CN101634649B - Parallel reactor system and sample research method thereof - Google Patents
Parallel reactor system and sample research method thereof Download PDFInfo
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- CN101634649B CN101634649B CN2008101884682A CN200810188468A CN101634649B CN 101634649 B CN101634649 B CN 101634649B CN 2008101884682 A CN2008101884682 A CN 2008101884682A CN 200810188468 A CN200810188468 A CN 200810188468A CN 101634649 B CN101634649 B CN 101634649B
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Abstract
The invention provides a parallel reactor system, which comprises an access control system, a plurality of reactor modules (at least two) and a temperature control device. Each reactor module is internally provided with a reactor, and at least one reactor module is internally provided with at least two reactors; each reactor module is provided with the temperature control device for leading the reactors therein at the same temperature; the inlet control system is provided with at least two materials inlets for respectively receiving the materials output by at least two material sources as well as a plurality of materials outlets which can be divided into a plurality of material outlet groups for corresponding to the reactor modules, and the material outlet in each group is respectively connected with the inlet of the reactor in the reactor module corresponding to the group; the output material of one material outlet of at least one group in the material outlet groups is different from that of the other material outlets in the same group, and at least two material outlets in different groups can output the same material.
Description
[technical field]
The present invention relates to a kind of reactor assembly and sample study method thereof, especially a kind of high flux parallel reactor system and the method that sample is studied.
[background technology]
In recent years, along with the development of technology, many have premium properties and widely used new material constantly is developed.The exploitation of understanding in depth not only material to the new material performance has very big benefit, and production application of material etc. is had better guide significance.
Along with the application of combinational chemistry in investigation of materials, the researcher can prepare the wide variety of materials sample simultaneously.Use traditional research method to study need to prepare wide variety of materials, not only R﹠D costs can improve and also research institute take time also can be very long, be unfavorable for the research and development of material.Like this, be difficult in than in the short time performance of a large amount of samples being studied with traditional research method.
Therefore, a kind of new research method of needs and system are used for studying simultaneously or prepare the wide variety of materials sample to solve the deficiencies in the prior art.
[summary of the invention]
The object of the present invention is to provide a kind of high flux parallel reactor system and sample study method thereof.
The invention provides a kind of parallel reactor system, it comprises inlet control system, a n reactor module (n 〉=2) and temperature control equipment.Be provided with reactor in each reactor module, each reactor all offers inlet and outlet, but sample loading in it, and having at least in the reactor module in the described n reactor module is provided with at least two reactors.Be provided with a temperature control equipment on each reactor module so that the reactor in it has a common temperature.Described inlet control system is provided with at least two material inlets in order to receive the material of at least two material source outputs respectively.Described inlet control system also is provided with a plurality of material outlets, and this material outlet can be divided into n material outlet group with the corresponding described n reactor module of difference, and every group material outlet joins with the inlet that this organizes the reactor in the pairing reactor module respectively.The material component that has at least a material outlet in a group to export in described n material outlet group is different from the material component that another material outlet is exported in this group, and its material component of being exported of the material outlet in same group is not identical to have two at least.
The invention still further relates to a kind of sample study method, it includes following steps: the mass transport that will come from least two material sources is to a plurality of material outlets, described a plurality of material outlet constitutes n material outlet group (n 〉=2), the material component that has at least a material outlet in a group to export in described n material outlet group is different from the material component that another material outlet is exported in this group, and the component of its material of being exported of material outlet in same group is not identical to have two at least; The material that described n material outlet group (n 〉=2) exported is input to the reactor module that is provided with reactor in n, every material outlet group is a corresponding reactor module respectively, and every group material outlet joins with the inlet that this organizes the reactor in the pairing reactor module respectively; The temperature of controlling each reactor module makes the reactor in it have a common temperature.
The invention still further relates to a kind of sample study method, it includes following steps: establish the reactor module (n 〉=2) of reactor in corresponding n, at least two kinds of materials are distributed into n group streams; Described n group streams correspondence is transported in the described n reactor module, make each streams in each group be transported to respectively in each reactor of a corresponding reactor module of this group, and make that to be transported at least two materials from the reactor of different reactor module identical, be transported to the material difference at least two reactors at least one reactor module; Control the temperature of a described n reactor module, make that the reactor in each reactor module is in essentially identical temperature, and at least two different reactor modules are in different temperature.
Like this, parallel reactor of the present invention system just can study the sample in the reactor in a plurality of reactor modules under different conditions simultaneously.
[description of drawings]
Fig. 1 is the configuration diagram of parallel reactor of the present invention system.
Fig. 2 is the synoptic diagram of a reactor module in the parallel reactor system shown in Figure 1.
Fig. 3 is the synoptic diagram of an embodiment of parallel reactor of the present invention system.
