CN115041110A - Liquid-liquid heterogeneous reaction strengthening method and device - Google Patents
Liquid-liquid heterogeneous reaction strengthening method and device Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 114
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000005728 strengthening Methods 0.000 title claims abstract description 10
- 239000012429 reaction media Substances 0.000 claims abstract description 28
- 238000012546 transfer Methods 0.000 claims abstract description 20
- 239000006185 dispersion Substances 0.000 claims abstract description 8
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- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 28
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 14
- 239000007791 liquid phase Substances 0.000 description 11
- FGGJBCRKSVGDPO-UHFFFAOYSA-N hydroperoxycyclohexane Chemical compound OOC1CCCCC1 FGGJBCRKSVGDPO-UHFFFAOYSA-N 0.000 description 8
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
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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
- B01J19/0053—Details of the reactor
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- 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
- B01J19/0066—Stirrers
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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
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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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
- B01J19/24—Stationary reactors without moving elements inside
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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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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Abstract
The invention discloses a liquid-liquid heterogeneous reaction strengthening method and a device, wherein a liquid-liquid heterogeneous reaction medium is introduced into a reactor through a liquid drop generator to generate a large amount of micron or millimeter-scale liquid drops, so that the mass transfer area of liquid-liquid two phases is increased, and the liquid-liquid heterogeneous reaction strengthening method and the device are matched with a mixing member arranged in the reactor to promote the uniform dispersion of the liquid-liquid two phases in the reactor and improve the liquid-liquid mass transfer rate and the reaction efficiency.
Description
Technical Field
The invention relates to the technical field of petrochemical industry and coal chemical industry, in particular to a liquid-liquid heterogeneous reaction strengthening method and a device.
Background
In chemical industry, liquid-liquid phase reaction processes are widely applied, such as nitration, sulfonation and alkylation in organic chemical industry, emulsion polymerization and suspension polymerization in polymer chemical industry, and the like. The liquid-liquid phase reaction is a process of series connection of mass transfer and reaction, and the mass transfer between phases is often the rate control step of the liquid-liquid phase reaction process. The liquid drops produced by the traditional methods of mechanical stirring, high-pressure mixing and the like have large diameters and poor distribution uniformity, and have no obvious effect on improving the mass transfer effect between liquid and liquid phases.
Compared with the conventional liquid drop, the micro liquid drop has the characteristics of small diameter, large specific surface area, high mass transfer efficiency and the like, and can greatly improve the liquid-liquid interfacial area and the liquid-liquid contact efficiency, thereby strengthening the liquid-liquid mass transfer process. In the liquid-liquid reactor, the dispersion characteristics of discrete phase droplets in the continuous phase have an important influence on liquid-liquid mixing and the contact area between phases, and therefore the dispersion state of the droplets is also an important evaluation index.
Disclosure of Invention
In view of the technical problems in the prior art, the present invention aims to provide a liquid-liquid heterogeneous reaction strengthening method and device, by using the device provided by the present invention, not only can liquid drops with a size of micron or millimeter level be generated, but also uniform mixing of liquid and liquid phases which are not mutually soluble in a reactor can be realized, and the reaction rate and the utilization efficiency of the device can be improved.
The invention can be realized by the following technical scheme:
the invention provides a liquid-liquid heterogeneous phase reaction strengthening method, which disperses discrete phase liquid in immiscible liquid-liquid heterogeneous reaction medium into micron or millimeter level liquid drops, and makes the liquid drops disperse uniformly, so as to increase the mass transfer area between phases in the heterogeneous reaction process and improve the reaction efficiency; the liquid-liquid heterogeneous phase reaction occurs in discrete phase liquid drops, the reaction medium in the continuous phase is subjected to mass transfer and enters the liquid drops to participate in the reaction, and the generated product stays in the liquid drops and/or is subjected to mass transfer from the liquid drops to enter the continuous phase.
In a preferred embodiment of the present invention, the conversion and selectivity of the reaction can be controlled by controlling the spatial dispersion state and/or size distribution and/or shape of the discrete phase droplets.
