CN114471300B - Microchannel assembly, microchannel mixing device, mixing system and application - Google Patents
Microchannel assembly, microchannel mixing device, mixing system and application Download PDFInfo
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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 assembly comprises a plurality of stacked thin sheets and lipophilic and/or hydrophilic fiber filaments filled between the cracks of the adjacent thin sheets, wherein a plurality of microchannels are formed between the fiber filaments, and the fiber filaments are clamped and fixed through the thin sheets. The microchannel mixing device and the system comprising the microchannel assembly can enable one or more disperse phases to form uniform and stable micron-sized particles in a continuous phase, improve the mixing efficiency between 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-liquid-solid and other contact mass transfer reactions.
Description
Technical Field
The invention belongs to the field of mass transfer reaction, and particularly relates to a micro-channel assembly, micro-channel mixing equipment and a 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, more mass transfer reaction processes such as gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid and the like are involved, and each reaction process involves a dispersed phase and a continuous phase except for a solid (generally, a catalyst) 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 substances are called as the dispersed phase, and the continuous medium is called as the continuous phase.
For the above-mentioned mass transfer reaction processes of gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid, etc., most of the mass transfer processes in the reaction are rate control steps, so that the mass transfer process of gas-liquid, liquid-liquid, 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, in order to enhance the mass transfer force of the gas-liquid two phases 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 and high equipment investment and 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 phases is greatly improved, the reaction rate can be greatly improved, the gas supply quantity is reduced, the reaction system is further reduced, the reaction heat is also more uniform, and the investment and the running cost are greatly reduced, so that the method has more advantages.
For example, in the oil hydrogenation process, CN103965959a proposes a multistage hydrogen-dissolving liquid phase hydrogenation reaction method, in which first, a circulating liquid material is mixed with a raw oil, and the mixture is heated by a heater; the hydrogen is divided into n paths and enters a heating furnace for heating; one path of hydrogen and liquid phase materials are mixed in a mixer to carry out first-stage hydrogen dissolution, the rest (n-1) path of hydrogen enters a hydrogen oil mixing component in the mixer through an inlet of a reactor bed layer to be mixed with the mixture after the reaction of the previous bed layer to carry out second-stage hydrogen dissolution, the final reaction product enters a stripping tower, part of stripping tower bottom oil enters a product tank, and part of stripping tower bottom oil is recycled. The method is used for dispersing the hydrogen into n paths to increase the dissolution and uniformity in the oil 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 more complicated, and on the other hand, a large amount of circulating oil is required to meet the hydrogen dissolution in the reaction process, and the investment and the energy consumption are still higher.
For the liquid-liquid mass transfer process, a liquid-liquid extraction process is typically used for separating a mixture by utilizing the different solubilities of the components in the system in the solvents, namely, utilizing the difference of the solubilities or partition coefficients of the materials in two mutually insoluble (or slightly soluble) solvents, the transfer of solute materials from one solvent to the other is a key factor affecting the extraction efficiency, and therefore the process of dispersing the dispersed phase into the continuous phase has an important influence on the reaction rate. In the method for extracting rare earth elements by using a micro-channel as proposed in patent CN105112658A, the method is a liquid-liquid extraction process, wherein P507 or P204 is added with 260# solvent oil diluent according to the volume ratio of 3:10-10:3 to obtain an organic phase; taking rare earth salt solution as water phase, and taking organic phase and water phase as 5:1-1:5 according to the ratio of 5.55X10 -10 ～4.17×10 -8 m 3 And (3) carrying out normal-temperature extraction on the volume flow rate/s in a micro-channel of the micro-reactor, and finally obtaining an extraction phase containing rare earth elements and raffinate. The method mainly aims to combine the advantages of high specific surface area, high mass transfer rate, short response time and the like of a microchannel, and the aim of efficiently extracting rare earth is fulfilled by efficiently contacting a disperse phase and a continuous phase in the microchannel through the contact of a two-phase interface in the microchannel. However, since the method of the present invention uses a microchannel reactor, the method is applicable only to the field where the throughput is small, and the microchannel reactor required for high throughput is very large and uneconomical, and thus is not applicable.
In summary, in the mass transfer reaction process of gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid, and the like, the two-phase mixing or 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 residence time, insufficient conversion rate, and the like caused by low mass transfer process rate.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a micro-channel assembly, micro-channel mixing equipment, 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 continuous phase, improve the mixing efficiency between 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 needing to be contacted and transferred.