Fig. 4 is the synoptic diagram of another embodiment of parallel reactor of the present invention system.
Fig. 5 is a kind of combination synoptic diagram of reaction conditions among the embodiment shown in Figure 4.
Fig. 6 is a kind of synoptic diagram that catalyst type distributes in the reaction conditions shown in Figure 5.
Fig. 7 is the another kind of synoptic diagram that catalyst type in the reaction conditions distributes among the embodiment shown in Figure 5.
Fig. 8 is another synoptic diagram that catalyst type in the reaction conditions distributes among the embodiment shown in Figure 5.
Fig. 9 is the synoptic diagram of reaction conditions among the embodiment of parallel reactor of the present invention system.
Figure 10 is the synoptic diagram of an embodiment of parallel reactor of the present invention system.
Figure 11 is a kind of combination synoptic diagram of reaction conditions among the embodiment shown in Figure 10.
Figure 12 is the synoptic diagram of another embodiment of parallel reactor of the present invention system.
Figure 13 is another synoptic diagram of a reaction module of parallel reactor of the present invention system.
Figure 14 is the synoptic diagram of an embodiment of parallel reactor of the present invention system.
[embodiment]
In high flux parallel reactor of the present invention system, it can measure the characteristic of the sample in the reactor in a plurality of reactor modules simultaneously under the combination of differential responses condition.Described reaction conditions comprises temperature (Temperature, T), pressure (Pressure, P), air speed (Space Velocity, SV), feed composition (FeedComposition, FC), sample particle size (Particle Size, PS), the raw material mixture ratio (Feed Ratio, FR), the kind of sample dilution ratio and sample etc.Like this, the combination of different reaction conditions just includes but not limited to following kind, such as: 1. the various combination of reaction conditions in the kind of temperature, pressure, air speed, feed composition, sample particle size, raw material mixture ratio, sample dilution ratio and sample etc. and two reaction conditionss of another one reaction conditions composition; 2. the various combination of three reaction conditionss forming of a reaction conditions in the kind of temperature, pressure, air speed, feed composition, sample particle size, raw material mixture ratio, sample dilution ratio and sample etc. and two other reaction conditions; 3. the various combination of four reaction conditionss forming of a reaction conditions in the kind of temperature, pressure, air speed, feed composition, sample particle size, raw material mixture ratio, sample dilution ratio and sample etc. and other three reaction conditionss; 4. the various combination of five reaction conditionss forming of a reaction conditions in the kind of temperature, pressure, air speed, feed composition, sample particle size, raw material mixture ratio, sample dilution ratio and sample etc. and other four reaction conditionss; 5. the various combination of six reaction conditionss forming of a reaction conditions in the kind of temperature, pressure, air speed, feed composition, sample particle size, raw material mixture ratio, sample dilution ratio and sample etc. and other five reaction conditionss; Or the various combination of seven reaction conditionss forming of a reaction conditions in the kind of 6. temperature, pressure, air speed, feed composition, sample particle size, raw material mixture ratio, sample dilution ratio and sample etc. and other six reaction conditionss etc.Certainly, reaction conditions just has more combination more at most.Like this, just can determine the response of sample under the differential responses condition fast, and from then on obtain process conditions.In parallel reactor of the present invention system, described sample can be catalyzer.
As shown in Figure 1, it is a configuration diagram of parallel reactor of the present invention system.It comprises material origin system 200, inlet control system 201, reactor module system 202 and control of export system 203.Described material origin system 200 links to each other with described inlet control system 201; Described inlet control system 201 comprises that material distribution device or material distribute and material controlling device enters in the reactor of correspondence in the reactor module system 202 after making material by inlet control system 201; The outlet of reactor can link to each other with control of export system 203.In embodiments of the present invention, described reactor module system 202 comprises n reactor module M1 to Mn, and wherein n is more than or equal to 2.On each reactor module, be respectively arranged with a temperature control equipment 204 so that the reactor in it has a common temperature; Described a plurality of temperature control equipment can be identical also can be inequality.Include one or more in sampling apparatus, pressure control device, gathering-device or the circulating device etc. in the described control of export system 203.
