CN106179148B - A kind of microreactor accurately amplified, preparation method and applications - Google Patents

A kind of microreactor accurately amplified, preparation method and applications Download PDF

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Publication number
CN106179148B
CN106179148B CN201610574054.8A CN201610574054A CN106179148B CN 106179148 B CN106179148 B CN 106179148B CN 201610574054 A CN201610574054 A CN 201610574054A CN 106179148 B CN106179148 B CN 106179148B
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channel
microreactor
liquid
feed
preparation
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CN106179148A (en
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巨少华
彭金辉
姜峰
郭胜惠
许磊
代林晴
张利华
肖毕权
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Ningbo Jugu Intelligent Equipment Co.,Ltd.
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Kunming University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093Microreactors, e.g. miniaturised or microfabricated reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00819Materials of construction
    • B01J2219/00835Comprising catalytically active material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00851Additional features
    • B01J2219/00855Surface features
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00851Additional features
    • B01J2219/00858Aspects relating to the size of the reactor
    • B01J2219/0086Dimensions of the flow channels

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Micromachines (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The present invention relates to a kind of microreactor accurately amplified, preparation method and applications, belong to micro- chemical technology field.The microreactor accurately amplified includes feed inlet, at least two channel, discharge port and connecting pipe, connecting pipe includes the connecting tube between the feed pipe connected between feed inlet and channel, at least two channel and the discharge pipe that is connected between channel and discharge port, the feed entrance of feed pipe to discharging inlet tubing diameter gradual change from big to small.The microreactor accurately amplified combines printing to be made using 3D printing technique and fluid mechanical emulation simulation system.The microreactor can be applied in gas liquid reaction, reactive liquid solution, liquid-solid reaction, liquid-liquid reaction and liquid-liquid-solid reaction.The present invention solves the problems, such as that this very promising chemical industry equipment of microreactor accurately amplifies, realize the integrated of thousands of a microchannels, import and export the connection of main channel and internal thousands of a channels, it is ensured that temperature, pressure, the flow pattern in each channel are highly consistent.

Description

A kind of microreactor accurately amplified, preparation method and applications
Technical field
The present invention relates to a kind of microreactor accurately amplified, preparation method and applications, belong to micro- chemical technology field.
Background technology
Microreactor has heat and mass efficient, the unique advantages such as green, safety, and revolutionary as chemical industry equipment New results, have boundless application prospect.The moment that material may be implemented in microreactor, uniformly mixing was passed with efficient Heat, therefore many reactions that cannot achieve in conventional reactor can be realized in microreactor.And microreactor Micro-word indicates that the channel of process fluid is other in the micron-scale, without refer to micro-reactor apparatus appearance and size is small or the yield of product It is small.It can include theoretically thousands of microchannel in microreactor, therefore can also realize very high yield.
But existing problem is, it is strictly hang-up to produce the microreactor with thousands of microchannels.Perfect condition Under, microreactor amplification should use " port number superposition(Numbering up)" mode, that is, increase the mode of functional unit, but It is that this mode means that and wants the thousands of a microchannels of process, and is also possible to complicated knot in each channel The structure of structure, the contact channel between main channel and this thousands of a channel is more complicated, because also needing to ensure each logical Temperature, pressure, the flow pattern in road are all highly consistent.Therefore, the method for current amplification microreactor is to take one in the world at present The amplification mode of kind compromise:" reaction chamber expansion ", such as grade even Centimeter Level is expanded as by micron order.It so really can be with The treating capacity of reactor is greatly improved, the pressure in channel is reduced.However, this scheme can but change some bases of microreactor Eigen, for example, by stably stratified flow or slug flow transfer become traditional turbulent flow, micron-sized stabilization fluid-flow contact become liquid Drip the unstable contact of continuous coalescence, controllable known mass transfer interface becomes uncontrollable mass transfer interface, micro- anti-to reduce Answer the reaction efficiency or selectivity of process so that the advantage of micro fluid reaction is unable to give full play.In addition, using with multiple channels Lamination of metal plates method the increase of number of active lanes, but the connection between its main channel and internal thousands of a channels may be implemented Still it is difficult to realize, and sealing, the encapsulation in channel etc. is all extremely difficult.
