CN105259801B - The method and system and its application that a kind of atmosphere is steadily switched fast - Google Patents
The method and system and its application that a kind of atmosphere is steadily switched fast Download PDFInfo
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- CN105259801B CN105259801B CN201510639555.5A CN201510639555A CN105259801B CN 105259801 B CN105259801 B CN 105259801B CN 201510639555 A CN201510639555 A CN 201510639555A CN 105259801 B CN105259801 B CN 105259801B
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Abstract
The method and system and its application that a kind of atmosphere is steadily switched fast, can solve existing commutation valve system can not steadily replace atmosphere in microreactor quick and completely, and then the problem of the reliability of impact analysis process, repeatability and accuracy.The airflow-reversing unit of the present invention is switched fast the charge air flow flowed to the downstream；Inlet pressure controller and pressure transmitter jointly control the pressure difference nearly zero between charge air flow, make handoff procedure steadily quick.The concentration of component of the achievable downstream airflow of the present invention is steadily switched fast in a manner of close to ideal rectangle ripple.Present invention can apply to analyze the solid particle multistage reaction in-situ process based on atmosphere switching；And diffusion and the back-mixing of quantitatively characterizing microreactor interior air-flow.
Description
Technical field
The present invention relates to a kind of flow constituents switching method and system and its application, and in particular to a kind of atmosphere is steadily quick
Switching method and system and its application, belong to fluid control technology and chemical analysis technology field.
Background technology
Atmosphere (the component of gas is frequently involved in instrument system, chemical reaction analytical equipment and pyroreaction experimental provision
And concentration) Fast transforms or container conduit residual gas displacement.Prior art often using single or simple combination hand,
Automatic diverter valve realizes the commutation of air-flow, and then converts atmosphere or replace the residual gas of container conduit.These conventional meanses
Atmosphere displacement rapid (≤1s), completely (the 1 ‰ of residual volume≤concentration amount of switched), the small (pressure oscillation of fluctuation can not be met simultaneously
≤ 1 ‰, 2 DEG C of temperature fluctuation) performance requirement, and then can not meet that multistage gas-solid fast reaction analysis is wanted to atmosphere displacement
Ask.Normal conditions, the principal element for restricting the complete replacing velocity of gas is the structurally and operationally condition of container conduit；But near
Like the miniature vessel pipeline of laminar flow, the performance for the valve system that commutates will significantly affect the speed and stationarity of gas displacement, and
The stability of the pressure and temperature of system.
Chinese Patent Application No. is CN201510175580.2, Publication No. CN104749206A, publication date are 2015 7
The moon 1, priority date disclose for the application for a patent for invention on April 14th, 2014《A kind of gas-solid reaction based on original position decoupling
Analytical equipment and analysis method》；The original position of multistage reaction is realized in the invention using atmosphere commutation instants and temperature quick regulation
Decoupling Analysis, gas-solid reaction is can obtain from taking place to the gas release sequence of reaction end overall process, and then resolving reaction
Process；The invention is applied to numerous gas-solid reaction process analysis procedure analyses with multistage response feature；It is newest original in this field
Property invention.But for the reaction that reaction speed is very fast, the reaction time is more important less than 20s or initial reaction stage process, existing gas
The performance of atmosphere handoff technique will significantly affect the concentration and system pressure stability of reactive gas species, so as to significantly affect initial stage
Course of reaction (conversion ratio 0~30%), and then the reliability of impact analysis method and process.Therefore conventional switch means can not protect
Demonstrate,prove reliability, repeatability and the accuracy of analysis process.
For example, grain diameter is usual in the reaction time that higher than 700 DEG C conditions are burnt less than 100 μm of carbon-based solid fuel
It is shorter than 60s, and reacts that to start to reach the most fast time to burn rate be typically 1~3s；Switched using atmosphere and start particle combustion
Just need to switch to combustion gas by most fast (≤1s), in a manner of most steady (state such as pressure, temperature is without fluctuation) by atmosphere during burning
Atmosphere, ensure burning be it is determined that, it is known and controllable under conditions of carry out.
Chinese Patent Application No. is CN201410148319.9, Publication No. CN103908928A, publication date are 2014 7
The application for a patent for invention on the moon 8 discloses《A kind of decoupling reactor based on atmosphere switching》；The invention make it that reactor is approximate
Laminar flow, it is switched fast beneficial to atmosphere in reactor, so as to beneficial to the Decoupling Analysis in situ for realizing multistage reaction.Foregoing two
The application practice that technology is combined shows, is connected using the routine in the field, even if being less than using the preferable response time
10ms, valve body effective drift diameter are less than 2mm miniature electromagnetic valve, the rising of reactor afterbody atmosphere handoff procedure gas component concentrations
Time (τ0.99) still greater than 3.5s；The time is obviously unsatisfactory for the requirement that atmosphere switching starts multistage response analysis, it is impossible to protects
Demonstrate,prove reliability, repeatability and the accuracy of result.
Atmosphere is quick in chemical reaction analytical equipment, replaces completely, or analysis carbon-based fuel combustion of solid etc. is with more
Elementary reaction feature and the faster course of reaction of reaction speed are, it is necessary to realize gas concentration rising edge and concentration trailing edge close to reason
The rectangle concentration peak thought, and then reliable, stable reaction atmosphere is provided for each stage of reaction.Therefore, it is necessary to develop high-performance
The steady fast switching system of atmosphere, it is most important that it reacts the multistage development of Decoupling Analysis technology in situ.
