Continuous production device for topramezone intermediate

Abstract

The utility model relates to the technical field of pesticide production equipment, in particular to a topramezone intermediate continuous production device which comprises a microchannel reaction unit, the microchannel reaction unit is provided with a reaction area and a quenching area, an outlet of the reaction area is communicated with an inlet of the quenching area, and temperature control pipelines are arranged on the outer sides of the reaction area and the quenching area; the device further comprises a solid raw material batching unit and a liquid raw material supply unit, a discharging port of the solid raw material batching unit is communicated with a feeding port of the premixing unit, a discharging port of the premixing unit and a discharging port of the liquid raw material supply unit are communicated with an inlet of the reaction area, an outlet of the quenching area is communicated with a feeding port of the continuous extraction unit, and a discharging port of the continuous extraction unit is communicated with a discharging port of the continuous extraction unit. And an organic phase outlet of the continuous extraction unit is communicated with an inlet of the evaporation and concentration unit. According to the utility model, the solid raw material is prepared into a solution by using the solid raw material proportioning unit and the premixing unit, and the solution dissolved with the solid raw material and a liquid raw material are introduced into the micro-channel reaction unit for reaction and continuous extraction, so that the reaction efficiency is improved.

Description

Technical Field

[0001] The utility model relates to the technical field of pesticide production equipment, in particular to a continuous production device for a fenpyrotone intermediate. Background Art

[0002] Topramezone, also known as pyrazoline, is a highly selective benzoate pyrazolone herbicide developed by BASF in Germany. Topramezone contains both pyrazole and isoxazole rings and is a 4-hydroxyphenylpyruvate dioxidase (4-HPPD) inhibitor. It inhibits carotenoid synthesis, interferes with chloroplast function, and ultimately causes weed chlorosis and necrosis. Topramezone boasts a broad spectrum of herbicides, high herbicidal activity, good compatibility, excellent safety, rapid effectiveness, and environmental friendliness. It is the safest herbicide for cornfields and one of the least toxic to mammals.

[0003] There are two main methods for synthesizing fenpyrazone: carboxyl chlorination to form an ester followed by rearrangement and CO insertion. The carboxyl chlorination to form an ester followed by rearrangement method uses a carboxylic acid derivative as a raw material and synthesizes fenpyrazone through a three-step reaction of chlorination, esterification, and rearrangement. This method has a low synthesis cost, but the synthesis process is complex. In addition, since the synthetic raw materials contain carboxylic acid groups, which are generally derived from cyano hydrolysis or aldehyde oxidation, the raw material preparation is relatively difficult. The CO insertion method synthesizes fenpyrazone from a brominated intermediate and hydroxypyrazole under palladium catalyst and carbon monoxide high pressure conditions. This method uses 3-nitro-o-xylene or 2,3-dimethylaniline as the starting material. The raw materials are easily available and the yield is relatively high. 3-[3-Bromo-2-methyl-6-(methylsulfonyl)phenyl]-4,5-dihydroisoxazole is prepared by the addition reaction of 2-methyl-3-bromo-6-methylsulfonylbenzaldehyde oxime with ethylene and is a key intermediate in the CO insertion carbonylation process. 2-Methyl-3-bromo-6-methylsulfonylbenzaldehyde oxime is obtained via an oximation reaction, which requires demanding process conditions and has a decisive influence on the overall yield of the entire synthetic route. Currently, most companies use traditional batch reactions in kettles to synthesize 2-methyl-3-bromo-6-methylsulfonylbenzaldehyde oxime, resulting in low yields. The main reasons for this are: 1. The high heat released by the reaction can easily lead to excessively high reaction temperatures, making precise temperature control difficult; 2. The unstable structure of the oximation product can easily lead to damage during post-processing to quench the reaction. Utility Model Content

[0004] Aiming at the problem that the yield of 2-methyl-3-bromo-6-methylsulfonylbenzaldehyde oxime synthesized by traditional kettle-type batch reaction in the existing technology is low, the utility model provides a continuous production device for a fenpyroxene intermediate, which utilizes a solid raw material batching unit and a premixing unit to prepare a solid raw material into a solution, and then introduces the solution containing the solid raw material and the liquid raw material into a microchannel reaction unit for reaction and continuous extraction, thereby improving the reaction efficiency.

[0005] The technical solution of this utility model is as follows:

[0006] A continuous production device for a fenpyrazone intermediate comprises a microchannel reaction unit, wherein the microchannel reaction unit is provided with a reaction zone and a quenching zone, wherein the outlet of the reaction zone is connected to the inlet of the quenching zone, and the quenching zone is provided with a quenching agent inlet. Temperature control pipelines are provided on the outsides of the reaction zone and the quenching zone, and the temperature control pipelines are connected to a high and low temperature circulation device. The temperature of the reaction zone and the quenching zone can be controlled separately by the temperature control pipelines. The microchannel reaction unit comprises one or more microchannel reactors.

