CN109200961A - A kind of continuous flow production control method, the device and system of microreactor - Google Patents
A kind of continuous flow production control method, the device and system of microreactor Download PDFInfo
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- CN109200961A CN109200961A CN201810937700.1A CN201810937700A CN109200961A CN 109200961 A CN109200961 A CN 109200961A CN 201810937700 A CN201810937700 A CN 201810937700A CN 109200961 A CN109200961 A CN 109200961A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D27/00—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00
- G05D27/02—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00 characterised by the use of electric means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
Abstract
The present invention relates to continuous flow production control method, the device and system of a kind of microreactor, this method includes detecting the constituent and the corresponding constituent content data of each constituent of reaction raw materials；Simulation reaction process determines simulation reaction product；The corresponding simulation constituent content data of the component data and simulation reaction product component of analysis mode reaction product, determine the first analysis data；The component data and the corresponding content data of real reaction product component for acquiring real reaction product, determine the second analysis data；Data and the second analysis data are analyzed in comparative analysis first, determine the first comparative analysis result data；If the first analysis data change with the second analysis data, reaction condition is adjusted according to the first comparative analysis result data and/or reaction raw materials match, determine control program, control microreactor carries out target product production.Using the above method or device or system energy Real Time Monitoring reaction process, reaction raw materials proportion and/or reaction condition are adjusted in real time.
Description
Technical field
The present invention relates to miniature chemical industry technical applications, and in particular to a kind of continuous flow production controlling party of microreactor
Method, device and system.
Background technique
In recent years, the important technical that microreaction technology is strengthened as chemical process, is increasingly becoming research and application
Hot spot, around " transport " core process of Chemical Manufacture, the substantially diminution of dependence characteristics size, microreactor is being passed
During matter, heat transfer etc., efficiency improves 10~100 times compared with conventional equipment.For certain fast reaction processes, microreactor tool
Various advantages such as there are good safety, process control and can directly amplify.
Currently, the autoclave production process of traditional intermittent mode is transformed into for the reaction process of heat and mass control
Continuous production process is a Main way of microreactor application.Especially in the energy, pharmacy, fine chemical product, chemical industry
The quantitative production aspect of mesosome, hazardous chemical, the application of microreactor are more extensive.The application of microreactor is main at this stage
It is to realize that the raw material of fixed mixing ratio inputs using constant flow pump under the conditions of determining raw material proportioning, while controlling the temperature of reactor assembly
Degree, pressure and other parameters realize stable product output.However harsher production process is required for some reaction conditions,
The minor change (such as flow, temperature, pressure oscillation) or inside reactor catalytic efficiency of input condition, microchannel surface with
There is the influence such as cumulative effect in reaction process, and reaction product will appear fluctuation and cause the unstable of output product.
And the control to microreactor system at present, often the monitoring of the inputs such as flow, temperature, pressure is controlled,
In the case where continuous flow production operation, detection and adjust control hand that analysis for product and the case where changing still lack
Section.
Summary of the invention
In view of this, it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of continuous flows of microreactor
Production control method, device and system, when solving analysis and ingredient in continuous flow production operation, to product and changing
The case where lacking detection and adjusting control.
The present invention provides a kind of microreactor continuous flow production control method, described to include:
Detect the constituent and the corresponding constituent content data of each constituent of reaction raw materials；
According to the data of the corresponding constituent content of the constituent of the reaction raw materials, simulation reaction process, determine described in
Simulation reaction product during simulation reaction；
According to the simulation reaction product, analyze the simulation reaction product component data and the simulation reaction product
The corresponding simulation constituent content data of component, determine the first analysis data；
The component data and the corresponding content data of the real reaction product component for acquiring real reaction product determine the
Two analysis data；
First analysis data described in comparative analysis and the second analysis data, determine the first comparative analysis result data；
If the first analysis data described in the comparative analysis change with the second analysis data, according to described first
Comparative analysis result data adjusts reaction condition and/or reaction raw materials proportion, determines control program；
Microreactor, which is controlled, according to the control program carries out target product production.
Optionally, the determining control program, comprising:
It is matched according to the adjustment reaction condition and/or reaction raw materials, determines and set several control programs；
The several control programs of setting are compared, determine target control scheme.
Optionally, the simulation reaction process, comprising: according to the corresponding constituent content of the constituent of the reaction raw materials
Data, the proportion of simulation reaction condition and reaction raw materials determines the simulation reaction product during the simulation reaction.
