Production device of substituted pyrazole acid compound

Abstract

The utility model provides a production device of a substituted pyrazole acid compound. The production device comprises an oxidation reaction unit, a hydrolysis reaction unit, a first solid-liquid separator, an alkaline hydrolysis reaction unit, an acidification reaction unit, a second solid-liquid separator, a pulping kettle, a third solid-liquid separator and a first drying machine. According to the production device provided by the utility model, substituted pyrazole acid compounds and potassium sulfate can be obtained through separation at the same time, the generation of waste acid, waste gas and waste salt in the production device is reduced, and the process is clean, green and environment-friendly. And an ethanol recovery tower is arranged in the reaction process, so that the comprehensive utilization of ethanol is realized, and the economical efficiency of the product is improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical equipment, and specifically relates to a production device for substituted pyrazole acid compounds. Background Art

[0002] O-formamidobenzamide insecticides are a class of highly effective, low-toxic insecticides that are widely used in the agricultural field. 3-Bromo-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxylic acid (referred to as substituted pyrazole acid compounds) is an important intermediate of o-formamidobenzamide insecticides, which is generally obtained by oxidation and hydrolysis of 3-bromo-1-(3-chloro-2-pyridinyl)-4,5-dihydro-1H-pyrazole-5-carboxylic acid ethyl ester (referred to as brominated pyrazole compounds). The process of producing this intermediate will produce a large amount of wastewater and waste salt after separating the product due to the use of potassium persulfate and sulfuric acid, which is difficult to treat. Optimizing the production equipment of this intermediate, avoiding the impact of wastewater and waste salt on the environment while obtaining the product, improving resource utilization, and realizing clean production are crucial to enhancing the economic value of chlorantraniliprole. Utility Model Content

[0003] The utility model provides a production device for substituted pyrazole acid compounds which has the advantages of clean process, high efficiency, convenience, high economy and green environmental protection.

[0004] The utility model provides a production device for substituted pyrazole acid compounds, characterized in that it includes: an oxidation reaction unit, a hydrolysis reaction unit, a first solid-liquid separator, an alkaline hydrolysis reaction unit, an acidification reaction unit, a second solid-liquid separator, a pulping kettle, a third solid-liquid separator, and a first dryer. The discharge port of the oxidation reaction unit is connected to the feed port of the hydrolysis reaction unit, and the discharge port of the hydrolysis reaction unit is connected to the feed port of the first solid-liquid separator; the solid phase outlet of the first solid-liquid separator is sequentially connected to the alkaline hydrolysis reaction unit, the acidification reaction unit, and the second solid-liquid separator, and the liquid phase outlet of the first solid-liquid separator is sequentially connected to the first neutralization kettle and the solvent recovery unit; the solid phase outlet of the second solid-liquid separator is sequentially connected to the pulping kettle, the third solid-liquid separator, and the first dryer, and the liquid phase outlet of the second solid-liquid separator is sequentially connected to the second neutralization kettle, the evaporation unit, the crystallization kettle, the fourth solid-liquid separator, the refining kettle, the fifth solid-liquid separator, and the second dryer;

[0005] The hydrolysis reaction unit is provided with a water phase inlet, the first neutralization kettle, the alkaline hydrolysis reaction unit and the second neutralization kettle are all provided with a potassium hydroxide solution inlet, the acidification reaction unit is provided with a sulfuric acid inlet, the pulping kettle is provided with a pulping solvent inlet, and the refining kettle is provided with a refining solvent inlet.

[0006] In an optional embodiment, the solvent recovery unit includes a distillation kettle and a distillation tower; the distillation kettle is provided with a feed inlet, a light component outlet at the top of the kettle, and a heavy component outlet at the bottom of the kettle, and the distillation tower is provided with a feed inlet, a water phase outlet at the top of the tower, and a DMF outlet at the bottom of the tower; the discharge port of the first neutralization kettle is connected to the feed inlet of the distillation kettle, and the light component outlet at the top of the distillation kettle is connected to the feed inlet of the distillation tower.

