CN101415485B - Micro-reactor system - Google Patents

Micro-reactor system Download PDF

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Publication number
CN101415485B
CN101415485B CN200780012236.5A CN200780012236A CN101415485B CN 101415485 B CN101415485 B CN 101415485B CN 200780012236 A CN200780012236 A CN 200780012236A CN 101415485 B CN101415485 B CN 101415485B
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heat
module
heat exchange
exchange
reacting
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CN101415485A (en
Inventor
多米尼克·罗贝热
尼古拉斯·比勒尔
伯廷·齐默尔曼
赖纳德·福伯特
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Lonza AG
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Lonza AG
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Priority claimed from PCT/EP2007/002831 external-priority patent/WO2007112945A1/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093Microreactors, e.g. miniaturised or microfabricated reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00783Laminate assemblies, i.e. the reactor comprising a stack of plates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00801Means to assemble
    • B01J2219/00804Plurality of plates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00801Means to assemble
    • B01J2219/0081Plurality of modules
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00819Materials of construction
    • B01J2219/00822Metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00819Materials of construction
    • B01J2219/00824Ceramic
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00851Additional features
    • B01J2219/00858Aspects relating to the size of the reactor
    • B01J2219/0086Dimensions of the flow channels
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00851Additional features
    • B01J2219/00867Microreactors placed in series, on the same or on different supports
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00873Heat exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00889Mixing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00891Feeding or evacuation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/0095Control aspects
    • B01J2219/00984Residence time
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00993Design aspects
    • B01J2219/00997Strategical arrangements of multiple microreactor systems

Abstract

A micro-reactor system assembly comprises a stack of at least n process modules (1-6), wherein n is an integer equal to or greater than 1, made from a rigid first material and comprising at least one reactive fluid passage (1A, 1B, 2A, 3A, 6A) for accommodating and guiding a reactive fluid, and at least n+1 heat exchange modules (7, 8) made from a ductile second material other than said first material and comprising at least one heat exchange fluid passage (7A, 8A) for accommodating and guiding a heat exchange fluid, wherein each process module (1-6) is sandwiched between two adjacent heat exchange modules (7, 8).

Description

Micro-reactor system
Technical field
The present invention relates to micro-reactor system, it comprises at least n processing module and n+1 heat exchange module at least, and wherein each processing module is sandwiched between two adjacent heat exchange modules.
Background technology
Microreactor is a reaction unit; It is used for one or more reactant reactions (mixture that comprises two or more reactants usually), and be used for to a certain extent through before mixing, mix and/or mix the reaction that said reactant is controlled in back heating or cooling or the said reactant of heat buffering.The microreactor that is used for realization chemical reaction in the zonule like this can be known from for example EP-A-0688242, EP-A-1031375, WO-A-2004/045761 and US-A-2004/0109798.
The chemical reaction that in microreactor, carries out can be divided into so-called A type reaction and Type B reaction basically.
A type reaction, organometallic reaction for example is very fast chemical reaction and in mixing chamber, directly take place during mixed reactant, usually in 1 second scope.They can be called as the reaction by mixed processing control.In order to let all reactant complete reactions and for fear of accessory substance, such A type reaction requires to handle mixing fast with effectively of fluid, and effectively thermal control.Such A type reaction requires not have or the very short afterreaction time usually, and therefore can in the microreactor with little resident volume or afterreaction volume, realize well.For the residence time of this type reaction usually in less than 20 seconds scope.
On the contrary, Type B reaction, the acetyl acylation reaction of Wittig reaction (Wittig reaction) or aromatic amine and diketene (diktene) for example, faster or slower, the common reaction time is in the scope in 1 second to 10 minute.They receive concentration or dynamics Controlling and carry out.In order to make reactant reaction fully and avoid accessory substance, the reaction of this type Type B does not require this reactant of very fast mixing, and requires can control in entire reaction time internal reaction condition.Therefore, the size of resident volume and afterreaction volume must so be set, and promptly can easily and handle fluid under the condition of accurately control in this microreactor maintenance for a long time.Yet, because the little and expensive micro-structural of size up to now, realizes that with traditional microreactor so long residence time is difficult.Therefore, traditional microreactor major part is used for the reaction of A type.
Summary of the invention
Therefore, the purpose of this invention is to provide improved micro-reactor system, it is suitable for guaranteeing required residence time, and temperature control is possible in this residence time.
This purpose is solved by micro-reactor system according to claim 1, and it comprises following storehouse:
At least n processing module (1-6), wherein n is equal to or greater than 1 integer.Each processing module (1-6) is processed by first material of rigidity; And comprise at least one reacting fluid passage (1A, 1B, 2A, 3A, 6A); This reacting fluid passage passes said processing module (1-6); And between at least one reacting fluid inlet port (1C, 1D, 2C, 2D, 3C, 6C) and at least one reacting fluid outlet (1E, 1F, 2E, 3D, 6D), be used to hold and guide reacting fluid.Wherein, under the situation that at least two processing modules (1-6) arranged, connect on said at least two processing modules (1-6) function; And
At least n+1 heat exchange module (7,8); Its second material by deformable that is different from said first material or flexible is processed; And comprise at least one heat-exchange fluid passage (7A, 8A); This heat-exchange fluid passage passes said heat exchange module (7,8) inside, and between its at least one heat-exchange fluid inlet port (7B, 8B) and at least one heat-exchange fluid outlet (7C, 8C), is used to hold and guide heat-exchange fluid; Connect on the wherein said heat exchange module of n+1 at least (7, the 8) function
Wherein each processing module (1-6) is sandwiched between two adjacent heat exchange modules (7,8).
