Method for recovering reaction mother liquor of chlorantraniliprole and recovery processing equipment

Abstract

The application discloses a chlorantraniliprole reaction mother liquor recovery method and recovery processing equipment, comprising the following steps: S1: K acid and K amine are dissolved in a solvent a; S2: an acid-binding agent b is added, and temperature is controlled to drop methylsulfonyl chloride for condensation reaction; S3: after the reaction is completed, water is added to cool and crystallize; S4: centrifugation is carried out to obtain chlorantraniliprole; S5: after alkalization, the reaction mother liquor is extracted to separate an organic phase; S6: the organic phase is distilled to obtain a distillate main product; and S7: the distillate main product is dehydrated through a molecular sieve. The application has the advantages that: in the chlorantraniliprole synthesis, the selected solvent a and the acid-binding agent b can make the reaction yield greater than 94%; meanwhile, the reaction solvent a can meet the requirements of the reaction, direct separation with water, and extraction and dissolution of the acid-binding agent b in water; in the mother liquor recycling, the selected solvent a and the acid-binding agent b meet the conditions of molecular sieve dehydration, and the recovery rate of the solvent a and the acid-binding agent b is more than 95%.

Description

Technical Field

[0001] This invention relates to the field of pesticide chemistry, specifically to a method and equipment for recovering mother liquor from chlorantraniliprole reactions. Background Technology

[0002] Chlorantraniliprole, with the chemical formula C18H14BrCl2N5O2, is a compound that activates ryanodine receptors in insects, leading to excessive release of intracellular calcium ions. It has a highly effective killing effect on lepidopteran pest larvae and is mainly used to control pests such as rice leaf rollers and rice stem borers. Its effective period lasts for more than 15 days and it is classified as a slightly toxic pesticide.

[0003] Currently, there are many methods for preparing chlorantraniliprole, with two commonly used methods. Method one involves adding 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylic acid (K acid), 2-amino-5-chloro-N,3-dimethylbenzamide (K amine), and an acid-binding agent to a solvent, followed by a condensation reaction with the dropwise addition of methanesulfonyl chloride to obtain chlorantraniliprole, as described in patent CN101072767B. Method two involves first acyl chlorinating 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylic acid (K acid) to prepare K acyl chloride. The first method involves condensing 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazol-5-carboxylic acid (K acid) to form K acyl chloride, which is then condensed with 2-amino-5-chloro-N,3-dimethylbenzamide (K amine) and subsequently methylated with a methylamine solution to obtain chlorantraniliprole, as described in patents CN115745959B. Each method has its advantages and disadvantages. Method one is simple to operate and has a high yield, but it uses highly toxic methanesulfonyl chloride, and the solvent and acid-binding agent are difficult to recover, resulting in low utilization. Methods two and three avoid methanesulfonyl chloride, but the operation steps are lengthy, and the yield is relatively low.

[0004] The reaction solvents used in the synthesis of chlorantraniliprole generally include acetonitrile, 1,2-dioxane, tetrahydrofuran, DMF (N,N-dimethylformamide), DMAC (N,N-dimethylacetamide), DCE (1,2-dichloroethane), chloroform, dichloromethane, and NMP (N-methylpyrrolidone), while the acid-binding agents used include triethylamine, pyridine, 3-methylpyridine, aniline, and sodium carbonate. Current research on the preparation process of chlorantraniliprole focuses on product yield and quality, neglecting the recovery and utilization of reaction solvents and acid-binding agents. Methods for the recovery and utilization of chlorantraniliprole reaction solvents and acid-binding agents are still underdeveloped. The reaction solvents used in the synthesis of chlorantraniliprole can be water-soluble or water-insoluble, while the acid binders are generally water-soluble. Since chlorantraniliprole has very strict requirements for moisture content during the reaction, the reaction mother liquor is usually distilled after pH adjustment, and then dehydrated and separated by distillation column. This has the disadvantages of high energy consumption, high operational requirements, low recovery rate, and large equipment investment. Therefore, there is an urgent need for a method and equipment for recovering chlorantraniliprole reaction mother liquor to solve the above problems. Summary of the Invention

[0005] The purpose of this invention is to provide a method and equipment for recovering the mother liquor from the chlorantraniliprole reaction, so as to overcome the above-mentioned shortcomings in the prior art.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] A method for recovering mother liquor from chlorantraniliprole reactions includes the following steps:

[0008] S1: Dissolve 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylic acid (K acid) and 2-amino-5-chloro-N,3-dimethylbenzamide (K amine) in solvent a;

[0009] S2: Add acid-binding agent b, and control the temperature by adding methanesulfonyl chloride dropwise to carry out the condensation reaction;

[0010] S3: After the reaction is complete, add water to cool and crystallize;

[0011] S4: Centrifuge to obtain chlorantraniliprole;

[0012] S5: After alkalizing the mother liquor, the organic phase is extracted and separated.

