CN212915629U - Reaction device for 3-chloro-4-fluorobenzotrifluoride - Google Patents
Reaction device for 3-chloro-4-fluorobenzotrifluoride Download PDFInfo
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- CN212915629U CN212915629U CN202020973683.XU CN202020973683U CN212915629U CN 212915629 U CN212915629 U CN 212915629U CN 202020973683 U CN202020973683 U CN 202020973683U CN 212915629 U CN212915629 U CN 212915629U
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Abstract
The application belongs to the field of chemical equipment, and relates to a reaction device for 3-chloro-4-fluoro benzotrifluoride, which comprises a reactor, wherein a shaft rotation driving mechanism is arranged on the reactor, the shaft rotation driving mechanism is connected with a reaction stirring paddle through a motor shaft, the reaction stirring paddle is positioned in the reactor, the reaction device also comprises a rectifying device connected with the reactor, the rectifying device is internally provided with a rectifying stirring paddle along the axial direction, and the motor shaft is in transmission connection with the rectifying stirring paddle. The utility model discloses a rectifier unit jointly uses separation 3-chlorine-4-fluorine benzotrifluoride and 3, 4-difluoro benzotrifluoride with the reactor to be provided with the rectification stirring rake in rectifier unit, stir the gas-liquid phase among the rectifier unit and make its abundant contact thereby optimize purification effect and efficiency. The rectification stirring paddle is driven by the rotary driving mechanism of the reactor, so that the operation is convenient and the space is saved.
Description
Technical Field
The utility model belongs to the field of chemical industry equipment, relates to a reaction unit, especially relates to a reaction unit who is used for 3-chlorine-4-fluorine benzotrifluoride.
Background
The molecular formula of the 3-chloro-4-fluorobenzotrifluoride is C7H3ClF4Is a common pesticide intermediate. The 3-chloro-4-fluorotrifluorotoluene is obtained by reacting 3, 4-dichlorotrifluorotoluene with potassium fluoride to perform fluorine substitution, and the reaction is performed under a high-temperature condition. Because the potassium fluoride is excessive in order to improve the conversion rate in the reaction process, the generated product 3-chloro-4-fluorobenzotrifluoride can react with the potassium fluoride to generate the 3, 4-difluorobenzotrifluoride under the high-temperature condition. Since the boiling points of the product 3-chloro-4-fluorotrifluorotoluene and 3, 4-difluorotrifluorotoluene are close to each other, they are difficult to separate by distillation.
For example, chinese patent application [ publication No.: CN102267871A discloses a preparation method of 3-chloro-4-fluorotrifluorotoluene, which is characterized in that the preparation method comprises the fluorination reaction of 3, 4-dichlorotrifluorotoluene and anhydrous potassium fluoride in a polar aprotic solvent in the presence of a catalyst, wherein the catalyst contains a copper halide and a crown ether. After the fluorination reaction is finished, rectification under reduced pressure is carried out.
In the technical scheme, although a mode of adopting the reduced pressure rectification to extract the product is provided, no specific matched equipment is provided, the efficiency is lower by adopting the traditional rectification device, and the yield of the product is low.
Disclosure of Invention
The present application aims to solve the above problems and provide a reaction apparatus for 3-chloro-4-fluorobenzotrifluoride.
In order to achieve the above purpose, the utility model adopts the following technical proposal:
the application creatively provides a reaction device for 3-chloro-4-fluorobenzotrifluoride, which comprises a reactor, wherein a shaft rotation driving mechanism is arranged on the reactor, the shaft rotation driving mechanism is connected with a reaction stirring paddle through a motor shaft, the reaction stirring paddle is positioned in the reactor, and the reaction device is characterized in that: the reactor also comprises a rectifying device connected with the reactor, wherein a rectifying stirring paddle is arranged in the rectifying device along the axial direction, and a motor shaft is in transmission connection with the rectifying stirring paddle.
In the above reaction apparatus for 3-chloro-4-fluorotrifluorotoluene, the rectifying apparatus comprises a rectifying tower body, wherein a plurality of layers of tower plates are horizontally arranged in the rectifying tower body at intervals, the rectifying stirring paddle comprises a rectifying stirring shaft and a plurality of groups of rectifying stirring blades arranged on the rectifying stirring shaft, and the rectifying stirring blades are arranged between two adjacent tower plates.