In addition, residence time distribution curve, i.e. RTD curves, the mixed characteristic of fluid in actual chemical reactor can be characterized,
The flowing in reactor and reaction condition are described available for founding mathematical models, be reactor and its operate with it is important according to
According to；Therefore, the important process that RTD curves are chemical reactors is obtained.Conventional impulse method and step method, which inject tracer, to react
In device, detection reactor exit tracer concentration changes with time to obtain RTD curves.Impulse method normal open excess pressure at present
(syringe or pulse compression gas) make minimum gas enter reactor (such as：Journal of Chemical Industry and Engineering, 2013,64 (3):867-876).It is right
The pressure of tracer and initial flow rate will cause original flow field that larger fluctuation and repetition occurs in microreactor, this method
Property it is difficult to ensure that, need many experiments to be averaging (general more than 20 times), this method is being applied to Per>=30 situation is likely to
Cause test result inaccurate reliable and cumbersome, time-consuming with data processing for experiment.Step method (such as：
Combustionand Flame,2011,158:1638-1645) be another residence time destribution characteristic research method.Rank
Jump method realizes the step of air-flow concentration using magnetic valve or six-way valve, but at present used by step method disclosed in domestic and foreign literature
Gas handoff technique can not answer pairing approximation laminar flow (such as Per>=30) system.Therefore, the residence time of microreactor point
Cloth curve needs to develop more high performance gas concentration impulse generator or air-flow switching system.
The content of the invention
The present inventor is directed to listed problem in background technology and has carried out system and in-depth study.Examined by experiment
Survey and analysis, inventor have found that the gas concentration that the outlet of atmosphere switching system is actual under different situations rises not rapid enough, switching
The time that concentration is thoroughly stablized afterwards is longer, at least one of mainly following four aspect of its reason：When to be switched state
Multichannel air flow rate has big difference (such as more than twice), and this can cause re-starts compared with handoff procedure pipeline each point flow and pressure
Distribution produces fluctuation, and then causes handoff procedure unstable；Second, be passed through the air-flow pressure head of reactor apparently higher than or be less than
The pressure head of air-flow is emptied, causes gas pressure and flow concussion in handoff procedure system and then fluctuation and slowly stabilization occurs；Three
It is that reversal valve combination is not excellent, has used threeway or multiple-pass joint to carry out connecting line so that pipeline has obvious dead band
Volume, new air-flow can not cause gas slowly in dead space volume to spread by scavenging pipeline completely；Needed so as to cause concentration thoroughly to be stablized
The time wanted lengthens；Fourth, actual internal area catastrophe point is excessive in valve body and pipeline, or the actual internal area and pipeline of pipeline
Actual internal area have big difference, cause whirlpool or dead space volume occur, so as to which back-mixing and diffusion occur, to cause concentration complete
The stable time needed lengthens.
Based on the studies above, the present invention steadily can not replace minisize reaction quick and completely to solve existing commutation valve system
Atmosphere in device, and then the problem of the reliability of impact analysis process, repeatability and accuracy, and then propose that a kind of atmosphere is steadily fast
The method and system of speed switching and its application.
The present invention provides a kind of method that atmosphere is steadily switched fast to solve the above problems, and methods described is to be based on two
Come what is realized, two-way charge air flow A, B passes through simple tube for road charge air flow A, B, all the way outlet air-flow and at least one magnetic valve
Road and the airflow-reversing unit being made up of two direct-acting electromagnetic valves of one and the above, are connected to outlet air-flow and air-discharging
Stream；Continuously and stably inlet air flow stream reversing unit, airflow-reversing unit switch two-way charge air flow A, B to two-way charge air flow A, B,
Chronologically set and form outlet air-flow and emptying air-flow respectively, realize that air-flow is switched fast；Two-way is detected using pressure transmitter
The pressure state of charge air flow A, B, the back pressure of emptying air-flow is adjusted using inlet pressure controller, makes two-way charge air flow A, B
Pressure state it is identical so that in air-flow handoff procedure, the pressure and stability of flow of two-way charge air flow A, B；And then realize
The atmosphere of outlet air-flow is steadily switched fast.
The present invention additionally provides a kind of steady fast switching system of atmosphere to solve the above problems, and the switching system includes
Two air inlets, a gas outlet, two air inlets connect two-way charge air flow A, B respectively, and two-way charge air flow A, B passes through letter
Single-pipeline and air-flow reversing unit are connected to gas outlet and evacuation port, and the airflow-reversing unit includes at least one two direct acting
Formula magnetic valve, the gas outlet connect downstream gas circuit；Two-way charge air flow A, B continuously and stably inlet air flow stream reversing unit, gas
Reversing unit switching two-way charge air flow A, B is flowed, two-way charge air flow A, B is chronologically set and flows to gas outlet and emptying respectively
Mouthful, the switching of downstream atmosphere is realized, the interior Y-shaped runner close to gas outlet of the airflow-reversing unit is provided centrally with two
The reversing valve core of direct-acting electromagnetic valve；The air inlet of the evacuation port connection inlet pressure controller, inlet pressure controller
Gas outlet empties；Pressure transmitter is connected between two-way charge air flow A, B；Inlet pressure controller is used to adjust emptying air-flow
Back pressure, make pressure transmitter detect differential pressure value nearly zero, that is, ensure two-way charge air flow pressure state it is identical.
Switch the atmosphere in microreactor steadily, quickly, completely using the steady fast switching system of atmosphere of the present invention,
Specifically：The gas outlet of the steady fast switching system of atmosphere of the present invention is connected to microreactor；Atmosphere is steadily quick
The power of electromagnetic valve line of switching system is connected to the output switch parameter interface of programmable controller；Programmable controller and computer
Communicated by communication cable；According to atmosphere switch need set magnetic valve switching electricity sequential in a computer；Set micro-
Type reactor, and flow into the state of Z (Z >=2) road air-flow of the steady fast switching system of atmosphere；Then trigger magnetic valve it is logical,
Power-down procedure completes atmosphere handoff procedure；Flow area equivalent diameter D≤40mm of each section of the microreactor；The atmosphere
Steadily operation length L≤1200mm, the pipeline between the gas outlet of fast switching system and the conversion zone of the microreactor
Inner volume V≤100mL；Z (Z >=2) road air flow rate is arranged so that the apparent speed of air-flow of each section of the microreactor
Angle value is located at 0.05~20m/s scopes；By above-mentioned technical method complete microreactor in atmosphere it is steady, quick, complete
Switching.