[0013] S6: Distill the organic phase to obtain the main distillate product;

[0014] S7: The main product of the distillation is dehydrated by molecular sieve. The dehydrated solution is a mixture of solvent a and acid-binding agent b. After the content is detected, the ratio is recalculated and reused.

[0015] Preferably, solvent a is one of 1,2-dichloroethane, chloroform, benzene, and toluene.

[0016] Preferably, the acid-binding agent b is one of triethylamine, aniline, pyridine, and 3-methylpyridine.

[0017] Preferably, the molar ratio of each raw material is: K acid: K amine: methanesulfonyl chloride: acid binder = 1: 0.9~1.2: 1.0~1.4: 1.0~1.5.

[0018] Preferably, the condensation reaction temperature is -5°C to 20°C, and the reaction time is 2-6 hours.

[0019] Preferably, the extraction and separation is a two-stage extraction, where the extractant is reaction solvent a. The first extraction is a direct layer extraction after alkalizing the mother liquor, and the second extraction is a second extraction with reaction solvent a added to the aqueous layer after the first extraction. The organic phases from the two extractions are then combined.

[0020] Preferably, the amount of the secondary extractant used is 1 / 3 to 2 / 3 of the water layer volume.

[0021] Preferably, the molecular sieve is fed in a liquid phase, and the water content of the solution after molecular sieve treatment is less than 0.1%.

[0022] A chlorantraniliprole reaction mother liquor recovery and processing device, used in S5 of the above-mentioned chlorantraniliprole reaction mother liquor recovery method, includes a distillation flask, a condenser, a three-tailed connector, a receiving bottle, and a safety bottle. The condenser is connected to the distillation flask via a distillation head. The condenser is connected to the three-tailed connector via a clamp assembly. The clamp assembly is used to maintain a sealed connection between the condenser and the three-tailed connector and to control the rotation of the three-tailed connector. Each tail end of the three-tailed connector is connected to a receiving bottle. The safety bottle is connected to a gas nozzle on the three-tailed connector via a hose. The safety bottle is also connected to a negative pressure pump and a vacuum gauge.

[0023] Preferably, the clamp assembly includes a first clamping ring connected to the condenser pipe and a second clamping ring connected to the head of the three-tail pipe. A tension component is hinged on the second clamping ring, and a hook body matching the tension component is provided on the first clamping ring. The hook body can be rotated along the first clamping ring.

[0024] In the above technical solution, the beneficial effects of the present invention are:

[0025] The solvent a and acid-binding agent b selected in the synthesis of chlorantraniliprole can achieve a reaction yield greater than 94%. Simultaneously, direct extraction and separation can be achieved in the mother liquor extraction process; that is, the reaction solvent a meets the requirements of the reaction, direct separation from water, and extraction of the acid-binding agent b dissolved in water. In the mother liquor recovery and reuse, the solvent a and acid-binding agent b meet the conditions for molecular sieve dehydration, and the recovery rate of solvent a and acid-binding agent b reaches over 95%. This invention's technology produces chlorantraniliprole with fewer side reactions, higher yield, simple mother liquor recovery operation, low energy consumption, high recovery rate, and low equipment investment.

[0026] It should be understood that the foregoing general description and the following detailed description are exemplary and illustrative only, and are not intended to limit this disclosure.

[0027] This application provides an overview of various implementations or examples of the technology described in this disclosure, and is not a full disclosure of the entire scope or all features of the disclosed technology. Attached Figure Description

[0028] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this invention. For those skilled in the art, other drawings can be obtained based on these drawings.

[0029] Figure 1 This is a schematic diagram of the recycling and processing equipment of the present invention;

[0030] Figure 2 This is a schematic diagram of the connection structure between the condenser tube and the three-tailed connector of the present invention;

[0031] Figure 3 This is a schematic diagram of the clamp assembly structure of the present invention;

[0032] Figure 4 This is a front cross-sectional view of the connection between the condenser tube and the three-tailed pipe of the present invention.

