CN217527484U - Production device of benzoxazinone - Google Patents
Production device of benzoxazinone Download PDFInfo
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- CN217527484U CN217527484U CN202221347950.8U CN202221347950U CN217527484U CN 217527484 U CN217527484 U CN 217527484U CN 202221347950 U CN202221347950 U CN 202221347950U CN 217527484 U CN217527484 U CN 217527484U
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Abstract
The utility model discloses a benzoxazinone production device belongs to pesticide production facility field, including be used for replacing pyrazole formic acid and acylation reagent to take place acylation reaction and prepare the first reactor of replacing pyrazole acyl chloride, be used for anthranilic acid and carbonylation reagent to take place cyclization reaction and prepare the second reactor of replacing isatoic anhydride, acylation reaction liquid and cyclization reaction liquid take place the third reactor of coupling reaction preparation benzoxazinone, the reactant export of first reactor and second reactor all is connected with the feed end of third reactor; the utility model discloses can realize continuous production, simplify the production procedure, reduction in production cost, improvement production efficiency.
Description
Technical Field
The utility model relates to a production device of benzoxazinone belongs to pesticide production facility field.
Background
2- (3-bromo-1- (3-chloro-2-pyridyl) -1H-5-pyrazolyl) -6-chloro-8-methyl-4H-benzo [ d ] [1,3] oxazine-4-one is benzoxazinone for short, and is an important intermediate for producing high-efficiency low-grade pesticide chlorantraniliprole. Patent CN100422177C and patent CN100376565C disclose a method for preparing benzoxazinone by coupling reaction using 3-bromo-1- (3-chloropyridin-2-yl) -1H-pyrazole-5-carboxylic acid (substituted pyrazolecarboxylic acid for short) and 2-amino-3-methyl-5-chlorobenzoic acid (anthranilic acid for short) as raw materials and substituted pyrazolecarboxylic acid and 8-methyl-6-chloro-2H-3,1-benzoxazine-2,4- (1H) -dione (substituted isatoic anhydride for short) as raw materials, respectively, in the batch tank type production process, in order to ensure product yield, not only batch addition of materials is required, but also the feeding amount and corresponding process conditions at each stage need to be strictly regulated, the operation is complicated, the production efficiency is low, continuous production is difficult to achieve, in addition, in the production process, excess methanesulfonyl chloride is required to be added as a coupling agent, and excess acid-binding agent is required to be added, and the methanesulfonate produced in the reaction process needs to be separated and treated and recovered at a high excess production cost.
Patent CN113402512a adopts 3-bromo-1- (3-chloro-2-pyridyl) -1H-pyrazole-5-carbonyl chloride (substituted pyrazole acyl chloride for short) to replace substituted pyrazole carboxylic acid, but water generated in the kettle type production process can cause hydrolysis of substituted pyrazole acyl chloride, and in order to ensure that the substituted pyrazole carboxylic acid generated by hydrolysis can participate in the reaction, methanesulfonyl chloride is additionally added, so that the problems of complicated production process and high cost cannot be effectively solved.
In view of the foregoing, it is apparent that the prior art has inconvenience and disadvantages in practical use, and thus, needs to be improved.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to above not enough, provide a production device of benzoxazinone, can realize continuous production, simplify the production flow, reduction in production cost, improvement production efficiency.
For solving the technical problem, the utility model discloses a following technical scheme: a production device of benzoxazinone comprises a first reactor, a second reactor and a third reactor, wherein the first reactor is used for preparing substituted pyrazole acyl chloride through acylation reaction of substituted pyrazole formic acid and an acylation reagent, the second reactor is used for preparing substituted isatoic anhydride through cyclization reaction of anthranilic acid and a carbonylation reagent, acylation reaction liquid and cyclization reaction liquid are subjected to coupling reaction to prepare benzoxazinone, and reactant outlets of the first reactor and the second reactor are connected with a feed end of the third reactor.
Further, the first reactor is provided with a substituted pyrazolecarboxylic acid inlet, an acylating reagent inlet and an acylation reaction liquid outlet; the second reactor is provided with an anthranilic acid inlet, a carbonylation reagent inlet and a cyclization reaction liquid outlet; the third reactor is provided with an acylation reaction liquid inlet, a cyclization reaction liquid inlet and a coupling reaction liquid outlet;
the acylation reaction liquid inlet is communicated with the acylation reaction liquid outlet, and the cyclization reaction liquid inlet is communicated with the cyclization reaction liquid outlet.
