Oxidation hydrolysis reaction system for substituted pyrazoline
By designing a replacement pyrazoline oxidation and hydrolysis reaction system with a variety of reactors and separators, the problems of high extra-added processing costs and low resource utilization efficiency in chemical production are solved, and clean production and resource recycling are achieved, and the protection of environment.
Patent Information
- Application Number
- CN202421216048.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-30
- Publication Date
- 2025-02-25
- Estimated Expiration
- 2034-05-30
AI Technical Summary
In chemical production, oxidation and hydrolysis reaction systems that replace pyrazoline have high extra-administered treatment costs and low resource utilization efficiency, and improper handling may damage the ecological environment.
A reaction system including oxidation reactor, hydrolysis reactor, acidification reactor, solid-liquid separator, distillation kettle, neutralization kettle, dryer and other equipment is designed to achieve clean production and reduce waste by optimizing the process and equipment connection. Salt and wastewater production and recycling by-products of potassium sulfate and ethanol.
It realizes clean production, reduces production costs, improves resource utilization efficiency, reduces waste generation, and protects the environment.
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Figure CN222518549U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of chemical equipment, and specifically relates to an oxidative hydrolysis reaction system for substituted pyrazoline. Background Art
[0002] 3-Bromo-1-(3-chloro-2-pyridinyl)-4,5-dihydro-1H-pyrazole-5-carboxylic acid ethyl ester (referred to as substituted pyrazoline) can be synthesized into 3-bromo-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxylic acid (referred to as substituted pyrazole acid) through oxidation reaction and hydrolysis reaction, which is mainly used as a key intermediate of diamide insecticides such as chlorantraniliprole and cyantraniliprole.
[0003] In general chemical production, the potassium salt in the reaction system after the oxidation reaction between substituted pyrazoline and the oxidant potassium persulfate is directly outsourced for treatment as hazardous waste. The high outsourcing treatment fee increases the production cost. When preparing substituted pyrazole acid through hydrolysis reaction, a large amount of alkali and acid is consumed, resulting in a large amount of ethanol-containing wastewater and waste salt. Directly discharging it as wastewater reduces the efficiency of resource utilization. If it is not handled properly, it will also damage the ecological environment. Utility Model Content
[0004] The utility model provides an oxidation hydrolysis reaction system for substituted pyrazoline with simple process, low production cost, green environmental protection and clean production. The system comprises an oxidation reactor, a first solid-liquid separator, a first distillation kettle, a hydrolysis reactor, an acidification reactor, a second solid-liquid separator, a first washing and separation unit and a first dryer; the solid phase outlet of the first solid-liquid separator and the liquid phase outlet of the second solid-liquid separator are both connected with the feed port of the neutralization kettle, the discharge port of the neutralization kettle is connected with the evaporation unit, the crystallization kettle, the third solid-liquid separator, the dissolution kettle, the fourth solid-liquid separator and the second dryer in sequence; the neutralization kettle is provided with a potassium hydroxide solution inlet, the hydrolysis reactor is provided with a hydrolysis reagent inlet, the acidification reactor is provided with a dilute sulfuric acid inlet, and the dissolution kettle is provided with a detergent inlet.
[0005] In an optional embodiment, the evaporation unit includes a primary steamer, a first distillation tower, and a second distillation tower; the discharge port of the neutralization kettle is connected to the feed port of the primary steamer, the top outlet of the primary steamer is connected to the middle and lower inlet of the first distillation tower, the bottom outlet of the primary steamer is connected to the feed port of the crystallization kettle, and the top outlet of the first distillation tower is connected to the middle and lower inlet of the second distillation tower; a solvent outlet is provided at the bottom of the first distillation tower, an ethanol outlet is provided at the top of the second distillation tower, and a recovered water outlet is provided on the upper side line of the second distillation tower.
