CN211411969U - Micro-channel reactor - Google Patents
Micro-channel reactor Download PDFInfo
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- CN211411969U CN211411969U CN201921106109.8U CN201921106109U CN211411969U CN 211411969 U CN211411969 U CN 211411969U CN 201921106109 U CN201921106109 U CN 201921106109U CN 211411969 U CN211411969 U CN 211411969U
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- 239000007791 liquid phase Substances 0.000 claims abstract description 118
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 63
- 238000010438 heat treatment Methods 0.000 claims abstract description 59
- 239000003921 oil Substances 0.000 claims description 51
- 229910001220 stainless steel Inorganic materials 0.000 claims description 21
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- WAIPAZQMEIHHTJ-UHFFFAOYSA-N [Cr].[Co] Chemical compound [Cr].[Co] WAIPAZQMEIHHTJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005388 borosilicate glass Substances 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
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- 238000005485 electric heating Methods 0.000 claims description 2
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000004809 Teflon Substances 0.000 claims 1
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- 239000000047 product Substances 0.000 description 94
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 60
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 45
- 239000003795 chemical substances by application Substances 0.000 description 45
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 45
- 239000000463 material Substances 0.000 description 31
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Abstract
The utility model discloses a microchannel reactor, microchannel reactor include micromixer (a) and microreactor (b), and wherein micromixer (a) export is connected through connecting line (7) with microreactor (b) entry, the micromixer includes: water phase raw materials entry (1), oil phase raw materials entry (2), mixing channel (3), tapered micromesh hole (4), mixer sleeve pipe (5), mixer nozzle (6), the microreactor includes: the device comprises a gas-phase product outlet (8), a liquid-phase raw material inlet (9), a reactor outer wall (10), a reaction channel (11), a heating pipe wall (12), a liquid-phase product outlet (13), a gas-phase raw material inlet (14) and a heating medium inlet (15).
Description
Technical Field
The utility model relates to a microchannel reactor.
Background
The microchannel reactor is a novel process strengthening technology for carrying out chemical reaction, heat exchange, mixing, separation and control in a three-dimensional structure process fluid channel between 10 and 1000 micrometers, and is a highly integrated micro reaction system. Compared with the conventional reactor, the microchannel reactor has extremely small mass and heat transfer distance, so that the temperature gradient, the concentration gradient, the pressure gradient and the like are obviously increased, the heat and mass transfer efficiency and the space utilization rate can be improved, the reaction temperature, the reaction time and the material proportion are accurately controlled, and the microchannel reactor has intrinsic safety. Meanwhile, the microchannel reactor is produced in a large scale by adopting a quantity amplification mode, the development period is short, and no amplification effect exists.
In 1981, Turkerman D.B. and Pease R.F. put forward the concept of micro-channel heat sink for the first time, and successfully solved the thermal barrier problem faced by large-scale and ultra-large-scale integrated circuits. In 1985, Swift g. et al first developed a micro-scale heat exchanger for heat exchange of two fluids. In 1996, Lerous J.J. and Ehrfeld.W. respectively systematically illustrate the application principle and unique advantages of the microchannel reactor in the field of chemical engineering. Therefore, the micro-channel reaction technology concept rapidly draws attention of the research institutions and companies in the developed countries, such as the important research institutions of the united states, germany, uk, france, japan, and the like, colleges and universities, and many large chemical companies (such as MIT of the mart institute of technology, PNNL in the northwest pacific country, DuPont, BASF, IMM of the minitechnology institute of mad, Bayer, UOP, germany, and the like) have successively conducted research on micro-chemical engineering and technology. The micro-reactor mainly realizes the heat and mass transfer strengthening effect in the reaction process through the micro-scale effect generated by a special micro-scale structure, and has achieved a lot of breakthrough achievements in the micro-channel technology in the field of organic synthesis mainly based on liquid phase reaction, while the application of the micro-channel technology of a heterogeneous reaction system has certain limitation, and more micro-scale structures with specific effects need to be developed to realize the efficient heat and mass transfer effect in the specific heterogeneous reaction process.
