous designs method processing is: 90 * 90 * 90mm
3, combustion catalyst and dehydration catalyst fillable volume be 100ml approximately.
(the Temperature Distribution situation of d1～d5) is depicted in Fig. 2 dehydration layer each point in reactor of the present invention, and reactor ethene production capacity and reactivity worth partial data are listed in table 1.Reactor catalysis bed temperature distribution map and reactivity worth data show, packed bed microreactor of the present invention is applicable to the bio-ethanol catalytic dehydration and produces ethene.
Table 1, microreactor of the present invention are produced 0.3～1.0Nm
3/ h C
2H
4Reactor performance;
Claims (6)
1. bio-ethanol Dehydration ethene packed bed microreactor, its main body is formed by stacking by 〉=2 groups of microchannel plate cores, described plate core is divided into two classes by function, be respectively to realize the heat-absorbing plate core of catalytic and dehydration reaction and the heat liberation board core of catalyst combustion reaction, two class plate cores have many parallel microchannels flat boards by 〉=1 and are formed by stacking, press from both sides dividing plate between every two plate cores, it is characterized by:
Microchannel on the flat board of described microchannel connects dull and stereotyped, and between the flat board of a plate core of formation, without the dividing plate stack, all there is an open end that is used for catalyst filling in each flat board; It is lateral opening that each dull and stereotyped dual-side has 1-2 the bar shaped that connects flat board, this lateral opening input and/or output channel that is used for medium on the adjacent panel core that formed;
Have 2-4 the bar shaped that connects dividing plate on described dividing plate lateral opening, its with plate core flat board on lateral opening or plate core flat board on the microchannel be connected, lateral opening equal in length on its length and plate core;
Overlapping microchannel plate core forms some runners of catalytic and dehydration reaction and catalyst combustion reaction, describedly consists of at least one medium flow process plate groups in order to some runners of realizing same reaction, every adjacent two plate cores alternately and the alternate cross-flow of medium arrange;
Be arranged in parallel in order to the lateral opening of the same reaction medium that circulates on dividing plate, and in order to the lateral opening adjacent setting of the differential responses medium that circulates; If the identical adjacent two plate in-core MEDIA FLOW of function are on the contrary, therebetween on each dividing plate and plate core the lateral opening number in order to this reaction medium that circulates be 1; If the identical adjacent two plate in-core MEDIA FLOW of function are to identical, therebetween on each dividing plate and plate core the lateral opening number in order to this reaction medium that circulates be 2;
If the identical arbitrary neighborhood two plate in-core MEDIA FLOW of function are on the contrary, i.e. plate core series connection, have on the dividing plate between all plate cores adjacent 2 lateral opening; If MEDIA FLOW is to identical in adjacent two heat-absorbing plate cores, namely the plate core is in parallel, and adjacent two heat liberation board in-core MEDIA FLOW are on the contrary, have on the dividing plate between two heat-absorbing plate cores in parallel 3 lateral opening; If contain two and in parallel with the upper plate core in order to all flow process plate groups of carrying out two reactions, in and the yoke plate core between the dividing plate of one at least on have 4 lateral opening.
2. according to the described packed bed microreactor of claim 1, it is characterized by: consist of the medium flow process plate groups of 2-10 series connection in order to realize some runners of same reaction, each flow process plate groups is made of 2-4 runner parallel combination.
3. according to the described packed bed microreactor of claim 1, it is characterized by: width or the open end width of all parallel microchannels on the lateral opening length of the bar shaped on dividing plate 〉=plate core flat board.
4. according to the described packed bed microreactor of claim 1, wherein in order to the open end of all plate cores of carrying out same reaction towards identical; Respectively cover a shrouding in formed two open ends, wherein a side seal board is provided with a plurality of charging apertures, is used for the input of combustion reaction raw material, and fuel advances from the first charging aperture, and air advances from each charging aperture respectively, and the fluid distribution hole is sucked in each charging.
5. according to the described packed bed microreactor of claim 1, parallel microchannels on the flat board of described formation plate core and lateral opening be to form through two-sided the scribing of chemical etching on thickness is the sheet material of 0.1-1mm, or described plate core is made by a slab line cutting processing; Described plate core upper channel has the equivalent diameter of at least 0.5～10mm, the thick 0.3～0.8mm that is generally of described dividing plate.
6. according to the described packed bed microreactor of claim 1 or 4, it is characterized by: closely be connected by diffusion welding (DW) or soldering after plate core and dividing plate ordered arrangement, the open end shrouding after catalyst filling with bolted.
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| CN 200910220045 CN102068950B (en) | 2009-11-20 | 2009-11-20 | Packed bed microreactor for preparing ethylene by dehydration of bioethanol |
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| CN112973596B (en) * | 2021-03-01 | 2023-05-12 | 安徽华尔泰化工股份有限公司 | Microchannel continuous flow reactor |
Citations (3)
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|---|---|---|---|---|
| CN201206102Y (en) * | 2008-03-19 | 2009-03-11 | 北京石油化工学院 | Laminated self-heating micro hydrogen making reactor |
| US7608160B2 (en) * | 2004-10-13 | 2009-10-27 | Rheonix, Inc. | Laminated microfluidic structures and method for making |
| CN101580227A (en) * | 2009-06-22 | 2009-11-18 | 浙江大学 | Self-heating type alcohol reforming hydrogen production micro channel reactor with micro-lug boss array structure |
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2009
- 2009-11-20 CN CN 200910220045 patent/CN102068950B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7608160B2 (en) * | 2004-10-13 | 2009-10-27 | Rheonix, Inc. | Laminated microfluidic structures and method for making |
| CN201206102Y (en) * | 2008-03-19 | 2009-03-11 | 北京石油化工学院 | Laminated self-heating micro hydrogen making reactor |
| CN101580227A (en) * | 2009-06-22 | 2009-11-18 | 浙江大学 | Self-heating type alcohol reforming hydrogen production micro channel reactor with micro-lug boss array structure |
Non-Patent Citations (2)
| Title |
|---|
| Catalytic dehydration of bioethanol to ethylene over TiO2/γ-Al2O3 catalysts in microchannel reactors;Guangwen Chen et al.;《Catalysis Today》;20071231;第125卷;111-119 * |
| Guangwen Chen et al..Catalytic dehydration of bioethanol to ethylene over TiO2/γ-Al2O3 catalysts in microchannel reactors.《Catalysis Today》.2007,第125卷111-119. |
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