This is n processing module and this n+1 each self-forming of heat exchange module module independently at least at least; It limits at least one fluid passage; Be reacting fluid passage or heat-exchange fluid passage, extend fully the inside of the module between this at least one inlet port and this at least one outlet.
Through processing module and the heat exchange module of being processed by different materials is provided, being respectively this processing module and heat exchange module, to select following first and second materials be possible:
For this processing module; Can select reaction to this reactant; Especially first material anticorrosive and/or resistance to compression is best, and preferably be selected from the group that comprises stainless steel, nickel-base alloy, tungsten, tantalum, titanium, pottery, silicon, graphite and/or the appropriate combination of one or more said first materials.
For this heat exchange module; Can select second material of flexible; It is to heat transmission and/or sealing, and especially hot conduction is best, and preferably is selected from the group that comprises aluminium, aluminium alloy, copper, copper alloy, silver and silver alloy and/or the appropriate combination of one or more said second materials.
So, have the processing module separately and the micro-reactor system of heat exchange module through providing, to its certain responsibilities, promptly carry out this chemical reaction or control treatment temperature, each said module of optimization becomes possibility.
Advantageously, independent module is provided respectively, allows element standardization this micro-reactor system to this chemical reaction processing and the control of this temperature.Therefore, have different residence times for differential responses provide, different fluid volume, the different different micro-reactor system that shifts heats or the like become possibility.For example, the heat exchange module with the more major path that is used to hold heat-exchange fluid is provided, allows to same processing module supply or remove more heats.
This first material is rigidity relatively, and this second material compares flexible.Preferably, be used for second material reversible ground (promptly flexibly) or residual (remainingly) (being plasticity) distortion under pressure of the flexible of this heat exchange module.With heat exchange module be pressed in adjacent, by on the processing module of processing as comparison rigidity first materials such as stainless steels, the contact-making surface of this heat exchange module is out of shape a little, thereby does not need extra sealing between processing module and the heat exchange module.
Compare with traditional microreactor (wherein in order to provide good heat transfer process fluid and the wall thickness between the heat-exchange fluid to reduce as far as possible),, independently processing module and heat exchange module are provided according to the present invention.Although this has increased the distance (before this, this is considered to disadvantageous) between reacting fluid and the heat-exchange fluid, owing to the certain responsibilities about them makes these standalone module optimizations, can reach better processing and temperature control surprisingly.
Each processing module is sandwiched between two heat exchange modules, and each heat exchange module that is not placed on the end of this microreactor is sandwiched between two processing modules.Heat exchange module in this micro-reactor system end can be placed on respectively between first, second frame mounting and the processing module.
According to the preferred embodiment of this micro-reactor system, the said processing module of n at least comprises:
Mixing module, its at least one reacting fluid passage comprises the mixer that is used to receive and mix at least two kinds of reacting fluids; And alternatively
At least one thermal conditioning module is arranged on the upper reaches of said mixing module, is used for before getting into said mixing module, adjusting the temperature of said reacting fluid; And
At least one keeps module, is arranged on the downstream of this mixing module, is used to hold this reacting fluid mixture.
Use allows continuous reactions step is introduced more reacting fluids continuously more than a mixing module.At said mixing module; This reacting fluid mixes in the mixer of a part that constitutes this at least one reacting fluid passage; And leave after the said mixer, be accommodated in first the keeping in the volume an of part of this at least one reacting fluid passage of same formation.Said mixer can have the combination construction like plug flow mixing or reverse mixing, and the said first maintenance volume can comprise the straight passage of one or more cardinal principles that is connected by bend pipe.Preferably, provide maintenance to produce first of laminar flow and hold volume.
The temperature of the reacting fluid in this mixing module can quilt two the heat exchange module controls adjacent with said mixing module.There, heat or cold heat-exchange fluid be provided at these two heat exchange modules this at least one heat-exchange fluid passage in each, it is through heat transmission supply or remove the heat from this processing module.
As top pointed, before mixing two or more reacting fluids, said reacting fluid can be heated or cooled.In addition, one or more thermal conditioning modules can be provided at the upper reaches of said mixing module.Reacting fluid to be heated for each or cool off, said thermal conditioning module comprises at least one reacting fluid passage.When flowing through said reacting fluid passage, two heat exchange modules heating that each reacting fluid quilt is adjacent with said thermal conditioning module or cooling, similar before to the description of this mixing module.Through different channel volume is provided, heats discretely or cool off this different reactant and become possibility.
After leaving this mixing module, the reacting fluid of this mixing can be accommodated in one or more maintenance modules.There, the reacting fluid mixture that leaves this mixing module gets at least one the reacting fluid passage in this maintenance module, and said at least one the reacting fluid passage of flowing through leaves this maintenance module then.In said at least one the reacting fluid passage process of flowing through; With with mix the identical mode of description with heat exchange module about this before, said reacting fluid mixture can quilt two heat exchange modules heating, cooling or the heat adjacent with each holding module cushion.The difference of (differenctly formed) the reacting fluid passage that has difformity through providing keeps module, obtains the different conservation conditions possibility that becomes.It also is possible that two or more maintenance modules that are connected with each other are provided; Each keeps module to be sandwiched between the heat exchange module; Thereby under this condition, can obtain big maintenance volume and (depend on flow velocity) thus to obtain the big retention time (residence time), especially the temperature of this reacting fluid mixture can be controlled in residence time easily and accurately.
