CN101274252A - Catalytic process exploitation apparatus and method - Google Patents

Abstract

A catalytic procedure development apparatus is disclosed, comprising a fresh reactant source, a control valve, a sampling valve, a temperature control device, a first reactor with high transferring rate and a second reactor with low transferring rate; performances at different longitudinal positions of a catalyst bed of a composite plug flow reactor can be simulated by inputting the fresh reactants and ejections of the first reaction in diverse proportions to the second reactor; and the influence to reaction course by these substances can also be tested by inputting other substances into the second reactor, such as reaction products, byproducts and pollutants and toxic substances which are likely present in industrial reactor raw materials. Dynamics, quality transfer and heat transfer performances of the composite plug flow reactor can be tested by sampling and analyzing ejections of the first reactor and the second reactor. In addition, the invention also relates to a method for development of the catalytic procedure. Accordingly, the device and the method of the invention can speed up the course of industrialization scale.

Description

A kind of development device of Catalytic processes and method

[technical field]

The present invention relates to a kind of devices and methods therefor that is used for catalytic process exploitation, this device and method can be used for being found to commercial catalyst for application and laminar flow Catalytic processes thereof so that the quick exploitation of lower cost is a kind of at first from it.Especially, the present invention refers in particular to a kind of laboratory scale piston flow reactor device and reaches the method for amplifying (scale-up) its Catalytic processes fast.

[background technology]

In order to amplify (scale-up) a kind of laminar flow Catalytic processes, just need the influence of research reaction time (time onstream), reactant residence time (residence time), catalyst particle size, shape and its other features and temperature curve (temperature profile) to reaction rate and catalyst selectivity.In the research of traditional amplification, what the first step related to earlier usually is selecting catalyst and some intrinsic propestieses that determine selected catalyst.In order to reduce the influence of mass transfer to operating process, the operation of this step often is to select the catalyst or the powder catalyst of the crushing of process dilution to carry out under isothermy.When the operation of this step begins, need test the changeability of reaction process, its main purpose is to determine the influence to reaction rate and catalyst selectivity of air speed, pressure and reactant residence time.Like this, the employed catalyst activity of this step is reached optionally definite six wheat harvesting periods that often need to year.Last in this step operating process still needs the changeability of reaction process is tested again, is used for determining whether above characteristic can change along with the reaction time.

Secondly, select the described catalyst of commercial size in isothermal reactor, to test.The catalyst of so-called commercial size, its catalyst compared to above-mentioned crushing has bigger particle size or has specific shape, is used for reducing the pressure drop in the operating process.Because reactant or product enter or leave the restriction that quality is transmitted in the catalyst hole process in course of reaction, the reaction rate and the selectivity of general large-size particle catalyst are relatively poor.When the beginning and finish of this operating process, also often need study with detecting catalyst activity and selectivity the changeability of technology equally, so just need about year again.In addition, this step often uses laboratory-scale reactors to carry out.

The reactor of the checking scale with one or more reaction tubes is normally selected in final step for use, the catalyst of the described commercial size of test under the condition of thermal insulation.The about 25.4mm of the internal diameter of described reaction tube (1 inch) can increase to about 101.6mm (4 inches) in some cases.In addition, in order better to probe into the influence that heat transmits, described reactor is standing puts 6-8 reaction tube, and the distance between reaction tube is provided with according to the distance that commercial scale adopts.In an exothermic reaction, as in tubular reactor or in the piston flow reactor that does not have special heat extraction equipment, the variation of temperature curve depends on the degree that removes reaction heat continuously.Variation of temperature has remarkable influence to selection of catalysts, reaction rate and activity.In the test of this step, often can measure the trend of reaction generation focus or temperature control.Equally, this step often needs the time more than a year.

As seen, the finishing the normal time of needs more than 3 years of this series of steps, and usually differ and obtain institute surely and be useful on and amplify needed data.For a lot of catalyst, its reaction rate and selectivity are relevant with the time that reactant residence time and reactor continue to react.This relation is the result of catalyst condition or specifications vary, and this variation to be the continuous variation that gas or liquid are formed owing to the time of catalyst reaction or from reactor inlet to exit procedure cause.Such as catalyst run into material such as hydrogen sulfide and ammonia and with its reaction in, the water oxidation that catalyst can be formed in the conversion process can form cover layer and catalyst poisoning etc. in its surface, thereby cause catalyst condition or specifications vary.In addition, since reactant and product surface-catalyzed reactions takes place in catalyst pores and accumulate the reduction that also can cause mass transfer rate (masstransfer rate) in the hole.

Recently, the high flux experimental technique is used to new catalyst and Catalytic processes thereof are studied.These high flux experimental techniques are generally carried out under the influence that reduces heat biography and matter biography, and it only needs seldom to measure the catalyst of (being less than 2 milliliters) and have very high rates of heat transfer.Yet, this technology, such as United States Patent (USP) the 6th, 149, No. 882 and the 6th, 869, disclosed for No. 799, though can the intrinsic performance of different catalyst to be selected be compared, can not be provided for amplifying needed data.

So, need a kind of research method of new high flux Catalytic processes and device thereof in order to overcome the defective of prior art.

[summary of the invention]

The object of the present invention is to provide a kind of devices and methods therefor with lower cost, this device and method is used to develop and a kind ofly is found to the commercial catalysis flow process of using at first from it.

Described catalysis development device can be simultaneously with one or more catalyst of one or more formal testings.

In one embodiment of the invention, fresh reactant is imported in laboratory scale first piston flow reactor, and this first reactor has higher conversion ratio, as 60-80%.The effluent of all or part of first reactor can be by the input of laboratory scale second piston flow reactor inlet wherein, this second reactor has lower conversion ratio, as 5-20%, and the height of the catalyst layer of its loading is less than the height of the catalyst that loads in described first reactor.Simultaneously, also can import quantitative fresh reactant thing in addition in second reactor, be input to the ratio of the effluent and the quantitative fresh reactant thing of described first reactor in described second reactor like this by adjustment, described second reactor just can be used for simulating the performance of a selected section (cross-sectional slice) of a commercial scale piston flow reactor.

In another embodiment of the present invention, what be provided with in addition also that one or more and described second reactor be arranged in parallel has a piston flow reactor than low-conversion, is defined as the 3rd reactor.The 3rd reactor equally can be in order to the effluent of importing described first reactor with higher conversion and fresh reactant.Simultaneously, the catalyst layer of the 3rd reactor loading is more shallow than the catalyst layer in described first reactor equally.When a plurality of the 3rd reactors all are mounted with identical catalyst, by effluent and the fresh reactant thing ratio of controlling first reactor in the different input different reactors, like this, just can simulate the characteristic of different sections (different slices) in the commercial scale piston flow reactor simultaneously.In addition, also can describedly in the past have and import other quantitative material,, come of the influence of these materials of simulation test different sections in the commercial scale piston flow reactor as product, accessory substance or pollutant etc. than the piston flow reactor of low-conversion.By in good time change in the first reactor effluent and fresh reactant thing ratio or add described other material, after the feed that can come simulation test to work as described variation enters reactor, in the process that this variation of catalyst aims is adjusted and after the elimination of the feed condition of described variation, this feed condition of catalyst aims is eliminated in the process of recovering the back, the transient response of the different sections of industrial-scale reactor beds.