Optionally, the first analysis data and the second analysis data analysis are compared and are changed, comprising: described the
The variation for being greater than or equal to centesimal data deviation occurs for one analysis data and the second analysis data analysis comparison.
A kind of continuous flow production control device of microreactor, comprising:
Detection module detects the constituent and the corresponding constituent content data of each constituent of reaction raw materials；
Analog module, for the data of the corresponding constituent content of constituent according to the reaction raw materials, simulation reaction
Process determines the simulation reaction product during simulation reaction；
Analysis module, for analyzing component data and the institute of the simulation reaction product according to the simulation reaction product
The corresponding simulation constituent content data of simulation reaction product component are stated, determine the first analysis data；
Acquisition module, for acquiring the component data of real reaction product and the real reaction product component is corresponding contains
Data are measured, determine the second analysis data；
Contrast module determines the first comparison for the first analysis data described in comparative analysis and the second analysis data
Analysis result data；
Determining module changes for working as the first analysis data described in the comparative analysis with the second analysis data
When, reaction condition is adjusted according to the first comparative analysis result data and/or reaction raw materials match, determines control program；
Control module carries out target product production for controlling microreactor according to the control program.
A kind of continuous flow production control system of microreactor, comprising: control module, raw material input module, on-line mass spectroscopy
Instrument, microreactor module, micro-fluidic chip, collection of products device；
The raw material input module communication ends of the control module are connected with the communication ends of the raw material input module, are used for
Detect the constituent and the corresponding constituent content data of each constituent of reaction raw materials；
The on-line mass spectroscopy instrument communication ends of the control module are connected with the communication ends of the on-line mass spectroscopy instrument, for acquiring
Component data and the real reaction product component corresponding content data of the on-line mass spectroscopy instrument to real reaction product；
The delivery outlet of the raw material input module is connected with the input port of the microreactor module, for raw material is defeated
The microreactor module is arrived out；
The delivery outlet in the channel of the micro-fluidic chip is connected with the input port of the on-line mass spectroscopy instrument, described micro-fluidic
First delivery outlet in the channel of chip is connected with collection of products device, fills for reaction product to be output to the collection of products
It sets；
Second delivery outlet in the channel of the micro-fluidic chip is connected with the input port of on-line mass spectroscopy instrument, for that will react
The sample of product is output to the on-line mass spectroscopy instrument, and on-line mass spectroscopy instrument tests and analyzes the constituent content of Product samples.
Optionally, further includes: water-bath；
Water-bath communication ends in the control module are connected with the communication ends of water-bath by the communications cable, for controlling
The temperature of water-bath processed；
The microreactor module is placed in water-bath, for controlling the temperature of microreactor module.
Optionally, the raw material input module specifically includes: constant flow pump；
The communication ends of the raw material input module of the control module are connected with the communication ends of the constant flow pump, for controlling
The flow of constant flow pump started and stopped while controlling reaction raw materials conveying.
Optionally, it is set between second delivery outlet in the channel of the micro-fluidic chip and the input port of the on-line mass spectroscopy instrument
There is sample injector；
Second delivery outlet in the channel of the micro-fluidic chip is connected with the input port of the sample injector, for that will react
The sample of product is output to sample injector and the sample gas of reaction product is turned to gas；
The delivery outlet of the sample injector is connected with the input port of the on-line mass spectroscopy instrument, for extracting the gas after gasifying
It is output to the on-line mass spectroscopy instrument, detects the gas content.
Optionally, described to be specifically included according to microreactor module: microreactor, coil pipe, counterbalance valve；
The microreactor is connected with the coil pipe, and stop is reacted in microreactor for adjusting the reaction raw materials
Time；
The coil pipe is connected with the counterbalance valve, for controlling the pressure of real reaction system.