Preferably, this processing module be used to hold and guide the reacting fluid passage of reacting fluid to comprise flat passage (flat channel).Ideally, this flow path of microreactor is narrow pipe, and its diameter is usually less than 1mm.Yet, stratiform non-turbulent flow if desired, this flow velocity is limited by said small bore (section).In order to increase flow velocity, a plurality of so narrow pipes can be provided.But there, the stoichiometry in all pipes must be controllable, and for all pipes, this residence time must be controlled to be identical, and this can not extremely guarantee in the system of reality.
As preferred embodiment propose should flat passage, be equivalent to the combination of parallel pipe.Therefore flow velocity can be enlarged markedly, and keeps the stratiform non-turbulent flow simultaneously.
The result proves that the ratio of width to height was suitable for bringing forth good fruit in the scope at 1: 4 to 1: 50.Preferably, said wide/height ratio is set in 1: 4 to 1: 30 scope.More preferably, said wide/height ratio is set in 1: 5 to 1: 25 scope.In an exemplary embodiment, width, the height of 10mm and the length of 1844mm for this flat channel selecting 2.0mm produce wide/height ratio of 1: 5.In a further embodiment, be chosen as 1.4mm, 0.9mm and 0.5mm respectively, produce the wide/height ratio of 1: 7.14,1: 11.11 and 1: 20 respectively through the width that detects.
Because the processing fluid major part in the minute widths of this passage, single tube can be kept laminar flow, and this flow velocity (handling the volume of fluid in the unit interval) increases simultaneously.And, in the preferred embodiment, only must control the stoichiometry in the single volume.
For before indicate, promptly have the passage of 2.0mm, 1.4mm, 0.9mm and 0.5mm width respectively, recorded that residence time was respectively 5.7,10.2,15.9 and 22.6 seconds under the flow velocity of 100ml/min.Can know that from above-mentioned measurement the little reaction for specific combines through the different module that will have different residence times, almost can select this residence time arbitrarily.Especially can obtain nearly 30 minutes residence time, or preferably reach 20 minutes, more preferably reach 10 minutes.
In a preferred embodiment, this micro-reactor system comprises the processing module of at least two series connection, and each is sandwiched between two adjacent heat exchange modules.For example, one or more mixing modules can with the thermal conditioning module combinations before at least one, be used for before mixing, this reacting fluid being transferred to optimum temperature, and/or at least one keeps module, be used to this reacting fluid mixture required residence time be provided.During mixing and keeping, this adjacent heat exchange module control of module mixed and kept to the temperature of this reacting fluid mixture can by quilt with each.Alternatively, the auxiliary mixing module of the thermal conditioning module before having can be combined in two and keep between the modules, with through supplying with the carrying out that further reacting fluid allows subsequent reactions.
The reacting fluid passage of two processing modules subsequently can outsidely connect.There, can use outside dismountable or be fixedly coupled device (coupling) like pipe, accessory etc.Especially, pipe can be soldered or melting welding to these modules, perhaps can use swagelok snap joint connector.Although dismountable aerial lug can be reused individual module easily and therefore improved flexibility, fixing pipe has advantageously been avoided dead space volume (dead volume) and can have been increased the stability of whole micro-reactor system extraly.
Preferably; At least one heat-exchange fluid passage of in heat exchange module this comprises at least one heat-exchange fluid inlet port; It is connected with at least one heat-exchange fluid interface channel that the first heat-exchange fluid holder perhaps provides in adjacent processing module; And at least one heat-exchange fluid outlet, it is connected with the second heat-exchange fluid holder or the heat-exchange fluid interface channel that in adjacent processing module, provides.Therefore, two heat exchange modules a processing module is clipped in the middle can be connected with each other logical through this at least one the heat-exchange fluid interface channel that is provided in this processing module.Advantageously, between said two heat exchange modules, do not need extra heat-exchange fluid connector.
If said heat exchange module is processed by the material of flexible; And be compressed against on this processing module; Because the slight plasticity or the strain of the contact-making surface of this heat exchange module, do not need extra sealing at the interface place of this at least one heat-exchange fluid interface channel of the processing module through connecting two adjacent heat exchange modules.Yet; In a further advantageous embodiment; Interface place at heat-exchange fluid inlet port and/or heat-exchange fluid outlet; Extra seal can be provided, and auxiliary seal is somebody's turn to do the heat-exchange fluid connector interface between two continuous heat exchange modules, and it passes the heat exchange module that this is clipped in the middle via this at least one heat-exchange fluid interface channel.Such sealing preferably can be lip ring.Especially, the rigid seal processed such as its special teflon of can serving as reasons.Because this heat exchange module is processed by the material of flexible, it is possible using rigid seal, avoids the use of elastic sealing element such as the rubber or the silicon etc. that possibly become fragile like this.
This of heat exchange module at least one hold the heat-exchange fluid passage of this heat-exchange fluid can be for producing (height) turbulent flow of said heat-exchange fluid, this helps increasing the heat transmission from heat exchange module to this adjacent processing module.Preferably, realize that Reynolds number is equal to or greater than 2600.
