CN112546988A - Reaction device for solid phase surface fluorination - Google Patents
Reaction device for solid phase surface fluorination Download PDFInfo
- Publication number
- CN112546988A CN112546988A CN201910919025.4A CN201910919025A CN112546988A CN 112546988 A CN112546988 A CN 112546988A CN 201910919025 A CN201910919025 A CN 201910919025A CN 112546988 A CN112546988 A CN 112546988A
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- solid phase
- reaction
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 66
- 238000003682 fluorination reaction Methods 0.000 title claims abstract description 36
- 239000007790 solid phase Substances 0.000 title claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 62
- 230000005540 biological transmission Effects 0.000 claims abstract description 57
- 238000002955 isolation Methods 0.000 claims abstract description 40
- 238000007789 sealing Methods 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims description 6
- 125000006850 spacer group Chemical group 0.000 claims 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 18
- 239000011737 fluorine Substances 0.000 abstract description 18
- 229910052731 fluorine Inorganic materials 0.000 abstract description 18
- 239000007789 gas Substances 0.000 description 37
- 238000005192 partition Methods 0.000 description 14
- 239000000463 material Substances 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- -1 perfluoro compound Chemical class 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- 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
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to the technical field of solid phase surface fluorination treatment, and provides a reaction device for solid phase surface fluorination, which comprises a reactor, a stirring piece and a driving piece, wherein a reaction chamber, a transmission chamber and an isolation chamber are arranged in the reactor, the transmission end of the stirring piece is arranged in the transmission chamber, the output end of the driving piece is arranged in the isolation chamber, the transmission end of the stirring piece is in transmission connection with the output end of the driving piece, and sealing liquid is arranged in the isolation chamber. According to the reaction device for the solid phase surface fluorination, disclosed by the embodiment of the invention, the fluorine gas is effectively prevented from corroding the output end of the driving part, and the sealing property of the reaction device is ensured.
Description
Technical Field
The invention relates to the technical field of solid phase surface fluorination treatment, in particular to a reaction device for solid phase surface fluorination.
Background
With the research on the utilization of fluorine gas, fluorine gas fluorination is applied to various fields, and due to the particularity of fluorine gas, the requirement on a reaction system is very high, and particularly the requirement on the sealing property of the reaction system is more severe. When the driving end of the driving motor is installed, a common sealing ring encounters fluorine gas and reacts with the fluorine gas, the sealing performance of a reaction system is affected, and the fluorination efficiency is low and the fluorination is incomplete during the fluorination reaction.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides the reaction device for the solid-phase surface fluorination, which effectively prevents fluorine gas from corroding the output end of the driving part and ensures the sealing property of the reaction device.
The reaction device for solid phase surface fluorination comprises a reactor, a stirring piece and a driving piece, wherein a reaction chamber, a transmission chamber and an isolation chamber are arranged in the reactor, the transmission end of the stirring piece is arranged in the transmission chamber, the output end of the driving piece is arranged in the isolation chamber, the transmission end of the stirring piece is in transmission connection with the output end of the driving piece, and sealing liquid is arranged in the isolation chamber.
According to the reaction device for solid-phase surface fluorination, the interior of the reactor is divided into the reaction chamber, the transmission chamber and the isolation chamber, the transmission end of the stirring piece is arranged in the transmission chamber, the output end of the driving piece is arranged in the isolation chamber, and the sealing liquid is arranged in the isolation chamber, so that the output end of the driving piece is soaked in the sealing liquid, the corrosion of fluorine gas to the driving piece is effectively prevented, the sealing performance of the reaction device is ensured, the fluorination efficiency is further improved, and the complete fluorination of the solid-phase surface is ensured.
According to one embodiment of the invention, a partition member for separating the reaction chamber, the transmission chamber and the separation chamber is arranged in the reactor, the partition member is hermetically connected with the inner wall of the reactor, and the separation chamber is arranged below the transmission chamber along the height direction of the reactor. Through set up the separator in the reactor, guarantee the independent sealed of reaction chamber, transmission chamber and isolation chamber, improve the leakproofness of whole reactor.
According to one embodiment of the invention, the stirring member comprises a stirring shaft, a transmission end of the stirring shaft is arranged in the transmission chamber, the stirring end of the stirring shaft passes through the through hole on the isolating member and extends into the reaction chamber along the axial direction of the stirring shaft, and the stirring shaft is connected with the through hole in a sealing manner. The stirring of the solid-phase materials in the reaction chamber is realized, the full contact between the solid-phase materials and the fluorine gas is ensured, the fluorination efficiency is improved, and the complete fluorination is ensured.