The 3D printing technique rapidly developed in recent years is also begun to for producing microreactor, but accurate without that can solve Amplify the problem of microreactor in ground.
Invention content
The problem of existing for the above-mentioned prior art and deficiency, the present invention provide a kind of microreactor accurately amplified, system Preparation Method and its application.The present invention solves the problems, such as that this very promising chemical industry equipment of microreactor accurately amplifies, and realizes Integrated, the connection of inlet and outlet main channel and internal thousands of a channels of thousands of a microchannels, and ensure each logical Temperature, pressure, the flow pattern in road are all highly consistent, and the invention is realized by the following technical scheme.
A kind of microreactor accurately amplified, including feed inlet, at least two channel, discharge port and connecting pipe, connecting tube Road include connecting tube between the feed pipe connected between feed inlet and channel, at least two channel and channel and discharge port it Between the discharge pipe that connects, the feed entrance of feed pipe to discharging inlet tubing diameter gradual change from big to small.
The feed entrance of the feed pipe is gradient to 0.2mm to discharging inlet tubing diameter from 0.5mm.
The connecting pipe is Y types symmetrically or non-symmetrically, and T-type is double-Y shaped, double-T shaped, Ψ types, camber, stepped one Kind or a variety of combinations.
The channel is straight channel, leads to multiple wedge-shaped or arc area channels, curved channel, helical duct, broken line The combination in one or more of road, sieve pore channel, irregular channel.
Single channel is equipped with single heat exchange unit.
The heat exchange unit includes single heat exchanger channels and its connecting pipe and liquid in-out mouth.
The channel is micron order or grade.
On the channel catalyst is equipped with using dipping, reaction solidification, heat-treating methods.
The port number that the microreactor includes is thousands of even more.
The port number that the microreactor includes is no less than 100.
The port number that the microreactor includes is no less than 1000.
The port number that the microreactor includes is not less than 10000.
The port number that the microreactor includes is no less than 100000.
The port number that the microreactor includes is no less than 1000000.
The port number that the microreactor includes is no less than 10000000.
The port number that the microreactor includes is no less than 100000000.
The above-mentioned microreactor accurately amplified is micro-mixer and/or micro- heat exchanger.
The flow pattern of each phase is one or more combinations of laminar flow, slug flow, drip or turbulent flow in above-mentioned channel.
A kind of microreactor preparation method accurately amplified, is as follows:
(1)The response characteristic of single channel to be amplified, feed inlet, discharge port and connecting pipe is studied, is determined Structure and size, pressure, flow, flow pattern, the optimum value of temperature in single channel;
(2)By step(1)The structure and size in obtained single channel, pressure, flow, flow pattern, the input of the optimum value of temperature Into 3D printing model, 2 channels are at least integrated, and add connecting pipe, realized between each channel and channel and charging Linking between mouth and discharge port obtains the 3D printing model of accurate amplification microreactor;
(3)By step(2)The 3D printing model of obtained accurate amplification microreactor carries out analogue simulation, optimization include into Material mouth, discharge port, each connecting pipe, the structure snd size in each channel;
(4)It will be through step(3)Structure snd size after optimization are to step(2)The 3D of obtained accurate amplification microreactor is beaten Stamp type is modified, and repeats analogue simulation and modification, number of repetition according to circumstances depending on, obtain final 3D printing model;
(5)3D printing equipment is selected according to required precision and printed material, by step(4)Obtain final 3D printing model It is input in the corresponding 3D printing software of selected 3D printing equipment, carries out two dimensionization slicing treatment, successively increase material printing, according to institute The difference of choosing printing type is post-processed accordingly, the microreactor accurately amplified.
The step(2)3D printing model in, feed inlet is two micro- liquid storage pipes of capsule, and the micro- liquid storage pipe of capsule passes through Y-shaped structure leads to feed pipe interface channel;Discharge port is split-phase pipeline, is equipped in the top and bottom of split-phase pipeline a diameter of The outlet tube of 5mm.