The microchannel assembly comprises a plurality of stacked thin sheets and a plurality of layers of lipophilic and/or hydrophilic fiber filaments filled between the cracks of the adjacent thin sheets, wherein a plurality of microchannels are formed between the fiber filaments, and the fiber filaments are clamped and fixed through the thin sheets; the fiber filaments can be arranged in a single layer or multiple layers, preferably 1-50 layers, more preferably 1-5 layers; when the fiber yarns are arranged in multiple layers, the projection of two adjacent layers of fiber yarns along the vertical direction of the sheet is preferably a net structure; the mesh shape in the mesh structure can be any shape, such as one or more of a polygon, a circle, an ellipse, etc.; in each layer of fiber filaments, the spacing between adjacent fiber filaments is generally 0.5-50 μm, preferably the fiber filaments are distributed at equal intervals, and the fiber filaments are distributed along any one direction of transverse direction, longitudinal direction or oblique direction of the surface of the sheet; the filaments may be of any curvilinear shape, preferably a periodically varying curvilinear shape, such as wavy, zigzag, etc., preferably the filaments of the same layer are of the same shape, more preferably the filaments of all layers are of the same shape.
The diameter of the fiber filaments is generally 0.5 to 50. Mu.m, preferably 0.5 to 5. Mu.m, more preferably 0.5 to 1. Mu.m. The lipophilic fiber yarn is generally selected from at least one of polyester fiber yarn, nylon fiber yarn, polyurethane fiber yarn, polypropylene fiber yarn, polyacrylonitrile fiber yarn and polyvinyl chloride fiber yarn, or fiber yarn materials with surfaces subjected to lipophilic treatment; the hydrophilic fiber yarn is generally selected from carboxyl (-COOH), amido (-CONH-) and amino (-NH) in main chain or side chain 2 Polymer with hydrophilic groups such as (-), or hydroxyl (-OH), and the more hydrophilic groups, the better the hydrophilicity, such as polypropylene fiber, polyamide fiber, acrylic fiber, or fiber yarn from materials hydrophilic treated by physical or chemical methods. Selecting lipophilicityAlso hydrophilic filaments, are mainly related to the nature of the dispersed phase. In general, when the disperse phase is lipophilic, lipophilic ultrafine fiber filaments are selected, and when the disperse phase is hydrophilic, hydrophilic ultrafine fiber filaments are selected, so that the disperse phase is favorable for adhesion and spreading of the surface of the ultrafine fiber filaments in the micro-channel and is dispersed into droplets with smaller and uniform size, and the dispersion uniformity of the disperse phase in the continuous phase is improved. When the dispersed phase is a gas phase, either or a combination of both of the lipophilic type and the hydrophilic type may be employed.
The thickness of the sheet is generally 0.05mm to 5mm, preferably 0.1 to 1.5mm. The material of the sheet is generally determined according to the property and operation condition of the overcurrent material, and can be any one or more of metal, ceramic, organic glass or polyester, etc., preferably stainless steel (such as model number of SS30403, SS 30508, SS32168, SS31603, etc.) in metal. The shape of the sheet is not limited, and may be any of rectangle, square, polygon, circle, ellipse, sector, etc., preferably rectangle or square.
In the microchannel assembly of the invention, the size and number of the flakes can be designed and adjusted according to the actual requirements of the reaction. Typically, sheets of the same shape and size are used in microchannel assemblies. The microchannel mixing assembly of the invention may be disposed directly within a reactor for material mixing.
The invention also provides a micro-channel mixing device, which comprises the micro-channel component and a shell, wherein the micro-channel component is fixed in the shell, one end of the shell is provided with an inlet for feeding the disperse phase material and the continuous phase material, and the other end of the shell is provided with an outlet for flowing out the mixed material; the micro-channel assembly 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 inlet of the shell and the feeding end, a discharging distribution space is arranged between the outlet of the shell and the discharging end, and in order to prevent short circuit of materials, the micro-channel assembly is ensured to flow from the feeding end to the discharging end in the micro-channel assembly, and all the other ends of the micro-channel assembly are in sealing connection with the shell except the feeding end and the discharging end.
In the microchannel mixing device, a plurality of microchannel assemblies can be arranged in the shell in series so as to improve the mixing effect.