Chinese patent CN201811039937 discloses a microchannel reactor with inserted fins, both of which can realize homogeneous mixing of high-efficiency liquid phase systems, but the mixing effect of immiscible liquid phase systems with large physical property difference is not very ideal, and the phenomenon of inhomogeneous mixing and even blockage can occur more easily in the application of heterogeneous systems such as gas-solid, liquid-solid, etc., and it has certain difficulty in large-scale production.
Disclosure of Invention
The invention aims to solve the technical problem of providing a microchannel reactor which is suitable for the mixed reaction separation multi-process coupling of a heterogeneous system based on a microchannel technology.
A microchannel reactor comprises a micromixer (a) and a microreactor (b), wherein an outlet of the micromixer is connected with an inlet of the microreactor through a connecting pipeline (7); the micromixer includes: water phase raw materials entry (1), oil phase raw materials entry (2), mixing channel (3), micromesh hole (4), mixer sleeve pipe (5), mixer nozzle (6), the microreactor includes: a gas-phase product outlet (8), a liquid-phase raw material inlet (9), a reactor outer wall (10), a reaction channel (11), a heating pipe wall (12), a liquid-phase product outlet (13), a gas-phase raw material inlet (14) and a heating medium inlet (15); the number of the micro mixers (a) is more than or equal to 2, preferably even number and symmetrically distributed; the micromixer (a) is positioned at the symmetrical positions of both sides of the microreactor (b), and the included angle between the central axis of the micromixer and the central axis of the microreactor is 30-150 degrees, preferably 60-120 degrees. The mixing channel (3) in the micro mixer (a) is an annular space I with an annular space interval of 10-1000 microns formed between the mixer sleeve (5) and the mixer nozzle (6), and the annular space interval is preferably 50-750 microns, and more preferably 400-600 microns. The micromesh (4) is distributed on the side surface of the columnar body of the mixer nozzle (6) and is selected from a folded micromesh, a trapezoidal micromesh or a Z-shaped micromesh. The hydraulic diameter of the folded micro-sieve pores is 5-500 microns, preferably 20-200 microns, the aperture ratio is 1-70%, preferably 10-20%, and the folded included angle is 20-160 degrees, preferably 60-120 degrees. The hydraulic diameter of the ladder-shaped micromesh is 10-400 microns, preferably 40-200 microns, the aperture ratio is 8-60%, preferably 20-30%, and the ladder-shaped folding angle is 30-80 degrees, preferably 30-60 degrees. The Z-shaped micro-sieve pore hydraulic diameter is 5-300 microns, preferably 40-100 microns, the aperture ratio is 15-30%, preferably 12-25%, and the Z-shaped included angle is 10-80 degrees, preferably 15-40 degrees. The liquid-phase raw material inlet (9) of the microreactor is a folded baffle with an inclination angle of 5-45 degrees, and an annular space II with an annular space interval of 100-500 micrometers, preferably 200-300 micrometers, is formed between the tail end of the folded baffle and the outer wall (10) of the microreactor. The reaction channel (11) is an annular space III with an annular space interval of 500-5000 microns, preferably 1000-4000 microns, and more preferably 2000-3000 microns, formed between the heating pipe wall (12) and the outer wall (10) of the reactor. In the microchannel reactor, a mixer sleeve (5) and a mixer spraying group (6) are made of stainless steel, glass and high-molecular polymer materials, preferably Hastelloy C, special borosilicate glass and polytetrafluoroethylene plastic; the outer wall (10) and the heating pipe wall (12) of the reactor are made of stainless steel and ceramic materials, preferably Hastelloy C and silicon carbide ceramic, the coaxiality of the mixer sleeve (5) and the mixer nozzle (6) is ensured to be within the range of phi 0.5-5 microns during assembly, and the coaxiality of the outer wall (10) and the heating pipe wall (12) is ensured to be within the range of phi 5-50 microns during assembly. The micro-channel reactor is heated by adopting heat conduction oil or electric heating.
Compared with the prior art, the microchannel device provided by the invention integrates multiple functions of mixing, reacting and separating, can be used for multi-process coupling of a heterogeneous reaction system, and can more efficiently perform a reaction process with balanced reaction property in the microchannel device
Drawings
FIG. 1 is a schematic structural diagram of a microchannel reactor provided by the present invention.