[0033] Figure 5 For the present invention Figure 4 Enlarged structural diagram at point A;

[0034] Figure 6 This is a side cross-sectional view of the connection between the condenser tube and the three-tail pipe of the present invention.

[0035] Explanation of reference numerals in the attached figures:

[0036] 1. Distillation flask; 2. Condenser; 3. Three-tailed connector; 4. Receiving bottle; 5. Safety bottle; 6. Distillation head; 7. Negative pressure pump; 8. Vacuum gauge; 9. First clamping ring; 10. Second clamping ring; 11. Hook connector; 12. Swing rod; 13. Pull rod; 14. Locking post; 15. Hook groove; 16. Sliding groove; 17. Arc-shaped slider; 18. Lever; 19. Limiting post; 20. Limiting hole. Detailed Implementation

[0037] To make the objectives, technical solutions, and advantages of the embodiments of this disclosure clearer, the technical solutions of the embodiments of this disclosure will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this disclosure. All other embodiments obtained by those skilled in the art based on the described embodiments of this disclosure without creative effort are within the scope of protection of this disclosure.

[0038] The present invention provides a method for recovering mother liquor from chlorantraniliprole reactions, comprising the following steps:

[0039] S1: Dissolve 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylic acid (K acid) and 2-amino-5-chloro-N,3-dimethylbenzamide (K amine) in solvent a;

[0040] S2: Add acid-binding agent b, control the temperature and add methanesulfonyl chloride dropwise to carry out condensation reaction. The reaction temperature is -5℃~20℃ and the reaction time is 2~6 hours.

[0041] S3: After the reaction is complete, add water to cool and crystallize;

[0042] S4: Centrifuge to obtain chlorantraniliprole;

[0043] S5: After the mother liquor is alkalized, the organic phase is separated by a first extraction. The mother liquor after the first extraction is then separated by a second extraction using reaction solvent a. The organic phases from the two extractions are combined. The amount of the second extraction solvent used is 1 / 3 to 2 / 3 of the volume of the water layer.

[0044] S6: Obtain the main product by organic phase distillation. The organic phase distillation is a conventional atmospheric pressure distillation and negative pressure distillation. The water content of the solution after distillation is 1-3%.

[0045] S7: The main product of the distillation fraction is dehydrated by molecular sieve. The molecular sieve is fed in liquid phase. The water content of the solution after molecular sieve treatment is less than 0.1%. The molecular sieve is one of the conventional 3A, 4A, and 5A molecular sieves. The dehydrated solution is a mixed solution of solvent a and acid-binding agent b. After the content is detected, the ratio is recalculated and reused.

[0046] The solvent a is one of 1,2-dichloroethane, chloroform, benzene, and toluene; the acid-binding agent b is one of triethylamine, aniline, pyridine, and 3-methylpyridine.

[0047] The solvent a and acid-binding agent b selected in the synthesis of chlorotoluamide allow the reaction to proceed normally without affecting the yield.

[0048] In the mother liquor recovery, the selected solvent a can achieve direct extraction and separation from water.

[0049] In molecular sieve dewatering, the selected solvent a and acid-binding agent b meet the conditions for molecular sieve dewatering.

[0050] The molar ratio of each raw material is: K acid: K amine: methanesulfonyl chloride: acid binder = 1: 0.9~1.2: 1.0~1.4: 1.0~1.5.

[0051] The following are two specific implementation methods:

[0052] Example 1

[0053] Synthesis of chlorantraniliprole: 100g of ketal acid, 68g of ketal amine, 300g of reaction solvent DCE (1,2-dichloroethane), and 75g of pyridine were added to a 500mL four-necked flask equipped with a mechanical stirrer and a reflux tube. 50g of methanesulfonyl chloride was added dropwise at a controlled temperature of 10-15°C. After the addition was complete, the reaction was carried out for 5-8 hours. 200g of water was added to induce crystallization for 2 hours. After centrifugation, approximately 154g of chlorantraniliprole was obtained after drying. The mother liquor was then used in the recovery process.

[0054] Extraction and separation of mother liquor: The pH of the centrifuged mother liquor was adjusted to 10-12 with sodium hydroxide. The mother liquor was allowed to stand and separated. The organic phase was collected. The aqueous phase was extracted again with 150g DCE. The organic phase was collected and the organic phases were combined.