[0007] It also includes a solid raw material batching unit and a liquid raw material supply unit. The discharge port of the solid raw material batching unit is connected to the feed port of the premixing unit. The discharge port of the premixing unit and the discharge port of the liquid raw material supply unit are respectively connected to the inlet of the reaction zone. The outlet of the quenching zone is connected to the feed port of the continuous extraction unit. The organic phase outlet of the continuous extraction unit is connected to the inlet of the evaporation and concentration unit. The water phase outlet of the continuous extraction unit is connected to the sewage treatment system.

[0008] The lining materials of the solid raw material batching unit, liquid raw material supply unit, premixing unit, microchannel reaction unit and continuous extraction unit are all corrosion-resistant materials, preferably one or more of acid and alkali resistant stainless steel, glass lining and polytetrafluoroethylene.

[0009] Furthermore, the solid raw material dispersing unit includes a raw material dispersing device and a catalyst dispersing device. The raw material dispersing device is provided with a first solvent inlet and a main raw material inlet. The main raw material inlet is used to add solid raw materials into the raw material dispersing device, and the number of main raw material inlets can be adjusted according to the type of solid raw materials; the catalyst dispersing device is provided with a second solvent inlet and a catalyst inlet. The catalyst inlet is used to add solid catalyst into the catalyst dispersing device, and the number of catalyst inlets can be adjusted according to the type of solid catalyst.

[0010] Furthermore, the premixing unit is a static mixer.

[0011] Furthermore, the quenching agent inlet is communicated with the discharge port of the quenching agent supply unit, and the quenching agent supply unit supplies the acid solution or the alkaline solution to the quenching zone through the quenching agent inlet.

[0012] Furthermore, the continuous extraction unit comprises at least two extraction devices connected in series, the organic phase outlet of each extraction device is respectively connected to the inlet of the evaporation and concentration unit, the evaporation and concentration unit is preferably a falling film evaporator, and each extraction device is respectively connected to the extractant supply unit.

[0013] Furthermore, metering devices are respectively provided between the discharge port of the solid raw material batching unit and the feed port of the premixing unit, between the discharge port of the liquid raw material supply unit and the inlet of the reaction zone, between the discharge port of the premixing unit and the inlet of the reaction zone, between the quenching agent inlet and the discharge port of the quenching agent supply unit, and between each extraction device and the extractant supply unit. The metering device is preferably a metering pump, and the material of the metering pump is polytetrafluoroethylene, homopolypropylene, 304 stainless steel, 316L stainless steel or 2205 stainless steel.

[0014] Furthermore, a filtering device is provided between the discharge port of the premixing unit and the inlet of the reaction zone and / or between the discharge port of the solid raw material batching unit and the feed port of the premixing unit. The filtering device can remove suspended solids in the solution to ensure that the solution entering the microchannel reaction unit is a homogeneous solution.

[0015] Furthermore, the reaction zone includes at least two reaction chambers connected in series, and the quenching zone includes at least two quenching chambers connected in series. The inlet and outlet of the reaction zone are respectively provided on the reaction chambers at both ends, and the inlet and outlet of the quenching zone are respectively provided on the quenching chambers at both ends. The reaction chamber provided with the outlet of the reaction zone is connected to the quenching chamber provided with the inlet of the quenching zone, and the quenching chamber connected to the reaction chamber is also provided with a quenching agent inlet. Both the reaction chamber and the quenching chamber are removable.

[0016] The beneficial effects of the present invention are:

[0017] The utility model provides a continuous production device for a fenpyroxene intermediate, which utilizes a solid raw material batching unit and a premixing unit to prepare a solid raw material into a solution, and introduces the solution containing the solid raw material and a liquid raw material into a microchannel reaction unit for reaction. The microchannel reaction unit has a small size and a large specific surface area, which can improve the mass transfer and heat transfer rates, increase effective collisions between molecules, and is beneficial to improving production safety and reducing production energy consumption. At the same time, temperature control pipelines are arranged on the outside of the reaction zone and the quenching zone, which is beneficial to accurately control the temperature of the reaction zone and the quenching zone, solving the problems of difficult control of reaction conditions and easy destruction of products in the oximation reaction. The utility model also utilizes a continuous extraction unit to perform multi-stage extraction on the reaction mother liquor discharged from the microchannel reaction unit, thereby improving the reaction yield. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0019] Figure 1 Schematic diagram of the connection relationship of the continuous production device of the fenpyraclostrobin intermediate in Example 1.

