CN102068950A - 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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- CN102068950A CN102068950A CN2009102200459A CN200910220045A CN102068950A CN 102068950 A CN102068950 A CN 102068950A CN 2009102200459 A CN2009102200459 A CN 2009102200459A CN 200910220045 A CN200910220045 A CN 200910220045A CN 102068950 A CN102068950 A CN 102068950A
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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 bio-ethanol catalytic dehydration system ethene, particularly methyl alcohol/hydrogen catalytic combustion and the integrated microreactor of 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, be that raw material production ethene can be avoided depending on unduly petroleum resources with living beings ethanol.And, the biological ethane technological process is short, equipment investment is little, ethene purity height, especially be the constantly perfect of raw material system ethanol technology along with the fast-developing of biotechnology with large living beings, the production cost of ethanol legal system ethene will more become to rationalizing, and also will have more the market competitiveness as the substitute technology or the additional technology of producing ethene with natural gas or light petroleum cut.
Because to prepare ethylene process is the endothermic reaction to catalytic dehydration of ethanol, this process is responsive to heat transfer condition, require the catalyst reactor diameter of axle to 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 big, heating and cooling are slow, catalyst loading and unloading inconvenience.With hydrocarbon or its economy of hydrogen fuel combustion heat supplying is with the obvious advantage, it is integrated to be convenient to reactor.
Board-like microreactor is little owing to its channel characteristics yardstick, 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 the combustion chamber, makes each cavity temperature distribution uniform, stop up, cause fluid distribution variation but the distributor micropore is subject to catalytic combustion thermal-flame sintering; 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 that is used for two phase flow reaction among the patent USP7241423, integrated heat transfer path with regulation and control reactant or product temperature, also is a kind of stacked configuration on the reactor, contains some on the flat board and connects dull and stereotyped duct and straight channel.This plate-type reactor adopts micrometer-class yardstick passage, under the still jejune condition of catalyst wall carrier technology, can not realize the beaded catalyst filling, and it is ethylene reaction produced therefore not to be suitable for the bio-ethanol catalytic dehydration.
Summary of the invention
The object of the invention provides a kind of bio-ethanol dehydration system 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 in order to the heat-absorbing plate core of realization 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 per two plate cores, the orderly arrangement of plate core and dividing plate closely is connected by diffusion welding (DW) or soldering, 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 panels core that formed; It is lateral opening to have 2-4 the bar shaped that connects dividing plate on the described dividing plate, its with plate core flat board on lateral opening or plate core flat board on the microchannel be connected the lateral opening equal in length on its length and the plate core;
The microchannel plate core that overlaps forms some runners of catalytic and dehydration reaction and catalyst combustion reaction, describedly constitutes 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 the reaction logistics is by equidirectional mobile plate core quantity in each flow process.
In reactor features as mentioned above,
In order to realize that some runners of same reaction constitute the medium flow process plate groups of 2-10 series connection, each flow process plate groups is constituted by 2-4 runner parallel connection.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 the dividing plate, in order to the lateral opening adjacent setting of circulation differential responses medium; The identical adjacent two plate in-core MEDIA FLOW of function are when opposite, and the lateral opening number in order to this reaction medium that circulates is 1 on each dividing plate and the plate core therebetween; If the identical adjacent two plate in-core MEDIA FLOW of function are to identical, then therebetween on each dividing plate and the plate core the lateral opening number in order to this reaction medium that circulates be 2.
When the identical any adjacent two plate in-core MEDIA FLOW of function on the contrary, i.e. plate core series connection, then 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, i.e. plate core parallel connection, and adjacent two heat liberation board in-core MEDIA FLOW are on the contrary, then on the dividing plate between two heat-absorbing plate cores in parallel, have 3 lateral opening; And when containing two and with the parallel connection of upper plate core in order to all flow process plate groups of carrying out two reactions, then in and the yoke plate core between the dividing plate of one at least on have 4 lateral opening.The width or the open end width of all parallel microchannels on the lateral opening length of bar shaped on the dividing plate 〉=plate core flat board.Parallel microchannels on the flat board of described formation plate core and lateral opening be on thickness is the sheet material of 0.1-1mm, to form through two-sided the scribing of chemical etching, 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.