In the above reaction apparatus for 3-chloro-4-fluorotrifluorotoluene, the rectifying stirring blades in each group of rectifying stirring blades are uniformly arranged along the circumference of the rectifying stirring shaft, and a plurality of liquid flow holes are arranged on the rectifying stirring blades at intervals.
In the above-mentioned reaction apparatus for 3-chloro-4-fluorotrifluorotoluene, the lower end edge of the rectifying and stirring blade is corrugated.
In the above-mentioned reaction apparatus for 3-chloro-4-fluorobenzotrifluoride, the corrugated edge at the lower end of the rectifying stirring blade is composed of a plurality of alternately arranged grooves and protrusions, each protrusion of the rectifying stirring blade is arranged in one-to-one correspondence with the liquid flow holes, and the liquid flow holes are oval with major diameters arranged along the horizontal direction.
In the above reaction apparatus for 3-chloro-4-fluorotrifluorotoluene, at least two of the following transmission connection modes of the motor shaft and the rectification stirring paddle are adopted:
the rectification stirring paddle is characterized in that a driving wheel is fixedly arranged on a motor shaft along the axial direction, a driven wheel is fixedly arranged on the rectification stirring paddle along the axial direction, and the driven wheel is in transmission connection with the driving wheel through a toothed chain or a gear set.
Preferably, the gear set comprises a small gear in meshing transmission connection with the driving wheel and a large gear connected with the small gear, the large gear is in meshing transmission connection with the driven wheel, and the diameter of the large gear is larger than that of the small gear.
And secondly, the shaft rotation driving mechanism is a double-shaft motor with two motor shafts, one of the two motor shafts is connected with the reaction stirring paddle, and the other motor shaft is connected with the rectification stirring paddle.
In the above reaction device for 3-chloro-4-fluorobenzotrifluoride, the middle section of the rectifying tower body is provided with a feed inlet, the top end of the rectifying tower body is provided with a gas outlet and a reflux port, the gas outlet is connected with the inlet of a condenser through a pipeline, the outlet of the condenser is connected with the inlet of a reflux tank through a pipeline, the reflux tank is respectively connected with the reflux port and a top product tank, the bottom of the rectifying tower body is provided with a liquid outlet and a gas return port, the liquid outlet is connected with the inlet of a reboiler, the reboiler is connected with the gas return port, and the bottom of the rectifying tower body is also connected with a bottom product tank.
In the reaction device for 3-chloro-4-fluorotrifluorotoluene, the rectification stirring shaft is rotationally connected with the interlayer tower plate.
Compared with the prior art, the application has the advantages that:
1. the utility model discloses a rectifier unit jointly uses separation 3-chlorine-4-fluorine benzotrifluoride and 3, 4-difluoro benzotrifluoride with the reactor to be provided with the rectification stirring rake in rectifier unit, stir the gas-liquid phase among the rectifier unit and make its abundant contact thereby optimize purification effect and efficiency. The rectification stirring paddle is driven by the rotary driving mechanism of the reactor, so that the operation is convenient and the space is saved.
2. The rectification stirring blades are provided with liquid flow holes and wavy edges, can reduce resistance, increase stirring depth, are suitable for the rectification tower body, form special turbulence on fluid, increase the handling capacity of the unit sectional area of the rectification tower body and improve the mass transfer effect.
3. In one embodiment, the reduction is carried out by matching a large gear with a small gear, so as to control the reasonable rotating speed ratio of the rectification stirring paddle to the reaction stirring paddle.
4. The utility model discloses mainly design to the lab scale stage, practiced thrift the energy, simple structure has optimized the purification process in the 3-chlorine-4-fluorine benzotrifluoride synthetic process.
Drawings
Fig. 1 is a block diagram provided in the present application.
Fig. 2 is another block diagram provided in the present application.
Fig. 3 is a partial block diagram provided in the present application.