[0007] In an optional embodiment, the heavy component outlet at the bottom of the distillation kettle is connected to the feed inlet of the crystallization kettle.

[0008] In an optional embodiment, the water phase outlet at the top of the distillation tower is connected to the water phase inlet of the hydrolysis reaction unit.

[0009] In an optional embodiment, a mixing kettle is further included; the DMF outlet of the kettle of the distillation tower is connected to the feed inlet of the mixing kettle.

[0010] In an optional embodiment, the liquid phase outlet of the third solid-liquid separator is connected to the feed inlet of the second neutralization kettle.

[0011] In an optional embodiment, the evaporation unit includes a preheater, a heater, a separator, and a compressor; the discharge port of the second neutralization kettle is connected to the tube side inlet of the preheater, the tube side outlet of the preheater is connected to the tube side inlet of the heater, the tube side outlet of the heater is connected to the feed port of the separator, the concentrated liquid outlet of the separator is respectively connected to the tube side inlet of the heater and the feed port of the crystallization kettle, the steam outlet of the separator is connected to the shell side inlet of the heater via the compressor, and the shell side outlet of the heater is connected to the shell side inlet of the preheater.

[0012] In an optional embodiment, it also includes an ethanol recovery tower; the ethanol recovery tower is provided with a feed inlet, an ethanol outlet, and a water phase outlet; the shell side outlet of the preheater is connected to the feed inlet of the ethanol recovery tower, and the water phase outlet of the ethanol recovery tower is connected to the feed inlet of the pulping kettle.

[0013] In an optional embodiment, the ethanol outlet of the ethanol recovery tower is connected to the feed inlet of the refining kettle.

[0014] In an optional embodiment, an ethanol distillation kettle is further included; the liquid phase outlet of the fifth solid-liquid separator is connected to the feed inlet of the ethanol distillation kettle.

[0015] Compared with the prior art, the technical solution provided by the utility model has the following advantages:

[0016] 1. The production device provided by the utility model obtains a reaction solution containing a substituted pyrazole acid compound and potassium sulfate through an oxidation reaction unit, a hydrolysis reaction unit, a first solid-liquid separator, an alkaline hydrolysis reaction unit, and an acidification reaction unit. The second solid phase separated by the second solid-liquid separator is processed by a pulping kettle, a third solid-liquid separator, and a first dryer to obtain a high-purity substituted pyrazole acid compound. The second liquid phase separated by the second solid-liquid separator is processed by a second neutralization kettle, an evaporation unit, a crystallization kettle, a fourth solid-liquid separator, a refining kettle, a fifth solid-liquid separator, and a second dryer to obtain a high-purity by-product potassium sulfate. In addition, the heavy component outlet at the bottom of the solvent recovery unit is connected to the feed port of the crystallization kettle, and the liquid phase outlet of the third solid-liquid separation unit is connected to the feed port of the second neutralization kettle, so that the high-purity by-product potassium sulfate is further recovered, so that no waste acid, waste gas, or waste salt is generated in the production device, and the process is clean and green.

[0017] 2. The establishment of the solvent recovery unit realizes the recovery of water and the reaction solvent DMF. The water phase outlet at the top of the distillation tower is connected to the water phase inlet of the hydrolysis reaction unit, and the DMF outlet at the bottom of the distillation tower is connected to the feed inlet of the mixing kettle, which realizes the comprehensive utilization of water and solvent DMF and reduces the generation of wastewater. The ethanol produced in the production process is separated by the evaporation unit and the ethanol recovery tower and then enters the refining kettle for the refining of crude potassium sulfate, realizing the comprehensive utilization of ethanol, thereby improving the economic efficiency of the product.