In a preferred embodiment, through first dull and stereotyped being connected to each other with second flat board processed processing module.At the contact-making surface of said first and second flat boards, can be provided for holding this at least one reacting fluid passage of at least one reacting fluid through modes such as milling, etchings.Preferably, said at least one reacting fluid passage is a micro-structural.Through solder, solder brazing, sintering, melting welding, bonding etc. said first and second flat boards are connected to each other after; Except this at least one reacting fluid inlet port and this at least one reacting fluid outlet, this at least one the reacting fluid passage that is used to hold this reacting fluid is wrapped in this processing module fully.
Through be provided for holding at least one heat-exchange fluid passage of at least one heat-exchange fluid at first and second one or two dull and stereotyped contact-making surfaces; Heat exchange module can be processed similarly, first and second dull and stereotyped the linking together through solder, melting welding etc. afterwards.Perhaps, middle flat board can be sandwiched between said first and second flat boards, and said middle flat board comprises one or more cuttings (cut-out).After said first, middle and second flat board be connected to each other, said cutting defined at least one the heat-exchange fluid passage that is used to hold at least one heat-exchange fluid with the corresponding surfaces of said first and second flat boards.
The processing module that externally connects and the combination of the heat exchange module that is connected in inside provide the preferred plan that is used for this at least one reacting fluid loop and this at least one heat exchange flow body loop are separated and avoid cross pollution.
In a preferred embodiment, through at least the first and second frame mountings, the storehouse of processing module and heat exchange module is pressed each other.There, through one or more pulling force anchors or pull bar, said first and second frame mountings can be drawn toward each other, thus this processing module and heat exchange module are pressed between two frame mountings each other.
In a preferred embodiment, each said frame mounting comprises inside and outside framework alternatively.In further preferred embodiment according to Figure 17; A frame mounting is made up of structural detail; And second frame mounting form by outside and inner frame; Wherein this first frame mounting directly is anchored on this external frame through pull bar, and said external frame is pushed against said inner frame this first frame mounting and is positioned on the middle module stack.
Can said pull bar be provided at the center and/or the edge of this micro-reactor system.So, said modularization micro-reactor system can easily be assembled into the module with different numbers.
Advantageously, cavity (cavity) is provided in the central area of this first and second frame mounting, thus promote said first and second frame mountings each other near the time, the circumferential section of these modules obtains higher pressure.This helps increasing the sealing characteristics of this microreactor.
In most preferred embodiment, a heat exchange module serves as the adjacent modules of two continuous processing modules,, in this micro-reactor system, heat exchange module and processing module is provided in an alternating manner that is.Advantageously, this storehouse starts from and ends at heat exchange module.If two Continuous Heat Switching Modules interconnect through the heat-exchange fluid interface channel that is provided in to be clipped in the processing module therebetween; But with regard to the identical heat exchange module of utilization structure; Wherein each second module is rotated (the rich longitudinal axis 180 degree rotations of about 180 degree; If this heat-exchange fluid of supposition flows from right to left), thus this at least one outlet of this first heat exchange module, this at least one heat-exchange fluid interface channel and this at least one heat-exchange fluid inlet port of this second heat exchange module subsequently of being provided in this adjacent processing module are aligned with each other.
At least one heat-exchange fluid outlet of this of this at least one heat-exchange fluid inlet port of the heat exchange module that begins most of whole microprocessor system assembly and last heat exchange module; Can communicate with the first and second heat-exchange fluid holders respectively; Thereby this heat-exchange fluid flows to this second holder from this first holder; Vice versa, heats thus, cools off or hot this processing module that cushions this micro-reactor system.There, in abutting connection with this first with this first and second frame mounting of last heat exchange module in inlet port and outlet can be provided respectively.
At the heat exchange module that is positioned at this microreactor extra heat-exchange fluid inlet port and heat-exchange fluid outlet can be provided, its with the 3rd, heat-exchange fluid holder such as the fourth class communicates.So for example first heat-exchange fluid of heat can flow to the 3rd holder through the heat exchange module that is clipped in the middle this thermal conditioning module from this first holder, heat the reactant of the thermal conditioning module of flowing through thus.So, the second cold heat-exchange fluid can flow to this second holder through the heat exchange module that is clipped in the middle this maintenance module from the 4th holder, and cooling should be handled fluid in residence time thus.
As stated; In a preferred embodiment; Continuous heat exchange module is identical substantially; Wherein each second module is rotated about 180 degree, thereby this at least one heat-exchange fluid outlet of this first heat exchange module, this at least one heat-exchange fluid interface channel and this at least one heat-exchange fluid inlet port of this second adjacent heat exchange module of being provided in this adjacent processing module are communicated with each other.Therefore this heat-exchange fluid with the zigzag linear flow through this microreactor.The quantity that depends on processing module and heat exchange module for inlet port and outlet with whole microreactor adapt, is necessary to provide two heat exchange modules adjacent one another are.For fear of said two adjacent heat exchange modules, can they be separated through one blind (blind module) is set.Perhaps, for example, this second frame mounting (outlet of this microreactor can be provided in it) can be rotated about 180 degree (rich trunnion axis 180 degree rotations suppose that this heat-exchange fluid flows from right to left) and be complementary with the outlet with this last heat exchange module.Perhaps, for example, can use second frame mounting of (shifted) inlet port that has displacement.