Described piston flow reactor can be fixed bed reactors (Fixed BedReactors), packed bed reactor (Packed Bed Reactors), trickle bed reactor (Trickle BedReactors) and the monolith honeycomb reactor (Monolithic Reactors) of one way or cycling.Described laboratory scale piston flow reactor is meant that the internal diameter of each section reactor of piston flow reactor is 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 2.438m (8 feet), preferably less than 1.219m (4 feet), more preferably less than 0.304m (1 foot); Except that crossing the inertia dilution, the useful load of catalyst is less than 800 grams, preferably less than 400 grams, more preferably less than 25 grams.

Like this, by the test of different test conditions, many characteristics of industrially scalable reactor after just can simulating, thereby the process of quickening industrially scalable.

[description of drawings]

Fig. 1 is the device schematic diagram of piston flow reactor of the present invention.

Shown in Figure 2 be the device schematic diagram that is used to simulate the multistage piston flow reactor of isothermal of adiabatic reactor of the present invention.

Fig. 3 is the schematic diagram of an embodiment of reactor of the present invention and separator assembling.

Fig. 4 is the schematic diagram of another embodiment of reactor of the present invention and separator assembling.

Fig. 5 is the schematic diagram of another embodiment of reactor of the present invention and separator assembling.

[preferred embodiment]

As shown in Figure 1, it is an embodiment of laboratory scale reaction unit of the present invention.In this embodiment, described reaction unit is a compound plural serial stage piston flow reactor.This reaction unit can be used for studying matter biography, heat biography and the dynamics of relevant with longitude in plant-scale piston flow reactor (longitudinally dependent).In the present embodiment, this piston flow reactor is fixed bed reactors.Referring to shown in Figure 1, fixed bed reactors 11 are defined as first reactor, are provided with the beds 13 of commercial size in it.Fresh reactant thing autoreaction thing source 15 enters reactor 11 and reacts.The effluent that the reaction back forms is discharged the back from reactor 11 and is entered corresponding laboratory scale fixed bed reactors 17-1 respectively by control valve (control valve) 19-1 to 17-n to 19-n.Described control valve 19-1 does not enter the fixed bed reactors 17-1 that be arranged in parallel the flow to 17-n to the 19-n controllable sub.Reactor 17-1 is provided with corresponding beds 21-1 respectively to 21-n in 17-n.This beds 21-1 is lower to the conversion ratio of 21-n, and it dilutes with the assurance beds with inert particle operates under the condition of isothermal.Beds 21-1 roughly is controlled to be 25% or littler to the conversion ratio of 21-n, the conversion ratio of preferred 5-20%, and its thickness of bed layer is less than the thickness of beds 13.In addition, reactant source 15 also can by control valve 23-1 to the quantitative fresh reactant thing of 23-n supply to fixed bed reactors 17-1 in 17-n.

In exothermic reaction, supply with fixed bed reactors 17-1 to the process of 17-n fresh reactant thing from reactant source 15,18 pairs of described fresh reactant things of heater are set usually carry out preheating.Reactor 17-1 is provided with sampling valve 25-1 to 25-n to the 17-n exit, can sample to the effluent of 17-n to reactor 17-1.As shown in Figure 1, sampling valve 25-1 only samples to the effluent of 17-n to reactor 17-1 to 25-n, also can sampling valve 14 also can be set in the exit of reactor 11 come the effluent of reactor 11 is sampled as required certainly.In the present embodiment, sampling valve 14 and all or part of sampling valve 25-1 and 25-n may be defined as first sampling valve.As shown in Figure 1, reaction unit also includes another feed source 29, and one or more in the 17-n are given reactor 17-1 by control valve 31 quantitative feed in this feed source 29.As shown in Figure 1, feed source 29 only links to each other with reactor 17-n by control valve 31, yet, present embodiment is not limited in this, and feed source 29 can link to each other or corresponding different reactor 17-1 is provided with each self-corresponding control valve to 17-n and links to each other with feed source 29 by one or more in the 17-n of control valve 31 and reactor 17-1.In one embodiment, contain reactant, byproduct of reaction or pollutant etc. in the feed in feed source 29.

The effluent of reactor 11 and fresh reactant thing in reactant source 15 supply response device 17-1 to 17-n can be respectively control valve 19-1 by correspondence enter into corresponding reactor 17-1 to 17-n to 19-n and 23-1 to 23-n.Reactor 11 has higher conversion ratio usually, as 60-80%.When reactor 11 when set conversion ratio is operated under as 80% condition, can adjust the effluent of reactor 11 and reactant source 15 supply response device 17-1 to 19-n and 23-1 to 23-n to the ratio between the fresh reactant thing of 17-n by control valve 19-1, and then can adjust the conversion ratio of reactor 17-1 to 17-n, it is between 0 to 80%.With reactor 17-1 is example, and control valve 19-1 and 23-1 only make the effluent of reactor 11 enter among the reactor 17-1, and the thickness of control beds 21-1 transforms about 5% the effluent that enters the reactor 11 among the reactor 17-1 in reactor 11 again.Like this, beds 21-1 just is equivalent to a section (cross-sectional slice) of the piston flow reactor catalyst layer of conversion ratio between 80-85%.Similarly, control valve 19-2 and 23-2 make the material that enters reactor 17-2 have 40% conversion ratio, and the thickness of control catalyst layer 21-2 makes this material transform about 5% again, like this, catalyst layer 21-2 just can be used for simulating a section of the catalyst layer of conversion ratio between 40-45%.And then catalyst layer 21-1 just can be used to simulate the performance of a piston flow reactor along the section of any lengthwise position of catalyst layer to 21-n.Duplicate characteristics and the performance that the continuous longitudinal component of big catalyst layer was measured and analyzed at the continuous vertical position of compound piston flow reactor catalyst layer by catalyst layer 21-1 among reactor 17-1 and the 17-n and 21-n, thereby measure the characteristics of the beds that also can't know at present and vertical distribution of performance.

In one embodiment, adjust the concentration of supplying with selected reactor 17-1 trace components in the fresh reactant thing of 17-n by feed source 29, such as the concentration that increases specific trace components (trace components), quantize under the substantial length of operation condition, trace components is in the influence of catalyst layer different piece in the reaction.So just can determine vertical position of the key of recombination catalyst layer in the Industrial Catalysis system.At these positions, catalyst is more easily poisoned or owing to poison inhibitory reaction or generation byproduct is taken place.