Technical solution provided by the present application can include the following benefits: the continuous flow of the microreactor produces control
System, by control module to the sunykatuib analysis data of reaction raw materials, with the actually detected reaction product data pair of on-line mass spectroscopy instrument
Than analysis, the situation after changing according to date comprision is had adjusted, and controlling party has been determined according to data situation
Case, solve the problems, such as because product occur fluctuation cause to export it is unstable, realize to reaction product it is real-time analysis and control
System, ensure that final product stablizes output.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is a kind of flow chart of microreactor continuous flow production control method provided in an embodiment of the present invention；
Fig. 2 is a kind of structural schematic diagram of microreactor continuous flow production control device provided in an embodiment of the present invention；
Fig. 3 is a kind of structural schematic diagram of microreactor continuous flow production control system provided in an embodiment of the present invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
In current continuous flow production, carrying out reaction production using microreactor is a kind of common production method, when
When raw material is produced, raw material needs are reacted in microreactor, but can be because of some flows, temperature, pressure in reaction
The influence of fluctuation causes the unstable output of output product, and before raw material is reacted, if the ratio of reaction raw materials
With the uncertain reaction that also will affect microreactor of reaction condition, cause product qualified.
To solve the above-mentioned problems, the embodiment of the invention provides a kind of continuous flow production control method of microreactor,
Include:
Detect the constituent and the corresponding constituent content data of each constituent of reaction raw materials；
According to the data of the corresponding constituent content of the constituent of the reaction raw materials, simulation reaction process, determine described in
Simulation reaction product during simulation reaction；According to the simulation reaction product, the component of the simulation reaction product is analyzed
Data and the corresponding simulation constituent content data of the simulation reaction product component, determine the first analysis data；It receives practical anti-
The component data and the corresponding content data of the real reaction product component for answering product, determine the second analysis data；To score
The first analysis data and the second analysis data are analysed, determine the first comparative analysis result data；If the comparative analysis
The first analysis data change with the second analysis data, are adjusted according to the first comparative analysis result data anti-
It answers condition and/or reaction raw materials to match, determines control program；Microreactor, which is controlled, according to the control program carries out target product
Production.
In the present embodiment, continuous flow production in, when reaction raw materials are inputted, by detect reaction raw materials composition at
Divide and the corresponding constituent content digital simulation of the constituent of each reaction raw materials generates simulation reaction product, realizes reaction
The process of on-line monitoring and the online simulation reaction of raw material, and the constituent content data of analog product and reaction raw materials is complete
It is compared and analyzed at the real reaction product composition data after reaction, when comparative analysis data result changes then according to change
Change situation to be adjusted, implement control program adjusted, realizes the on-line analysis of product, to when adjusting control hand
Section improves production stability of the product in continuous flow reaction.
The technical solution of the above embodiment of the present invention is described in detail using several specific embodiments below.
Embodiment one
Fig. 1 is a kind of flow chart of the continuous flow production control method of microreactor provided in an embodiment of the present invention, such as Fig. 1
Shown, the method for the present embodiment can specifically include following steps:
S101, the constituent and the corresponding constituent content data of each constituent for detecting reaction raw materials；
Raw material refers to that production needs raw material to be reacted, including liquid charging stock and solid material, gas raw material in Chemical Manufacture.Instead
Should can be liquid and liquid reactions, can for liquid and solid reaction, be also possible to gas raw material and liquid charging stock reaction.Needle
Reaction to solid and liquid, 200 microns of particles below are made in solid material, and then evenly dispersed suspension is defeated in the liquid phase
Enter reaction system.For the interface special designing that gas and liquid reactions are by gas and liquid mixed interface, guarantee input
Gas, which is distributed in liquid in the form of uniform bubble, realizes reaction.Reaction raw materials use liquid charging stock and liquid in the present embodiment
Raw material reaction.
Constituent can be individual molecule, atom, ion and/or micel, atomic group, ion cluster.
Content data is the amount for certain ingredient for including in a kind of reaction raw materials.Such as certain solution contains certain molecule 50%.
The whole components of reaction raw materials are identified and analyzed into reaction raw materials input module for sense command, determine
In certain liquid at the content for being grouped as and determining each ingredient.
S102, the data according to the corresponding constituent contents of constituent of the reaction raw materials, simulation reaction process determine
Simulation reaction product during the simulation reaction；
Simulation reaction process is the reaction condition of calculating simulation and the proportion data of reaction raw materials, and reaction condition includes reaction
Temperature, pressure, flow, proportion data are the type and fixed proportion data that reaction raw materials need to input.According to determining reaction
The physical data of the reaction condition and reaction raw materials that need calculates the reaction constant during reacting corresponding, can be generation
The thermodynamic equilibrium constant that the endothermic reaction or heat dissipation reaction need, and establish chemical equilibrium equation formula and carry out simulation reaction calculating, simulation
The result of reaction is simulation reaction product.