[0006] In an optional embodiment, the first washing and separation unit includes a first washing kettle and a fifth solid-liquid separator; the discharge port of the first washing kettle is connected to the feed port of the fifth solid-liquid separator, the liquid phase outlet of the fifth solid-liquid separator is connected to the feed port of the neutralization kettle, and the solid phase outlet of the fifth solid-liquid separator is connected to the feed port of the first dryer.
[0007] In an optional embodiment, the recovery water outlet of the second distillation tower is connected to the feed inlet of the first washing tank.
[0008] In an optional embodiment, a second washing and separation unit is also provided; the second washing and separation unit includes a second washing kettle and a sixth solid-liquid separator; the discharge port of the second washing kettle is connected to the feed port of the sixth solid-liquid separator, the liquid phase outlet of the sixth solid-liquid separator is connected to the feed port of the neutralization kettle, and the solid phase outlet of the sixth solid-liquid separator is connected to the feed port of the hydrolysis reactor.
[0009] In an optional embodiment, the recovery water outlet of the second distillation tower is connected to the feed inlet of the second washing tank.
[0010] In an optional embodiment, a detergent recovery unit is also provided; the detergent recovery unit includes a second distillation kettle and a third distillation tower; the liquid phase outlet of the fourth solid-liquid separator is connected to the feed inlet of the second distillation kettle, the top outlet of the second distillation kettle is connected to the middle and lower inlet of the third distillation tower, and the top detergent outlet of the third distillation tower is connected to the inlet of the dissolution kettle.
[0011] In an optional embodiment, a first batching tank, a second batching tank, and a solvent recovery tank are further provided; the first batching tank is provided with a solvent inlet, a raw material liquid inlet, and a raw material liquid outlet; the second batching tank is provided with a solvent inlet, an oxidant inlet, and an oxidant outlet; the solvent recovery outlet of the first distillation kettle and the bottom solvent outlet of the first distillation tower are both connected to the inlet of the solvent recovery tank, the discharge port of the solvent recovery tank is connected to the solvent inlet of the first batching tank and the second batching tank, and the raw material liquid outlet of the first batching tank and the oxidant outlet of the second batching tank are both connected to the feed port of the oxidation reactor.
[0012] In an optional embodiment, it also includes a hydrolysis reagent preparation tank; the hydrolysis reagent preparation tank is provided with a potassium hydroxide inlet, a water inlet, and a hydrolysis reagent outlet; the hydrolysis reagent outlet of the hydrolysis reagent preparation tank is connected to the feed inlet of the hydrolysis reactor.
[0013] In an optional embodiment, the recovery water outlet of the second distillation tower is connected to the water inlet of the hydrolysis reagent preparation tank.
[0014] Compared with the prior art, the technical solution provided by the utility model has the following advantages:
[0015] 1. The reaction system provided by the utility model obtains the product substituted pyrazole acid after the substituted pyrazoline is subjected to oxidation reaction, hydrolysis reaction and acidification reaction in sequence, while reducing the generation of waste salt and waste water, recovering by-product potassium sulfate and ethanol, realizing clean production and improving the economic benefits of chemical production.
[0016] 2. By connecting the solid phase outlet of the first solid-liquid separator and the liquid phase outlet of the second solid-liquid separator to the inlet of the neutralization kettle, and then sequentially passing through the neutralization kettle, evaporation unit, crystallization kettle, third solid-liquid separator, dissolution kettle, fourth solid-liquid separator, and second dryer for neutralization, evaporation, crystallization, washing, separation, and drying, potassium sulfate salt with certain economic value is obtained, thereby avoiding the generation of waste salt.
[0017] 3. By setting up an evaporation unit, not only concentrated potassium salt is obtained, solvent DMF and water are recovered, but also high-purity ethanol that can be sold directly is recovered. The recovered water outlet of the second distillation tower is connected to the water inlet of the hydrolysis reagent preparation tank or to the inlet of the first washing kettle or to the inlet of the second washing kettle. It can prepare the hydrolysis reagent and return to the first washing and separation unit as a detergent, and can also return to the second washing and separation unit as a detergent, which reduces the generation of wastewater and saves resources.