Catalyst layer 21-1 can have different components to 21-n, such as, catalyst layer 21-1 and 21-2 are mounted with the catalyst granules of crushing and the catalyst granules of commercial size respectively, and the dilution particle that all is mounted with inertia in two catalyst layers is operated in isothermy in order to guarantee catalyst layer.The matter that so just can measure any lengthwise position section of catalyst layer passes, heat passes and dynamics.For different application, catalyst layer 21-1 is mounted with the catalyst granules with different chemical or physics to 21-n, so just can measure the different vertically performances of the different catalysts of section in compound piston flow reactor.

Enter reactor 17-1 thermal loss or its temperature in the 17-n process for fear of the effluent of reactor 11 and raise, often on pipeline in coupled reaction device 11 and 17-1 to 17-n and the control valve covering insulating material to avoid above-mentioned situation.In addition, can to 17-n temperature control equipment 33 and 35 be set respectively to reactor 11 and reactor 17-1 and control its temperature, perhaps for different demands, reactor 11 and reactor 17-1 also can be provided with common temperature control equipment to 17-n.In addition, the fresh reactant thing from reactant source 15 supply response device 17-1 to 17-n carries out preheating through heater 18 after often need coming out from reactant source 15.Heater 18 can adopt the known direct mode of heating of industry that reactant is heated, as sand-bath heater coil (heating coil in afluidized sand bath) or infrared heating furnace etc., so that the catalyst layer at reactor inlet place reaches suitable temperature conditions.

In exothermic reaction, in Fischer-Tropsch synthesis, the heat conduction media is arranged in the temperature control equipment 33,35, as circulating boiling water, be used for reactor 11 and 17-1 are derived to keep reactor a stationary temperature to the reaction heat of 17-n.In the endothermic reaction, in paraffin dehydrogenation or catalytic reforming reaction, temperature control equipment 33,35 is provided with heater, as electric heater in order to give reactor 11 and 17-1 to the 17-n heat supply so that reactor maintains constant predetermined temperature.Certainly, for existing exothermic reaction the endothermic reaction is arranged again, temperature control equipment 33,35 can be corresponding is provided with refrigeration or the heating sand-bath comes corresponding reactor is operated.

(not shown) in one embodiment, reactor 11 and 17-1 to 17-n can be parallel to each other be arranged at a temperature control equipment, in sand-bath, like this, the structure of reactor is just compact, and the height of sand-bath also needn't as reactor 11 and 17-1 to 17-n is vertical be provided with when being provided with height.Certainly, sampling valve 25-1 and 25-n are arranged at outside the sand-bath, so that safeguard in the reaction or adjusting.When effluent has various states to 17-n from reactor 11 and 17-1, on the one hand, 11 outlets of coupled reaction device and reactor 17-1 need have higher Reynolds number or use agitator to form piston flow with the fluid of avoiding pipeline to the pipeline of 17-n inlet, on the other hand, sampling valve 25-1 and 25-n such as adopt at dynamically sampling valve, and other that can be also perhaps that the present invention describes form the mode of piston flow to avoid fluid.

According to different goals of the invention, as amplification or other purposes etc., reaction unit of the present invention and method thereof can be used to detect the operating parameter of piston flow reactor under various objectives.Such as, under the condition of different reaction temperatures, pressure, catalyst shape and size, detect the activity and the relation in reaction time (time on stream) that are associated with longitude.Certainly also can detect the technological parameter that other are associated with longitude, these technological parameters comprise different air speeds, reactant and side reaction thing, different operating temperature and pressure, reaction time, different catalyst size and shape and conversion ratio, yield, dynamics and selection rate; The parameter that also has catalyst physics and chemical characteristic to change in addition is as the growth of active sites crystallization size, oxidation and active sites surface coating etc.

The data that obtain according to the reaction of required research and needs, use conventional methods as gas chromatographic analysis/mass spectral analysis (GC/MS) to the effluent of 17-n for raw material and reactor 17-1, ultraviolet (UV) or infrared (IR) characterize the characteristic of reactant and product, or adopting X-ray diffraction (XRD), infrared diffuse or the known spectroscopy techniques of other industries characterize catalyst system.The attribute of performance of relevant with the catalyst layer lengthwise position like this system just can access quantification.Therefore, can come optimization system according to the catalytic reaction kinetics information that obtains and the attribute of performance of every bit, and according to the catalyst granules different physics that diverse location has in catalyst layer and chemical property designs catalyst system so that it reaches maximum yield or selection rate in local environment.

As shown in Figure 1, the reactor 17-1 catalyst of filling in the 17-n can be catalyst crushing or grained catalyst or commercial size.Amplify required data in order to obtain reactor, most of test all is to carry out under isothermy.Under isothermy, react to 17-n in order to ensure reactor 17-1, can the catalyst granules of catalyst layer 21-1 and 21-n be diluted with inert particle, inert particle and catalyst granules, the ratio of the two often is 8 to 10 to 1.When needs were measured under adiabatic condition, according to the situation of the diameter and the reaction heat of reactor, reactor 17-1 catalyst in the 17-n can carry out the dilution of less degree.Catalyst granules depends on multiple factor with the dilution proportion of particles, as the activity of reaction heat and catalyst granules etc.Certainly, for the industry personnel, for the reaction of given catalyst, reactor diameter and a catalyst size, it can determine appropriate catalyst particle and dilution proportion of particles by once simply testing.

For the commercial size catalyst in the piston flow reactor, its exemplary particles size is at 1 to 5 millimeter.Crush or powder catalyst is often prepared by the catalyst of commercial size, and its exemplary particles size is at 0.10 to 0.20 millimeter, and certainly, its size under the condition that keeps catalytic performance is the smaller the better.Usually, for the reactor that is mounted with the commercial size catalyst, the internal diameter of reactor is 10 times of reduced size in dilution or the catalyst granules, and its minimum of a value often is 10-50 millimeter (a 0.4-2 inch).The internal diameter of reactor of catalyst that is mounted with crushing is often for the 5-12 millimeter, and it is less than the internal diameter of the reactor that is mounted with the commercial size catalyst.Owing to have a less resistance to mass tranfer, crushing or powder catalyst often than the catalyst activity height of commercial size.So, particularly in exothermic reaction, can have the identical operations temperature with the similar reactor that is mounted with the commercial size catalyst in order to ensure being mounted with reactor crushing or powder catalyst, in being mounted with reactor crushing or powder catalyst, the ratio of inertia dilution particle and catalyst granules is greater than the ratio in the reactor that is mounted with the commercial size catalyst, and is identical with the unit volume thermal discharge (heatrelease per unit volume) of guaranteeing two kinds of catalyst reactor beds like this.From the elasticity consideration of reactor 11 different application, the reactor inside diameter of the catalyst layer of the crushing that usually more excellent is is mounted with is identical with the internal diameter of the reactor of the catalyst layer that is mounted with required commercial size.Certainly, can be by the internal diameter of reactor that thermal conducting sleeve reduces to be mounted with the catalyst layer of crushing be set in reactor.