The microchannel mixing device of the present invention may be used in processes involving and dispersing a dispersed phase into a continuous phase, such as providing feed for mass transfer reactions such as gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid, and the like. 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 producing hydrogen peroxide by an anthraquinone method and the like; absorption reactions of acid gases, e.g. SO 3 Absorbed by sulfuric acid, NO 2 Absorbed by dilute nitric acid, CO 2 、SO 2 、H 2 S and the like are absorbed by alkali liquor; oxidation reactions of organic matters, such as oxidation process in the process of producing hydrogen peroxide by an anthraquinone method, oxidation of chain alkane to acid, oxidation of paraxylene to produce terephthalic acid, oxidation of cyclohexane to produce cyclohexanone, oxidation of acetaldehyde to produce acetic acid, oxidation of ethylene to produce acetaldehyde and the like; chlorination of organic substances, such as benzene chlorination into benzene chloride, toluene chlorination into toluene chloride, dodecane chlorination, ethylene chlorination, etc.; other organic reactions such as hydroxylation of methanol to acetic acid, absorption of isobutylene by sulfuric acid, sulfation of alcohol by sulfur trioxide, polymerization of olefins in organic solvents, hydration of olefins, hydrolysis of oils and fats, and the like.
The micro-channel mixing device can be arranged outside the reactor or can be arranged inside the reactor; as reaction feed, the present microchannel mixing device may be used in part or in whole for mixing.
The invention also provides a micro-channel mixing system, which comprises the micro-channel mixing equipment, primary mixing equipment and a pipeline for communicating the materials mixed by the primary mixing equipment to an inlet of the micro-channel mixing equipment; the primary mixing equipment is used for primarily mixing the disperse phase raw material and the continuous phase raw material to form a mixed fluid; the primary mixing device may employ any one or a combination of conventional devices having a mixing function, such as a static mixer, a colloid mill, a shearing machine, a stirred tank, a ceramic membrane tube, or 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 disperse phase raw material and the continuous phase raw material are mixed through a pipeline, the mixture is introduced into a micro-channel mixing device through an inlet, the disperse phase raw material and the continuous phase raw material flow through micro-channels formed among fiber filaments in a micro-channel assembly, and the mixture is continuously cut for a plurality of times through the fiber filaments to form a mixed fluid containing a large amount of micron-sized particles, and the mixed fluid is discharged from an outlet to serve as reaction feed.
In the process of the present invention, the micro-scale particles in the mixed fluid formed by the micro-channel mixing apparatus generally have a size of 0.5 to 900. Mu.m, preferably 0.5 to 50. Mu.m.
In the method of the invention, preferably, after the dispersed phase raw material and the continuous phase raw material are preliminarily mixed, the mixture is introduced into micro-channel mixing equipment; the primary mixing can be carried out by adopting any one or a combination of a plurality of conventional devices with mixing functions, such as a static mixer, a colloid mill, a shearing machine, a stirring kettle, a ceramic membrane tube and the like, more preferably, the ceramic membrane tube device is generally in a shell-and-tube structure, one or a plurality of membrane tubes are contained in a shell, wherein continuous raw materials are introduced into the tube bundle, disperse phase raw materials are introduced into a cavity outside the tube bundle, and the disperse phase raw materials enter the tube bundle from outside the tube bundle through nano/micron pore channels on the wall of the membrane tube to form nano/micron particles under the pushing of pressure difference or concentration difference and are dispersed into a continuous phase, so that a large number of micron particles are uniformly dispersed in the continuous phase.
In the method of the invention, when the disperse 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 both the dispersed phase and the continuous phase are liquid phases, the mass ratio of the dispersibility to the continuous phase is 1:1000 to 1:1, preferably 1:50 to 1:300; the mixing conditions are generally as follows: normal temperature to 380 ℃ and 0.1 to 20.0MPaG.
In the method, generally, the particle size of the mixed fluid formed by the micro-channel mixing equipment is 0.5-900 mu m, and when the dispersion uniformity is more than or equal to 80%, the mass transfer reaction rate can be greatly improved when 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 be used as the feed of the reaction process as long as the dispersion phase particles are between 0.5 and 900 mu m.