The present invention compared with prior art, it is the most prominent the characteristics of and significant beneficial effect be：Using two direct acting
Formula magnetic valve causes the mechanism for converting atmosphere the execution time to be shorter than 10ms；The atmosphere switch unit of the present invention can realize flow trim
Two-way charge air flow chronologically alternately flow into downstream gas circuit or emptying；Close to the Y-shaped stream of gas outlet in airflow-reversing unit
The reversing valve core for being provided centrally with two direct-acting electromagnetic valves in road, the connected mode of this pipeline avoid depositing for pipeline bypass
, and then dead volume is avoided, after farthest ensure that switching action performs preceding and execution, the gas flowing in pipeline is
Piston flow, make gas displacement quick, thorough；Pressure difference nearly zero between pre-cut scavenging flow is made using inlet pressure controller, so as to cut
Change moment, the disturbance of the stream condition parameter such as pressure, flow is minimum so that atmosphere immediate stability is to dbjective state after switching；It is comprehensive
Upper effect, the present invention can preferably be used for the steady of atmosphere and be switched fast, it is possible to achieve the concentration of component of downstream atmosphere is with close
Preferable square wave mode switches over；And then optimal atmosphere handoff technique side is provided for instrument system or high-end science apparatus
Case.Application process, system of the invention can solve the problems, such as that atmosphere is steadily switched fast in microreactor, and then directly promote
Enter the development of multistage reaction Decoupling Analysis technology in situ；It can also be that convenient acquisition microreactor is reliable, accurately stop
Time distribution curve provides safeguard, and then diffusion and the back-mixing characteristics of quantitatively characterizing microreactor interior air-flow.
Brief description of the drawings
Fig. 1 illustrates that the basic structure of the steady fast switching system of atmosphere of the present invention；Fig. 2 is basic structure
Connection diagram when airflow-reversing unit is made up of three two-position three way direct-acting electromagnetic valves；Fig. 3 is the gas of basic structure
Connection diagram when stream reversing unit is made up of a two-position four-way direct-acting electromagnetic valve；Fig. 4 is the air-flow of basic structure
Connection diagram when reversing unit is made up of a two-position five-way direct-acting electromagnetic valve；Fig. 5 is become using the individual pressure of X (X=2)
Device is sent to detect the connection diagram of X (X=2) road stream pressure state respectively；Fig. 6 is to expand to increase on the basis of basic structure
Add the structural representation of the individual airflow-reversing units of N (N=2)；Fig. 7 is that increase N (N=2) is expanded on the basis of system shown in Figure 2
The structural representation of individual same airflow reversing unit；Fig. 8 is that expansion increase N (N=2) is individual not on the basis of system shown in Figure 2
With the structural representation of pattern airflow-reversing unit；Fig. 9 is the method signal using atmosphere in present invention switching microreactor
Figure.Figure 10 is using technical solution of the present invention and the comparing result using gas performance of handoffs in routine techniques microreactor；
Figure 11 is the repeated result that impulse method surveys RTD curves, and in figure, abscissa represents time, longitudinal axis Im(t) (Torr) is Process Gas
The concentration-response that body analytical equipment (this experiment uses process mass spectrograph) obtains, the response and concentration value are proportional.
Specific embodiment
Specific embodiment one：Illustrate present embodiment with reference to Fig. 1, present embodiment provides a kind of atmosphere and steadily quickly cut
Method and system are changed, methods described is come real based on two-way charge air flow A and B, all the way outlet air-flow and at least one magnetic valve
Existing, the air-flow that two-way charge air flow A, B forms by simple pipeline and by two direct-acting electromagnetic valves of one and the above changes
To unit 1, outlet air-flow and emptying air-flow are connected to；Two-way charge air flow A, B continuously and stably inlet air flow stream reversing unit 1,
Airflow-reversing unit 1 switches two-way charge air flow (A, B), chronologically sets and forms outlet air-flow and emptying air-flow respectively, realizes
Air-flow is switched fast；Using the pressure state of pressure transmitter detection two-way charge air flow A, B, adjusted using inlet pressure controller
The back pressure of section emptying air-flow, makes the pressure state of two-way charge air flow A, B identical so that in air-flow handoff procedure, two-way enters
Gas air-flow A, B pressure and stability of flow；And then realize that the atmosphere of outlet air-flow is steadily switched fast.It is above is described steady fast
The engineering philosophy that speed switching atmosphere is followed.
A kind of steady fast switching system of atmosphere, the switching system include two air inlets, a gas outlet, and two are entered
Gas port connects two-way charge air flow A and B respectively, and two-way charge air flow A, B is connected to by simple pipeline and air-flow reversing unit 1
Gas outlet and evacuation port, the airflow-reversing unit 1 includes at least one two direct-acting electromagnetic valves, under the gas outlet connection
Faint breath road；Continuously and stably inlet air flow stream reversing unit 1, airflow-reversing unit 1 switch two-way air inlet gas to two-way charge air flow A, B
A, B are flowed, two-way charge air flow A, B is chronologically set and flows to gas outlet and evacuation port respectively, realize the switching of downstream atmosphere, institute
State the reversing valve core for being provided centrally with two direct-acting electromagnetic valves of the interior Y-shaped runner close to gas outlet of airflow-reversing unit 1；
The air inlet of the evacuation port connection inlet pressure controller 2, the gas outlet emptying of inlet pressure controller 2；The two-way enters
Pressure transmitter 3 is connected between gas air-flow A, B；Inlet pressure controller 2 is used for the back pressure for adjusting emptying air-flow, makes pressure transmitter
The differential pressure value nearly zero of 3 detections, that is, ensure that the pressure state of two-way charge air flow A, B is identical.
Make it that the execution that atmosphere switches is most rapid using two direct-acting electromagnetic valves, and economic, reliable, repeatability height；Gas
The reversing valve core for being provided centrally with two direct-acting electromagnetic valves of the interior Y-shaped runner close to gas outlet of reversing unit 1 is flowed, it is this
The connected mode of pipeline can realize air-flow switching and avoid pipeline dead volume, and the gas in pipeline flows approximate piston flow all the time,
Quickly, thoroughly replaced beneficial to gas；Jointly control the pressure between charge air flow with inlet pressure controller 2 and pressure transmitter 3
Difference nearly zero, makes the perturbation amplitude of the pipeline conditions parameter such as switching instantaneous pressure, flow minimum so that atmosphere can be steady rapidly after switching
Determine to dbjective state.To sum up effect, the technical scheme can preferably be used for the steady of atmosphere and be switched fast, it is possible to achieve lower faint breath
The concentration of component of atmosphere switches in a manner of close to preferable square wave, and then is provided most for instrument system or high-end science apparatus
Good atmosphere handoff technique scheme.The system can solve the problems, such as that atmosphere is steadily switched fast in microreactor, Jin Erzhi
Connect the development for promoting the multistage to react Decoupling Analysis technology in situ.The system can also be convenient acquisition microreactor it is reliable,
Accurate residence time destribution (RTD) curve provides safeguard, and then diffusion and the back-mixing of quantitatively characterizing microreactor interior air-flow
Feature.