Constituting as above, the reactor of feature also comprises side seal board: be fastened on the outside in order to the open end of all plate cores of carrying out same reaction respectively, with bolted, during stack, the open end of all plate cores of carrying out same reaction is 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 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, and material is distributed in each bar passage in every laminate.
The present invention has the bio-ethanol legal system ethene packed bed microreactor of above-mentioned feature, comes down to the consersion unit of reinforcement of a kind of endothermic reaction and exothermal reaction process and process integration.
Exothermic reaction in this integrated reactor is a catalyst combustion reaction, and as the catalytic combustion of hydrogen-oxygen, the catalytic combustion of liquid methanol, hydrogen can be that hydrogen tail gas etc. is carried in pure hydrogen or hydrogen containing tail gas such as anode of fuel cell tail gas, the absorption of natural gas hydrogen preparation transformation.In the 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 the 3rd, the 5th all runners of flow process plate groups respectively, also can at interval several flow processs add the classification air, complete oxidation is transformed into partial oxidation reaction in the 1st flow process plate groups at this moment, this place's bed temperature rise reduces, focus is eliminated in the reactor, produces desirable Temperature Distribution then.The classification air is controlled respectively by some mass-flow gas meters, or utilizes the fine distribution of classification charging duct allocation proportion few in number on the combustion chamber shrouding.
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 the endothermic reaction passage, as: the steam reformation of methanol to produce hydrogen reaction, CO water gas shift reactions etc. are just filled in heat recipient passage and are reacted corresponding catalyst with each.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 taked not have dividing plate with some thin plates then and is overlaped into one deck; The 2nd, directly to require the metal printed line cutting of the degree of depth.The passage processing 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 multichannel core is flowed, thereby control flow 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 the multithread road in parallel, the parallel edges of at least one dividing plate was established lateral openingly between multithread in parallel road, adds the input and/or the output channel of reaction logistics on another reaction runner between multithread in parallel road, need have on the dividing plate 3 or 4 lateral opening.Because of dividing plate plays heat transfer effect simultaneously, its thinner thickness, the present invention selects 0.3～0.8mm for use, and the plate of other thickness is also optional certainly.
Constitute two sides on all microchannel plates of each plate core establish at least 1 lateral opening must be because burn the adjacent two-layer dehydration runner of reaction runner by lateral opening connection the on this interlayer 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 to be 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 orderly arrangement board core, dividing plate and end pressure strip, need 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.
Because in order to carrying out all runner interphase distributions of two reactions, and the only several millimeters of each the bar catalytic reaction passage equivalent diameter on the runner, the catalytic dehydration of ethanol reaction can be at 10-100h in the reactor
-1Down operation of high-speed, the reaction bed Controllable Temperature is 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 be implemented in a large amount of beaded catalysts of filling in the micro passage reaction; But be used for the operation down of bio-ethanol dehydration system 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; Among the 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, on each heat-absorbing plate core 1 and heat liberation board core 2 and dividing plate 3, all have lateral opening 4.1 folder of the adjacent two layers plate core one deck that is used to carry out catalytic and dehydration reaction (heat absorption) is used to carry out the plate core 2 of catalyst combustion reaction (heat release), and by lateral opening 4 being communicated with and becoming the serial or parallel connection runner plate on the sidewall on the plate core 2, plate core 1 and 2 is staggered, all plate cores fit tightly formation in order to carry out the multipaths plate groups of two catalytic reactions (catalytic combustion and catalytic dehydration), whenever flow through in some runner plates separately two plate cores of each catalytic reaction logistics change once and flow in this enforcement, and promptly each flow process plate groups is constituted by two runner plate parallel connections.Dividing plate 3 top hole counts be respectively 2,3,4 and by 2,3,4,3,2,3,4... arranges in proper order, distance equates between lateral opening 4 its length on the dividing plate and runner plate top edge two passes, open on the first laminate core 11 lateral opening, then open on the first laminate core 22 lateral opening, also open 2 lateral opening so that first laminate cores 2 and 2 in parallel connections of the second laminate core on the second laminate core 1.