[0018] 3. A preheater, evaporator, separator and compressor are set up in the evaporation unit. The steam separated by the separator enters the compressor for compression to obtain high-temperature and high-pressure steam. The steam is used as hot coal of the heater and preheater to heat the materials in the pipe process, reducing the heating and cooling load of public works and realizing energy recovery and utilization. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the specific implementation methods of the utility model or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the utility model. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0020] Figure 1 A schematic diagram of the structure of the device used in Example 1 of the utility model;

[0021] Figure 2 A schematic diagram of the structure of the device used in Example 2 of the present utility model;

[0022] Figure 3 A schematic diagram of the structure of the device used in Example 3 of the present utility model;

[0023] Figure 4 A schematic diagram of the structure of the device used in Example 4 of the utility model;

[0024] Figure 5 A schematic diagram of the structure of the device used in Example 5 of the utility model;

[0025] Figure 6 This is a schematic diagram of the structure of the device used in Example 6 of the utility model.

[0026] Description of reference numerals:

[0027] 1-oxidation reaction unit, 2-hydrolysis reaction unit, 3-first solid-liquid separator, 4-first neutralization kettle, 5-solvent recovery unit, 51-distillation kettle, 52-rectification tower, 6-alkaline hydrolysis reaction unit, 7-acidification reaction unit, 8-second solid-liquid separator, 9-beating kettle, 10-third solid-liquid separator, 11-first dryer, 12-second neutralization kettle, 13-evaporation unit, 131-preheater, 132-heater, 133-separator, 134-compressor, 14-crystallization kettle, 15-fourth solid-liquid separator, 16-refining kettle, 17-fifth solid-liquid separator, 18-second dryer, 19-ethanol recovery tower, 20-mixing kettle, 21-ethanol distillation kettle. DETAILED DESCRIPTION

[0028] The technical solution of the utility model will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0029] In the present invention, unless otherwise clearly specified or limited, the connection mode between various units or devices should be understood in a broad sense. For example, it can be direct pipeline connection, or it can be connected through pipelines connected to conventional conveying, metering, control, and temporary storage equipment such as pumping equipment, metering equipment, valves and pipe fittings, intermediate tanks, etc. It can be fixed connection or detachable connection. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0030] In the utility model, various components of the production device, such as dynamic tubular reactor, reaction kettle, solid-liquid separator, neutralization kettle, distillation kettle, distillation tower, mixing kettle, pulping kettle, preheater, separator, heater, compressor, crystallization kettle, refining kettle, dryer, recovery tower, as well as pipe fittings, valves, controllers, feed pumps, etc. can be purchased from the market, but the entire reaction device cannot be purchased from the market and is not known to those skilled in the art.

[0031] The utility model is further described below in conjunction with the accompanying drawings and embodiments.

[0032] Please refer to Figure 1-Figure 6 The utility model provides a production device for substituted pyrazole acid compounds. Example

[0033] This embodiment provides a production device for substituted pyrazole acid compounds, and its structural schematic diagram is as follows Figure 1 As shown, an oxidation reaction unit 1, a hydrolysis reaction unit 2, a first solid-liquid separator 3, an alkaline hydrolysis reaction unit 6, an acidification reaction unit 7, a second solid-liquid separator 8, a pulping kettle 9, a third solid-liquid separator 10, and a first dryer 11. The discharge port of the oxidation reaction unit 1 is connected with the feed port of the hydrolysis reaction unit 2, and the discharge port of the hydrolysis reaction unit 2 is connected with the feed port of the first solid-liquid separator 3; the solid phase outlet of the first solid-liquid separator 3 is connected with the alkaline hydrolysis reaction unit 6, the acidification reaction unit 7, and the second solid-liquid separator 8 in sequence, and the liquid phase outlet of the first solid-liquid separator 3 is connected with the first neutralization kettle 4 and the solvent recovery unit 5 in sequence; the solid phase outlet of the second solid-liquid separator 8 is connected with the pulping kettle 9, the third solid-liquid separator 10, and the first dryer 11 in sequence, and the liquid phase outlet of the second solid-liquid separator 8 is connected with the second neutralization kettle 12, the evaporation unit 13, the crystallization kettle 14, the fourth solid-liquid separator 15, the refining kettle 16, the fifth solid-liquid separator 17, and the second dryer 18 in sequence;

[0034] The hydrolysis reaction unit 2 is provided with a water phase inlet, the first neutralization kettle 4, the alkaline hydrolysis reaction unit 6, and the second neutralization kettle 12 are all provided with a potassium hydroxide solution inlet, the acidification reaction unit 7 is provided with a sulfuric acid inlet, the pulping kettle 9 is provided with a pulping solvent inlet, and the refining kettle 16 is provided with a refining solvent inlet.

