Device for producing o-fluoronitrobenzene and recovering catalyst

Abstract

The utility model provides a device for producing o-fluoronitrobenzene and recovering a catalyst. The device comprises a reaction kettle, a cooling kettle, a plate-and-frame filter, a rectifying tower and a finished product storage tank which are communicated, the reaction kettle is communicated with a DMF (Dimethyl Formamide) metering tank, an o-chloronitrobenzene metering tank and a potassium fluoride metering tank, and the reaction kettle is also provided with a catalyst adding port; a gas outlet of the reaction kettle is communicated with the first condenser through a reflux pipeline, and a liquid outlet of the first condenser is communicated with the reaction kettle; a gas outlet of the first condenser is sequentially communicated with an alkali spray tower and a water spray tower; a solid outlet of the plate-and-frame filter is communicated with the drying tank and the catalyst recovery tank; a filtrate outlet of the plate-and-frame filter communicates with the rectifying tower; a gas outlet of the rectifying tower is communicated with a solvent recovery tank and a finished product storage tank through a second condenser. According to the device, the catalyst in the reaction process can be recycled, the solvent can be recycled, tail gas generated in the production process is effectively treated, and the whole process is more environment-friendly.

Description

Technical Field

[0001] The utility model relates to the technical field of organic synthesis, and particularly relates to a device for producing o-fluoronitrobenzene and recovering a catalyst. Background Art

[0002] o-Fluoronitrobenzene is a commonly used chemical product. There are many patent literatures on the synthesis of o-fluoronitrobenzene, but most of the reactions have low conversion rates, many by-products, low solvent recovery rates, poor catalyst effects or expensive catalysts that are difficult to recover, resulting in high production costs of o-fluoronitrobenzene. For example, most processes for producing o-fluoronitrobenzene use sulfolane as a solvent, but the recovery of sulfolane is difficult, and the nitro compounds in it are prone to explosion at high temperatures. Using dimethyl sulfoxide as a solvent, the odor during the reaction is also difficult to solve, and the COD of the wastewater generated in the above process is also high, making the wastewater treatment difficult. Based on the above technical problems, it is necessary to provide a device for producing o-fluoronitrobenzene. Summary of the Utility Model

[0003] The technical problem to be solved by the utility model is: aiming at the deficiencies existing in the prior art, to provide a device for producing o-fluoronitrobenzene and recovering a catalyst. This device can not only recover the catalyst in the reaction process, but also recycle the solvent, and the tail gas generated in the production process is effectively treated, making the whole process more environmentally friendly.

[0004] To solve the above technical problem, the technical solution of the utility model is:

[0005] A device for producing o-fluoronitrobenzene and recovering a catalyst, including a reaction kettle, a cooling kettle, a plate and frame filter press, a rectification tower, and a finished product storage tank that are connected.

[0006] The reaction kettle is connected to a DMF metering tank, an o-chloronitrobenzene metering tank, and a potassium fluoride metering tank. The reaction kettle is also provided with a catalyst addition port. The gas outlet of the reaction kettle is connected to a first condenser through a reflux pipeline, and the liquid outlet of the first condenser is connected to the reaction kettle. The gas outlet of the first condenser is sequentially connected to an alkali spray tower and a water spray tower. The solid outlet of the plate and frame filter press is connected to a drying tank and a catalyst recovery tank. The filtrate outlet of the plate and frame filter press is connected to the rectification tower. The gas outlet of the rectification tower is connected to a solvent recovery tank and a finished product storage tank through a second condenser.

[0007] Preferably, a porous filter plate is provided at the gas outlet of the first condenser.

[0008] Preferably, cooling coils are provided in the cooling kettle.

[0009] Preferably, a first stirring device is provided inside the cooling kettle. The first stirring device includes a first stirring motor and a first stirring shaft connected to the output shaft of the first stirring motor. A plurality of first stirring blades are provided on the first stirring shaft; the cooling coil is sleeved outside the first stirring shaft and the first stirring blades.

[0010] Preferably, spray trays communicating with the spray liquid inlets are provided at the tops of both the water spray tower and the alkali spray tower.

[0011] Preferably, at least one porous liquid distribution plate is provided below the spray trays in both the water spray tower and the alkali liquid spray tower.

[0012] Preferably, a second stirring device is provided inside the drying tank. The second stirring device includes a second stirring motor, a hollow second stirring shaft connected to the output shaft of the second stirring motor, and a plurality of hollow second stirring blades communicating with the hollow second stirring shaft; the bottom end of the hollow second stirring shaft is communicated with a steam storage tank through a rotary joint.

[0013] Preferably, a plurality of porous flow disturbance plates are provided on the inner wall of the second condenser; the plurality of porous flow disturbance plates are arranged alternately.

[0014] Due to the adoption of the above technical solutions, the beneficial effects of the present utility model are:

[0015] The present utility model provides a device for producing o-fluoronitrobenzene and recovering a catalyst, including a reaction kettle, a cooling kettle, a plate and frame filter, a rectifying tower, and a finished product storage tank which are connected in series; the reaction kettle is connected to a DMF metering tank, an o-chloronitrobenzene metering tank, and a potassium fluoride metering tank, and a catalyst inlet is further provided on the reaction kettle; the gas outlet of the reaction kettle is connected to a first condenser through a reflux pipeline, and the liquid outlet of the first condenser is connected to the reaction kettle; the gas outlet of the first condenser is successively connected to an alkali spray tower and a water spray tower; the solid outlet of the plate and frame filter is connected to a drying tank and a catalyst recovery tank; the filtrate outlet of the plate and frame filter is connected to the rectifying tower; the gas outlet of the rectifying tower is connected to a solvent recovery tank and a finished product storage tank through a second condenser. This device can realize the recycling of the catalyst and the solvent during the production process, greatly reducing the production cost of the product; moreover, it can also treat the tail gas in the production to avoid environmental pollution.