The plate core 1 channel opener end that carries out catalytic dehydration of ethanol reaction in alternate the being used to 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, catalyst grain size of being loaded 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 constitutes by cross-flow passage and dividing plate, behind populated catalyst, seal by side seal board.Wherein, on the catalytic combustion side seal board, establish stratified combustion air feed mouth, first charging aperture is located on going up of plate core or the following shrouding, fuel (as hydrogen or methyl alcohol etc.) all enters burning zone by 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, and the 1st grade of air capacity accounts for total amount 40-50%, and the 2nd grade accounts for total amount 50-60%, because the static pressure that is reflected at the generation of reactor front end is always greater than tail end, the front end that causes burning easily accumulates heat, so should make the exothermic heat of reaction amount of reaction front end low as far as possible, helps bed temperature and 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 the about 100ml of dehydration catalyst fillable volume.
(the Temperature Distribution situation of d1～d5) is depicted among Fig. 2 dehydration layer each point in the reactor of the present invention, and reactor ethene production capacity and reactivity worth partial data are listed in the table 1.Reactor catalysis bed temperature distribution map and reactivity worth data show that packed bed microreactor of the present invention is applicable to bio-ethanol catalytic dehydration production ethene.
Table 1, microreactor of the present invention are produced 0.3～1.0Nm
3/ h C
2H
4Reactor performance;
Claims (8)
1. ethene packed bed microreactor is made in a bio-ethanol dehydration, 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 in order to the heat-absorbing plate core of realization 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 per two plate cores, it is characterized by:
Microchannel on the flat board of described microchannel connects dull and stereotyped, no dividing plate stack between the flat board of a plate core of formation, 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 panels core that formed;
It is lateral opening to have 2-4 the bar shaped that connects dividing plate on the described dividing plate, its with plate core flat board on lateral opening or plate core flat board on the microchannel be connected the lateral opening equal in length on its length and the plate core;
The microchannel plate core that overlaps forms some runners of catalytic and dehydration reaction and catalyst combustion reaction, describedly constitutes 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.
2. according to the described packed bed microreactor of claim 1, it is characterized by:
Be arranged in parallel in order to the lateral opening of the same reaction medium that circulates on the dividing plate, and in order to the lateral opening adjacent setting of circulation differential responses medium; If the identical adjacent two plate in-core MEDIA FLOW of function are on the contrary, then therebetween on each dividing plate and the 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, then therebetween on each dividing plate and the plate core the lateral opening number in order to this reaction medium that circulates be 2.
3. according to the described packed bed microreactor of claim 2, it is characterized by:
If the identical any adjacent two plate in-core MEDIA FLOW of function are on the contrary, promptly the plate core is connected, then 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, i.e. plate core parallel connection, and adjacent two heat liberation board in-core MEDIA FLOW are on the contrary, then on the dividing plate between two heat-absorbing plate cores in parallel, have 3 lateral opening; If contain two and with the parallel connection of upper plate core in order to all flow process plate groups of carrying out two reactions, then in and the yoke plate core between the dividing plate of one at least on have 4 lateral opening.
4. according to the described packed bed microreactor of claim 1, it is characterized by: constitute 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 constituted by 2-4 runner parallel connection.
5. according to the described packed bed microreactor of claim 1, it is characterized by: the width or the open end width of all parallel microchannels on the lateral opening length of the bar shaped on the dividing plate 〉=plate core flat board.
6. 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 first charging aperture, and air advances from each charging aperture respectively, and fluid distribution hole is sucked in each charging.
7. 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 on thickness is the sheet material of 0.1-1mm, to form through two-sided the scribing of chemical etching, 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.
8. according to claim 1 or 6 described packed bed microreactors, it is characterized by: plate core and dividing plate are arranged the back in order and closely are connected by diffusion welding (DW) or soldering, the open end shrouding behind catalyst filling with bolted.
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN 200910220045 CN102068950B (en) | 2009-11-20 | 2009-11-20 | Packed bed microreactor for preparing ethylene by dehydration of bioethanol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112625034A (en) * | 2021-01-04 | 2021-04-09 | 张家港威胜生物医药有限公司 | Preparation method of vinpocetine |
| CN112973596A (en) * | 2021-03-01 | 2021-06-18 | 安徽华尔泰化工股份有限公司 | Microchannel continuous flow reactor |
Family Cites Families (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 |
| CN101580227B (en) * | 2009-06-22 | 2011-04-27 | 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
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112625034A (en) * | 2021-01-04 | 2021-04-09 | 张家港威胜生物医药有限公司 | Preparation method of vinpocetine |
| CN112973596A (en) * | 2021-03-01 | 2021-06-18 | 安徽华尔泰化工股份有限公司 | Microchannel continuous flow reactor |
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