Specific embodiment two：Illustrate present embodiment with reference to Fig. 1, in present embodiment, the switching system inner flow passage
Effective drift diameter be 1mm~4mm.It is arranged such, rationally improves air velocity, and makes Bottomhole pressure closer to like piston flow,
Therefore the residual of pipe interior air-flow after handover can be slowed down, and then accelerate the speed of atmosphere switching, and it is to use to be easy to manufacture.This
The other compositions and annexation of embodiment are identical with embodiment one.
Specific embodiment three：Illustrate present embodiment with reference to Fig. 1, in present embodiment, the difference of the pressure transmitter 3
It is the differential pressure by the inlet pressure controller 2 to the Real-time Feedback of pressure transmitter 3 in -100Pa~100Pa to press value stabilization
Value carries out negative-feedback and automatically adjusted to realize.It is arranged such, intelligently controls the pressure difference nearly zero between charge air flow (A, B)；Make to cut
The perturbation amplitude for changing the pipeline conditions parameter such as instantaneous pressure, flow minimizes so that atmosphere immediate stability is to target after switching
State, so that reliability, repeatability and the accuracy of atmosphere switching greatly improve；It is and easy to operate and use.This embodiment party
The other compositions and annexation of case are identical with embodiment one or two.
Specific embodiment four：Illustrate present embodiment with reference to Fig. 1 and Fig. 2, the airflow-reversing unit of present embodiment by
Three two-position three way direct-acting electromagnetic valve compositions, the Heng Tong gas port of two of which magnetic valve 4 and 5 make the airflow-reversing unit 1
Two air inlets, connect two-way charge air flow A and B respectively, one of one of magnetic valve 4 switching gas port and magnetic valve 5 cuts
Ventilation mouth be connected with two of magnetic valve 6 switching gas ports respectively, and another of magnetic valve 4 switches the another of gas port and magnetic valve 5
Outer switching gas port, which confluxes, makees the evacuation port of the airflow-reversing unit 1, and the Heng Tong gas port of magnetic valve 6 makees the airflow-reversing
The gas outlet of unit 1.
Charge air flow A and B flow are set to zero from arranges value in pipeline, then from acyclic homologically trioial be arranges value, it is necessary to purge pipeline
Residual gas in system, the thorough stabilization of flow, pressure and air-flow component need the long period；And downstream pipe is likely to relate to
And during the disassembling operations to pipeline, particularly downstream connection chemical reactor, many situations need frequently to change material or tune
Whole installation.Therefore set by the present embodiment, can control the switching electricity condition of three two-position three way direct-acting electromagnetic valves to cause two
Road charge air flow is not passed through downstream, and is flowed out from evacuation port；It is easy to the dismounting and adjustment of downstream pipe, container.By this implementation
Scheme, it is also convenient for manufacturing and uses.Other compositions and annexation of the present embodiment and embodiment one, two or three-phase
Together.
Specific embodiment five：Illustrate present embodiment with reference to Fig. 1 and Fig. 3, the airflow-reversing unit of present embodiment is
One two-position four-way direct-acting electromagnetic valve 7；Two air inlets of magnetic valve 7 connect two-way charge air flow A, B respectively；Magnetic valve 7
Gas outlet connection downstream gas circuit；The air inlet of the exhaust outlet connection inlet pressure controller 2 of magnetic valve 7.It is arranged such, it is maximum
Reduce to degree magnetic valve quantity, reduce manufacturing cost, simplify connection, be easy to use.Other groups of the present embodiment
Into identical with embodiment one, two or three with annexation.
Specific embodiment six：Illustrate present embodiment with reference to Fig. 1 and Fig. 4, the airflow-reversing unit of present embodiment is
One two-position five-way direct-acting electromagnetic valve 8；Two air inlets of the magnetic valve 8 connect two-way charge air flow A, B respectively；It is described
The gas outlet connection downstream gas circuit of magnetic valve 8；Two exhaust outlets of the magnetic valve 8 connect inlet pressure controller 2 after confluxing
Air inlet.It is arranged such, farthest reduces magnetic valve quantity, reduces manufacturing cost, while simplify to electromagnetism
The technical requirements of valve inner flow passage, reduce body size and be easy to manufacture.Other compositions and annexation of the present embodiment with
Embodiment one, two or three are identical.
Specific embodiment seven：Illustrate present embodiment, two direct-acting electromagnetic valves of present embodiment with reference to Fig. 1~4
Valve element be balanced type poppet valve core.It is arranged such, each road air-flow is of equal value, is easy to flexibly use.Other groups of the present embodiment
Into identical with embodiment four, five or six with annexation.
Specific embodiment eight：Illustrate present embodiment with reference to Fig. 1~4, the magnetic valve of this implementation is short stroke, fast-response
Magnetic valve；The energization response time of the magnetic valve is less than 4ms, and the power-off response time is less than 2ms.It is arranged such, is easy to implement
The switching of more speed, residence time distribution curve is set to realize high reliability, repeatability and accuracy.The present embodiment its
It forms identical with embodiment four, five, six or seven with annexation.
Specific embodiment nine：With reference to the explanation present embodiment of Fig. 1~5, the side of pressure difference between this examinations charge air flow
Formula is in every all separately installed pressure transmitter in charge air flow all the way, and then the pressure of the every charge air flow all the way of collection
Value, manually or automatically pressure differential of the contrast per charge air flow all the way, and then adjust inlet pressure controller 2, controls air inlet
Pressure difference nearly zero between air-flow A, B；The technical implementation way of pressure difference instead of specific implementation between the present embodiment detection charge air flow
By the technical scheme of installation pressure transmitter between charge air flow in scheme one to eight.It is arranged such, is easily installed.This embodiment party
The other parts composition and annexation of case are identical with any embodiment in embodiment one to eight.