[0055] Dehydration and reuse of mother liquor: Organic phase distillation, collection of fractions, pumping of fractions into an exchange column packed with 4A molecular sieves, collection of exchange liquid, water content of exchange liquid less than 0.1%, detection of DCE and pyridine content in exchange liquid and direct reuse in chlorantraniliprole synthesis.

[0056] Example 2

[0057] Synthesis of chlorantraniliprole: 100g of ketal acid, 68g of ketal amine, 300g of chloroform, and 75g of pyridine were added to a 500mL four-necked flask equipped with a mechanical stirrer and a reflux tube. 50g of methanesulfonyl chloride was added dropwise while maintaining a temperature of 10-15°C. After the addition was complete, the reaction was carried out for 5-8 hours. 200g of water was added to induce crystallization for 2 hours. After centrifugation, approximately 152g of chlorantraniliprole was obtained after drying. The mother liquor was then used in the recovery process.

[0058] Extraction and separation of mother liquor: The pH of the centrifuged mother liquor was adjusted to 10-12 with sodium hydroxide. The mother liquor was allowed to stand and separated. The organic phase was collected. The aqueous phase was extracted again with 150g DCE. The organic phase was collected and the organic phases were combined.

[0059] Dehydration and reuse of mother liquor: Organic phase distillation, collection of fractions, pumping of fractions into an exchange column packed with 4A molecular sieves, collection of exchange liquid, water content of exchange liquid less than 0.1%, detection of chloroform and pyridine content in exchange liquid and direct reuse in chlorantraniliprole synthesis.

[0060] The advantages of this scheme are: the solvent a and acid-binding agent b selected in the synthesis of chlorotoluamide can achieve a reaction yield greater than 94%; at the same time, direct extraction and separation can be achieved in the mother liquor extraction and separation, that is, the reaction solvent a can meet the requirements of the reaction, the requirement of direct separation from water, and the requirement of extracting the acid-binding agent b dissolved in water; the solvent a and acid-binding agent b selected in the mother liquor recovery and utilization meet the conditions of molecular sieve dehydration, and the recovery rate of solvent a and acid-binding agent b is over 95%.

[0061] The technology of this invention produces chlorantraniliprole with fewer side reactions and higher yield. The mother liquor recovery operation is simple, energy consumption is low, recovery rate is high, and equipment investment is small. Compared with the traditional recovery process, equipment investment is reduced by 20%, energy consumption is reduced by 30%, and the recovery rate of reaction solvent and acid binder is increased by 30%.

[0062] Please see Figure 1-6 This invention provides a chlorantraniliprole reaction mother liquor recovery and processing device, which is used in S5 of the above-mentioned chlorantraniliprole reaction mother liquor recovery method. It includes a distillation flask 1, a condenser 2, a three-tailed connector 3, a receiving bottle 4, and a safety bottle 5. The condenser 2 is connected to the distillation flask 1 through a distillation head 6. The condenser 2 is connected to the three-tailed connector 3 through a clamp assembly. The clamp assembly is used to maintain the sealed connection between the condenser 2 and the three-tailed connector 3 and to control the rotation of the three-tailed connector 3. Each tail end of the three-tailed connector 3 is connected to a receiving bottle 4. The safety bottle 5 is connected to the gas nozzle on the three-tailed connector 3 through a hose. The safety bottle 5 is also connected to a negative pressure pump 7 and a vacuum gauge 8.

