CN114471300A - Micro-channel assembly, micro-channel mixing equipment, mixing system and application - Google Patents
Micro-channel assembly, micro-channel mixing equipment, mixing system and application Download PDFInfo
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- CN114471300A CN114471300A CN202011169968.9A CN202011169968A CN114471300A CN 114471300 A CN114471300 A CN 114471300A CN 202011169968 A CN202011169968 A CN 202011169968A CN 114471300 A CN114471300 A CN 114471300A
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Images
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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00783—Laminate assemblies, i.e. the reactor comprising a stack of plates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00801—Means to assemble
- B01J2219/00804—Plurality of plates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00889—Mixing
Abstract
The invention discloses a micro-channel assembly, micro-channel mixing equipment, a mixing system and application. The microchannel component comprises a plurality of stacked sheets and oleophilic and/or hydrophilic fiber yarns filled between gaps of the adjacent sheets, wherein a plurality of microchannels are formed between the fiber yarns, and the fiber yarns are clamped and fixed through the sheets. The micro-channel mixing equipment and the micro-channel mixing system comprising the micro-channel assembly can enable one or more dispersed phases to form uniform and stable micron-sized particles in a phase state in a continuous phase, improve the mixing efficiency among materials, improve the reaction rate and the conversion depth, and have wide application prospects in the contact mass transfer reaction processes of gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid and the like.
Description
Technical Field
The invention belongs to the field of mass transfer reaction, and particularly relates to a microchannel component, microchannel mixing equipment and a microchannel mixing system, which can be widely applied to mass transfer reaction processes in the fields of petroleum, chemical industry, light industry, medicine, environmental protection and the like.
Background
In the fields of petroleum, chemical industry, light industry, medicine, environmental protection and the like, the mass transfer reaction processes of gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid and the like are involved, except for solids (the solids are generally catalysts), each reaction process relates to a dispersed phase and a continuous phase and a process of dispersing the dispersed phase into the continuous phase, wherein the dispersed phase refers to a system formed by highly dispersing one or more substances in a certain medium, the dispersed substance is called as the dispersed phase, and the continuous medium is called as the continuous phase.
For the above-mentioned gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid and other mass transfer reaction processes, the mass transfer process in most reactions is a rate control step, so that the gas-liquid, liquid-liquid mass transfer process, i.e. the process of dispersing the dispersed phase into the continuous phase, has an important influence on the reaction rate. For the gas-liquid reaction process, generally, in order to enhance the mass transfer force of the gas-liquid two-phase, under the condition that the efficiency of the gas-liquid mixing equipment is limited, the gas quantity provided by the system is far greater than the gas quantity consumed by the reaction, so that the problems of low reaction rate, uneven reaction heat, high equipment investment and high energy consumption are caused, and if the efficiency of the gas-liquid mixing equipment is greatly improved, the gas phase is efficiently dispersed in the liquid phase, the mass transfer efficiency of the gas-liquid two-phase is greatly improved, the reaction rate can be greatly improved, the gas supply quantity can be reduced, so that the reaction system is further reduced, the reaction heat is more uniform, and the investment and the operation cost are greatly reduced, thereby having more advantages.
For example, in the oil hydrogenation process, CN103965959A proposes a liquid phase hydrogenation reaction method of multi-stage dissolved hydrogen, in which firstly, a circulating liquid material is mixed with raw oil, and the mixture enters a heater for heating; dividing hydrogen into n paths, and heating in a heating furnace; one path of hydrogen and liquid phase materials are mixed in a mixer to carry out first-stage hydrogen dissolution, the rest (n-1) paths of hydrogen enter a hydrogen-oil mixing component in a reactor through an inlet of a reactor bed layer to be mixed with a mixture after the reaction of the previous bed layer, second-stage hydrogen dissolution is carried out, the final reaction product enters a stripping tower, one part of bottom oil of the stripping tower enters a product tank, and the other part of the bottom oil is recycled. The method disperses the hydrogen for n paths to increase the dissolving amount and uniformity in the oil product so as to improve the hydrogenation reaction rate, but because a conventional mixer is commonly used in the hydrogen-oil mixing process, on one hand, the process flow of introducing the hydrogen for multiple times is complex, and on the other hand, in order to meet the hydrogen dissolving amount in the reaction process, a large amount of circulating oil is also needed, and the investment and the energy consumption are still high.