The step(3)Analogue simulation software be COMSOL, fluent or MATLAB.
The step(5)Middle post-processing is the cleaning on microreactor surface, the cleaning and dredging in channel.
Above-mentioned steps(5)Two dimensionization slicing treatment is by the modified 3D printing model along Z-direction by equal Thickness is divided into a series of X-Y scheme.
A kind of application of the microreactor accurately amplified, the microreactor accurately amplified are single-phase or heterogeneous reaction, Including gas liquid reaction, reactive liquid solution, liquid-solid reaction, liquid-liquid reaction and liquid-liquid-solid reaction.
The gas liquid reaction is that gas absorbs, aeration, gas elute.
The reactive liquid solution is liquid liquid solvent extraction, organic synthesis.
The liquid-solid reaction is coprecipitation solia particle.
The beneficial effects of the invention are as follows:
(1)The present invention solves the problems, such as that this very promising chemical industry equipment of microreactor accurately amplifies, and realizes into Integrated, the connection of inlet and outlet main channel and internal thousands of a channels of thousand a microchannels up to ten thousand, and ensure each channel Temperature, pressure, flow pattern are all highly consistent.
(2)The present invention ensure that micro fluid reaction heat transfer passes on the basis of in the order of magnitude improving microreactor treating capacity The advantage of matter, is of great significance.
(3)Operating method of the present invention is simple, strong operability, wide adaptability, and different originals can be selected according to no system The advantages such as material, have broad application prospects.
Description of the drawings
Fig. 1 is 1 microreactor dimensional structure diagram of the embodiment of the present invention;
Fig. 2 is 1 microreactor perspective view of the embodiment of the present invention;
Fig. 3 is 1 microreactor reaction channel zone cross-sectional schematic diagram of the embodiment of the present invention.
In figure:The feed inlet of a- material As, the feed inlet of b- materials B, c- feed pipes, d- reaction channels region, e- dischargings Area, the single heat exchanger channels of f-, the single channels g-.
Specific implementation mode
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
The microreactor accurately amplified, including feed inlet, 1000 channels, discharge port and connecting pipe, connecting pipe Feed pipe including being connected between feed inlet and channel, the connecting tube between channel and what is connected between channel and discharge port go out Pipe material, the feed entrance of feed pipe to discharging inlet tubing diameter gradual change from big to small;Wherein feed pipe is fed into Mouth is gradient to 0.2mm to discharging inlet tubing diameter from 0.5mm, and single channel is equipped with single heat exchange unit, heat exchange unit packet Include single heat exchanger channels and its connecting pipe and liquid in-out mouth(As shown in Figure 3).
The microreactor accurately amplified is applied to the extraction that copper and iron separation is related specifically to during liquid liquid solvent extraction Reaction.
The microreactor preparation method accurately amplified, is as follows:
(1)The response characteristic of single channel to be amplified, feed inlet, discharge port and connecting pipe is studied, is determined The structure in single channel is straight channel, size, pressure, flow, flow pattern, the optimum value of temperature;
(2)By step(1)The structure in obtained single channel is straight channel, size is 0.3 × 0.2 × 140mm(High, wide, It is long), pressure 0.2Mpa, two phase flow be respectively 0.01L/min, flow pattern be double interfaces laminar flow, temperature is room temperature, pH value is 1.5, feed pipe is that bis- " Y " are input in 3D printing model, integrates 1000 channels, and add connecting pipe, realizes each Being connected between channel and between channel and inlet port and outlet port, obtains the 3D printing model of accurate amplification microreactor, In the process feed inlet is two diameter 10mm, and a height of micro- liquid storage pipe of 50mm capsules is further ensured that it is every that water-oil phase enters Pressure when a channel is consistent, and the feed entrance of double Y-shaped feed pipes is gradient to discharging inlet tubing diameter from 0.5mm 0.2mm, discharge port are the split-phase pipeline of diameter 20mm, high 50mm, there is the outlet tube point of a diameter of 5mm at the top and bottom of it Oil, water two-phase reactor is not drawn into(Dimensional structure diagram is as shown in Figure 1, perspective view is as shown in Figure 2);
(3)By step(2)The 3D printing model of obtained accurate amplification microreactor is carried out through COMSOL software emulations Simulation, optimization includes feed inlet, discharge port, each connecting pipe, the structure snd size in each channel, the specific steps are:Setting Channel design size is global variable, carries out physical arrangement modeling, respectively viscosity, the density etc. of annex solution liquid two-phase extraction system Parameter adds CFD Laminar Flows and pipeline flow module, scanning of the addition to channel size and structural parameters in computing module And majorized function is added, simulation calculating is carried out, the structural parameters optimized;