Specific embodiment ten：Illustrate present embodiment with reference to Fig. 1~6, the atmosphere switching system of present embodiment is also wrapped
Include the airflow-reversing unit of N number of extension, N >=1；Often increase the airflow-reversing unit of an extension, its gas outlet is connected to
One air inlet of the airflow-reversing unit of installation.
More specifically, Fig. 6 illustrates N=2, that is, increase by two airflow-reversing units and realize that four tunnel charge air flows are steadily quick
The concrete technical scheme of switching.Application method is that switching action, setting switching sequence are that A1 or A2 switches to B1 or B2 each time,
Or B1 or B2 switch to A1 or A2；Simultaneously before the action of airflow-reversing unit 1, airflow-reversing unit 1 and 2 is set to act,
So that the charge air flow of pre-switch flow to the evacuation port of airflow-reversing unit 1 before the action of airflow-reversing unit 1.
The embodiment can realize that the steady of N+2 (N >=1) road air-flow is switched fast；And then promote any multistage reaction
The further development of Decoupling Analysis technology in situ.Other compositions and annexation of the present embodiment and embodiment one to
Any embodiment is identical in nine.
Specific embodiment 11：Illustrate present embodiment with reference to Fig. 6~8, present embodiment extends increased air-flow and changed
To the type of magnetic valve used in unit be two-position three way direct-acting electromagnetic valve, two-position four-way direct-acting electromagnetic valve, two-position five-way it is straight
One or both of type solenoid valve or three kinds.It is arranged such, is easy to connection, flexible Application.
It is particularly preferred that the airflow-reversing unit 1 in the steady fast switching system downstream of connection atmosphere is by three two-position three ways
Direct-acting electromagnetic valve forms, and annexation is the same as specific embodiment four；Extend magnetic valve used in increased airflow-reversing unit
Type is one kind in two-position four-way direct-acting electromagnetic valve and two-position five-way direct-acting electromagnetic valve.It is arranged such, both reduces electricity
Magnet valve quantity, can set again makes all air-flows obstructed magnetic valve switching electricity condition downstream.The present embodiment it is other
Composition and annexation are identical with embodiment ten.
Specific embodiment 12：Illustrate present embodiment with reference to Fig. 9 and Figure 10, present embodiment is by a kind of described gas
The steady fast switching system of atmosphere is used for atmosphere steady, quick, completely in switching microreactor；Specific Implementation Technology
It is：
The gas outlet of the steady fast switching system of atmosphere of the present invention is connected to microreactor；Atmosphere is steadily quick
The power of electromagnetic valve line of switching system is connected to the output switch parameter interface of programmable controller；Programmable controller and computer
Communicated by communication cable；
According to atmosphere switch need set magnetic valve switching electricity sequential in a computer；Set microreactor,
And flow into the state of Z (Z >=2) road air-flow of the steady fast switching system of atmosphere；Then it is complete to trigger magnetic valve switching electricity program
Into atmosphere handoff procedure；
Equivalent diameter D≤40mm of the flow area of each section of the microreactor；The atmosphere, which is steadily switched fast, is
Operation length L≤1200mm, pipeline inner volume V≤100mL between the conversion zone of the gas outlet of system and the microreactor；
Z (Z >=2) road air flow rate be arranged so that the apparent velocity amplitude of air-flow of each section of the microreactor positioned at 0.05~
20m/s scopes.
Steady, quick, the complete switching of atmosphere in microreactor is completed by above-mentioned technical method.
Figure 10 is the instance data that the embodiment switches atmosphere in the microreactor of 900 DEG C of conditions.The example
It it is on July 9th, 2014 by CN201410148319.9, Publication No. CN103908928A, publication date of Chinese Patent Application No.
Application for a patent for invention《A kind of decoupling reactor based on atmosphere switching》Atmosphere switches to reality in disclosed microreactor
Example.It compared for of the invention (not using the connection of the present invention with existing conventional airflow-reversing technology and not controlling by experiment test
The nearly more excellent effect zero) each reached of pressure difference between charge air flow.Application background is the carbon-based combustion of solid of tissue microreactor
Expect the decoupling burning in situ of particle, it is necessary to which Ar is switched into 15%O2/ 85%Ar.Because coke burns most rapid rate in 1~3s
(temperature is more high shorter) place occurs；Therefore it is required that time (the τ that the conversion zone gas concentration of microreactor rises and stablized0.99)
It is shorter than 1s.
Figure 10 is that the embodiment exports detection O in microreactor2Time (the τ that concentration rises and stablized0.99).Can be with
Find out the steady fast switching system of atmosphere using the present invention, O2Concentration rises and thoroughly stable time (τ0.99) it is shorter than 1s (buttons
Except about 0.5s after the intrinsic backmix effect of mass spectrum capillary sampling pipe).And use routine techniques O2What concentration rose and thoroughly stablized
Time (τ0.99) it is 6~8s (about 5~7.5s after the deduction intrinsic backmix effect of mass spectrum capillary sampling pipe), process O2Concentration rises
To O2Time (τ between the thorough stabilization of concentration0.99) in section, O2Concentration is uncertain, be it is uncontrollable and unknowable, therefore
Time (τ0.99) it is longer than the time (general 1~3s temperature is more high shorter) that coke burning most rapid rate occurs, it can cause to test number
According to extremely unreliable, test result can not reflect understand, true O2Reaction rule under concentration.In summary, routine techniques can not
Meet the requirement that decoupling burning in situ switches to atmosphere.And the present invention can meet above-mentioned requirements comprehensively, so beneficial to deeper into
The intrinsic response characteristic of the carbon-based fuel particle of solid is analyzed on ground, and the decoupling burning rule in situ to study close to real industrial provides
More accurately course of reaction data.