Furthermore, the first reactor, the second reactor and the third reactor are dynamic tubular reactors, the dynamic tubular reactors are provided with reaction cavities and heat exchange cavities, and stirring shafts are arranged in the reaction cavities.
Furthermore, the first reactor and the third reactor are both provided with exhaust ports, and the exhaust port of the first reactor is communicated with the air inlet of the first condenser; and the exhaust port of the third reactor is communicated with the air inlet of the second condenser.
Further, the first reactor is provided with a first condensate inlet which is communicated with a condensate outlet of the first condenser.
Furthermore, the second reactor is provided with an exhaust port, and the exhaust port of the second reactor is communicated with the air inlet of the third condenser;
the second reactor is provided with a second condensate inlet which is communicated with a condensate outlet of the third condenser.
Further, the device comprises a solid-liquid separator, wherein the solid-liquid separator is connected to the discharge end of the third reactor; the solid-liquid separator is one of a centrifugal machine, a filter and a filter press; the solid-liquid separator is provided with a material inlet, a liquid phase outlet and a wet product outlet.
The dryer is arranged at the discharge end of the solid-liquid separator; the dryer is one of a flash evaporation dryer, a vacuum dryer, a roller dryer, a belt dryer, a film dryer and a rotary drum dryer.
Further, the solid-liquid separator is also provided with a first washing reagent inlet.
The device further comprises a distillation still, wherein the distillation still is arranged between the third reactor and the solid-liquid separator, the distillation still is provided with a coupling reaction liquid inlet, a second washing reagent inlet and a material outlet, the coupling reaction liquid inlet is communicated with the coupling reaction liquid outlet, and the material outlet is communicated with the material inlet.
The utility model adopts the above technical scheme afterwards, compare with prior art, be equipped with following advantage:
the utility model is used for a first reactor that replaces pyrazole formic acid and acylation reagent to carry out acyl chlorination reaction place with be used for providing anthranilic acid and carbonylation reagent and carry out cyclization reaction place second reactor and directly be linked together with the third reactor, can realize acyl chlorination reaction, cyclization reaction and replace the continuous of pyrazole acyl chloride and the coupling reaction of replacing isatoic anhydride are gone on, acyl chlorination reaction directly is used for coupling reaction with the reaction liquid of cyclization reaction, the distillation desolventizing of acylation reaction liquid has been left out, aftertreatment such as the solid-liquid separation of cyclization reaction liquid, the production flow has been simplified, can realize continuous production, and the production efficiency is improved, the use of intermediate treatment device has also been reduced, and the production cost is reduced.
The present invention will be described in detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic structural view of example 1;
FIG. 2 is a schematic view of the structure of embodiment 2.
In the figure, the position of the upper end of the main shaft,
1-a first reactor, 11-substituted pyrazolecarboxylic acid inlet, 12-acylating agent inlet, 13-acylation reaction liquid outlet, 14-first condensate inlet, 2-a second reactor, 21-anthranilic acid inlet, 22-carbonylation agent inlet, 23-cyclization reaction liquid outlet, 24-second condensate inlet, 3-a third reactor, 31-acylation reaction liquid inlet, 32-cyclization reaction liquid inlet, 33-coupling reaction liquid outlet, 4-solid-liquid separator, 41-material inlet, 42-liquid phase outlet, 43-product wet material outlet, 44-first washing agent inlet, 5-dryer, 6-first condenser, 7-second condenser, 8-third condenser, 9-distillation still, 91-coupling reaction liquid inlet, 92-second washing agent inlet, and 93-material outlet.
Detailed Description
In order to clearly understand the technical features, objects, and effects of the present invention, embodiments of the present invention will be described with reference to the accompanying drawings.
Example 1
As shown in fig. 1, this embodiment provides a production apparatus of benzoxazinone, comprising a first reactor 1, a second reactor 2, and a third reactor 3, wherein the reactant outlets of the first reactor 1 and the second reactor 2 are connected to the feed end of the third reactor 3.