As shown in Figure 2, it is provided with reactor R for the synoptic diagram of a reactor module Mi in the parallel reactor of the present invention system in it.In n reactor module of the embodiment of the invention, have at least in the reactor module to be provided with at least 2 reactors, can be provided with at least 1 reactor in other reactor modules.Described reactor is provided with outlet and inlet, and is mounted with sample in it.Described sampling apparatus, as sampling valve, can sample to the draw-off of each reactor outlet is used for analyzing.Described pressure control device is used for the pressure in the controlling reactor; Described gathering-device can be used for the draw-off of reactor is collected.This pressure control device or gathering-device can comprise following framework: 1) each reactor is provided with a pressure control device or gathering-device; 2) reactor module is provided with a common pressure control device or gathering-device; 3) reactor module is provided with more than one pressure control device or gathering-device; 4) pressure control device or gathering-device are controlled the pressure of the reactor in the different reactor module or the collection of draw-off simultaneously, at this moment, the reactor of this pressure control device or gathering-device control all is to come from different reactor modules, more than one reactor is perhaps arranged from identical reactor module; 5) combination of above four kinds of situations.In one embodiment of the invention, the reactor in each reactor module has identical pressure.Described circulating device can be input to the circulation of the draw-off of certain or some reactors in the material source or the porch of reactor.The draw-off of described reactor can be handled through tripping device or through other devices earlier before being recycled input.
In embodiments of the present invention, described inlet control system is provided with the material that at least two material inlets 205 receive at least two material source outputs respectively, this inlet control system also is provided with a plurality of material outlets 206 to form a n material outlet group corresponding described n reactor module respectively, and each material outlet group is joined with the inlet that this organizes the reactor in the pairing reactor module respectively.By described inlet control system, have at least the component of the material that a material outlet in a group exports to be different from the composition of the material that another material outlet is exported in this group in described n material outlet group, and the component of its material of being exported of material outlet in same group is not identical to have two in the n group material outlet at least.The quantity of material outlet can be one or morely in the described material outlet group, and it is relevant with the quantity of reactor in the reactor module.Described material component difference comprises that described material is to be made up of different materials respectively, or described material is made up of identical material respectively, but the component in each material has different ratio etc.
As shown in Figure 3, it is an embodiment of parallel reactor of the present invention system.In this embodiment, described material origin system comprises two material sources 10 and 11; Described inlet control system 201 comprises two material controlling devices, as mass flow control appts (Mass Flow Controller, MFC) 101 and 102 and two material distribution device 103 and 104.Described reactor module system comprise parallel reactor module M1 and with parallel reactor module M1 parallel reactor module M2 separated from one another.Be provided with two reactor R1-1 and R1-2 among the described reactor module M1.Be provided with a reactor R2-1 in the described second parallel reactor module.Reactor R1-1, R1-2 and R2-1 are provided with corresponding entrance and exit, all are mounted with the catalyzer sample in it.Reactor module M1 is provided with a common temperature control equipment 20 so that reactor R1-1 and R1-2 have common temperature T 1.The second reactor module M2 also is provided with a temperature control equipment 21 so that reactor R2-1 has temperature T 2.Under different reaction bars, T1 and T2 can be identical or different.In the present embodiment, described reactor is reaction tube.Can supply raw materials in described material source 10 and 11, such as the fresh reactant thing, and from the draw-off of other reactors, the material that can in it, import from described reactor inlet that some pollutant or other are relevant.Described material source 10 links to each other with 102 inlet with mass flow control appts 101 respectively with 11. Material distribution device 103 and 104 inlet link to each other with 102 outlet with mass flow control appts 101 respectively.The outlet of material distribution device 103 respectively with module M1 and module M2 in reactor R1-1 and the inlet of R2-1 link to each other.The inlet of the second reactor R1-2 among the outlet of material distribution device 104 and the module M1 links to each other.Like this, the material from material source 10 just enters in the different reactor module reactors respectively.At this moment, three material outlets that material distribution device 103 and 104 is provided with are divided into respectively corresponding described two reactor modules of two material outlet groups, and each material outlet group is joined with the inlet that this organizes the reactor in the pairing reactor module respectively.In the present embodiment, material source 10 is different with 11 material components that provided.Like this, R1-1 is different with the material component that R1-2 is transfused to for reactor module M1 internal reaction device, and the reactor R1-1 in the module M1 is identical with the material component that the interior R2-1 of module M2 is transfused to.In embodiments of the present invention, also the flow that flowmeter is used for detecting each volume control device can be set in the mass flow control appts exit.
Described reactor R1-1, the outlet of R1-2 and R2-1 can be directly and next equipment, links to each other as product collector or next stage reactor.In addition, also can be respectively arranged with sampling valve 110,111 and 120 at each reactor exit.Sampling valve 110,111 and 120 are respectively arranged with opening 113,114 and 123 be used for to the draw-off of respective reaction device sample and with analytical equipment such as gas chromatograph (Gas Chromatography, GC) and/or the mass chromatography instrument (Mass Spectrum MS) waits and links to each other.Certainly, as previously mentioned, also pressure control device or material circulation device can be set in the exit of reactor.