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 disperse phase is easy to be dissociated from a continuous phase, phase separation occurs, and the reaction mass transfer process is influenced. For this purpose, the disperse phase and the continuous phase to be mixed are introduced into a microchannel mixing device according to the invention, and the feed is fed through the microchannels formed between the filaments in the microchannel assembly and is continuously cut a plurality of times through the filaments to form a mixed fluid containing a large amount of micron-sized particles, which is then used as a reaction feed. Because of the special micro-channel structure of the micro-channel device and the surface property of the filled superfine lipophilic or hydrophilic fiber yarn between the adjacent thin sheet seams, the mixed feeding material of the disperse phase and the continuous phase is forcedly cut into a mixed material containing uniform particles with micron size, the mixed material has very stable existence state and very high specific surface area, which is critical to the reaction mass transfer process, and particularly has better reaction promotion effect on the reaction processes of low reaction rate, long required residence time, high material viscosity, no mutual solubility between the two phases and the like. In addition, the lipophilic or hydrophilic property of the superfine fiber yarn filled in the micro-channel device is mainly determined according to the lipophilic or hydrophilic property of the disperse phase, so that the disperse phase characteristic is the same as the surface characteristic of the superfine fiber yarn, the contact and spreading of the disperse phase material on the surface of the fiber yarn are enhanced, the two phases are uniformly mixed, the dispersion uniformity in the continuous phase is improved, and the mixed phase is repeatedly cut by the superfine fiber yarn in the micro-channel for a plurality of times, so that the mixed phase can be dispersed into smaller and more uniform-size particles.
The invention has the following technical effects: (1) The mixed fluid obtained by mixing the disperse phase and the continuous phase by adopting the microchannel mixing component has the characteristics of small particle size, high dispersion uniformity and stable existence state, greatly increases the mass transfer area of the two phases, and eliminates the mass transfer reaction resistance, thereby maintaining higher mass transfer reaction rate, and particularly has great improvement effect on the reaction process with large mass transfer resistance; (2) Because the invention is developed based on the principle of forced repeated cutting of the material by the lipophilic/or hydrophilic fiber yarn in the micro-channel, the invention still has good mixing effect on material systems with high material viscosity, immiscibility between two 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 disperse phase is uniformly dispersed in the continuous phase, and can enable the dispersibility and the continuous phase to form micron-sized particles with the size and the dispersion uniformity, and the size and the dispersion uniformity of the disperse phase are key factors capable of realizing efficient mass transfer reaction, so that the method has promotion effect on various mass transfer reaction processes.
Drawings
FIG. 1 is a schematic diagram of a microchannel mixing device of the present invention.
FIG. 2 is a schematic illustration of a "" half-channel "microchannel of a microchannel mixing assembly.
Wherein 1 is a disperse phase raw material, 2 is a continuous phase raw material, 3 is a micro-channel mixing device inlet, 4 is a micro-channel mixing device outlet, 5 is a micro-channel mixing device, 6 is a micro-channel mixing device shell, 7 is a micro-channel component, 8 is a micro-channel sheet, 9 is a gap between micro-channel sheets, 10 is a fiber yarn, 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 micro-channels ("" type micro-channels) between filaments in the micro-channel sheet slit.
Detailed Description
The invention will now be described in more detail with reference to the accompanying drawings and examples, which are not intended to limit the invention thereto.
Taking fig. 1 as an illustration of the application process of the microchannel mixing device of the invention:
firstly, after the disperse phase raw material 1 and the continuous phase raw material 2 are mixed in a pipeline, the mixture is introduced into a micro-channel mixing device 5 through a micro-channel mixing device inlet 3, the material firstly enters a feeding distribution space 11 of a micro-channel mixing device shell 6, after the material is distributed, the material enters a gap 9 between micro-channel sheets arranged in a micro-channel assembly 7, a plurality of times of continuous cutting is carried out on the material through fiber filaments 10 filled between the gap 9, a mixed fluid containing a large number of micron-sized particles is formed as the feeding of a reactor 13, and the mixed fluid leaves as a reaction product 14 after the mass transfer reaction is completed.
The micro-channel mixing equipment is applied to aviation kerosene liquid phase hydrogenation reaction. Specific reaction conditions, procedures and equipment are shown in comparative example 1, example 1 and example 2. The raw oil is a normal line from an atmospheric and vacuum device of a certain factory, the specific properties are shown in table 1, and the protective agent/catalyst adopted in the hydrogenation reaction is FBN-03B01/FH-40A which is used for smoothing petrochemical institute.