[0035] In a specific implementation, the raw material bromopyrazole compound and the oxidizing agent potassium persulfate enter an oxidation reaction unit 1 composed of a primary dynamic tubular reactor to undergo an oxidation reaction to obtain a reaction solution containing a substituted pyrazole ester compound, potassium pyrosulfate and potassium persulfate that does not participate in the reaction. The reaction solution enters a hydrolysis reaction unit 2 composed of a primary dynamic tubular reactor. The potassium pyrosulfate and the potassium persulfate that do not participate in the reaction in the reaction solution undergo a hydrolysis reaction with water to generate potassium sulfate and sulfuric acid that are soluble in water. The hydrolyzed solution enters a first solid-liquid separator 3 to separate a first solid-phase substituted pyrazole ester compound and a first liquid phase containing potassium sulfate and sulfuric acid. The first solid phase enters an alkaline hydrolysis reaction unit 6 composed of a secondary series of reactors to undergo an alkaline hydrolysis reaction with potassium hydroxide that enters the alkaline hydrolysis reaction unit 6 to obtain a reaction solution containing a substituted pyrazole acid salt compound and ethanol. The reaction solution enters an acidification reaction unit 7 composed of a secondary series of reactors to react with sulfuric acid that enters the acidification reaction unit 7 to generate a substituted pyrazole acid compound that is insoluble in water. The acidified solution enters a second solid-liquid separator 8 to separate the second liquid phase to obtain a second solid-phase substituted pyrazole acid compound. The second solid phase The mixture enters the beating kettle 9, is mixed and stirred with the beating solvent to remove impurities, and then is separated by the third solid-liquid separator 10 and then enters the first dryer 11 for drying to obtain a product replacing the pyrazole acid compound. The second liquid phase containing ethanol, sulfuric acid and potassium sulfate separated by the second solid-liquid separator 8 enters the second neutralization kettle 12, and undergoes an acid-base neutralization reaction with potassium hydroxide in the second neutralization kettle 12 to neutralize the sulfuric acid into potassium sulfate to obtain a second neutralized liquid. The second neutralized liquid enters the evaporation unit 13, and the concentrated liquid after the water and ethanol are evaporated enters the crystallization kettle 14 for cooling and crystallization, and then enters the fourth The solid-liquid separator 15 separates the crude potassium sulfate, and the crude potassium sulfate enters the refining kettle 16, where the impurities in the crude potassium sulfate are dissolved by the refining solvent, and then enters the fifth solid-liquid separator 17 to separate the solid. The collected solid enters the second dryer 18 for drying to obtain by-product potassium sulfate. The first solid-liquid separator 3 separates the first liquid phase whose main components are water, DMF, potassium sulfate and sulfuric acid. The first liquid phase enters the first neutralization kettle 4 to undergo an acid-base neutralization reaction with the potassium hydroxide entering the first neutralization kettle 4 to obtain a first neutralized liquid. The first neutralized liquid enters the solvent recovery unit 5 to evaporate and recover water and DMF.

[0036] Optionally, the oxidation reaction unit 1, the hydrolysis reaction unit 2, the alkaline hydrolysis reaction unit 6, and the acidification reaction unit 7 are all made of at least one stage of dynamic tubular reactors or reactors connected in series.