Further, the first reactor 1 is used for providing a place for preparing substituted pyrazole acyl chloride by carrying out acyl chlorination reaction on substituted pyrazole formic acid and an acylation reagent, and the first reactor 1 is provided with a substituted pyrazole formic acid inlet 11, an acylation reagent inlet 12 and an acylation reaction liquid outlet 13; the second reactor 2 is used for providing a place for preparing substituted isatoic anhydride by cyclization reaction of anthranilic acid and a carbonylation reagent, and the second reactor 2 is provided with an anthranilic acid inlet 21, a carbonylation reagent inlet 22 and a cyclization reaction liquid outlet 23; the third reactor 3 is used for providing a place for preparing benzoxazinone through coupling reaction between acylation reaction liquid and cyclization reaction liquid, the third reactor 3 is provided with an acylation reaction liquid inlet 31, a cyclization reaction liquid inlet 32 and a coupling reaction liquid outlet 33, wherein the acylation reaction liquid inlet 31 is communicated with the acylation reaction liquid outlet 13 of the first reactor 1, and the cyclization reaction liquid inlet 32 is communicated with the cyclization reaction liquid outlet 23 of the second reactor 2.
The utility model discloses in, first reactor 1, second reactor 2, third reactor 3 are dynamic tubular reactor, are equipped with reaction chamber and heat transfer chamber, be equipped with the (mixing) shaft in the reaction chamber. The reaction cavity of the dynamic tubular reactor is used for providing a place for material reaction, a stirring paddle or a stirring fin is arranged on a central stirring shaft in the reaction cavity, stirring and mixing are realized through rotation, and the effective liquid holdup in the reaction cavity is 1-200L; the heat exchange cavity is used for exchanging heat to the reaction cavity through circulating heat exchange media.
As gas is generated in the processes of acylation reaction of 3-bromo-1- (3-chloro-2-pyridyl) -1H-pyrazole-5-carboxylic acid (substituted pyrazole carboxylic acid for short) in the first reactor 1 and coupling reaction of substituted pyrazole acyl chloride and substituted isatoic anhydride in the third reactor 3, in order to avoid the generated gas from occupying the inner space of the reactors and reducing the processing capacity of the reactors, preferably, the first reactor 1 and the third reactor 3 are both provided with exhaust ports, the exhaust port of the first reactor 1 is communicated with the gas inlet of the first condenser 6, and the exhaust port of the third reactor 3 is communicated with the gas inlet of the second condenser 7.
The first condenser 6 and the second condenser 7 are both provided with a gas outlet and a condensate outlet and are used for separating gas generated in the reaction process and recovering a solvent; the first condenser 6 may also recover the acylating agent.
The o-aminobenzoic acid and the carbonylation reagent generate hydrogen chloride in the cyclization reaction process in the second reactor 2, preferably, the second reactor 2 is provided with an exhaust port, the exhaust port of the second reactor 2 is communicated with the air inlet of the third condenser 8, the hydrogen chloride gas generated in the reaction process is directly discharged, and the use of an acid binding agent can be reduced. The third condenser is also provided with a gas outlet and a condensate outlet and is used for separating gas generated in the reaction process and recovering the solvent.
The gas generated by the acylation reaction of the 3-bromo-1- (3-chloro-2-pyridyl) -1H-pyrazole-5-formic acid and the acylating agent in the first reactor 1 entrains the solvent and the acylating agent which does not participate in the reaction when entering the first condenser 6 from the exhaust port, preferably, the first reactor 1 is provided with a first condensate inlet 14, and the first condensate inlet 14 is communicated with a condensate outlet of the first condenser 6 so as to return the acylating agent which does not participate in the reaction to the first reactor 1.
The production device further comprises a solid-liquid separator 4, the solid-liquid separator 4 is connected to the discharge end of the third reactor 3, the solid-liquid separator 4 is used for performing solid-liquid separation on the coupling reaction liquid flowing out of the third reactor 3 to obtain a wet product, the solid-liquid separator 4 is one of a centrifugal machine, a filter and a filter press, and the solid-liquid separator 4 is provided with a material inlet 41, a liquid phase outlet 42 and a wet product outlet 43.