S103, according to the simulation reaction product, component data and the simulation for analyzing the simulation reaction product are anti-
The corresponding simulation constituent content data of product component are answered, determine the first analysis data；
The simulation reaction product that simulation reaction obtains is analyzed, analysis obtains the component data in simulation reaction product
And the corresponding simulation constituent content data of the simulation reaction product component, and by its simulation reaction product component data and
The corresponding simulation constituent content data of the simulation reaction product component are as the first analysis data.
S104, the component data and the corresponding content data of the real reaction product component for acquiring real reaction product,
Determine the second analysis data；
Real reaction raw material completes output real reaction product after real reaction, analyzes the component and group of real reaction product
Divide corresponding content, and the component of real reaction product and the corresponding content data of real reaction product component be acquired,
As the second analysis data.
First analysis data described in S105, comparative analysis and the second analysis data, determine the first comparative analysis result
Data；
The first analysis data of comparative analysis are the component data and simulation reaction product component of simulation reaction product
Corresponding simulation constituent content data, the second analysis data are the component data and real reaction product component of real reaction product
Corresponding content data, by the component data of simulation reaction product and the corresponding content data of simulation reaction product component and reality
The component data and the corresponding content data of real reaction product component of reaction product compare and analyze, and the result of analysis is made
For the first comparative analysis result data.
If S106, the first analysis data change with the second analysis data, according to first pair of score
Result data adjustment reaction condition and/or reaction raw materials proportion are analysed, determines control program；
First analysis data are the component data and the corresponding simulation component of simulation reaction product component of simulation reaction product
Content data；Second analysis data are the component data and the corresponding content number of real reaction product component of real reaction product
According to；First comparative analysis result data is the first analysis data and the second analysis data, i.e. simulation reaction product component is corresponding
The component data and the corresponding content data of real reaction product component of content data and real reaction product, when comparative analysis institute
It states the first analysis data to change with the second analysis data, reaction condition is adjusted according to the first comparative analysis result data
And/or reaction raw materials proportion, determine control program.
Optionally, control program the adjustment reaction condition and/or reaction raw materials can match according to, determine setting number
A control program；
It is compared according to the determining several control programs of setting, determines target control scheme.
Further, the first analysis data change with the second analysis data analysis comparison, can be first point
Analysis data and the second analysis data analysis comparison change more than or equal to centesimal data deviation.
S107, microreactor progress target product production is controlled according to the control program；
Control program is the several control programs of setting.
Target product is the required final product of production.
Microreactor is continuous according to continuing after the proportion of target control scheme adjustment reaction condition and/or reaction raw materials
Stream production.
It should be noted that in each step, all sending and receiving comprising data, for the readability of embodiment,
Not yet explicitly write the process that data receive and sent in each step exactly.
In the present embodiment, continuous flow production in, when reaction raw materials are inputted, by detect reaction raw materials composition at
Divide and the corresponding constituent content digital simulation of the constituent of each reaction raw materials generates simulation reaction product, realizes reaction
The process of on-line monitoring and the online simulation reaction of raw material, and the constituent content data of analog product and reaction raw materials is complete
It is compared and analyzed at the real reaction product composition data after reaction, when comparative analysis data result changes then according to change
Change situation to be adjusted, implement new control program, realizes the on-line analysis of product, to when adjusting control means,
Complete steady production of the product in continuous flow reaction.
Corresponding to a kind of continuous flow production control method of microreactor provided in an embodiment of the present invention, the embodiment of the present invention
A kind of continuous flow production control device of microreactor is also provided.See below embodiment.
Embodiment two
Fig. 2 is a kind of structural schematic diagram of microreactor continuous flow production control device provided in an embodiment of the present invention.Such as
Shown in Fig. 2, a kind of continuous flow production control device of microreactor includes:
Detection module 201, for detecting the constituent and the corresponding constituent content of each constituent of reaction raw materials
Data；
Analog module 202 is used for simulation reaction process, determines the simulation reaction product during the simulation reaction；
Analysis module 203, for analyze the simulation reaction product component data and the simulation reaction product component
Corresponding simulation constituent content data, determine the first analysis data；
Acquisition module 204, for acquire real reaction Product samples component data and the real reaction Product samples
The corresponding content data of component determines the second analysis data；
Contrast module 205 determines first pair for the first analysis data described in comparative analysis and the second analysis data
Compare analysis result data；
Further, contrast module 205 is specifically used for: the first analysis data and the second analysis data analysis pair
Than changing, including the first analysis data and the second analysis data analysis comparison change more than or equal to percent
One data deviation.