[0063] Specifically, the distillation flask 1, condenser 2, and safety bottle 5 are all fixed by an iron stand. A heating device is installed below the distillation flask 1. The upper end of the distillation flask 1 is sealed to the distillation head 6, and a thermometer is installed on the upper end of the distillation head 6. The distillation head 6 is sealed to the condenser 2, which has two water inlets, one higher and one lower, requiring cold water to enter from the bottom and exit from the top. The condenser 2 is inclined, with the end connected to the distillation head 6 being higher. The condenser 2 is sealed to the three-tail connector 3. All these sealing connections are achieved through a wedge-shaped fitting tube structure and the application of sealing materials such as Vaseline, ensuring a seal while allowing axial relative rotation. The three-tail connector 3 has three independent liquid receiving ports. These components are used to receive low-boiling-point impurities in the first fraction, the main product in the target fraction, and high-boiling-point residues in the last fraction, respectively, achieving precise fractional collection of components. The switching method is achieved by rotating the three-tailed connector 3 to bring the corresponding tail end to its lowest position. The clamp assembly applies elastic tension along the direction of the connection between the three-tailed connector 3 and the condenser tube 2, ensuring a seal without affecting the rotation of the three-tailed connector 3. The receiving bottle 4 is sealed to the three-tailed connector 3 and tightened by a rubber band, which is then fitted onto the gas nozzle of the three-tailed connector 3 to fix the tension. The safety bottle 5, in conjunction with the negative pressure pump 7, generates a negative pressure environment to achieve negative pressure distillation. The vacuum gauge 8 detects the pressure inside the safety bottle 5 to ensure safety. In practical use, the reagent in the distillation flask 1 evaporates upon heating and is introduced into the condenser tube 2 through the distillation head 6. It then condenses into a liquid in the condenser tube 2 and flows downwards to enter the three-tailed connector 3. From there, it flows into the target receiving bottle 4 via the designated path of the three-tailed connector 3. During this process, the safety bottle 5 and the negative pressure pump 7 work together to achieve negative pressure distillation, ensuring stable product output. Furthermore, the clamp assembly ensures a sealed connection between the condenser tube 2 and the three-tailed connector 3, while also allowing for rotation of the three-tailed connector 3. This replaces the traditional method of securing the three-tailed connector 3 with rubber bands, resulting in a more stable seal. Moreover, when adjusting the three-tailed connector 3, there is no need to repeatedly disassemble and reassemble the rubber bands, eliminating the risk of seal failure and ensuring a high recovery rate.

[0064] As a preferred technical solution in this embodiment, the clamp assembly includes a first clamping ring 9 connected to the condenser pipe 2 and a second clamping ring 10 connected to the head of the three-tailed connector 3. A tension component is hinged on the second clamping ring 10, and a hook body 11 matching the tension component is provided on the first clamping ring 9. The hook body 11 can rotate along the first clamping ring 9. Specifically, both the first clamping ring 9 and the second clamping ring 10 are clamp structures, specifically two semi-circular clamps hinged at one end and detachably connected at the other end by fasteners, thereby facilitating installation onto the head of the condenser pipe 2 or the three-tailed connector 3; the inner... The walls are equipped with buffer pads to prevent rigid clamping of glass products such as condenser tube 2 or three-tailed pipe 3, ensuring safe use. The first clamping ring 9 is equipped with a fork block that engages with the lower water inlet of condenser tube 2. When the first clamping ring 9 is installed on condenser tube 2, the fork block engages with the lower water inlet of condenser tube 2, positioning the first clamping ring 9. The second clamping ring 10 is detachably equipped with a U-shaped ring. When the second clamping ring 10 is installed on the head of three-tailed pipe 3, the U-shaped ring wraps around the air nozzle of three-tailed pipe 3, and then the two ends are inserted into the second clamping ring 10 with damping, thereby positioning the second clamping ring 10 and causing three-tailed pipe 3 to rotate synchronously with the second clamping ring 10. The tension assembly applies an elastic tension when connecting the hook body 11, and the direction of this elastic tension satisfies the tight connection between the condenser tube 2 and the three-tail connector 3; the hook body 11 moves along the first clamping ring 9, that is, it rotates around the axis of the first clamping ring 9. The first clamping ring 9 is installed after the condenser tube 2 and is coaxial with the condenser tube 2, that is, the hook body 11 can rotate around the axis of the condenser tube 2, and the rotation of the hook body 11 is coaxial with the rotation of the three-tail connector 3; the rotation range of the three-tail connector 3 adjusting the working position of each tail port is ±90° with the air nozzle facing upward as the reference.