[0020] Figure 1 Among them, 1-catalyst high-speed disperser, 2-raw material high-speed disperser, 3-static mixer, 4-first microchannel reactor, 5-second microchannel reactor, 6-first extraction device, 7-second extraction device, 8-falling film evaporator. DETAILED DESCRIPTION

[0021] In order to enable those skilled in the art to better understand the technical solutions of the present invention, the following will be combined with the drawings of the embodiments of the present invention to clearly and completely describe the technical solutions of the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts should fall within the scope of protection of the present invention.

[0022] Example 1

[0023] A continuous production device for a fenpyroxene intermediate includes a microchannel reaction unit, the microchannel reaction unit including a first microchannel reactor 4 and a second microchannel reactor 5. The first microchannel reactor 4 serves as a reaction zone, and the second microchannel reactor 5 serves as a quenching zone. The first microchannel reactor 4 is provided with five reaction chambers connected in series, wherein the first reaction chamber is provided with an inlet for the first microchannel reactor 4, and the fifth reaction chamber is provided with an outlet for the first microchannel reactor 4. The second microchannel reactor 5 is provided with five quenching chambers connected in series, wherein the first quenching chamber is provided with an inlet for the second microchannel reactor 5, and the fifth quenching chamber is provided with an outlet for the second microchannel reactor 5. The outlets of the first microchannel reactor 4 and the inlet of the second microchannel reactor 5 are connected. The first quenching chamber is also provided with a quenching agent inlet, which is connected to a discharge port of a quenching agent supply unit. A metering pump is provided between the quenching agent inlet and the discharge port of the quenching agent supply unit. Independent temperature control pipelines are provided on the outsides of the first microchannel reactor 4 and the second microchannel reactor 5, respectively, and the temperature control pipelines are connected to a high and low temperature circulation device. Among them, the first microchannel reactor 4 and the second microchannel reactor 5 are RMCS1010 microchannel reactors purchased from Shandong Haomai Chemical Technology Co., Ltd., and the high and low temperature circulation device is an HM-C refrigeration and heating constant temperature system purchased from Wuxi Guanya Constant Temperature Refrigeration Technology Co., Ltd.

[0024] The system further comprises a solid raw material batching unit and a liquid raw material supply unit. The solid raw material batching unit comprises a raw material high-speed disperser 2 and a catalyst high-speed disperser 1. The raw material high-speed disperser 2 is provided with a first solvent inlet and a main raw material inlet; the catalyst high-speed disperser 1 is provided with a second solvent inlet and a catalyst inlet. Both the raw material high-speed disperser 2 and the catalyst high-speed disperser 1 are provided with sight glasses. The discharge port of the raw material high-speed disperser 2 and the discharge port of the catalyst high-speed disperser 1 are respectively connected to the feed port of the static mixer 3 through a metering pump and a filtering device. The discharge port of the static mixer 3 is connected to the inlet of the first microchannel reactor 4 through a metering pump and a filtering device. The discharge port of the liquid raw material supply unit is connected to the inlet of the first microchannel reactor 4 through a metering pump. The outlet of the second microchannel reactor 5 is connected to the feed port of the first extraction device 6. The aqueous phase outlet of the first extraction device 6 is connected to the feed port of the second extraction device 7. The aqueous phase outlet of the second extraction device 7 is connected to the sewage treatment system. The organic phase outlet of the first extraction device 6 and the organic phase outlet of the second extraction device 7 are respectively connected to the inlet of the falling film evaporator 8, the liquid inlet of the first extraction device 6 and the liquid inlet of the second extraction device 7 are respectively connected to the extractant supply unit, and a metering pump is provided between the liquid inlet of the first extraction device 6 and the liquid inlet of the second extraction device 7 and the extractant supply unit, and the material of each metering pump is polytetrafluoroethylene.

[0025] The lining materials of the solid raw material batching unit, the liquid raw material supply unit, the premixing unit, the microchannel reaction unit and the continuous extraction unit are all made of polytetrafluoroethylene.

[0026] Directions:

[0027] Step 1: First, add a certain amount of DMF to a catalyst high-speed disperser, then turn on the catalyst high-speed disperser, and add sodium ethoxide to the catalyst high-speed disperser in a closed manner. The catalyst high-speed disperser is used to evenly mix the sodium ethoxide and DMF to obtain a uniform catalyst solution. During the mixing process, the sodium ethoxide can be observed through a sight glass to see if it is completely dissolved. First, add a certain amount of DMF to a raw material high-speed disperser, then turn on the raw material high-speed disperser, and add 4-methylsulfonyl-2,3-dimethylbromobenzene to the raw material high-speed disperser in a closed manner. The raw material high-speed disperser is used to evenly mix the 4-methylsulfonyl-2,3-dimethylbromobenzene and DMF to obtain a uniform reactant solution. During the mixing process, the 4-methylsulfonyl-2,3-dimethylbromobenzene can be observed through a sight glass to see if it is completely dissolved.