In the present embodiment, the material source is at least two, among the module M1 at least two reactors can be set, and also two or more reactors can be set among the module M2.As shown in Figure 4, it is another embodiment synoptic diagram of parallel reactor of the present invention system.This embodiment and shown in Figure 3 roughly the same.Difference is to be provided with among the reactor module M2 two reactor R2-1 and R2-2.Temperature control equipment 21 makes reactor R2-1 and R2-2 have a common temperature T 2.The outlet of reactor R2-2 can be directly and next equipment, links to each other as product collector or next stage reactor.In addition, also can be respectively arranged with sampling valve 121 at each reactor exit, it is provided with opening 124 and is used for the draw-off of reactor is sampled and linked to each other with analytical equipment such as GC and/or MS etc.At this moment, 4 material outlets that material distribution device 103 and 104 is provided with are divided into respectively corresponding described two reactor modules of two material outlet groups, and each material outlet group is joined with the inlet that this organizes the reactor in the pairing reactor module respectively.Material source 10 is different with 11 material components that provided.Like this, reactor R1-1 is different with the material component that R1-2 is transfused among the reactor module M1; Reactor R2-1 among the module M2 is also different with the material component that R2-2 is transfused to.Reactor R1-1 in the module M1 is identical with the material component that the interior reactor R2-1 of module M2 is transfused to; Reactor R1-2 in the module M1 is identical with the material component that the interior reactor R2-2 of module M2 is transfused to.
With reactor assembly shown in Figure 4 is example, and it can be studied Catalytic processes under different reaction conditions combinations.With the example that is combined as of air speed and temperature, certainly, it also can be the various combination of other reaction conditionss.The air speed of mass flow control appts 101 control raw materials 10 is SV1, and the air speed of mass flow control appts 102 control raw materials 11 is SV2.As shown in Figure 5, in one embodiment, suppose that SV1 and SV2 and T1 and T2 are all differing from each other.Like this,, just can study in identical temperature for the reactor in the same module, under different air speeds and the different feed composition, the characteristic of the sample in the reactor; For the reactor in the different modules, as reactor R1-1 and R2-1, just can study in identical air speed, under identical feed composition and the different temperature, the characteristic of sample in the reactor; Perhaps for reactor,, just can study under different temperature, different air speed and equal material component the characteristic of the sample in the reactor as R1-1 and R2-2.
At different research demands, the reaction conditionss such as kind of air speed, pressure, feed composition, sample particle size, raw material mixture ratio, sample dilution ratio and sample can have different combinations.Such as, when the kind that need under different air speeds and temperature, study catalyzer during, just can take the combination of different reaction conditionss to the influencing of Catalytic processes.Be example still with reactive system shown in Figure 4, shown in Fig. 6-8, in Fig. 6, reactor R1-1, R1-2 is mounted with the catalyzer C1 of identical type among R2-1 and the R2-2; In Fig. 7, the catalyzer in reactor R1-1 and the R2-1 is C1, and the catalyzer in reactor R1-2 and the R2-2 is C2; Perhaps in Fig. 8, the catalyzer among reactor R1-1 and the R2-2 is C1, and the catalyzer among reactor R1-2 and the R2-1 is C2.Wherein, C1 is different from C2.Like this, just can compare, and then obtain needed information the characteristic of the reactor sample of same module and the characteristic of the reactor sample between disparate modules.Such as in Fig. 8,, just can study under identical temperature the characteristic of different types of catalyzer under different air speeds and different feed composition for the reactor in the same reactor module.Simultaneously, the reactor concerning between disparate modules, just can study under identical air speed, different catalyzer under different temperature and identical feed composition characteristic or identical catalyzer in different air speeds, characteristic under different temperature and the different feed composition etc.In different research needs, reactor R1-1, R1-2, the catalyst type among R2-1 and the R2-2 also can be differing from each other.SV1 and SV2 and T1 and T2 also can be mutually the same.
Because the reactor in each reactor module can reach more than two, at this moment, for a reactant source, it is by the identical material of the input of the different reactor in a module simultaneously just behind a corresponding mass flow control appts and the distributor.In embodiments of the present invention, owing to have two different material sources at least, so such as when having three material sources, described parallel reactor system still can have two reactor modules, than as shown in Figure 3-4.Certainly, each reactor module also can comprise the reactor of other quantity, such as being three.At this moment, the distributor that described parallel reactor system just has three material sources, three corresponding mass volume control devices and three correspondences, distributor link to each other with different reactor in two modules respectively.As shown in Figure 9, just can under different condition combinations, study the sample properties in each reactor.