The microchannel mixing device is applied to the selective hydrodeolefination of the reformed oil. Specific reaction conditions, procedures and equipment are shown in comparative example 2, example 3 and example 4. The raw oil 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 which smoothes the petrochemical institute.
TABLE 1 Properties of aviation kerosene feedstock
TABLE 2 reforming of produced oil feedstock Properties
Comparative example 1
In the aviation kerosene liquid phase hydrogenation process, a conventional static mixer is adopted for mixing aviation kerosene raw materials and hydrogen, and the model is SL 2.3/25-6.4-500.
Hydrogen accounts for 0.22% of the mass of the aviation kerosene raw material. Introducing the hydrogen-oil mixture into the aviation kerosene hydrogenation reactor from the top of the reactor, and enabling the hydrogen-oil mixture to undergo hydrogenation reaction in a catalyst bed layer filled in the reactor. The mixing condition of the hydrogen oil is that: the temperature is 55-60 ℃ and the pressure is 4.2MPaG; the aviation kerosene hydrogenation reaction conditions are as follows: the temperature is 280-320 ℃, the pressure is 4.0MPaG, and the airspeed is 4.0h -1 The protective agent/catalyst is FBN-03B01/FH-40A of the smooth petrochemical institute.
Taking aviation kerosene raw materials in table 1 as raw materials, mixing the raw materials with hydrogen, and carrying out hydrogenation reaction to obtain a hydrogenation product. The properties of the hydrogen oil mixture and the properties of the product are shown in Table 3.
Comparative example 2
In the liquid-phase hydrogenation olefin removal process of the reformed oil, the reformed oil and hydrogen are mixed by a conventional static mixer, and the model is SV2.3/25-2.5-500.
Hydrogen represented 0.102% of the mass of the reformate feedstock. Introducing the hydrogen-oil mixture into the inlet of the reactor for hydrogenation and olefin removal of the reformed oil from the bottom of the reactor, and enabling the hydrogen-oil mixture to undergo 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 1.8MPaG; the liquid phase hydrogenation olefin removal reaction conditions of the reforming generated oil are as follows: the temperature is 120-160 ℃, the pressure is 1.7MPaG, and the airspeed is 10.0h -1 The catalyst is FHDO-18 of smooth petrochemical institute.
The reformate raw materials in table 1 are used as reaction raw materials, and hydrogenation reaction is carried out after the reformate raw materials are mixed with hydrogen to obtain hydrogenation products. The properties of the hydrogen oil mixture and the properties of the product are shown in Table 3.
Example 1
The microchannel mixing device shown in figure 1 is adopted, the thin sheets in the microchannel mixing component are made of stainless steel, the thickness of the thin sheets is 1.0mm, 2 layers of nylon fiber filaments with the diameter of 1 mu m are filled between the thin sheet cracks, and the fiber filaments are distributed at equal intervals with the interval of 1 mu m. The fiber yarn is in a curve shape with a wavy line periodically changing.
The dispersed phase material was hydrogen and the continuous phase material was aviation kerosene material shown in Table 1. Hydrogen accounts for 0.22% of the mass of the aviation kerosene raw material. After being mixed by a pipeline, the aviation kerosene raw material and hydrogen are introduced into micro-channel mixing equipment to obtain mixed fluid containing a large amount of micron-sized particles, and the mixed fluid is introduced into an aviation kerosene hydrogenation reactor to carry out hydrogenation reaction. The mixing conditions of the microchannel mixing device are as follows: at a temperature of 55 to ultra-high60 ℃ 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 airspeed is 4.0h -1 。
The micro-channel mixing equipment provided by the invention is used for providing reaction feed for aviation kerosene hydrogenation reaction, and the properties and the product properties of the obtained mixture 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 primary mixing device adopts a static mixer with the model SL 2.3/25-6.4-500. The thin sheet in the micro-channel mixing equipment is made of stainless steel, the thickness of the thin sheet is 1.0mm, 5 layers of polypropylene fiber filaments with the diameter of 1 mu m are filled between the thin sheet cracks, and the fiber filaments are distributed at equal intervals, wherein the interval is 0.5 mu m. The superfine fiber is in a curve shape with the periodic variation of the wavy line.
