CN115646402A - Processing system and method for 2, 4-difluorobenzophenone - Google Patents
Processing system and method for 2, 4-difluorobenzophenone Download PDFInfo
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- CN115646402A CN115646402A CN202211115015.3A CN202211115015A CN115646402A CN 115646402 A CN115646402 A CN 115646402A CN 202211115015 A CN202211115015 A CN 202211115015A CN 115646402 A CN115646402 A CN 115646402A
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Abstract
The invention discloses a processing system and a processing method for 2, 4-difluorobenzophenone, which comprise a reaction kettle, a hydrolysis kettle, a water washing refining kettle and a distillation kettle, wherein the reaction kettle, the hydrolysis kettle, the water washing refining kettle and the distillation kettle are sequentially processed, and feeding is carried out between every two kettles through vacuum pumping equipment; the reaction kettle comprises a tank body, a top cover and a stirring mechanism, wherein the top cover is arranged at the top of the tank body. The reaction kettle of the processing system is provided with the stirring mechanism, the stirring mechanism is provided with the forward rotation stirring paddle which rotates forward along with the stirring rod, the reverse rotation stirring paddle rotates reversely through the transmission of the lower fluted disc, the gear and the upper fluted disc, the reaction kettle stirs raw materials through the forward rotation stirring paddle and the reverse rotation stirring paddle to form convection so as to fully stir and react the raw materials, the problem that the raw materials are not fully stirred and the reaction of the raw materials is not complete in the reaction kettle in the existing processing system is solved, and the preparation efficiency of the 2, 4-difluorobenzophenone is improved.
Description
Technical Field
The invention relates to the technical field of 2, 4-difluorobenzophenone processing, in particular to a processing system and a processing method for 2, 4-difluorobenzophenone.
Background
2, 4-difluorobenzophenone is used as an intermediate of pesticide flutriafol and is prepared by taking fluorobenzene, aluminum trichloride and o-fluorobenzoyl chloride as raw materials, firstly adding fluorobenzene and aluminum trichloride into a reaction kettle, dropwise adding the o-fluorobenzoyl chloride at 20-50 ℃, keeping the temperature and stirring until the reaction is finished, and then hydrolyzing, layering, washing and distilling to obtain the 2, 4-difluorobenzophenone.
The core of preparing 2, 4-difluorobenzophenone is a part of fluorobenzene, aluminum trichloride and o-fluorobenzoyl chloride which react in a reaction kettle, a stirring structure of the reaction kettle in a traditional processing system is composed of a stirring motor, a stirring rod and a stirring paddle, the effect of stirring raw materials by driving the stirring rod and the stirring paddle to rotate in a single direction through the stirring motor is poor, the raw materials in the reaction kettle are probably not stirred sufficiently, so that the raw materials are not reacted completely, and the preparation efficiency of the 2, 4-difluorobenzophenone is influenced, therefore, the processing system which is provided with the reaction kettle capable of stirring sufficiently and used for the 2, 4-difluorobenzophenone is required to solve the problems.
Disclosure of Invention
The invention aims to provide a processing system and a processing method for 2, 4-difluorobenzophenone, and aims to solve the problems that a stirring structure of a reaction kettle in the traditional processing system proposed in the background technology is composed of a stirring motor, a stirring rod and a stirring paddle, the effect of stirring raw materials by driving the stirring rod and the stirring paddle to rotate in a single direction through the stirring motor is poor, the raw materials in the reaction kettle are possibly not stirred sufficiently, so that the raw materials react incompletely, and the preparation efficiency of the 2, 4-difluorobenzophenone is influenced.
In order to achieve the purpose, the invention provides the following technical scheme: a processing system for 2, 4-difluorobenzophenone comprises a reaction kettle, a hydrolysis kettle, a water washing refining kettle and a distillation kettle, wherein the reaction kettle, the hydrolysis kettle, the water washing refining kettle and the distillation kettle are sequentially processed, and feeding is carried out between every two kettles through vacuum pumping equipment;
the reactor comprises a tank body, a top cover and a stirring mechanism, wherein the top cover is arranged at the top of the tank body, the stirring mechanism comprises a stirring rod of a stirring motor, the stirring motor, a forward rotation stirring paddle and a reverse rotation stirring paddle, the stirring motor is arranged at the middle part of the top cover, and the forward rotation stirring paddle and the reverse rotation stirring paddle are respectively arranged on the upper side and the lower side of the stirring rod so as to be used for fully stirring raw materials in the reactor.
Furthermore, the processing system further comprises a falling film absorption tower and an alkaline washing absorption tower, wherein the falling film absorption tower and the alkaline washing absorption tower sequentially treat tail gas of the reaction kettle, and the reaction kettle, the falling film absorption tower and the alkaline washing absorption tower are all supplied with air through vacuum air pumping equipment.
Further, rabbling mechanism still includes fluted disc, lower fluted disc, two gears and bears the frame reverse the stirring rake and install in the both sides of last fluted disc, and go up the fluted disc cover and establish in the puddler outside, the fluted disc is fixed on the puddler and is located the below of last fluted disc down, the both sides of bearing the frame all are provided with the circle axle, two the gear rotates respectively to be connected on the circle axle of bearing the frame, and this gear engagement sets up between last fluted disc and lower fluted disc, bear the frame and fix the inner wall at the jar body.
Furthermore, the stirring rod is fixedly connected with the forward rotation stirring paddle, when the stirring motor drives the stirring rod to rotate, the forward rotation stirring paddle rotates forward along with the stirring rod, and the reverse stirring paddle realizes reverse rotation through the lower fluted disc, the gear and the upper fluted disc.
Furthermore, the stirring rod is further provided with a limiting block above the lower fluted disc, and the upper fluted disc is sleeved outside the limiting block of the stirring rod.
Furthermore, the upper fluted disc and the lower fluted disc are both provided with teeth which are uniformly distributed in an annular array, and the teeth of the upper fluted disc and the teeth of the lower fluted disc are arranged oppositely.
Furthermore, the teeth of the upper fluted disc, the teeth of the lower fluted disc and the teeth of the gears are all arranged in a meshing manner.
Furthermore, the forward rotation stirring paddle and the reverse rotation stirring paddle are both of an X-shaped structure.
Further, the bottom of the jar body is provided with the discharge gate, one side of top cap is provided with the feed inlet, the opposite side of top cap is provided with the gas vent, and the gas vent is connected with vacuum pumping equipment and imports the falling liquid film absorption tower with gas.
A process for the manufacture of 2, 4-difluorobenzophenone comprising the steps of:
starting a stirring mechanism of the reaction kettle, operating a stirring motor and driving a stirring rod to rotate, driving a forward rotation stirring paddle and a lower fluted disc to rotate forward by the stirring rod, driving the lower fluted disc by a gear, and reversely rotating an upper fluted disc and a reverse rotation stirring paddle;
step (B), the raw materials for processing the 2, 4-difluorobenzophenone are fluorobenzene, aluminum trichloride and o-fluorobenzoyl chloride, the fluorobenzene and the aluminum trichloride are metered and then added into a reaction kettle for stirring, the reaction kettle stirs the raw materials through a forward stirring paddle and a reverse stirring paddle to form convection so that the raw materials are fully stirred and reacted, then the o-fluorobenzoyl chloride is slowly dripped at the temperature of 20-50 ℃, the temperature is kept at 35-36 ℃ for a period of time until the reaction is finished, and a crude product of the 2, 4-difluorobenzophenone is prepared;
inputting tail gas generated in the reaction kettle into a falling film absorption tower through vacuum pumping equipment to obtain a 30% byproduct hydrochloric acid, and absorbing the tail gas through an alkaline washing absorption tower;
conveying the 2, 4-difluorobenzophenone crude product to a hydrolysis kettle through vacuum pumping equipment, adding hydrochloric acid and water into the hydrolysis kettle, and layering to obtain an aluminum hydroxide aqueous solution and a material hydrolyzed by the 2, 4-difluorobenzophenone;
step (E), conveying the hydrolyzed material of the 2, 4-difluorobenzophenone to a washing refining kettle, and adding water to wash for two times to obtain a material of the 2, 4-difluorobenzophenone after washing;
and (F) conveying the material washed by the 2, 4-difluorobenzophenone into a distillation still, slowly heating the distillation still, distilling the material washed by the 2, 4-difluorobenzophenone, and ending the distillation when no distillate is at the top of the distillation still to obtain the 2, 4-difluorobenzophenone product.
Compared with the prior art, the invention has the beneficial effects that:
the reaction kettle of the processing system is provided with the stirring mechanism, the stirring mechanism is provided with the forward rotation stirring paddle which rotates along with the stirring rod in the forward direction, the reverse rotation stirring paddle rotates in the reverse direction through the transmission of the lower fluted disc, the gear and the upper fluted disc, the reaction kettle stirs raw materials through the forward rotation stirring paddle and the reverse rotation stirring paddle to form convection so that the raw materials are fully stirred and reacted, the problem that the raw materials are not fully stirred in the reaction kettle in the existing processing system to cause incomplete reaction of the raw materials is solved, and the preparation efficiency of the 2, 4-difluorobenzophenone is improved.
Drawings
FIG. 1 is a block diagram of the present invention;
FIG. 2 is a schematic perspective view of the inside of the reaction vessel according to the present invention;
FIG. 3 is a schematic view of a front view of a stirring mechanism of a reaction kettle according to the present invention;
FIG. 4 is a schematic perspective view of a stirring mechanism of a reaction vessel according to the present invention;
FIG. 5 is a schematic perspective view of the connection between the contra-rotating stirring paddle and the upper fluted disc of the present invention;
FIG. 6 is a perspective view of the gear of the present invention mounted on the carriage;
FIG. 7 is an enlarged view of the structure at A in FIG. 2 according to the present invention;
FIG. 8 is an enlarged view of the structure at B in FIG. 3 according to the present invention.
In the figure: 1. a tank body; 11. a discharge port; 2. a top cover; 21. a feed inlet; 22. an exhaust port; 3. a stirring mechanism; 31. a stirring motor; 32. a stirring rod; 321. a limiting block; 33. a forward rotation stirring paddle; 34. reversing the stirring paddle; 35. an upper fluted disc; 36. a lower fluted disc; 37. a gear; 38. a carrier; 381, round axis.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Referring to fig. 1-8, the present invention provides a technical solution: a processing system for 2, 4-difluorobenzophenone comprises a reaction kettle, a hydrolysis kettle, a water washing refining kettle and a distillation kettle, wherein the reaction kettle, the hydrolysis kettle, the water washing refining kettle and the distillation kettle are sequentially processed, residual liquid and solid waste are required to be treated after distillation of the distillation kettle, and feeding is carried out between every two kettles through vacuum pumping equipment;
the reaction kettle comprises a tank body 1, a top cover 2 and a stirring mechanism 3, wherein the top cover 2 is arranged at the top of the tank body 1, the stirring mechanism 3 comprises a stirring motor 31, a stirring rod 32 of the stirring motor 31, a forward rotation stirring paddle 33 and a reverse rotation stirring paddle 34, the stirring motor 31 is arranged in the middle of the top cover 2, and the forward rotation stirring paddle 33 and the reverse rotation stirring paddle 34 are respectively arranged on the upper side and the lower side of the stirring rod 32 so as to be used for fully stirring raw materials in the reaction kettle.
In this embodiment, as shown in fig. 1, the processing system further includes a falling film absorption tower and an alkaline washing absorption tower, the falling film absorption tower and the alkaline washing absorption tower sequentially treat the exhaust gas of the reaction kettle, the falling film absorption tower and the alkaline washing absorption tower treat the exhaust gas and then need to treat the sewage, and the reaction kettle, the falling film absorption tower and the alkaline washing absorption tower are all supplied with air through vacuum air pumping equipment.
In this embodiment, as shown in fig. 3, 4, and 8, the stirring mechanism 3 further includes an upper fluted disc 35, a lower fluted disc 36, two gears 37, and a supporting frame 38, and the reverse stirring paddle 34 is installed on two sides of the upper fluted disc 35, the upper fluted disc 35 is sleeved outside the stirring rod 32, the lower fluted disc 36 is fixed on the stirring rod 32 and located below the upper fluted disc 35, circular shafts 381 are respectively disposed on two sides of the supporting frame 38, the two gears 37 are respectively rotatably connected to the circular shafts 381 of the supporting frame 38, the gears 37 are engaged and disposed between the upper fluted disc 35 and the lower fluted disc 36, and the supporting frame 38 is fixed on the inner wall of the tank 1.
In this embodiment, puddler 32 and corotation stirring rake 33 fixed connection, when agitator motor 31 drive puddler 32 rotated, corotation stirring rake 33 rotated along with the puddler 32 forward, and the contrarotation stirring rake 34 realized reverse rotation through lower fluted disc 36, gear 37 and last fluted disc 35, and this reation kettle stirs the raw materials of downside through corotation stirring rake 33 forward, stirs the raw materials of upside through the contrarotation stirring rake 34 reverse, makes it form the convection current thereby fully stirring the raw materials.
In this embodiment, as shown in fig. 4, a limiting block 321 is further disposed above the lower fluted disc 36 of the stirring rod 32, the upper fluted disc 35 is sleeved outside the limiting block 321 of the stirring rod 32, and the upper fluted disc 35 is limited by the limiting block 321, so that the upper fluted disc 35 rotates at a fixed position.
In the present embodiment, as shown in fig. 4, the upper toothed disc 35 and the lower toothed disc 36 are both provided with uniformly distributed teeth in an annular array, and the teeth of the upper toothed disc 35 are disposed opposite to the teeth of the lower toothed disc 36.
In this embodiment, the teeth of the upper gear 35, the teeth of the lower gear 36, and the teeth of the gear 37 are all engaged, so that when the stirring rod 32 drives the lower gear 36 to rotate, the lower gear 36 can drive the gear 37 to rotate, and the gear 37 drives the upper gear 35 to rotate reversely.
In the present embodiment, as shown in fig. 4, the forward rotation paddles 33 and the reverse rotation paddles 34 are both provided in an X-shaped configuration.
In the embodiment, as shown in fig. 2, a discharge port 11 is arranged at the bottom of the tank body 1, a feed port 21 is arranged at one side of the top cover 2, an exhaust port 22 is arranged at the other side of the top cover 2, and the exhaust port 22 is connected with a vacuum pumping device to input gas into the falling film absorption tower.
A process for the manufacture of 2, 4-difluorobenzophenone comprising the steps of:
step (A), starting a stirring mechanism 3 of the reaction kettle, wherein a stirring motor 31 runs and drives a stirring rod 32 to rotate, the stirring rod 32 drives a forward rotation stirring paddle 33 and a lower fluted disc 36 to rotate forward, the lower fluted disc 36 is driven by a gear 37, and an upper fluted disc 35 and a reverse rotation stirring paddle 34 rotate reversely;
step (B), the raw materials for processing the 2, 4-difluorobenzophenone are fluorobenzene, aluminum trichloride and o-fluorobenzoyl chloride, the fluorobenzene and the aluminum trichloride are metered and then added into a reaction kettle for stirring, the reaction kettle stirs the raw materials through a forward stirring paddle 33 and a reverse stirring paddle 34 to form convection so that the raw materials are fully stirred and reacted, then the o-fluorobenzoyl chloride is slowly dripped at the temperature of between 20 and 50 ℃, the temperature is kept at between 35 and 36 ℃ for a period of time until the reaction is finished, and a crude product of the 2, 4-difluorobenzophenone is prepared;
inputting tail gas generated in the reaction kettle into a falling film absorption tower through vacuum pumping equipment to obtain a 30% byproduct hydrochloric acid, and absorbing the tail gas through an alkaline washing absorption tower;
conveying the 2, 4-difluorobenzophenone crude product to a hydrolysis kettle through vacuum material pumping equipment, adding hydrochloric acid and water into the hydrolysis kettle, and layering to obtain an aluminum hydroxide aqueous solution and a hydrolyzed material of the 2, 4-difluorobenzophenone;
step (E), conveying the hydrolyzed material of the 2, 4-difluorobenzophenone to a washing refining kettle, and adding water to wash for two times to obtain a material of the 2, 4-difluorobenzophenone after washing;
and (F) conveying the material washed by the 2, 4-difluorobenzophenone into a distillation still, slowly heating the distillation still, distilling the material washed by the 2, 4-difluorobenzophenone, and ending the distillation when no distillate is at the top of the distillation still to obtain the 2, 4-difluorobenzophenone product.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A processing system for 2, 4-difluorobenzophenone, characterized by: the device comprises a reaction kettle, a hydrolysis kettle, a washing refining kettle and a distillation kettle, wherein the reaction kettle, the hydrolysis kettle, the washing refining kettle and the distillation kettle are sequentially processed, and feeding is carried out between every two kettles through vacuum pumping equipment;
the reaction kettle comprises a tank body (1), a top cover (2) and a stirring mechanism (3), wherein the top cover (2) is installed at the top of the tank body (1), the stirring mechanism (3) comprises a stirring rod (32) of a stirring motor (31), the stirring motor (31), a forward rotation stirring paddle (33) and a reverse rotation stirring paddle (34), the stirring motor (31) is arranged in the middle of the top cover (2), and the forward rotation stirring paddle (33) and the reverse rotation stirring paddle (34) are respectively arranged on the upper side and the lower side of the stirring rod (32) so as to be used for fully stirring raw materials in the reaction kettle.
2. A processing system for 2, 4-difluorobenzophenone as in claim 1 wherein: the processing system further comprises a falling film absorption tower and an alkaline washing absorption tower, wherein the falling film absorption tower and the alkaline washing absorption tower sequentially treat tail gas of the reaction kettle, and gas is supplied among the reaction kettle, the falling film absorption tower and the alkaline washing absorption tower through vacuum gas extraction equipment.
3. A processing system for 2, 4-difluorobenzophenone as in claim 1 wherein: rabbling mechanism (3) still include fluted disc (35), lower fluted disc (36), two gears (37) and bear frame (38), reverse stirring rake (34) and install the both sides at last fluted disc (35), and go up fluted disc (35) cover and establish the puddler (32) outside, fluted disc (36) are fixed on puddler (32) and are located the below of fluted disc (35) down, the both sides of bearing frame (38) all are provided with round axle (381), two gear (37) rotate respectively and connect on round axle (381) of bearing frame (38), and this gear (37) meshing sets up between last fluted disc (35) and lower fluted disc (36), bear frame (38) and fix the inner wall at jar body (1).
4. A processing system for 2, 4-difluorobenzophenone as in claim 3, wherein: the stirring rod (32) is fixedly connected with the forward rotation stirring paddle (33), when the stirring motor (31) drives the stirring rod (32) to rotate, the forward rotation stirring paddle (33) rotates forward along with the stirring rod (32), and the reverse rotation stirring paddle (34) realizes reverse rotation through the lower fluted disc (36), the gear (37) and the upper fluted disc (35).
5. A processing system for 2, 4-difluorobenzophenone as in claim 3, wherein: the stirring rod (32) is located the top of fluted disc (36) down and still is provided with stopper (321), go up fluted disc (35) cover and establish stopper (321) outside at stirring rod (32).
6. A processing system for 2, 4-difluorobenzophenone as in claim 3, wherein: go up fluted disc (35) and lower fluted disc (36) and all be provided with the tooth of annular array evenly distributed, the tooth of going up fluted disc (35) sets up with the tooth of lower fluted disc (36) is relative.
7. A processing system for 2, 4-difluorobenzophenone as in claim 6 wherein: the teeth of the upper fluted disc (35), the teeth of the lower fluted disc (36) and the teeth of the gear (37) are all arranged in a meshed mode.
8. A processing system for 2, 4-difluorobenzophenone as in claim 1 wherein: the forward rotation stirring paddle (33) and the reverse rotation stirring paddle (34) are both of X-shaped structures.
9. A processing system for 2, 4-difluorobenzophenone as in claim 1 wherein: the bottom of the jar body (1) is provided with discharge gate (11), one side of top cap (2) is provided with feed inlet (21), the opposite side of top cap (2) is provided with gas vent (22), and gas vent (22) are connected with vacuum pumping equipment and import falling liquid film absorption tower with gas.
10. A process for the preparation of 2, 4-difluorobenzophenone according to any of claims 1 to 9, characterized in that: the method comprises the following steps:
step (A), starting a stirring mechanism (3) of the reaction kettle, enabling a stirring motor (31) to operate and drive a stirring rod (32) to rotate, enabling the stirring rod (32) to drive a forward rotation stirring paddle (33) and a lower fluted disc (36) to rotate forward, enabling the lower fluted disc (36) to be driven through a gear (37), and enabling an upper fluted disc (35) and a reverse rotation stirring paddle (34) to rotate reversely;
step (B), the raw materials for processing the 2, 4-difluorobenzophenone are fluorobenzene, aluminum trichloride and o-fluorobenzoyl chloride, the fluorobenzene and the aluminum trichloride are metered and then added into a reaction kettle for stirring, the reaction kettle is stirred by a forward rotation stirring paddle (33) and a reverse rotation stirring paddle (34) to form convection current so that the raw materials are fully stirred and reacted, then the o-fluorobenzoyl chloride is slowly dripped at the temperature of 20-50 ℃, the temperature is kept at 35-36 ℃ for a period of time until the reaction is finished, and a crude product of the 2, 4-difluorobenzophenone is prepared;
inputting tail gas generated in the reaction kettle into a falling film absorption tower through vacuum pumping equipment to obtain a 30% byproduct hydrochloric acid, and absorbing the tail gas through an alkaline washing absorption tower;
conveying the 2, 4-difluorobenzophenone crude product to a hydrolysis kettle through vacuum material pumping equipment, adding hydrochloric acid and water into the hydrolysis kettle, and layering to obtain an aluminum hydroxide aqueous solution and a hydrolyzed material of the 2, 4-difluorobenzophenone;
step (E), conveying the hydrolyzed material of the 2, 4-difluorobenzophenone to a washing refining kettle, and adding water to wash for two times to obtain a material of the 2, 4-difluorobenzophenone after washing;
and (F) conveying the material washed by the 2, 4-difluorobenzophenone into a distillation still, slowly heating the distillation still, distilling the material washed by the 2, 4-difluorobenzophenone, and ending the distillation when no distillate is at the top of the distillation still to obtain the 2, 4-difluorobenzophenone product.
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| CN202211115015.3A CN115646402A (en) | 2022-09-14 | 2022-09-14 | Processing system and method for 2, 4-difluorobenzophenone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116474396A (en) * | 2023-05-09 | 2023-07-25 | 河北傲格化工有限公司 | 5-chlorovaleryl chloride purifying device |
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2022
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116474396A (en) * | 2023-05-09 | 2023-07-25 | 河北傲格化工有限公司 | 5-chlorovaleryl chloride purifying device |
| CN116474396B (en) * | 2023-05-09 | 2023-09-12 | 河北傲格化工有限公司 | 5-chlorovaleryl chloride purifying device |
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