For the liquid-liquid mass transfer process, typically the liquid-liquid extraction process, is a unit operation for separating a mixture by utilizing different solubilities of components in a solvent in a system, that is, a method for transferring solute substances from one solvent to another solvent by utilizing the difference of solubilities or distribution coefficients of the substances in two solvents which are not mutually soluble (or slightly soluble), wherein the liquid-liquid mass transfer rate is a key factor influencing the extraction efficiency, and therefore, the process of dispersing a dispersed phase into a continuous phase has an important influence on the reaction rate. For example, patent CN105112658A proposes a method for extracting rare earth elements by using micro-channels, which is a liquid-liquid extraction process, firstly, adding P507 or P204 into 260# solvent oil diluent according to a volume ratio of 3: 10-10: 3 to obtain an organic phase; taking a rare earth salt solution as a water phase, and taking an organic phase and the water phase according to the phase ratio of 5: 1-1: 5 and 5.55 multiplied by 10-10～4.17×10-8m3And (3) carrying out normal-temperature extraction on the volume flow rate/s in a microchannel of the microreactor to finally obtain an extraction phase containing the rare earth elements and raffinate. The method mainly aims to combine the advantages of high interface area, high mass transfer rate, short response time and the like of the micro-channel, and the aim of efficiently extracting the rare earth is fulfilled by efficiently contacting a dispersed phase and a continuous phase in the micro-channel through the contact of two phase interfaces in the micro-channel. However, because the method of the invention uses the microchannel reactor, the method is only suitable for the field with smaller processing capacity, and the method needs the microchannel reactor with high processing capacityThe reactor is very bulky and uneconomical and therefore not suitable.
In summary, for mass transfer reaction processes such as gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid, etc., a two-phase mixing process or a two-material mixing process is a key step of the progress of the prior art, and is a process route capable of effectively solving the problems of low reaction rate, long retention time, insufficient conversion rate, etc. caused by low rate of the mass transfer process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a micro-channel assembly, a micro-channel mixing device, a mixing system and application. The microchannel assembly, the device and the system can enable one or more disperse phases to form uniform and stable micron-sized particles in a phase state in a continuous phase, improve the mixing efficiency among materials, improve the reaction rate and the conversion depth, and have wide application prospects in the processes of gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid and the like which need to be contacted with mass transfer.
The microchannel component comprises a plurality of stacked sheets and a plurality of layers of oleophilic and/or hydrophilic fiber yarns filled between gaps of the adjacent sheets, wherein a plurality of microchannels are formed between the fiber yarns, and the fiber yarns are clamped and fixed by the sheets; the fiber yarns can be arranged in a single layer or multiple layers, preferably 1-50 layers, and more preferably 1-5 layers; when the fiber yarns are arranged in a multilayer mode, the projections of two adjacent layers of fiber yarns along the vertical direction of the sheet are preferably of a net structure; the shape of the mesh in the mesh structure can be any shape, such as one or more combinations of polygons, circles, ellipses and the like; in each layer of fiber yarns, the distance between adjacent fiber yarns is generally 0.5-50 μm, preferably equal distance arrangement, and the fiber yarns are arranged along any one direction of the transverse direction, the longitudinal direction or the oblique direction of the surface of the sheet; the fiber filaments may be in any curved shape, preferably in a periodically changing curved shape, such as a wave shape, a zigzag shape, etc., preferably the fiber filaments in the same layer have the same shape, and more preferably the fiber filaments in all layers have the same shape.
The diameter of the fiber yarn is generally 0.5-50 μm, preferably 0.5-5 μm, and more preferably 0.5-1 μm. The oleophilic fiber is selected from polyester fiber and nylonAt least one of fiber yarn, polyurethane fiber yarn, polypropylene fiber yarn, polyacrylonitrile fiber yarn and polyvinyl chloride fiber yarn, or fiber yarn material with oleophylic surface treatment; the hydrophilic fiber is generally selected from carboxyl (-COOH), amido (-CONH-), amino (-NH) with main chain or side chain2-. The selection of lipophilic or hydrophilic filaments is primarily related to the nature of the dispersed phase. Generally, when the dispersed phase is lipophilic, lipophilic microfiber filaments are selected, and when the dispersed phase is hydrophilic, hydrophilic microfiber filaments are selected, so that the dispersed phase is favorably adhered to and spread on the surfaces of the microfiber filaments in the microchannel, and is dispersed into liquid drops with smaller and uniform sizes, and the dispersion uniformity of the dispersed phase in the continuous phase is improved. When the dispersed phase is a gas phase, it may be oleophilic or hydrophilic or a combination thereof.
The thickness of the thin sheet is generally 0.05 mm-5 mm, preferably 0.1-1.5 mm. The material of the sheet is generally determined according to the properties of the overflowing material and the operating conditions, and can be any one or more of metal, ceramic, organic glass, polyester and the like, and stainless steel (such as SS30403, SS30408, SS32168, SS31603 and the like) materials in metal are preferred. The shape of the sheet is not limited, and may be any of a rectangle, a square, a polygon, a circle, an ellipse, a fan, and the like, and a rectangle or a square is preferable.
In the microchannel assembly, the size and the number of the sheets can be designed and adjusted according to the actual needs of the reaction. Typically, the microchannel module employs sheets of the same shape and size. The microchannel mixing assembly of the invention may be disposed directly within a reactor for material mixing.