[0018] 4. After the detergent dissolves and removes impurities from the crude sulfate, it enters the detergent recovery unit for recovery and then returns to the dissolution kettle for recycling. This not only obtains high-purity sulfate, but also realizes the application of detergents, reduces the generation of three wastes, and is also of positive significance to environmental protection, green and sustainable development. 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 reactor, 2-first solid-liquid separator, 3-first distillation kettle, 4-hydrolysis reactor, 5-acidification reactor, 6-second solid-liquid separator, 7-first washing separation unit, 71-first washing kettle, 72-fifth solid-liquid separator, 8-first dryer, 9-neutralization kettle, 10-evaporation unit, 101-primary steaming kettle, 102-first distillation tower, 103-second distillation tower, 11-crystallization kettle, 12-third solid-liquid separator, 13-dissolution kettle, 14-fourth solid-liquid separator, 15-second dryer, 16-second washing separation unit, 161-second washing kettle, 162-sixth solid-liquid separator, 17-detergent recovery unit, 171-second distillation kettle, 172-third distillation tower, 18-hydrolysis reagent preparation tank, 191-first batching tank, 192-second batching tank, 193-solvent recovery tank. 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, solid-liquid separator, distillation kettle, washing kettle, dryer, neutralization kettle, distillation tower, crystallization kettle, dissolution kettle, batching tank, solvent recovery tank and pipe fittings, valves, controller, feed pump, 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] In addition, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.
[0032] The utility model is further described below in conjunction with the accompanying drawings and embodiments.
[0033] Please refer to Figure 1-Figure 6 The utility model provides an oxidative hydrolysis reaction system for substituted pyrazoline. Example
[0034] This embodiment provides an oxidative hydrolysis reaction system for substituted pyrazoline, and its structural schematic diagram is shown in FIG. Figure 1 As shown, it includes an oxidation reactor 1, a first solid-liquid separator 2, a first distillation kettle 3, a hydrolysis reactor 4, an acidification reactor 5, a second solid-liquid separator 6, a first washing and separation unit 7, and a first dryer 8; the solid phase outlet of the first solid-liquid separator 2 and the liquid phase outlet of the second solid-liquid separator 6 are both connected to the feed port of the neutralization kettle 9, and the discharge port of the neutralization kettle 9 is connected to the evaporation unit 10, the crystallization kettle 11, the third solid-liquid separator 12, the dissolution kettle 13, the fourth solid-liquid separator 14, and the second dryer 15 in sequence; the neutralization kettle 9 is provided with a potassium hydroxide solution inlet, the hydrolysis reactor 4 is provided with a hydrolysis reagent inlet, the acidification reactor 5 is provided with a dilute sulfuric acid inlet, and the dissolution kettle 13 is provided with a detergent inlet.
[0035] In a specific implementation, the raw material substituted pyrazoline and the oxidant potassium persulfate enter an oxidation reactor 1 composed of a dynamic tubular reactor in the presence of a reaction solvent DMF to undergo an oxidation reaction to obtain an oxidized liquid containing substituted pyrazole acid esters. The oxidized liquid enters a first solid-liquid separator 2 for separation. The liquid phase separated from the first solid-liquid separator 2 enters a first distillation kettle 3. The solvent DMF is distilled off from the top of the first distillation kettle 3. The heavy components at the bottom of the first distillation kettle 3 enter a hydrolysis reactor 4 composed of a dynamic tubular reactor to undergo a hydrolysis reaction with a hydrolysis reagent potassium hydroxide solution to obtain a hydrolyzed liquid containing substituted pyrazole acid esters. The hydrolyzed liquid enters an acidification reactor 5 composed of a dynamic tubular reactor to react with dilute sulfuric acid to generate an acidified liquid containing substituted pyrazole acid, ethanol, potassium sulfate, sulfuric acid, and water. The acidified liquid enters a second solid-liquid separator 6 for separation. After the second solid-liquid separator is heated to 40 ℃, the reaction mixture is stirred for 2 hours. The solid phase separated by 6 enters the first washing and separation unit 7, and after washing, enters the first dryer 8 for drying to obtain the product substituted pyrazole acid. The solid phase containing mixed potassium salt and a small amount of DMF separated by the first solid-liquid separator 2 and the liquid phase containing ethanol, potassium sulfate, sulfuric acid and water separated by the second solid-liquid separator 6 enter the neutralization kettle 9 and undergo hydrolysis and neutralization reaction with potassium hydroxide solution under certain conditions. The formed neutralized liquid enters the evaporation unit 10 to evaporate water, ethanol and DMF. The obtained heavy components enter the crystallization kettle 11 for cooling and crystallization, and then enter the third solid-liquid separator 12 to separate crude potassium sulfate. The crude potassium sulfate enters the dissolution kettle 13 and is washed with detergent methanol to remove impurities on the surface of potassium sulfate, and then enters the fourth solid-liquid separator 14 to separate the solid phase and the liquid phase. The solid phase separated by the fourth solid-liquid separator 14 is dried by the second dryer 15 to obtain by-product potassium sulfate.