[0037] Optionally, the first dryer 11 and the second dryer 18 are both selected from one of a disc dryer, a rake dryer, a vacuum dryer, a drum dryer, a belt dryer, and a film dryer. Example

[0038] This embodiment provides a production device for substituted pyrazole acid compounds, and its structural schematic diagram is as follows Figure 2As shown, the difference from Example 1 is that the solvent recovery unit 5 includes a distillation kettle 51 and a distillation tower 52 connected in series in sequence, the discharge port of the first neutralization kettle 4 is connected to the feed port of the distillation kettle 51, the light component outlet at the top of the distillation kettle 51 is connected to the feed port at the middle and lower part of the distillation tower 52, the water phase outlet at the top of the distillation tower 52 is connected to the water phase inlet of the hydrolysis reaction unit 2, the heavy component outlet at the bottom of the distillation kettle 51 is connected to the feed port of the crystallization kettle 14, the oxidation reaction unit 1 and the hydrolysis reaction unit 2 both use two-stage dynamic tubular reactors in series, and the alkaline hydrolysis reaction unit 6 and the acidification reaction unit 7 both use a single-stage reactor.

[0039] In specific implementation, in order to improve the separation efficiency and obtain high-purity DMF and water, on the basis of Example 1, the first neutralized liquid containing DMF, potassium sulfate and water enters the distillation kettle 51 for distillation, and the light component whose main components are water and DMF is separated from the light component outlet at the top of the distillation kettle 51. The light component at the top of the distillation kettle enters the distillation tower 52, and after distillation, water is separated from the water phase outlet at the top of the tower to obtain water, and DMF is separated from the DMF outlet at the bottom of the tower to obtain DMF. The water separated at the top of the distillation tower 52 is returned to the hydrolysis reaction unit 2. In order to fully recover the by-product potassium sulfate, the heavy component whose main component is potassium sulfate is separated from the heavy component outlet at the bottom of the distillation kettle 51. It enters the crystallization kettle 14, is mixed with the concentrated liquid from the evaporation unit 13, and then cooled and crystallized. It is separated by the fourth solid-liquid separator 15 to obtain crude potassium sulfate. The crude potassium sulfate enters the refining kettle 16, is refined by the refining solvent, and then is sequentially separated by solid-liquid separation and dried to obtain the by-product potassium sulfate. Example

[0040] This embodiment provides a production device for substituted pyrazole acid compounds, and its structural schematic diagram is as follows Figure 3 As shown, the difference from Example 1 is that in this embodiment, the evaporation unit 13 is composed of a preheater 131, a heater 132, a separator 133, and a compressor 134. The discharge port of the second neutralization kettle 12 is connected to the tube side inlet of the preheater 131, the tube side outlet of the preheater 131 is connected to the tube side inlet of the heater 132, the tube side outlet of the heater 132 is connected to the feed port of the separator 133, the concentrated liquid outlet of the separator 133 is respectively connected to the tube side inlet of the heater 132 and the feed port of the crystallization kettle 14, the steam outlet of the separator 133 is connected to the shell side inlet of the heater 132 through the compressor 134, and the shell side outlet of the heater 132 is connected to the shell side inlet of the preheater 131, wherein the preheater 131 and the heater 132 are both shell and tube heat exchangers, the oxidation reaction unit 1 and the hydrolysis reaction unit 2 are both primary reactors, and the alkaline hydrolysis reaction unit 6 and the acidification reaction unit 7 are both secondary series dynamic tubular reactors.

[0041] In specific implementation, on the basis of Example 1, the second neutralization liquid obtained by the second neutralization kettle 12 enters the tube side of the preheater 131, enters the tube side of the heater 132 for heating after preheating, and then enters the separator 133 for gas-liquid separation. The concentrated liquid portion after separation returns to the heater 132, is forced to circulate between the heater 132 and the separator 133, and part enters the crystallization kettle 14 for cooling and crystallization. The steam with main components of water and ethanol separated by the separator 133 enters the compressor 134 for compression, and the compressed high-temperature and high-pressure steam enters the shell side of the heater 132 to heat the second neutralization liquid in the tube side of the heater 132. After providing heat energy, it condenses into evaporative condensate and enters the shell side of the preheater 131 to preheat the second neutralization liquid in the tube side of the preheater 131, thereby saving the cooling water consumption for steam cooling, saving energy, and improving energy utilization.