The invention also provides micro-channel mixing equipment which comprises the micro-channel assembly and a shell, wherein the micro-channel assembly is fixed in the shell, one end of the shell is provided with an inlet for feeding a dispersed phase material and a continuous phase material, and the other end of the shell is provided with an outlet for discharging a mixed material; the microchannel component in the shell is divided into a feeding end and a discharging end along the crack direction, a feeding distribution space is arranged between the shell inlet and the feeding end, a discharging distribution space is arranged between the shell outlet and the discharging end, in order to prevent material short circuit, the material is ensured to flow to the discharging end from the feeding end in the microchannel component, and except the feeding end and the discharging end, all the other ends of the microchannel component are connected with the shell in a sealing way.
In the microchannel mixing device, a plurality of microchannel components connected in series can be arranged in the shell to improve the mixing effect.
The microchannel mixing device can be applied to processes involving a dispersed phase and a continuous phase in a reaction process and dispersing the dispersed phase into the continuous phase, such as supplying feeding materials for mass transfer reaction processes of gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid and the like. Specifically, the method can be applied to hydrogenation of hydrocarbon oil raw materials (gasoline, diesel oil, residual oil, wax oil, heavy oil, coal tar and dirty oil), olefin hydrogenation, fatty acid ester hydrogenation, ketone hydrogenation, hydrogenation process in hydrogen peroxide produced by an anthraquinone method and the like; absorption of acid gases, e.g. SO3Absorbed by sulfuric acid, NO2Absorbed by dilute nitric acid and CO2、SO2、H2S and the like are absorbed by alkali liquor; oxidation reaction of organic matters, such as oxidation process in the process of producing hydrogen peroxide by anthraquinone method, oxidation of chain alkane into acid, oxidation of p-xylene into terephthalic acid, oxidation of cyclohexane into cyclohexanone, oxidation of acetaldehyde into acetic acid, oxidation of ethylene into acetaldehyde, etc.; chlorination of organic matters, such as benzene into benzene chloride, toluene into toluene chloride, dodecyl alkane, ethylene and the like; other organic reactions such as hydroxylation of methanol to acetic acid, absorption of isobutylene by sulfuric acid, sulfation of alcohols by sulfur trioxide, polymerization of olefins in organic solvents, hydration of olefins, hydrolysis of fats and oils, and the like.
The microchannel mixing device can be arranged outside the reactor or internally arranged inside the reactor; as the reaction feed, it may be partially or wholly mixed using the present microchannel mixing device.
The invention also provides a micro-channel mixing system, which comprises the micro-channel mixing equipment, primary mixing equipment and a pipeline for connecting the materials mixed by the primary mixing equipment to the inlet of the micro-channel mixing equipment; the primary mixing device is used for primary mixing of the dispersed phase raw material and the continuous phase raw material to enable the dispersed phase raw material and the continuous phase raw material to become a mixed fluid; the primary mixing device can adopt any one or more of conventional devices with mixing function, such as a static mixer, a colloid mill, a shearing machine, a stirring kettle, a ceramic membrane tube and the like.
In the micro-channel mixing system, one or more micro-channel mixing devices can be arranged according to actual needs, and the micro-channel mixing devices can be connected in series or in parallel.
The invention also provides an application method of the micro-channel mixing equipment, which comprises the following steps: after the dispersed phase raw material and the continuous phase raw material are mixed through a pipeline and are introduced into a microchannel mixing device through an inlet, the dispersed phase raw material and the continuous phase raw material flow through a microchannel formed by fiber filaments in a microchannel assembly and are continuously cut for many times through the fiber filaments to form a mixed fluid containing a large number of micron-sized particles, and the mixed fluid is discharged from an outlet to be used as reaction feeding.
In the method of the present invention, the micron-sized particles in the mixed fluid formed by the microchannel mixing device generally have a size of 0.5 to 900 μm, preferably 0.5 to 50 μm.
In the method, preferably, the dispersed phase raw material and the continuous phase raw material are initially mixed and then introduced into micro-channel mixing equipment; the primary mixing can adopt any one or a plurality of combinations of conventional equipment with mixing function, such as a static mixer, a colloid mill, a shearing machine, a stirring kettle or a ceramic membrane tube, and the like, more preferably adopts the ceramic membrane tube equipment which is generally in a shell-and-tube structure, one or a plurality of bundles of membrane tubes are contained in a shell, wherein a continuous raw material is introduced into the tube bundle, a disperse phase raw material is introduced into a cavity outside the tube bundle, and the disperse phase raw material enters the tube bundle from the outside of the tube bundle to form nano/micron particles through nano/micron pore channels on the tube wall of the membrane tube under the push of pressure difference or concentration difference and is dispersed into the continuous phase, so that a large number of micron particles are uniformly dispersed in the continuous phase.