The production device further comprises a dryer 5, the dryer 5 is arranged at the discharge end of the solid-liquid separator 4, the dryer 5 is used for drying wet materials of products to obtain the chlorantraniliprole, and the dryer 5 can be one of a flash evaporation dryer, a vacuum dryer, a roller dryer, a belt dryer, a film dryer and a drum dryer.
The method for producing benzoxazinone by the utility model is as follows:
(1) Respectively conveying a mixed solution of 3-bromo-1- (3-chloro-2-pyridyl) -1H-pyrazole-5-formic acid (substituted pyrazole formic acid for short) and a solvent and an acylating reagent to a first reactor for acyl chlorination reaction to obtain an acylation reaction solution containing substituted pyrazole acyl chloride;
(2) Respectively conveying the mixed solution of the 2-amino-3-methyl-5-chlorobenzoic acid and the solvent and the mixed solution of the carbonylation reagent and the solvent to a second reactor for cyclization reaction to obtain cyclization reaction liquid containing substituted isatoic anhydride;
(3) Enabling acylation reaction liquid containing substituted pyrazole acyl chloride obtained from the first reactor and cyclization reaction liquid containing substituted isatoic anhydride obtained from the second reactor to enter a third reactor simultaneously for coupling reaction to obtain coupling reaction liquid containing benzoxazinone;
(4) And filtering and drying the coupling reaction liquid flowing out of the third dynamic reactor to obtain the product benzoxazinone.
Example 2
As shown in fig. 2, the present embodiment provides a benzoxazinone production apparatus, and is different from embodiment 1 in that: the production device further comprises a distillation kettle 9, the distillation kettle 9 is arranged between the third reactor 3 and the solid-liquid separator 4, the distillation kettle 9 is provided with a coupling reaction liquid inlet 91 and a material outlet 93, the coupling reaction liquid inlet 91 is communicated with the coupling reaction liquid outlet 33 of the third reactor 3, the material outlet 93 is communicated with the material inlet of the solid-liquid separator 4, the distillation kettle 9 is used for concentrating the coupling reaction liquid, the purpose is to increase the precipitation rate of products, and the product yield is improved.
The hydrogen chloride gas generated in the process of cyclization reaction of the anthranilic acid and the carbonylation reagent in the second reactor 2 enters the third condenser 8 from the exhaust port and carries with the solvent and the carbonylation reagent, preferably, the second reactor 2 is provided with a second condensate inlet 24, and the second condensate inlet 24 is communicated with a condensate outlet of the third condenser 8, so that the carbonylation reagent which does not participate in the reaction returns to the second reactor 2.
Preferably, the solid-liquid separator 4 is further provided with a first washing reagent inlet 44, and the first washing reagent inlet 44 is used for adding a washing reagent into the solid-liquid separator 4, washing and separating wet products, and removing impurities attached to the surfaces of the products to improve the purity of the products.
The distillation still 9 is further provided with a second washing reagent inlet 92, and the second washing reagent inlet 92 is used for adding a washing reagent into the distillation still after the concentration is finished to carry out pulping and washing on the concentrated coupling reaction liquid, so that impurities are dissolved in the washing reagent, and the product purity is improved.
The utility model discloses a third reactor is direct to be linked together with the reactant export of first reactor and second reactor, has realized the continuous preparation and the direct application of two kinds of raw materialss of substituted pyrazole acyl chloride, substituted isatoic anhydride, has left out the processing flow and the equipment of acylation reaction and cyclization reaction back end, has simplified the production flow, can realize continuous production, improves production efficiency.
In the present invention, the manner of communication between the various units or devices is to be understood in a broad sense unless otherwise explicitly stated or limited; for example, the pipe connection may be direct pipe connection or pipe connection through a pipe chain machine, or may be pipe connection through conventional transportation, metering, control, and temporary storage devices such as pumping devices, metering devices, valve pipes, intermediate tanks, or may be fixed connection or detachable connection. The specific meaning of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The foregoing is illustrative of the best mode of the invention, and details not described herein are within the common general knowledge of a person of ordinary skill in the art. The protection scope of the present invention is subject to the content of the claims, and any equivalent transformation based on the technical teaching of the present invention is also within the protection scope of the present invention.