When needs are studied under more reaction conditions, but the quantity of the quantity of increment material source or reactor.As shown in figure 10, it is an embodiment of parallel reactor of the present invention system.In this embodiment, described parallel reactor system includes three material sources 10,11 and 12, three mass flow control appts 101,102 and 103, three distributors 104,105 and 106 and three reactor module M1, M2 and M3.Described reactor module M1 is respectively arranged with reactor R1-1, R1-2 and R1-3 among M2 and the M3, R2-1, R2-2 and R2-3 and R3-1, R3-2 and R3-3.Reactor is provided with corresponding entrance and exit, is mounted with the catalyzer sample in it.Described material source 10,11 links to each other with 103 inlet with mass flow control appts 101,102 respectively with 12.Distributor 104,105 links to each other with 103 outlet with mass flow control appts 101,102 respectively with 106.The outlet of distributor 104 respectively with module M1, M2 module M3 in reactor R1-1, R2-1 and the inlet of R3-1 link to each other.The outlet of distributor 105 respectively with module M1, M2 and M3 in reactor R1-2, R2-2 and the inlet of R3-2 link to each other.The outlet of distributor 106 respectively with module M1, M2 and M3 in reactor R1-3, R2-3 and the inlet of R3-3 link to each other.Have at least two different material components can be provided in described three material sources 10,11 and 12.
Wherein, the outlet of reactor can be directly and next equipment, links to each other as product collector or next stage reactor.In addition, also can be respectively arranged with sampling valve 110,111,112,120,121,122,130,131 and 132 at each reactor exit.Sampling valve 110,111,112,120,121,122,130,131 and 132 can be respectively arranged with opening 113,114, and 115,123,124,125,133,134 and 135 are used for the draw-off of respective reaction device is sampled.
Referring to shown in Figure 10, in the present embodiment, reactor module M1 is provided with a common temperature control equipment 20 so that reactor R1-1, R1-2 and R1-3 have common temperature T 1.Reactor module M2 also is provided with a common temperature control equipment 21 so that reactor R2-1, R2-2 and R2-3 have common temperature T 2.Reactor module M3 also is provided with a common temperature control equipment 22 so that reactor R3-1, R3-2 and R3-3 have common temperature T 3.In addition, in the present embodiment, reactor module M1, reactor module M2 and reactor module M3 can be respectively arranged with a pressure control device (not shown), have an identical pressure in order to the reactor of controlling respectively in it.Certainly, also can be provided with pressure control device to each reactor as required, be used for controlling separately the pressure of each reactor, perhaps same pressure control device links to each other with reactor in the different reactor module respectively.
In the present embodiment, still with the example that is combined as of air speed and temperature.As shown in figure 10, the air speed of mass flow control appts 101 control raw materials is SV1; The air speed of mass flow control appts 102 control raw materials is SV2; The air speed of mass flow control appts 103 control raw materials is SV3.Wherein, it is all inequality to suppose that SV1, SV2 and SV3 and T1, T2 and T3 can distinguish.Like this, as shown in figure 11, the reactor in each reactor module, just can study under the identical temperature conditions and the characteristic under the different air speeds.For the reactor between reactor module, just can study the characteristic under different temperature and the similar and different air speed.Certainly, under the combination of certain reaction condition, described air speed selection portion is as required divided identical or all identical.Described T1, T2 and T3 also can be mutually the same or part is identical.In addition, also can be under the reaction conditions of the various combination of the kind of temperature, pressure, air speed, feed composition, sample particle size, raw material mixture ratio, sample dilution ratio and sample the characteristic of research catalyzer.In addition, in an embodiment, the reactor in the reactor module also can be other quantity, and has two reactors in one of them module at least.
Like this, in concrete different application, just can be chosen in the characteristic that corresponding reaction conditions gets off to study Catalytic processes.
As shown in figure 12, it is an embodiment of high flux parallel reactor of the present invention system.In this embodiment, described parallel reactor system includes material source 10 and 11, a pair of mass flow control appts 101 and 102, a pair of distributor 103 and 104.Reactor module M1 and module M2.Described reactor module M1 comprises the first order module M1a and the second level module M1b of two-stage series connection at least.Described parallel reactor module M2 also comprises the first order module M2a and the second level module M2b of two-stage series connection at least.Be respectively arranged with reactor M1a-1 and M1a-2 and M2a-1 and M2a-2 among first order module M1a and the M2a.Be provided with reactor M1b-1 and M1b-2 and M2b-1 and M2b-2 among second level module M1b and the M2b.Each reactor is provided with corresponding entrance and exit, all is mounted with the catalyzer sample in it.The outlet of reactor M1a-1 and M1a-2 and M2a-1 and M2a-2 links to each other with the inlet of M1b-2 and M2b-1 and M2b-2 with reactor M1b-1 respectively, can be respectively arranged with corresponding sampling valve 110,111,120 and 121 therebetween.Described sampling valve 110,111,120 and 121 can offer opening 1100,1110 respectively, and 1200 and 1210 are used for the draw-off of reactor is sampled.Described reactor M1b-1 links to each other with next equipment respectively with the outlet of M1b-2 and M2b-1 and M2b-2.In addition, also can be respectively arranged with sampling valve 112,113,122 and 123 at each reactor M1b-1 and M1b-2 and 12b-1 and 12b-2 exit.Sampling valve 112,113,122 and 123 can be respectively arranged with opening 1120,1130, and 1220 and 1230 are used for the draw-off of second reactor is sampled.