[0028] Step 2: The catalyst solution and the reactant solution are respectively added into a static mixer through corresponding metering pumps according to the feed mass ratio, and mixed to obtain a mixed solution.

[0029] Step 3: The temperature of the first microchannel reactor is controlled at -25°C by regulating the temperature and flow of the circulating medium in the temperature control pipeline outside the first microchannel reactor, and then the required reaction amount is pumped into the first microchannel reactor by a metering pump. The reaction liquid flows out of the first microchannel reactor and enters the second microchannel reactor. The temperature of the second microchannel reactor is controlled at -20°C by regulating the temperature and flow of the circulating medium in the temperature control pipeline outside the second microchannel reactor, and the metering pump is used to simultaneously pump the mixed solution and n-butyl nitrite into the first microchannel reactor. A hydrochloric acid aqueous solution is pumped into the device to quench the reaction and control the reaction process. The reaction mother liquor first enters the first extraction device, and at the same time, the extraction agent 1,2-dichloroethane is added to the first extraction device by a metering pump. The feed amount can be regulated by a valve. The aqueous phase after extraction and separation enters the second extraction device, and at the same time, the extraction agent 1,2-dichloroethane is added to the second extraction device by a metering pump. The feed amount can be regulated by a valve to perform secondary extraction. The organic phase after extraction and separation enters the falling film evaporator for concentration to obtain 2-methyl-3-bromo-6-methylsulfonylbenzaldehyde oxime.

[0030] Although the present invention has been described in detail with reference to the accompanying drawings and in conjunction with preferred embodiments, the present invention is not limited thereto. Without departing from the spirit and essence of the present invention, persons of ordinary skill in the art may make various equivalent modifications or substitutions to the embodiments of the present invention, and such modifications or substitutions shall fall within the scope of the present invention. Any changes or substitutions that can be easily conceived by persons skilled in the art within the technical scope disclosed in the present invention shall fall within the scope of protection of the present invention.

Claims

1. A continuous production device for a fenpyrazone intermediate, comprising a microchannel reaction unit, characterized in that: The microchannel reaction unit is provided with a reaction zone and a quenching zone, the outlet of the reaction zone is connected to the inlet of the quenching zone, the quenching zone is provided with a quenching agent inlet, and temperature control pipelines are provided outside the reaction zone and the quenching zone, and the temperature control pipelines are connected to the high and low temperature circulation device; It also includes a solid raw material batching unit and a liquid raw material supply unit. The discharge port of the solid raw material batching unit is connected to the feed port of the premixing unit. The discharge port of the premixing unit and the discharge port of the liquid raw material supply unit are respectively connected to the inlet of the reaction zone. The outlet of the quenching zone is connected to the feed port of the continuous extraction unit. The organic phase outlet of the continuous extraction unit is connected to the inlet of the evaporation and concentration unit. The water phase outlet of the continuous extraction unit is connected to the sewage treatment system.

2. The continuous production device for a fenpyrazone intermediate according to claim 1, wherein: The solid raw material dispensing unit comprises a raw material dispersing device and a catalyst dispersing device. The raw material dispersing device is provided with a first solvent inlet and a main raw material inlet. The catalyst dispersing device is provided with a second solvent inlet and a catalyst inlet.

3. The continuous production device for a fenpyrazone intermediate according to claim 1, wherein: The premixing unit is a static mixer.

4. The continuous production device for a fenpyrazone intermediate according to claim 1, wherein: The quenching agent inlet is communicated with the discharge port of the quenching agent supply unit.

5. The continuous production device for a fenpyrazone intermediate according to claim 4, wherein: The continuous extraction unit comprises at least two extraction devices connected in series, the organic phase outlet of each extraction device is respectively connected to the inlet of the evaporation and concentration unit, and each extraction device is respectively connected to the extraction agent supply unit.

6. The continuous production device for a fenpyrazone intermediate according to claim 5, wherein: Metering devices are respectively provided between the discharge port of the solid raw material batching unit and the feed port of the premixing unit, between the discharge port of the liquid raw material supply unit and the inlet of the reaction zone, between the discharge port of the premixing unit and the inlet of the reaction zone, between the quenching agent inlet and the discharge port of the quenching agent supply unit, and between each extraction device and the extraction agent supply unit.

7. The continuous production device for a fenpyrazone intermediate according to claim 1, wherein: A filtering device is provided between the discharge port of the premixing unit and the inlet of the reaction zone and / or between the discharge port of the solid raw material batching unit and the feed port of the premixing unit.

8. The continuous production device for a fenpyrazone intermediate according to claim 1, wherein: The reaction zone comprises at least two reaction chambers connected in series, the quenching zone comprises at least two quenching chambers connected in series, and the quenching agent inlet is arranged on the quenching chamber connected to the reaction chamber.

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