[0042] Optionally, the preheater 131 and the heater 132 are both selected from a shell-and-tube heat exchanger or a wound tube heat exchanger. Example

[0043] This embodiment provides a production device for substituted pyrazole acid compounds, and its structural schematic diagram is as follows Figure 4 As shown, the difference from Example 3 is that this embodiment is further provided with an ethanol recovery tower 19, the feed port of the ethanol recovery tower 19 is connected to the shell side outlet of the preheater 131, the water phase outlet of the ethanol recovery tower 19 is connected to the inlet of the pulping kettle 9, the liquid phase outlet of the third solid-liquid separator 10 is connected to the feed port of the second neutralization kettle 12, the oxidation reaction unit 1 and the hydrolysis reaction unit 2 both use two-stage series reactors, and the alkaline hydrolysis reaction unit 6 and the acidification reaction unit 7 both use a one-stage dynamic tubular reactor.

[0044] In specific implementation, in order to separate ethanol and water and reduce production costs, on the basis of Example 3, the steam whose main components are water and ethanol separated by the separator 133 is compressed by the compressor 134, and then enters the shell side of the heater 132 and the preheater 131 in sequence, and flows out from the shell side outlet of the preheater 131 to enter the ethanol recovery tower 19 for distillation separation of ethanol and water. In order to further recover the potassium sulfate produced in the production process, reduce the generation of waste salt, and improve the utilization rate of water, the water separated by distillation in the ethanol recovery tower 19 enters the pulping kettle 9 as a pulping solvent to pulp and wash the second solid phase from the second solid-liquid separator 8 to remove salt in the product. The third liquid phase containing sulfuric acid and potassium sulfate separated by the third solid-liquid separator 10 enters the second neutralization kettle 12, and is mixed with the second liquid phase separated from the second solid-liquid separator 8 and then neutralized with the potassium hydroxide solution entering the second neutralization kettle 12. The by-product potassium sulfate is recovered after evaporation, crystallization and refining. Example

[0045] This embodiment provides a production device for substituted pyrazole acid compounds, and its structural schematic diagram is as follows Figure 5 As shown, the difference from Example 3 is that this embodiment also includes a distillation kettle 51 and a distillation tower 52 connected in series in sequence, the discharge port of the first neutralization kettle 4 is connected to the feed port of the distillation kettle 51, the light component outlet at the top of the distillation kettle 51 is connected to the feed port at the lower part of the distillation tower 52, the top water phase outlet of the distillation tower 52 is connected to the water phase inlet of the hydrolysis reaction unit 2, the heavy component outlet at the bottom of the distillation kettle 51 is connected to the feed port of the crystallization kettle 14, and the concentrated liquid outlet of the separator 133 is respectively connected to the tube side inlet of the heater 132 and the feed port of the crystallization kettle 14.

[0046] In specific implementation, on the basis of Example 3, in order to improve the separation efficiency and obtain high-purity DMF and water, on the basis of Example 3, the first neutralized liquid containing DMF, potassium sulfate and water enters the distillation kettle 51 for distillation, and the light component whose main components are water and DMF is separated from the light component outlet at the top of the distillation kettle 51. The light component at the top of the kettle enters the distillation tower 52, and after distillation, water is separated from the water phase outlet at the top of the tower to obtain water, and DMF is separated from the DMF outlet at the bottom of the tower to obtain DMF. The water separated at the top of the distillation tower 52 is returned to the hydrolysis reaction unit 2. In order to fully recover the by-product potassium sulfate, the heavy component whose main component is potassium sulfate is separated from the heavy component outlet at the bottom of the distillation kettle 51. It enters the crystallization kettle 14, is mixed with the concentrated liquid from the evaporation unit 13, and then cooled and crystallized. It is separated by the fourth solid-liquid separator 15 to obtain crude potassium sulfate. The crude potassium sulfate enters the refining kettle 16, is refined by the refining solvent, and then is sequentially separated by solid-liquid separation and dried to obtain the by-product potassium sulfate. Example