In the method, when the dispersed phase is a gas phase and the continuous phase is a liquid phase, the mass fraction of the gas phase in the liquid phase is generally 0.001-30%, preferably 0.01-10%; when the dispersed phase and the continuous phase are both liquid phases, the mass ratio of the dispersibility to the continuous phase is 1: 1000-1: 1, preferably 1: 50-1: 300; the mixing conditions are generally as follows: normal temperature to 380 ℃ and 0.1 to 20.0 MPaG.
In the method, the particle size of the mixed fluid formed by the micro-channel mixing equipment is 0.5-900 microns under the general condition, and when the dispersion uniformity is more than or equal to 80 percent, the mass transfer reaction rate can be greatly improved when the feeding is provided for the reaction process, and a better reaction effect can be achieved. Of course, according to the actual requirement of the mass transfer reaction process, no matter whether the dispersion uniformity of the particles is more than or equal to 80%, the mixed fluid can also be used as the feeding material of the reaction process as long as the dispersion phase particles are between 0.5 and 900 μm.
When two-phase or multi-phase mixing is carried out by adopting conventional mixing equipment, the problems of uneven mixing and unstable state exist, so that a dispersed phase is easy to dissociate from a continuous phase, and the phase separation occurs, thereby influencing the reaction mass transfer process. Therefore, the disperse phase and the continuous phase which need to be mixed are introduced into the microchannel mixing equipment, so that the feeding material passes through the microchannel formed among the fiber filaments in the microchannel component and is continuously cut for many times through the fiber filaments to form mixed fluid containing a large number of micron-sized particles, and the mixed fluid is used as reaction feeding material. Because of the special micro-channel structure of the micro-channel equipment and the surface properties of the filled superfine oleophilic or hydrophilic fiber filaments between the gaps of the adjacent sheets, the mixed feeding of the dispersed phase and the continuous phase is forcedly cut into mixed materials containing uniform particles with micron-sized particles, the existing state of the mixed materials is very stable, the specific surface area is very high, and the mixed materials are very important for reaction mass transfer processes, and especially have better reaction promoting effect on reaction processes with low reaction rate, long required retention time, high material viscosity, immiscible phases and the like. In addition, the oleophylic or hydrophilic selection of the superfine fiber filaments filled in the microchannel device is mainly determined according to the oleophylic or hydrophilic properties of the dispersed phase, and the purpose is to ensure that the properties of the dispersed phase are the same as the surface properties of the superfine fiber filaments, so that the contact and spreading of the dispersed phase materials on the surfaces of the fiber filaments are facilitated to be enhanced, the two phases are uniformly mixed, the dispersion uniformity in the continuous phase is improved, and meanwhile, the mixed phase is repeatedly cut by the superfine fiber filaments in the microchannel, so that the mixed phase can be dispersed into smaller particles with more uniform sizes.
The invention has the following technical effects: (1) the mixed fluid obtained by mixing the dispersed phase and the continuous phase by adopting the micro-channel mixing component has the characteristics of small particle size, high dispersion uniformity and stable existing state, greatly increases the mass transfer area of the two phases, eliminates the mass transfer reaction resistance, keeps higher mass transfer reaction rate and particularly has great improvement effect on the reaction process with large mass transfer resistance; (2) the invention is developed based on the principle that oleophylic \ or hydrophilic fiber in the micro-channel forcibly cuts materials repeatedly, so the invention still has good mixing effect on material systems with high viscosity, immiscible phases and the like, and overcomes the defects of other mixing equipment; (3) the method has wide application range, can realize that a very small amount of dispersed phase is uniformly dispersed in the continuous phase, and simultaneously can ensure that the dispersibility and the continuous phase form micron-sized particles with the size and the dispersion uniformity, and the size and the dispersion uniformity of the dispersed phase are key factors for realizing high-efficiency mass transfer reaction, so the method has promotion effect on a plurality of mass transfer reaction processes.
Drawings
FIG. 1 is a schematic view of a microchannel mixing device of the present invention.
FIG. 2 is a schematic view of a "K-type" microchannel mixing assembly.
Wherein, 1 is a dispersed phase raw material, 2 is a continuous phase raw material, 3 is an inlet of a micro-channel mixing device, 4 is an outlet of the micro-channel mixing device, 5 is the micro-channel mixing device, 6 is a shell of the micro-channel mixing device, 7 is a micro-channel component, 8 is a micro-channel sheet, 9 is a crack between the micro-channel sheets, 10 is a fiber filament, 11 is a feeding distribution space, 12 is a mixed fluid formed by the micro-channel device, 13 is a reactor, and 14 is a reaction product; 15 are the microchannels between the filaments in the slot of the microchannel sheet ("kappa" microchannels).
Detailed Description
The invention is described in detail below with reference to the figures and examples, but the invention is not limited thereby.