[0036] Furthermore, the oxidation reactor 1, the hydrolysis reactor 4 and the acidification reactor 5 are all dynamic tubular reactors. Example
[0037] This embodiment provides an oxidative hydrolysis reaction system for substituted pyrazoline, and its structural schematic diagram is shown in FIG. Figure 2 As shown, the difference from Example 1 is that in this embodiment, the evaporation unit 10 is composed of a primary steamer 101, a first distillation tower 102, and a second distillation tower 103, the outlet of the neutralization kettle 9 is connected to the inlet of the primary steamer 101, the heavy component outlet at the bottom of the primary steamer 101 is connected to the inlet of the crystallization kettle 11, the top outlet of the primary steamer 101 is connected to the middle and lower inlet of the first distillation tower 102, the top outlet of the first distillation tower 102 is connected to the middle and lower inlet of the second distillation tower 103, the bottom of the first distillation tower 102 is provided with a solvent outlet, the top of the second distillation tower 103 is provided with an ethanol outlet, and the upper side line of the second distillation tower 103 is provided with a recovered water outlet.
[0038] In specific implementation, on the basis of Example 1, the neutralized liquid of potassium sulfate, DMF, ethanol and water in the neutralization kettle 9 enters the primary steaming kettle 101 for concentration, the heavy components at the bottom of the kettle after concentration in the primary steaming kettle 101 enter the crystallization kettle 11 for cooling and crystallization, the light components of DMF, ethanol and water at the top of the primary steaming kettle 101 enter the first distillation tower 102 for distillation, the solvent DMF separated from the bottom of the first distillation tower 102 is recovered, the light components separated from the top of the first distillation tower 102 enter the second distillation tower 103, ethanol is recovered from the top of the second distillation tower 103, and water is recovered from the side line of the upper part of the second distillation tower 103, thereby improving the solvent separation efficiency. Example
[0039] This embodiment provides an oxidative hydrolysis reaction system for substituted pyrazoline, and its structural schematic diagram is shown in FIG. Figure 3 As shown, the difference from Example 2 is that in this embodiment, the first washing and separation unit 7 is composed of a first washing kettle 71 and a fifth solid-liquid separator 72, the solid phase outlet of the second solid-liquid separator 6 is connected to the inlet of the first washing kettle 71, the outlet of the first washing kettle 71 is connected to the inlet of the fifth solid-liquid separator 72, the solid phase outlet of the fifth solid-liquid separator 72 is connected to the inlet of the first dryer 8, the liquid phase outlet of the fifth solid-liquid separator 72 is connected to the inlet of the neutralization kettle 9, and the recovered water outlet of the second distillation tower 103 is connected to the inlet of the first washing kettle 71.