The preferable minimum constructive height of reactor depends on considering of stirring or heat release.In isothermal operation, when stirring into to limiting factor, the selection of height for reactor just needs effectively to avoid the by-pass flow of reactant.Particularly for the reactor that loads the commercial size catalyst, it is 50 times of catalyst granules average diameter highly at least, promptly is 50 to 250 millimeters.

As shown in Figure 1, when feed source 29 behind the specific material of selected reactor 17-1 provisional adding in the 17-n, reactor 17-1 can be used to the transient response that simulation test recombination catalyst layer difference produces the temporary variation of this feed component to 17-n, and can monitor in described predetermined substance adition process or add that post-reactor changes (Time Dependent) in time and the reaction that takes place.

In one embodiment of the invention, fluids such as reactant and other feed things, product and byproduct of reaction can be gaseous state, liquid state or its mixed state, as gaseous state and the mixing of liquid state or the mixing of two or more immiscible liquid.To containing the fluid of gaseous material, can utilize traditional back pressure regulator and gas flow control system to control with mass flow controller.For quantitative fluid liquid, often select for use as Luo Si holddown (Ruska pump) or syringe pump (Syringe pump) it is entered in the hyperbaric environment.In addition, when the effluent of fresh reactant thing, reactor 11 or the component supplied with by feed source 29 comprise the multiple fluid state, particularly immiscible each other, during as water and hydrocarbon or gas and liquid, just need avoid fluid to flow with piston flow (laminar flow) form.In one embodiment of the invention, sampling valve can be selected the dynamic sampling valve such as grade that provides as Norway ProservAS company for use or as United States Patent (USP) the 4th, 035,168 separators that disclosed, certainly, also can use agitator that ProservAS company provides that the fluid of needs sampling is stirred samples to it rapidly after multi-mode fluid is evenly mixed.Between the immiscible raw material or between the effluent of raw material and reactor, when it is admitted to reactor, perhaps has multi-mode effluent when entering reactor 17-1 to 17-n as what transport reactor 11 was discharged, fluid-transporting tubing needs higher Reynolds number, its principle just is similar to the fuel injection system of automobile engine, certainly, also can use Proserv AS company or be positioned at the Admix company in Manchester, New Hampshire city the agitator that provides to realize the abundant mixing of different fluid, like this under the situation, having needs to do some simple tests often and guarantees that fluid is flowed through and mix behind the described device.When sampling, regular meeting is provided with the sample memory that links to each other with reactor by double block valve, and this sample memory is in the environment of normal pressure or a little higher than normal pressure.After gaseous material and liquid fully mix in conveyance conduit, open double block valve and make mixed fluid enter sample memory, close double block valve then and remove sample memory and sample is wherein analyzed.There is certain density inert gas in regular meeting in sampling and analytic process, and as argon gas, it helps the material balance of fluid, so that convection cell carries out Accurate Analysis.When described fluid does not fully mix, just gas-liquid separator need be set, then by gaseous material and liquid being analyzed respectively as the overall Carbon balance analytical method of helium or argon gas internal standard method and related gaseous material and liquid, at this moment, this situation can thereunder be provided with the fluid sample memory and finish by the gaseous sample memory is set above conveyance conduit.

When the characteristic of research piston flow reactor, what pay particular attention to is absorption or the reaction at catalyst surface of raw material components, product or accessory substance.Such as, in the synthetic and hydrocracking reaction, materials such as ammonia, carbon monoxide and hydrogen sulfide can take the activity of such catalysts position, reduce reaction rate and influence to product selectivity at cobalt-based catalysis Fischer-Tropsch.The reaction that is caused by this class material often needs the regular hour to reach balance, and after removing this type of material in from the reaction raw materials to the reactor, the reacting recovery original state also needs to spend the regular hour.

Ammonia be known can be synthetic and the material of hydrocracking catalyst reaction with co-based fischer-tropsch, it can cause the reduction even the inefficacy of catalyst activity.Except in raw material except that deammoniation, often utilize hydrogen to remove the ammonia of catalyst surface.In order to test the influence of ammonia different parts in composite catalyst bed, a detection reaction device (probe reactor) (not shown) can be set, and add a certain amount of ammonia by arbitrary grade porch at a detection reaction device, so just can reproduce because the existence of ammonia and to the influence at the selected position of recombination catalyst layer in the raw material.Control the transform level at selected catalyst position by the local pressure of adjusting temperature, rate of flow of fluid or reactant in the detection reaction device, so just can determine the influence of ammonia under different reaction conditions.In addition, for by the composite catalyst of ammonia pollution, by adjusting in the input detection reaction device concentration of hydrogen in one or more levels, so also can test of the influence of ever-increasing hydrogen, as the lost efficacy position of maximums of those catalyst activities to the composite catalyst different parts.

For carbon monoxide, it can tightly cover on the Co based Fischer-Tropsch synthesis catalyst surface, thereby reduces the surface that hydrogen can be used, and becomes a factor of restriction hydrogen reaction speed.By adjusting the concentration ratio of hydrogen and carbon monoxide in the raw material that selected multistage reactor 17-1 imports in the 17-n, the change in concentration that just can test hydrogen and carbon monoxide is to reaction rate and optionally influence.

Be known that at present at the Fischer-Tropsch of piston flow reactor synthetic and heavy oil concentrates and conversion process in the water that increases reaction rate is had positive effect.Adding water that quantitative water can study adding in the 17-n to selected reactor 17-1 to the selected vertical position reaction rate of recombination catalyst layer with optionally influence.

In the reaction of hydrotreatment, utilize mensuration Joseph Conrad inferior (Conrad son) carboloy residue to detect the effect of hydrotreatment usually.Wax also can form certain influence to fischer-tropsch synthetic catalyst.Usually, in Fischer-Tropsch synthesis,, will stop reactant to leave catalyst surface to catalyst surface diffusion and product in case carbon and heavy wax are deposited on the catalyst.Like this, some side reactions take place with regard to regular meeting in the reactant of the sediment of catalyst surface or not diffusion, thereby reduce activity of such catalysts.At beds is under the situation of commercial size catalyst, because the evolving path of commercial size catalyst is very long, under the limited easily condition of diffusion, will influence the bulk life time of catalyst and the performance that needs very high cost to remove maintenance system.Certainly, by add the above-mentioned substance of different molar fractions (molecular weight fractions) in 17-n one or more to selected reactor 17-1, just can determine it is to which having the greatest impact partly in the recombination catalyst layer.In addition, also can be by can in 17-n, feeding the effect that hydrogen, water or lightweight solvent are determined different catalyst regeneration technology to the corresponding reactor 17-1 that contains above-mentioned substance, thus determine catalyst regeneration technology preferably.These come from tar sand, shale for those processing, and the heavy charge of heavy oil precipitation and coal etc. is most important.Contain many pollutants that make catalyst poisoning at these heavy charges,, consider that from economic feasibility in-situ regeneration is unique method often just for the increase that reduces to remove to change the cost that fouled catalyst brings through fresh catalyst commonly used.