The application of the microchannel mixing device of the invention is illustrated by way of example in the accompanying figure 1:
firstly, conducting pipeline mixing on a dispersed phase raw material 1 and a continuous phase raw material 2, then introducing the mixture into a micro-channel mixing device 5 through a micro-channel mixing device inlet 3, firstly enabling the materials to enter a feeding distribution space 11 of a micro-channel mixing device shell 6, enabling the materials to enter a gap 9 between micro-channel sheets arranged in a micro-channel assembly 7 after the materials are distributed, continuously cutting the materials for many times through fiber yarns 10 filled in the gap 9 to form a mixed fluid containing a large number of micron-sized particles as a feeding material of a reactor 13, and leaving the mixed fluid as a reaction product 14 after mass transfer reaction is completed.
The micro-channel mixing equipment is applied to the aviation kerosene liquid phase hydrogenation reaction. The specific reaction conditions, procedures and equipment are shown in comparative example 1, example 1 and example 2. The raw oil is from the normal line of an atmospheric and vacuum distillation unit of a certain plant, the specific properties are shown in the table 1, and the protective agent/catalyst adopted in the hydrogenation reaction is FBN-03B01/FH-40A which smooths the research institute of petrochemical industry.
The micro-channel mixing device is applied to selective hydrogenation and olefin removal reaction of the reformate. The specific reaction conditions, procedures and equipment are shown in comparative example 2, example 3 and example 4. The raw oil used is reformed oil from a certain factory, the specific properties are shown in Table 2, and the catalyst used in the hydrogenation reaction is FHDO-18 of the research institute of petrochemical engineering.
TABLE 1 aviation kerosene feedstock Properties
TABLE 2 reformate feedstock Properties
Comparative example 1
In the aviation kerosene liquid phase hydrogenation process, the aviation kerosene raw material and hydrogen are mixed by adopting a conventional static mixer, and the model is SL 2.3/25-6.4-500.
The hydrogen accounts for 0.22 percent of the weight of the aviation kerosene raw material. Introducing the hydrogen-oil mixed material into a aviation kerosene hydrogenation reactor from the top of the reactor, and carrying out hydrogenation reaction in a catalyst bed filled in the reactor. The hydrogen-oil mixing conditions are as follows: the temperature is 55-60 ℃, and the pressure is 4.2 MPaG; the aviation kerosene hydrogenation reaction conditions are as follows: the temperature is 280-320 ℃, the pressure is 4.0MPaG, and the space velocity is 4.0h-1The protective agent/catalyst is FBN-03B01/FH-40A of the comforting petrochemical research institute.
The aviation kerosene raw materials in the table 1 are used as raw materials, and are mixed with hydrogen to carry out hydrogenation reaction to obtain a hydrogenation product. The properties of the hydrogen oil blend and product properties are shown in Table 3.
Comparative example 2
In the liquid-phase hydrogenation and olefin removal process of the reformate, the reformate is mixed with hydrogen by adopting a conventional static mixer, and the model is SV 2.3/25-2.5-500.
The hydrogen gas accounted for 0.102% of the mass of the reformate feedstock. Introducing the hydrogen-oil mixed material from the bottom of the reactor into the inlet of the reformate hydrodeolefination reactor to cause the hydrogen-oil mixed material to carry out hydrogenation reaction in a catalyst bed filled in the reactor. The hydrogen-oil mixing conditions are as follows: the temperature is 120-160 ℃, and the pressure is 1.8 MPaG; the reaction conditions of the liquid-phase hydrogenation and olefin removal of the reformate are as follows: the temperature is 120-160 ℃, the pressure is 1.7MPaG, and the space velocity is 10.0h-1The catalyst is FHDO-18 of the comforting petrochemical research institute.
The reformate raw material in table 1 was used as a reaction raw material, and was mixed with hydrogen gas and subjected to hydrogenation reaction to obtain a hydrogenated product. The properties of the hydrogen oil blend and product properties are shown in Table 3.
Example 1
By adopting the micro-channel mixing equipment shown in the attached figure 1, the sheets in the micro-channel mixing component are made of stainless steel, the thickness of each sheet is 1.0mm, 2 layers of nylon fiber yarns with the diameter of 1 mu m are filled between the cracks of the sheets, and the nylon fiber yarns are arranged at equal intervals, wherein the intervals are 1 mu m. The fiber filaments are in the shape of a curve with periodically changing wavy lines.
The dispersed phase raw material was hydrogen and the continuous phase raw material was the aviation kerosene raw material shown in table 1. The hydrogen accounts for 0.22 percent of the weight of the aviation kerosene raw material. After the aviation kerosene raw material and hydrogen are mixed by a pipeline and then are introduced into a micro-channel mixing device, a mixed fluid containing a large number of micron-sized particles is obtained and is introduced into an aviation kerosene hydrogenation reactor to carry out hydrogenation reaction. The mixing conditions of the microchannel mixing device were: the temperature is 55-60 ℃, and the pressure is 4.4-4.5 MPaG; the aviation kerosene hydrogenation reaction conditions are as follows: the temperature is 260-280 ℃, the pressure is 4.0MPaG, and the space velocity is 4.0h-1。
The microchannel mixing device of the invention provides reaction feed for the aviation kerosene hydrogenation reaction, and the properties and product properties of the obtained mixed material are shown in table 3.