In a preferred embodiment of the present invention, the size distribution range of the discrete phase droplets is 1 μm to 10 mm.
In a preferred embodiment of the invention, the liquid-liquid heterogeneous reaction strengthening method is to disperse discrete phase liquid in a liquid-liquid heterogeneous reaction medium which is not mutually soluble into micron-sized droplets and uniformly disperse the micron-sized droplets, the liquid-liquid heterogeneous reaction occurs in the discrete phase droplets, and the reaction medium in a continuous phase is transferred into the droplets to participate in the reaction; further preferably, the product formed is mass transferred from within the droplets into the continuous phase. The micron-sized liquid drops increase the mass transfer area of the liquid-liquid two phases, the liquid-liquid two phases are uniformly dispersed in the reactor, and the liquid-liquid mass transfer rate and the reaction efficiency are improved.
The method of the present invention is suitable for liquid-liquid heterogeneous reactions including, but not limited to, nitration, sulfonation, alkylation, peroxide decomposition, emulsion polymerization, suspension polymerization, and the like.
The invention further provides a liquid-liquid multiphase reaction device for implementing the method, which comprises the following components:
a reactor main body to serve as a place where a liquid-liquid multiphase reaction medium is reacted;
a liquid inlet for introducing immiscible liquid-liquid multiphase reaction medium;
a droplet generator for dispersing discrete phase liquid in the multi-phase reaction medium into micron or millimeter scale droplets;
mixing means for uniformly dispersing and mixing the multi-phase reaction medium;
and a liquid discharge port for discharging the reaction liquid generated in the reactor main body.
In a preferred embodiment of the invention, the droplet generator breaks the discrete phase liquid into micron or millimeter sized droplets by any combination of one or more of micro-flow channel, fluid shear, mechanical agitation, external field action, and the like.
In some preferred embodiments: the micro-channel action mode is selected from one or more of a micropore method, a micropore membrane method and a microfluidic method.
In some preferred embodiments: the fluid shearing action mode is selected from one or more of jet shearing crushing method, rotational flow shearing crushing method and jet impact crushing method.
In some preferred embodiments: the external field action mode is selected from one or more of electric field action, ultrasonic field action and hypergravity field action.
The technical scheme of the invention is as follows: the liquid drop generator is arranged inside the reactor main body and/or outside the reactor main body, and at least one liquid drop generator is arranged.
The technical scheme of the invention is as follows: the mixing means include, but are not limited to, a stirrer and/or a jet nozzle and/or a draft tube and/or a packing, preferably a jet nozzle.
In some preferred embodiments: when the mixing component is selected from a stirrer, at least one layer of stirring paddle is arranged on the stirrer.
In some preferred embodiments: when the mixing member is selected from a jet nozzle, the jet nozzle is centrally and/or eccentrically arranged to the reactor body.
In some preferred embodiments: when the mixing member is selected from a guide shell, the diameter of the guide shell is 0.3-0.9 times of the diameter of the reactor main body, and the height of the guide shell is 0.4-0.7 times of the height of the reactor main body.
In some preferred embodiments: when the mixing member selects the filler, at least one layer of the filler is filled, and the height of the filler layer is 0.5-1.5 times of the diameter of the reactor main body.
In some preferred embodiments: a liquid-liquid multiphase reaction apparatus for carrying out the method of the present invention comprises:
a reactor main body to serve as a place where a liquid-liquid multiphase reaction medium is reacted;
a liquid inlet for introducing a liquid-liquid multiphase reaction medium which is immiscible with each other;
the micro-droplet generator is used for dispersing the discrete phase liquid in the multi-phase reaction medium into micro-scale droplets;
a jet nozzle for uniformly dispersing and mixing the multi-phase reaction medium;
and a liquid discharge port for discharging the reaction liquid generated in the reactor main body.
Compared with the prior art, the invention introduces the liquid-liquid multiphase reaction medium into the reactor through the liquid drop generator to generate a large amount of micron or millimeter-scale liquid drops, increases the mass transfer area of the liquid-liquid two phases, and simultaneously is matched with the mixing component arranged in the reactor to promote the uniform dispersion of the liquid-liquid two phases in the reactor, thereby improving the mass transfer rate of the liquid-liquid and the reaction efficiency.