In addition, polynuclear armatic hydrocarbon also is the present known material that can influence catalyst performance.It reduces activity of such catalysts and selectivity in the hydrogenation treatment by form the carbonaceous cover layer on the catalyst activity position.By just can determine the influence of the different longitudinal position of its recombination catalyst layer in piston flow reactor at selected reactor 17-1 adding polynuclear armatic hydrocarbon in 17-n one or more.So just can determine polynuclear armatic hydrocarbon to which position of recombination catalyst layer has the greatest impact, and then can take corresponding method to improve the design of system and the performance of raising catalyst.

In another embodiment of the present invention, reactor 17-1 is complete mixing flow (Fullback-mixed) reactor to the one or more of 17-n.In the complete mixing flow reactor, the concentration of raw material thing, product and the distribution of catalyst are identical everywhere, so it just can be equivalent to a narrow horizontal component in the beds of plant-scale piston flow reactor.Enter the effluent of reactor 17-1 reactor 11 of complete mixing flow reactor in the 17-n and the concentration between fresh reactant by control, described complete mixing flow reactor just can reproduce the characteristic of the selected horizontal component of recombination catalyst layer in the piston flow reactor.In one embodiment, the complete mixing flow reactor can be two-phase fluidised bed reactor, three phase slurry bed bioreactor or three-phase fluidized bed reactor.

In addition, in other embodiments of the invention, obtain to amplify the data etc. of Catalytic processes as the characteristic of testing different catalysts simultaneously or being loaded into the method such as make comparisons of the catalyst of specification already of returning with difformity and size of loading respectively in the catalyst of crushing in the reactor and other reactors.Utilize these results, just can design a composite catalyst bed, the intrinsic propesties of its each layer catalyst all passes the environment facies coupling with local dynamics and matter.Like this, the general reaction of system longitudinally changes, thereby determines the optimum process performance at each vertical position in the compound reactor.

When the beds of reactor 17-1 in the 17-n for crushing or the fine catalyst particle, and when reactor is operated in isothermy, obtain at first reaction rate and optionally data result can be considered to catalyst in the selectivity and the intrinsic reaction rate thereof in when beginning reaction, get rid of promptly that matter passes and heat passes the reaction rate of influence; Subsequently, the carrying out along with reaction just comprised the influence that catalyst ageing brought in the intrinsic reaction rate that obtains.In any case, the macroreaction speed of this moment equals the intrinsic reaction rate, and the efficiency factor that promptly is exactly reaction is 1.In addition, for fresh and aging catalyst, optionally data result can come directly to weigh the essential selectivity of catalyst and the relation of conversion ratio.These data are extremely important for the model of setting up the industrialization piston flow reactor.

When reactor 17-1 is mounted with the catalyst granules of commercial size to the partial reaction device among the 17-n, during that another part is mounted with crushing or fine catalyst particle, two reactors that are assembled with the different catalysts particle are in parallel reacting under isothermy under the control of identical temperature control equipment, thereby determine for the very important efficiency factor relevant with lengthwise position of industrialization Catalytic processes and other information by the comparison of two kinds of reactor performances like this.

In addition, by analysis, thereby can obtain the relation data of the apparent reaction rates and the time of staying to the effluent of the reactor that is mounted with the commercial size catalyst granules.Like this, under the known situation of intrinsic reaction rate,, just can directly obtain the relation of efficiency factor and conversion ratio by the relation data of its conversion ratio and the time of staying for catalyst crushing and commercial size.At this moment, the diameter of known efficiency factor, intrinsic reaction rate and full-size catalyst granules (relevant) with the thickness L of beds, thus can determine the relation of the effective diffusivity of full-size catalyst granules by the Thiele modulus with respect to conversion ratio.

Like this, resulting data just can be used to probe into the mechanism that matter passes retardance.As, have at the reactor inlet place that lower diffusivity shows since the influence of the initial product of raw material components, reaction maybe in considering fluid during the true dividing potential drop of a certain component raw material components in the concentration on the catalyst activity position less than the former of expection concentration thereby on catalyst hole or surface, form matter biography resistance.When having lower diffusivity at reactor exit, it shows that product accumulation or effluent fluid and catalyst takes place reacts.When reaction relates to multiple reactant with different diffusivitys, because efficiency factor can be reflected in the variation of component between gaseous material and the catalyst surface, so apparent reaction rates and selectivity are all often relevant with efficiency factor.

Behind the finite data of test data that obtains two bank of reactor and intrinsic activation energy, just can set up the performance that a reactor model is used to predict multistage adiabatic reactor, the data that obtain from adiabatic reactor can be used as the test to reactor model again like this.In addition, from the possibility occurrence and the happening part of adiabatic reactor in service measurable focus or temperature control the heat release Catalytic processes.

In one embodiment of the invention, definable reactor 17-1 is second reactor to the whole of 17-n, and the 3rd reactor is set separately as required, even the 4th reactor etc., perhaps according to different test requests, definable reactor 17-1 is second reactor to the part of 17-n, and part is the 3rd reactor, even the 4th reactor etc., by that analogy.Difference classification corresponding to reactor, definable control valve 23-1 is first control valve to the whole of 23-n, control valve 19-1 is second control valve to the whole of 19-n, and the 3rd control valve and the 4th control valve etc. are set as required separately, and perhaps control valve 23-1 is first control valve to the part of 23-n, part is the 3rd control valve, even the 5th control valve etc., control valve 19-1 is second control valve to the part of 19-n, and part is the 4th control valve, even the 6th control valve etc., by that analogy.The different definition mode of corresponding reactor, sampling valve 14 and whole sampling valve 25-1 may be defined as first sampling valve to 25-n, and second sampling valve etc. is set separately, perhaps sampling valve 14 and sampling valve 25-1 are defined as first sampling valve to the part among the 25-n, even sampling valve 25-1 is defined as second sampling valve the 3rd sampling valve etc. to the another part among the 25-n.More than definition only is the definition of carrying out for the convenience of different setting of corresponding reactor and description, and it is not construed as limiting the invention.Certainly, also can use any define method easily that helps testing and describing.

In adiabatic reactor, the temperature in the reactor constantly changes, and controls just may produce focus when bad and the temperature runaway phenomenon takes place.Simultaneously, because the response parameter in the adiabatic reactor is in the continuous variation, like this,, just can not obtain in the adiabatic reactor specifically as this reactor of direct measurement, information accurately.The reactor that a complete adiabatic reactor is divided into plural serial stage helps to study the information of diverse location in the beds.Yet the continuity of controlling the response parameter between the adjacent two-stage reactor will face difficulty.