Example 2
The micro-channel mixing device and the mixing system shown in the attached figure 1 are adopted, and the preliminary mixing device adopts a static mixer with the model number of SL 2.3/25-6.4-500. The thin slices in the micro-channel mixing equipment are made of stainless steel, the thickness of the thin slices is 1.0mm, 5 layers of polypropylene fiber yarns with the diameter of 1 mu m are filled between gaps of the thin slices, the fiber yarns are arranged at equal intervals, and the interval is 0.5 mu m. The superfine fiber filaments are in the shape of a curve with periodically changed wavy lines.
The dispersed phase raw material was hydrogen and the continuous phase raw material was the aviation kerosene raw material shown in table 1. The hydrogen accounts for 0.21 percent of the weight of the aviation kerosene raw material. After uniformly mixing the aviation kerosene raw material and hydrogen by a static mixer, introducing the aviation kerosene raw material and the hydrogen into the micro-channel mixing equipment to obtain a mixed fluid containing a large number of micron-sized particles, and introducing the mixed fluid into an aviation kerosene hydrogenation reactor to perform hydrogenation reaction. The mixing conditions of the preliminary mixing equipment and the micro-channel mixing equipment are as follows: the temperature is 55-60 ℃, and the pressure is 4.4-4.5 MPaG; the aviation kerosene hydrogenation reaction conditions are as follows: the temperature is 260-280 ℃, the pressure is 4.0MPaG, and the space velocity is 4.0h-1。
The microchannel mixing system of the invention provides reaction feed for the aviation kerosene hydrogenation reaction, and the properties and product properties of the obtained mixed material II are shown in Table 3.
Example 3
The microchannel mixing device shown in figure 1 is adopted, the thin sheet in the microchannel mixing device is made of stainless steel, the thickness of the thin sheet is 1.5mm, 2 layers of polypropylene fiber yarns with the diameter of 1 mu m are filled between the gaps of the thin sheet, and the superfine fiber yarns are arranged at equal intervals, wherein the interval is 0.5 mu m. The fiber filaments are in the shape of a curve with periodically changing wavy lines.
The dispersed phase raw material was hydrogen gas, and the continuous phase raw material was the reformate raw material shown in table 2. Hydrogen gas accounted for 0.014% of the mass of the reformate feedstock. After being mixed by a pipeline, the aviation kerosene raw material and hydrogen are introduced into the micro-channel mixing equipment to obtain a mixed fluid containing a large number of micron-sized particles, and the mixed fluid is introduced into the reformate hydrodeolefination reactor to carry out hydrodeolefination reaction. The mixing conditions of the microchannel mixing device were: the temperature is 55-60 ℃, and the pressure is 1.65 MPaG; the hydrogenation reaction conditions of the reformate are as follows: the temperature is 130-150 ℃, the pressure is 1.6MPaG, and the space velocity is 10.0h-1。
The microchannel mixing device of the present invention provides reaction feed for the reformate hydrogenation reaction, and the properties and product properties of the resulting mixed materials are shown in table 3.
Example 4
The micro-channel mixing system described in figure 1 was used, and the preliminary mixing equipment used a static mixer, model SX 2.3/25-2.5-450. The thin slices in the micro-channel mixing equipment are made of stainless steel, the thickness of each thin slice is 1.0mm, 5 layers of polyamide fiber yarns with the diameter of 1 mu m are filled between gaps of the thin slices, the polyamide fiber yarns are arranged at equal intervals, and the intervals are 1 mu m. The superfine fiber filaments are in the shape of a curve with periodically changed wavy lines.
The dispersed phase raw material was hydrogen gas, and the continuous phase raw material was the reformate raw material shown in table 2. Hydrogen gas accounted for 0.014% of the mass of the reformate feedstock. After uniformly mixing the aviation kerosene raw material and hydrogen through a static mixer, introducing the aviation kerosene raw material and the hydrogen into a microchannel device to obtain a mixed fluid containing a large number of micron-sized particles, and introducing the mixed fluid into a reformate hydrodeolefination reactor to perform hydrodeolefination reaction. The mixing conditions of the preliminary mixing equipment and the micro-channel mixing equipment are as follows: the temperature is 55-60 ℃, and the pressure is 1.45MPaG, respectively; the hydrogenation reaction conditions of the reformate are as follows: the temperature is 130-150 ℃, the pressure is 1.4MPaG, and the space velocity is 12.0h-1。
The microchannel mixing system of the present invention provides reaction feed for the reformate hydrogenation reaction, and the properties and product properties of the resulting mixed materials are shown in table 3.