Drawings
FIG. 1 is a schematic view of a liquid-liquid multiphase reaction apparatus according to the present invention.
FIG. 2 is a schematic view of the structure of another liquid-liquid multiphase reaction apparatus provided in the present invention.
FIG. 3 is a schematic view of the structure of another liquid-liquid multiphase reaction apparatus provided by the present invention.
FIG. 4 is a schematic view of the structure of another liquid-liquid multiphase reaction apparatus provided by the present invention.
Wherein: 1-a reactor body; 2-a liquid inlet; 3-a droplet generator; 4-a mixing member; 5-liquid discharge port.
Detailed Description
The following examples are provided to further illustrate the liquid-liquid multiphase reaction enhancement method and apparatus provided by the present invention, but the scope of the present invention is not limited thereto:
fig. 1 to 4 show a liquid-liquid multiphase reactor provided by the present invention, which comprises a reactor main body 1, a liquid inlet 2, a droplet generator 3, a mixing member 4 and a liquid outlet 5. The reactor body 1 is used as a place for carrying out a reaction as a liquid-liquid multiphase reaction medium; the liquid inlet 2 is used for introducing immiscible liquid-liquid multiphase reaction media; the droplet generator 3 is used for dispersing the discrete phase liquid in the multi-phase reaction medium into micron or millimeter-scale droplets; mixing means 4 for homogeneously dispersing and mixing the multi-phase reaction medium; a liquid discharge port 5 for discharging the reaction liquid generated in the reactor main body. The main difference between fig. 1-4 is the selection of different forms of mixing elements including, but not limited to, agitators and/or jet nozzles and/or guide cylinders and/or fillers. The mixing member shown in fig. 1 is selected from a stirrer, and at least one layer of stirring paddle is arranged on the stirrer; the mixing member shown in fig. 2 is selected from jet nozzles, which are centrally and/or eccentrically arranged in the reactor body; the mixing elements shown in FIG. 3 are selected from guide cylinders having a diameter of 0.3 to 0.9 times the diameter of the reactor body and a height of 0.4 to 0.7 times the height of the reactor body; the mixing member shown in fig. 4 is filled with at least one layer of packing, and the height of the packing layer is 0.5-1.5 times of the diameter of the reactor main body. Mixing construction is an important means to promote uniform dispersion of the two liquid-liquid phases within the reactor.
The droplet generator can select one or more of the action modes of micro-channel, fluid shearing, mechanical stirring, external field action and the like to be combined randomly to break the discrete-phase liquid into micron or millimeter-sized droplets. In some embodiments, the microchannel functions in a manner selected from the group consisting of one or more of a microporous method, a microporous membrane method, and a microfluidic method; the fluid shearing action mode is selected from one or more of a jet flow shearing crushing method, a rotational flow shearing crushing method and a jet flow impact crushing method; the external field action mode is selected from one or more combinations of electric field action, ultrasonic field action and hypergravity field action. The liquid drop generator is arranged inside the reactor main body and/or outside the reactor main body, and at least one liquid drop generator is arranged.
In the specific implementation process, a liquid-liquid multiphase reaction medium is introduced into the reactor through the liquid drop generator to generate a large amount of micron or millimeter-sized liquid drops, so that the mass transfer area of the liquid phase and the liquid phase is increased, and meanwhile, the uniform dispersion of the liquid phase and the liquid phase in the reactor is promoted through a mixing member arranged in the reactor, so that the mass transfer rate of the liquid phase and the reaction efficiency are improved. The reaction takes place in discrete phase droplets, the reaction medium in the continuous phase is mass-transferred into the droplets to participate in the reaction, and the produced product stays in the droplets and/or is mass-transferred from the droplets into the continuous phase.
Further, the conversion rate and selectivity of the above reaction can be controlled by controlling the spatially dispersed state and/or size distribution and/or shape of the discrete phase droplets.