Specific embodiment 13：Illustrate present embodiment with reference to Fig. 9, present embodiment equals a kind of atmosphere of the present invention
Steady fast switching system is used to analyze the multistage reaction in-situ process that solid particle is switched based on atmosphere；The microreactor
Each section is pipe and internal diameter is 2mm~25mm；The gas outlet of the steady fast switching system of atmosphere and the microreactor
Conversion zone between operation length L≤400mm, pipeline inner volume V≤20mL；Contain in the conversion zone of the microreactor
Solid-state reactants；Z (Z >=2) road air flow rate is arranged so that the apparent velocity amplitude of air-flow of each section of the microreactor
Positioned at 0.05~5m/s scopes；
The microreactor connection procedure gas analyzing apparatus；The sampling pipe of the process gas analytical equipment is internal diameter
Capillary sampling pipe less than 200 μm, the frequency of detection and the record gas concentration response of process gas analytical equipment are higher than 2HZ；
Operation length L≤800mm, pipeline inner volume V between the conversion zone of the microreactor and the thief hatch of capillary sampling pipe
≤50mL；
The NM other operations of the present embodiment are identical with embodiment 12.
Steady, quick, the complete switching of atmosphere in microreactor is completed by above-mentioned technical method；Switched each time
Journey, the transformation period of the gas component concentrations of reactor reaction section are shorter than 0.5s；Reaction cutting by atmosphere in microreactor
Change and be divided into M (M >=2) the individual stage, detect and record gas concentration response by process gas analytical equipment come in analysis reactor
Switch course of reaction occurred with atmosphere, and calculate quantitative result；Realize that the carbon-based fuel particle of solid is cut based on atmosphere with this
The analysis test of any multistage reaction in-situ changed.
Specific embodiment 14：With reference to Fig. 9 and explanation present embodiment, present embodiment by the present invention a kind of atmosphere
Steady fast switching system is used for diffusion and the back-mixing characteristics of quantitatively characterizing microreactor interior air-flow；The microreactor is each
The equivalent diameter of the flow area of section is 2mm~30mm；The gas outlet of the steady fast switching system of atmosphere and described miniature
Operation length L≤400mm, pipeline inner volume V≤20mL between the conversion zone of reactor；Z (Z >=2) road air flow rate
It is arranged so that the apparent velocity amplitude of air-flow of each section of the microreactor is located at 0.05~5m/s scopes；
The microreactor connection procedure gas analyzing apparatus；The sampling pipe of the process gas analytical equipment is internal diameter
Capillary sampling pipe less than 200 μm, the frequency of detection and the record gas concentration response of process gas analytical equipment are higher than 5HZ；
Operation length L≤800mm, pipeline inner volume V between the conversion zone of the microreactor and the thief hatch of capillary sampling pipe
≤50mL；
The output switch parameter of the programmable controller exports for transistor DC 24V, and the response of output point switching electricity
Time≤1ms；It is A-B-A to set and be passed through the sequential of microreactor interior air-flow, B air-flows component containing tracer and tracer component
Volumetric concentration≤10%；The residence time distribution curve of tracer component, i.e. RTD curves are obtained by this kind of air-flow handoff procedure；
Then the zero dimension variance of RTD curves is calculated；Finally calculate the Peclet numbers of microreactor, i.e. iterative following equation
In Per：
In formula：Represent the zero dimension variance of RTD curve of the tracer component in microreactor；Represent microreactor
Peclet numbers, the relative size of convective mass transfer speed and diffusion mass transfer speed is characterized, i.e. air-flow component is in microreactor
Diffusion and back-mixing degree, bigger sign back-mixing degree is smaller, air-flow is closer to like laminar flow.
The NM other operations of the present embodiment are identical with embodiment 12.
Diffusion and back-mixing characteristics by above method quantitatively characterizing microreactor interior air-flow.Peclet numbers are bigger, micro-
Type reactor exit detects the obtained smaller (Pe of concentration curve distortion levelrWhen being wider than 5s more than 50, concentration peak, concentration
The distortion of detection can be neglected).
Specific embodiment 15：Illustrate present embodiment with reference to Fig. 9, a kind of atmosphere described in present embodiment is steadily fast
The application process of fast switching system, tested using step method and obtain RTD curves；When each section of flow area of the microreactor
Equivalent diameter be 20mm~30mm, and when the inner volume of microreactor is 40mL~70mL, the air-flow switching is A-B-A
The time of process is arranged to 10s~200s；When each section of flow area of the microreactor equivalent diameter for 2mm~
20mm, and when the inner volume of microreactor is 10mL~40mL, the air-flow switching is the time of A-B-A processes to be arranged to 5s
~200s.The embodiment measures the Pe of microreactorrSimple to operate, Data Post is easy.The present embodiment does not refer to
Other operations it is identical with embodiment 14.
Specific embodiment 16：Illustrate present embodiment, a kind of atmosphere described in present embodiment with reference to Fig. 9 and Figure 11
The application of steady fast switching system, tested using impulse method and obtain RTD curves；When each section of circulation of the microreactor is cut
The equivalent diameter in face is 20mm~30mm, and when the inner volume of microreactor is 40mL~70mL, the air-flow switching is A-
The time of B-A processes is arranged to 200ms~800ms；When the equivalent diameter of each section of flow area of the microreactor is 2mm
~20mm, and when the inner volume of microreactor is 10mL~40mL, the air-flow switching is to be arranged to the time of A-B-A processes
80ms~400ms.The missing gas injection of the embodiment is rapid and minimum to pipeline flow disturbance, measures the Pe of microreactorr
It is time-consuming it is short, conventional efficient is high, gas tracer dosage is few, Data Post is easy, reliable results.The present embodiment is NM
Other operations are identical with embodiment 14.
Figure 11 is that the embodiment tests under the conditions of 900 DEG C the diffusion of microreactor interior air-flow and one of back-mixing characteristics
Instance data.Tested using impulse method and obtain RTD curves；The time of A-B-A processes is arranged to 200ms；A is Ar, B 10%
CO2/ 90%Ar.Longitudinal axis I in figurem(t) (Torr) it is dense to be that process gas analytical equipment (this experiment uses process mass spectrograph) obtains
Degree response, the response and concentration value are proportional.From experimental measurements as can be seen that what microreactor outlet detected
CO2Concentration peak repeatability is fabulous, calculates Pe using the result tested three times respectivelyr, it is as a result Per=87 ± 0.2.Prove the reality
Applying scheme has higher reliability and accuracy.In addition, the process of present embodiment pulsing is to the air-flow in reactor
Flow effect is minimum, and the state parameter such as reactor pressure, flow, temperature does not disturb, therefore the embodiment can obtain
Relatively reliable and accurate impulse method RTD curves are obtained, (stream condition such as stream field and pressure, flow has relative to routine techniques
Compared with large disturbances) there is unrivaled advantage.