Further purpose, advantage and characteristic can obtain from dependent claims and described embodiments of the invention.In addition:
Description of drawings
Fig. 1 shows that all accessories are at the stereogram of the micro-reactor system of a side according to one embodiment of the invention;
Fig. 2 shows the stereogram of this micro-reactor system Rotate 180 degree shown in Figure 1;
Fig. 3 shows the front cross sectional view of the thermal conditioning module of this micro-reactor system shown in Figure 1;
Fig. 4 shows this thermal conditioning module of seeing Fig. 3 from the left side;
Fig. 5 shows the front cross sectional view of the mixing module of this micro-reactor system shown in Figure 1;
Fig. 6 shows among Fig. 5 the enlarged drawing in the upper left corner that is designated " X ";
Fig. 7 shows the front cross sectional view of maintenance (the keeping retention) module of this micro-reactor system among Fig. 1;
Fig. 8 shows the vertical view cutaway drawing of seeing this mixing module of Fig. 7 from above;
Fig. 9 shows the enlarged drawing of the reacting fluid inlet port of this mixing module shown in Figure 8;
Figure 10 shows the front cross sectional view of another maintenance module of this microreactor among Fig. 1;
Figure 11 shows the vertical view cutaway drawing of seeing this mixing module of Figure 10 from above;
Figure 12 shows the enlarged drawing of reacting fluid inlet port of this mixing module of Figure 10;
Figure 13 shows the front cross sectional view of first heat exchange module;
Figure 14 shows the side sectional view of the heat exchange module of Figure 13;
Figure 15 shows the front cross sectional view of second heat exchange module;
Figure 16 shows the side sectional view of the heat exchange module of Figure 15; And
Figure 17 shows the vertical section of micro-reactor system according to an embodiment of the invention.
The specific embodiment
This micro-reactor system according to an embodiment of the invention; Like Fig. 1 and shown in Figure 2, comprise first frame mounting 10, first heat exchange module 7 in order, as the thermal conditioning module of processing module 1, second heat exchange module 8, mixing module 2, another first heat exchange module 7, the maintenance module 3 of regarding other processing module as, another second heat exchange module 8, other maintenance module 4,5 and 6 (each be sandwiched in two heat exchange modules 7 respectively, between 8) and second frame mounting 9 as another processing module.Like this, at said first and second frame mountings 10, first or second heat exchange module 7,8 and the processing module 1-6 alternately is provided between 9.
Can be clear that from Figure 14,16 each heat exchange module 7,8 comprises the first dull and stereotyped 7M, 8M respectively, middle dull and stereotyped 70, the 80 and second dull and stereotyped 7N, 8N, they connect together through solder.This centre flat board comprises the pattern of parallel straight channel form, and wherein two passages are connected by semi-ring in succession, so that form a continuous sinusoidal pattern.The said pattern of this centre dull and stereotyped 70,80 thus respectively and this inner surface of this first and second dull and stereotyped 7M, 7N and 8M, 8N limits heat- exchange fluid passage 7A, 8A is used to hold the heat-exchange fluid in this heat exchange module 7,8.End at this pattern; Through hole is formed at this first dull and stereotyped 7M, 8M; And at the relative end of this pattern; Another through hole is formed at this second dull and stereotyped 7N, 8N, thereby defines heat-exchange fluid inlet port 7B, 8B and heat-exchange fluid outlet 7C, 8C respectively, and they communicate with this heat- exchange fluid passage 7A, 8A.
Can find out that from Figure 13-16 this first and second heat exchange module 7,8 is identical substantially, wherein this second heat exchange module 8 is rotated about 180 degree.Like this; When assembling; The heat-exchange fluid inlet port 8B of the outlet 7C of first heat exchange module 7 and second heat exchange module 8 is aligned with each other, and the inlet port 7B of the heat-exchange fluid outlet 8C of this second heat exchange module 8 and next first heat exchange module 7 is also like this.
Can find out from Fig. 3,5,7 and 10; Each processing module 1-3,6 comprises two through hole 1H-3H, 6H; When assembling; One of them is corresponding with heat-exchange fluid inlet port 7B, 8B, and another heat-exchange fluid outlet 7C, 8C with first and second heat exchange modules 7,8 that are clipped in the middle said each processing module 1-3,6 is corresponding.Therefore; Can find out from Fig. 1,2 and 17; When assembling, be used for holding and guide in first heat exchange module 7 and the heat-exchange fluid passage 7A of the heat-exchange fluid in second heat exchange module 8,8A are communicated with through the heat-exchange fluid interface channel that is formed by the through hole that is clipped in one of processing module 1-6 between said first heat exchange module 7 and second heat exchange module 8 each other.
This heat-exchange fluid inlet port 7B of this heat exchange module that begins most 7 through the passage in the first connecting portion 12A that is provided at this first frame mounting 10 and is attached thereto, communicates with the first heat-exchange fluid holder (not shown).This heat-exchange fluid outlet 8C of this last heat exchange module 8 through the passage in the second connecting portion 12B that is provided at this second frame mounting 9 and is attached thereto, communicates with the second heat-exchange fluid holder (not shown).Like this; For example the heat-exchange fluid of temperature can the zigzag line, from this first holder, and 7,8 groups of first and second heat exchange modules, second framework 9 and the second connecting portion 12B that communicate through this first connecting portion 12A, this first framework 10, via the heat-exchange fluid interface channel that provides in the processing module 1-6 that is clipped in the middle of said first and second heat exchange modules 7,8; Flow into second holder; Thus, through the dull and stereotyped heat exchange of these modules, heat all processing module 1-6 subsequently.