(4)It will be through step(3)Structure snd size after optimization are to step(2)The 3D of obtained accurate amplification microreactor is beaten Stamp type is modified, and repeats analogue simulation and modification, number of repetition according to circumstances depending on, obtain final 3D printing model;
(5)3D printing equipment is selected according to required precision and printed material, by step(4)Obtain final 3D printing model It is input in the corresponding 3D printing software of selected 3D printing equipment, carries out two dimensionization slicing treatment, use class ABS photocuring trees Fat is printed using SLA laser curing forming techniques, successively increases material printing, after printing, uses alcohol in ultrasound immediately Cleaning is printed obtained reactor surface and inner passage, is injected alcohol into channel using pump in wave rinse bath, and dredging is internal Channel, drying, the microreactor amplified.
The microreactor of the present invention is applied in the extraction reaction of copper and iron separation, specific experiment result and parameter, which compare, sees Table 1.
Table 1
The experiment of the extraction reaction detached by the copper and iron of embodiment 1 it is found that the microreactor of the present invention ensure it is each Temperature, pressure, the flow pattern in channel are highly consistent, while ensure that on the basis of in the order of magnitude improving microreactor treating capacity The advantage of micro fluid reaction heat and mass.
Embodiment 2
The microreactor accurately amplified, including feed inlet, 10000 channels, discharge port and connecting pipe, connecting pipe Feed pipe including being connected between feed inlet and channel, the connecting tube between channel and what is connected between channel and discharge port go out Pipe material, the feed entrance of feed pipe to discharging inlet tubing diameter gradual change from big to small;Wherein feed pipe is fed into Mouth is gradient to 0.2mm to discharging inlet tubing diameter from 0.5mm, and single channel is equipped with single heat exchange unit, heat exchange unit packet Include single heat exchanger channels and its connecting pipe and liquid in-out mouth(As shown in Figure 3).
It applies the gas in gas liquid reaction to absorb the microreactor accurately amplified, is related specifically to sig water and absorbs sulphur Change the reaction of hydrogen.
The microreactor preparation method accurately amplified, is as follows:
(1)The response characteristic of single channel to be amplified, feed inlet, discharge port and connecting pipe is studied, is determined The structure in single channel is straight channel, size, pressure, flow, flow pattern, the optimum value of temperature;
(2)By step(1)The structure in obtained single channel is internal to have the helical channel of wedge-shape diversion bank, size to be Diameter 0.23mm, pressure 0.2Mpa, pressure 0.3Mpa, gas-liquid flow are respectively that 50mL/min and 20mL/min, flow pattern are Slug flow, passage length 240mm, temperature is 60 DEG C, feed pipe is that " Y " is input in 3D printing model, integrates 10000 Channel, and add connecting pipe realizes being connected between each channel and between channel and inlet port and outlet port, obtains essence The really 3D printing model of amplification microreactor, feed inlet is two a diameter of 30mm, a height of micro- storage of 80mm capsules in the process Liquid pipe is consistent come pressure when being further ensured that aqueous vapor two-phase enters each channel, and the feed entrance of Y-shaped feed pipe is to going out Material inlet tubing diameter is gradient to 0.2mm from 0.5mm, and discharge port is a diameter of 30mm, the split-phase pipeline of a height of 80mm, in Qi Ding Portion and bottom have the outlet tube of a diameter of 5mm that gas and water two-phase is drawn reactor respectively;
(3)By step(2)The 3D printing model of obtained accurate amplification microreactor is carried out through fluent software emulations Simulation, optimization includes feed inlet, discharge port, each connecting pipe, the structure snd size in each channel;
(4)It will be through step(3)Structure snd size after optimization are to step(2)The 3D of obtained accurate amplification microreactor is beaten Stamp type is modified, and repeats analogue simulation and modification, number of repetition according to circumstances depending on, obtain final 3D printing model
(5)3D printing equipment is selected according to required precision and printed material, by step(4)Obtain final 3D printing model It is input in the corresponding 3D printing software of selected 3D printing equipment, carries out two dimensionization slicing treatment, be divided by equal thickness Then a series of two bit pattern obtains micro- reaction of the Ti alloy materials of acid-alkali-corrosive-resisting using metal sintering 3D printing method Device;After printing, use immediately alcohol clear up in ultrasonic cleaner print obtained reactor surface and inner passage, Alcohol is injected into channel using pump, dredges inner passage, drying, the microreactor amplified.