Therefore, directly just may be difficult to obtain the characteristics such as dynamics, matter biography and heat biography of adiabatic reactor by the characteristic that detects adiabatic reactor.

As shown in Figure 2, in one embodiment of the invention, it utilizes laboratory scale isothermal reactor to simulate to be mounted with the characteristic in the adiabatic reactor of same catalyst bed, so just cost that can the be lower Catalytic processes of a kind of industrial adiabatic reactor of exploitation fast.In the present embodiment, described laboratory scale isothermal reactor is a combined multi-stage piston flow reactor 607, and its reactor 61,63 and 65 parallel to each other by three and series connection is formed, and is mounted with catalyst bed interval 62,64 and 66 in it respectively.Definable reactor 61,63 and 65 is respectively the first order, the second level and third level reactor.Raw material source 60 links to each other with the inlet of first order reactor 61 by fresh reactant conduit 70; Between the inlet of the outlet of reactor 61 and reactor 63, between the inlet of the outlet of reactor 63 and the reactor 65 and exit of reactor 65 can be respectively arranged with sampling apparatus 67,68 and 69, and the outlet of reactor 65 can link to each other with a separator (not shown) by sampling valve 69. Sampling apparatus 67,68 and 69 also offers an opening 601,602 and 603 respectively, in order to the effluent of carrying the respective reaction device to device that this opening links to each other in.In addition, also can fresh reactant conduit 70 being provided with sampling apparatus (not shown) comes fresh material is carried out sampling analysis.Be respectively arranged with temperature control equipment on reactor 61,63 and 65, it comprises that first, second and third temperature control equipment 604,605 and 606 is in order to control the temperature of respective reaction device 61,63 and 65 respectively.In the present embodiment, described reactor 61,63 and 65 all can be operated under isothermy.In addition, can be provided with preheating device (not shown),, also can in first order reactor 61, be provided with preheating device certainly in order to raw material is heated to suitable temperature in raw material source 60 and 61 of first order reactors.

Because the length temperature along reactor in adiabatic reactor is constantly to change, so when simulating the catalysis characteristics of an adiabatic reactor, just need at first to determine the temperature of the temperature control equipment on each grade isothermal reactor with multistage isothermal reactor.Usually, can determine the caused temperature variations that reacts in the temperature of the temperature control equipment on the first order reactor and the first order reactor earlier in given reaction condition and the data under the Catalytic processes by what operate in practice that adiabatic reactor obtains, as the situation of intensification/cooling; And then the temperature by the temperature control equipment on the first order reactor and in course of reaction the variations in temperature in the first order reactor determine the control temperature of second level reactor; Determine control temperature of third level reactor or the like by calculating then to second level reactor.Like this, after the temperature of each temperature control equipment was determined, described isothermal reactor just can be simulated the characteristic of adiabatic reactor.

In the present embodiment, the temperature of first temperature control equipment, 604 control first order reactors 61 is T1; The temperature of second temperature control equipment, 605 control second level reactors 63 is T2; The temperature of the 3rd temperature control equipment 606 control third level reactors 65 is T3.Wherein, T1, T2 are different with T3.Certainly, determine corresponding different temperature T 1, T2 and T3 or use a common temperature control equipment to control the temperature of every stage reactor 61,63 and 65 respectively according to different application and operating condition.

Like this, in the present embodiment, just can be by the first order, the second level and the third level reactor 61 that is isothermal reactor, the characteristic of the different continuous catalyst bed interval in 63 and 65 beds of simulating respectively in the adiabatic reactor, thereby can obtain by catalyst bed interval 62,64 and the 66 Catalytic processes characteristics of forming that are loaded into a composite catalyst bed in the adiabatic reactor.Because the ease for operation of isothermal reaction in the present embodiment, just can be simulated an operational characteristic in plant-scale adiabatic reactor by comparatively simple, safe mode by isothermal reactor.

Operating the continuous piston flow reactor of two-stage at least, such as when a complete beds being divided into multistage catalyst bed interval, the effluent of upper level reactor will be through entering in the next stage reactor behind one section conveyance conduit, like this, the effluent that guarantees the upper level reactor still keeps the continuity or the uniformity of parameter of materials when entering in the next stage reactor behind the conveyance conduit, and the variation that material state etc. do not take place just seems extremely important.

In a specific chemical technology and given following time of reaction condition, when the effluent of A reactor is a homogeneous phase, promptly single phase, during as the gas phase attitude, often this homogeneous phase effluent just can directly transmit by the conveyance conduit between the superior and the subordinate's reactor.In addition, in some reactions, described effluent is heterogeneous, and is typical in gas phase and liquid phase.Described gas phase can comprise gas, steam or its mixture; May include water, oil phase, other things that do not dissolve each other in the described liquid phase and reach emulsion etc. mutually.

Usually, have a plurality of different material components in the heterogeneous effluent, and material component has separately state in each.When the material component in the described heterogeneous effluent was in thermodynamical equilibrium (Thermodynamic Equilibrium) between described gas phase and liquid phase, this effluent also can directly transmit by the conveyance conduit between the superior and the subordinate's reactor.

Yet, some the reaction in, as hydrodesulfurization reaction (Hydrodesulphurization, HDS) in, the material component in the heterogeneous effluent is not in thermodynamic equilibrium state.At this moment, if the heterogeneous effluent of discharging from the upper level reactor directly is transported in the process of next stage reactor by conveyance conduit, material component wherein, the states such as dividing potential drop of component just may change, thereby the effluent of upper level reactor just can not keep the continuity or the uniformity of parameter of materials when entering in the next stage reactor.Like this, for the measurement of Catalytic processes and optimization, just may have bigger adverse effect.

In one embodiment of the present of invention as shown in Figure 3, it can well keep material transmission continuity or uniformity in the heterogeneous fluid transmission course.In the present embodiment, combined multi-stage piston flow reactor 707 can be laboratory scale piston flow reactor, and its reactor 71 and reactor 73 parallel to each other by two and series connection are formed.Definable reactor 71 is a first order reactor, and definition reactor 73 is a second level reactor.Be mounted with beds 72 and 74 in the reactor 71 and 73 respectively, be respectively arranged with temperature control equipment 701 and 702 on it, this temperature control equipment 701 can be identical with 702, also can be different.Raw material source 70 can be conveyed into raw material in first reactor 71 by feed line road 77.In the present embodiment, also be provided with a separator 703 at first reactor 71 and 73 of second level reactors.The exit of first order reactor 71 is provided with effluent pipeline 78, and it can link to each other with the inlet of described separator 703.Simultaneously, separator 703 is provided with gas-phase transport pipeline 75 and links to each other with the inlet of second level reactor 73 respectively with liquid phase conveyance conduit 76; The exit of second level reactor 73 also is provided with effluent pipeline 78.When reacting, raw material enters in the first order reactor 71 and reacts, the heterogeneous effluent of first order reactor enters in the described separator 703 and is separated into gaseous fluid and liquid phase fluid, subsequently, gaseous fluid and liquid phase fluid enter the reaction of carrying out next step in the reactor of the second level via gas-phase transport pipeline 75 and liquid phase conveyance conduit 76 respectively.

