CN116672981A - Microreactor based on fractal Sierbin triangle structure, application thereof and method for hydroformylation of gas-liquid olefin - Google Patents
Microreactor based on fractal Sierbin triangle structure, application thereof and method for hydroformylation of gas-liquid olefin Download PDFInfo
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- CN116672981A CN116672981A CN202210161787.4A CN202210161787A CN116672981A CN 116672981 A CN116672981 A CN 116672981A CN 202210161787 A CN202210161787 A CN 202210161787A CN 116672981 A CN116672981 A CN 116672981A
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- 239000007788 liquid Substances 0.000 title claims abstract description 39
- 150000001336 alkenes Chemical class 0.000 title claims abstract description 25
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000007037 hydroformylation reaction Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 239000012530 fluid Substances 0.000 claims abstract description 9
- 238000007789 sealing Methods 0.000 claims description 28
- 230000001154 acute effect Effects 0.000 claims description 4
- 238000012546 transfer Methods 0.000 abstract description 12
- 239000012429 reaction media Substances 0.000 abstract description 3
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 12
- 239000007791 liquid phase Substances 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 239000000376 reactant Substances 0.000 description 7
- 150000001299 aldehydes Chemical class 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- FXHGMKSSBGDXIY-UHFFFAOYSA-N heptanal Chemical compound CCCCCCC=O FXHGMKSSBGDXIY-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- BHVGMUDWABJNRC-UHFFFAOYSA-N (±)-2-methylhexanal Chemical compound CCCCC(C)C=O BHVGMUDWABJNRC-UHFFFAOYSA-N 0.000 description 3
- GGRQQHADVSXBQN-FGSKAQBVSA-N carbon monoxide;(z)-4-hydroxypent-3-en-2-one;rhodium Chemical compound [Rh].[O+]#[C-].[O+]#[C-].C\C(O)=C\C(C)=O GGRQQHADVSXBQN-FGSKAQBVSA-N 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 239000003446 ligand Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960000074 biopharmaceutical Drugs 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003256 environmental substance Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
-
- 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
-
- 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
- B01J19/0053—Details of the reactor
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/49—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reaction with carbon monoxide
- C07C45/50—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reaction with carbon monoxide by oxo-reactions
- C07C45/505—Asymmetric hydroformylation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention provides a micro-reactor based on a fractal Sierbin base triangle structure, application thereof and a method for gas-liquid olefin hydroformylation reaction. The micro-reactor is provided with a first inlet and a second inlet of a micro-channel, a second inlet and a micro-channel, wherein the first inlet and the second inlet of the micro-channel are communicated with the second inlet and the second outlet of the micro-channel through the micro-channel, and the micro-channel is of a structure based on a fractal Sierbinski triangle and can be used for multiphase fluid reactions, such as gas-liquid olefin hydroformylation reactions. The invention adopts the micro-channel based on the fractal Sierbin triangle structure, which can promote the contact of multiphase reaction media such as gas liquid, gas liquid and the like, strengthen multiphase mass transfer efficiency and further improve reaction efficiency.
Description
Technical Field
The invention relates to the technical field of microreactors, in particular to a microreactor based on a fractal Sierbinski triangle structure, application thereof and a gas-liquid olefin hydroformylation reaction method.
Background
The gas-liquid, liquid-liquid, gas-liquid multiphase reactions are widely occurring reaction processes in the chemical industry, such as hydrogenation, oxidation, chlorination, fluorination, absorption, etc. In these reaction systems, mixing of the reactants, mass transfer has a very large influence on the overall reaction process. For this reason, it is necessary to develop a chemical reactor with high efficiency.
The microchannel reactor has the advantages of large specific surface area, short diffusion transfer path, strong controllability and the like, can remarkably strengthen mass transfer and heat transfer processes, and can provide a clean and safe chemical production process, thus having great advantages for fast, strong exothermic (or endothermic) and mass transfer limited multiphase reactions.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a micro-reactor based on a fractal sierbins triangle structure, its use and a method for hydroformylation of gas-liquid olefins, which promote contact of multiphase reaction media such as gas-liquid, gas-liquid and the like, strengthen multiphase mass transfer efficiency, and further improve reaction efficiency.