The burr that reactor surface is removed using grinding machine is carried out the cleaning in pipeline using pickle, then uses compressed air It blows internal raffinate and residue off, obtains the microreactor product with 10000 channels.
The microreactor of the present invention is applied to the reaction that sig water absorbs hydrogen sulfide gas, specific experiment result and parameter Comparison is shown in Table 2.
Table 2
The experiment of stink damp precursor reactant is absorbed by the sig water of embodiment 2 it is found that the microreactor of the present invention ensures Temperature, pressure, the flow pattern in each channel are highly consistent, while in the order of magnitude improve microreactor treating capacity on the basis of It ensure that the advantage of micro fluid reaction heat and mass.
Embodiment 3
The microreactor accurately amplified, including feed inlet, 100 channels, discharge port and connecting pipe, connecting pipe packet Include the discharging connected between connecting tube and channel and discharge port between the feed pipe connected between feed inlet and channel, channel Pipeline, the feed entrance of feed pipe to discharging inlet tubing diameter gradual change from big to small;The wherein feed entrance of feed pipe It is gradient to 0.2mm to discharging inlet tubing diameter from 0.5mm, single channel is equipped with single heat exchange unit, and heat exchange unit includes Single heat exchanger channels and its connecting pipe and liquid in-out mouth(As shown in Figure 3).
It applies the gas in reactive liquid solution to absorb the microreactor accurately amplified, is more particularly to directed to In3+And Fe3+、 Zn2+Microfluid extraction and separation.
The microreactor preparation method accurately amplified, is as follows:
(1)The response characteristic of single channel to be amplified, feed inlet, discharge port and connecting pipe is studied, is determined The structure in single channel is straight channel, size, pressure, flow, flow pattern, the optimum value of temperature;
(2)By step(1)The structure in obtained single channel is straight channel, size is 0.6 × 0.05 × 140mm(Wide, It is high, long), pressure 0.2Mpa, two phase flow be respectively 0.01 L/min, flow pattern laminar flow, temperature be room temperature, pH value 0.432, Feed pipe is that Y-shaped is input in 3D printing model, integrates 100 channels, and adds connecting pipe, realize each channel it Between and channel and inlet port and outlet port between be connected, obtain the 3D printing model of accurate amplification microreactor, herein mistake Journey middle charging aperture is two micro- liquid storage pipes of capsule come pressure when being further ensured that water phase and an oil phase enters each channel consistent, " Y " The feed entrance of type feed pipe is gradient to 0.2mm to discharging inlet tubing diameter from 0.5mm, and discharge port is a diameter of 30mm, The split-phase pipeline of a height of 80mm has the outlet tube of a diameter of 5mm that oil, water two-phase are drawn reaction respectively at the top and bottom of it Device;
(3)By step(2)The 3D printing model of obtained accurate amplification microreactor is carried out through fluent software emulations Simulation, optimization includes feed inlet, discharge port, each connecting pipe, the structure snd size in each channel;
(4)It will be through step(3)Structure snd size after optimization are to step(2)The 3D of obtained accurate amplification microreactor is beaten Stamp type is modified, and repeats analogue simulation and modification, number of repetition according to circumstances depending on, obtain final 3D printing model
(5)3D printing equipment is selected according to required precision and printed material, by step(4)Obtain final 3D printing model It is input in the corresponding 3D printing software of selected 3D printing equipment, carries out two dimensionization slicing treatment, press and use class ABS photocuring trees Fat is printed using SLA laser curing forming techniques;Alcohol is used to clear up what printing obtained in ultrasonic cleaner immediately Reactor surface and inner passage inject alcohol into channel using pump, dredge inner passage, drying, that is amplified is micro- anti- Answer device.