Example 1
A liquid-liquid multiphase reactor as shown in figure 1 is adopted, a droplet generator generates droplets with the diameter of 550 mu m-2.4 mm by a jet flow shearing and crushing action mode, a mixing member is selected from a stirrer with a layer of stirring paddle, and a liquid outlet is positioned at the height of 1 time of the liquid level. The reaction medium is cyclohexane solution (continuous phase) of cyclohexyl hydroperoxide with the mass concentration of 3% and sodium hydroxide aqueous solution (discrete phase) with the mass concentration of 30%, the volume ratio of the continuous phase to the discrete phase is 90:10, the reaction is carried out at the temperature of 95 ℃ and under the normal pressure, the rotating speed of a stirrer is 200rpm, and the reaction time is 20 min. The reaction is carried out in the discrete phase liquid drop, the cyclohexyl hydroperoxide firstly enters the liquid drop from the mass transfer of the continuous phase, and then is decomposed in the liquid drop to generate cyclohexanol and cyclohexanone, and the generated cyclohexanol and cyclohexanone are further subjected to mass transfer from the liquid drop to the continuous phase. The experimental result shows that the decomposition rate of the cyclohexyl hydroperoxide is 95.3 percent, the total yield of the cyclohexanone and the cyclohexanol is 92.4 percent, and the weight ratio of the cyclohexanone: cyclohexanol 1.17: 1.
Comparative example 1
Under the same operating conditions as in example 1, the only difference from example 1 is that the liquid-liquid two-phase reaction medium is introduced into the reactor via a conventional pipe (the discrete phase is introduced into the reactor in the form of droplets with a diameter of 1-3 cm). The experimental result shows that the decomposition rate of the cyclohexyl hydroperoxide is 76.5 percent, the total yield of the cyclohexanone and the cyclohexanol is 82.6 percent, and the molar ratio of the cyclohexanone: cyclohexanol 0.92: 1.
Comparative example 2
Under the same operating conditions as in example 1, the only difference from example 1 is that no stirrer is provided in the reactor. The experimental result shows that the decomposition rate of the cyclohexyl hydroperoxide is 90.4 percent, the total yield of the cyclohexanone and the cyclohexanol is 89.5 percent, and the weight ratio of the cyclohexanone: cyclohexanol 1.01: 1.
Example 2
Using a liquid-liquid multiphase reactor as shown in FIG. 2, under the same operating conditions as in example 1, the only difference from example 1 is that the droplet generator produces droplets having a diameter of 300 μm to 1.5mm by means of a micropore method, the mixing member being selected from centrally disposed jet nozzles. The experimental result shows that the decomposition rate of the cyclohexyl hydroperoxide is 98.5 percent, the total yield of the cyclohexanone and the cyclohexanol is 97.6 percent, and the ratio of the cyclohexanone: cyclohexanol is 1.32: 1.
Example 3
The liquid-liquid multiphase reactor shown in FIG. 3 is used, under the same operation conditions as those of example 1, and differs from example 1 only in that the droplet generator generates droplets with a diameter of 400 μm to 2mm by the action of the rotational flow shear coupling applied electric field, and the mixing member is selected from a guide cylinder with a diameter of 0.6 times the diameter of the reactor and a height of 0.5 times the height of the reactor main body. The experimental result shows that the decomposition rate of the cyclohexyl hydroperoxide is 97.6 percent, the total yield of the cyclohexanone and the cyclohexanol is 93.5 percent, and the weight ratio of the cyclohexanone: cyclohexanol 1.25: 1.
Example 4
The liquid-liquid multiphase reactor as shown in fig. 4 is used, under the same operation conditions as those of example 1, the difference from example 1 is only that the droplet generator generates droplets with the diameter of 650 μm-3 mm by the action of microfluid coupling and an external ultrasonic field, the mixing member is selected from fillers, the height of the filler layer is 1.1 times of the diameter of the reactor, and 3 layers are filled. The experimental result shows that the decomposition rate of the cyclohexyl hydroperoxide is 91.4 percent, the total yield of the cyclohexanone and the cyclohexanol is 92.3 percent, and the weight ratio of the cyclohexanone: cyclohexanol 1.13: 1.