To achieve the above and other related objects, a first aspect of the present invention provides a micro-reactor based on a fractal sierbias triangle structure, the micro-reactor being provided with a first inlet and outlet of a micro-channel, a second inlet and outlet of the micro-channel, and a micro-channel, the first inlet and outlet of the micro-channel being communicated with the second inlet and outlet of the micro-channel via the micro-channel, the micro-channel having a fractal sierbias triangle structure.
Preferably, the method further comprises at least one of the following technical characteristics:
a1 The micro-channel comprises a micro-channel first inlet and outlet flow channel, a fractal-based Shellbinsky triangle flow channel and a micro-channel second inlet and outlet flow channel, wherein the micro-channel first inlet and outlet is communicated with the micro-channel first inlet and outlet flow channel, the micro-channel first inlet and outlet flow channel is communicated with the junction of the triangular vertex in the fractal-based Shellbinsky triangle flow channel, and the micro-channel second inlet and outlet flow channel is communicated with the flow channel on the bottom edge of the triangle in the fractal-based Shellbinsky triangle flow channel;
a2 The depth of the micro-channel is 0.5-1 mm;
a3 The width of the micro-channel is 0.5-1 mm.
More preferably, in the feature a 1), at least one of the following technical features is further included:
a11 The fractal-based Shelloski triangular flow passage comprises a plurality of first junctions outside the triangular base in the fractal-based Shelloski triangular flow passage and a plurality of second junctions arranged at the triangular base in the fractal-based Shelloski triangular flow passage;
the first junction parts are communicated to form a plurality of first branch flow passages which form an acute angle or an obtuse angle with the bottom edge of the triangle;
a12 The length of the first inlet and outlet flow passage of the micro channel is 8-12 mm;
a13 The length of the second inlet and outlet flow passage of the micro channel is 8-12 mm.
Still more preferably, in the feature a 11), the microchannel further includes a plurality of second branch flow channels, which are communicated with a plurality of second junctions provided at the triangle base in the fractal-based sierbide triangle flow channel, and the plurality of second branch flow channels are communicated with the microchannel second inlet and outlet flow channels after being joined.
Preferably, the method further comprises at least one of the following technical characteristics:
b1 The micro-reactor further comprises a micro-channel plate, a sealing piece and a cover plate, wherein the micro-channel plate is provided with the micro-channel and a sealing groove, the sealing groove is arranged around the micro-channel, the sealing piece is arranged in the sealing groove, and the cover plate covers the micro-channel plate and is connected with the micro-channel plate;
b2 The microreactor is also provided with a temperature control unit.
More preferably, in feature b 1), the micro-reactor further comprises a fixing plate, and the cover plate is provided between the fixing plate and the micro-channel plate.
Still more preferably, the fixing plate partially or entirely covers the cover plate.
In a second aspect the invention provides the use of a microreactor based on a fractal sierbins triangle structure as described above for a multiphase fluid reaction. Specifically, the multiphase fluid reaction is a gas-liquid olefin hydroformylation reaction. The microreactor is used for carrying out the gas-liquid olefin hydroformylation reaction, but the application of other chemical, environmental, medical and other reaction systems is not excluded.
The third aspect of the invention provides a method for the hydroformylation of gas-liquid olefins, which is characterized in that the hydroformylation of gas-liquid olefins is carried out in the micro-reactor based on the fractal Sierbinski triangle structure.
As described above, the invention has at least one of the following advantageous effects:
1) The invention adopts the micro-channel based on the fractal Sierbin triangle structure, which can promote the contact of multiphase reaction media such as gas liquid, gas liquid and the like, strengthen multiphase mass transfer efficiency and further improve reaction efficiency.