[0047] This embodiment provides a production device for substituted pyrazole acid compounds, and its structural schematic diagram is as follows Figure 6 As shown, the difference from Example 5 is that this embodiment is further provided with an ethanol recovery tower 19, a mixing kettle 20, and an ethanol distillation kettle 21, the solvent recovery unit 5 includes a distillation kettle 51 and a distillation tower 52 connected in series in sequence, the discharge port of the first neutralization kettle 4 is connected to the feed port of the distillation kettle 51, the heavy component outlet at the bottom of the distillation kettle 51 is connected to the feed port of the crystallization kettle 14, the light component outlet at the top of the distillation kettle 51 is connected to the feed port of the middle and lower part of the distillation tower 52, the top water phase outlet of the distillation tower 52 is connected to the water phase inlet of the hydrolysis reaction unit 2, the tower bottom DMF outlet of the distillation tower 52 is connected to the feed port of the mixing kettle 20, the ethanol outlet of the ethanol recovery tower 19 is connected to the feed port of the refining kettle 16, and the liquid phase outlet of the fifth solid-liquid separator 17 is connected to the inlet of the ethanol distillation kettle 21.

[0048] In the specific implementation, in order to realize the comprehensive utilization of solvent DMF, on the basis of Example 5, the first neutralized liquid containing DMF, potassium sulfate and water enters the distillation kettle 51 for distillation, and the light component whose main components are water and DMF is separated from the light component outlet of the kettle top of the distillation kettle 51. The light component at the top of the kettle enters the distillation tower 52 and is separated from the water phase outlet at the top of the tower after distillation to obtain water, and DMF is separated from the DMF outlet of the tower kettle to obtain DMF. The water separated at the top of the distillation tower 52 is returned to the hydrolysis reaction unit 2, and the DMF separated by distillation in the distillation tower 52 enters the mixing kettle 20 and is mixed with the mixture. The raw materials are mixed uniformly to prepare a slurry, and a heavy component whose main component is potassium sulfate is separated from the heavy component outlet at the bottom of the distillation kettle 51 and enters the crystallization kettle 14. The heavy component is mixed with the concentrated liquid from the evaporation unit 13 and then cooled and crystallized. The crude potassium sulfate is separated by the fourth solid-liquid separator 15 to obtain crude potassium sulfate. The crude potassium sulfate enters the refining kettle 16. The ethanol distilled from the ethanol recovery tower 19 is used as a refining solvent. The refined liquid is separated by the fifth solid-liquid separator 17. The separated liquid enters the ethanol distillation kettle 21 to distill and recover ethanol. The separated solid is dried in a dryer to obtain by-product potassium sulfate.

[0049] The above description is only a specific embodiment of the present disclosure, so that those skilled in the art can understand or implement the present disclosure. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present disclosure. Therefore, the present disclosure will not be limited to the embodiments described herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A production device for substituted pyrazole acid compounds, characterized in that: include: An oxidation reaction unit (1), a hydrolysis reaction unit (2), a first solid-liquid separator (3), an alkaline hydrolysis reaction unit (6), an acidification reaction unit (7), a second solid-liquid separator (8), a pulping kettle (9), a third solid-liquid separator (10), and a first dryer (11); The discharge port of the oxidation reaction unit (1) is connected to the feed port of the hydrolysis reaction unit (2), and the discharge port of the hydrolysis reaction unit (2) is connected to the feed port of the first solid-liquid separator (3); the solid phase outlet of the first solid-liquid separator (3) is connected to the alkaline hydrolysis reaction unit (6), the acidification reaction unit (7), and the second solid-liquid separator (8) in sequence, and the liquid phase outlet of the first solid-liquid separator (3) is connected to the first neutralization kettle (4) and the solvent recovery unit (5) in sequence; the solid phase outlet of the second solid-liquid separator (8) is connected to the pulping kettle (9), the third solid-liquid separator (10), and the first dryer (11) in sequence, and the liquid phase outlet of the second solid-liquid separator (8) is connected to the second neutralization kettle (12), the evaporation unit (13), the crystallization kettle (14), the fourth solid-liquid separator (15), the refining kettle (16), the fifth solid-liquid separator (17), and the second dryer (18) in sequence; The hydrolysis reaction unit (2) is provided with a water phase inlet, the first neutralization kettle (4), the alkaline hydrolysis reaction unit (6), and the second neutralization kettle (12) are all provided with a potassium hydroxide solution inlet, the acidification reaction unit (7) is provided with a sulfuric acid inlet, the pulping kettle (9) is provided with a pulping solvent inlet, and the refining kettle (16) is provided with a refining solvent inlet.