Provide adjustment module 1 as first processing module, it shows in Fig. 3,4 more in detail.Said adjustment module 1 comprises the first reacting fluid passage 1A; It communicates with the first reacting fluid inlet port 1C and the first reacting fluid outlet 1F; And the second reacting fluid passage 1B, it communicates with the second reacting fluid inlet port 1D and the second reacting fluid outlet 1E.Through this first reacting fluid inlet port 1C, 1A supplies first reacting fluid to this first reacting fluid passage.Through this second reacting fluid inlet port 1D, supply second reacting fluid to this second reacting fluid passage.
Said adjustment module 1 comprises the first and second dull and stereotyped 1M, 1N (Fig. 4), and it is connected to each other through solder etc.Through etching, milling etc., in the contact-making surface of this first and/or second dull and stereotyped 1M, 1N, cut out sine-shaped reacting fluid passage 1A, 1B.
When flowing to the said first reacting fluid outlet 1F through the said first reacting fluid passage 1A, the temperature of said first reacting fluid is regulated by two heat exchange modules 7,8 that are clipped in the middle said adjustment module 1.There, this heat-exchange fluid of the said heat exchange module 7,8 of flowing through, rely on the heat exchange module of dull and stereotyped 1M through contacting said adjustment module, 1N dull and stereotyped 7N, 8M heat conduction supply or remove the heat of said first reacting fluid.
Mixing module 2 as second processing module is shown in Fig. 5,6.Although do not show in detail that said mixing module 2 comprises first and second flat boards, is similar to above-mentioned this adjustment module 1.In said mixing module, the reacting fluid passage 2A that comprises the mixer 2G and the first maintaining part 2I is provided.
The first reacting fluid inlet port 2C that communicates with said reacting fluid passage 2A is connected with this first reacting fluid outlet 1F of this adjustment module 1 through the joint outer part (not shown).The same second reacting fluid inlet port 2D that communicates with this reacting fluid passage 2A is connected with this second reacting fluid outlet 1E of this adjustment module 1 similarly.Like this, this first and second reacting fluid after said adjustment module 1, flows into the mixer 2G of the passage 2A that is positioned at this mixing module 2 respectively, and wherein said two kinds of reacting fluids are mixed with each other.Can suitably select the geometry of this mixer 2G, shown in the enlarged drawing of Fig. 6, be used for mixing this reacting fluid with best mode.After the mixing, resulting processing fluid flows into the first maintaining part 2I of this reacting fluid passage 2A, and this passage 2A is substantially shaped as flat passage, and the processing fluid of laminar flow substantially is provided thus.
The shape that the geometry that it is emphasized that this processing module and heat exchange module 1-6,7,8 passage is not limited to shown in the figure and describes about preferred embodiment, but can be chosen as any suitable design.
The mixing that is positioned at this mixer 2G and the first maintaining part 2I and resident during, two heat exchange modules, 7, the 8 control temperature that this chemical reaction can be clipped in the middle by this said mixing module 2.
This handles fluid, leaves this reacting fluid passage 2A through reacting fluid outlet 2E, gets into the reacting fluid inlet port 3C that first shown in Fig. 7-9 keeps module 3.There, this reacting fluid outlet 2E is connected through (not shown)s such as pipe are outside with reacting fluid inlet port 3C.This keeps module 3, as other keeps module 4-6, mainly comprises the first dull and stereotyped 3M-6M that is connected with the second dull and stereotyped 3N-6N through solder, melting welding etc.Between said two flat boards, provide passage 3A-6A to be used for during residence time, holding this processing fluid.There, sine-shaped basically flat passage is carved the contact-making surface that (carve) goes into this first and/or second flat board through quilts such as etching, millings.
When flowing through said reacting fluid passage 3A, this handles adjacent two heat exchange modules, 7, the 8 control temperature of fluid quilt and said maintenance module 3, as before to the description of this adjustment module 1 and mixing module 2.
After reacting fluid outlet 3D leaves this first maintenance module 3; This reacting fluid gets into maintenance module 4-6 subsequently via the reacting fluid inlet port separately that is connected with the reacting fluid outlet of previous maintenance module, as before to the description of this reacting fluid inlet port 3C and this reacting fluid outlet 2E.Like this, before leaving this micro-reactor system through the outlet 6D of this last processing module, this reacting fluid all maintenance module 4-6 subsequently that can flow through.
This residence time in each keeps module 3-6 keeps volume by this, and promptly the passage 3A-6A of this maintaining part (width * highly) * length defines divided by flow velocity.Thus, different widths, length and/or height through single passage is provided can obtain different residence times.So, combining through the different maintenance module that will have different channel geometries, this residence time almost can be selected arbitrarily.
Can find out from the contrast of Fig. 9 and 12; It shows this reacting fluid inlet port 3C, the 6C of this first and the 4th maintenance module 3 and 6 respectively; Limit the flat width of channel of this reacting fluid passage 3A, 6A respectively, can process the width that is equal to or greater than this reacting fluid inlet port less than (Fig. 9), substantially.