2) The micro-reactor based on the fractal Shellbinsky triangle structure can be used for multiphase fluid reaction, can precisely control reaction conditions, ensures reaction safety and improves reaction efficiency.
Drawings
Fig. 1 is a schematic diagram of the structure of the 0-2-order sierbins triangle fractal, and a schematic diagram of the microchannel structure based on the 2-order sierbins triangle structure.
(a) Is a 0-2 order Shellbinsky triangle.
(b) Is a1 st order Shellbinsky triangle.
(c) Is a2 nd order Shellbinsky triangle.
(d) Is a schematic diagram of a micro-channel structure based on a 2-order Shellbinskii triangle structure.
FIG. 2 is a schematic structural diagram of a fixed plate in a microreactor based on a fractal Sierbin triangle structure according to the invention.
FIG. 3 is a schematic diagram of the structure of microchannel plates, seals and seal grooves in a microreactor based on fractal Sierbin triangle structure of the present invention.
FIG. 4 is a schematic diagram of the overall structure of a microreactor based on a fractal Sierbinski triangle structure according to the present invention.
Reference numerals
1. First inlet and outlet of micro-channel
2. Second inlet and outlet of micro-channel
3. Microchannel
31. First inlet and outlet flow passage of micro-channel
32. Fractal Sierbin-based triangular runner
321. First junction
322. Second junction
33. Microchannel second inlet and outlet runner
34. Second branch flow passage
4. Microchannel plate
5. Cover plate
6. Sealing groove
7. Fixing plate
Detailed Description
The invention is further illustrated below with reference to examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. The experimental methods and reagents not specifying the formulation in the following examples were carried out or configured under conventional conditions or conditions suggested by the manufacturer.
The micro-reactor based on the fractal Sierbinski triangle structure is provided with a micro-channel first inlet and outlet 1, a micro-channel second inlet and outlet 2 and a micro-channel 3, wherein the micro-channel first inlet and outlet 1 is communicated with the micro-channel second inlet and outlet 2 through the micro-channel 3, and the micro-channel 3 is provided with the Sierbinski triangle structure based on the fractal.
The invention provides a reaction device with high-efficiency mass and heat transfer capability, enriches the internal channel structure design of the existing micro-channel reactor, and the micro-reactor based on the fractal Sierbin base triangle structure is easy to manufacture and remarkably enhances mass and heat transfer. The Shellbinsky triangle in the fractal graph, as shown in figure 1, can be skillfully applied to a microreactor to achieve the effect of enhancing heat and mass transfer, can be mainly applied to the fields of energy chemical industry, biopharmaceuticals and the like, and is particularly suitable for reaction occasions involving multiphase fluids such as gas-liquid, gas-liquid and the like.
In a specific embodiment, the micro-channel 3 comprises a micro-channel first inlet and outlet flow channel 31, a fractal-based sierbine triangle flow channel 32 and a micro-channel second inlet and outlet flow channel 33, wherein the micro-channel first inlet and outlet 1 is communicated with the micro-channel first inlet and outlet flow channel 31, the micro-channel first inlet and outlet flow channel 31 is communicated with a junction part of the triangular peaks in the fractal-based sierbine triangle flow channel 32, and the micro-channel second inlet and outlet flow channel 33 is communicated with a flow channel on the bottom side of the triangle in the fractal-based sierbine triangle flow channel 32.
In a specific embodiment, the fractal-based xierbinski triangular flow passage 32 includes a plurality of first junctions 321 based on the outside of the base of the triangle in the fractal xierbinski triangular flow passage 32 and a plurality of second junctions 322 provided on the inside of the triangle in the fractal xierbinski triangular flow passage 32;
the first junction 321 is communicated to form a plurality of first branch flow passages, and the first branch flow passages form an acute angle or an obtuse angle with the bottom side of the triangle.
In a specific embodiment, the micro-channel 3 further includes a plurality of second branch flow channels 34, which are communicated with a plurality of second junction portions 322 provided on the basis of the triangle base in the fractal sierbide triangle flow channel 32, and the plurality of second branch flow channels 34 are communicated with the micro-channel second inlet/outlet flow channel 33 after being joined.