According to one embodiment of the invention, the driving member is arranged outside the reactor, the outer wall of the isolation chamber is provided with a mounting hole, the output end of the driving member passes through the mounting hole and is connected with the transmission end of the stirring shaft arranged in the transmission chamber, and the output end of the driving member is hermetically connected with the mounting hole.
According to one embodiment of the invention, the output end of the driving part is provided with a driving wheel, the transmission end of the stirring shaft is provided with a transmission wheel, and the isolating part is provided with a long round hole for enabling the driving wheel to be meshed and connected with the transmission wheel.
According to one embodiment of the invention, the reaction chamber is communicated with a gas inlet pipeline, and the inlet end of the gas inlet pipeline is provided with a gas heater. The device is used for heating the gas introduced into the reaction chamber and improving the fluorination rate.
According to one embodiment of the invention, a temperature display is arranged in the reaction chamber, and the temperature in the reaction chamber is monitored in real time.
According to one embodiment of the invention, the top side of the reactor is provided with a gas outlet along the height direction of the reactor, and the bottom side of the reactor is provided with a solid phase discharge port along the height direction of the reactor.
According to an embodiment of the present invention, the partition includes a first partition plate disposed in a height direction of the reactor and having the same height as the reactor, and a second partition plate disposed in a direction perpendicular to the height of the reactor.
According to one embodiment of the invention, the axis of the stirring shaft is perpendicular to the height direction of the reactor.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is a schematic diagram showing the structure of a reaction apparatus for solid phase surface fluorination according to an embodiment of the present invention.
Reference numerals:
1: a reactor; 2: a reaction chamber; 3: a transmission chamber; 4: an isolation chamber; 5: sealing liquid; 6: a stirring shaft; 7: a drive member; 8: a first separator plate; 9: a second separator plate; 10: an air intake duct; 11: a gas heater; 12: an air outlet pipe; 13: a solid-phase discharge port; 14: a blade.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the description of the embodiments of the present invention, it should be noted that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the embodiments of the present invention and simplifying the description, but do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the embodiments of the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the embodiments of the present invention, it should be noted that, unless explicitly stated or limited otherwise, the terms "connected" and "connected" are to be interpreted broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. Specific meanings of the above terms in the embodiments of the present invention can be understood in specific cases by those of ordinary skill in the art.
In embodiments of the invention, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through intervening media. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of an embodiment of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
As shown in fig. 1, an embodiment of the present invention provides a reaction apparatus for solid phase surface fluorination, including a reactor 1, a stirring member, and a driving member 7, wherein a reaction chamber 2, a transmission chamber 3, and an isolation chamber 4 are disposed in the reactor 1, a transmission end of the stirring member is disposed in the transmission chamber 3, an output end of the driving member 7 is disposed in the isolation chamber 4, the transmission end of the stirring member is in transmission connection with the output end of the driving member 7, and a sealing liquid 5 is disposed in the isolation chamber 4. It can be understood that, through separating reactor 1 internal partitioning for reaction chamber 2, transmission chamber 3 and isolation chamber 4, guarantee the mutual independence of each chamber sealed, and set up the transmission end of stirring piece in transmission chamber 3, establish the output of driving piece 7 in isolation chamber 4, set up sealing liquid 5 in isolation chamber 4, make the output of driving piece 7 soak and establish in sealing liquid 5, effectively prevent the corruption of fluorine gas to driving piece 7, guarantee reaction unit's leakproofness, and then improve the efficiency of fluoridizing, guarantee that the solid phase surface is fluoridized completely, improve the utilization ratio of fluorine gas. It should be noted that in this embodiment, the material of the reactor 1 is a metal material, preferably a steel material; the stirring piece is made of metal, preferably steel; the driving piece 7 is a driving motor and drives the stirring piece to rotate; the sealing liquid 5 is a liquid phase material resistant to fluorine gas, preferably fluoropolyether oil. In one example, the inner wall surface of the reactor 1 is provided with an anticorrosive protective layer, which is preferably a perfluoro compound that does not react with fluorine gas.
In one embodiment of the present invention, a partition is provided in the reactor 1 to separate the reaction chamber 2, the transmission chamber 3 and the separation chamber 4, the partition is hermetically connected to the inner wall of the reactor 1, and the separation chamber 4 is provided below the transmission chamber 3 in the height direction of the reactor 1. It can be understood that by arranging the partition in the reactor 1, the independent sealing of the reaction chamber 2, the transmission chamber 3 and the isolation chamber 4 is ensured, and the sealing performance of the whole reactor 1 is improved. It should be noted that the reactor 1 in this embodiment has a rectangular parallelepiped structure with a cavity inside.