In the figure: (a) micro-mixer: an aqueous phase raw material inlet (1); an oil phase raw material inlet (2); a mixing channel (3); a conical micromesh (4); a mixer sleeve (5); mixer nozzle (6) (b) microreactor: a gas phase product outlet (8); a liquid phase raw material inlet (9); a reactor outer wall (10); a reaction channel (11); a heating tube wall (12); a liquid phase product outlet (13); a gas phase feed inlet (14); a conduction oil inlet (15); a connecting pipeline (7).
FIG. 2 is a top view of a microchannel reactor provided by the present invention.
FIG. 3 is a schematic structural view of a micromixer inner micromixer mesh according to the present invention
In the figure: (c) folding type micromesh holes; (d) ladder-shaped micromesh holes; (e) and (4) Z-shaped micromesh holes.
FIG. 4 is a schematic view of the layout of the micromixer holes
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
The following examples are carried out in microreactors according to the requirements of the process of the invention.
[ example 1 ]
The microchannel device main body is processed by stainless steel 316L and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro mixer is 100 microns, the aperture ratio is 15 percent, the structure included angle is 90 degrees, the annular space interval of the mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 30 degrees, the annular space of the liquid phase raw material inlet is 250 microns, and the annular space interval of the reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The analysis of the crude caprolactone shows that the conversion of cyclohexanone in this process is 89.2% and the selectivity of caprolactone is 97.1%.
[ example 2 ]
The microchannel device main body is made of stainless steel 316L, and is provided with 2 micro mixers which are symmetrically distributed on two sides of the microreactor, the included angle between the micro mixers and the central axis of the microreactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the mixer nozzle is 100 microns, the aperture ratio is 15 percent, the structural included angle is 90 degrees, the annular space interval of a mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the microreactor is 30 degrees, the annular space of the liquid phase raw material inlet is 250 microns, and the annular space interval of a reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed a cyclohexanone conversion of 88.8% and a caprolactone selectivity of 94.5% during the process.
[ example 3 ]
The microchannel device main body is made of stainless steel 316L, and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 60 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro mixer is 100 microns, the aperture ratio is 15 percent, the structural included angle is 90 degrees, the annular space interval of the mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 30 degrees, the annular space of the liquid phase raw material inlet is 250 microns, and the annular space interval of the reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed a cyclohexanone conversion of 87.1% during the process and a caprolactone selectivity of 92.2%.
[ example 4 ]
The microchannel device main body is processed by stainless steel 316L and is provided with 4 micro-mixers which are uniformly distributed around the micro-reactor, the included angle between the micro-mixers and the central axis of the micro-reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro-sieve pore structure is 200 microns, the aperture ratio is 15 percent, the structure included angle is 90 degrees, the annular gap interval of a mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro-reactor is 30 degrees, the annular gap of the liquid phase raw material inlet is 250 microns, and the annular gap interval of a reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed a cyclohexanone conversion of 87.7% during the process and a caprolactone selectivity of 93.3%.
[ example 5 ]
The microchannel device main body is processed by stainless steel 316L and is provided with 4 micro-mixers which are uniformly distributed around the micro-reactor, the included angle between the micro-mixers and the central axis of the micro-reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro-mixer is 100 microns, the aperture ratio is 10 percent, the structural included angle is 90 degrees, the annular space interval of a mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro-reactor is 30 degrees, the annular space of a liquid phase raw material inlet is 250 microns, and the annular space interval of a reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed a cyclohexanone conversion of 87.3% during the process and a caprolactone selectivity of 93.6%.
[ example 6 ]
The microchannel device main body is made of stainless steel 316L, and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro mixer is 100 microns, the aperture ratio is 15 percent, the structural included angle is 120 degrees, the annular space interval of the mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 30 degrees, the annular space of the liquid phase raw material inlet is 250 microns, and the annular space interval of the reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed a cyclohexanone conversion of 86.6% during the process and a caprolactone selectivity of 94.9%.
[ example 7 ]
The microchannel device main body is processed by stainless steel 316L and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro mixer is 100 microns, the aperture ratio is 15 percent, the structure included angle is 90 degrees, the annular space interval of the mixing channel is 750 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 30 degrees, the annular space of the liquid phase raw material inlet is 250 microns, and the annular space interval of the reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed 85.5% conversion of cyclohexanone and 94.5% selectivity to caprolactone.
TABLE 1
[ example 8 ]
The microchannel device main body is made of stainless steel 316L, and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro mixer is 100 microns, the aperture ratio is 15 percent, the structural included angle is 90 degrees, the annular space interval of the mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 40 degrees, the annular space of the liquid phase raw material inlet is 250 microns, and the annular space interval of the reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed a cyclohexanone conversion of 88.9% and a caprolactone selectivity of 94.2% during the process.
[ example 9 ]
The microchannel device main body is processed by stainless steel 316L and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro mixer is 100 microns, the aperture ratio is 15 percent, the structure included angle is 90 degrees, the annular space interval of the mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 30 degrees, the annular space of the liquid phase raw material inlet is 500 microns, and the annular space interval of the reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed 85.2% conversion of cyclohexanone and 94.2% selectivity to caprolactone.
[ example 10 ]
The microchannel device main body is made of stainless steel 316L, and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro mixer is 100 microns, the aperture ratio is 15 percent, the structure included angle is 90 degrees, the annular space interval of a mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 30 degrees, the annular space of a liquid phase raw material inlet is 250 microns, and the annular space interval of a reaction channel is 5000 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed 85.6% conversion of cyclohexanone and 94.2% selectivity to caprolactone.
[ example 11 ]
The microchannel device main body is processed by stainless steel 316L and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro mixer is 100 microns, the aperture ratio is 15 percent, the structure included angle is 90 degrees, the annular space interval of the mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 30 degrees, the annular space of the liquid phase raw material inlet is 250 microns, and the annular space interval of the reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 5 microns, and the coaxiality of the micro reactor sleeve is phi 10 microns. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed 83.2% conversion of cyclohexanone and 91.5% selectivity to caprolactone.
[ example 12 ]
The microchannel device main body is processed by stainless steel 316L and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro mixer is 100 microns, the aperture ratio is 15 percent, the structure included angle is 90 degrees, the annular space interval of the mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 30 degrees, the annular space of the liquid phase raw material inlet is 250 microns, and the annular space interval of the reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 20 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed 82.3% conversion of cyclohexanone and 90.4% selectivity to caprolactone.
[ example 13 ]
The microchannel device main body is processed by stainless steel 316L and is provided with 4 micro-mixers which are uniformly distributed around the micro-reactor, the included angle between the micro-mixers and the central axis of the micro-reactor is 90 degrees, a trapezoidal micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro-sieve pore structure is 100 microns, the aperture ratio is 15 percent, the structural included angle is 45 degrees, the annular gap interval of a mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro-reactor is 30 degrees, the annular gap of a liquid phase raw material inlet is 250 microns, and the annular gap interval of a reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed a cyclohexanone conversion of 87.5% during the process and a caprolactone selectivity of 94.8%.
[ example 14 ]
The microchannel device main body is made of stainless steel 316L, and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 90 degrees, a Z-shaped micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro-sieve pore structure is 100 microns, the aperture ratio is 15 percent, the structural included angle is 30 degrees, the annular gap interval of a mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 30 degrees, the annular gap of a liquid phase raw material inlet is 250 microns, and the annular gap interval of a reaction channel is 2500 microns. The coaxiality of the micro mixer sleeve is phi 1 micron, and the coaxiality of the micro reactor sleeve is phi 10 micron. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The crude caprolactone analysis showed a cyclohexanone conversion of 86.3% and a caprolactone selectivity of 95.2% during the process.
TABLE 2
Comparative example 1
The microchannel device main body is made of stainless steel 316L, and is provided with 4 micro mixers which are uniformly distributed around the micro reactor, the included angle between the micro mixer and the central axis of the micro reactor is 90 degrees, a folded micro-sieve pore structure is adopted on a mixer nozzle, the hydraulic diameter of the micro mixer is 100 microns, the aperture ratio is 15 percent, the structure included angle is 90 degrees, the annular space interval of a mixing channel is 500 microns, the inclination angle of a liquid phase raw material inlet of the micro reactor is 30 degrees, the annular space of a liquid phase raw material inlet is 250 microns, and the annular space interval of a reaction channel is 5000 microns. The coaxiality of the micro mixer sleeve is phi 10 micrometers, and the coaxiality of the micro reactor sleeve is phi 50 micrometers. And (3) building a microchannel reaction device by referring to a device schematic diagram shown in FIG. 1, wherein the device is used for temperature control through a cold-hot all-in-one machine, and reaction products can be collected from a liquid phase outlet of the microreactor. The device is used for caprolactone synthesis, and a metering pump is used for respectively conveying a water phase raw material containing a catalyst and an oil phase raw material containing a water-carrying agent, wherein the mass fraction of hydrogen peroxide in the water phase raw material is 50%, the mass fraction of the catalyst is 2%, and the mass fraction of toluene containing the water-carrying agent in the oil phase raw material is 50%. The two materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50 ℃. The liquid at the outlet of the micro mixer enters the micro reactor through a connecting pipeline to be used as a liquid-phase raw material, enters the micro reactor through a liquid-phase raw material inlet, is in countercurrent contact with air entering from a lower gas-phase inlet to carry out cyclohexanone oxidation reaction, and provides heat required by the reaction through a heating medium in a heating pipe wall. The temperature of the reaction channel is controlled to be 90 ℃ by heating heat conducting oil in the pipe wall, the reaction pressure is normal pressure, the residence time of reaction materials is controlled to be 10min by adjusting the flow rate of the metering pump and the length of the reaction channel, and the gas-liquid ratio in the reaction channel is controlled to be 10:1 by adjusting the gas mass flow meter. And a liquid-phase product of the microreactor is taken as a target product crude product-caprolactone and is discharged from a liquid-phase product outlet, a gas-phase product carries a water-carrying agent and water and is discharged from a gas-phase product outlet, and the gas-phase product is cooled and then is recycled through oil-water separation. The analysis of the crude caprolactone showed that the conversion of cyclohexanone was 70.6% and the selectivity to caprolactone was 90.2% during the process.
As can be seen from Table 1: the reaction effect of example 1 is much higher than that of comparative example 1, which shows that the coaxiality parameter of the microchannel device of the invention has a great influence on the practical use effect.
Claims (19)
1. A microchannel reactor comprises a micromixer (a) and a microreactor (b), wherein an outlet of the micromixer is connected with an inlet of the microreactor through a connecting pipeline (7); characterized in that the micromixer comprises: a water phase raw material inlet (1), an oil phase raw material inlet (2), a mixing channel (3), a micromesh hole (4), a mixer sleeve (5) and a mixer nozzle (6); the microreactor comprises: a gas-phase product outlet (8), a liquid-phase raw material inlet (9), a reactor outer wall (10), a reaction channel (11), a heating pipe wall (12), a liquid-phase product outlet (13), a gas-phase raw material inlet (14) and a heating medium inlet (15); the number of the micro mixers (a) is more than or equal to 2, and the micro mixers (a) are even and are symmetrically distributed; the micromixer (a) is positioned at the symmetrical positions of both sides of the microreactor (b), and the included angle between the central axis of the micromixer and the central axis of the microreactor is 30-150 degrees.
2. The microchannel reactor of claim 1 wherein the axis of the micromixer is at an angle of 60 to 120 ° to the axis of the microreactor.
3. The microchannel reactor according to claim 1, wherein the mixing channel (3) in the micromixer (a) is an annular space I with an annular gap interval of 10 to 1000 μm formed between the mixer sleeve (5) and the mixer nozzle (6).
4. The microchannel reactor of claim 3, wherein the annular space I has an annular gap spacing of 50 to 750 microns.
5. The microchannel reactor according to claim 1, wherein the micromesh (4) is distributed on the side of the column of the mixer nozzle (6) and is selected from a zigzag micromesh, a ladder micromesh, or a Z-micromesh.
6. The microchannel reactor of claim 5, wherein the folded micro-sieve holes have a hydrodynamic diameter of 5 to 500 microns, an opening ratio of 1 to 70%, and a folded included angle of 20 to 160 °.
7. The microchannel reactor of claim 6, wherein the pleated micro-mesh has a hydrodynamic diameter of 20 to 200 microns, an aperture ratio of 10 to 20%, and a pleat angle of 60 to 120 °.
8. The microchannel reactor of claim 5, wherein the ladder-type micro-sieve holes have a hydraulic diameter of 10 to 400 μm, an open ratio of 20 to 30%, and a ladder-type folding angle of 30 to 80 °.
9. The microchannel reactor of claim 8, wherein the ladder-type micro-mesh has a hydrodynamic diameter of 40 to 200 μm, an open porosity of 20 to 30%, and a ladder-type folding angle of 30 to 60 °.
10. The microchannel reactor of claim 5, wherein the Z-shaped micro-sieve holes have a hydrodynamic diameter of 5 to 300 microns, an opening ratio of 12 to 30%, and an included angle of 10 to 80 ° in the Z-shape.
11. The microchannel reactor of claim 10, wherein the Z-shaped microsieve has a hydrodynamic diameter of 40 to 100 microns, an open porosity of 15 to 25%, and an included Z-shape angle of 15 to 40 °.
12. The microchannel reactor according to claim 1, wherein the liquid phase raw material inlet (9) of the microreactor is a folded baffle plate with an inclination angle of 5-45 degrees, and an annular space II with an annular space interval of 100-500 microns is formed between the end of the folded baffle plate and the outer wall (10) of the microreactor.
13. The microchannel reactor according to claim 12, wherein the annular space II is formed between the end of the folded baffle and the outer wall (10) of the microreactor with an annular space interval of 200 to 300 μm.
14. The microchannel reactor according to claim 1, wherein the reaction channel (11) is an annular space III having an annular gap distance of 500 to 5000 μm formed between the wall (12) of the heating tube and the outer wall (10) of the reactor.
15. The microchannel reactor of claim 14 wherein the reaction channel (11) is an annular space iii having an annular gap spacing of 1000 to 4000 micrometers formed between the wall (12) of the heating tube and the outer wall (10) of the reactor.
16. The microchannel reactor of claim 1 wherein the mixer sleeve (5) and the mixer nozzle (6) are made of stainless steel, glass, and polymeric polymer; the outer wall (10) of the reactor and the wall (12) of the heating pipe are made of stainless steel and ceramic materials.
17. The microchannel reactor of claim 16 wherein the mixer sleeve (5) and the mixer nozzle (6) are made of stainless steel 316L, hastelloy C, specialty borosilicate glass, teflon plastic; the outer wall (10) and the heating pipe wall (12) of the reactor adopt stainless steel 316L, Hastelloy C and silicon carbide ceramics.
18. The microchannel reactor of claim 1 wherein the mixer sleeve (5) and the mixer nozzle (6) are assembled to ensure concentricity within the range of 0.5 to 5 microns, and the reactor outer wall (10) and the heater tube wall (12) are assembled to ensure concentricity within the range of 5 to 50 microns.
19. The microchannel reactor of claim 1, wherein the microchannel reactor is heated by conduction oil or electric heating.
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| CN112237891A (en) * | 2019-07-16 | 2021-01-19 | 中国石油化工股份有限公司 | Microchannel device and use thereof |
| CN114425276A (en) * | 2020-09-18 | 2022-05-03 | 中国石油化工股份有限公司 | Reactor and application thereof in preparation of carbon dioxide hydrocarbon by oxidative coupling of methane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112237891A (en) * | 2019-07-16 | 2021-01-19 | 中国石油化工股份有限公司 | Microchannel device and use thereof |
| CN112237891B (en) * | 2019-07-16 | 2025-07-04 | 中国石油化工股份有限公司 | Microchannel device and its application |
| CN114425276A (en) * | 2020-09-18 | 2022-05-03 | 中国石油化工股份有限公司 | Reactor and application thereof in preparation of carbon dioxide hydrocarbon by oxidative coupling of methane |
| CN114425276B (en) * | 2020-09-18 | 2023-08-15 | 中国石油化工股份有限公司 | Reactor and application thereof in preparation of carbon dioxide by oxidative coupling of methane |
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