The dispersed phase material was hydrogen and the continuous phase material was aviation kerosene material shown in Table 1. Hydrogen accounts for 0.21% of the mass of the aviation kerosene raw material. Uniformly mixing the aviation kerosene raw material and hydrogen through a static mixer, then introducing the mixture into the micro-channel mixing equipment to obtain a mixed fluid containing a large amount of micron-sized particles, and introducing the mixed fluid into an aviation kerosene hydrogenation reactor to carry out hydrogenation reaction. The mixing conditions of the primary mixing device and the micro-channel mixing device 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 airspeed is 4.0h -1 。
The micro-channel mixing system provides reaction feed for aviation kerosene hydrogenation reaction, and the properties and product properties of the obtained mixture II are shown in Table 3.
Example 3
The micro-channel mixing equipment shown in the attached figure 1 is adopted, the thin sheet in the micro-channel mixing equipment is made of stainless steel, the thickness of the thin sheet is 1.5mm, 2 layers of polypropylene fiber filaments with the diameter of 1 mu m are filled between the thin sheet cracks, and the superfine fiber filaments are distributed at equal intervals, wherein the interval is 0.5 mu m. The fiber yarn is in a curve shape with a wavy line periodically changing.
The dispersed phase material was hydrogen gas, and the continuous phase material was a reformed oil material shown in table 2. Hydrogen represents 0.014% of the mass of the reformate feedstock.The aviation kerosene raw material and hydrogen are mixed by a pipeline and then introduced into the micro-channel mixing equipment to obtain a mixed fluid containing a large amount of micron-sized particles, and the mixed fluid is introduced into a reforming generated oil hydrodeolefine reactor to carry out hydrodeolefine reaction. The mixing conditions of the microchannel mixing device are as follows: the temperature is 55-60 ℃ and the pressure is 1.65MPaG; the hydrogenation reaction conditions of the reforming generated oil are as follows: the temperature is 130-150 ℃, the pressure is 1.6MPaG, and the airspeed is 10.0h -1 。
The microchannel mixing device provides reaction feed for hydrogenation reaction of reformed oil, and the properties and product properties of the obtained mixture are shown in Table 3.
Example 4
The micro-channel mixing system shown in the attached figure 1 is adopted, and the primary mixing equipment adopts a static mixer, and the model is SX2.3/25-2.5-450. The thin sheet in the micro-channel mixing equipment is made of stainless steel, the thickness of the thin sheet is 1.0mm, 5 layers of polyamide fiber filaments with the diameter of 1 mu m are filled between the thin sheet cracks, and the fiber filaments are distributed at equal intervals with the interval of 1 mu m. The superfine fiber is in a curve shape with the periodic variation of the wavy line.
The dispersed phase material was hydrogen gas, and the continuous phase material was a reformed oil material shown in table 2. Hydrogen represents 0.014% of the mass of the reformate feedstock. Uniformly mixing the aviation kerosene raw material and hydrogen through a static mixer, introducing the mixture into micro-channel equipment to obtain mixed fluid containing a large amount of micron-sized particles, and introducing the mixed fluid into a hydrogenation olefin removal reactor for reforming generated oil to perform hydrogenation olefin removal reaction. The mixing conditions of the primary mixing device and the micro-channel mixing device are as follows: the temperature is 55-60 ℃ and the pressure is 1.45MPaG; the hydrogenation reaction conditions of the reforming generated oil are as follows: the temperature is 130-150 ℃, the pressure is 1.4MPaG, and the airspeed is 12.0h -1 。
The microchannel mixing system provides reaction feed for hydrogenation reaction of reformed oil, and the properties and product properties of the obtained mixture are shown in Table 3.
TABLE 3 reactor feed properties and product properties
In the conventional dispersing and mixing process of the disperse phase and the continuous phase, the aim is to uniformly mix the disperse phase and the continuous phase, disperse the disperse phase into particles with smaller size and more uniform uniformity, obtain the particle size of the disperse phase through a high-speed camera, and obtain the particle uniformity of the disperse phase through selecting a plurality of characteristic particles, wherein the smaller the particle size of the disperse phase and the higher the particle uniformity of the disperse phase are, which indicates that the better the mixing and dispersing effects are. For the convenience of identification and measurement, the disperse phase can be replaced by tracers with different colors. For this reason, the method for measuring the mixing and dispersing effect of the present example and comparative example is as follows: and mixing the disperse phase and the continuous phase under the same condition by different mixing and dispersing methods (such as a conventional static mixer and a microchannel mixer), obtaining at least 10 groups of mixed material samples by each group of methods, shooting the particle size of the disperse phase in the mixed material samples by using a British IX i-SPEED 5 high-SPEED camera, adding the particles of the disperse phase in the photo, calculating the percentage content of the particles with various sizes, and obtaining a normal distribution map of the particles with various sizes, thereby obtaining the particle uniformity.