As shown in Figure 3, in an embodiment of the present invention, the flow resistance that a current-limiting apparatus 705 is controlled gaseous fluid is set on conveyance conduit 75, on gaseous fluid, to produce pressure differential.Suppose that the pressure on first order reactor 71 and the separator 703 is P1; At this moment, because the existence of current-limiting apparatus 705, the pressure of second level reactor 73 is P2 just, and P1＞P2.Like this, on gas-phase transport pipeline 75, just produced a pressure differential Δ P=P1-P2.Because the existence of pressure differential (pressure drop) Δ P, when this Δ P is enough to overcome the frictional force in the liquid phase conveyance conduit 76 and/or enters the gravity of the liquid phase fluid in the liquid phase liquid phase conveyance conduit 76, just can be pressed into liquid phase conveyance conduit 76 to liquid phase fluid and then enter in the second level reactor 73.It is very little and be unlikely to influence follow-up reaction like this, just can to drive liquid phase fluid and this pressure differential by means of the pressure differential Δ P that produces on the gaseous fluid.Described current-limiting apparatus 705 can be a flow-limiting valve, aditus laryngis or other current-limiting modes etc.Behind the gas-phase transport pipeline of selecting suitable dimension and shape, as capillary etc., this pipeline itself is also just controlled the flow resistance of gaseous fluid to play the effect of current limliting as current-limiting apparatus 705.

In addition, in the present embodiment, can be on current-limiting apparatus 705 or gas-phase transport pipeline 75 two ends be provided with the variation that differential pressure pickup (not shown) is measured pressure differential deltap P.By the physical characteristic of Δ P and gaseous fluid, just can calculate the information of gaseous substance.

Continuation is referring to shown in Figure 3, and when Δ P is too for a short time when being not enough to drive liquid phase fluid, described liquid phase fluid will constantly accumulation in separator 703; When Δ P was enough big, liquid phase fluid will constantly be pressed in the second level reactor 73 and all be pressed into up to all liquid phase fluids.In the time of in all liquid phase fluids all are pressed into second level reactor 73, gaseous fluid will enter in the second level reactor 73 from liquid phase conveyance conduit 76, like this, Δ P will descend, and liquid phase fluid will be accumulated again along with the carrying out of reaction and occupy liquid phase conveyance conduit 76.Δ P can return to predetermined value again subsequently, and liquid phase fluid can be pressed empty again.Like this, owing to be input to the raw material of first order reactor 71 and the limitation of reaction, often just be difficult in the balance of keeping liquid level 704 in the separator 703, and can not keep the liquid and gas fluid to supply uniformly, its flow is in the continuous fluctuation, is very disadvantageous to subsequent reactions like this.

In a preferred embodiment, in described separator 703, be provided with the variation that liquid level inductor 706 is used for monitoring liquid level 704, simultaneously, the signal of these liquid level inductor 706 outputs can be used to control described current-limiting apparatus 705, drive liquid phase fluid to produce suitable Δ P, so that liquid level 704 is in preposition.So just can avoid the fluctuation of liquid and gas fluid, be convenient to the carrying out of subsequent reactions.It is contactless, optics, laser induced etc. that described liquid level inductor can adopt.Be preferably and use the non-contact optical induction installation.Like this, when realizing that liquid phase substance by behind the stable supplying of liquid phase conveyance conduit 76, just can calculate the flow information of liquid phase fluid by the physical characteristic of Δ P and liquid phase fluid.

At some low pressure reactions, as the low pressure Fischer-Tropsch synthetic in, although pressure differential Δ P is very little, its also be this reaction can not bear, particularly big or when multistage reactor is arranged more when each stage reactor length, will cause whole pressure drop bigger, to the adverse influence that causes of reaction.In addition, owing to adjust pressure differential deltap P to keep liquid level 704 by liquid level inductor 706 and current-limiting apparatus 705.In the process of adjusting Δ P, just also might produce some influences, and then have influence on flowing of fluid in the first order reactor 71 pressure in the first order reactor 71.

Referring to shown in Figure 4, it is similar to embodiment shown in Figure 3.In the present embodiment, cancelled the current-limiting apparatus 705 that is arranged on the gas-phase transport pipeline 75.Owing to do not had the existence of current-limiting apparatus 705, just eliminated the pressure differential that produces owing to gas-phase transport pipeline 75.Simultaneously, be provided with a liquid pump 707 in liquid phase conveyance conduit 76 and carry liquid phase fluid, and can monitor the variation of liquid level 704 and its output signal is flowed to liquid pump 707 to keep liquid level 704 at a preposition by liquid level inductor 706, can guarantee the uniformity that liquid phase fluid flows like this.When the pressure on first order reactor 71 and the separator 703 was P1, the pressure of second level reactor 73 was P1 just also.Owing to do not had pressure differential on the gas-phase transport pipeline 75, adjust Δ P on the gas-phase transport pipeline 75 like that in order to keep liquid level 704 shown in also just needn't image pattern 3, thereby the pressure that has reduced in the reactor changes.Like this, just can eliminate under the situation that guarantee the liquid phase fluid steady flow, guarantee well carrying out of reaction in the pressure drop that reaches on the reactor between reactor.

In the present embodiment, described liquid pump 707 can be positive displacement pump (Positive displacement pump) or centrifugal pump (Centrifuge pump) etc., preferably uses positive displacement pump.Simultaneously, liquid pump 707 is preferably the function with measurement, so that the flow velocity of real-time detection liquid phase fluid.For liquid phase fluid is distributed in the second level reactor 73 uniformly, can in second level reactor 73, be provided with sprayer unit (not shown), be distributed in uniformly in the beds 74 thereby make after the liquid phase fluid of liquid phase conveyance conduit 76 conveyings enters first order reactor 73.In addition, in the present embodiment, also can be provided with check-valves (not shown) to prevent the liquid refluence in liquid phase conveyance conduit 76 in liquid pump 707 backs.

As seen, in an embodiment of the present invention, separate by heterogeneous effluent first order reactor 71, gaseous fluid and the interactional possibility of liquid phase fluid in course of conveying have been reduced, guaranteed continuity or uniformity in the material transmission, thereby multistage reactor just can better be simulated the performance of a beds of being made up of the beds of described multistage reactor.In addition, owing to separate, just can carry out sampling analysis to the component of effluent more accurately, thereby avoid traditional the heterogeneous fluid incomplete problem of sampling by 703 pairs of heterogeneous effluents of separator.