In the figure, a reactor 1, a shaft rotation driving mechanism 10, a motor shaft 11, a driving wheel 110, a reaction stirring paddle 12, a rectifying device 2, a rectifying tower body 20, a tower plate 200, a feed inlet 201, an air outlet 202, a reflux inlet 203, a liquid outlet 204, a gas return opening 205, a rectifying stirring paddle 21, a rectifying stirring shaft 210, a rectifying stirring blade 211, a liquid flow hole 212, a driven wheel 213, a gear set 3, a pinion 30, a bull gear 31, a condenser 4, a reflux tank 5 and a reboiler 6.
Detailed Description
Further illustrated by the following specific examples;
example one
As shown in figure 1, the reaction device for 3-chloro-4-fluorotrifluorotoluene comprises a reactor 1, wherein a shaft rotation driving mechanism 10 is arranged on the reactor 1, the shaft rotation driving mechanism 10 is connected with a reaction stirring paddle 12 through a motor shaft 11, the reaction stirring paddle 12 is positioned in the reactor 1, the reaction device also comprises a rectification device 2 connected with the reactor 1, the rectification stirring paddle 21 is arranged in the rectification device 2 along the axial direction, and the motor shaft 11 is in transmission connection with the rectification stirring paddle 21. A rectification stirring paddle 21 is arranged in the rectification device 2, and gas and liquid phases in the rectification device 2 are stirred to be fully contacted, so that the purification effect and efficiency are optimized.
The motor shaft 11 is axially and fixedly provided with a driving wheel 110, the rectification stirring paddle 21 is axially and fixedly provided with a driven wheel 213, and the driven wheel 213 is in transmission connection with the driving wheel 110 through a gear set 3.
Specifically, the gear set 3 includes a small gear 30 in meshing transmission connection with the driving wheel 110 and a large gear 31 connected with the small gear 30, the large gear 31 and the small gear 30 are both connected to the base through a gear shaft, the large gear 31 is in meshing transmission connection with the driven wheel 213, and the diameter of the large gear 31 is larger than that of the small gear 30. Preferably, the diameter ratio of the large gear 31 to the small gear 30 is 10: 1-5: 1, so as to achieve the effect of speed reduction.
The rectifying device 2 comprises a rectifying tower body 20, and a feeding hole 201 is arranged at the middle section of the rectifying tower body 20. The top end of the rectifying tower body 20 is provided with an air outlet 202 and a reflux opening 203, the air outlet 202 is connected with the inlet of the condenser 4 through an air outlet pipe, the outlet of the condenser 4 is connected with the inlet of the reflux tank 5 through a condenser outlet pipe, the reflux tank 5 is provided with two outlets, and the two outlets of the reflux tank 5 are respectively connected with the reflux opening 203 and a top product tank (not shown in the figure) for collecting light component products. The bottom of rectifying column body 20 has liquid outlet 204 and gas return port 205, and liquid outlet 204 passes through the entry of drain pipe connection reboiler 6, and reboiler 6 passes through gas outlet connection gas return port 205, and the bottom of rectifying column body 20 still is connected with bottom product jar (not shown in the figure) through the bottom discharging pipe for collect heavy ends product.
In this embodiment, the rectifying tower body 20 is a rectifying tower with commercially available trays, the rectifying tower body 20 is internally provided with a plurality of trays 200 at horizontal intervals, the rectifying stirring paddle 21 comprises a rectifying stirring shaft 210 and a plurality of groups of rectifying stirring blades 211 arranged on the rectifying stirring shaft 210, and the rectifying stirring blades 211 are arranged between two adjacent trays 200. The rectification stirring shaft 210 is axially and rotationally connected with the interlayer tray 200 through a bearing or other shaft rotating connection parts.
It should be understood by those skilled in the art that the design of the number of plates of the rectifying column body 20, the temperatures at the top and bottom of the rectifying column, the feeding temperature, the reflux ratio, the position of the feeding port, etc. is calculated according to the parameters such as the composition of the actual material and the feeding amount, and will not be described herein.