[0040] In specific implementation, on the basis of Example 2, the solid phase separated from the second solid-liquid separator 6 enters the first washing kettle 71, in which the acid and salt in the solid phase separated from the second solid-liquid separator 6 are dissolved and washed with the recovered water separated by the second distillation tower 103, and the washed solution enters the fifth solid-liquid separator 72 to separate the solid phase and the liquid phase, and the solid phase separated from the fifth solid-liquid separator 72 is dried to obtain the substituted pyrazole acid, and the liquid phase separated from the fifth solid-liquid separator 72 enters the neutralization kettle 9 to undergo a hydrolysis and neutralization reaction with the solid phase separated from the first solid-liquid separator 2, thereby further improving the purity of the substituted pyrazole acid. Example
[0041] This embodiment provides an oxidative hydrolysis reaction system for substituted pyrazoline, and its structural schematic diagram is shown in FIG. Figure 4As shown, the difference from Example 2 is that in this embodiment, a second washing and separation unit 16 is further provided between the distillation kettle 3 and the hydrolysis reactor 4, and the second washing and separation unit 16 is composed of a second washing kettle 161 and a sixth solid-liquid separator 12, the bottom outlet of the distillation kettle 3 is connected to the inlet of the second washing kettle 161, the outlet of the second washing kettle 161 is connected to the inlet of the sixth solid-liquid separator 162, the liquid phase outlet of the sixth solid-liquid separator 162 is connected to the inlet of the neutralization kettle 9, the solid phase outlet of the sixth solid-liquid separator 162 is connected to the inlet of the hydrolysis reactor 4, and the recovered water outlet of the second distillation tower 103 is connected to the inlet of the second washing kettle 161.
[0042] In specific implementation, in order to reduce the influence of mixed potassium salts on the reaction during the hydrolysis reaction, on the basis of Example 2, the heavy components at the bottom of the kettle separated by the first distillation kettle 3 enter the second washing kettle 161, and are pulped and washed with the recovered water of the second distillation tower 103. The washed solution enters the sixth solid-liquid separator 162 for separation, and the liquid phase containing the mixed potassium salt separated by the sixth solid-liquid separator 162 enters the neutralization kettle 9 for neutralization. After the solid phase containing the substituted pyrazole ester is separated by the sixth solid-liquid separator 162, it enters the hydrolysis reactor 4 to undergo a hydrolysis reaction with the hydrolysis reagent potassium hydroxide solution. Example
[0043] This embodiment provides an oxidative hydrolysis reaction system for substituted pyrazoline, and its structural schematic diagram is shown in FIG. Figure 5 As shown, the difference from Example 2 is that this embodiment is further provided with a detergent recovery unit 17, and the detergent recovery unit 17 is composed of a second distillation kettle 171 and a third distillation tower 172, the liquid phase outlet of the fourth solid-liquid separator 14 is connected to the inlet of the second distillation kettle 171, the top outlet of the second distillation kettle 171 is connected to the middle and lower inlet of the third distillation tower 172, and the top detergent outlet of the third distillation tower 172 is connected to the inlet of the dissolution kettle 13.
[0044] In specific implementation, on the basis of Example 2, the liquid phase separated by the fourth solid-liquid separator 14 enters the second distillation kettle 171 for distillation, the light components at the top of the kettle separated by the second distillation kettle 171 enter the third distillation tower 172 for distillation, and the light components at the top of the tower separated by the third distillation tower 172 enter the dissolution kettle 13 as a detergent to wash the impurities adsorbed by the crude potassium sulfate, thereby improving the utilization rate of the detergent. Example
[0045] This embodiment provides an oxidative hydrolysis reaction system for substituted pyrazoline, and its structural schematic diagram is shown in FIG. Figure 6As shown, the difference from Example 5 is that this embodiment is further provided with a first washing and separation unit 7, a second washing and separation unit 16, a hydrolysis reagent preparation tank 18, a first batching tank 191, a second batching tank 192, and a solvent recovery tank 193. The first washing and separation unit 7 is composed of a first washing kettle 71 and a fifth solid-liquid separator 72, and the second washing and separation unit 16 is composed of a second washing kettle 161 and a sixth solid-liquid separator 162.