In the present embodiment, from the material of material source 10 and 11 respectively through mass flow control appts 101 and 102 and distributor 103 and 104 after enter respectively in the reactor in first module 11 and second module 12.First order module M1a and second level module M1b can be respectively arranged with temperature control equipment 20a with 20b or be provided with a common temperature control equipment so that first order module M1a has identical temperature T 1 with second level module M1b.First order module M2a and second level module M2b also can be respectively arranged with temperature control equipment 21a with 21b or be provided with a common temperature control equipment so that first order module 12a has identical temperature T 2 with second level module 12b.Certainly, first order module M1a can be different with the temperature of second level module M1b.The temperature of first order module M2a and second level module M2b also can be different.So just can under different reaction conditionss, test the characteristic of the catalyzer in the reactor.
In embodiments of the present invention, material source and reactor module can all be at least two.Every grade of module also is provided with a pressure control device in order to difference control module internal pressure.Certainly, each reactor can be provided with pressure control device separately.Second level module internal reaction device quantity is identical with reactor quantity in the corresponding first order module, and like this, the reactor quantity in the reactor module just can be carried out respective change, and is certain, and two reactors will be arranged in the first order reactor module at least.
As shown in figure 13, it is another synoptic diagram of reactor module among the present invention.With reactor module Mi shown in Figure 2 is example, in it multiple lines and multiple rows reactor can be set, thereby form the array of a reactor.In addition, as shown in figure 14, it is an embodiment of parallel reactor of the present invention system.This embodiment and Figure 10 are close, and difference is to have only in the present embodiment two material sources 10 and 12.Material source 10 links to each other with two mass flow control appts simultaneously.Like this, for the reactor in the same reactor module, just have the reactor that receives identical material and exist.At this moment, just can carry out other research as required.In an embodiment of the present invention, as required, a material source also can connect two or more mass flow control appts simultaneously, and certainly, a mass flow control appts connects a distributor.In one embodiment of the invention, parallel reactor of the present invention system can include two material sources, four reactor modules that be arranged in parallel, four pressure control devices, four temperature control equipments, eight mass flow control appts and eight distributors.A material source connects four mass flow control appts.Reactor module of a pressure control device control is so that reactor wherein has identical pressure.Reactor module of temperature control equipment control so that reactor wherein have an identical temperature.Be provided with eight reactors in each module, it links to each other with eight distributors respectively.The pressure of described intermodule and temperature can be identical or different.Like this, study the characteristic of Catalytic processes by the reaction conditions of setting various combination.
In addition, in the present invention in one embodiment, be example with Fig. 4 or Figure 10, in the time will under identical material input condition, studying the characteristic of a large amount of Catalytic processes simultaneously, material source 10 and 11 or material source 10,11 with 12 the input materials identical, a common material source perhaps is set.So just satisfy specific demand.In addition, when having identical material source, the material that comes out from same distributor also can all enter in the reactor in the same reactor module, 36 passages and 128 channel parallel reactor assemblies such as the research and development of inferior Shen science and technology (Shanghai) research and development centre so also can carry out a large amount of research simultaneously.
In an embodiment of the present invention, the material outlet on the described material distribution device all is to link to each other with the inlet of different reactors, and under certain conditions, two or more material outlets also can link to each other with the inlet of same reactor.
In parallel reactor of the present invention system, each reactor module is provided with a common temperature control equipment.Like this, the manufacturing of reactor module just be easier to and easily the temperature of controlling reactor so that it all has identical temperature.In themopositive reaction, in Fischer-Tropsch synthesis, temperature control equipment can have various ways, as is circulating boiling water or fluidization sand-bath.In thermonegative reaction, in paraffin dehydrogenation or catalytic reforming reaction, temperature control equipment can be the fluidization sand-bath or it is provided with heating arrangement, as electric heater, in order to corresponding reactor module is heated so that reactor maintains the temperature of setting.
In addition, in parallel reactor of the present invention system, described reactor can comprise the isothermal piston flow reactor, so just can be used to simulate the characteristic of plant-scale catalyst reactor.Described piston flow reactor can comprise fixed bed reactors, trickle bed reactor or monolith honeycomb reactor.Simultaneously, described reactor can comprise laboratory scale piston flow reactor.Described laboratory scale piston flow reactor is meant the internal diameter of piston flow reactor less than 101.6mm (4 inches), preferably less than 50.5mm (2 inches), more preferably less than 25.4mm (1 inch).Its length is less than 2.4m (8 feet), preferably less than 1.2m (4 feet), more preferably less than 0.3m (1 foot); The charging capacity of catalyzer is less than 800 grams, preferably less than 400 grams, more preferably less than 25 grams.
High flux parallel reactor of the present invention system can be used to study the multifrequency nature of Catalytic processes, such as heat biography, matter biography, dynamics, efficiency factor, shape, pore structure, activity and the selectivity etc. of catalyzer, thus the combination of the reaction conditions that is optimized and preferred catalyzer sample.
With device synoptic diagram shown in Figure 4 is example.As needs research reactor R1-1, R1-2, when the heat of catalyzer passes characteristic among R2-1 or the R2-2, can along beds vertically, in beds, be provided with thermopair.When having only a thermopair that is arranged on its beds middle part in the reactor, be preferably the centre place that this thermopair is arranged on as close as possible beds.When being provided with two or three thermopairs that are arranged on its beds middle part in the reactor, be preferably these thermopairs successively along the length direction setting of beds.The heat that like this, just can obtain this catalyzer under different reaction conditionss passes characteristic.In parallel reactor of the present invention system, be preferably and in reactor, be provided with at least three thermopairs and measure temperature characterisitic in the beds, and this thermopair sets gradually along the length of beds.
When reactant is drawn with respect to the time corresponding to the concentration of reactants of continuous lengthwise position along beds during by beds.Like this, along resulting figure, the slope of its every bit is exactly system's reaction rate at that time.Draw the dynamic information that log-log graph just may obtain catalyzer to reaction rate with along the concentration of reactants of beds.
Reactor matter passes the acquisition of data, mostly is to test under isothermy, reacts under isothermy in order to ensure reactor, and available inert particle is diluted the beds in the reactor.Catalyst granules depends on multiple factor with the dilution proportion of particles, as the activity of reaction heat and catalyst granules etc.Like this, utilize reactor assembly of the present invention just can obtain the preferable inert particle and the dilution ratio of catalyst granules.
A kind of efficiency factor of catalyzer equals the ratio of macroreaction speed and its intrinsic reaction rate of this catalyzer.In the method for a simplification, often think that the catalyzer of crushing does not have matter to pass retardance, so its macroreaction speed just is considered to the intrinsic reaction rate of this catalyzer.Like this, just can in reactor R1-1 and R2-1, load the catalyzer of commercial size, in reactor R1-2 and R2-2, load the catalyzer of crushing of the same race.Like this, just can study variation of the catalyst efficiency factor under the efficiency factor of catalyzer under the uniform temp and the different temperatures etc.
Usually, the particle size of commercial size catalyzer is at the 1-5 millimeter.Crush or powder catalyst is often prepared by the catalyzer of commercial size, and its exemplary particles size is at the 0.10-0.20 millimeter, and certainly, its size under the condition that keeps catalytic performance is the smaller the better.Owing to have a less resistance to mass tranfer, crushing or powder catalyst often than the catalyst activity height of commercial size.So, reactor in order to ensure the catalyzer that is mounted with crushing can have the identical operations temperature with the allogeneic reaction utensil that is mounted with the commercial size catalyzer, in the reactor of the catalyzer that is mounted with crushing, the ratio of inertia dilution particle and catalyst granules is greater than the ratio in the reactor that is mounted with the commercial size catalyzer, puts/recept the caloric close with the unit volume of guaranteeing two kinds of catalyst reactor beds like this.
In addition, also can in different reactors, load the catalyzer of difformity or particle size, like this, just can study the characteristic of the catalyst granules of under similar and different reaction conditions difformity or size.In addition, also study in different reactions, in MTO (Methanol to Olefin), different materials is to influence of catalyst deactivation and regeneration etc.As required, also can be provided with sampling valve between material source quality volume control device is used for material is sampled.
Claims (20)
1. parallel reactor system, it comprises inlet control system, n reactor module, n 〉=2, and temperature control equipment, be provided with reactor in the described reactor module, and have at least in the described reactor module and be provided with at least two reactors, each reactor all offers inlet and outlet, but sample loading in it, also be provided with temperature control equipment on each reactor module so that the reactor in it has an identical temperature, it is characterized in that: described inlet control system is provided with at least two material inlets in order to receive the material of at least two material source outputs respectively, also be provided with a plurality of material outlets, this material outlet is divided into n material outlet group with the corresponding described n reactor module of difference, every group material outlet joins with the inlet that this organizes the reactor in the pairing reactor module respectively, the material component that has at least a material outlet in a group to export in described n material outlet group is different from the material component that another material outlet is exported in this group, and the component of its material of being exported of material outlet in same group is not identical to have two at least.