As can be seen from the mixing effect of the embodiment and the comparative example, the micro-channel mixing device and the mixing system provided by the invention have the advantages that the micro-size particles in the mixed material obtained by the micro-channel mixing device are small in size, high in dispersion uniformity and stable in existence, so that the two-phase mass transfer area can be greatly increased, the mass transfer reaction resistance is eliminated, and the high mass transfer reaction rate is maintained. When the catalyst is used for the hydrogenation reaction of aviation kerosene, compared with the prior aviation kerosene technology, the catalyst can adopt more moderate conditions, such as lower temperature and pressure and higher airspeed, so as to achieve better hydrogenation effect. When the catalyst is used for the liquid-phase hydrogenation olefin removal reaction of the reforming generated oil, the olefin removal effect is obviously improved under mild conditions, and compared with the bromine index at the outlet of the olefin removal reactor, the bromine index is obviously reduced when the catalyst is mixed by adopting conventional mixing equipment, so that the catalyst reaches a very ideal technical index.
Claims (26)
1. A microchannel assembly, characterized in that: comprises a plurality of stacked thin sheets and a plurality of layers of lipophilic and/or hydrophilic fiber filaments filled between the cracks of the adjacent thin sheets, wherein a plurality of micro-channels are formed between the fiber filaments, and the fiber filaments are clamped and fixed through the thin sheets;
in each layer of fiber yarn, the distance between adjacent fiber yarns is 0.5-50 μm; the diameter of the fiber filaments is 0.5-50 mu m;
the number of the fiber yarn layers is 1-50; when the fiber yarns are arranged in multiple layers, the projection of two adjacent layers of fiber yarns along the vertical direction of the thin sheet is a net structure; each layer of fiber filaments 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 yarn is in any curve shape; the thickness of the thin sheet is 0.05 mm-5 mm;
in each layer of fiber filaments, adjacent fiber filaments are distributed at equal intervals; the fiber yarn is in a periodically-changing curve shape; the shape of the filaments of all layers is the same.
2. The microchannel assembly according to claim 1, wherein: the number of the fiber yarn layers is 1-5.
3. The microchannel assembly according to claim 1, wherein: the diameter of the fiber filaments is 0.5-5 mu m.
4. A microchannel assembly according to claim 3, wherein: the diameter of the fiber filaments is 0.5-1 mu m.
5. The microchannel assembly according to claim 1, wherein: the lipophilic fiber yarn is at least one selected from polyester fiber yarn, nylon fiber yarn, polyurethane fiber yarn, polypropylene fiber yarn, polyacrylonitrile fiber yarn, polyvinyl chloride fiber yarn or fiber yarn materials with surfaces subjected to lipophilic treatment.
6. The microchannel assembly according to claim 1, wherein: the hydrophilic fiber yarn is selected from one or more of natural high molecular polymers with hydrophilic groups in main chains or side chains or fiber yarn materials with surfaces subjected to hydrophilic and oleophobic treatment.
7. The microchannel assembly according to claim 1, wherein: the thickness of the thin sheet is 0.1-1.5 mm.
8. The microchannel assembly according to claim 1, wherein: the sheet is made of any one of metal, ceramic or polyester materials.
9. The microchannel assembly according to claim 1, wherein: the shape of the thin sheet is any one of rectangle, circle, ellipse or fan.
10. Use of the microchannel assembly of claim 1 in a gas-liquid, liquid-liquid, gas-liquid-solid and liquid-solid contacting mass transfer reaction process.
11. Use of the microchannel assembly of claim 1 in a reactor, wherein: the microchannel assembly is directly disposed within the reactor for material mixing.
12. A microchannel mixing device, characterized by: the microchannel mixing device comprising the microchannel assembly of claim 1 or 2 and a housing.