In a specific embodiment, the length of the first inlet and outlet channel 31 of the micro channel is 8-12 mm, so that the fluid flow can be fully developed.
In a specific embodiment, the length of the second inlet and outlet flow channel 33 of the micro-channel is 8-12 mm, so that the flow of the fluid can be fully developed.
In a specific embodiment, the depth of the micro-channel 3 is 0.5-1 mm, and the processing precision and performance of the micro-reactor are good.
In a specific embodiment, the width of the micro-channel 3 is 0.5-1 mm, and the processing precision and performance of the micro-reactor are good.
In a specific embodiment, the micro-reactor further comprises a micro-channel plate 4, a sealing member and a cover plate 5, wherein the micro-channel plate 4 is provided with micro-channels 3 and sealing grooves 6, the sealing grooves 6 are arranged around the micro-channels 3, the sealing member is arranged in the sealing grooves 6, and the cover plate 5 covers the micro-channel plate 4 and is connected with the micro-channels. The material of the microchannel plate 4 and the cover plate 5 may be polytetrafluoroethylene, and the microchannel 3 may be obtained by mechanically etching the microchannel plate 4. The sealing groove 6 is used for installing sealing elements, namely, sealing elements are installed between the microchannel plate 4 and the cover plate 5 between the sealing groove 6 for sealing. The sealing groove 6 may be 1.5mm deep and 2mm wide.
In a specific embodiment, as shown in fig. 2, the microreactor further comprises a fixing plate 7, and the cover plate 5 is disposed between the fixing plate 7 and the microchannel plate 4. The material of the fixing plate 7 may be stainless steel, and the cover plate 5 is pressed by the fixing plate 7.
In a specific embodiment, the fixing plate 7 partially or completely covers the cover plate 5. As shown in fig. 4, the fixing plate 7 partially covers the cover plate 5.
The microchannel plate 4 may be 5mm thick and provided with a number of threaded openings distributed around, e.g. 12 Φ9 openings. The cover plate 5 may be 2mm thick and provided with a number of threaded openings distributed around, for example 12 phi 9 openings. The fixing plate 7 can be provided with a plurality of threaded holes on the periphery, such as 12 3/8 inch threaded holes, and the plate thickness can be 5mm. The thickness of the integral microreactor may be 12mm.
In a specific embodiment, the micro-reactor is further provided with a temperature control unit, which can be a heat exchange module (such as a micro-channel plate far cover plate side), a heating and heat preservation module (such as a water bath unit or an oil bath unit, etc.).
As shown in fig. 3, as a specific example, the material of the microchannel plate 4 is polytetrafluoroethylene, the microchannels 3 can be obtained by mechanically etching the microchannel plate 4, the overall size of the reactor is 120×120×5mm, the depth of the microchannels is 1mm, and the width is 0.5mm. Around the microchannel 3 a ring of sealing grooves 6 with a depth of 1.5mm and a width of 2mm is provided for mounting the seal. Threaded holes are respectively formed in corresponding positions of the fixing plate 7, the cover plate 5 and the microchannel plate 4, and connection can be achieved through screws and threads.
A method for the hydroformylation of gas-liquid olefins, which is carried out in the microreactor based on the fractal Sierbinski triangle structure. Specifically, a mixed reactant solution containing olefin and catalyst with a certain concentration and synthesis gas enter the micro-reactor based on the fractal Sierbin triangle structure from a first inlet and outlet 1 of a micro-channel to react, and are discharged from a second inlet and outlet 2 of the micro-channel.