TABLE 3 reactor feed Properties and product Properties
As is well known to those skilled in the art, in the conventional dispersing and mixing process of the dispersed phase and the continuous phase, the aim is to uniformly mix the dispersed phase and the continuous phase and disperse the dispersed phase into particles with smaller size and more uniform uniformity, the size of the dispersed phase particles can be obtained by a high-speed camera with the dispersing and mixing effect, the uniformity of the dispersed phase particles can be obtained by selecting a plurality of characteristic particles, and the smaller the size of the dispersed phase particles is, the higher the uniformity of the dispersed phase particles is, and the better the mixing and dispersing effect is. For the convenience of identification and measurement, the disperse phase can be replaced by different colors of tracers. Therefore, the method for measuring the mixing and dispersing effect of the present example and the comparative example is as follows: mixing the dispersed phase and the continuous phase by different mixing and dispersing methods (such as a conventional static mixer and a micro-channel mixer) under the same condition, wherein each method at least obtains 10 groups of mixed material samples, shooting the particle size of the dispersed phase in the mixed material samples by using a British IX i-SPEED 5 high-SPEED camera, summing the dispersed phase particles in the pictures, calculating the percentage content of the particles with various sizes, obtaining a normal distribution graph of the particles with various sizes, and further obtaining the uniformity of the particles.
It can be seen from the mixing effects of the present embodiment and the comparative example that, after the microchannel mixing device and the mixing system of the present invention are adopted, the micron-sized particles in the mixed material obtained by the microchannel mixing device have small size, high dispersion uniformity and stable existing state, so that the two-phase mass transfer area can be greatly increased, the mass transfer reaction resistance can be eliminated, and the high mass transfer reaction rate can be maintained. For example, when the catalyst is used for the hydrogenation reaction of aviation kerosene, more mild conditions, such as lower temperature and pressure and higher space velocity, can be adopted to achieve better hydrogenation effect compared with the existing aviation kerosene technology. When the catalyst is used for the liquid-phase hydrogenation and olefin removal reaction of reformate, the olefin removal effect is obviously improved under a mild condition, and the bromine index of the outlet of the olefin removal reactor is obviously reduced compared with that of the conventional mixing equipment, so that the ideal technical index is achieved.
Claims (31)
1. A microchannel assembly, comprising: the composite film comprises a plurality of stacked sheets and a plurality of layers of oleophilic and/or hydrophilic fiber yarns filled between gaps of the adjacent sheets, wherein a plurality of micro-channels are formed between the fiber yarns, and the fiber yarns are clamped and fixed through the sheets.
2. The microchannel assembly of claim 1, wherein: the number of the fiber yarn layers is 1-50, and more preferably 1-5.
3. The microchannel assembly of claim 1, wherein: when the fiber is arranged in multiple layers, the projections of the adjacent two layers of fiber filaments along the vertical direction of the sheet are in a net structure.
4. The microchannel assembly of claim 1, wherein: in each layer of the fiber yarns, the distance between adjacent fiber yarns is generally 0.5-50 μm, and the adjacent fiber yarns are preferably arranged at equal intervals.
5. The microchannel assembly of claim 1, wherein: each layer of fiber filaments is arranged along any one of the transverse direction, the longitudinal direction or the oblique direction of the surface of the sheet.
6. The microchannel assembly of claim 1, wherein: the fiber filaments are in any curved shape.
7. The microchannel assembly of claim 1 or 6, wherein: the fiber filaments are in a shape of a curve which changes periodically.
8. The microchannel assembly of claim 1 or 6, wherein: the fiber filaments in the same layer have the same shape.
9. The microchannel assembly of claim 1 or 6, wherein: the filaments of all layers are of the same shape.
10. The microchannel assembly of claim 1, wherein: the diameter of the fiber filament is generally 0.5-50 μm, preferably 0.5-5 μm, and more preferably 0.5-1 μm.
11. The microchannel assembly of claim 1, wherein: the oleophylic fiber yarn is at least one of polyester fiber yarn, nylon fiber yarn, polyurethane fiber yarn, polypropylene fiber yarn, polyacrylonitrile fiber yarn, polyvinyl chloride fiber yarn or fiber yarn material with oleophylic surface treatment.
12. The microchannel assembly of claim 1, wherein: the hydrophilic fiber is selected from one or more of natural high molecular polymers with hydrophilic groups on main chains or side chains or fiber materials with surfaces subjected to hydrophilic and oleophobic treatment.
13. The microchannel assembly of claim 1, wherein: the thickness of the thin sheet is 0.05 mm-5 mm, preferably 0.1-1.5 mm.
14. The microchannel assembly of claim 1, wherein: the thin sheet is made of any one of metal, ceramic, organic glass or polyester materials.
15. The microchannel assembly of claim 1, wherein: the shape of the sheet is any one of rectangle, square, polygon, circle, ellipse or fan.
16. Use of the microchannel assembly of claim 1 in liquid, liquid-liquid, gas-liquid-solid, and liquid-solid contact mass transfer reactions.
17. Use of a microchannel assembly according to claim 1 in a reactor, wherein: the microchannel component is directly arranged in the reactor and used for material mixing.