[0046] In the specific implementation, in order to improve the utilization rate of the recovered solvent, realize the recycling of resources, improve economic benefits, and develop social benefits and environmental benefits together. On the basis of Example 5, the solvent DMF distilled from the top of the first distillation kettle 3 and the heavy component solvent DMF at the bottom of the tower separated by the first distillation tower 102 enter the solvent recovery tank 193 for recovery, and the recovered DMF is used as the solvent of the first batching tank 191 and the second batching tank 192 respectively. In the first batching tank 191, the recovered DMF and the raw material substituted pyrazoline are mixed into a raw material liquid. In the second batching tank 192, the recovered DMF and the oxidant are mixed into an oxidant solution. The raw material liquid and the oxidant solution enter the oxidation reactor 1, and an oxidation reaction occurs in the oxidation reactor 1. The heavy component at the bottom of the kettle after distillation in the first distillation kettle 3 and the recovered water separated by the second distillation tower 103 are washed and dissolved in the second washing kettle 161. After washing, they enter the sixth solid-liquid separator 162 for separation. The liquid phase separated by the sixth solid-liquid separator 162 enters the neutralization kettle 9 for neutralization, and the solid phase separated by the sixth solid-liquid separator 162 enters the In the hydrolysis reactor 4, the potassium hydroxide solution and the recovered water separated by distillation in the second distillation tower 103 are prepared into a hydrolysis reagent of a certain concentration in the hydrolysis reagent preparation tank 18. The hydrolysis reagent enters the hydrolysis reactor 4 and undergoes a hydrolysis reaction with the solid phase separated by the sixth solid-liquid separator 162. The hydrolyzed liquid enters the acidification reactor 5 and reacts with sulfuric acid to generate an acidified liquid containing substituted pyrazole acid. The acidified liquid enters the second solid-liquid separator 6 to separate the solid phase and the liquid phase. The solid phase separated by the second solid-liquid separator 6 enters the first washing kettle 71. In the first washing kettle 71, the solid phase separated by the second solid-liquid separator 6 is dissolved and washed by the recovered water of the second distillation tower 103. After washing, it enters the fifth solid-liquid separator 72. The solid phase separated by the fifth solid-liquid separator 72 is dried to obtain the product substituted pyrazole acid. The liquid phase separated by the fifth solid-liquid separator 72 enters the neutralization kettle 9 and undergoes a hydrolysis and neutralization reaction with the oxidant separated by the first solid-liquid separator 2.
[0047] 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 substituted pyrazoline oxidative hydrolysis reaction system, characterized in that: include: An oxidation reactor (1), a first solid-liquid separator (2), a first distillation kettle (3), a hydrolysis reactor (4), an acidification reactor (5), a second solid-liquid separator (6), a first washing and separation unit (7), and a first dryer (8); The solid phase outlet of the first solid-liquid separator (2) and the liquid phase outlet of the second solid-liquid separator (6) are both connected to the feed port of the neutralization kettle (9), and the discharge port of the neutralization kettle (9) is sequentially connected to the evaporation unit (10), the crystallization kettle (11), the third solid-liquid separator (12), the dissolution kettle (13), the fourth solid-liquid separator (14), and the second dryer (15); The neutralization kettle (9) is provided with an inlet for potassium hydroxide solution, the hydrolysis reactor (4) is provided with an inlet for hydrolysis reagent, the acidification reactor (5) is provided with an inlet for dilute sulfuric acid, and the dissolution kettle (13) is provided with an inlet for detergent.
2. The oxidative hydrolysis reaction system of a substituted pyrazoline according to claim 1, characterized in that: The evaporation unit (10) comprises a primary distillation kettle (101), a first distillation tower (102), and a second distillation tower (103); The discharge port of the neutralization kettle (9) is connected to the feed port of the primary steam kettle (101), the top outlet of the primary steam kettle (101) is connected to the middle and lower inlet of the first distillation tower (102), the bottom outlet of the primary steam kettle (101) is connected to the feed port of the crystallization kettle (11), and the top outlet of the first distillation tower (102) is connected to the middle and lower inlet of the second distillation tower (103); A solvent outlet is provided at the bottom of the first distillation tower (102), an ethanol outlet is provided at the top of the second distillation tower (103), and a recovered water outlet is provided at the side line of the upper part of the second distillation tower (103).