[0065] As a preferred embodiment, the tension assembly includes a swing rod 12 hinged to the second clamping ring 10. A pull rod 13 is elastically extended at the end of the swing rod 12, and a locking post 14 is provided at the end of the pull rod 13. A hook groove 15 matching the locking post 14 is provided on the hook body 11. The lower end of the hook groove 15 is bent towards the second clamping ring 10. Specifically, a connecting seat is provided on the second clamping ring 10. The swing rod 12 includes two parallel bent rods and a first connecting post connecting the two bent rods. The two bent rods and the connecting post are approximately H-shaped. The pull rod 1... 3 includes two telescopic rods and a second connecting post. The locking post 14 is connected to the extended end of the two telescopic rods, while the second connecting post is connected between the other ends of the two telescopic rods. A spring is connected between the first connecting post and the second connecting post. The spring maintains elastic tension so that the pull rod 13 has a tendency to retract. The end of the locking post 14 passes through the side of the pull rod 13 for easy operation. The hook groove 15 is L-shaped with an open upper end and a lower end that bends and extends a certain length towards the second clamping ring 10. The pull rod 13 needs to extend outward a certain length to connect the locking post 14 and the hook groove 15. In practical use, after installing the first clamping ring 9 on the condenser pipe 2 and the second clamping ring 10 on the three-tailed connector 3, the swing rod 12 is rotated so that the locking pin 14 at the end of the pull rod 13 approaches the hook body 11. Then, the pull rod 13 is pulled to extend, so that the locking pin 14 smoothly enters the hook groove 15 until the lower bent end of the locking pin 14 is embedded in the hook groove 15. This keeps the first clamping ring 9 and the second clamping ring 10 connected together with tension, and the three-tailed connector 3 is tightly connected to the condenser pipe 2. Furthermore, by rotating the hook body 11 on the first clamping ring 9, the first clamping ring 9 and the second clamping ring 10 can rotate synchronously to adjust the angle of the three-tailed connector 3.

[0066] As a preferred embodiment, the first clamping ring 9 is provided with a sliding groove 16, and an arc-shaped slider 17 connected to the hook body 11 is movably disposed in the sliding groove 16. The hook body 11 is provided with a limiting component for limiting its own movement. The limiting component is triggered when the three-tailed tube 3 rotates to switch the corresponding collection positions of each receiving bottle 4, and at this time, the locking post 14 is engaged with the lower bent end of the hook groove 15. Specifically, the end face of the first clamping ring 9 near the three-tailed tube 3 is provided with a slot through which the arc-shaped slider 17 moves. The hook body 11 is also disposed on the outside of this end face of the first clamping ring 9 and is fixedly connected to the arc-shaped slider 17. The limiting component includes a lever 18 that is elastically rotatably disposed in the hook body 11. The upper end of the lever 18 extends into the lower bent portion of the hook groove 15. A limiting post 19 is movably disposed in the hook body 11. The lower end of lever 18 is movably connected to limit post 19, which movably passes through arc-shaped slider 17. The first clamping ring 9 is provided with three limit holes 20 that match the limit post 19. Each limit hole 20 corresponds to one of the three working positions of the three-tailed pipe 3. Furthermore, lever 18 is connected to hook body 11 through elastic elements such as torsion springs that resist rotation, and the rotation position is set in the middle. The lower end of lever 18 is provided with a frame-shaped part, and the limit post 19 is provided with a sliding part that matches the frame-shaped part. The frame-shaped part and the sliding part are movably connected so that the swing of lever 18 is linked with the movement of limit post 19. Under the elastic force of lever 18, the upper end of lever 18 is kept blocked at the position where the lower end of hook groove 15 bends and changes direction, while the lower end of lever 18 is linked with limit post 19 and kept inside arc-shaped slider 17.In practical use, after the condenser tube 2 and the three-tailed connector 3 are sealed and connected as required, the first clamping ring 9 is installed on the condenser tube 2 and positioned, and the second clamping ring 10 is installed on the head of the three-tailed connector 3 and positioned. The rocker arm 12 is rotated and the pull rod 13 is pulled to make the locking pin 14 embed into the hook groove 15. When the locking pin 14 moves to the lower bent portion within the hook groove 15, the locking pin 14 is released. Under the elastic force, the locking pin 14 automatically moves towards the lower bent end of the hook groove 15 and pushes the upper end of the lever 18. The lever 18 then moves in conjunction with the limiting pin 19 to insert into the corresponding limiting hole 20. This achieves a tight connection between the first clamping ring 9 and the second clamping ring 10, and also limits the hook body 11 to the first clamping ring 9. When the angle of the three-tailed connector 3 needs to be changed, the locking pin 14 is first pulled away from the second clamping ring 10. The lever 18 then rotates elastically and the limiting post 19 moves away from the corresponding limiting hole 20. The hook body 11 resumes rotation, which allows the second clamping ring 10 to rotate synchronously and drive the three-tailed pipe 3 to rotate and switch angles. After the three-tailed pipe 3 switches to the correct angle, the limiting post 19 aligns with another target limiting hole 20. The locking post 14 is released, and under the elastic force, the locking post 14 automatically moves deeper into the bent end of the hook groove 15. The lever 18 is pushed again, and the limiting post 19 moves again to insert into the corresponding limiting hole 20, so that the hook body 11 is limited again, ensuring the stability of the working angle of the three-tailed pipe 3. In addition, the locking post 14 is always in a pulled state during the above process, which generates more elastic tension on the pull rod 13 and applies it to the second clamping ring 10, thereby ensuring a more stable seal during the rotation of the three-tailed pipe 3.