Further, the partition comprises a first partition plate 8 and a second partition plate 9, the first partition plate 8 is disposed along the height direction of the reactor 1, and the height of the first partition plate 8 is the same as the height of the reactor 1, and the second partition plate 9 is disposed along the direction perpendicular to the height of the reactor 1. It can be understood that the first isolation plate 8 is arranged in the reactor 1 along the vertical direction, the inner cavity of the reactor 1 is divided into two parts, and the edges of the first isolation plate 8 are respectively welded with the inner walls of the corresponding sides in the reactor 1, so that the sealing performance of the welding position is ensured. The second isolation plate 9 is arranged in the reactor 1 along the horizontal direction, as shown in fig. 1, the second isolation plate 9 divides the chamber on the right side of the first isolation plate 8 into two parts, the chamber on the left side of the first isolation plate 8 is the reaction chamber 2, the chamber on the upper side of the second isolation plate 9 is the transmission chamber 3, and the chamber on the lower side of the second isolation plate 9 is the isolation chamber 4. The left side of the second isolation plate 9 is welded with the first isolation plate 9, and the rest three sides are respectively welded with the inner walls of the front side, the right side and the rear side of the reactor 1, so that the sealing performance of the welding position is ensured. It is worth to say that the isolation chamber 4 is arranged below the transmission chamber 3, and the sealing liquid 5 is injected into the isolation chamber 4, so that the output end of the driving piece 7 is soaked, and the contact between the fluorine gas and the driving piece 7 is avoided. The amount of sealing liquid 5 injected is sufficient to ensure that the output end of the driver 7 is completely immersed.
In one embodiment of the invention, the stirring member comprises a stirring shaft 6, a transmission end of the stirring shaft 6 is arranged in the transmission chamber 3, the stirring end of the stirring shaft 6 passes through a through hole on the isolating member and extends into the reaction chamber 2 along the axial direction of the stirring shaft 6, and the stirring shaft 6 is connected with the through hole in a sealing way. The stirring of the solid-phase material in the reaction chamber 2 is realized, the full contact between the solid-phase material and the fluorine gas is ensured, the fluorination efficiency is improved, and the complete fluorination is ensured.
Further, the axis of the stirring shaft 6 is perpendicular to the height direction of the reactor 1. It will be appreciated that the agitator shaft 6 is disposed horizontally along the length of the reactor 1 to achieve maximum agitation range. The transmission end of the stirring shaft 6 is arranged in the transmission chamber 3 and is in transmission connection with the output end of the driving part 7, and the stirring end of the stirring shaft 6 is arranged in the reaction chamber 2 and is used for stirring solid-phase materials in the reaction chamber 2. The first isolation plate 8 is provided with a through hole matched with the stirring shaft 6 in installation, and the stirring shaft 6 and the through hole are installed in a dynamic sealing mode so as to prevent fluorine gas from entering the transmission chamber 3 from the reaction chamber 2. It is worth explaining that the stirring end of the stirring shaft 6 is evenly provided with a plurality of groups of blade sets along the axial direction, and each group of blade sets comprises a plurality of blades 14 evenly arranged along the circumferential direction of the stirring shaft 6 so as to ensure the stirring effect on solid-phase materials.
In one embodiment of the present invention, the driving member 7 is disposed outside the reactor 1, the outer wall of the isolation chamber 4 is provided with a mounting hole, the output end of the driving member 7 passes through the mounting hole and is connected with the transmission end of the stirring shaft 6 disposed in the transmission chamber 3, and the output end of the driving member 7 is hermetically connected with the mounting hole. It can be understood that the driving member 7 is disposed at the right side of the reactor 1, the right side wall of the isolation chamber 4 is provided with a mounting hole, and the output end of the driving member 7 passes through the mounting hole and is in dynamic sealing connection with the mounting hole to prevent the sealing liquid 5 from leaking. The output end of the driving piece 7 is in transmission connection with the transmission end of the stirring shaft 6, so that the stirring shaft 6 is driven to rotate.
In one embodiment of the invention, the output end of the driving member 7 is provided with a driving wheel, the driving end of the stirring shaft 6 is provided with a driving wheel, and the isolating member is provided with a long round hole for meshing connection of the driving wheel and the driving wheel. It can be understood that the output end of the driving part 7 is provided with a driving wheel, the driving wheel is immersed in the sealing liquid, and the transmission end of the stirring shaft 6 in the transmission chamber 3 is provided with a transmission wheel. The second isolation plate 9 is provided with a long round hole, the driving wheel passes through the long round hole and is meshed with the driving wheel, and the driving wheel can rotate in the long round hole. It is worth to say that the axis of the driving wheel and the axis of the driving wheel are both arranged along the horizontal direction and are parallel, the opening direction of the long circular hole is perpendicular to the axis of the driving wheel and is arranged horizontally, part of the wheel body of the driving wheel penetrates through the long circular hole and enters the sealing liquid 5, meshing of the driving wheel and the driving wheel is guaranteed, and the driving effect is achieved.
