WO2023273645A1 - 微反应器 - Google Patents

微反应器 Download PDF

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Publication number
WO2023273645A1
WO2023273645A1 PCT/CN2022/092970 CN2022092970W WO2023273645A1 WO 2023273645 A1 WO2023273645 A1 WO 2023273645A1 CN 2022092970 W CN2022092970 W CN 2022092970W WO 2023273645 A1 WO2023273645 A1 WO 2023273645A1
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WIPO (PCT)
Prior art keywords
channel
mixing
microreactor
microreactor according
section
Prior art date
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Ceased
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PCT/CN2022/092970
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English (en)
French (fr)
Inventor
冯俊杰
孙冰
杨哲
朱红伟
徐伟
赵辰阳
刘聿嘉
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China Petroleum and Chemical Corp
Sinopec Research Institute of Safety Engineering Co Ltd
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China Petroleum and Chemical Corp
Sinopec Research Institute of Safety Engineering Co Ltd
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Application filed by China Petroleum and Chemical Corp, Sinopec Research Institute of Safety Engineering Co Ltd filed Critical China Petroleum and Chemical Corp
Priority to US18/575,912 priority Critical patent/US20240335812A1/en
Priority to EP22831472.0A priority patent/EP4364838B1/en
Publication of WO2023273645A1 publication Critical patent/WO2023273645A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/006—Baffles
    • 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
    • B01J2219/00002—Chemical plants
    • B01J2219/00004—Scale aspects
    • B01J2219/00011—Laboratory-scale plants
    • B01J2219/00013—Miniplants
    • 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
    • B01J2219/00761—Details of the reactor
    • B01J2219/00763—Baffles
    • B01J2219/00765—Baffles attached to the reactor wall
    • 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
    • B01J2219/0081—Plurality of modules
    • B01J2219/00813—Fluidic connections
    • 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
    • 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
    • B01J2219/0095—Control aspects
    • B01J2219/00952—Sensing operations
    • B01J2219/00954—Measured properties
    • B01J2219/00959—Flow
    • 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
    • B01J2219/0095—Control aspects
    • B01J2219/00984—Residence time

Definitions

  • the invention relates to the technical field of microchemical industry, in particular to a microreactor.
  • a microreactor is a micro-device made of a solid substrate with the help of special micro-processing technology that can be used for chemical reactions or material mixing.
  • the "micro" of the microreactor means that the channel of the process fluid is generally at the micron level, and there are currently plans to reach the millimeter level.
  • the microreactor has the characteristics of small volume, large specific surface area, high reaction efficiency, and precise control. In terms of application, it has broad application prospects and is expected to become an efficient and safe revolutionary technology in the chemical industry.
  • the microreactor Due to the characteristics of small scale, mostly in laminar flow state and significant interfacial interaction, the flow and transfer characteristics of microreactors are very different from those of conventional reactors, and the design concept is also different.
  • the microreactor mainly adopts the static mixing method, that is, it does not rely on external forces such as ultrasound, electric field, and magnetic field, and only uses the channel structure design and the control of fluid flow properties to complete the mixing of reactants. It has the characteristics of stability, simplicity, and wide application range.
  • FIG. 1 shows another conventional microreactor 200 .
  • the microreactor comprises a plurality of mixing units connected in succession.
  • the outer profile 201 of each mixing unit has an arcuate profile only at the upstream end, and this arcuate profile does not extend to the side.
  • the sides of the outer contour 201 are formed by fold lines at both ends.
  • An inlet and an outlet are respectively formed at opposite ends of the outer contour 201 .
  • the outlet 202 of a single mixing unit is a straight channel with constant section.
  • a zigzag-shaped first blocking portion 203 and a circular second blocking portion 204 are also provided in a single mixing unit.
  • the second blocking portion 204 is closer to the outlet of the mixing unit than the first blocking portion 203 .
  • the zigzag side profile of the outer profile 201 makes the energy loss of the fluid larger and the pressure drop increased. In addition, this will also increase the ineffective mixing area on the rear side of the first blocking part, and the impact effect of the two fluids will be deteriorated, resulting in poor mixing efficiency.
  • the structure of the outlet 202 of the mixing unit will cause the fluid to have a certain tendency of "backtracking" after hitting the first barrier 203 . This is bad for mixing efficiency and increases pressure drop.
  • FIG. 1 For the microreactor in Fig. 1, experiments were carried out under liquid-liquid mixing conditions. Water and isooctyl alcohol are delivered from the inlet at a speed of 0.3m/s.
  • Figure 2 and Figure 3 show the mixing and pressure conditions of the microreactor in Figure 1, respectively. It can be seen from Figure 2 that the microreactor requires fluids to pass through at least 8 mixing units to achieve effective mixing between fluids. Effective mixing here is defined as the concentration difference between the left and right sides of the chamber in the mixing unit is less than 0.5%. It can be seen from Figure 3 that the pressure drop when the fluid passes through 8 mixing units in the microreactor to effective mixing is about 8680 Pa.
  • Fig. 1 An experiment on the efficiency of carbon dioxide absorption by alkanolamine was carried out for the microreactor in Fig. 1 .
  • the experimental process is to use alcohol amines to absorb carbon dioxide at low temperature, and then heat to release the carbon dioxide from the chemical solvent.
  • the mixed gas of carbon dioxide with a volume fraction of 12% and the diethanolamine solution with a concentration of 30wt.% enter the microreactor through two branches under the condition of 8MPa, wherein the gas feed is 5-10Nm 3 /h, The liquid phase feed is 50-80L/h.
  • the results show that the highest carbon dioxide absorption rate does not exceed 92%.
  • the present invention proposes a microreactor that enhances the mixing process, which can be used to avoid or at least reduce at least one of the above problems.
  • a microreactor which includes a plurality of mixing units connected in sequence along the longitudinal direction, each mixing unit includes an outer casing, and a flow chamber is formed in the outer casing, and the opposite two sides of each mixing unit along the longitudinal direction The ends respectively form an inlet part and an outlet part, and the inlet part and the outlet part are connected to the flow chamber; the mixing unit also includes a first barrier part arranged in the flow chamber, so that the flow chamber forms The first forward passage is defined by the first side profile of the outer shell and the first blocking portion, and the second side profile of the outer shell opposite to the first side profile and the first blocking portion The defined second advancing channel, and a mixing area between the first blocking portion and the outlet portion, both the first advancing channel and the second advancing channel communicate with the mixing area; wherein , at the downstream ends of the first advance channel and the second advance channel, the microreactor is further provided with protrudingly extending but spaced from the first side profile and the second side profile relative to each other There is an open
  • the arrangement of the auxiliary guide part can make the fluids in the first forward channel and the second forward channel impact each other more violently; on the other hand, it can greatly reduce the low flow rate part in the mixing area and reduce the ineffective mixing area.
  • the mixing efficiency of the microreactor can be effectively improved.
  • the surface of the auxiliary air guiding part facing the first advancing channel or the second advancing channel is configured as a plane or an arc surface.
  • the extension lines of the ends of the pair of auxiliary deflectors facing the surface of the first advancing channel or the second advancing channel can intersect in the mixing area.
  • the auxiliary guide part is configured such that the included angle between the main movement directions of the fluid in the first forward channel and the second forward channel exceeds 90°.
  • the cross-sections of the first advancing channel and the second advancing channel are kept constant.
  • the lateral dimension of the auxiliary air guide part does not exceed the lateral dimension of the first blocking part.
  • the auxiliary air guiding part is configured symmetrically.
  • the distance between the auxiliary guide part and the first blocking part in the longitudinal direction is 1/6 to 1/2, preferably 1/4 to 1/2 of the longitudinal dimension of the entire flow chamber. 1/3.
  • first side profile and the second side profile are arranged opposite to each other in an axisymmetric manner, and respectively include an arc-shaped upstream section and a linear downstream section, and the upstream section and the downstream section segments are connected smoothly.
  • the first blocking portion includes a straight middle section extending transversely and straight edge sections connected to both ends of the middle section, and the edge sections are oriented toward An upstream bevel forms an angle between the edge section and the middle section.
  • the linear downstream sections of the first side profile and the second side profile are inclined in such a way that they are relatively close to the downstream; the linear downstream sections are arranged parallel to the edge section , so that the cross-section of the channel between the downstream section and the edge section remains constant.
  • the upstream end of said edge segment is aligned with the upstream end of said rectilinear downstream segment.
  • the longitudinal length of the first barrier part accounts for 1/4 to 1/2 of the longitudinal length of the flow cavity.
  • the inlet and outlet of each mixing unit are connected to the flow cavity and communicate with the flow cavity of the adjacent mixing unit; wherein, the middle section of the first barrier Directly opposite to the entrance portion, the transverse dimension of the middle section is no more than three times the maximum cross-sectional dimension of the entrance portion.
  • the angle between the opposite edge segments is not less than 50°.
  • the first blocking portion is centrally arranged in the flow chamber in a transverse direction perpendicular to the longitudinal direction, and includes a transversely extending linear middle section and a rectilinear edge sections at both ends, the edge sections are inclined upstream relative to the middle section to form a knuckle between the edge sections and the middle section; wherein the middle section includes a plurality of part of the fluid can flow to the mixing area through the gap between the blocking elements, and collide with the fluid flowing into the mixing area through the first advancing channel and the second advancing channel.
  • an expansion channel gradually expanding longitudinally toward the downstream is formed between the outlet portion of one mixing unit and the inlet portion of the next mixing unit.
  • the expansion slope of the expansion channel of the inlet portion is constant.
  • the smallest cross-sectional dimension of the expansion channel is no less than 1/4 of the largest cross-sectional dimension of the expansion channel.
  • the maximum cross-sectional dimension of the expansion channel is between 100 micrometers and 2 centimeters.
  • the ratio of the maximum cross-sectional dimension of the expansion channel to the maximum transverse dimension of the flow chamber is between 1/10 and 1/2.
  • Fig. 1 has shown the schematic structural diagram of a kind of existing microreactor
  • Fig. 2 has shown the microreactor in Fig. 1 when the mixing efficiency schematic diagram of liquid-liquid mixing
  • Fig. 3 has shown the microreactor in Fig. 1 the pressure drop schematic diagram when liquid-liquid mixing
  • Figure 4 shows a schematic structural diagram of a microreactor according to an embodiment of the present invention
  • Figure 5 shows a partial enlarged view of the microreactor in Figure 4.
  • Fig. 6 has shown the microreactor in Fig. 4 when liquid-liquid mixing liquid flow path schematic diagram
  • Fig. 7 has shown the microreactor in Fig. 4 when the mixing efficiency schematic diagram of liquid-liquid mixing
  • Fig. 8 shows the schematic diagram of the pressure drop of the microreactor in Fig. 4 when liquid-liquid mixing
  • Fig. 9 has shown the microreactor in Fig. 4 when the liquid flow path schematic diagram when gas-liquid mixing
  • Fig. 10 shows the liquid flow path schematic diagram of the microreactor in Fig. 4 when nitrification reaction
  • Fig. 11 has shown the schematic structural diagram of the microreactor according to another embodiment of the present invention.
  • Fig. 12 shows a schematic structure diagram of a microreactor according to another embodiment of the present invention.
  • longitudinal refers to the direction in which the fluid generally flows, that is, the length direction of the entire microreactor, for example, in FIG. 5, it should be understood as the direction extending up and down in the paper.
  • horizontal refers to the direction perpendicular to the "longitudinal”, that is, the width direction of the entire microreactor, for example, in FIG. 5, it should be understood as the left-right extension direction in the paper.
  • lateral dimension and “longitudinal dimension” refer to the projected dimensions of the relevant portion in the transverse direction and in the longitudinal direction, respectively.
  • upstream refers to the side to which the fluid is supplied
  • downstream conversely refers to the side to which the fluid flows.
  • FIG. 4 shows one embodiment of a microreactor 300 of the present invention.
  • the microreactor 300 comprises a plurality of mixing units 310 connected one after the other along the longitudinal direction. An embodiment of eleven mixing units 310 is shown in FIG. 4 . However, it should be understood that more or fewer mixing units 310 may be provided as desired.
  • the microreactor 300 also comprises a fluid inlet channel 302 connected upstream of a first mixing unit of successively connected mixing units.
  • the fluid inlet channel 302 communicates with the first inlet branch 301 and the second inlet branch 304 respectively.
  • the fluid can enter the fluid inlet channel 302 through the first inlet branch 301 and the second inlet branch 304 , and thus enter the mixing unit 310 to achieve mixing.
  • the fluid here can be gas, fluid, or any other suitable fluid medium.
  • the microreactor 300 also includes a fluid output channel that is connected downstream of the last mixing unit in the sequentially connected mixing units, and is used to deliver the mixed (even reacted) fluid in the microreactor 300 for further processing. processing or use, etc.
  • FIG. 5 shows a partially enlarged view of the microreactor 300 in FIG. 4 .
  • the mixing unit 310 is formed as a planar mixing unit including an outer case 350 in a flat form.
  • the outer housing 350 is configured axisymmetrically along the longitudinal axis and thus comprises two oppositely arranged side profiles, namely a first side profile 352 and a second side profile 354 .
  • Each side profile includes a circular arc-shaped upstream section 312 and a rectilinear downstream section 313 .
  • the linear downstream section 313 is smoothly connected with the arc-shaped upstream section 312 .
  • the two oppositely arranged upstream sections 312 may be configured to be relatively inclined in a downstream direction, thereby enabling the outer shell to form a substantially inverted heart-shaped shape.
  • a flow chamber 330 is enclosed within the housing.
  • an inlet portion 320 and an outlet portion 322 are provided at opposite longitudinal ends of the outer casing, respectively. Both the inlet portion 320 and the outlet portion 322 communicate with the flow chamber 330 .
  • an expansion passage 314 gradually expanding longitudinally toward the downstream is formed between the outlet portion 322 of one mixing unit and the inlet portion 320 of the next mixing unit.
  • the profile of the expansion channel 314 is a linear profile.
  • the fluid can diverge into the flow chamber through the expansion channel 314 . It is easy to understand that the smallest cross-sectional size of the expansion channel 314 is the size of the inlet portion 320 , and the largest cross-sectional size is the size of the outlet portion 322 .
  • the expansion channel 314 may be formed as a constriction 315 connecting between the flow chambers of the previous mixing unit and the flow chambers of the following mixing unit.
  • each mixing unit 310 forms a shape similar to a "spade" as a whole.
  • the mixing unit 310 further includes a first barrier 311 disposed in the flow chamber.
  • first blocking portion 311 can be formed by a solid stopper, or can also be formed by a through hollow of the outer casing as shown in FIG. 4 , as long as it can prevent fluid from flowing therethrough.
  • the expansion channel 314 is configured to expand gradually toward the downstream in the longitudinal direction, so that the fluid can impact the first blocking portion 311 at a high speed. In this way, a flow state with high turbulence and high speed difference can be formed, and the mixing between fluids is promoted. At the same time, the expansion channel 314 can also facilitate lateral movement of fluid, thereby reducing longitudinal "backflow" that would increase pressure drop.
  • the first barrier 311 includes a central section 311B laterally and centrally disposed within the flow chamber.
  • the middle section 311B extends transversely to face the entrance portion 320 and is in a straight line structure.
  • the first blocking portion 311 also includes linear edge sections 311A and 311C connected to both ends of the middle section 311B.
  • the free ends of edge segments 311A and 311C are each sloped more upstream relative to central segment 311B such that a knuckle is formed between edge segments 311A and 311C and central segment 311B.
  • the angle between the two edge segments 311A and 311C is not less than 50°.
  • a linear downstream segment 313 may be arranged parallel to the above-mentioned edge segments 311A and 311C to form an advancing channel of constant cross-section therebetween.
  • the constant cross-section of the advancing channel means that the cross-section of the advancing channel along the direction perpendicular to the advancing direction of the fluid has a constant size.
  • the forward channels are symmetrically arranged, wherein a first forward channel 317 is defined between the first side profile 352 and the first blocking portion 311, a second forward channel 318 is defined between the second side profile 354 and the first Between the blocking parts 311. Additionally, edge segments 311A and 311C are aligned at the upstream ends with corresponding downstream segments 313 . The distance between the edge segments 311A and 311C and the arc-shaped upstream end 312 of the outer casing also keeps the cross-section of the counterflow channel formed therebetween relatively constant. This keeps the fluid relatively concentrated when flowing through the reverse flow channel and the forward channel, thereby providing a better basis for downstream fluid mixing, making the impact of fluid mixing stronger, and improving the mixing efficiency between fluids. In addition, relatively many counterflow channels are designed, which makes it difficult to form a "dead zone" here, or the area of the formed "dead zone” is relatively small.
  • the transverse dimension of the above-mentioned middle section 311B is not more than 3 times, preferably not more than 2 times, the maximum cross-sectional dimension of the above-mentioned expansion channel 314 .
  • edge segments 311A and 311C taper toward the free end.
  • the width of edge segments 311A and 311C remains constant.
  • the overall longitudinal length of the first blocking portion 311 accounts for 1/4 to 1/2 of the longitudinal length of the entire flow cavity, preferably accounts for 1/3 to 1/2 of the longitudinal length of the entire flow cavity. Between the downstream of the first blocking portion 311 and the outlet portion, the so-called “second blocking portion” disposed directly downstream of the first blocking portion 311 in the existing solution may no longer be provided.
  • a mixing region 319 is formed in the entire region between the downstream of the first blocking portion 311 and the upstream of the constriction 315 of the outlet portion. Since the first blocking portion 311 occupies a large longitudinal length of the entire flow chamber, the downstream section 313 and the first blocking portion 311 have a stronger guiding effect on the fluid, and there are fewer "dead zones" in the flow chamber (especially the mixing area) . This can increase the liquid holdup and throughput of the microreactor 300 .
  • the microreactor is also provided with The profile 354 (the downstream section thereof) protrudes relative to each other extending but spaced apart auxiliary flow guides 316 .
  • the auxiliary flow guide 316 is configured to encourage the fluids in the first forward passage 317 and the second forward passage 318 to flow into the mixing region 319 opposite to each other and to strengthen the impingement on each other.
  • the fluid in the first advancing channel 317 and the second advancing channel 318 can change the flow direction through the action of the auxiliary flow guiding part 316, and make the included angle between their main moving directions exceed 90°.
  • auxiliary flow guide part 316 is also beneficial to make the residence time of different fluids that need to be mixed and reacted in the mixing area 319 closer.
  • the increase of the mixing area and the closeness of the mixing time are conducive to improving the uniformity and controllability of the reaction process.
  • this helps to improve the mixing efficiency.
  • this also makes the chemical reaction process more stable and controllable, with fewer by-products.
  • FIG. 4 and FIG. 5 only show the case where each mixing unit 310 is provided with a pair of auxiliary air guides 316 , it should be understood that more pairs of auxiliary air guides 316 may be provided as required.
  • the surface of the auxiliary guide part 316 facing the first advancing channel 317 and the second advancing channel 318 can be configured as a plane or an arc, so as to change the direction of the fluid as required.
  • the extension lines of the ends of the pair of auxiliary flow guides 316 respectively facing the surfaces of the first advancing channel 317 or the second advancing channel 318 can intersect in the mixing area. This is beneficial to strengthen the impact of fluid.
  • the lateral dimension of a single auxiliary air guiding portion 316 does not exceed the lateral dimension of the first blocking portion 311 .
  • the total lateral dimension of the pair of auxiliary air guides 316 does not exceed the lateral dimension of the first blocking portion 311 . This is beneficial to improve the utilization rate of the mixing area 319 downstream of the first barrier 311 , and reduce the "dead zone" without increasing the pressure drop, thereby improving the mixing efficiency.
  • the auxiliary air guide 316 is configured symmetrically. However, it should be understood that, according to specific application requirements, the auxiliary air guiding portion 316 may also be configured asymmetrically.
  • the distance between the auxiliary guide part 316 and the first blocking part 311 in the longitudinal direction is 1/6 to 1/2, more preferably 1/4 to 1/3 of the longitudinal dimension of the entire flow chamber .
  • the two streams of fluid collide closer to the first blocking portion 311 under the action of the auxiliary flow guiding portion 316 , which is beneficial to reduce the area of the low flow velocity region in the mixing unit 310 and improve mixing efficiency.
  • the overall lateral dimension of the mixing unit 310 may be between 100 microns and 5 cm, and the overall thickness may be between 100 microns and 2 cm.
  • the cross-sectional dimension of the fluid inlet channel 304 and the largest cross-sectional dimension of each expansion channel 314 may be between 100 microns and 2 centimeters, preferably between 100 microns and 1 centimeter.
  • the smallest cross-sectional dimension of the expansion channel 314 is not less than 1/4 of the size of the fluid inlet channel 304 .
  • the ratio of the maximum cross-sectional dimension of the expansion channel 314 to the maximum transverse dimension of the flow chamber is between 1/10 and 1/2.
  • the above size design is conducive to the adjustment of the relative balance between improving the mixing efficiency and reducing the pressure drop. With the above design, the transfer area (specific surface area) of the microprocessor 300 can reach up to about 60000m 2 /m 3 .
  • the above microreactor 300 can be used not only as a reactor but also as a mixer, and can also be combined with a heat exchange unit, a collection unit or other reaction/mixing units to realize a complete set of functions. It should be understood that, in addition to the above-mentioned microreactor 300, in order to realize the mixing and reaction of fluids, other devices or devices such as pumps, pipelines, flow meters, valves, and control systems may also be provided.
  • the microreactor 300 can be used for single-phase systems, gas-liquid systems, liquid-liquid systems, etc., and can also be used for solid-containing multi-phase systems with low solid holdup and small size.
  • the chemical reactions applicable to the microreactor 300 of the present invention include oxidation, peroxidation, reduction, addition, replacement, substitution, polymerization, nitration, epoxidation, alkylation, hydrogenation, dehydrogenation, organometallic reactions, Carbonylation, alkoxylation, halogenation, dehalogenation, carboxylation, arylation, coupling, condensation, dehydration, alcoholysis, hydrolysis, ammonolysis, etherification, ketonization, saponification, isomerization, diazotization , Azolation, and enzyme-catalyzed reactions.
  • the fluid when the fluid enters the flow chamber 330 through the outlet portion 322 of the previous mixing unit, the expansion channel 314, and the inlet portion 320 of the latter mixing unit, the fluid can be impacted at a high speed.
  • the first blocking portion 311 Since the first blocking portion 311 is zigzag and the flow of the fluid is dispersed, the fluid can quickly change its direction laterally and flow to the above-mentioned reverse flow channel. In the region upstream of the first blocking portion 311 , a flow state with high turbulence and high speed difference can be formed, thereby promoting the mixing between fluids. At the same time, the fluid will not "return the same way", or most of the fluid will not “return the same way”. This avoids "back mixing” and keeps the residence time of the fluid relatively constant, resulting in a more controllable flow of the fluid, helping to precisely control and enhance the mixing and reaction process.
  • the fluid when the fluid bypasses the edge sections 311A and 311C of the first blocking portion 311 in the counterflow channel, the fluid generally moves along an arc-shaped trajectory, and can aggravate local disturbances at the edge sections 311A and 311C to further enhance the mixing effect .
  • the two streams pass through the straight forward passage, and after leaving the forward passage, relatively enter into the mixing area 319 , and thus violently impact and mix together under the action of the auxiliary flow guiding part 316 .
  • the mixed fluid can leave the mixing unit through the constriction 315 and enter the next mixing unit through the expansion channel at the inlet of the latter mixing unit for further mixing.
  • This structure increases local flow velocity, shear rate, and turbulence while reducing mass transfer distance, further enhancing mixing and/or reaction processes.
  • the mixing units 310 must be exactly the same, for example, the first barrier part 311 and/or the auxiliary flow guiding part 316 may have different structures and/or sizes.
  • the microreactor can also be used together with other tubular or tank reactors.
  • microreactor 300 of the present invention The beneficial effects of the microreactor 300 of the present invention will be further demonstrated through multiple embodiments below.
  • the mixing efficiency of the microreactor 300 of the present invention was tested using a system containing fluorescent dyes. Mixing efficiency can be measured by measuring and calculating the mixing factor at the outlet.
  • the specific calculation formula is:
  • ⁇ represents the mixing factor
  • SD AIOD is the relative standard deviation of the target outlet concentration
  • SD AIOD is the relative standard deviation of the concentration before mixing. The closer the mixing factor ⁇ is to 0, the worse the mixing effect is, and the closer to 1, the better the mixing effect.
  • the safranin aqueous solution and water are respectively passed into the microreactor 300 of the present invention through the first entering branch 301 and the second entering branch 302, and the flow rate of entering the first entering branch 301 and the second entering branch 302 is 20L/ min. It has been determined that the mixing factor ⁇ measured at the outlet is 0.9 (the mixing factor of the existing microreactor 200 in FIG. 1 is about 0.6), and the pressure drop is about 0.1 MPa. This shows that the microreactor 300 of the present invention can achieve better fluid mixing without causing excessive pressure drop.
  • a liquid-liquid mixing efficiency experiment was carried out for the microreactor 300 .
  • the microreactor 300 as a whole is shown in FIG. 4 , and the stainless steel base plate is machined to form a microchannel with a depth of about 500 microns.
  • Water and isooctyl alcohol were introduced into the first inlet branch 301 and the second inlet branch 302 respectively, and a precision syringe pump was used to realize the feeding, and the inlet flow rate was controlled to be about 0.3m/s.
  • the cross-sectional dimension of the fluid entry channel 304 is 550 microns.
  • the mixing unit 310 has a maximum lateral dimension of about 3.5mm and a longitudinal dimension (excluding the inlet and outlet) of about 2.5mm.