Determining module 206 is adjusted for the first comparative analysis result data, determines control program,
Further, determining module 206 is specifically used for: being matched according to the adjustment reaction condition and/or reaction raw materials, really
Determine control program, wherein determining that control program includes: to match according to the adjustment reaction condition and/or reaction raw materials, determination is set
Fixed number control program；It is compared according to the determining several control programs of setting, determines target control scheme.
Control module 207 carries out target product production for controlling microreactor according to control program.
In the present embodiment, in continuous flow production, when reaction raw materials are inputted, detection reaction raw materials can be passed through
Constituent and the corresponding constituent content data of the constituent of each reaction raw materials, analog module simulation generate simulation reaction
Product realizes the on-line monitoring of reaction raw materials and the process of online simulation reaction, and passes through contrast module for analog product
Constituent content data are completed the real reaction product component content data after reacting with reaction raw materials and are compared and analyzed, and comparison is worked as
Analysis data result is then adjusted according to situation of change when changing, and determining module determines new control program, and use is above-mentioned
Device realizes the on-line analysis of product, to control means are when adjusted, and improves the product in continuous flow reaction
Production stability.
In order to more clearly introduce the hardware system for realizing the embodiment of the present invention, correspond to provided in an embodiment of the present invention one
The continuous flow production control method of kind microreactor, the embodiment of the present invention also provide a kind of continuous flow production control of microreactor
System.See below embodiment.
Embodiment three
Fig. 3 is a kind of microreactor continuous flow production control system structural schematic diagram.As shown in figure 3, a kind of microreactor
Continuous flow production control system include:
Control module 301, raw material input module 302, on-line mass spectroscopy instrument 303, microreactor module 304, micro-fluidic chip
305, collection of products device 306；
The raw material input module communication ends of control module 301 are connected with the communication ends of the raw material input module 302, use
In the constituent and the corresponding constituent content number of each constituent of the reaction raw materials for detecting the raw material input module 302
According to；
Optionally, control module 301 can use industrial PC, and simulation computation model program is write in industrial PC, until
There are two communication ends, respectively 303 communication ends of 302 communication ends of raw material input module and on-line mass spectroscopy instrument for few tool；This programme is implemented
Five communication ends are used in example, are respectively as follows: two 302 communication ends of raw material input module, 303 communication ends of on-line mass spectroscopy instrument,
In optinal plan, other two communication ends can be used for being connected with water-bath 307, micro-fluidic chip 305.The communication ends are equal
It can be RS485 communication ends, the communications cable that communication ends are connected may each be the RS485 communications cable；Industrial PC also has
Certain dustproof and waterproof function.
Control module 301 is industrial PC in explanation below.
Further, raw material input module 302 specifically includes constant flow pump 3021: the raw material input of the control module 301
The communication ends of module are connected with the communication ends of the constant flow pump 3021, for controlling starting and stopping, together for constant flow pump 3021
When control reaction raw materials conveying flow；
The embodiment of the present invention is realized in the input mode of microreactor raw material, uses constant flow pump, and traditional approach, such as logical
Overcurrent meter detection flows, adjust the aperture of material inlet valve, realize the adjusting of flow, but the precision detected is not high, adjust flow
Range it is little, flow rate accuracy is not high and unstable.And constant flow pump is used, raw material can be automatically controlled by control module realize
The input of fixed mixing ratio, the conveying of fluid flow, more accurate stabilization；And conveying substance is not contacted with the external world, it is anti-pollution, more
Practical convenient.
Optionally, raw material input module 302 is set as two constant flow pumps 3021 and two head tanks 3022 in the present embodiment
It is connected respectively by anti-corrosion pipe, anti-corrosion pipe can be stainless steel tube.
Specifically, two head tanks 3022 distinguish phase by stainless steel tube respectively with two constant flow pumps 3021 to the present embodiment
Two communication ends of connection, industrial PC are communicated with two of two constant flow pumps 3021 respectively by two RS485 communications cables
End is respectively connected with.