[0067] The foregoing has only described certain exemplary embodiments of the present invention by way of illustration. Undoubtedly, those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the foregoing drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A method for recovering mother liquor from chlorantraniliprole reactions, characterized in that, Includes the following steps: S1: Dissolve 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylic acid (K acid) and 2-amino-5-chloro-N,3-dimethylbenzamide (K amine) in solvent a; S2: Add acid-binding agent b, and control the temperature by adding methanesulfonyl chloride dropwise to carry out the condensation reaction; S3: After the reaction is complete, add water to cool and crystallize; S4: Centrifuge to obtain chlorantraniliprole; S5: After alkalizing the mother liquor, the organic phase is extracted and separated. S6: Distill the organic phase to obtain the main distillate product; S7: The main product of the distillation is dehydrated by molecular sieve. The dehydrated solution is a mixture of solvent a and acid-binding agent b. After the content is detected, the ratio is recalculated and reused.

2. The method for recovering the mother liquor from the chlorantraniliprole reaction according to claim 1, characterized in that, The solvent a is one of 1,2-dichloroethane, chloroform, benzene, and toluene.

3. The method for recovering the mother liquor from the chlorantraniliprole reaction according to claim 1, characterized in that, The acid-binding agent b is one of triethylamine, aniline, pyridine, and 3-methylpyridine.

4. The method for recovering the mother liquor from the chlorantraniliprole reaction according to claim 1, characterized in that, The molar ratio of each raw material is: K acid: K amine: methanesulfonyl chloride: acid binder = 1: 0.9~1.2: 1.0~1.4: 1.0~1.

5.

5. The method for recovering the mother liquor from the chlorantraniliprole reaction according to claim 1, characterized in that, The condensation reaction temperature is -5℃ to 20℃, and the reaction time is 2-6 hours.

6. The method for recovering the mother liquor from the chlorantraniliprole reaction according to claim 1, characterized in that, The extraction and separation described herein is a two-stage extraction, with the extractant being the reaction solvent a. The first extraction is a direct layer extraction after alkalizing the mother liquor, and the second extraction is a second extraction after adding the reaction solvent a to the aqueous layer following the first extraction. The organic phases from the two extractions are then combined.

7. The method for recovering the mother liquor from the chlorantraniliprole reaction according to claim 6, characterized in that, The amount of the secondary extractant used is 1 / 3 to 2 / 3 of the water layer volume.

8. The method for recovering the mother liquor from the chlorantraniliprole reaction according to claim 1, characterized in that, The molecular sieve is fed in a liquid phase, and the solution after molecular sieve treatment has a water content of less than 0.1%.

9. A chlorantraniliprole reaction mother liquor recovery and processing device, used in S5 of the chlorantraniliprole reaction mother liquor recovery method according to any one of claims 1 to 8, comprising a distillation flask (1), a condenser (2), a three-tail connector (3), a receiving bottle (4), and a safety bottle (5), characterized in that, A condenser tube (2) is connected to a distillation head (6) on a distillation flask (1). The condenser tube (2) is connected to a three-tailed connector (3) via a clamp assembly. The clamp assembly is used to maintain a sealed connection between the condenser tube (2) and the three-tailed connector (3) and to control the rotation of the three-tailed connector (3). Each tail end of the three-tailed connector (3) is connected to a receiving bottle (4). A safety bottle (5) is connected to a gas nozzle on the three-tailed connector (3) via a hose. A negative pressure pump (7) and a vacuum gauge (8) are also connected to the safety bottle (5).

10. The method for recovering the mother liquor from the chlorantraniliprole reaction according to claim 9, characterized in that, The clamp assembly includes a first clamp (9) connected to the condenser tube (2) and a second clamp (10) connected to the head of the three-tail pipe (3). A tension assembly is hinged on the second clamp (10), and a hook body (11) matching the tension assembly is provided on the first clamp (9). The hook body (11) can be rotated along the first clamp (9).

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