18. A microchannel mixing device, comprising: the apparatus comprising a microchannel assembly as claimed in any one of claims 1 to 6 and a housing.
19. The apparatus of claim 18, wherein: the micro-channel assembly is fixed in the shell, one end of the shell is provided with an inlet for feeding dispersed phase materials and continuous phase materials, and the other end of the shell is provided with an outlet for discharging mixed materials; the microchannel component in the shell is divided into a feeding end and a discharging end along the crack direction, a feeding distribution space is arranged between the shell inlet and the feeding end, a discharging distribution space is arranged between the shell outlet and the discharging end, in order to prevent material short circuit, the material is ensured to flow to the discharging end from the feeding end in the microchannel component, and except the feeding end and the discharging end, all the other ends of the microchannel component are connected with the shell in a sealing way.
20. The apparatus of claim 18, wherein: a plurality of micro-channel assemblies connected in series are arranged in the shell.
21. Use of the microchannel mixing device of claim 18 in gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid mass transfer reactions.
22. The micro-channel mixing device of claim 18, wherein the micro-channel mixing device is used in hydrogenation of hydrocarbon oil raw materials, hydrogenation of olefins, hydrogenation of fatty acid esters, hydrogenation of ketones, hydrogenation of hydrogen peroxide produced by an anthraquinone process, absorption reaction of acid gases, oxidation of hydrogen peroxide produced by an anthraquinone process, oxidation of chain alkanes to acids, oxidation of p-xylene to terephthalic acid, oxidation of cyclohexane to cyclohexanone, oxidation of acetaldehyde to acetic acid, oxidation of ethylene to acetaldehyde, chlorination of benzene to benzene chloride, chlorination of toluene to toluene chloride, chlorination of dodecane, chlorination of ethylene, hydroxylation of methanol to acetic acid, absorption of isobutylene to sulfuric acid, sulfation of alcohols to sulfur trioxide, polymerization of olefins in organic solvents, hydration of olefins or hydrolysis of fats and oils.
23. Use according to claim 20, characterized in that: the microchannel mixing device is arranged outside the reactor or arranged inside the reactor.
24. A method of using the microchannel mixing device of claim 18, comprising: after the dispersed phase raw material and the continuous phase raw material are mixed through a pipeline and are introduced into a microchannel mixing device through an inlet, the dispersed phase raw material and the continuous phase raw material flow through a microchannel formed by fiber filaments in a microchannel assembly and are continuously cut for many times through the fiber filaments to form a mixed fluid containing a large number of micron-sized particles, and the mixed fluid is discharged from an outlet to be used as reaction feeding.
25. The method of claim 24, wherein: the micro-scale particle size in the mixed fluid formed by the micro-channel mixing equipment is 0.5-900 μm, preferably 0.5-50 μm.
26. The method of claim 24, wherein: preliminarily mixing the dispersed phase raw material and the continuous phase raw material, and introducing the mixture into micro-channel mixing equipment; the preliminary mixing adopts any one or a combination of a plurality of static mixers, colloid mills, shearing machines, stirred tanks or ceramic membrane tubes.
27. The method of claim 25, wherein: the method is characterized in that ceramic membrane tube equipment is adopted and is of a shell-and-tube structure, one or more bundles of membrane tubes are contained in a shell, wherein a continuous raw material is introduced into a tube bundle, a disperse phase raw material is introduced into a cavity outside the tube bundle, the disperse phase raw material enters the tube bundle from the outside of the tube bundle through a nano/micron pore channel on the wall of the membrane tube under the pushing of pressure difference or concentration difference to form nano/micron particles, and the nano/micron particles are dispersed into a continuous phase, so that a large number of micron-sized particles are uniformly dispersed in the continuous phase.
28. The method of claim 24, wherein: when the dispersed phase is a gas phase and the continuous phase is a liquid phase, the mass fraction of the gas phase in the liquid phase is 0.001-30%; when the dispersed phase and the continuous phase are both liquid phases, the mass ratio of the dispersibility to the continuous phase is 1: 1000-1: 1.
29. A microchannel mixing system, comprising: the system comprises the microchannel mixing device of any one of claims 18 to 20, a primary mixing device and a pipeline for connecting the material mixed by the primary mixing device to the inlet of the microchannel mixing device.
30. The system of claim 29, wherein: the primary mixing equipment is used for primarily mixing the dispersed phase raw material and the continuous phase raw material to form a mixed fluid; the primary mixing equipment is any one or combination of a static mixer, a colloid mill, a shearing machine, a stirring kettle or a ceramic membrane tube.
31. The system of claim 29, wherein: one or more microchannel mixing devices are arranged, and the microchannel mixing devices are connected in series or in parallel.
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|---|---|---|---|---|
| CN115041110A (en) * | 2022-06-20 | 2022-09-13 | 浙江大学 | Liquid-liquid heterogeneous reaction strengthening method and device |
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Effective date of registration: 20231220 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |