Turbulence member, reactor and microreactor
By incorporating flow-disrupting components into the microreactor and the reactor, the problem of low mass and heat transfer efficiency in the microreactor was solved, enabling a highly efficient material mixing and reaction process.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- CHINA PETROLEUM & CHEMICAL CORP
- Filing Date
- 2022-12-08
- Publication Date
- 2026-04-21
AI Technical Summary
Microreactors suffer from problems such as large system pressure drop, low reaction flux, and short material residence time during mass and heat transfer, which limit their application and promotion.
The system employs flow-turbulence components, including a first flow-turbulence component and a second flow-turbulence component, to promote fluid turbulence and improve material mixing uniformity and reaction efficiency by setting flow-turbulence channels and holes in the reactor and microreactor.
This increased the flow rate of reactants, reduced the pressure drop, and made the reactants more uniformly mixed, thus achieving a rapid and stable reaction process.
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Figure CN118162069B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of chemical reaction apparatus technology, and more specifically to a flow-disrupting component, a reactor, and a microreactor. Background Technology
[0002] Microreactors are reaction devices with microstructures (channels, sieves, and grooves, etc.) that can form micron-scale dispersed single-phase or multiphase systems to enhance the reaction process. They offer advantages such as small characteristic scale, high transfer efficiency, and near-plug flow, enabling precise control of fluids and reaction conditions. However, the unique small scale of microreactors, while improving mass and heat transfer, also brings problems such as large system pressure drop, low reaction throughput, and short material residence time, severely limiting their application and widespread adoption. Tubular reactors are continuous-operation reactors with a large length-to-diameter ratio, belonging to plug flow reactors. These reactors can be very long; for example, the reactor tubes for propylene dimerization can be measured in kilometers. Tubular reactors have low backmixing, resulting in high volumetric efficiency (production capacity per unit volume), making them particularly suitable for applications requiring high conversion rates or with cascaded side reactions. To ensure uniform mixing of materials passing through a tubular reactor, internal components are typically installed inside. Combining microreactors and tubular reactors to achieve micron-scale dispersion and enhanced reaction processes throughout the entire reaction apparatus, while simultaneously enabling high-throughput industrial production, is of great significance. Summary of the Invention
[0003] The purpose of this invention is to provide a flow-disrupting component that can turbulentize the flowing fluid, thereby maintaining the fluid in a turbulent state and enabling more uniform mixing of fluids containing two or more materials, thereby ensuring stable and rapid reactions between the materials in the fluid.
[0004] To achieve the above objectives, the present invention provides a flow-disrupting component, the flow-disrupting component comprising:
[0005] A first flow-disrupting component, comprising a flow-disrupting fluid, wherein the flow-disrupting fluid is provided with a flow-disrupting channel extending axially along the flow-disrupting fluid; and
[0006] The second flow-disrupting component is disposed at the end of the flow-disrupting fluid. The second flow-disrupting component includes a component support and a protrusion disposed on the component support. At least one of the component support and the protrusion is provided with a flow-disrupting hole that allows fluid to pass through.
[0007] The above technical solution, by setting a first turbulence component and a second turbulence component, can better turbulent the fluid flowing through the turbulence component, thereby making the mixture of materials more uniform and facilitating the reaction between materials when the fluid contains two or more materials.
[0008] Preferably, the turbulence-inducing fluid comprises a plurality of corrugated plates having crests and troughs, and the plurality of corrugated plates are stacked on top of each other such that a corresponding turbulence-inducing channel is formed between adjacent corrugated plates.
[0009] Preferably, the component support has an arcuate support surface that protrudes toward the end away from the turbulent fluid; and / or
[0010] The protrusion is provided with a protruding arc-shaped surface that protrudes toward the end away from the turbulent fluid.
[0011] Preferably, the turbulence hole includes a first turbulence hole disposed in the component support; and / or
[0012] The turbulence hole includes a second turbulence hole disposed on the protrusion.
[0013] Preferably, the turbulence hole is elongated.
[0014] Preferably, the second turbulence member includes a plurality of protrusions, which are distributed circumferentially along the member support.
[0015] A second aspect of the present invention provides a reactor comprising a tube body and a plurality of flow-turbing components disposed within the tube body. The flow-turbing components are distributed along the axial direction of the tube body, and the flow-turbing components are those provided by the present invention, wherein the axial direction of the flow-turbing components is consistent with the axial direction of the tube body. By incorporating the flow-turbing components provided by the present invention into the reactor, the fluid flowing through the reactor can be better maintained in a turbulent state, thereby resulting in more uniform mixing of materials in the fluid and promoting stable reactions between materials.
[0016] Preferably, the spacing between adjacent flow-disrupting components is 5%-50% of the length of the pipe body; and / or
[0017] Along the flow direction of the fluid, the second turbulence member of the turbulence member is disposed downstream of the first turbulence member.
[0018] A third aspect of the present invention provides a microreaction device, the microreaction device comprising:
[0019] A feeding unit, the feeding unit being configured to provide reactants; and
[0020] A reaction unit is provided downstream of the feeding unit. The reaction unit includes a microreactor connected to the feeding unit and a reactor located downstream of and connected to the microreactor. The reactor is the reactor provided by the present invention.
[0021] By incorporating the reactor provided by this invention into a microreactor, the throughput of reactants can be increased, the pressure drop reduced, and the reactants kept in a turbulent state. As a result, the reactants are mixed more uniformly, enabling a rapid and stable reaction.
[0022] Preferably, the feeding unit includes a plurality of feeding tanks arranged in parallel with each other, wherein each feeding tank is in fluid communication with the microreactor; and / or
[0023] The reaction unit includes multiple microreactors and multiple reactors connected in series with each other, and the multiple microreactors and multiple reactors are alternately distributed along the flow direction of the material. Attached Figure Description
[0024] Figure 1 This is a front view schematic diagram of the turbulence-disrupting component according to a preferred embodiment of the present invention;
[0025] Figure 2 yes Figure 1 A three-dimensional structural schematic diagram of the first turbulence component in the shown turbulence components;
[0026] Figure 3 yes Figure 1 A three-dimensional structural schematic diagram of the second turbulence component in the turbulence-disrupting components shown;
[0027] Figure 4 This is a schematic diagram of the overall structure of the microreactor according to a preferred embodiment of the present invention.
[0028] Explanation of reference numerals in the attached figures
[0029] 40-Breakthrough component; 42-First bleedthrough component; 420-Breakthrough fluid; 420a-Corrugated plate; 422-Breakthrough channel; 44-Second bleedthrough component; 440-Component support; 440a-Arcted surface of support; 442-Protrusion; 442a-Arcted surface of protrusion; 444-Breakthrough hole; 444a-First bleedthrough hole; 444b-Second bleedthrough hole; 80-Microreactor; 82-Feeding unit; 820-Feed tank; 822-Transfer pump; 84-Reaction unit; 840-Microreactor; 86-Post-processing unit; 88-Heat exchanger. Detailed Implementation
[0030] In this invention, unless otherwise stated, directional terms such as "up," "down," "left," and "right" are generally understood in conjunction with the accompanying drawings and the orientation shown in actual application, while "inner" and "outer" refer to the inner and outer contours of the component.
[0031] It should be noted that the reactor may include a tube body and multiple flow-turbating components 40 disposed within the tube body. The multiple flow-turbating components 40 may be distributed at intervals along the axial direction of the tube body. The reactor will be described in detail later and will not be repeated here.
[0032] This invention provides a flow-disrupting component, combined with Figure 1 , Figure 2 and Figure 3 As shown, the flow-dispersing component 40 includes a first flow-dispersing component 42 and a second flow-dispersing component 44. The first flow-dispersing component 42 includes a flow-dispersing fluid 420, which is provided with a flow-dispersing channel 422 extending along the axial direction of the flow-dispersing fluid 420. It should be noted that when the flow-dispersing component 40 is placed in the reactor, the flow-dispersing channel 422 can extend along the axial direction of the tube body, that is, the axial direction of the flow-dispersing fluid 420 is consistent with the axial direction of the tube body. The second flow-dispersing component 44 is disposed at the end of the flow-dispersing fluid 420. Preferably, in the direction of fluid flow, the second flow-dispersing component 44 can be disposed downstream of the first flow-dispersing component 42. The second flow-dispersing component 44 includes a component support 440 and a protrusion 442 disposed on the component support 440. At least one of the component support 440 and the protrusion 442 is provided with a flow-dispersing hole 444 that allows fluid to pass through. By providing the first turbulence-disrupting member 42 and the second turbulence-disrupting member 44, the fluid flowing through the turbulence-disrupting member 40 can be better agitated. This allows for more uniform mixing of materials when two or more are mixed in the fluid, thus facilitating the reaction between the materials. The turbulence-disrupting member 40 is particularly suitable for reactors. When the turbulence-disrupting member 40 is placed inside the reactor, the first turbulence-disrupting member 42 can be positioned on the side facing the fluid, while the second turbulence-disrupting member 44 can be positioned on the side away from the fluid. Thus, in the direction of fluid flow, the first turbulence-disrupting member 42 faces the fluid, while the second turbulence-disrupting member 44 moves away from the fluid.
[0033] like Figure 2As shown, the turbulence-inducing fluid 420 may include multiple corrugated plates 420a, each having crests and troughs. These corrugated plates 420a are stacked on top of each other to form corresponding turbulence-inducing channels 422 between adjacent plates. For example, the crests and troughs of adjacent corrugated plates 420a may be staggered to form corresponding turbulence-inducing channels 422. It is understood that in adjacent corrugated plates 420a, the crest of one plate 420a faces the trough of another plate 420a to jointly enclose and form the corresponding turbulence-inducing channel 422. Using stacked corrugated plates 420a to form the turbulence-inducing fluid 420 not only enables the first turbulence-inducing member 422 to achieve its turbulence-inducing effect but also facilitates its fabrication. The turbulence-inducing fluid 420 may be columnar. It should be noted that multiple square corrugated plates 420a can be stacked together and adapted to obtain columnar turbulent fluid 420, which facilitates assembly into the pipe body.
[0034] To further enhance the turbulence-disrupting effect of the second turbulence-disrupting component 44, multiple protrusions 442 can be provided, and these protrusions 442 can be distributed circumferentially along the component support 440. For example... Figure 3 As shown, the entire second spoiler component 44 is petal-shaped.
[0035] like Figure 3 As shown, the component support 440 may be provided with a support arcuate surface 440a protruding toward the end away from the turbulent fluid 420, which can improve the turbulence effect of the second turbulence component 44; in addition, in order to further improve the turbulence effect of the second turbulence component 44 on the flowing fluid, the protrusion 442 may be provided with a protrusion arcuate surface 442a protruding toward the end away from the turbulent fluid 420.
[0036] In addition, a first turbulence hole 444a can be provided on the component support 440, wherein the first turbulence hole 444a can be elongated; in order to further improve the turbulence effect, multiple first turbulence holes 444a can be provided on the component support 440, and the multiple first turbulence holes 444a can be arranged side by side.
[0037] It is understood that a second turbulence hole 444b can be provided on the protrusion 442, wherein the second turbulence hole 444b can be elongated; in order to further improve the turbulence effect, multiple second turbulence holes 444b can be provided on the protrusion 442, and the multiple second turbulence holes 444b can be arranged side by side.
[0038] The present invention also provides a reactor comprising a tube body and a plurality of flow-disrupting members 40 disposed within the tube body. The plurality of flow-disrupting members 40 are axially distributed along the tube body, wherein the flow-disrupting members 40 are those provided by the present invention, and the axial direction of the flow-disrupting fluid 420 is consistent with the axial direction of the tube body. It is understood that when the flow-disrupting members 40 are disposed within the tube body, the flow-disrupting fluid 420 of the first flow-disrupting member 42 can extend axially along the tube body. It is also understood that when the first flow-disrupting member 42 and the second flow-disrupting member 44 are provided, the plurality of first flow-disrupting members 42 and the second flow-disrupting member 44 can be alternately distributed in the fluid flow direction. By providing the flow-disrupting members 40 provided by the present invention in the reactor, the fluid flowing through the reactor can be better maintained in a turbulent state, thereby making the material in the fluid more uniformly mixed, thus promoting stable reactions between materials. In addition, the reactor can increase the flux of the flowing fluid and reduce the pressure drop.
[0039] The spacing between adjacent flow-disrupting components 40 can be set to 5%-50% of the length of the pipe body. In this way, flow-disrupting components can be reasonably set in the pipe body, which can not only effectively turbulent the fluid, but also avoid setting too many flow-disrupting components in the pipe body, thus effectively controlling costs.
[0040] In order to better turbulent the flowing fluid, the second turbulence member 44 in the turbulence member 40 may be disposed downstream of the first turbulence member 42 along the flow direction of the fluid.
[0041] Alternatively, an outer tube can be fitted over the outside of the tube body, creating a gap between the outer tube and the tube body. This gap can be configured to allow a heat exchange medium to pass through, which exchanges heat with the fluid flowing through the tube body.
[0042] Furthermore, multiple pipe bodies connected in series can be provided. Each pipe body can be provided with multiple flow-dispersing components 40 distributed along the axial direction of the corresponding pipe body. The multiple flow-dispersing components 40 can be spaced apart along the axial direction of the pipe body. The inner diameter of the pipe body can be 1-40cm, preferably 5-20cm; in addition, the length of the pipe body can be 0.3-100m, preferably 0.5-50m.
[0043] The present invention also provides a microreactor 80, which includes a feed unit 82 configured to provide reactants. The microreactor 80 further includes a reaction unit 84 disposed downstream of the feed unit 82. The reaction unit 84 includes a microreactor 840 connected to the feed unit 82 and a reactor disposed downstream of and connected to the microreactor 840. It is understood that, in the flow direction of the reactants, the reactor can be disposed downstream of the microreactor 840. The reactor is the reactor provided by the present invention. By incorporating the reactor provided by the present invention into the microreactor 80, the throughput of the reactants used to generate the product can be increased, the pressure drop reduced, and the reactants kept in a turbulent state. Therefore, the reactants are mixed more uniformly, enabling a rapid and stable reaction.
[0044] like Figure 4 As shown, the feeding unit 82 may include a plurality of feed tanks 820 arranged in parallel with each other, wherein each feed tank 820 may be in fluid communication with the microreactor 840. It is understood that the number of feed tanks 820 may correspond to the number of types of reactants.
[0045] To better transport the reactants, a transfer pump 822 can be installed on the connecting pipeline between the feed tank 820 and the microreactor 840. Correspondingly, transfer pumps 822 can be installed corresponding to their respective feed tanks 820. For example, three transfer pumps 822 can be installed to transport three different materials respectively.
[0046] In the reaction unit 84, multiple microreactors 840 and multiple reactors connected in series can be set up. The multiple microreactors 840 and multiple reactors can be alternately distributed along the flow direction of the reactants. By setting up multiple microreactors 840 and multiple reactors that are alternately distributed, the throughput and the reaction rate can be further increased.
[0047] Furthermore, along the flow direction of the reactants, such as Figure 4 As shown, a post-processing unit 86 can be provided downstream of the reaction unit 84. The post-processing unit 86 can be configured to perform subsequent processing on the reaction products according to actual needs, such as static stratification, neutralization, washing, drying, etc.
[0048] like Figure 4 As shown, a heat exchanger 88 capable of exchanging heat with materials containing reaction products can be provided between the reaction unit 84 and the post-processing unit 86.
[0049] The effects of the present invention will be further illustrated below through examples and comparative examples.
[0050] Example
[0051] Example 1
[0052] by Figure 4 The microreactor 80 shown is used for the synthesis of di-tert-butyl peroxide. It includes three feed tanks 820 arranged in parallel to each other to hold sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Three transfer pumps 822, corresponding to the three feed tanks 820, are also provided to transfer the sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Two microreactors 840 and two reactors provided by this invention are provided in fluid communication with the feed tanks 820, with the two microreactors 840 and the two reactors alternately distributed in the direction of reactant flow. Furthermore, a post-processing unit 86 is provided downstream of the reaction unit 84. The post-processing unit 86 is capable of static stratification of the material containing the reaction products, and the separated oil phase undergoes neutralization, washing, and drying steps. A heat exchanger 88, capable of heat exchange with the material containing the reaction products, is provided between the reaction unit 84 and the post-processing unit 86. The reactor is equipped with a flow-dispersing component 40, which includes a first flow-dispersing component 42 and a second flow-dispersing component 44 disposed at the end of the first flow-dispersing component 42 and located downstream of the first flow-dispersing component 42. The component support 440 of the second flow-dispersing component 44 is provided with a plurality of first flow-dispersing holes 444a, and the spacing between adjacent flow-dispersing components 40 is 40% of the length of the tube body.
[0053] In the reaction process, concentrated sulfuric acid with a volume concentration of 80%, tert-butanol with a volume concentration of 99%, and hydrogen peroxide with a volume concentration of 30% were used. The molar ratio of hydrogen peroxide:tert-butanol:sulfuric acid was 1:2.05:1.6. Figure 4 As shown, three streams of material are pumped into reaction unit 82 by corresponding transfer pumps 822. Specifically, the first microreactor 840 located upstream in reaction unit 82 is a sheet-type microchannel reactor with a liquid holding capacity of 400 ml and a controlled temperature of 35°C; the first reactor located upstream in reaction unit 84 has an inner diameter of 6 cm and a length of 21 m, with a controlled temperature of 46°C; the second microreactor 840 located downstream in reaction unit 82 has a controlled temperature of 46°C; the second reactor located downstream in reaction unit 82 has an inner diameter of 6 cm and a length of 20 m, with a controlled temperature of 52°C; and the heat exchanger 88 has a controlled temperature of 30°C. The material obtained from the reaction, containing the product di-tert-butyl peroxide, enters the post-processing unit 86 for water-oil two-phase separation; subsequently, the obtained oil phase is neutralized, washed with water, and dried to obtain the product di-tert-butyl peroxide, while the waste acid in the aqueous phase is recycled. After the reaction was completed, the conversion rate of hydrogen peroxide was 99.1%, and the purity of the product was 99.3%.
[0054] Example 2
[0055] by Figure 4 The microreactor 80 shown is used for the synthesis of di-tert-butyl peroxide. It includes three feed tanks 820 arranged in parallel to each other to hold sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Three transfer pumps 822, corresponding to the three feed tanks 820, are also provided to transfer the sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Two microreactors 840 and two reactors provided by this invention are provided in fluid communication with the feed tanks 820, with the two microreactors 840 and the two reactors alternately distributed in the direction of reactant flow. Furthermore, a post-processing unit 86 is provided downstream of the reaction unit 84. The post-processing unit 86 is capable of static stratification of the material containing the reaction products, and the separated oil phase undergoes neutralization, washing, and drying steps. A heat exchanger 88, capable of heat exchange with the material containing the reaction products, is provided between the reaction unit 84 and the post-processing unit 86. The reactor is equipped with a flow-dispersing component 40, which includes a first flow-dispersing component 42 and a second flow-dispersing component 44 disposed at the end of the first flow-dispersing component 42 and located downstream of the first flow-dispersing component 42. The component support 440 of the second flow-dispersing component 44 is provided with a plurality of first flow-dispersing holes 444a, and the spacing between adjacent flow-dispersing components 40 is 40% of the length of the tube body.
[0056] In the reaction process, concentrated sulfuric acid with a volume concentration of 80%, tert-butanol with a volume concentration of 99%, and hydrogen peroxide with a volume concentration of 30% were used. The molar ratio of hydrogen peroxide:tert-butanol:sulfuric acid was 1:2.05:1.6. Figure 4 As shown, three streams of material are pumped into reaction unit 82 by corresponding transfer pumps 822. Specifically, the first microreactor 840 located upstream in reaction unit 82 is a sheet-type microchannel reactor with a liquid holding capacity of 300 ml and a controlled temperature of 35°C; the first reactor located upstream in reaction unit 84 has an inner diameter of 6 cm and a length of 21 m, with a controlled temperature of 46°C; the second microreactor 840 located downstream in reaction unit 82 has a controlled temperature of 46°C; the second reactor located downstream in reaction unit 82 has an inner diameter of 6 cm and a length of 20 m, with a controlled temperature of 52°C; and the heat exchanger 88 has a controlled temperature of 30°C. The material obtained from the reaction, containing the product di-tert-butyl peroxide, enters the post-processing unit 86 for water-oil two-phase separation; subsequently, the obtained oil phase is neutralized, washed with water, and dried to obtain the product di-tert-butyl peroxide, while the waste acid in the aqueous phase is recycled. After the reaction was completed, the conversion rate of hydrogen peroxide was 99.2% and the purity of the product was 99.3%.
[0057] Example 3
[0058] by Figure 4 The microreactor 80 shown is used for the synthesis of di-tert-butyl peroxide. It includes three feed tanks 820 arranged in parallel to each other to hold sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Three transfer pumps 822, corresponding to the three feed tanks 820, are also provided to transfer the sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Two microreactors 840 and two reactors provided by this invention are provided in fluid communication with the feed tanks 820, with the two microreactors 840 and the two reactors alternately distributed in the direction of reactant flow. Furthermore, a post-processing unit 86 is provided downstream of the reaction unit 84. The post-processing unit 86 is capable of static stratification of the material containing the reaction products, and the separated oil phase undergoes neutralization, washing, and drying steps. A heat exchanger 88, capable of heat exchange with the material containing the reaction products, is provided between the reaction unit 84 and the post-processing unit 86. The reactor is equipped with a flow-dispersing component 40, which includes a first flow-dispersing component 42 and a second flow-dispersing component 44 located at the end of the first flow-dispersing component 42 and downstream of the first flow-dispersing component 42. The spacing between adjacent flow-dispersing components 40 is 40% of the length of the tube body. The component support 440 of the second flow-dispersing component 44 has a support arc surface 440a. A plurality of first flow-dispersing holes 444a are provided on the component support 440. The first flow-dispersing holes 444a are elongated.
[0059] In the reaction process, concentrated sulfuric acid with a volume concentration of 80%, tert-butanol with a volume concentration of 99%, and hydrogen peroxide with a volume concentration of 30% were used. The molar ratio of hydrogen peroxide:tert-butanol:sulfuric acid was 1:2.05:1.6. Figure 4 As shown, three streams of material are pumped into reaction unit 82 by corresponding transfer pumps 822. Specifically, the first microreactor 840 located upstream in reaction unit 82 is a sheet-type microchannel reactor with a liquid holding capacity of 200 ml and a controlled temperature of 35°C; the first reactor located upstream in reaction unit 84 has an inner diameter of 6 cm and a length of 21 m, with a controlled temperature of 46°C; the second microreactor 840 located downstream in reaction unit 82 has a controlled temperature of 46°C; the second reactor located downstream in reaction unit 82 has an inner diameter of 6 cm and a length of 20 m, with a controlled temperature of 52°C; and the heat exchanger 88 has a controlled temperature of 30°C. The material obtained from the reaction, containing the product di-tert-butyl peroxide, enters the post-processing unit 86 for water-oil two-phase separation; subsequently, the obtained oil phase is neutralized, washed with water, and dried to obtain the product di-tert-butyl peroxide, while the waste acid in the aqueous phase is recycled. After the reaction was completed, the conversion rate of hydrogen peroxide was 99.3% and the purity of the product was 99.4%.
[0060] Example 4
[0061] by Figure 4 The microreactor 80 shown is used for the synthesis of di-tert-butyl peroxide. It includes three feed tanks 820 arranged in parallel to each other to hold sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Three transfer pumps 822, corresponding to the three feed tanks 820, are also provided to transfer the sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Two microreactors 840 and two reactors provided by this invention are provided in fluid communication with the feed tanks 820, with the two microreactors 840 and the two reactors alternately distributed in the direction of reactant flow. Furthermore, a post-processing unit 86 is provided downstream of the reaction unit 84. The post-processing unit 86 is capable of static stratification of the material containing the reaction products, and the separated oil phase undergoes neutralization, washing, and drying steps. A heat exchanger 88, capable of heat exchange with the material containing the reaction products, is provided between the reaction unit 84 and the post-processing unit 86. The reactor is equipped with a flow-dispersing component 40, which includes a first flow-dispersing component 42 and a second flow-dispersing component 44 located at the end of the first flow-dispersing component 42 and downstream of the first flow-dispersing component 42. The spacing between adjacent flow-dispersing components 40 is 30% of the length of the tube body. The component support 440 of the second flow-dispersing component 44 has a support arc-shaped surface 440a. A plurality of second flow-dispersing holes 444b are provided on the protrusion 442. The second flow-dispersing holes 444b are elongated.
[0062] In the reaction process, concentrated sulfuric acid with a volume concentration of 80%, tert-butanol with a volume concentration of 99%, and hydrogen peroxide with a volume concentration of 30% were used. The molar ratio of hydrogen peroxide:tert-butanol:sulfuric acid was 1:2.05:1.6. Figure 4 As shown, three streams of material are pumped into reaction unit 82 by corresponding transfer pumps 822. Specifically, the first microreactor 840 located upstream in reaction unit 82 is a sheet-type microchannel reactor with a liquid holding capacity of 300 ml and a controlled temperature of 35°C; the first reactor located upstream in reaction unit 84 has an inner diameter of 6 cm and a length of 21 m, with a controlled temperature of 46°C; the second microreactor 840 located downstream in reaction unit 82 has a controlled temperature of 46°C; the second reactor located downstream in reaction unit 82 has an inner diameter of 6 cm and a length of 20 m, with a controlled temperature of 52°C; and the heat exchanger 88 has a controlled temperature of 30°C. The material obtained from the reaction, containing the product di-tert-butyl peroxide, enters the post-processing unit 86 for water-oil two-phase separation; subsequently, the obtained oil phase is neutralized, washed with water, and dried to obtain the product di-tert-butyl peroxide, while the waste acid in the aqueous phase is recycled. After the reaction was completed, the conversion rate of hydrogen peroxide was 99.4%, and the purity of the product was 99.4%.
[0063] Example 5
[0064] by Figure 4 The microreactor 80 shown is used for the synthesis of di-tert-butyl peroxide. It includes three feed tanks 820 arranged in parallel to each other to hold sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Three transfer pumps 822, corresponding to the three feed tanks 820, are also provided to transfer the sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Two microreactors 840 and two reactors provided by this invention are provided in fluid communication with the feed tanks 820, with the two microreactors 840 and the two reactors alternately distributed in the direction of reactant flow. Furthermore, a post-processing unit 86 is provided downstream of the reaction unit 84. The post-processing unit 86 is capable of static stratification of the material containing the reaction products, and the separated oil phase undergoes neutralization, washing, and drying steps. A heat exchanger 88, capable of heat exchange with the material containing the reaction products, is provided between the reaction unit 84 and the post-processing unit 86. The reactor is equipped with a flow-dispersing component 40, which includes a first flow-dispersing component 42 and a second flow-dispersing component 44 located at the end of the first flow-dispersing component 42 and downstream of the first flow-dispersing component 42. The spacing between adjacent flow-dispersing components 40 is 20% of the length of the tube body. The protrusion 442 of the second flow-dispersing component 44 has a protrusion arc-shaped surface 442a, and a plurality of second flow-dispersing holes 444b are provided on the protrusion 442. The second flow-dispersing holes 444b are elongated.
[0065] In the reaction process, concentrated sulfuric acid with a volume concentration of 80%, tert-butanol with a volume concentration of 99%, and hydrogen peroxide with a volume concentration of 30% were used. The molar ratio of hydrogen peroxide:tert-butanol:sulfuric acid was 1:2.05:1.6. Figure 4As shown, three streams of material are pumped into reaction unit 82 by corresponding transfer pumps 822. Specifically, the first microreactor 840 located upstream in reaction unit 82 is a sheet-type microchannel reactor with a liquid holding capacity of 300 ml and a controlled temperature of 35°C; the first reactor located upstream in reaction unit 84 has an inner diameter of 6 cm and a length of 21 m, with a controlled temperature of 46°C; the second microreactor 840 located downstream in reaction unit 82 has a controlled temperature of 46°C; the second reactor located downstream in reaction unit 82 has an inner diameter of 6 cm and a length of 20 m, with a controlled temperature of 52°C; and the heat exchanger 88 has a controlled temperature of 30°C. The material obtained from the reaction, containing the product di-tert-butyl peroxide, enters the post-processing unit 86 for water-oil two-phase separation; subsequently, the obtained oil phase is neutralized, washed with water, and dried to obtain the product di-tert-butyl peroxide, while the waste acid in the aqueous phase is recycled. After the reaction was completed, the conversion rate of hydrogen peroxide was 99.5%, and the purity of the product was 99.5%.
[0066] Example 6
[0067] by Figure 4 The microreactor 80 shown is used for the synthesis of di-tert-butyl peroxide. It includes three feed tanks 820 arranged in parallel to each other to hold sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Three transfer pumps 822, corresponding to the three feed tanks 820, are also provided to transfer the sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Two microreactors 840 and two reactors provided by this invention are provided in fluid communication with the feed tanks 820, with the two microreactors 840 and the two reactors alternately distributed in the direction of reactant flow. Furthermore, a post-processing unit 86 is provided downstream of the reaction unit 84. The post-processing unit 86 is capable of static stratification of the material containing the reaction products, and the separated oil phase undergoes neutralization, washing, and drying steps. A heat exchanger 88, capable of heat exchange with the material containing the reaction products, is provided between the reaction unit 84 and the post-processing unit 86. The reactor includes a flow-dispersing component 40, which comprises a first flow-dispersing component 42 and a second flow-dispersing component 44 located at the end of the first flow-dispersing component 42 and downstream of it. The spacing between adjacent flow-dispersing components 40 is 10% of the length of the tube body. The component support 440 of the second flow-dispersing component 44 has a support arcuate surface 440a and a plurality of first flow-dispersing holes 444a are provided on the component support 440. The protrusion 442 of the second flow-dispersing component 44 has a protrusion arcuate surface 442a and a plurality of second flow-dispersing holes 444b are provided on the protrusion.
[0068] In the reaction process, concentrated sulfuric acid with a volume concentration of 80%, tert-butanol with a volume concentration of 99%, and hydrogen peroxide with a volume concentration of 30% were used. The molar ratio of hydrogen peroxide:tert-butanol:sulfuric acid was 1:2.05:1.6. Figure 4 As shown, three streams of material are pumped into reaction unit 82 by corresponding transfer pumps 822. Specifically, the first microreactor 840 located upstream in reaction unit 82 is a sheet-type microchannel reactor with a liquid holding capacity of 280 ml and a controlled temperature of 35°C; the first reactor located upstream in reaction unit 84 has an inner diameter of 6 cm and a length of 21 m, with a controlled temperature of 46°C; the second microreactor 840 located downstream in reaction unit 82 has a controlled temperature of 46°C; the second reactor located downstream in reaction unit 82 has an inner diameter of 6 cm and a length of 20 m, with a controlled temperature of 52°C; and the heat exchanger 88 has a controlled temperature of 30°C. The material obtained from the reaction, containing the product di-tert-butyl peroxide, enters the post-processing unit 86 for water-oil two-phase separation; subsequently, the obtained oil phase is neutralized, washed with water, and dried to obtain the product di-tert-butyl peroxide, while the waste acid in the aqueous phase is recycled. After the reaction was completed, the conversion rate of hydrogen peroxide was 99.6%, and the purity of the product was 99.4%.
[0069] Example 7
[0070] by Figure 4The microreactor 80 shown is used for the synthesis of di-tert-butyl peroxide. It includes three feed tanks 820 arranged in parallel to each other to hold sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Three transfer pumps 822, corresponding to the three feed tanks 820, are also provided to transfer the sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Two microreactors 840 and two reactors provided by this invention are provided in fluid communication with the feed tanks 820, with the two microreactors 840 and the two reactors alternately distributed in the direction of reactant flow. Furthermore, a post-processing unit 86 is provided downstream of the reaction unit 84. The post-processing unit 86 is capable of static stratification of the material containing the reaction products, and the separated oil phase undergoes neutralization, washing, and drying steps. A heat exchanger 88, capable of heat exchange with the material containing the reaction products, is provided between the reaction unit 84 and the post-processing unit 86. The reactor includes a flow-dispersing component 40, which comprises a first flow-dispersing component 42 and a second flow-dispersing component 44 located at the end of the first flow-dispersing component 42 and downstream of it. The spacing between adjacent flow-dispersing components 40 is 10% of the length of the tube body. The component support 440 of the second flow-dispersing component 44 has a support arc-shaped surface 440a, and a plurality of first flow-dispersing holes 444a are provided on the component support 440. The first flow-dispersing holes 444a are elongated. The protrusion 442 of the second flow-dispersing component 44 has a protrusion arc-shaped surface 442a, and a plurality of second flow-dispersing holes 444b are provided on the protrusion.
[0071] In the reaction process, concentrated sulfuric acid with a volume concentration of 80%, tert-butanol with a volume concentration of 99%, and hydrogen peroxide with a volume concentration of 30% were used. The molar ratio of hydrogen peroxide:tert-butanol:sulfuric acid was 1:2.05:1.6. Figure 4 As shown, three streams of material are pumped into reaction unit 82 by corresponding transfer pumps 822. Specifically, the first microreactor 840 located upstream in reaction unit 82 is a sheet-type microchannel reactor with a liquid holding capacity of 300 ml and a controlled temperature of 35°C; the first reactor located upstream in reaction unit 84 has an inner diameter of 6 cm and a length of 21 m, with a controlled temperature of 46°C; the second microreactor 840 located downstream in reaction unit 82 has a controlled temperature of 46°C; the second reactor located downstream in reaction unit 82 has an inner diameter of 16 cm and a length of 1 m, with a controlled temperature of 52°C; and the heat exchanger 88 has a controlled temperature of 30°C. The material obtained from the reaction, containing the product di-tert-butyl peroxide, enters the post-processing unit 86 for water-oil two-phase separation; subsequently, the obtained oil phase is neutralized, washed with water, and dried to obtain the product di-tert-butyl peroxide, while the waste acid in the aqueous phase is recycled. After the reaction was completed, the conversion rate of hydrogen peroxide was 99.3% and the purity of the product was 99.2%.
[0072] Example 8
[0073] by Figure 4 The microreactor 80 shown is used for the synthesis of di-tert-butyl peroxide. It includes three feed tanks 820 arranged in parallel to each other to hold sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Three transfer pumps 822, corresponding to the three feed tanks 820, are also provided to transfer the sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Two microreactors 840 and two reactors provided by this invention are provided in fluid communication with the feed tanks 820, with the two microreactors 840 and the two reactors alternately distributed in the direction of reactant flow. Furthermore, a post-processing unit 86 is provided downstream of the reaction unit 84. The post-processing unit 86 is capable of static stratification of the material containing the reaction products, and the separated oil phase undergoes neutralization, washing, and drying steps. A heat exchanger 88, capable of heat exchange with the material containing the reaction products, is provided between the reaction unit 84 and the post-processing unit 86. The reactor includes a flow-dispersing component 40, which comprises a first flow-dispersing component 42 and a second flow-dispersing component 44 located at the end of the first flow-dispersing component 42 and downstream of it. The spacing between adjacent flow-dispersing components 40 is 10% of the length of the tube body. The component support 440 of the second flow-dispersing component 44 has a support arc-shaped surface 440a, and a plurality of first flow-dispersing holes 444a are provided on the component support 440. The first flow-dispersing holes 444a are elongated. The protrusion 442 of the second flow-dispersing component 44 has a protrusion arc-shaped surface 442a, and a plurality of second flow-dispersing holes 444b are provided on the protrusion 442. The second flow-dispersing holes 444b are elongated.
[0074] In the reaction process, concentrated sulfuric acid with a volume concentration of 80%, tert-butanol with a volume concentration of 99%, and hydrogen peroxide with a volume concentration of 30% were used. The molar ratio of hydrogen peroxide:tert-butanol:sulfuric acid was 1:2.05:1.6. Figure 4As shown, three streams of material are pumped into reaction unit 82 by corresponding transfer pumps 822. Specifically, the first microreactor 840 located upstream in reaction unit 82 is a sheet-type microchannel reactor with a liquid holding capacity of 280 ml and a controlled temperature of 35°C; the first reactor located upstream in reaction unit 84 has an inner diameter of 16 cm and a length of 1 m, with a controlled temperature of 46°C; the second microreactor 840 located downstream in reaction unit 82 has a controlled temperature of 46°C; the second reactor located downstream in reaction unit 82 has an inner diameter of 6 cm and a length of 20 m, with a controlled temperature of 52°C; and the heat exchanger 88 has a controlled temperature of 30°C. The material obtained from the reaction, containing the product di-tert-butyl peroxide, enters the post-processing unit 86 for water-oil two-phase separation; subsequently, the obtained oil phase is neutralized, washed with water, and dried to obtain the product di-tert-butyl peroxide, while the waste acid in the aqueous phase is recycled. After the reaction was completed, the conversion rate of hydrogen peroxide was 99.3% and the purity of the product was 99.3%.
[0075] Example 9
[0076] by Figure 4 The microreactor 80 shown is used for the synthesis of di-tert-butyl peroxide. It includes three feed tanks 820 arranged in parallel to each other to hold sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Three transfer pumps 822, corresponding to the three feed tanks 820, are also provided to transfer the sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Two microreactors 840 and two reactors provided by this invention are provided in fluid communication with the feed tanks 820, with the two microreactors 840 and the two reactors alternately distributed in the direction of reactant flow. Furthermore, a post-processing unit 86 is provided downstream of the reaction unit 84. The post-processing unit 86 is capable of static stratification of the material containing the reaction products, and the separated oil phase undergoes neutralization, washing, and drying steps. A heat exchanger 88, capable of heat exchange with the material containing the reaction products, is provided between the reaction unit 84 and the post-processing unit 86. The reactor includes a flow-dispersing component 40, which comprises a first flow-dispersing component 42 and a second flow-dispersing component 44 located at the end of the first flow-dispersing component 42 and downstream of it. The spacing between adjacent flow-dispersing components 40 is 10% of the length of the tube body. The component support 440 of the second flow-dispersing component 44 has a support arcuate surface 440a. Multiple first flow-dispersing holes 444a are provided on the component support 440. The first flow-dispersing holes 444a are elongated. Multiple protrusions 442 of the second flow-dispersing component 44 are distributed circumferentially along the component support 440. Each protrusion 442 has a protrusion arcuate surface 442a and multiple second flow-dispersing holes 444b are provided on the protrusion. The second flow-dispersing holes 444b are elongated.
[0077] In the reaction process, concentrated sulfuric acid with a volume concentration of 80%, tert-butanol with a volume concentration of 99%, and hydrogen peroxide with a volume concentration of 30% were used. The molar ratio of hydrogen peroxide:tert-butanol:sulfuric acid was 1:2.05:1.6. Figure 4 As shown, three streams of material are pumped into reaction unit 82 by corresponding transfer pumps 822. Specifically, the first microreactor 840 located upstream in reaction unit 82 is a sheet-type microchannel reactor with a liquid holding capacity of 300 ml and a controlled temperature of 35°C; the first reactor located upstream in reaction unit 84 has an inner diameter of 16 cm and a length of 1 m, with a controlled temperature of 46°C; the second microreactor 840 located downstream in reaction unit 82 has a controlled temperature of 46°C; the second reactor located downstream in reaction unit 82 has an inner diameter of 16 cm and a length of 1 m, with a controlled temperature of 52°C; and the heat exchanger 88 has a controlled temperature of 30°C. The material obtained from the reaction, containing the product di-tert-butyl peroxide, enters the post-processing unit 86 for water-oil two-phase separation; subsequently, the obtained oil phase is neutralized, washed with water, and dried to obtain the product di-tert-butyl peroxide, while the waste acid in the aqueous phase is recycled. After the reaction was completed, the conversion rate of hydrogen peroxide was 99.2% and the purity of the product was 99.3%.
[0078] Example 10
[0079] by Figure 4The microreactor 80 shown is used for the synthesis of di-tert-butyl peroxide. It includes three feed tanks 820 arranged in parallel to each other to hold sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Three transfer pumps 822, corresponding to the three feed tanks 820, are also provided to transfer the sulfuric acid, hydrogen peroxide, and tert-butanol, respectively. Two microreactors 840 and two reactors provided by this invention are provided in fluid communication with the feed tanks 820, with the two microreactors 840 and the two reactors alternately distributed in the direction of reactant flow. Furthermore, a post-processing unit 86 is provided downstream of the reaction unit 84. The post-processing unit 86 is capable of static stratification of the material containing the reaction products, and the separated oil phase undergoes neutralization, washing, and drying steps. A heat exchanger 88, capable of heat exchange with the material containing the reaction products, is provided between the reaction unit 84 and the post-processing unit 86. The reactor includes a flow-dispersing component 40, which comprises a first flow-dispersing component 42 and a second flow-dispersing component 44 located at the end of the first flow-dispersing component 42 and downstream of it. The spacing between adjacent flow-dispersing components 40 is 30% of the length of the tube body. The component support 440 of the second flow-dispersing component 44 has a support arcuate surface 440a. Multiple first flow-dispersing holes 444a are provided on the component support 440. The first flow-dispersing holes 444a are elongated. Multiple protrusions 442 of the second flow-dispersing component 44 are distributed circumferentially along the component support 440. Each protrusion 442 has a protrusion arcuate surface 442a and multiple second flow-dispersing holes 444b are provided on the protrusion. The second flow-dispersing holes 444b are elongated.
[0080] In the reaction process, concentrated sulfuric acid with a volume concentration of 80%, tert-butanol with a volume concentration of 99%, and hydrogen peroxide with a volume concentration of 30% were used. The molar ratio of hydrogen peroxide:tert-butanol:sulfuric acid was 1:2.05:1.6. Figure 4As shown, three streams of material are pumped into reaction unit 82 by corresponding transfer pumps 822. Specifically, the first microreactor 840 located upstream in reaction unit 82 is a sheet-type microchannel reactor with a liquid holding capacity of 300 ml and a controlled temperature of 35°C; the first reactor located upstream in reaction unit 84 has an inner diameter of 16 cm and a length of 1 m, with a controlled temperature of 46°C; the second microreactor 840 located downstream in reaction unit 82 has a controlled temperature of 46°C; the second reactor located downstream in reaction unit 82 has an inner diameter of 16 cm and a length of 1 m, with a controlled temperature of 52°C; and the heat exchanger 88 has a controlled temperature of 30°C. The material obtained from the reaction, containing the product di-tert-butyl peroxide, enters the post-processing unit 86 for water-oil two-phase separation; subsequently, the obtained oil phase is neutralized, washed with water, and dried to obtain the product di-tert-butyl peroxide, while the waste acid in the aqueous phase is recycled. After the reaction was completed, the conversion rate of hydrogen peroxide was 99.1% and the purity of the product was 99.2%.
[0081] Comparative Example
[0082] Di-tert-butyl peroxide was synthesized using the same method as in Example 1, except that no turbulence-inducing components were installed in the reactor. After the reaction was completed, the conversion rate of hydrogen peroxide was found to be 90.1%, and the purity of the product was 89.2%.
[0083] Therefore, it can be seen that using the microreactor 80 provided by the present invention to synthesize di-tert-butyl peroxide can result in a higher conversion rate of the reactants and a higher purity of the product obtained from the reaction.
[0084] The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various specific technical features in any suitable manner. To avoid unnecessary repetition, the present invention will not describe the various possible combinations separately. However, these simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.
Claims
1. A flow-disrupting component, characterized in that, The turbulence-disrupting component (40) includes: A first turbulence member (42) includes a turbulence fluid (420), the turbulence fluid (420) being provided with a turbulence channel (422) extending axially along the turbulence fluid (420), wherein the turbulence fluid (420) includes a plurality of corrugated plates (420a), the corrugated plates (420a) having crests and troughs, the plurality of corrugated plates (420a) being stacked on top of each other such that a corresponding turbulence channel (422) is formed between adjacent corrugated plates (420a); and a second turbulence member (44), the second turbulence member (44) being disposed at the downstream end of the turbulence channel (422) of the turbulence fluid (420), the second turbulence member (44) including a member support (440) and a... A plurality of protrusions (442) are placed on the component support (440) and distributed circumferentially along the component support (440). The component support (440) is provided with a support arcuate surface (440a) protruding toward the end away from the turbulent fluid (420). The protrusions (442) are provided with protruding arcuate surfaces (442a) protruding toward the end away from the turbulent fluid (420). The component support (440) and the protrusions (442) are respectively provided with turbulence holes (444) that allow fluid to pass through. The turbulence holes (444) include a first turbulence hole (444a) provided on the component support (440) and a second turbulence hole (444b) provided on the protrusion (442).
2. The flow-disrupting component according to claim 1, characterized in that, The turbulence hole (444) is elongated.
3. A reactor, characterized in that, The reactor includes a tube body and a plurality of flow-disrupting components (40) disposed within the tube body. The plurality of flow-disrupting components (40) are distributed along the axial direction of the tube body. The flow-disrupting components (40) are the flow-disrupting components (40) as described in claim 1 or 2, wherein the axial direction of the flow-disrupting fluid (420) is consistent with the axial direction of the tube body.
4. The reactor according to claim 3, characterized in that, The spacing between adjacent flow-disrupting components (40) is 5%-50% of the length of the pipe body.
5. A microreactor, characterized in that, The microreactor (80) includes: Feeding unit (82), said feeding unit (82) being configured to provide reactants; and A reaction unit (84) is disposed downstream of the feed unit (82). The reaction unit (84) includes a microreactor (840) that is connected to the feed unit (82) and a reactor disposed downstream of and connected to the microreactor (840), wherein the reactor is the reactor described in claim 3 or 4.
6. The microreactor according to claim 5, characterized in that, The feeding unit (82) includes a plurality of feeding tanks (820) arranged in parallel with each other, wherein each feeding tank (820) is in fluid communication with the microreactor (840); The reaction unit (84) includes a plurality of microreactors (840) and a plurality of reactors connected in series with each other, the plurality of microreactors (840) and the plurality of reactors being alternately distributed along the flow direction of the material.
Citation Information
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