The microreactor of the present invention is applied to In3+And Fe3+、Zn2+Microfluid extraction and separation, specific experiment result and Parameter is relatively shown in Table 3.
Table 3
Pass through the In of embodiment 33+And Fe3+、Zn2+Microfluid extraction and separation reaction experiment it is found that the present invention's is micro- anti- It answers device to ensure that the temperature, pressure, flow pattern in each channel are highly consistent, while in the order of magnitude improving microreactor treating capacity On the basis of ensure that the advantage of micro fluid reaction heat and mass.
Embodiment 4
The microreactor accurately amplified, including feed inlet, be not less than 10000 channels, discharge port and connecting pipe, even Take over road includes the connecting tube between the feed pipe connected between feed inlet and channel, channel and connects between channel and discharge port The discharge pipe connect, the feed entrance of feed pipe to discharging inlet tubing diameter gradual change from big to small;The charging of feed pipe Entrance is gradient to 0.2mm to discharging inlet tubing diameter from 0.5mm;Connecting pipe is asymmetric Y types and stepped combination;It is logical Road is that straight channel and curved channel combine, and single channel is equipped with single heat exchange unit, and heat exchange unit includes single heat exchanger channels And its connecting pipe and liquid in-out mouth, channel are micron order or grade.
The above-mentioned microreactor accurately amplified can be applied in liquid-liquid reaction.
Embodiment 5
The microreactor accurately amplified, including feed inlet, be not less than 10000000 channels, discharge port and connecting tube Road, connecting pipe include connecting tube between the feed pipe connected between feed inlet and channel, channel and channel and discharge port Between the discharge pipe that connects, the feed entrance of feed pipe to discharging inlet tubing diameter gradual change from big to small;Feed pipe Feed entrance to discharging inlet tubing diameter be gradient to 0.2mm from 0.5mm;Connecting pipe be asymmetric double-T shaped, camber and Ψ types combine;Channel is curved channel, helical duct, broken line channel, sieve pore channel and curved channel combination, is set on single channel Have a single heat exchange unit, heat exchange unit includes single heat exchanger channels and its connecting pipe and liquid in-out mouth, channel be micron order or Grade.
The above-mentioned microreactor accurately amplified can be applied in liquid-liquid-solid reaction.
Embodiment 6
The microreactor accurately amplified, including feed inlet, be not less than 10000000 channels, discharge port and connecting tube Road, connecting pipe include connecting tube between the feed pipe connected between feed inlet and channel, channel and channel and discharge port Between the discharge pipe that connects, the feed entrance of feed pipe to discharging inlet tubing diameter gradual change from big to small;Feed pipe Feed entrance to discharging inlet tubing diameter be gradient to 0.2mm from 0.5mm;Connecting pipe is Y types;Channel is curved channel, Single channel is equipped with single heat exchange unit, and heat exchange unit includes single heat exchanger channels and its connecting pipe and liquid in-out mouth, is led to Road is micron order or grade, uses dipping method to be equipped with metallic platinum catalyst on channel.
The above-mentioned microreactor accurately amplified can be applied in liquid-liquid-solid reaction.
The specific implementation mode of the present invention is explained in detail above in association with attached drawing, but the present invention is not limited to above-mentioned Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept Put that various changes can be made.