13. The microchannel mixing device of claim 12, wherein: the micro-channel component is fixed in the shell, one end of the shell is provided with an inlet for feeding the disperse phase material and the continuous phase material, and the other end of the shell is provided with an outlet for flowing out the mixed material; the micro-channel assembly 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 inlet of the shell and the feeding end, a discharging distribution space is arranged between the outlet of the shell and the discharging end, and in order to prevent short circuit of materials, the micro-channel assembly is ensured to flow from the feeding end to the discharging end in the micro-channel assembly, and all the other ends of the micro-channel assembly are in sealing connection with the shell except the feeding end and the discharging end.
14. The microchannel mixing device of claim 12, wherein: a plurality of micro-channel components connected in series are arranged in the shell.
15. Use of a microchannel mixing device according to claim 12 in a gas-liquid, liquid-liquid, gas-liquid-solid, liquid-solid mass transfer reaction process.
16. Use of a microchannel mixing device according to claim 12 in hydrogenation of hydrocarbon oil feedstock, hydrogenation of olefins, hydrogenation of fatty acid esters, hydrogenation of ketones, hydrogenation of hydrogen peroxide produced by the anthraquinone process, absorption of acid gases, oxidation of paraffins to acids, oxidation of para-xylene to terephthalic acid, oxidation of cyclohexane to cyclohexanone, oxidation of acetaldehyde to acetic acid, oxidation of ethylene to acetaldehyde, chlorination of benzene to chlorobenzene, chlorination of toluene to toluene, chlorination of dodecane, chlorination of ethylene, 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 or hydrolysis of oils and fats.
17. The use according to claim 16, characterized in that: the micro-channel mixing device is arranged outside the reactor or inside the reactor.
18. A method of using the microchannel mixing device of claim 12, comprising: after the disperse phase raw material and the continuous phase raw material are mixed through a pipeline, the mixture is introduced into a micro-channel mixing device through an inlet, the disperse phase raw material and the continuous phase raw material flow through micro-channels formed among fiber filaments in a micro-channel assembly, and the mixture is continuously cut for a plurality of times through the fiber filaments to form a mixed fluid containing a large amount of micron-sized particles, and the mixed fluid is discharged from an outlet to serve as reaction feed.
19. The application method according to claim 18, wherein: the micro-scale particle size in the mixed fluid formed by the micro-channel mixing device is 0.5-900 mu m.
20. The application method according to claim 19, wherein: the micro-scale particle size in the mixed fluid formed by the micro-channel mixing device is 0.5-50 mu m.
21. The application method according to claim 18, wherein: after preliminary mixing of the disperse phase raw material and the continuous phase raw material, introducing the mixture into micro-channel mixing equipment; the primary mixing adopts any one or a combination of a plurality of static mixers, colloid mills, shearing machines, stirring kettles or ceramic membrane tubes.
22. The application method according to claim 19, wherein: the ceramic membrane tube equipment is a shell-and-tube structure, one or more bundles of membrane tubes are contained in the shell, wherein continuous raw materials are introduced into the tube bundle, disperse phase raw materials are introduced into a cavity outside the tube bundle, and the disperse phase raw materials enter the tube bundle from outside the tube bundle through nano/micro pore channels on the wall of the membrane tubes to form nano/micro particles under the pushing of pressure difference or concentration difference and are dispersed into the continuous phase, so that a large number of micro particles are uniformly dispersed in the continuous phase.
23. The application method according to claim 18, wherein: when the disperse phase is a gas phase and the continuous phase is a liquid phase, the gas phase accounts for 0.001-30% of the mass fraction of the liquid phase; when the disperse phase and the continuous phase are both liquid phases, the mass ratio of the dispersibility to the continuous phase is 1:1000-1:1.
24. A microchannel mixing system, characterized by: the microchannel mixing system comprising a microchannel mixing device according to any one of claims 12 to 14, a primary mixing device, and a line for communicating the material mixed by the primary mixing device to the inlet of the microchannel mixing device.
25. The microchannel mixing system of claim 24, wherein: the primary mixing equipment is used for primarily mixing the disperse phase raw material and the continuous phase raw material to form a mixed fluid; the primary mixing equipment is any one or a combination of a plurality of static mixers, colloid mills, shears, stirred tanks or ceramic membrane tubes.
26. The microchannel mixing system of claim 24, wherein: one or more micro-channel mixing devices are arranged, and the micro-channel mixing devices are connected in series or in parallel.
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