The embodiment of the present invention uses 303 analytic approach of on-line mass spectroscopy instrument, and traditional product assay has off-line analysis method, spectrum
Analytic approach.Off-line analysis method taken at regular intervals samples carry out analytical test, and whether the content for detecting key component in product closes
Lattice, analysis elapsed time are longer；Spectra methods is the side that the detection of the structure of matter or chemical component is carried out using characteristic spectrum
Method.Material absorbing characteristic spectrum, such as ultraviolet spectra, infrared spectroscopy, but this analysis method is the spectrum for specific groups
Feature is detected, and is difficult to accomplish detection while Multiple components in product, and the accuracy of quantitative detection is lower.And it is online
Spectrometer analysis method is analyzed using the measurement of the mass-to-charge ratio of sample ion, by the mass spectrum and relevant information of sample,
The content of various ingredients in product is detected simultaneously, and for the qualitative, quantitative of available sample as a result, accuracy is high, analysis speed is fast.
301 on-line mass spectroscopy instrument communication ends of control module are connected with the communication ends of the on-line mass spectroscopy instrument 303, for receiving
Component data and the real reaction product component corresponding content data of the on-line mass spectroscopy instrument 303 to real reaction product.
The RS485 communication ends of the on-line mass spectroscopy instrument of industrial PC and the RS485 communication port of the on-line mass spectroscopy instrument 303 are logical
The RS485 communications cable is crossed to be connected.
The delivery outlet of raw material input module 302 is connected with the input port of the microreactor module 304, is used for raw material
It is output to the microreactor module 304；
Two delivery outlets of two constant flow pumps 3021 pass through two stainless steel tubes respectively and are connected, and by two stainless steel tubes
It is connected by efferent duct, efferent duct is as the delivery outlet of raw material input module 302 and the input port phase of microreactor module 304
Connection.
Further, the continuous flow production control system of microreactor further includes water-bath 307: in control module 301
Water-bath communication ends are connected with the communication ends of water-bath 307 by the communications cable, for controlling the temperature of water-bath 307.It is micro-
Reactor module 303 is placed in water-bath 307, for controlling the temperature of microreactor module 303.Control module 301 can be
Industrial PC can control water-bath 307 by industrial PC when reaction raw materials need to heat when being reacted and be added
Thermal response, if reaction condition changes, industrial PC can pass through the control adjustment reaction temperature of water-bath 307 according to situation of change
Degree.
Optionally, microreactor module 304 specifically includes: microreactor 3041, coil pipe 3042, counterbalance valve 3043.It is micro- anti-
It answers device 3041 to be connected with coil pipe 3042, reacts residence time in microreactor for adjusting the reaction raw materials；Coil pipe
3042 are connected with counterbalance valve 3043, for controlling the pressure of the real reaction system.The input port of microreactor 3041 with
The efferent duct of two constant flow pumps 3021 is connected.
The input port in the channel of micro-fluidic chip 305 is connected with the delivery outlet of the raw material input module 302, described micro-
First delivery outlet in the channel of fluidic chip 305 is connected with collection of products device 306, described for reaction product to be output to
Collection of products device 306；
Second delivery outlet in the channel of micro-fluidic chip 305 is connected with the input port of on-line mass spectroscopy instrument 303, and being used for will be anti-
The sample of product is answered to be output to the on-line mass spectroscopy instrument 303.
Micro-fluidic chip 305 is equipped with channel, and channel is divided into two delivery outlets, respectively first delivery outlet in channel and the
Two delivery outlets.First delivery outlet in channel is connected directly with collection of products device 306, can also be connected by anti-corrosion pipe.
Second delivery outlet is connected with the input port of on-line mass spectroscopy instrument 303, for the sample of reaction product to be output to the online matter
Spectrometer 303.
First delivery outlet in the channel of micro-fluidic chip 305 is passed through collection of products device 306 in progress reaction product and collects
While the second delivery outlet abstraction reaction product in millesimal reaction product sample be output to on-line mass spectroscopy instrument 303.
Optionally, two delivery outlets in the channel of micro-fluidic chip 305 can be T-type structure structure, and the first delivery outlet is straight
Diameter can be set to 1mm, and second delivery outlet can be set to 0.01mm.