3. The oxidative hydrolysis reaction system of a substituted pyrazoline according to claim 2, characterized in that: The first washing and separation unit (7) comprises a first washing tank (71) and a fifth solid-liquid separator (72); The discharge port of the first washing kettle (71) is connected to the feed port of the fifth solid-liquid separator (72), the liquid phase outlet of the fifth solid-liquid separator (72) is connected to the feed port of the neutralization kettle (9), and the solid phase outlet of the fifth solid-liquid separator (72) is connected to the feed port of the first dryer (8).
4. The oxidative hydrolysis reaction system of a substituted pyrazoline according to claim 3, characterized in that: The recovered water outlet of the second distillation tower (103) is connected to the feed inlet of the first washing tank (71).
5. The oxidative hydrolysis reaction system of a substituted pyrazoline according to claim 2, characterized in that: A second washing and separation unit (16) is also provided; The second washing and separation unit (16) comprises a second washing tank (161) and a sixth solid-liquid separator (162); The discharge port of the second washing tank (161) is connected to the feed port of the sixth solid-liquid separator (162), the liquid phase outlet of the sixth solid-liquid separator (162) is connected to the feed port of the neutralization tank (9), and the solid phase outlet of the sixth solid-liquid separator (162) is connected to the feed port of the hydrolysis reactor (4).
6. The oxidative hydrolysis reaction system of a substituted pyrazoline according to claim 5, characterized in that: The recovered water outlet of the second distillation tower (103) is connected to the feed inlet of the second washing kettle (161).
7. The oxidative hydrolysis reaction system of a substituted pyrazoline according to claim 1 or 2, characterized in that: A detergent recovery unit (17) is also provided; The detergent recovery unit (17) includes a second distillation kettle (171) and a third distillation tower (172); The liquid phase outlet of the fourth solid-liquid separator (14) is connected to the feed inlet of the second distillation kettle (171), the top outlet of the second distillation kettle (171) is connected to the middle and lower inlet of the third distillation tower (172), and the top detergent outlet of the third distillation tower (172) is connected to the inlet of the dissolution kettle (13).
8. The oxidative hydrolysis reaction system of a substituted pyrazoline according to claim 2, characterized in that: A first batching tank (191), a second batching tank (192), and a solvent recovery tank (193) are also provided; The first batching tank (191) is provided with a solvent inlet, a raw material liquid inlet, and a raw material liquid outlet; The second batching tank (192) is provided with a solvent inlet, an oxidant inlet, and an oxidant outlet; The solvent recovery outlet of the first distillation kettle (3) and the bottom solvent outlet of the first distillation tower (102) are both connected to the inlet of the solvent recovery tank (193), the discharge port of the solvent recovery tank (193) is connected to the solvent inlets of the first batching tank (191) and the second batching tank (192), and the raw liquid outlet of the first batching tank (191) and the oxidant outlet of the second batching tank (192) are both connected to the feed port of the oxidation reactor (1).
9. The oxidative hydrolysis reaction system of a substituted pyrazoline according to claim 2, characterized in that: Also included is a hydrolysis reagent preparation tank (18); The hydrolysis reagent preparation tank (18) is provided with a potassium hydroxide inlet, a water inlet, and a hydrolysis reagent outlet; The hydrolysis reagent outlet of the hydrolysis reagent preparation tank (18) is connected to the feed inlet of the hydrolysis reactor (4).
10. The oxidative hydrolysis reaction system of substituted pyrazoline according to claim 9, characterized in that: The recovered water outlet of the second distillation tower (103) is connected to the water inlet of the hydrolysis reagent preparation tank (18).