Claims (13)
1. a kind of method that atmosphere is steadily switched fast, methods described is to be based on two-way charge air flow (A, B), all the way outlet air-flow
Realized with least one magnetic valve, it is characterised in that：Two-way charge air flow (A, B) by simple pipeline and by one and with
On two direct-acting electromagnetic valves composition airflow-reversing unit (1), be connected to outlet air-flow and emptying air-flow；Two-way air inlet gas
(A, B) continuously and stably inlet air flow stream reversing unit (1) is flowed, airflow-reversing unit (1) switching two-way charge air flow (A, B), is pressed
Sequential is set forms outlet air-flow and emptying air-flow respectively, realizes that air-flow is switched fast；Entered using pressure transmitter detection two-way
The pressure state of gas air-flow (A, B), using inlet pressure controller adjust emptying air-flow back pressure, make two-way charge air flow (A,
B pressure state) is identical so that in air-flow handoff procedure, the pressure and stability of flow of two-way charge air flow (A, B)；And then
Realize that the atmosphere of outlet air-flow is steadily switched fast.
2. a kind of steady fast switching system of atmosphere, the switching system includes two air inlets, a gas outlet, and its feature exists
In：
Two air inlets connect two-way charge air flow (A, B) respectively, and two-way charge air flow (A, B) is changed by simple pipeline and air-flow
Gas outlet and evacuation port are connected to unit (1), the airflow-reversing unit (1) includes at least one two direct driving type electromagnetics
Valve, the gas outlet connect downstream gas circuit；
Continuously and stably inlet air flow stream reversing unit (1), airflow-reversing unit (1) switching two-way enter two-way charge air flow (A, B)
Gas air-flow (A, B), two-way charge air flow (A, B) is chronologically set and flow to gas outlet and evacuation port respectively, realize downstream atmosphere
Switching, the Y-shaped runner in the airflow-reversing unit (1) close to gas outlet is provided centrally with two direct-acting electromagnetic valves
Reversing valve core；
The air inlet of the evacuation port connection inlet pressure controller (2), the gas outlet emptying of inlet pressure controller (2)；Institute
State and pressure transmitter (3) is connected between two-way charge air flow (A, B)；Inlet pressure controller (2) is used for the back of the body for adjusting emptying air-flow
Pressure, the differential pressure value nearly zero for detecting pressure transmitter (3), that is, ensure that the pressure state of two-way charge air flow (A, B) is identical.
A kind of 3. steady fast switching system of atmosphere according to claim 2, it is characterised in that：Flowed in the switching system
The effective drift diameter in road is 1mm~4mm.
A kind of 4. steady fast switching system of atmosphere according to Claims 2 or 3, it is characterised in that：Inlet pressure controls
Device (2) carries out negative-feedback according to the differential pressure value of pressure transmitter (3) Real-time Feedback and automatically adjusted, and detects pressure transmitter (3)
Differential pressure value stabilization in -100Pa~100Pa.
A kind of 5. steady fast switching system of atmosphere according to claim 2, it is characterised in that：The airflow-reversing unit
(1) it is made up of three two-position three way direct-acting electromagnetic valves (4,5,6), the Heng Tong gas port of two of which magnetic valve (4,5) is right respectively
Should connect two-way charge air flow (A, B), two switching gas ports of the two of which magnetic valve (4,5) respectively with the 3rd electromagnetism
Two switching gas ports of valve (6) connect one to one, and two other switching gas port of the two of which magnetic valve (4,5) confluxes
Connect the air inlet of inlet pressure controller (2), the Heng Tong gas port connection downstream gas circuit of the 3rd magnetic valve (6).
A kind of 6. steady fast switching system of atmosphere according to claim 2, it is characterised in that：The airflow-reversing unit
(1) it is a two-position four-way direct-acting electromagnetic valve (7)；Two air inlets of the magnetic valve (7) connect two-way air inlet gas respectively
Flow (A, B)；The gas outlet connection downstream gas circuit of magnetic valve (7)；The exhaust outlet connection inlet pressure controller (2) of magnetic valve (7)
Air inlet.
A kind of 7. steady fast switching system of atmosphere according to claim 2, it is characterised in that：The airflow-reversing unit
(1) it is a two-position five-way direct-acting electromagnetic valve (8)；Two air inlets of the magnetic valve (8) connect two-way air inlet gas respectively
Flow (A, B)；The gas outlet connection downstream gas circuit of the magnetic valve (8)；Two exhaust outlets of the magnetic valve (8) connect after confluxing
The air inlet of inlet pressure controller (2).
A kind of 8. steady fast switching system of atmosphere according to claim 5,6 or 7, it is characterised in that：
The reversing valve core of the magnetic valve is balanced type poppet valve core；
Or the magnetic valve is short stroke, fast-response magnetic valve, the energization response time of the magnetic valve is less than 4ms, and power-off rings
It is less than 2ms between seasonable.
A kind of 9. steady fast switching system of atmosphere according to claim 2,5,6 or 7, it is characterised in that：The switching
System also includes the airflow-reversing unit of N number of extension, N >=1；Often increase the airflow-reversing unit of an extension, by its gas outlet
It is connected to an air inlet of mounted airflow-reversing unit.