The micro-reactor can also be connected with a feeding system, a flow control system, a temperature control system, a pressure control system, a gas-liquid separator, a tail gas analysis system and the like. Specifically, include CO and H 2 The flow of the mixed gas from the gas cylinder is controlled by a gas mass flowmeter; preparing a mixed solution containing olefin and catalyst in a certain concentration, controlling the flow rate by a syringe pump, and mixing the mixed solution with a catalyst comprising CO and H at a tee joint 2 The mixed gas of the two-phase gas-liquid mixture is converged to form a gas-liquid two-phase mixture, the gas-liquid two-phase mixture enters the micro-reactor from the first inlet and outlet 1 of the micro-channel, and is discharged from the second inlet and outlet 2 of the micro-channel after the reaction is finished, the gas-liquid mixture is separated in the gas-liquid separator to obtain a liquid-phase product, and a back pressure valve can be arranged at a gas outlet to control the pressure of the system. After multiple diversion and confluence based on fractal Sierbin triangle structure in microreactor, the reaction is carried outThe synthesis gas in the reactant is continuously contacted with the reactant solution, so that a relatively uniform and fully contacted two-phase mixture is formed, and the purpose of enhancing mass transfer is achieved. In addition, the micro-reactor can be provided with a temperature control unit and a device capable of heating and accurately controlling the temperature so as to ensure the constant reaction temperature.
Example 1
The micro-reactor of the embodiment is based on a2 nd order Shellbinse triangle (the side length of the maximum triangle is 40 mm), as shown in fig. 3, a micro-channel first inlet and outlet 1, a micro-channel second inlet and outlet 2 and a micro-channel 3 are arranged, the micro-channel first inlet and outlet 1 is communicated with the micro-channel second inlet and outlet 2 through the micro-channel 3, the micro-channel 3 is provided with a fractal Shellbinse triangle structure, the micro-channel 3 comprises a micro-channel first inlet and outlet channel 31, a fractal Shellbinse triangle channel 32, a micro-channel second inlet and outlet channel 33 and 5 second branch channels 34, the micro-channel first inlet and outlet 1 is communicated with the micro-channel first inlet and outlet channel 31, the micro-channel first inlet and outlet channel 31 is communicated with the vertex junction of the triangle in the fractal Shellbinse triangle channel 32, the fractal Shellbinse triangle channel 32 comprises a plurality of first junctions 321 outside the triangle base in the fractal Shellbinse triangle channel 32 and a plurality of second junctions 322 arranged on the triangle base in the fractal Shellbinse triangle channel 32; each first junction 321 is communicated to form a plurality of first branch flow passages, and the first branch flow passages form an acute angle or an obtuse angle with the bottom side of the triangle; the second branch flow passages 34 are communicated with a plurality of second junction portions 322 provided on the basis of the triangle base in the fractal sierbide triangle flow passage 32, and the 5 second branch flow passages 34 are joined and communicated with the microchannel second inlet and outlet flow passage 33. The length of the first inlet and outlet flow passage 31 of the micro channel is 10mm; the length of the second inlet and outlet flow passage 33 of the micro-channel is 10mm; the depth of the microchannel 3 is 0.5mm; the width of the microchannel 3 is 0.5mm; the micro-reactor further comprises a micro-channel plate 4, a sealing piece and a cover plate 5, wherein the micro-channel plate 4 is provided with a micro-channel 3 and a sealing groove 6, the sealing groove 6 is arranged around the micro-channel 3, the sealing piece is arranged in the sealing groove 6, and the cover plate 5 covers the micro-channel plate 4 and is connected with the micro-channel plate; the micro-reactor also comprises a fixed plate 7, and a cover plate 5 is arranged between the fixed plate 7 and the micro-channel plate 4; the fixing plate 7 partially covers the cover plate 5.
The olefin hydroformylation reaction was carried out using the microreactor of this example (as shown in FIG. 3), with a liquid holdup of 8mL. By H 2 CO (volume ratio 1/1) is used as gas phase raw material, 1-hexene is used as substrate olefin (4 mmol), rhodium dicarbonyl acetylacetonate (0.02 mmol) is used as catalyst, biphosphite (0.02 mmol) is used as catalyst ligand, and toluene is used as solvent (16 ml). The prepared reactant solution is added into a feed tank, continuously introduced into a microreactor through a liquid phase pump, and continuously and stably added with synthesis gas through a gas flowmeter. The reaction temperature of the microchannel reactor is set to 90 ℃, the reaction pressure is 0.3MPa, the gas-liquid ratio is 5, and the reaction residence time is 10 minutes. The reaction raw materials are mixed and then enter a micro-channel reactor for olefin hydroformylation reaction, and the reaction crude product is cooled and separated into gas and liquid to obtain a liquid-phase aldehyde product. The conversion rate of 1-hexene of the liquid-phase aldehyde product reaches 100% by gas chromatography, the selectivity of n-heptanal is 86%, and the selectivity of 2-methylhexanal is 1.5%.
Example 2
The olefin hydroformylation reaction was carried out using the microreactor of example 1, with a liquid holdup of 8mL. By H 2 CO (volume ratio 1/1) is used as gas phase raw material, 1-hexene is used as substrate olefin (4 mmol), rhodium dicarbonyl acetylacetonate (0.02 mmol) is used as catalyst, biphosphite (0.02 mmol) is used as catalyst ligand, and toluene is used as solvent (16 ml). The prepared reactant solution is added into a feed tank, continuously introduced into a microreactor through a liquid phase pump, and continuously and stably added with synthesis gas through a gas flowmeter. The reaction temperature of the microchannel reactor is set to 80 ℃, the reaction pressure is 0.2MPa, the gas-liquid ratio is 3, and the reaction residence time is 10 minutes. The reaction raw materials are mixed and then enter a micro-channel reactor for olefin hydroformylation reaction, and the reaction crude product is cooled and separated into gas and liquid to obtain a liquid-phase aldehyde product. The conversion rate of 1-hexene of the liquid-phase aldehyde product reaches 90 percent by gas chromatography and 3 spectrum measurement, the selectivity of n-heptanal is 75 percent, and the selectivity of 2-methylhexanal is 4.8 percent.
Comparative example 1
As a comparative example of example 1, olefin hydroformylation was carried out using a capillary microchannel reactor (PFA microcapillary spiral, microchannel inner diameter 0.8 mm) as the microreactor, and the reaction vessel was maintainedLiquid amount was 5mL. By H 2 CO (volume ratio 1/1) is used as gas phase raw material, 1-hexene is used as substrate olefin (4 mmol), rhodium dicarbonyl acetylacetonate (0.02 mmol) is used as catalyst, biphosphite (0.02 mmol) is used as catalyst ligand, and toluene is used as solvent (16 ml). The prepared reactant solution is added into a feed tank, continuously introduced into a microreactor through a liquid phase pump, and continuously and stably added with synthesis gas through a gas flowmeter. The reaction temperature of the microchannel reactor is set to 90 ℃, the reaction pressure is 0.3MPa, the gas-liquid ratio is 5, and the reaction residence time is 20 minutes. The reaction raw materials are mixed and then enter a micro-channel reactor for olefin hydroformylation reaction, and the reaction crude product is cooled and separated into gas and liquid to obtain a liquid-phase aldehyde product. The conversion rate of 1-hexene of the liquid-phase aldehyde product reaches 100% through gas chromatography, the selectivity of n-heptanal is 62.3%, and the selectivity of 2-methylhexanal is 2.9%.
The above examples are provided to illustrate the disclosed embodiments of the invention and are not to be construed as limiting the invention. In addition, many modifications and variations of the methods and compositions of the invention set forth herein will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the invention. While the invention has been specifically described in connection with various specific preferred embodiments thereof, it should be understood that the invention should not be unduly limited to such specific embodiments. Indeed, various modifications of the described modes for carrying out the invention which are obvious to those skilled in the art are intended to be within the scope of the present invention.
Claims (10)
1. The micro-reactor based on the fractal Shellbinsky triangle structure is characterized by being provided with a first micro-channel inlet and outlet (1), a second micro-channel inlet and outlet (2) and a micro-channel (3), wherein the first micro-channel inlet and outlet (1) is communicated with the second micro-channel inlet and outlet (2) through the micro-channel (3), and the micro-channel (3) is provided with the fractal Shellbinsky triangle structure.
2. The microreactor based on fractal sierbins triangle structure according to claim 1, characterized by further comprising at least one of the following technical features:
a1 The micro-channel (3) comprises a micro-channel first inlet and outlet flow channel (31), a fractal-based Shellbinskis triangle flow channel (32) and a micro-channel second inlet and outlet flow channel (33), wherein the micro-channel first inlet and outlet (1) is communicated with the micro-channel first inlet and outlet flow channel (31), the micro-channel first inlet and outlet flow channel (31) is communicated with a junction of triangular peaks in the fractal-based Shellbinskis triangle flow channel (32), and the micro-channel second inlet and outlet flow channel (33) is communicated with a flow channel on the bottom edge of a triangle in the fractal-based Shellbinskis triangle flow channel (32);
a2 The depth of the micro-channel (3) is 0.5-1 mm;
a3 The width of the micro-channel (3) is 0.5-1 mm.
3. Microreactor based on fractal sierbins triangle structure according to claim 2, characterized in that in feature a 1) at least one of the following technical features is included:
a11 -the fractal-based xierbinski triangular flow channel (32) comprises a number of first junctions (321) outside the base of the triangle in the fractal-based xierbinski triangular flow channel (32) and a number of second junctions (322) provided at the base of the triangle in the fractal-based xierbinski triangular flow channel (32);
the first junction (321) is communicated to form a plurality of first branch flow passages, and the first branch flow passages form an acute angle or an obtuse angle with the bottom side of the triangle;
a12 The length of the first inlet and outlet flow passage (31) of the micro-channel is 8-12 mm;
a13 The length of the micro-channel second inlet and outlet flow channel (33) is 8-12 mm.
4. A micro-reactor based on a fractal sierbins triangle structure as in claim 3, characterized in that in feature a 11), said micro-channel (3) further comprises a plurality of second branch flow channels (34) communicating with a plurality of second junctions (322) provided at the base of the triangle in said fractal sierbins triangle flow channel (32), said plurality of second branch flow channels (34) being joined and communicating with said micro-channel second inlet and outlet flow channel (33).
5. Microreactor based on fractal sierbins-triangle structure according to any one of claims 1 to 4, characterized by at least one of the following technical features:
b1 The micro-reactor further comprises a micro-channel plate (4), a sealing piece and a cover plate (5), wherein the micro-channel plate (4) is provided with the micro-channel (3) and a sealing groove (6), the sealing groove (6) is arranged around the micro-channel (3), the sealing piece is arranged in the sealing groove (6), and the cover plate (5) covers the micro-channel plate (4) and is connected with the micro-channel plate;
b2 The microreactor is also provided with a temperature control unit.
6. Microreactor based on fractal sierbine triangle structure according to claim 5, characterized in that in feature b 1) the microreactor further comprises a fixation plate (7), the cover plate (5) being arranged between the fixation plate (7) and the microchannel plate (4).
7. Microreactor based on fractal sierbine triangle structure according to claim 6, characterized in that the fixing plate (7) is partly or entirely covered on the cover plate (5).
8. Use of a microreactor based on fractal sierbin-triangle structures according to any one of claims 1 to 7 for multiphase fluid reactions.
9. The use according to claim 8, wherein the multiphase fluid reaction is a gas-liquid olefin hydroformylation reaction.
10. A process for the hydroformylation of a gas-liquid olefin, characterized in that the hydroformylation of a gas-liquid olefin is carried out in a microreactor based on fractal sierbins triangle structure according to any of claims 1 to 7.
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| CN202210161787.4A CN116672981A (en) | 2022-02-22 | 2022-02-22 | Microreactor based on fractal Sierbin triangle structure, application thereof and method for hydroformylation of gas-liquid olefin |
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