Claims (10)
1. A production device of benzoxazinone is characterized in that: the device comprises a first reactor (1) for preparing substituted pyrazole acyl chloride by acylation reaction of substituted pyrazole formic acid and an acylation reagent, a second reactor (2) for preparing substituted isatoic anhydride by cyclization reaction of anthranilic acid and a carbonylation reagent, and a third reactor (3) for preparing benzoxazinone by coupling reaction of acylation reaction liquid and cyclization reaction liquid, wherein reactant outlets of the first reactor (1) and the second reactor (2) are connected with a feed end of the third reactor (3).
2. The benzoxazinone production apparatus according to claim 1, characterized in that: the first reactor (1) is provided with a substituted pyrazole formic acid inlet (11), an acylating reagent inlet (12) and an acylation reaction liquid outlet (13); the second reactor (2) is provided with an anthranilic acid inlet (21), a carbonylation reagent inlet (22) and a cyclization reaction liquid outlet (23); the third reactor (3) is provided with an acylation reaction liquid inlet (31), a cyclization reaction liquid inlet (32) and a coupling reaction liquid outlet (33);
the acylation reaction liquid inlet (31) is communicated with the acylation reaction liquid outlet (13), and the cyclization reaction liquid inlet (32) is communicated with the cyclization reaction liquid outlet (23).
3. The benzoxazinone production apparatus according to claim 1, characterized in that: the reactor is characterized in that the first reactor (1), the second reactor (2) and the third reactor (3) are dynamic tubular reactors, the dynamic tubular reactors are provided with a reaction cavity and a heat exchange cavity, and a stirring shaft is arranged in the reaction cavity.
4. The benzoxazinone production apparatus according to claim 1, characterized in that: the first reactor (1) and the third reactor (3) are both provided with exhaust ports, and the exhaust port of the first reactor (1) is communicated with the air inlet of the first condenser (6); and the exhaust port of the third reactor (3) is communicated with the air inlet of the second condenser (7).
5. The benzoxazinone production apparatus according to claim 4, characterized in that: the first reactor (1) is provided with a first condensate inlet (14), and the first condensate inlet (14) is communicated with a condensate outlet of the first condenser (6).
6. The benzoxazinone production apparatus according to claim 4, characterized in that: the second reactor (2) is provided with an exhaust port, and the exhaust port of the second reactor (2) is communicated with the air inlet of the third condenser (8);
the second reactor (2) is provided with a second condensate inlet (24), and the second condensate inlet (24) is communicated with a condensate outlet of the third condenser (8).
7. A benzoxazinone production apparatus according to claim 2, characterized in that: the reactor comprises a solid-liquid separator (4), wherein the solid-liquid separator (4) is connected to the discharge end of the third reactor (3); the solid-liquid separator (4) is one of a centrifuge, a filter and a filter press; the solid-liquid separator (4) is provided with a material inlet (41), a liquid phase outlet (42) and a product wet material outlet (43).
8. The benzoxazinone production apparatus according to claim 7, characterized in that: the dryer (5) is arranged at the discharge end of the solid-liquid separator (4); the dryer (5) is one of a flash evaporation dryer, a vacuum dryer, a roller dryer, a belt dryer, a film dryer and a rotary drum dryer.
9. The benzoxazinone production apparatus according to claim 7, characterized in that: the solid-liquid separator (4) is also provided with a first washing reagent inlet (44).
10. The benzoxazinone production apparatus according to claim 7, characterized in that: still include stills (9), stills (9) are located between third reactor (3) and solid-liquid separator (4), stills (9) are equipped with coupling reaction liquid import (91), second washing reagent import (92) and material export (93), coupling reaction liquid import (91) is linked together with coupling reaction liquid export (33), material export (93) are linked together with material import (41).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221347950.8U CN217527484U (en) | 2022-05-31 | 2022-05-31 | Production device of benzoxazinone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221347950.8U CN217527484U (en) | 2022-05-31 | 2022-05-31 | Production device of benzoxazinone |
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| CN217527484U true CN217527484U (en) | 2022-10-04 |
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| CN202221347950.8U Active CN217527484U (en) | 2022-05-31 | 2022-05-31 | Production device of benzoxazinone |
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- 2022-05-31 CN CN202221347950.8U patent/CN217527484U/en active Active
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