As shown in fig. 3, each group of rectifying stirring vanes 211 has 3 to 5 rectifying stirring vanes 211, each rectifying stirring vane 211 is uniformly arranged along the circumference of the rectifying stirring shaft 210, and a plurality of liquid flow holes 212 are arranged on the rectifying stirring vanes 211 at intervals. The lower end edge of the rectifying stirring blade 211 is corrugated. The corrugated edge at the lower end of the rectifying stirring blade 211 is composed of a plurality of grooves and protrusions which are alternately arranged, each protrusion of the rectifying stirring blade 211 is arranged in one-to-one correspondence with the liquid flow hole 212, and the liquid flow hole 212 is oval with the major diameter arranged along the horizontal direction. The resistance can be reduced, the stirring depth is increased, the stirring device is suitable for the rectifying tower body, a special turbulent flow is formed on the fluid, the handling capacity of the unit sectional area of the rectifying tower body is increased, and the mass transfer effect is improved.
The reactor 1 comprises a shell, a shaft rotation driving mechanism 10 is arranged on the outer side of the shell and drives a reaction stirring paddle 12 in the shell to rotate, an inlet and an outlet are arranged on the reactor 1, the reactor 1 is connected with a feeding hole 201 of a rectifying tower body 20 through the outlet, and devices such as a heater for heating the inside of the shell and a vacuum pump for reducing pressure are arranged on the reactor 1. The shaft rotation driving mechanism 10 is specifically a rotating electric machine. The structure and principle of the reactor 1 and the rotating electrical machine are well known in the art and will not be described herein.
Example two
As shown in fig. 2, this embodiment is substantially the same as the first embodiment except that the shaft rotation driving mechanism 10 is a biaxial motor having two motor shafts 11, one of the two motor shafts 11 is connected to the reaction stirring paddle 12, and the other is connected to the rectifying stirring paddle 21. The occupation of space is reduced, and the energy consumption is reduced.
It should be understood by those skilled in the art that the two-shaft motor is a commercially available product, and the structure of the two-shaft motor adopted in the present embodiment is disclosed in the chinese utility model patent No. CN201720550202.2, and is not described herein.
EXAMPLE III
The embodiment is basically the same as the first embodiment, except that the driven wheel and the driving wheel are connected through a toothed chain transmission.
The working principle of the utility model is as follows:
starting a shaft rotation driving mechanism 10, putting reactants of sulfolane, potassium fluoride, a catalyst and 3, 4-dichlorotrifluorotoluene into a reactor 1, rectifying a product produced after the reactants react in the reactor 1 by a rectifying device 2 in time to obtain, and synchronously operating a reaction stirring paddle 12 and a rectifying stirring paddle 21 to accelerate gas-liquid contact, thereby improving the conversion rate of the reaction.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications, additions and substitutions for the specific embodiments described herein may be made by those skilled in the art without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.
Although the terms of reactor 1, shaft rotation driving mechanism 10, motor shaft 11, driving wheel 110, reaction stirring paddle 12, rectifying device 2, rectifying column body 20, tower plate 200, feed inlet 201, gas outlet 202, reflux inlet 203, liquid outlet 204, gas return 205, rectifying stirring shaft 210, rectifying stirring blade 211, liquid flow hole 212, driven wheel 213, pinion 30, bull gear 31, condenser 4, reflux drum 5, reboiler 6, etc. are used more herein, the possibility of using other terms is not excluded. These terms are used merely to more conveniently describe and explain the nature of the present invention and should not be interpreted as imposing any additional limitations that are contrary to the spirit of the present invention.
Claims (10)
1. A reaction device for 3-chloro-4-fluorobenzotrifluoride, which comprises a reactor (1), wherein a shaft rotation driving mechanism (10) is arranged on the reactor (1), the shaft rotation driving mechanism (10) is connected with a reaction stirring paddle (12) through a motor shaft (11), the reaction stirring paddle (12) is positioned in the reactor (1), and the reaction device is characterized in that: still include rectifier unit (2) of being connected with reactor (1), be provided with rectification stirring rake (21) along the axial in rectifier unit (2), motor shaft (11) are connected with rectification stirring rake (21) transmission.