Like Fig. 1, shown in 2, two pull bars 13 to pushing away each other, are pressing this heat exchange module that piles up 7,8 and processing module 1-6 to support each other first and second frame mountings 10,9 thus.Pull bar 13 is placed on the circumference (circumference) of this micro-reactor system; And the centre of surface at this frame mounting 10,9 that contacts with this heat exchange module 7,8 provides cavity to see Figure 17), can obtain elevated pressures at the circumference of this micro-reactor system.Therefore; This heat-exchange fluid inlet port 7B, 8B and the heat-exchange fluid outlet 7C of this heat exchange module 7,8,8C; It is provided at the circumference of this micro-reactor system equally, is pressed against the heat-exchange fluid interface channel 1H-6H that is positioned at this processing module 1-6 with elevated pressures.If this heat exchange module 7,8 is processed by toughness material such as aluminium, copper or its alloy, the perimeter edge of this inlet port and outlet can be out of shape under pressure a little, to the surface that is clipped in this processing module 1-6 therebetween good sealing is provided thus.Like this, the heat-exchange fluid outlet 7C of two heat exchange modules 7,8 subsequently, 8C and heat-exchange fluid inlet port 7B, 8B via this heat-exchange fluid interface channel 1H-6H in the processing module that is provided at this centre not the leakage current body communicate.
In addition, can provide around the sealing ring (sealing ring) of this heat-exchange fluid inlet port 7B, 8B and heat-exchange fluid outlet 7C, 8C.There, for example in this first and second dull and stereotyped 7M, 7N, 8M, 8N, cannelure can be provided respectively, hold the sealing ring (not shown) within it.Such sealing ring can be processed by rubber, silicon or special teflon (preferably) etc.
Description as from the front is understandable; According to micro-reactor system of the present invention owing to its modular construction provides high flexibility; And the different maintenance module that allows to have different hybrid channel geometries combines; Optional residence time is provided thus, especially Type B is reacted.Each said processing module 1-6 is by two adjacent heat exchange modules, 7,8 control temperature.Because heat is transmitted only by realizing that through this flat board 1M-8M of this heat exchange module 7,8 and processing module 1-6, the heat conduction of 1N-8N sealing etc. are dispensable.And, advantageously, can optimize this processing module 1-6 about this reactant that is contained in wherein, for example anticorrosive and/or pressure, and simultaneously, can optimize this heat exchange module that does not contact 7,8 about heat transmission and/or sealing characteristics with these reactants.
In the above-described embodiments; Heat exchange module 7,8 and processing module 1-6 be alternated each other, and this heat-exchange fluid is from first holder, through the first connecting portion 12A; Through all heat exchange modules 7,8, flow into second holder that is connected to the second connecting portion 12B with the zigzag line.Thus, the connector of all heat-exchange fluids of this heat exchange module 7,8 is provided at inside, has no extra connector.Advantageously, can use standardized processing module and heat exchange module, this make be easy to, modular mode assembles the different microreactors with different residence times etc. and becomes possibility.
In the above-described embodiments, adjustment module 1, mixing module 2 and four keep module 3-6 to combine in proper order with this.Yet any combination of these modules is possible.For example can provide more adjustment modules to be increased in the passage that wherein heats or cool off these reactants.Multistep is reacted suddenly, more polyhybird module can be provided.Can provide different maintenance module to realize required residence time.
In test sample, with like 100ml/ minute given flow velocity, the about 1844mm of passage length, channel height 10mm and the channel width 0.5-2mm of processing module, the residence time 6-22 second of having realized each module.Like this, can realize total residence time up to 30 minutes.
Unexpectedly, verified continuous processing module 1-6 continuous connects the not temperature control of this microreactor of appreciable impact.Because each processing module 1-6, especially each keeps module 3-6, can be controlled temperature (heating, cooling or heat buffering) from both sides very effectively, and reaction can be in this microreactor, in wide temperature range, carry out.Like the example among the said embodiment, preferably, heat exchange module 7,8 transmits heat from continuous processing module, perhaps with heat be passed to continuous processing module 1-6 (except begin most with last heat exchange module).
These reacting fluid passages in this processing module 1-6 form micro-structural through etching, milling or the like.Because this heat exchange module 7,8 is made respectively, they can be fabricated to and not have this micro-structural, reduce cost like this.In addition, because said heat exchange module 7,8 does not contact with these reactants, they do not need corrosion-resistant or high processing pressure, therefore allow to use material best concerning heat is transmitted.Especially can following material be used for heat exchange module.
Aluminium alloy AlMgSil (=EN AW-6082 or EN6082):
Figure GSB00000820814400191
On the contrary, this processing module 1-6 can be processed by following material, for example:

Claims (13)

1. micro-reactor system comprises following storehouse:
At least n processing module; Wherein n is equal to or greater than 1 integer, and each processing module is processed by first material of rigidity, and comprises at least one reacting fluid passage (1A, 1B, 2A, 3A, 6A); This reacting fluid passage passes said processing module; And between at least one reacting fluid inlet port (1C, 1D, 2C, 2D, 3C, 6C) and at least one reacting fluid outlet (1E, 1F, 2E, 3D, 6D), be used to hold and guide reacting fluid, wherein; Said at least two processing modules series connection is being arranged under the situation of two processing modules at least;
And n+1 heat exchange module at least; Each said heat exchange module is processed by second material of the flexible that is different from said first material, and comprises at least one heat-exchange fluid passage (7A, 8A), and it is inner that this heat-exchange fluid passage passes said heat exchange module; And between at least one heat-exchange fluid inlet port (7B, 8B) and at least one heat-exchange fluid outlet (7C, 8C); Be used to hold and guide heat-exchange fluid, wherein said n+1 at least heat exchange module series connection
Wherein each processing module is sandwiched between two adjacent heat exchange modules.