Claims (9)

1. a kind of preparation method of accurate amplification microreactor, it is characterised in that including feed inlet, no less than 100 channels, go out Material mouth and connecting pipe, connecting pipe include between the feed pipe connected between feed inlet and channel, no less than 100 channels Connecting tube and channel and discharge port between the discharge pipe that connects, the feed entrance of feed pipe to discharge opening pipeline diameter from Small gradual change is arrived greatly;Preparation method is as follows:
(1)The response characteristic of single channel to be amplified, feed inlet, discharge port and connecting pipe is studied, is determined single Structure and size, pressure, flow, flow pattern, the optimum value of temperature in channel;
(2)By step(1)Structure and size, pressure, flow, flow pattern, the optimum value of temperature in obtained single channel are input to 3D In printer model, no less than 100 channels are integrated, and add connecting pipe, realized between each channel and channel and charging Linking between mouth and discharge port obtains the 3D printing model of accurate amplification microreactor;The step(2)3D printing model In, feed inlet is two micro- liquid storage pipes of capsule, and the micro- liquid storage pipe of capsule leads to feed pipe interface channel by Y-shaped structure;Discharging Mouth is split-phase pipeline, and the outlet tube of a diameter of 5mm is equipped in the top and bottom of split-phase pipeline;
(3)By step(2)The 3D printing model of obtained accurate amplification microreactor carries out analogue simulation, and analogue simulation software is COMSOL, fluent or MATLAB, optimization includes feed inlet, discharge port, each connecting pipe, the structure in each channel and ruler It is very little, the specific steps are:Setting channel design size is global variable, carries out physical arrangement modeling, adds liquid-liquid diphase extraction respectively Viscosity, the density parameter of system are taken, CFD Laminar Flows and pipeline flow module are added, addition is to channel ruler in computing module Simultaneously majorized function is added in very little and structural parameters scannings, carries out simulation calculating, the structural parameters optimized;
(4)It will be through step(3)Structure snd size after optimization are to step(2)The 3D printing mould of obtained accurate amplification microreactor Type is modified, and repeats analogue simulation and modification, number of repetition according to circumstances depending on, obtain final 3D printing model;
(5)3D printing equipment is selected according to required precision and printed material, by step(4)Obtain final 3D printing model input Into the corresponding 3D printing software of selected 3D printing equipment, two dimensionization slicing treatment is carried out, successively increases material printing, is beaten according to selected The difference of print type is post-processed accordingly, the microreactor accurately amplified.
2. according to claim 1 accurately amplification microreactor preparation method, it is characterised in that the feed pipe into Material entrance is gradient to 0.2mm to discharge opening pipeline diameter from 0.5mm.
3. accurately amplifying the preparation method of microreactor according to claim 1, it is characterised in that the connecting pipe is pair One or more combinations of title or asymmetric Y types, T-type, double-Y shaped, double-T shaped, Ψ types, camber, step type.
4. according to claim 1 accurately amplification microreactor preparation method, it is characterised in that the channel be straight channel, In channel, curved channel, helical duct, broken line channel, sieve pore channel, irregular channel with multiple wedge shapes or arc area One or more of combinations.
5. according to the preparation method of the accurate amplification microreactor of claim 1 or 4, it is characterised in that set on single channel It includes heat exchanger channels and its connecting pipe and liquid in-out mouth to have single heat exchange unit, heat exchange unit.
6. according to the preparation method of the accurate amplification microreactor of claim 1 or 4, it is characterised in that the channel is micron Grade or grade.
7. according to the preparation method of the accurate amplification microreactor of claim 1 or 4, it is characterised in that the channel is equipped with Catalyst.
8. the preparation method of accurate amplification microreactor according to claim 1, it is characterised in that step(5)Described in after Processing is the cleaning on microreactor surface, the cleaning and dredging in channel.
9. the preparation method of accurate amplification microreactor according to claim 1, it is characterised in that described accurately to amplify Microreactor be single-phase or heterogeneous reaction, including gas liquid reaction, reactive liquid solution, liquid-solid reaction, liquid-liquid reaction and liquid-liquid-solid it is anti- It answers.
CN201610574054.8A 2016-07-21 2016-07-21 A kind of microreactor accurately amplified, preparation method and applications Active CN106179148B (en)

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