The above-mentioned embodiments are merely preferred embodiments of the present invention, and not intended to limit the present invention, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention, and the technical contents of the present invention, which are claimed, are all described in the claims.
Claims (10)
1. A liquid-liquid heterogeneous phase reaction strengthening method is characterized in that discrete phase liquid in a liquid-liquid heterogeneous phase reaction medium which is not mutually soluble is dispersed into micron or millimeter-scale liquid drops, and the micron or millimeter-scale liquid drops are uniformly dispersed in a continuous phase; the liquid-liquid heterogeneous phase reaction occurs in discrete phase liquid drops, the reaction medium in the continuous phase is subjected to mass transfer and enters the liquid drops to participate in the reaction, and the generated product stays in the liquid drops and/or is subjected to mass transfer from the liquid drops to enter the continuous phase.
2. The method according to claim 1, characterized in that the conversion and selectivity of the reaction are regulated by regulating the state of spatial dispersion and/or the size distribution and/or the shape of the droplets of the discrete phase.
3. The method of claim 1, wherein the discrete phase droplets have a size distribution in the range of 1 μm to 10 mm.
4. The method of claim 1, wherein the liquid-liquid heterogeneous reaction includes but is not limited to nitration, sulfonation, alkylation, peroxide decomposition, emulsion polymerization, suspension polymerization.
5. An apparatus for carrying out the method of any one of claims 1 to 4, comprising:
a reactor main body (1) for performing a reaction as a liquid-liquid multiphase reaction medium;
a liquid inlet (2) for introducing a liquid-liquid multiphase reaction medium which is immiscible with each other;
a droplet generator (3) for dispersing the discrete phase liquid in the multi-phase reaction medium into micron or millimeter-sized droplets; the liquid drop generators (3) are arranged inside the reactor body and/or outside the reactor body, and at least one liquid drop generator is arranged;
a mixing member (4) for homogeneously dispersing and mixing the multi-phase reaction medium;
a liquid discharge port (5) for discharging the reaction liquid generated in the reactor main body.
6. The device according to claim 5, wherein the droplet generator (2) breaks the discrete phase liquid into micron or millimeter sized droplets by one or more of any combination of micro flow channel, fluid shear, mechanical agitation, external field action.
7. The device of claim 6, wherein the micro flow channel functions in one or more selected from the group consisting of a micro-pore method, a micro-pore membrane method, and a micro-fluidic method.
8. The apparatus of claim 6, wherein the fluid shearing mode is selected from one or more of jet shearing fragmentation, rotational flow shearing fragmentation and jet impact fragmentation.
9. The device of claim 6, wherein the external field is applied by one or more selected from the group consisting of electric field, ultrasonic field, and high gravitational field.
10. Device according to claim 5, characterized in that the mixing means (3) comprise, but are not limited to, a stirrer and/or a jet nozzle and/or a guide cylinder and/or a packing.
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| CN117630302A (en) * | 2024-01-25 | 2024-03-01 | 清源创新实验室 | Device and method for measuring kinetic parameters of liquid-liquid heterogeneous intrinsic reaction |
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| CN111686665A (en) * | 2019-03-15 | 2020-09-22 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced reaction system |
| CN112169720A (en) * | 2019-07-04 | 2021-01-05 | 南京延长反应技术研究院有限公司 | Nano-micro interface enhanced reaction system |
| CN114471300A (en) * | 2020-10-28 | 2022-05-13 | 中国石油化工股份有限公司 | Micro-channel assembly, micro-channel mixing equipment, mixing system and application |
| CN112657439A (en) * | 2020-12-21 | 2021-04-16 | 山东建筑大学 | Liquid-liquid heterogeneous cyclone reactor based on multi-dimensional shearing action and reaction method |
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| CN117630302A (en) * | 2024-01-25 | 2024-03-01 | 清源创新实验室 | Device and method for measuring kinetic parameters of liquid-liquid heterogeneous intrinsic reaction |
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