  • the inlet portion 320 is facing the first blocking portion 311 in the flow cavity 330 .
  • the middle section 311B of the first blocking portion 311 has a longitudinal dimension of about 200 microns and a transverse dimension of about 1 mm.
  • the lengths of the edge segments 311A and 311B of the first barrier portion 311 are both about 800 microns, and the width is reduced from 200 microns to 100 microns.
  • the distance of the reverse flow of the upstream end 312 of the arcuate shape of the outer shell and the reverse flow channel formed by the edge segments 311A and 311B is 150 microns (compared with the reverse flow distance of the prior art center, which is obviously smaller to reduce the ineffective mixing area ).
  • a pair of auxiliary deflectors 316 are provided, and a single auxiliary deflector 316 has a lateral dimension of 450 microns and a longitudinal dimension of 200 microns.
  • the minimum cross-sectional dimension of the expansion channel 314 is 200 microns.
  • microreactor 300 is used to carry out the liquid-liquid mixing experiment, and the experimental conditions are the same as those for the existing microreactor shown in FIGS. 1 to 3 .
  • Figures 6 to 8 show the corresponding experimental results.
  • the velocity vector distribution of the liquid-liquid mixing process in the microreactor 300 is gradually symmetrical and uniform, and before the strong impact mixing in the mixing chamber, the parallelism and consistency of the fluid flow vector arrows are relatively high.
  • the velocity vector distribution is highly controllable. This facilitates accurate anticipation and control of mixing effects.
  • microreactor 300 can realize effective mixing after fluid passes through 4 mixing units.
  • Figure 8 shows that the pressure drop for fluid passing through 4 mixing units to effective mixing is about 8520 Pa.
  • the microreactor 300 of the present invention can achieve effective mixing of fluids with fewer mixing units 310 . That is to say, compared with the existing microreactor 200 of Fig. 1, the microreactor 300 of the present invention can greatly improve the mixing efficiency under the situation of maintaining low pressure drop and large flux, shorten the mixing time, and thus reduce the The number of mixing units required allows the microreactor to have a smaller volume.
  • the mixed reaction of methyl chloride and salicylic acid was carried out using the same microreactor 300 as in Example 2.
  • the experiment was carried out under the conditions of 22MPa and 350K by adding 25% salicylic acid to methyl chloride.
  • the results show that the required reaction time is about 230s, and the yield reaches 99%, which is 1% higher than the traditional method that needs 10h reaction time.
  • the micro-reactor 300 clearly shows the advantages of simple operation, low cost and greatly reduced space required during the experiment.
  • a gas-liquid mixing efficiency experiment was carried out for the microreactor 300 .
  • the overall microreactor 300 is shown in FIG. 4 , and the overall thickness (depth) is about 500 microns.
  • the largest transverse dimension (width) of the flow chamber is about 4mm, and the longitudinal dimension (excluding the inlet and outlet) is about 3mm.
  • the inlet portion 320 is facing the first blocking portion 311 in the flow cavity 330 .
  • the middle section 311B of the first blocking portion 311 has a longitudinal dimension of about 250 microns and a transverse dimension of about 1.2 mm.
  • the lengths of the edge segments 311A and 311B of the first blocking portion 311 are both about 1 mm, and the width is reduced from 250 ⁇ m to 150 ⁇ m.
  • the distance of the reverse flow of the upstream end 312 of the arcuate shape of the outer casing and the reverse flow channel formed by the edge segments 311A and 311B is 200 microns (compared with the reverse flow distance of the prior art center, which is obviously smaller to reduce the ineffective mixing area ).
  • a pair of auxiliary deflectors 316 are provided, and a single auxiliary deflector 316 has a lateral dimension of 450 microns and a longitudinal dimension of 200 microns.
  • the minimum cross-sectional dimension of the expansion channel 314 is 250 microns.
  • the above-mentioned microreactor 300 was used to carry out the gas-liquid mixing experiment.
  • the first inlet branch 301 and the second inlet branch 302 transport deionized water and air respectively, the operating temperature is 298K, the viscosity is 8.9 ⁇ 10 -4 Pa ⁇ s, the surface tension coefficient is 0.07N ⁇ m -1 , and the average inlet flow rate is is 0.3m/s.
  • the results show that for gas-liquid mixing, the microreactor 300 can achieve effective mixing after the fluid passes through 4 mixing units, and the pressure drop when the fluid passes through 4 mixing units to effective mixing is about 2.5 kPa.
  • the auxiliary flow guide part 316 can effectively change the flow direction of the fluid, adjust the impact angle, and effectively improve the mixing efficiency.
  • the microreactor 300 can greatly improve the mixing efficiency while maintaining a low pressure drop and a large flux, and the mixing time and the number of mixing units required , the overall volume and other aspects have advantages.
  • a nitrification reaction efficiency experiment was carried out for the microreactor 300 of the present invention.
  • the reactor is made of stainless steel, and the outer layer is equipped with a heat exchanger to realize the closed circulation flow of the heat transfer fluid, so as to realize the integration of mixing and heat transfer.
  • the existing general process for preparing isooctyl nitrate is to add isooctyl alcohol dropwise to the prepared mixed acid of sulfuric acid and nitric acid to carry out nitration reaction, and then undergo pickling, alkali washing and water washing to refine to obtain the finished product. Since the reaction is a strong exothermic reaction, in order to avoid the risk of thermal runaway, the feed rate of the traditional tank reactor is very slow, and the reaction process takes more than 1 hour.
  • the microreactor 300 is used to carry out the reaction to prepare isooctyl nitrate. It can not only strengthen the mixing and reaction rate, but also significantly increase the heat transfer rate and improve process safety.
  • Fig. 10 shows the flow path of the liquid in the experiment, which shows that the microreactor 300 can make the distribution of the liquid phase in the experiment process uniform and controllable, and the transfer efficiency is high.
  • the microreactor 300 can not only shorten the reaction residence time, but also realize efficient and directional conversion of reactants by controlling the reaction conditions. For example, in the reaction process where dinitrochlorobenzene is the target object, dinitrogen products account for more than 99% of the product.
  • the experimental process is to use alcohol amines to absorb carbon dioxide at low temperature, and then heat to release the carbon dioxide from the chemical solvent. Specifically, make the volume fraction be 12% carbon dioxide mixed gas and the diethanolamine solution of 30wt.% concentration under the condition of 8MPa respectively enter microreactor 300 through first entering branch 301 and second entering branch 302, wherein gas The feed is 5-10Nm 3 /h, and the liquid phase feed is 50-80L/h.
  • the microreactor 300 has the advantages of fast absorption speed, high absorption capacity, and high purity of recovered carbon dioxide.
  • FIG. 11 shows the structure of a microreactor 400 according to one embodiment of the present invention.
  • the structure of the microreactor 400 is similar to that of the microreactor 300 , the main difference is that the inlet of the microreactor 400 is configured as a channel 414 with a constant cross-sectional size.
  • the size of this channel 414 is the same as the smallest cross-sectional dimension of the constriction of the outlet portion.
  • FIG. 12 shows the structure of a microreactor 500 according to one embodiment of the present invention.
  • the structure of the microreactor 500 is similar to that of the microreactor 400, the difference mainly lies in the structure of the first barrier part 511.
  • the first barrier 511 includes a central section 511B laterally and centrally disposed within the flow chamber.
  • the middle section 511B extends transversely to face the entrance, and has a linear structure.
  • the middle section 511B in turn includes a plurality of blocking elements 5111 spaced apart from each other. The spacing between the barrier elements allows a portion of the fluid to pass directly to the mixing zone.
  • the fluid flowing directly to the mixing area can collide with the fluid flowing into the mixing area through the first advancing channel and the second advancing channel, so as to facilitate mixing.
  • the blocking element 5111 can be configured to be inclined.
  • the first blocking portion 311 further includes linear edge segments 511A and 511C disposed at both ends of the middle segment 511B.
  • the free ends of the edge sections 511A and 511C are both inclined more upstream relative to the middle section 311B as a whole, and may be more inclined relative to each blocking unit 5111 . This is conducive to the formation of a certain degree of turbulent flow here, which is beneficial to improve the mixing efficiency of the fluid.

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Abstract

一种微反应器（300），包括多个沿纵向依次连接的混合单元（310）。各个混合单元（310）包括外壳体（350），在外壳体（350）内形成流动腔（330）。各个混合单元（310）沿纵向方向的相反两端分别形成入口部（320）和出口部（322），入口部（320）和出口部（322）均连通到流动腔（330）。混合单元（310）还包括设置在流动腔（330）内的第一阻挡部（311），其在垂直于纵向的横向方向上居中地布置在流动腔（330）内，并处于入口部（320）和出口部（322）之间，以使流动腔（330）形成第一前进通道（317）、第二前进通道（318）和混合区域（319）。第一前进通道（317）和第二前进通道（318）与混合区域（319）相连通。在第一前进通道（317）和第二前进通道（318）的下游末端处，微反应器（300）还设置有从第一侧部轮廓（352）和第二侧部轮廓（354）相对于彼此凸出延伸但间隔开的辅助导流部（316）。

Description

微反应器
相关申请的交叉引用
本申请要求享有于2021年7月2日提交的题为“微反应器”的中国专利申请CN202110751886.3的优先权，该申请的全部内容通过引用结合于本文中。
技术领域
本发明涉及微化工技术领域，特别是涉及一种微反应器。
背景技术
微反应器是一种借助于特殊微加工技术、以固体基质制造的可用于进行化学反应或物质混合的微型装置。微反应器的“微”表示工艺流体的通道一般在微米级别，目前也有达到毫米级别的方案。
微反应器具有体积小、比表面积大、反应效率高、控制精确等特点，对于包含剧烈放热反应、有中间物或产物不稳定的反应、配比要求严格的快速反应、高温高压等条件的应用来说有着广阔的应用前景，有望成为化工产业高效、安全的革命性技术。
由于微反应器的尺度小、多处于层流状态以及界面作用显著等特点，其流动与传递特性与常规反应器差别很大，设计理念也有所区别。目前，微反应器主要采用静态混合方式，即不依靠超声、电场、磁场等外界动力，仅利用通道结构设计及流体流动性质的控制完成反应物混合，具有稳定、简便、适用范围广等特点。
图1显示了另一种现有的微反应器200。该微反应器包括多个依次连接的混合单元。各个混合单元的外轮廓201仅在上游末端具有弧形轮廓，且该弧形轮廓并未延伸向侧部。外轮廓201的侧部由两端折线形成。在外轮廓201的相反两端分别形成入口和出口。单个混合单元的出口202为截面恒定的直通道。另外，在单个混合单元内还设置有折线形的第一阻挡部203和圆形的第二阻挡部204。该第二阻挡部204相对于第一阻挡部203更加靠近混合单元的出口。由此，流体在经前一混合单元的出口202进入到后续紧邻的混合单元内时，会冲击在第一阻挡 部203上，再流向两侧分流，最后流向该混合单元的出口。
在该微反应器中，外轮廓201的折线形的侧部轮廓使得流体的能量损失较大，压降增加。另外，这还会导致第一阻挡部后侧的无效混合区域增加，两股流体的撞击效果变差，导致混合效率较差。
另外，对于上述微反应器来说，混合单元的出口202的结构会导致流体在冲击第一阻挡部203之后具有一定的“原路返回”的趋势。这对于混合效率来说是不利的，并且会增大压降。
针对图1中的微反应器在液液混合条件下进行实验。从入口处以0.3m/s的速度输送水和异辛醇。图2和图3分别显示了图1中的微反应器的混合情况和压力情况。从图2中可以看出，该微反应器需流体经过至少8个混合单元才能实现流体间的有效混合。这里的有效混合定义为混合单元内的腔体左右两侧的浓度差小于0.5％。从图3中可以看出，流体在微反应器内经过8个混合单元至有效混合时的压降约为8680帕。
类似地，针对图1中的微反应器在气液混合条件下进行实验。从入口处以0.3m/s的速度输送水和空气。实验结果为，该微反应器需流体经过至少6个混合单元才能实现流体间的有效混合，并且压降约为2.3千帕。
另外，针对图1中的微反应器进行醇胺吸收二氧化碳的效率的实验。实验过程为，在低温条件利用醇胺吸收二氧化碳，然后加热使二氧化碳从化学溶剂中释放出来。具体来说，使体积分数为12％的二氧化碳混合气体与30wt.％浓度的二乙醇胺溶液在8MPa条件下分别通过两个支路进入微反应器，其中气体进料为5-10Nm 3/h，液相进料为50-80L/h。结果表明，二氧化碳吸收率最高不超过92％。
发明内容
本发明提出了一种强化混合过程的微反应器，能用于避免或至少削弱以上问题中的至少一个。
根据本发明提出了一种微反应器，包括多个沿纵向方向依次连接的混合单元，各个混合单元均包括外壳体，在所述外壳体内形成流动腔，各个混合单元的沿纵向方向的相反两端分别形成入口部和出口部，所述入口部和出口部均连通到所述流动腔；所述混合单元还包括设置在所述流动腔内的第一阻挡部，以使所述流动腔形成由外壳体的第一侧部轮廓和所述第一阻挡部所限定的第一前进通道， 由外壳体的与所述第一侧部轮廓相对的第二侧部轮廓和所述第一阻挡部所限定的第二前进通道，以及位于所述第一阻挡部与所述出口部之间的混合区域，所述第一前进通道和所述第二前进通道均与所述混合区域相连通；其中，在所述第一前进通道和所述第二前进通道的下游末端处，所述微反应器还设置有从所述第一侧部轮廓和第二侧部轮廓相对于彼此凸出延伸但间隔开的辅助导流部，所述辅助导流部构造为促使所述第一前进通道和第二前进通道内的流体彼此相对地流入所述混合区域并彼此冲击。
通过辅助导流部的设置一方面能使第一前进通道和第二前进通道内的流体更加剧烈地彼此冲击；另一方面能大幅减少混合区域中的低流速部分，减少无效混合区。由此，可以有效地提高微反应器的混合效率。
在一个优选的实施例中，所述辅助导流部的朝向所述第一前进通道或第二前进通道的表面构造为平面或弧面。
在一个优选的实施例中，一对辅助导流部的朝向所述第一前进通道或第二前进通道的表面的末端的延长线能相交于所述混合区域内。
在一个优选的实施例中，所述辅助导流部构造为使得所述第一前进通道和第二前进通道内的流体的主运动方向之间的夹角超过90°。所述第一前进通道和第二前进通道的截面均保持恒定。
在一个优选的实施例中，所述辅助导流部的横向尺寸不超过所述第一阻挡部的横向尺寸。
在一个优选的实施例中，所述辅助导流部构造为对称的。
在一个优选的实施例中，所述辅助导流部与所述第一阻挡部在纵向方向上的距离为整个流动腔的纵向尺寸的1/6至1/2，优选地为1/4至1/3。
在一个优选的实施例中，所述第一侧部轮廓和第二侧部轮廓呈轴对称式相对设置，并分别包括圆弧形的上游段以及直线型的下游段，所述上游段和下游段平滑连接。
在一个优选的实施例中，所述第一阻挡部包括横向地延伸的直线型的中部段以及连接在所述中部段两端的直线型的边缘段，所述边缘段相对于所述中部段朝向上游倾斜，以在所述边缘段与所述中部段之间形成折角。
在一个优选的实施例中，所述第一侧部轮廓和第二侧部轮廓的直线型的下游段沿朝向下游相对靠近的方式倾斜；所述直线型的下游段与所述边缘段平行布 置，以使所述下游段与所述边缘段之间的通道的截面保持恒定。
在一个优选的实施例中，所述边缘段的上游端与所述直线型的下游段的上游端对齐。
在一个优选的实施例中，所述第一阻挡部的纵向长度占所述流动腔的纵向长度的1/4至1/2。
在一个优选的实施例中，各所述混合单元的入口部和出口部均连通到所述流动腔并与相邻的混合单元的流动腔相连通；其中，所述第一阻挡部的中部段与所述入口部正对，所述中部段的横向尺寸不超过所述入口部的最大截面尺寸的3倍。
在一个优选的实施例中，相对的边缘段之间的夹角不小于50°。
在一个优选的实施例中，所述第一阻挡部在垂直于纵向的横向方向上居中地布置在所述流动腔内，并包括横向地延伸的直线型的中部段以及设置在所述中部段两端的直线型的边缘段，所述边缘段相对于所述中部段朝向上游倾斜，以在所述边缘段与所述中部段之间形成折角；其中，所述中部段包括多个彼此间隔开的阻挡元件，部分流体能通过所述阻挡元件之间的间隔流向所述混合区域，与经第一前进通道和第二前进通道流入所述混合区域中的流体彼此冲击。
在一个优选的实施例中，在一个混合单元的出口部和下一个混合单元的入口部之间形成了一个沿纵向朝向下游逐渐扩张的扩张通道。
在一个优选的实施例中，所述入口部的扩张通道的扩张斜率为恒定的。
在一个优选的实施例中，所述扩张通道的最小截面尺寸不低于所述扩张通道的最大截面尺寸的1/4。
在一个优选的实施例中，所述扩张通道的最大截面尺寸在100微米至2厘米之间。
在一个优选的实施例中，所述扩张通道的最大截面尺寸与所述流动腔的最大横向尺寸之比在1/10至1/2之间。
附图说明
在下文中参考附图来对本发明进行更详细的描述。其中：
图1显示了一种现有的微反应器的示意性结构图；
图2显示了图1中的微反应器在液液混合时的混合效率示意图；
图3显示了图1中的微反应器在液液混合时的压降示意图；
图4显示了根据本发明的一个实施方案的微反应器的示意性结构图；
图5显示了图4中的微反应器的局部放大图；
图6显示了图4中的微反应器在液液混合时的液体流动路径示意图；
图7显示了图4中的微反应器在液液混合时的混合效率示意图；
图8显示了图4中的微反应器在液液混合时的压降示意图；
图9显示了图4中的微反应器在气液混合时的液体流动路径示意图；
图10显示了图4中的微反应器在硝化反应时的液体流动路径示意图；
图11显示了根据本发明的另一个实施方案的微反应器的示意性结构图；
图12显示了根据本发明的另一个实施方案的微反应器的示意性结构图。
在附图中，相同的部件使用相同的附图标记。附图并未按照实际的比例绘制。
具体实施方式
下面将结合附图对本发明作进一步说明。
在本发明中，“纵向”指的是流体大体上流动的方向，即整个微反应器的长度方向，例如在图5中应理解为纸面内的上下延伸方向。相应地，“横向”指的是垂直于该“纵向”的方向，即整个微反应器的宽度方向，例如在图5中应理解为纸面内的左右延伸方向。用语“横向尺寸”和“纵向尺寸”分别指相关部分在横向方向上和纵向方向上的投影尺寸。
在本发明中，“上游”指的是提供流体的一侧，而“下游”与之相反地指的是流体流向的一侧。
图4显示了本发明的微反应器300的一个实施方案。该微反应器300包括多个沿纵向方向依次连接的混合单元310。在图4中显示了11个混合单元310的实施方案。然而，应当理解的是，根据需要也可设置更多或更少个混合单元310。该微反应器300还包括连接在依次连接的混合单元中第一个混合单元的上游处的流体进入通道302。该流体进入通道302与第一进入支路301和第二进入支路304分别连通。流体可经第一进入支路301和第二进入支路304进入到流体进入通道302内，并由此进入到混合单元310中实现混合。这里的流体可以是气体、流体，或任何其他适当的流动性介质。微反应器300还包括连接在依次连接的混合单元中最后一个混合单元的下游出的流体输出通道，用于将在微反应器300中混合(甚至反应)后的流体输送出去，以便于进行进一步的处理或使用等。
图5显示了图4中的微反应器300的局部放大图。如图5所示，混合单元310形成为平面式混合单元，包括扁平形式的外壳体350。该外壳体350构造为沿纵向轴线轴对称式布置，并由此包括相对设置的两个侧部轮廓，即第一侧部轮廓352和第二侧部轮廓354。各个侧部轮廓均包括圆弧形的上游段312和直线型的下游段313。直线型的下游段313与圆弧形的上游段312平滑连接。两个相对布置的上游段312可构造为在朝向下游的方向上相对倾斜，从而使得外壳体能形成大体上呈倒心型的形状。在外壳体内包围形成流动腔330。
如图5所示，在外壳体的纵向相反两端处分别设置有入口部320和出口部322。入口部320和出口部322均与流动腔330相连通。根据本发明，在一个混合单元的出口部322和下一个混合单元的入口部320之间形成了一个沿纵向朝向下游逐渐扩张的扩张通道314。该扩张通道314的轮廓为直线型轮廓。由此，流体可以经扩张通道314以发散的形式进入到流动腔内。容易理解，扩张通道314的最小截面尺寸为入口部320的尺寸，而最大截面尺寸为出口部322的尺寸。扩张通道314可形成为连接在前一混合单元的流动腔与后一混合单元的流动腔之间的缩颈315。由此，使得各个混合单元310整体形成类似“黑桃”的形状。
如图4和5所示，混合单元310还包括设置在流动腔内的第一阻挡部311。应当理解的是，第一阻挡部311可由实心的挡块形成，也可如图4所示由外壳体的贯通镂空形成，只要其能阻碍流体由此流过即可。
根据本发明，扩张通道314设置成沿纵向朝向下游逐渐扩张，从而能够使流体高速地冲击第一阻挡部311。这样便可形成高湍动、高速差的流动状态，促进了流体之间的混合。同时，扩张通道314还能够促进流体向两侧运动，从而减少会导致压降增加的纵向“回流”。
第一阻挡部311包括在流动腔内横向居中地布置的中部段311B。中部段311B横向地延伸而与入口部320正对，并呈直线型结构。第一阻挡部311还包括连接在中部段311B的两端的直线型的边缘段311A和311C。边缘段311A和311C的自由端均相对于中部段311B更加朝向上游倾斜，使得在边缘段311A和311C与中部段311B之间形成折角。优选地，两个边缘段311A和311C之间的夹角不小于50°。
另外，还如图5所示，直线型的下游段313可与上述边缘段311A和311C平行布置，以在它们之间形成截面恒定的前进通道。前进通道的截面恒定是指前进 通道在沿着与流体前进方向垂直的方向上的截面具有恒定的尺寸。通过设置截面恒定的前进通道，能够增加流体的整体可控性，同时也可以提高后续导流后的撞击效果。
根据本发明，前进通道是对称布置的，其中第一前进通道317限定在第一侧部轮廓352与第一阻挡部311之间，第二前进通道318限定在第二侧部轮廓354与第一阻挡部311之间。另外，边缘段311A和311C与相应的下游段313在上游端处对齐。边缘段311A和311C与外壳体的圆弧形的上游端312之间的距离也使得它们之间形成的逆流通道的截面保持相对恒定。这使得流体流过逆流通道和前进通道时能保持相对集中，从而能为下游的流体混合提供较好的基础，使流体混合时的冲击更加强烈，进而提高流体之间的混合效率。另外，逆流通道设计得相对较多，这使得不容易在此处形成“死区”，或所形成的“死区”的面积相对较小。
上述中部段311B的横向尺寸不超过上述扩张通道314的最大截面尺寸的3倍，优选地不超过2倍。在一个实施例中，边缘段311A和311C沿朝向自由端的方向逐渐变窄。在另一个实施例中，边缘段311A和311C的宽度保持恒定。该第一阻挡部311整体的纵向长度占整个流动腔的纵向长度的1/4至1/2，优选地占整个流动腔的纵向长度的1/3至1/2。在该第一阻挡部311的下游至出口部之间可以不再设置现有方案中的设置在第一阻挡部311的正对下游处的所谓“第二阻挡部”。也就是说，在第一阻挡部311的下游、出口部的缩颈315的上游之间的整个区域内形成混合区域319。由于第一阻挡部311占整个流动腔的纵向长度较大，因此下游段313与第一阻挡部311对流体的引导作用更强，流动腔(尤其是混合区域)内的“死区”更少。这能够提高微反应器300的持液量和通量。
另外，在上述在第一前进通道317和所述第二前进通道318的下游末端处，所述微反应器还设置有从所述第一侧部轮廓352(其下游段)和第二侧部轮廓354(其下游段)相对于彼此凸出延伸但间隔开的辅助导流部316。辅助导流部316构造为促使第一前进通道317和第二前进通道318内的流体彼此相对地流入混合区域319并强化彼此冲击。在这里优选的是，第一前进通道317和第二前进通道318内的流体能经辅助导流部316的作用而改变流动方向，并使得它们的主运动方向之间的夹角超过90°。这有利于加剧流体之间的冲击和混合，并能有效地减小上述混合区域319中的“死区”，或者说“低流速部分”。另外，通过辅助导 流部316的设置还有利于使需要混合、反应的不同流体在混合区域319中停留的时间更加接近。对于需要进行反应的过程来说，混合区域增加和混合时间的接近有利于提高反应过程的均匀性和可控性。一方面这有利于提高混合效率。另一方面，这还能使化学反应过程更加稳定可控，并使副产物减少。
尽管图4和图5仅显示了每个混合单元310设置一对辅助导流部316的情况，然而应当理解的是，根据需要也可设置更多对的辅助导流部。辅助导流部316的朝向第一前进通道317和第二前进通道318的表面可以构造为平面的或弧形的，以根据需要来改变流体的方向。优选地，一对辅助导流部316的分别朝向第一前进通道317或第二前进通道318的表面的末端的延长线能相交于混合区域内。这有利于加强流体的冲撞。
单个辅助导流部316的横向尺寸不超过第一阻挡部311的横向尺寸。优选地，一对辅助导流部316的总的横向尺寸不超过第一阻挡部311的横向尺寸。这有利于提高第一阻挡部311下游的混合区域319的利用率，在不增加压降的同时减小“死区”，从而有利于提高混合效率。
在图4和图5所示的实施例中，辅助导流部316构造为对称的。然而应当理解的是，根据具体应用的需要，辅助导流部316也可构造为非对称的。
优选地，所述辅助导流部316与所述第一阻挡部311在纵向方向上的距离为整个流动腔的纵向尺寸的1/6至1/2，更优选为1/4至1/3。由此，两股流体在辅助导流部316的作用下在更加接近第一阻挡部311的位置完成撞击，这有利于减少混合单元310中的低流速区域的面积，提高混合效率。
在本发明中，混合单元310的整体横向尺寸可以在100微米至5厘米之间，整体厚度可以在100微米至2厘米之间。流体进入通道304的截面尺寸以及各个扩张通道314的最大截面尺寸可以在100微米至2厘米之间，优选地在100微米至1厘米之间。扩张通道314的最小截面尺寸不小于流体进入通道304的尺寸的1/4。扩张通道314的最大截面尺寸与流动腔的最大横向尺寸之比在1/10至1/2之间。上述尺寸设计有利于在提高混合效率与降低压降之间实现相对平衡的调节。经上述设计，微处理器300的传递面积(比表面积)最高可达到约60000m 2/m 3。
上述微反应器300既可用作为反应器，也可用作为混合器，同时还可与换热单元、收集单元或其他反应/混合单元等相结合以实现成套功能。应当理解的是，除上述微反应器300之外，为了实现流体的混合与反应，还可以设置另外的泵、 管路、流量计、阀门、控制系统等器件或设备。该微反应器300对于单相体系、气液体系和液液体系等均可使用，并且对于低固含率及故乡尺寸较小的含固多相体系也可使用。另外，本发明的微反应器300适用的化学反应包括氧化，过氧化，还原，加成，置换，取代，聚合，硝化，环氧化，烷基化，加氢，脱氢，有机金属反应，羰基化，烷氧基化，卤化，脱卤化，羧化，芳基化，偶联，缩合，脱水，醇解，水解，氨解，醚化，酮化，皂化，异构化，重氮化，偶氮化，以及酶催化反应等。
对于本发明的微反应器300来说，当流体经前一混合单元的出口部322、扩张通道314、后一混合单元的入口部320而再进入到流动腔330内时，可使流体高速冲击第一阻挡部311。由于第一阻挡部311是折线型的，并且流体的流动形式是分散的，所以流体能横向地迅速改变方向而流向上述逆流通道。第一阻挡部311上游的区域内，可以形成高湍动、高速差的流动状态，从而促进了流体之间的混合。同时，流体也不会“原路返回”，或者说绝大部分流体不会“原路返回”。这能避免“返混”，并能使流体的停留时间保持相对恒定，由此导致流体的流动过程更加可控，有助于精确地控制和强化混合和反应进程。
另外，在流体于逆流通道中绕过第一阻挡部311的边缘段311A和311C时，流体大体上沿弧形的轨迹运动，并能在边缘段311A和311C处加剧局部扰动而进一步增强混合效果。随后，两股流体经直线型的前进通道，在离开前进通道之后，相对进入到混合区域319内，并由此在辅助导流部316的作用下剧烈地冲击、混合到一起。混合后的流体可经缩颈315离开该混合单元并经后一混合单元的入口部的扩张通道再进入下一个混合单元进行进一步的混合。这种结构提高了局部流速、剪切速率及湍动程度，同时缩小了传质距离，进一步强化了混合和/或反应过程。
应当理解的是，在一个微反应器300中，所有的混合单元310不都必须完全相同，例如其中的第一阻挡部311和/或辅助导流部316可具有不同的结构和/或尺寸。另外，该微反应器也可与其他管式或釜式的反应器共同使用。
下面将通过多个实施例来对本发明的微反应器300的有益效果进行进一步体现。
实施例1
采用含有荧光染料的体系对本发明的微反应器300的混合效率进行实验。通 过测定并计算出口的混合因子，可以衡量混合效率。具体的计算公式为：
Figure PCTCN2022092970-appb-000001
其中，ψ表示混合因子，SD AIOD为目标物出口浓度的相对标准差，SD AIOD，0为混合之前的浓度相对标准差。该混合因子ψ越接近0代表混合效果越差，越接近1代表混合效果越好。
将番红水溶液和水分别通过第一进入支路301和第二进入支路302通入本发明的微反应器300，进入第一进入支路301和第二进入支路302流速均为20L/min。经测定，出口测定的混合因子ψ为0.9(图1的现有微反应器200的混合因子约为0.6)，压降约为0.1MPa。这表明本发明的微反应器300能够实现较好的流体混合，且不会造成过大的压降。
实施例2
针对微反应器300进行了液液混合效率实验。微反应器300整体如图4所示，由不锈钢基面板通过精雕机加工形成微通道，深度约为500微米。分别向第一进入支路301和第二进入支路302内通入水和异辛醇，采用精密注射泵实现进料，将进入流速控制为约0.3m/s。流体进入通道304的截面尺寸为550微米。混合单元310的最大横向尺寸约为3.5毫米，纵向尺寸(不包含入口部和出口部)约为2.5毫米。入口部320正对流动腔330内的第一阻挡部311。第一阻挡部311的中部段311B的纵向尺寸约为200微米，横向尺寸约为1毫米。第一阻挡部311的边缘段311A和311B的长度均约为800微米，宽度由200微米减缩至100微米。外壳体的圆弧形的上游端312与边缘段311A和311B所形成的逆流通道的逆向流动的距离为150微米(与现有技术中心的逆向流动距离相比明显更小，以减少无效混合区域)。设置了一对辅助导流件316，单个辅助导流件316的横向尺寸为450微米，纵向尺寸为200微米。扩张通道314的最小截面尺寸为200微米。
采用上述微反应器300进行液液混合实验，其实验条件与针对图1至3所示的现有微反应器的实验条件相同。图6至8显示了相应的实验结果。如图6所示，微反应器300的液液混合过程的速度矢量分布逐渐对称且均匀，并且在混合腔的强烈冲击混合之前，流体流动的矢量箭头的平行度、一致度较高。这说明在微反应器300的混合单元310中，速度矢量分布是高度可控的。这有利于对混合效果进行准确预期和控制。如图7所示，微反应器300可使流体经4个混合单元后就 实现有效混合。图8显示了流体经过4个混合单元至有效混合的压降约为8520帕。
经实验可以证明，本发明的微反应器300采用更少的混合单元310即可实现流体的有效混合。也就是说，与图1的现有微反应器200相比，本发明的微反应器300能在保持低压降、大通量的情况下大幅提高混合效率，缩短混合时间，并由此能减少所需的混合单元的数量，使微反应器可具有更小的体积。
实施例3
采用与实施例2相同的微反应器300进行氯甲烷和水杨酸的混合反应。实验由氯甲烷加25％水杨酸在22MPa、350K的条件下进行。结果表明，所需的反应时间约为230s，收率达99％，相比于需要10h反应时间的传统方法提高了1％的收率。并且，微反应器300在实验过程中明显表现出了操作简单、成本低及所需空间大幅缩小等优势。
实施例4
针对微反应器300进行了气液混合效率实验。微反应器300整体如图4所示，整体厚度(深度)约为500微米。流动腔的最大横向尺寸(宽度)约为4毫米，纵向尺寸(不包含入口部和出口部)约为3毫米。入口部320正对流动腔330内的第一阻挡部311。第一阻挡部311的中部段311B的纵向尺寸约为250微米，横向尺寸约为1.2毫米。第一阻挡部311的边缘段311A和311B的长度均约为1毫米，宽度由250微米减缩至150微米。外壳体的圆弧形的上游端312与边缘段311A和311B所形成的逆流通道的逆向流动的距离为200微米(与现有技术中心的逆向流动距离相比明显更小，以减少无效混合区域)。设置了一对辅助导流件316，单个辅助导流件316的横向尺寸为450微米，纵向尺寸为200微米。扩张通道314的最小截面尺寸为250微米。
采用上述微反应器300进行气液混合实验。第一进入支路301和第二进入支路302分别输送去离子水和空气，操作温度为298K，粘度为8.9×10 -4Pa·s，表面张力系数0.07N·m -1，进入流速均为0.3m/s。结果表明，对于气液混合来说，微反应器300可使流体经4个混合单元后就实现有效混合，且流体经过4个混合单元至有效混合时的压降约为2.5千帕。如图9所示，辅助导流部316可有效改变流体的朱运动方向，调整冲击角度，能够有效提高混合效率。
与图1中的现有微反应器的气液混合实验结果相比，微反应器300能在保持 低压降、大通量的情况下大幅提高混合效率，在混合时间和所需的混合单元数量、整体体积等方面均具有优势。
实施例5
针对本发明的微反应器300进行硝化反应效率实验。反应器由不锈钢制成，外层设置换热器来实现热传导液的闭路循环流动，以实现混合和传热的集成。
现有一般的制备硝酸异辛酯工艺是向配制好的硫酸、硝酸混和酸中滴加异辛醇进行硝化反应，再经酸洗、碱洗和水洗精制得到成品。由于该反应是强放热反应，为避免热失控风险，传统釜式反应器进料速度非常缓慢，反应过程需要1小时以上。
采用微反应器300进行反应来制备硝酸异辛酯。不仅可以强化混合及反应速率，还能显著提高移热速率，提高工艺安全性。图10对实验中的液体流动路径进行了显示，其表明了微反应器300能使实验过程中的液相分布均匀可控，且传递效率高。这导致微反应器300不仅能缩短反应停留时间，还能通过控制反应条件来实现反应物的高效定向转化。例如，在二硝基氯苯为目标物的反应过程可以实现产物中二硝产物占比超过99％。
实施例6
针对微反应器300进行醇胺吸收二氧化碳的效率的实验。微反应器300的结构与实施例4中的相同。
实验过程为，在低温条件利用醇胺吸收二氧化碳，然后加热使二氧化碳从化学溶剂中释放出来。具体来说，使体积分数为12％的二氧化碳混合气体与30wt.％浓度的二乙醇胺溶液在8MPa条件下分别通过第一进入支路301和第二进入支路302进入微反应器300，其中气体进料为5-10Nm 3/h，液相进料为50-80L/h。
结果表明，在高液气比条件下，二氧化碳吸收率超过95％，具有显著的吸收效果。相应地，微反应器300具有吸收速度快、吸收能力高、回收二氧化碳纯度高等优点。
图11显示了根据本发明的一个实施方案的微反应器400的结构。微反应器400与微反应器300的结构类似，其区别主要在于微反应器400中的入口部构造为截面尺寸恒定的通道414。该通道414的尺寸与出口部的缩颈的最小截面尺寸相同。
图12显示了根据本发明的一个实施方案的微反应器500的结构。微反应器 500与微反应器400的结构类似，其区别主要在于第一阻挡部511的结构。
第一阻挡部511包括在流动腔内横向居中地布置的中部段511B。中部段511B横向地延伸而与入口部正对，并呈直线型结构。中部段511B又包括多个彼此间隔开的阻挡元件5111。阻挡元件之间的间隔可供一部分流体直接通过并流向混合区域。直接流向混合区域的流体可与经第一前进通道和第二前进通道流入混合区域中的流体彼此冲击，以利于混合。阻挡元件5111可构造为倾斜的。
第一阻挡部311还包括设置在中部段511B两端的直线型的边缘段511A和511C。边缘段511A和511C的自由端均相对于中部段311B整体更加朝向上游倾斜，并且可以相对于各个阻挡单元5111更加倾斜。这有利于在此处形成一定程度的湍流，以利于提高流体的混合效率。
虽然已经参考优选实施例对本发明进行了描述，但在不脱离本发明的范围的情况下，可以对其进行各种改进并且可以用等效物替换其中的部件。尤其是，只要不存在结构冲突，各个实施例中所提到的各项技术特征均可以任意方式组合起来。本发明并不局限于文中公开的特定实施例，而是包括落入权利要求的范围内的所有技术方案。

Claims (20)

  1. 一种微反应器，包括多个沿纵向方向依次连接的混合单元，各个混合单元均包括外壳体，在所述外壳体内形成流动腔，各个混合单元的沿纵向方向的相反两端分别形成入口部和出口部，所述入口部和出口部均连通到所述流动腔；
    所述混合单元还包括设置在所述流动腔内的第一阻挡部，以使所述流动腔形成由外壳体的第一侧部轮廓和所述第一阻挡部所限定的第一前进通道，由外壳体的与所述第一侧部轮廓相对的第二侧部轮廓和所述第一阻挡部所限定的第二前进通道，以及位于所述第一阻挡部与所述出口部之间的混合区域，所述第一前进通道和所述第二前进通道均与所述混合区域相连通；
    其中，在所述第一前进通道和所述第二前进通道的下游末端处，所述微反应器还设置有从所述第一侧部轮廓和第二侧部轮廓相对于彼此凸出延伸但间隔开的辅助导流部，所述辅助导流部构造为促使所述第一前进通道和第二前进通道内的流体彼此相对地流入所述混合区域并彼此冲击。
  2. 根据权利要求1所述的微反应器，其特征在于，所述辅助导流部的朝向所述第一前进通道或第二前进通道的表面构造为平面或弧面。
  3. 根据权利要求1所述的微反应器，其特征在于，一对辅助导流部的朝向所述第一前进通道或第二前进通道的表面的末端的延长线能相交于所述混合区域内。
  4. 根据权利要求1到3中任一项所述的微反应器，其特征在于，所述辅助导流部构造为使得所述第一前进通道和第二前进通道内的流体的主运动方向之间的夹角超过90°，和/或
    所述第一前进通道和第二前进通道的截面均保持恒定。
  5. 根据权利要求1到3中任一项所述的微反应器，其特征在于，所述辅助导流部的横向尺寸不超过所述第一阻挡部的横向尺寸。
  6. 根据权利要求1到3中任一项所述的微反应器，其特征在于，所述辅助导流部构造为对称的。
  7. 根据权利要求1到3中任一项所述的微反应器，其特征在于，所述辅助导流部与所述第一阻挡部在纵向方向上的距离为整个流动腔的纵向尺寸的1/6至1/2。
  8. 根据权利要求1到3中任一项所述的微反应器，其特征在于，所述第一侧部轮廓和第二侧部轮廓呈轴对称式相对设置，并分别包括圆弧形的上游段以及直线型的下游段，所述上游段和下游段平滑连接。
  9. 根据权利要求8所述的微反应器，其特征在于，所述第一阻挡部在垂直于纵向的横向方向上居中地布置在所述流动腔内，并包括横向地延伸的直线型的中部段以及连接在所述中部段两端的直线型的边缘段，所述边缘段相对于所述中部段朝向上游倾斜，以在所述边缘段与所述中部段之间形成折角。
  10. 根据权利要求9所述的微反应器，其特征在于，所述第一侧部轮廓和第二侧部轮廓的直线型的下游段沿朝向下游相对靠近的方式倾斜；
    所述直线型的下游段与所述边缘段平行布置，以使所述下游段与所述边缘段之间的通道的截面保持恒定。
  11. 根据权利要求9所述的微反应器，其特征在于，所述边缘段的上游端与所述直线型的下游段的上游端对齐。
  12. 根据权利要求1到3中任一项所述的微反应器，其特征在于，所述第一阻挡部的纵向长度占所述流动腔的纵向长度的1/4至1/2。
  13. 根据权利要求9所述的微反应器，其特征在于，各所述混合单元的入口部和出口部均与相邻的混合单元的流动腔相连通；
    其中，所述第一阻挡部的中部段与所述入口部正对，所述中部段的横向尺寸不超过所述入口部的最大截面尺寸的3倍。
  14. 根据权利要求9所述的微反应器，其特征在于，相对的边缘段之间的夹角不小于50°。
  15. 根据权利要求8所述的微反应器，其特征在于，所述第一阻挡部在垂直于纵向的横向方向上居中地布置在所述流动腔内，并包括横向地延伸的直线型的中部段以及设置在所述中部段两端的直线型的边缘段，所述边缘段相对于所述中部段朝向上游倾斜，以在所述边缘段与所述中部段之间形成折角；
    其中，所述中部段包括多个彼此间隔开的阻挡元件，部分流体能通过所述阻挡元件之间的间隔流向所述混合区域，与经第一前进通道和第二前进通道流入所述混合区域中的流体彼此冲击。
  16. 根据权利要求1到3中任一项所述的微反应器，其特征在于，在一个混合单元的出口部和下一个混合单元的入口部之间形成了一个沿纵向朝向下游逐 渐扩张的扩张通道。
  17. 根据权利要求16所述的微反应器，其特征在于，所述扩张通道的扩张斜率为恒定的。
  18. 根据权利要求16所述的微反应器，其特征在于，所述扩张通道的最小截面尺寸不小于所述扩张通道的最大截面尺寸的1/4。
  19. 根据权利要求1到3中任一项所述的微反应器，其特征在于，所述扩张通道的最大截面尺寸在100微米至2厘米之间。
  20. 根据权利要求1到3中任一项所述的微反应器，其特征在于，所述扩张通道的最大截面尺寸与所述流动腔的最大横向尺寸之比在1/10至1/2之间。
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