2. The production device of a substituted pyrazole acid compound according to claim 1, characterized in that: The solvent recovery unit (5) comprises a distillation kettle (51) and a distillation tower (52); The distillation kettle (51) is provided with a feed inlet, a light component outlet at the top of the kettle, and a heavy component outlet at the bottom of the kettle, and the rectification tower (52) is provided with a feed inlet, a water phase outlet at the top of the tower, and a DMF outlet at the bottom of the tower; The discharge port of the first neutralization kettle (4) is connected to the feed port of the distillation kettle (51), and the light component outlet at the top of the distillation kettle (51) is connected to the feed port of the distillation tower (52).

3. The production device of a substituted pyrazole acid compound according to claim 2, characterized in that: The heavy component outlet at the bottom of the distillation kettle (51) is connected to the feed inlet of the crystallization kettle (14).

4. The production device of a substituted pyrazole acid compound according to claim 2, characterized in that: The water phase outlet at the top of the distillation tower (52) is connected to the water phase inlet of the hydrolysis reaction unit (2).

5. The production device of a substituted pyrazole acid compound according to claim 2, characterized in that: Also includes a mixing kettle (20); The DMF outlet of the bottom of the distillation tower (52) is connected to the feed inlet of the mixing kettle (20).

6. The production device of a substituted pyrazole acid compound according to claim 1, characterized in that: The liquid phase outlet of the third solid-liquid separator (10) is connected to the feed inlet of the second neutralization kettle (12).

7. A production device for substituted pyrazole acid compounds according to any one of claims 1 to 6, characterized in that: The evaporation unit (13) includes a preheater (131), a heater (132), a separator (133), and a compressor (134); The discharge port of the second neutralization kettle (12) is connected to the tube side inlet of the preheater (131), the tube side outlet of the preheater (131) is connected to the tube side inlet of the heater (132), the tube side outlet of the heater (132) is connected to the feed port of the separator (133), the concentrated liquid outlet of the separator (133) is respectively connected to the tube side inlet of the heater (132) and the feed port of the crystallization kettle (14), the steam outlet of the separator (133) is connected to the shell side inlet of the heater (132) via the compressor (134), and the shell side outlet of the heater (132) is connected to the shell side inlet of the preheater (131).

8. The production device of a substituted pyrazole acid compound according to claim 7, characterized in that: Also included is an ethanol recovery tower (19); The ethanol recovery tower (19) is provided with a feed inlet, an ethanol outlet, and a water phase outlet; The shell side outlet of the preheater (131) is connected to the feed inlet of the ethanol recovery tower (19), and the water phase outlet of the ethanol recovery tower (19) is connected to the feed inlet of the pulping kettle (9).

9. The production device of a substituted pyrazole acid compound according to claim 8, characterized in that: The ethanol outlet of the ethanol recovery tower (19) is connected to the feed inlet of the refining kettle (16).

10. The production device of substituted pyrazole acid compounds according to claim 9, characterized in that: Also included is an ethanol still (21); The liquid phase outlet of the fifth solid-liquid separator (17) is connected to the feed inlet of the ethanol distillation kettle (21).

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