2. according to the micro-reactor system of claim 1, wherein
Anticorrosive and the pressure of said first material, and be selected from the group of forming by stainless steel, nickel-base alloy, tungsten, tantalum, titanium, pottery, graphite, and/or the appropriate combination of one or more said first materials; And
Second material is heat conduction, and is selected from the group of being made up of aluminium, aluminium alloy, copper, copper alloy, silver and silver alloy, and/or the combination of one or more said second materials.
3. according to the micro-reactor system of claim 1 or 2, the wherein said processing module of n at least comprises:
Mixing module (2), its at least one reacting fluid passage (2A) comprises the mixer (2G) that is used to hold and mix at least two kinds of reacting fluids;
Alternatively, thermal conditioning module (1) is located at said mixing module (2) upper reaches, is used for getting into said mixing module (2) before, regulates the temperature of said at least two kinds of reacting fluids; And
Alternatively, one or more maintenance modules (3-6) are located at the downstream of this mixing module (2), are used to hold this reacting fluid mixture.
4. according to the micro-reactor system of claim 1 or 2, wherein
Said at least one reacting fluid passage (1A, 1B, 2A, 3A, 6A) is the passage of putting down, and comprises crooked and/or straight part, and each reacting fluid can be flowed along crooked route, and said flat passage has the wide/height ratio in 1: 4 to 1: 50 scope.
5. according to the micro-reactor system of claim 1 or 2, wherein
Said at least one reacting fluid passage (1A, 1B, 2A, 3A, 6A) is the passage of putting down, and comprises crooked and/or straight part, and each reacting fluid can be flowed along crooked route, and said flat passage has the wide/height ratio in 1: 4 to 1: 30 scope.
6. according to the micro-reactor system of claim 1 or 2, wherein
Said at least one reacting fluid passage (1A, 1B, 2A, 3A, 6A) is the passage of putting down, and comprises crooked and/or straight part, and each reacting fluid can be flowed along crooked route, and said flat passage has the wide/height ratio in 1: 5 to 1: 25 scope.
7. according to the microreactor of claim 1 or 2, the wherein said processing module of n at least comprises the processing module of at least two outside series connection.
8. according to the micro-reactor system of claim 1 or 2, the wherein said heat exchange module of n+1 at least comprises:
First heat exchange module (7), its at least one heat-exchange fluid inlet port (7B, 8B) communicates with the first heat-exchange fluid holder, with and heat-exchange fluid outlet (7C, 8C) communicate with subsequently heat exchange module (8);
Second heat exchange module (8), its at least one heat-exchange fluid outlet (7C, 8C) communicates with the second heat-exchange fluid holder, with and heat-exchange fluid inlet port (7B, 8B) communicate with the heat exchange module (7) of front; And alternatively
The heat exchange module that at least one is other is located between said first heat exchange module (7) and second heat exchange module (8), and connects with this first heat exchange module (7) and second heat exchange module (8);
Wherein the series connection of two continuous heat exchange modules realizes in inside through at least one heat-exchange fluid interface channel (1H, 2H, 3H, 6H), and this heat-exchange fluid passage is through this each of n processing module that is clipped in the middle by two continuous heat exchange modules at least.
9. according to the micro-reactor system of claim 1 or 2; Each of wherein said processing module of n at least and/or the said heat exchange module of n+1 at least comprises permanent each other first flat board (1M-8M) and second flat board (1N-8N) that connects, and each of wherein said reacting fluid passage, heat-exchange fluid passage, reacting fluid inlet port and reacting fluid outlet and/or heat-exchange fluid inlet port and heat-exchange fluid outlet (1A, 1B, 1C-1F, 2A, 2C-2E, 2G, 3A, 3C, 3D, 6A, 6C, 6D, 7A, 8A) is positioned between said first flat board (1M-8M) and second flat board (1M-8M).
10. according to the micro-reactor system of claim 9, wherein said first flat board (1M-8M) forever is connected through solder, solder brazing, melting welding, bonding making each other with second flat board (1N-8N).
11. according to the micro-reactor system of claim 9, each of wherein said reacting fluid passage, heat-exchange fluid passage, reacting fluid inlet port and reacting fluid outlet and/or heat-exchange fluid inlet port and heat-exchange fluid outlet (1A, 1B, 1C-1F, 2A, 2C-2E, 2G, 3A, 3C, 3D, 6A, 6C, 6D, 7A, 8A) is to obtain through the inner surface of at least one in ablate said first flat board (1M-8M) and second flat board (1N-8N).
12. according to the micro-reactor system of claim 9, wherein structurized in the middle of dull and stereotyped (70,80) be sandwiched between said first flat board and second flat board of the said heat exchange module of n+1 at least so that said heat-exchange fluid passage (7A, 8A) to be provided.
13. the micro-reactor system according to claim 1 or 2 further comprises:
First frame mounting (10); And
Second frame mounting (9),
Wherein said processing module of n at least and the said heat exchange module of n+1 are at least pressed by said first and second frame mountings (9,10) each other.
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