In an embodiment of the present invention, the reaction chamber 2 is communicated with a gas inlet pipe 10, and an inlet end of the gas inlet pipe 10 is provided with a gas heater 11 for heating the gas introduced into the reaction chamber 2 to increase the fluorination rate. In this embodiment, the introduced gas is a mixed gas of fluorine gas and nitrogen gas, and the heater 11 is arranged to preheat the mixed gas, so that the mixed gas reaches the reaction temperature, and the reaction efficiency of the fluorination reaction is ensured. It should be noted that the mixing ratio of fluorine gas and nitrogen gas in the mixed gas and the heating temperature are set according to the nature of the solid phase material in the actual production, and are not illustrated here.
In one embodiment of the present invention, a temperature display is provided in the reaction chamber 2 to monitor the temperature in the reaction chamber 2 in real time. It can be understood that the outer sidewall of the reaction chamber 2 is provided with an observation window for observing the reaction condition in the reaction chamber 2 in real time. For better monitoring the reaction temperature, a temperature display is arranged on the inner wall of the reaction chamber 2 visible by the observation window so as to adjust the heating temperature of the gas heater and ensure that the reaction chamber 2 is at the optimal fluorination reaction temperature.
In one embodiment of the invention, the top side of the reactor 1 is provided with a gas outlet in the height direction of the reactor 1, and the bottom side of the reactor 1 is provided with a solid phase discharge port 13 in the height direction of the reactor 1. It will be appreciated that the top side of the reactor 1 is provided with a gas outlet and is connected to a gas outlet pipe 12 for discharging the off-gas after completion of the reaction out of the reactor 1. The bottom side of the reactor 1 is provided with a solid-phase discharge port 13 for taking out the solid-phase material after fluorination, thereby realizing continuous fluorination production of the reactor 1.
The above-described embodiments of the apparatus are merely illustrative, and the units described as separate parts may or may not be physically separate, and parts displayed as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the modules may be selected according to actual needs to achieve the purpose of the solution of the present embodiment. One of ordinary skill in the art can understand and implement it without inventive effort.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The utility model provides a reaction unit for solid phase surface is fluoridized, a serial communication port, including reactor, stirring piece and driving piece, be equipped with reaction cavity, transmission cavity and isolation cavity in the reactor, the transmission end of stirring piece is established in the transmission cavity, the output of driving piece is established in the isolation cavity, the transmission end of stirring piece with the output transmission of driving piece is connected, be equipped with sealing liquid in the isolation cavity.
2. The reaction device for solid phase surface fluorination of claim 1, wherein a separator for separating the reaction chamber, the transmission chamber and the separation chamber is arranged in the reactor, the separator is connected with the inner wall of the reactor in a sealing way, and the separation chamber is arranged below the transmission chamber along the height direction of the reactor.
3. The reaction device for solid phase surface fluorination of claim 2 wherein said stirring member comprises a stirring shaft, the driving end of said stirring shaft is disposed in said driving chamber, the stirring end of said stirring shaft extends into said reaction chamber through the through hole of said spacer member in the axial direction of said stirring shaft, and said stirring shaft is sealingly connected to said through hole.
4. The reaction device for solid phase surface fluorination of claim 3, wherein said driving member is disposed outside said reactor, a mounting hole is disposed on the outer wall of said isolation chamber, the output end of said driving member passes through said mounting hole and is connected with the driving end of said stirring shaft disposed in said driving chamber, and the output end of said driving member is hermetically connected with said mounting hole.
5. The apparatus according to claim 4, wherein the output end of the driving member is provided with a driving wheel, the driving end of the stirring shaft is provided with a driving wheel, and the separating member is provided with an oblong hole for engaging and connecting the driving wheel and the driving wheel.
6. The reaction device for solid phase surface fluorination of claim 1 wherein the reaction chamber is communicated with a gas inlet pipe, and the inlet end of the gas inlet pipe is provided with a gas heater.
7. The reaction device for solid phase surface fluorination of claim 1 wherein a temperature display is provided in the reaction chamber.
8. The reaction apparatus for solid phase surface fluorination of claim 1 wherein a gas outlet is provided on the top side of the reactor in the height direction of the reactor and a solid phase discharge port is provided on the bottom side of the reactor in the height direction of the reactor.
9. The reaction device for solid phase surface fluorination of claim 2, wherein said spacer comprises a first spacer and a second spacer, said first spacer being disposed along the height direction of said reactor and having the same height as said reactor, said second spacer being disposed along the direction perpendicular to the height direction of said reactor.
10. The reaction device for solid phase surface fluorination of claim 3 wherein the axis of said stirring shaft is perpendicular to the height direction of said reactor.
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