Optionally, second delivery outlet in the channel of micro-fluidic chip 305 and the on-line mass spectroscopy instrument 303 in the present embodiment
Input port between be equipped with sample injector 308；Second delivery outlet in the channel of micro-fluidic chip 305 is defeated with the sample injector 308
Entrance is connected, and the sample gas for the sample of reaction product to be output to the progress reaction product of sample injector 308 turns to gas；Into
The delivery outlet of sample device 308 is connected with the input port of on-line mass spectroscopy instrument 303, is output to online matter for extracting the sample after gasifying
Spectrometer 303,303 test sample content of on-line mass spectroscopy instrument.
Detection reaction raw materials can be passed through in continuous flow production, when reaction raw materials are inputted using above system
Constituent and the corresponding constituent content digital simulation of the constituent of each reaction raw materials generate simulation reaction product, realize
The process of on-line monitoring and the online simulation reaction of reaction raw materials, and by the constituent content data of analog product with react
The real reaction product composition data that raw material completes after reaction compares and analyzes, then when comparative analysis data result changes
It is adjusted according to situation of change, implements new control program, realized the on-line analysis of product, when adjusting is controlled
Means complete steady production of the product in continuous flow reaction.
It is understood that same or similar part can mutually refer in the various embodiments described above, in some embodiments
Unspecified content may refer to the same or similar content in other embodiments.
It should be noted that in the description of the present invention, term " first ", " second " etc. are used for description purposes only, without
It can be interpreted as indication or suggestion relative importance.In addition, in the description of the present invention, unless otherwise indicated, the meaning of " multiple "
Refer at least two.
Any process described otherwise above or method description are construed as in flow chart or herein, and expression includes
It is one or more for realizing specific logical function or process the step of executable instruction code module, segment or portion
Point, and the range of the preferred embodiment of the present invention includes other realization, wherein can not press shown or discussed suitable
Sequence, including according to related function by it is basic simultaneously in the way of or in the opposite order, to execute function, this should be of the invention
Embodiment person of ordinary skill in the field understood.
It should be appreciated that each section of the invention can be realized with hardware, software, firmware or their combination.Above-mentioned
In embodiment, software that multiple steps or method can be executed in memory and by suitable instruction execution system with storage
Or firmware is realized.It, and in another embodiment, can be under well known in the art for example, if realized with hardware
Any one of column technology or their combination are realized: having a logic gates for realizing logic function to data-signal
Discrete logic, with suitable combinational logic gate circuit specific integrated circuit, programmable logic controller (PLC) (PLC),
Programmable gate array (PGA), field programmable gate array (FPGA) etc..
Those skilled in the art are understood that realize all or part of step that above-described embodiment method carries
It suddenly is that relevant hardware can be instructed to complete by program, the program can store in a kind of computer-readable storage medium
In matter, which when being executed, includes the steps that one or a combination set of embodiment of the method.
It, can also be in addition, each functional unit in each embodiment of the present invention can integrate in a processing module
It is that each unit physically exists alone, can also be integrated in two or more units in a module.Above-mentioned integrated mould
Block both can take the form of hardware realization, can also be realized in the form of software function module.The integrated module is such as
Fruit is realized and when sold or used as an independent product in the form of software function module, also can store in a computer
In read/write memory medium.
Storage medium mentioned above can be read-only memory, disk or CD etc..
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
Centainly refer to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be any
One or more embodiment or examples in can be combined in any suitable manner.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (10)
1. a kind of continuous flow production control method of microreactor characterized by comprising
Detect the constituent and the corresponding constituent content data of each constituent of reaction raw materials；
The simulation reaction mistake is determined according to the constituent and the corresponding constituent content data, simulation reaction process
Simulation reaction product in journey；
According to the simulation reaction product, the component data of the simulation reaction product and the group of the simulation reaction product are analyzed
Divide corresponding simulation constituent content data, determines the first analysis data；
The component data of real reaction product and the corresponding content data of component of the real reaction product are acquired, determine second
Analyze data；
First analysis data described in comparative analysis and the second analysis data, determine the first comparative analysis result data；
If the first analysis data change with the second analysis data, according to the first comparative analysis result data
Reaction condition and/or reaction raw materials proportion are adjusted, determines control program；
Microreactor, which is controlled, according to the control program carries out target product production.
2. the continuous flow production control method of microreactor according to claim 1, which is characterized in that the determining control
Scheme, comprising:
It is matched according to the adjustment reaction condition and/or reaction raw materials, determines and set several control programs；
The several control programs of setting are compared, determine target control scheme.