2. The reaction apparatus for 3-chloro-4-fluorotrifluorotoluene according to claim 1, wherein: the rectifying device (2) comprises a rectifying tower body (20), wherein a plurality of layers of tower plates (200) are horizontally arranged in the rectifying tower body (20) at intervals, the rectifying stirring paddle (21) comprises a rectifying stirring shaft (210) and a plurality of groups of rectifying stirring blades (211) arranged on the rectifying stirring shaft (210), and the rectifying stirring blades (211) are arranged between two adjacent tower plates (200).
3. The reaction apparatus for 3-chloro-4-fluorotrifluorotoluene according to claim 2, wherein: each rectification stirring blade (211) in each group of rectification stirring blades (211) is uniformly arranged along the circumferential direction of the rectification stirring shaft (210), and a plurality of liquid flow holes (212) are arranged on the rectification stirring blades (211) at intervals.
4. The reaction apparatus for 3-chloro-4-fluorotrifluorotoluene according to claim 3, wherein: the lower end edge of the rectification stirring blade (211) is corrugated.
5. The reaction apparatus for 3-chloro-4-fluorotrifluorotoluene according to claim 4, wherein: the corrugated edge at the lower end of the rectification stirring blade (211) is composed of a plurality of grooves and protrusions which are alternately arranged, each protrusion of the rectification stirring blade (211) is arranged in one-to-one correspondence with the liquid flow hole (212), and the liquid flow hole (212) is oval with a long diameter arranged along the horizontal direction.
6. The reaction apparatus for 3-chloro-4-fluorotrifluorotoluene according to claim 1, wherein: the motor shaft (11) is axially and fixedly provided with a driving wheel (110), the rectification stirring paddle (21) is axially and fixedly provided with a driven wheel (213), and the driven wheel (213) is in transmission connection with the driving wheel (110) through a toothed chain or a gear set (3).
7. The reaction apparatus for 3-chloro-4-fluorotrifluorotoluene according to claim 6, wherein: the gear set (3) comprises a small gear (30) in meshing transmission connection with the driving wheel (110) and a large gear (31) connected with the small gear (30), the large gear (31) is in meshing transmission connection with the driven wheel (213), and the diameter of the large gear (31) is larger than that of the small gear (30).
8. The reaction apparatus for 3-chloro-4-fluorotrifluorotoluene according to claim 1, wherein: the shaft rotation driving mechanism (10) is a double-shaft motor with two motor shafts (11), one of the two motor shafts (11) is connected with the reaction stirring paddle (12), and the other is connected with the rectification stirring paddle (21).
9. The reaction apparatus for 3-chloro-4-fluorotrifluorotoluene according to claim 2, wherein: the middle section of rectifying column body (20) is equipped with feed inlet (201), and the top of rectifying column body (20) has gas outlet (202) and backward flow mouth (203), gas outlet (202) are through the entry linkage of pipeline with condenser (4), and the entry of tube coupling backward flow jar (5) is passed through in the export of this condenser (4), and backward flow mouth (203) and top product jar are connected respectively in this backward flow jar (5), and the bottom of rectifying column body (20) has liquid outlet (204) and gas return mouth (205), the entry of reboiler (6) is connected in liquid outlet (204), gas return mouth (205) is connected in reboiler (6), the bottom of rectifying column body (20) still is connected with bottom product jar.
10. The reaction apparatus for 3-chloro-4-fluorotrifluorotoluene according to claim 3, wherein: the rectifying stirring shaft (210) is rotationally connected with the interlayer tower plate (200).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202020973683.XU CN212915629U (en) | 2020-06-01 | 2020-06-01 | Reaction device for 3-chloro-4-fluorobenzotrifluoride |
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| CN202020973683.XU CN212915629U (en) | 2020-06-01 | 2020-06-01 | Reaction device for 3-chloro-4-fluorobenzotrifluoride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115055144A (en) * | 2022-07-15 | 2022-09-16 | 常州新东化工发展有限公司 | System and process for producing o-chlorotrifluoromethylene |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115055144A (en) * | 2022-07-15 | 2022-09-16 | 常州新东化工发展有限公司 | System and process for producing o-chlorotrifluoromethylene |
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