2. parallel reactor as claimed in claim 1 system, it is characterized in that: described inlet control system is provided with at least three material inlets in order to receiving the material of at least three material sources outputs respectively, and the material component that has at least two material sources to be provided in described at least three material sources is different.
3. parallel reactor as claimed in claim 1 system is characterized in that: described inlet control system includes at least one material inlet in order to be received from the part or all of material that more than one reactor is discharged.
4. parallel reactor as claimed in claim 1 system, it is characterized in that: described inlet control system is controlled has at least the flow velocity of the material that a material outlet in a group exports to be different from the flow velocity of the material that another material outlet is exported in this group in described n the material outlet group, and the flow velocity of its material of being exported of material outlet in same group is not identical to have two at least.
5. parallel reactor as claimed in claim 1 system, it is characterized in that: described inlet control system includes material controlling device and material distribution device, described material controlling device comprises mass flow control appts, and described material distribution device is provided with described material outlet.
6. parallel reactor as claimed in claim 5 system, it is characterized in that: described mass flow control appts includes one or more mass flow control appts that are connected in a plurality of materials source simultaneously.
7. parallel reactor as claimed in claim 1 system, it is characterized in that: described parallel reactor system also comprises the control of export system that links to each other with reactor outlet, and this control of export system comprises one or more in sampling apparatus, pressure control device, gathering-device and the circulating device.
8. parallel reactor as claimed in claim 7 system is characterized in that: described control of export system includes and is connected in the equal modules simultaneously or the pressure control device of a plurality of reactors in the disparate modules has identical pressure to control these a plurality of reactors.
9. parallel reactor as claimed in claim 1 system is characterized in that: described control of export system includes the part or all of material that circulating device can discharge the autoreactor outlet fail back described reactor through described inlet control system.
10. parallel reactor as claimed in claim 1 system is characterized in that: described parallel reactor system further includes m second reactor module and connects with m reactor module in the described n reactor module respectively by described control of export system.
11. a sample study method, it includes following steps:
The mass transport that will come from least two material sources is to a plurality of material outlets, described a plurality of material outlet constitutes n material outlet group, n 〉=2, the material component that has at least a material outlet in a group to export in described n material outlet group is different from the material component that another material outlet is exported in this group, and the component of its material of being exported of material outlet in same group is not identical to have two at least;
With described n material outlet group, n 〉=2, the material of being exported is input to the reactor module that is provided with reactor in n, the reactor module that every material outlet group is corresponding respectively, and every group material outlet joins with the inlet that this organizes the reactor in the pairing reactor module respectively;
The temperature of controlling each reactor module makes the reactor in it have a common temperature.
12. method as claimed in claim 11 is characterized in that: described at least two material sources comprise at least three material sources, and the material component that has at least two material sources to be provided in described at least three material sources is different.
13. method as claimed in claim 11 is characterized in that: it also includes following steps: the part or all of material that more than one reactor is discharged is input in one or more reactors by one or more material outlets.
14. method as claimed in claim 11, it is characterized in that: have at least the flow velocity of the material that a material outlet in a group exports to be different from the flow velocity of the material that another material outlet is exported in this group in described n material outlet group, and the flow velocity of its material of being exported of material outlet in same group is not identical to have two at least.
15. method as claimed in claim 11, it is characterized in that: the mass transport that will come from least two material sources comprises that to a plurality of material outlets the material that will come from least two material sources is transported to a plurality of material outlets by at least two material controlling devices and at least two material distribution device, described material controlling device comprises mass flow control appts, and described material distribution device is provided with described material outlet.
16. method as claimed in claim 15 is characterized in that: the mass transport that will come from least two material sources comprises that to a plurality of material outlets the material that will come from a plurality of materials source is transported to a plurality of material outlets by a mass flow control appts.
17. method as claimed in claim 11, it is characterized in that: it also includes following steps: the material that autoreactor outlet is discharged is sent into a control of export system, and this control of export system comprises one or more in sampling apparatus, pressure control device, gathering-device or the circulating device.
18. method as claimed in claim 17 is characterized in that: described control of export system includes and is connected in the equal modules simultaneously or the pressure control device of a plurality of reactors in the disparate modules has identical pressure to control these a plurality of reactors.
19. method as claimed in claim 17 is characterized in that: described control of export system includes the part or all of material that circulating device can discharge the autoreactor outlet fail back described reactor through described inlet control system.
20. method as claimed in claim 11 is characterized in that: it also comprises the steps: the material that described reactor is discharged is input in one or more second reactors.
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