3. the continuous flow production control method of microreactor according to claim 1, which is characterized in that the simulation reaction
Process, comprising: according to the data of the corresponding constituent content of the constituent of the reaction raw materials, simulation reaction condition and reaction are former
The proportion of material determines the simulation reaction product during the simulation reaction.
4. the continuous flow production control method of microreactor according to claim 1, which is characterized in that first analysis
Data change with the second analysis data analysis comparison, comprising: the first analysis data and the second analysis number
The variation for being greater than or equal to centesimal data deviation occurs according to analysis comparison.
5. a kind of continuous flow of microreactor produces control device characterized by comprising
Detection module detects the constituent and the corresponding constituent content data of each constituent of reaction raw materials；
Analog module, for the data of the corresponding constituent content of constituent according to the reaction raw materials, simulation reaction process,
Determine the simulation reaction product during simulation reaction；
Analysis module, for according to the simulation reaction product, analyze the simulation reaction product component data and the mould
The quasi- corresponding simulation constituent content data of reaction product component, determine the first analysis data；
Acquisition module, for acquiring the component data and the corresponding content number of the real reaction product component of real reaction product
According to determining the second analysis data；
Contrast module determines the first comparative analysis for the first analysis data described in comparative analysis and the second analysis data
Result data；
Determining module, when changing for the first analysis data described in the comparative analysis and the second analysis data,
Reaction condition and/or reaction raw materials proportion are adjusted according to the first comparative analysis result data, determines control program；
Control module carries out target product production for controlling microreactor according to the control program.
6. a kind of continuous flow production control system of microreactor characterized by comprising control module, raw material input module,
On-line mass spectroscopy instrument, microreactor module, micro-fluidic chip, collection of products device；
The raw material input module communication ends of the control module are connected with the communication ends of the raw material input module, for detecting
The constituent of the reaction raw materials of the raw material input module and the corresponding constituent content data of each constituent；
The on-line mass spectroscopy instrument communication ends of the control module are connected with the communication ends of the on-line mass spectroscopy instrument, online for receiving
Component data and the real reaction product component corresponding content data of the mass spectrograph to real reaction product；
The delivery outlet of the raw material input module is connected with the input port of the microreactor module, for arriving feedstock transportation
The microreactor module；
The input port in the channel of the micro-fluidic chip is connected with the delivery outlet of the microreactor module, the micro-fluidic core
First delivery outlet in the channel of piece is connected with collection of products device, for reaction product to be output to the collection of products device；
Second delivery outlet in the channel of the micro-fluidic chip is connected with the input port of on-line mass spectroscopy instrument, is used for reaction product
Sample be output to the on-line mass spectroscopy instrument.
7. the continuous flow production control system of microreactor according to claim 6, which is characterized in that further include: water-bath
Pot；
Water-bath communication ends in the control module are connected with the communication ends of water-bath by the communications cable, for controlling water
The temperature of bath；
The microreactor module is placed in water-bath, for controlling the temperature of microreactor module.
8. the continuous flow production control system of microreactor according to claim 6, which is characterized in that the raw material input
Module specifically includes: constant flow pump；
The communication ends of the raw material input module of the control module are connected with the communication ends of the constant flow pump, for controlling constant current
The flow of pump started and stopped while controlling reaction raw materials conveying.
9. the continuous flow production control system of microreactor according to claim 6, which is characterized in that the micro-fluidic core
Sample injector is equipped between second delivery outlet in the channel of piece and the input port of the on-line mass spectroscopy instrument；
Second delivery outlet in the channel of the micro-fluidic chip is connected with the input port of the sample injector, is used for reaction product
Sample be output to sample injector the sample gas of reaction product turned into gas；
The delivery outlet of the sample injector is connected with the input port of the on-line mass spectroscopy instrument, for extracting the gas output after gasifying
To the on-line mass spectroscopy instrument, the gas content is detected.
10. the continuous flow production control system of microreactor according to claim 6, which is characterized in that described according to micro-
Reactor module specifically includes: microreactor, coil pipe, counterbalance valve；
The microreactor is connected with the coil pipe, for adjust the reaction raw materials reacted in microreactor stop when
Between；
The coil pipe is connected with the counterbalance valve, for controlling the pressure of real reaction system.
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