10. a kind of application of the steady fast switching system of atmosphere in claim 2~9 described in any claim, its feature
It is：
For switching the atmosphere in microreactor, it is specially：
The gas outlet of the switching system is connected to microreactor, power of electromagnetic valve line is connected to programmable controller
Output switch parameter interface, programmable controller are communicated with computer by communication cable；
According to atmosphere switch need set magnetic valve switching electricity sequential in a computer；Microreactor is set, and
The state of the Z roads air-flow of the steady fast switching system of atmosphere is flowed into, magnetic valve switching electricity program is then triggered and completes atmosphere switching
Process, Z >=2；
Equivalent diameter D≤40mm of the flow area of each section of the microreactor；The steady fast switching system of atmosphere
Operation length L≤1200mm, pipeline inner volume V≤100mL between the conversion zone of gas outlet and the microreactor；It is described
Z roads air flow rate is arranged so that the apparent velocity amplitude of air-flow of each section of the microreactor is located at 0.05~20m/s scopes；
Steady, quick, the complete switching of atmosphere in microreactor is completed by above-mentioned technical method.
11. the application of the steady fast switching system of atmosphere according to claim 10, it is characterised in that：By described one kind
The steady fast switching system of atmosphere is used to analyze the multistage reaction in-situ process that solid particle is switched based on atmosphere, is specially：
Each section of the microreactor is pipe and internal diameter is 2mm~25mm；The outlet of the steady fast switching system of atmosphere
Operation length L≤400mm, pipeline inner volume V≤20mL between mouth and the conversion zone of the microreactor；It is described miniature anti-
Answer and contain solid-state reactants in the conversion zone of device；Z roads air flow rate is arranged so that the gas of each section of the microreactor
Flow table sees velocity amplitude and is located at 0.05~5m/s scopes；
The microreactor connection procedure gas analyzing apparatus；The sampling pipe of the process gas analytical equipment is less than for internal diameter
200 μm of capillary sampling pipe, the frequency of detection and the record gas concentration response of process gas analytical equipment are higher than 2HZ；It is described
Operation length L≤800mm, pipeline inner volume V between the conversion zone of microreactor and the thief hatch of capillary sampling pipe≤
50mL；
Steady, quick, the complete switching of atmosphere in microreactor is completed by above-mentioned technical method；It is anti-in microreactor
Process is answered to be divided into M stage, M >=2 by the switching of atmosphere；Gas concentration response is detected and recorded by process gas analytical equipment
To switch course of reaction occurred in analysis reactor with atmosphere, and calculate quantitative result；Solid carbon-based fuel is realized with this
The analysis test for the multistage reaction in-situ that particle is switched based on atmosphere.
12. the application of the steady fast switching system of atmosphere according to claim 10, it is characterised in that：By described one kind
The steady fast switching system of atmosphere is used for diffusion and the back-mixing characteristics of quantitatively characterizing microreactor interior air-flow, is specially：
The equivalent diameter of the flow area of each section of the microreactor is 2mm~30mm；The atmosphere, which is steadily switched fast, is
Operation length L≤400mm, pipeline inner volume V≤20mL between the conversion zone of the gas outlet of system and the microreactor；Institute
State Z roads air flow rate and be arranged so that the apparent velocity amplitude of air-flow of each section of the microreactor is located at 0.05~5m/s scopes；
The microreactor connection procedure gas analyzing apparatus；The sampling pipe of the process gas analytical equipment is less than for internal diameter
200 μm of capillary sampling pipe, the frequency of detection and the record gas concentration response of process gas analytical equipment are higher than 5HZ；It is described
Operation length L≤800mm, pipeline inner volume V between the conversion zone of microreactor and the thief hatch of capillary sampling pipe≤
50mL；
The output switch parameter of the programmable controller exports for transistor DC 24V, and the response time of output point switching electricity
≤ 1ms；The sequential that setting is passed through microreactor interior air-flow is A-B-A, B air-flows component containing tracer and tracer component volume
Concentration≤10%；The residence time distribution curve of tracer component, i.e. RTD curves are obtained by this kind of air-flow handoff procedure；Then
Calculate the zero dimension variance of RTD curves；The Peclet numbers of microreactor are finally calculated, i.e., in iterative following equation
Per：
<mrow>
<msubsup>
<mi>&delta;</mi>
<mi>&Theta;</mi>
<mn>2</mn>
</msubsup>
<mo>=</mo>
<mfrac>
<mn>2</mn>
<mrow>
<msub>
<mi>Pe</mi>
<mi>r</mi>
</msub>
</mrow>
</mfrac>
<mo>-</mo>
<mfrac>
<mn>2</mn>
<mrow>
<msubsup>
<mi>Pe</mi>
<mi>r</mi>
<mn>2</mn>
</msubsup>
</mrow>
</mfrac>
<mrow>
<mo>(</mo>
<mn>1</mn>
<mo>-</mo>
<msup>
<mi>e</mi>
<mrow>
<mo>-</mo>
<msub>
<mi>Pe</mi>
<mi>r</mi>
</msub>
</mrow>
</msup>
<mo>)</mo>
</mrow>
</mrow>
In formula：Represent the zero dimension variance of RTD curve of the tracer component in microreactor；PerRepresent microreactor
Peclet numbers, the relative size of convective mass transfer speed and diffusion mass transfer speed is characterized, i.e. air-flow component is in microreactor
Diffusion and back-mixing degree, PerBigger sign back-mixing degree is smaller, air-flow is closer to like laminar flow；
Diffusion and back-mixing characteristics by above method quantitatively characterizing microreactor interior air-flow.
A kind of 13. application of the steady fast switching system of atmosphere according to claim 12, it is characterised in that：
Tested using step method and obtain RTD curves；When the equivalent diameter of each section of flow area of the microreactor is 20mm
~30mm, and when the inner volume of microreactor is 40mL~70mL, the air-flow switching is to be arranged to the time of A-B-A processes
10s~200s；When the equivalent diameter of each section of flow area of the microreactor is 2mm~20mm, and microreactor
When inner volume is 10mL~40mL, the air-flow switching is the time of A-B-A processes to be arranged to 5s~200s；
Or RTD curves are obtained using impulse method experiment；When the equivalent diameter of each section of flow area of the microreactor is
20mm~30mm, and when the inner volume of microreactor is 40mL~70mL, the air-flow switching is to set the time of A-B-A processes
It is set to 200ms~800ms；When the equivalent diameter of each section of flow area of the microreactor is 2mm~20mm, and it is miniature anti-
When answering the inner volume of device to be 10mL~40mL, the air-flow switching is the time of A-B-A processes to be arranged to 80ms~400ms.
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