In some reactions, liquid phase fluid also is heterogeneous, and in synthesizing as Fischer-Tropsch, liquid phase fluid includes water and oil phase.At this moment, just may be provided with agitating device (not shown) in separator 703 has heterogeneous liquid phase fluid and stirs the uniformity of guaranteeing in the liquid phase fluid course of conveying fully to mix described.Described stirring can be adopted mechanical agitation, magnetic agitation etc.In a preferred embodiment, adopt the ultrasonic wave agitating device, this device can be installed on the position near separator 703 bottoms, and it can stir liquid phase fluid fully, reduces the interference of liquid level inductor 706 as much as possible and avoids because stirring increases the temperature of liquid phase fluid.

As shown in Figure 3-4, compare, when the temperature of separator 703 is high, enters in the liquid phase fluid in the separator 703 easily the component of volatilization and will volatilize and enter into gaseous fluid with the temperature of first order reactor 71 exit effluents; When the temperature of separator 703 was hanged down, condensation just may take place and enter into liquid phase fluid in a part of gaseous fluid.No matter as seen the temperature of separator 703 is high or low, all can the component or the state of the effluent fluid of coupled first order reactor be exerted an influence.Like this, the next stage reactor receives between the fluid that fluid and upper level reactor exit discharge variation has taken place, thereby just can not guarantee continuity or the uniformity of fluid at transport process.In order to keep the stable of effluent component and state, the temperature that is preferably the described separator 703 of maintenance is identical with the temperature of described first order reactor 71 exit effluents, enters described separator 703 interior its states with regard to the effluent that guarantees first reactor as much as possible like this and does not change.

As shown in Figure 5, with first order reactor 71 is example, for entering separator 703 back temperature, the effluent of better guaranteeing first order reactor 71 do not change, described first order reactor 71 and separator 703 are one-body molded, like this, separator 703 and first order reactor 71 are in the individual system, thereby can guarantee the unanimity of temperature, just the possibility of better having avoided component, state to change.

In embodiments of the present invention, described multistage piston flow reactor 707 also can be made up of three or more parallel to each other and reactors series connection.Described separator can be installed on the exit of each stage reactor, and itself and reactor are provided with separately respectively, even one-body molded setting, and can current-limiting apparatus is set on the gas-phase transport pipeline or the liquid pump is set on the liquid phase conveyance conduit according to different being reflected at.In addition, described a plurality of tandem reactor also can vertically be provided with.

Claims (15)

1. device that is used to develop commercial scale laminar flow Catalytic processes, it comprises laboratory scale first piston flow reactor, laboratory scale second piston flow reactor, fresh reactant thing source, first control valve, second control valve, first sampling valve and temperature control equipment; It all offers inlet and outlet described first and second reactor, and it all is mounted with catalyst bed, described fresh reactant thing source links to each other with the inlet of described first reactor, it is characterized in that: described first reactor and second reactor are provided with described temperature control equipment, in order to keep common controllable temperature environment, the effluent of described fresh reactant thing source and described first reactor links to each other with the inlet of described second reactor by described first control valve and described second control valve respectively, described first sampling valve is set to link to each other with the outlet of described first reactor and second reactor, its effluent is sampled respectively, when described second reactor under the operating condition of temperature identical and pressure with described first reactor, its conversion ratio is not more than 25% of the first reactor conversion ratio.

2. device as claimed in claim 1, it is characterized in that: described device also includes the facility that links to each other with described first sampling valve, and it is used to analyze the feature of described reactor effluent.

3. device as claimed in claim 1, it is characterized in that: described device also comprises laboratory scale the 3rd piston flow reactor, the 3rd control valve, the 4th control valve and second sampling valve, described the 3rd reactor offers inlet and outlet, and it is mounted with catalyst bed, described fresh reactant thing source links to each other with the inlet of described the 3rd reactor by the 3rd control valve, in order to import a certain amount of fresh reactant thing, the outlet of described first reactor also links to each other with the inlet of described the 3rd reactor by described the 4th control valve, be used to import the effluent of the first quantitative reactor, described the 3rd reactor also is provided with described temperature control equipment, in order to keep controlled temperature environment, described second sampling valve links to each other with the outlet of described the 3rd reactor, in order to the effluent of described the 3rd reactor is sampled, when described the 3rd reactor with the identical temperature of described first reactor, under the operating condition of pressure and mass rate, its conversion ratio is not more than 25% of the first reactor conversion ratio.

4. device as claimed in claim 1, it is characterized in that: described device also includes the feed source, and being used for provides other material to described second reactor.

5. device as claimed in claim 4, it is characterized in that: described other feed is included in product or the accessory substance that reacts and generated in described first and second reactor.

6. device as claimed in claim 4, it is characterized in that: described other feed comprises the pollutant in the fresh reactant thing.

7. device as claimed in claim 1, it is characterized in that: described device also includes heater, and it is used for heating the fresh reactant thing that provides to described second reactor from described fresh reactant thing source.

8. device as claimed in claim 1 is characterized in that: when described second reactor under the operating condition of temperature identical and pressure with described first reactor, its conversion ratio is between 5-20%.

9. method that is used to develop commercial scale laminar flow Catalytic processes, it comprises:

Enter the mouth and outlet in being provided with, and be mounted with the porch input fresh reactant thing of laboratory scale first piston flow reactor of catalyst bed;

In being provided with inlet and outlet, and the effluent and the fresh reactant thing of the first quantitative reactor imported in the porch that is mounted with laboratory scale second piston flow reactor of catalyst bed, when described second reactor under the operating condition of temperature, pressure and the mass rate identical with described first reactor, its conversion ratio is not more than 25% of the first reactor conversion ratio;

Measure the characteristic of described first and second reactor effluent, thereby infer characteristic relevant in the laminar flow catalytic reactor with top rake.

10. method as claimed in claim 9, it is characterized in that: the catalyst bed of described first reactor and second reactor comprises catalyst granules and inertia dilution particle, selects a certain amount of described inertia dilution particle to operate under isothermy in order to guarantee reactor.

11. method as claimed in claim 9, it is characterized in that: described method also is included in and is provided with inlet and outlet, and the effluent and the fresh reactant thing of the first quantitative reactor imported in the porch that is mounted with laboratory scale the 3rd piston flow reactor of catalyst bed, when described the 3rd reactor with the identical temperature of described first reactor, under the operating condition of pressure and mass flow rate, its conversion ratio is not more than 25% of the first reactor conversion ratio, in addition, measure the effluent of the 3rd reactor, thereby infer other characteristics relevant with the piston flow reactor system.

12. method as claimed in claim 10, it is characterized in that: described method also is included in one or more a certain amount of other materials of porch input in described second reactor and the 3rd reactor, in order to the reaction of the selected part in the catalyst bed of test piston flow reactor to these other materials.

13. a method as claimed in claim 12 is characterized in that: described other materials are reaction product or the byproducts of reaction that react in first reactor.

14. a method as claimed in claim 12 is characterized in that: described other materials are the pollutants that exist in the fresh reactant thing.

15. a method as claimed in claim 9 is characterized in that: described method also comprises samples to the effluent of described first and second reactor.

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