[0016] A porous filter plate is provided at the gas outlet of the first condenser of this device. The setting of the porous filter plate can separate the liquid entrained in the gas, and the separated liquid re-enters the reaction kettle, which improves the product yield to a certain extent.

[0017] A cooling coil is provided inside the cooling kettle of this device, which greatly improves the contact efficiency between the condensed water and the liquid material, and thus improves the cooling efficiency.

[0018] Both the top of the water spray tower and the alkali spray tower of this device are provided with spray trays communicated with the spray liquid inlets; at least one porous liquid distribution plate is provided below the spray trays in the water spray tower and the alkali liquid spray tower. The combined setting of the porous liquid distribution plate and the spray tray will increase the contact efficiency between the spray liquid and the gas, thereby improving the spray absorption efficiency.

[0019] A plurality of porous flow disturbance plates are provided on the inner wall of the second condenser of this device; the plurality of porous flow disturbance plates are arranged staggered with each other, and the above setting can improve the condensation efficiency. Brief Description of the Drawings

[0020] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only the embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained according to the provided drawings.

[0021] Figure 1 It is a schematic structural diagram of Embodiment 1 of the present invention;

[0022] Figure 2 For Figure 1 The enlarged structural diagram at position A in

[0023] Figure 3 Is Figure 1 The enlarged structural diagram at position B in

[0024] In the figure, 1, reaction kettle; 2, cooling kettle; 3, plate and frame filter; 4, rectification tower; 5, finished product storage tank; 6, DMF metering tank; 7, o-chloronitrobenzene metering tank; 8, potassium fluoride metering tank; 9, catalyst addition port; 10, first condenser; 11, alkali spray tower; 12, water spray tower; 13, drying tank; 14, catalyst recovery tank; 15, second condenser; 16, solvent recovery tank; 17, cooling coil; 18, first stirring motor; 19, first stirring shaft; 20, first stirring blade; 21, porous filter plate; 22, spray tray; 23, porous liquid distribution plate; 24, second stirring motor; 25, hollow second stirring shaft; 26, hollow second stirring blade; 27, steam storage tank; 28, porous flow disturbance plate. Detailed Embodiments

[0025] In order to be able to more clearly understand the above-mentioned objects, features and advantages of the present invention, the following will further describe the solution of the present invention. It should be noted that, without conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other.

[0026] In the following description, numerous specific details are set forth to provide a thorough understanding of the present utility model. However, the present utility model may also be implemented in other ways different from those described herein. Obviously, the embodiments in the specification are only a part of the embodiments of the present utility model, rather than all of the embodiments.

[0027] Embodiment 1

[0028] As shown in the figure, a device for producing o-fluoronitrobenzene and recovering a catalyst includes a connected reaction kettle 1, a cooling kettle 2, a plate and frame filter 3, a rectifying column 4, and a finished product storage tank 5.

[0029] The reaction kettle 1 is connected to a DMF metering tank 6, an o-chloronitrobenzene metering tank 7, and a potassium fluoride metering tank 8. The reaction kettle 1 is also provided with a catalyst addition port 9. The gas outlet of the reaction kettle 1 is connected to a first condenser 10 through a reflux pipeline (not marked in the figure). The liquid outlet of the first condenser 10 is connected to the reaction kettle 1. The gas outlet of the first condenser 10 is successively connected to an alkali spray tower 11 and a water spray tower 12. The solid outlet of the plate and frame filter 3 is connected to a drying tank 13 and a catalyst recovery tank 14. The filtrate outlet of the plate and frame filter 3 is connected to the rectifying column 4. The gas outlet of the rectifying column 4 is connected to a solvent recovery tank 16 and a finished product storage tank 5 through a second condenser 15.

[0030] Based on the above settings, when preparing o-fluoronitrobenzene, a certain amount of DMF is added into the reaction kettle 1 as a solvent through the DMF metering tank 6, o-chloronitrobenzene is added as a raw material, potassium fluoride is added as a fluorinating agent, and tetramethylammonium chloride is added into the reaction kettle 1 as a catalyst through the catalyst addition port 9. The temperature is raised for reaction. The gas evolved during the reaction is condensed by the first condenser 10, and the condensed liquid enters the reaction kettle 1 through the reflux pipeline. The uncondensed gas is successively treated by the alkali spray tower 11 and the water spray tower 12. The reacted liquid is cooled by the cooling kettle 2 and then filtered by the plate and frame filter 3 to separate the catalyst from the reaction liquid. The catalyst enters the catalyst recovery tank 14 for reuse after being dried by the drying tank 13. The reaction liquid is rectified by the rectifying column 4, and the fractions at different temperatures are collected. After being condensed by the second condenser 15, they enter the solvent recovery tank 16 and the finished product storage tank 5 respectively.

[0031] Further, in this embodiment, a cooling coil 17 is provided in the cooling kettle 2, and a first stirring device is provided in the cooling kettle 2. The first stirring device includes a first stirring motor 18 and a first stirring shaft 19 connected to the output shaft of the first stirring motor 18. A plurality of first stirring blades 20 are provided on the first stirring shaft 19; the cooling coil 17 is sleeved outside the first stirring shaft 19 and the first stirring blades 20. Based on the above settings, when cooling the reaction liquid, condensed water is introduced into the cooling kettle 2 through the cooling coil 17, and the first stirring device is turned on. The first stirring shaft 19 and the first stirring blades 20 stir and cool the reaction liquid driven by the first stirring motor 18, greatly improving the cooling efficiency.

[0032] Further, in this embodiment, a porous filter plate 21 is provided at the gas outlet of the first condenser 10. The setting of the porous filter plate 21 can effectively separate the liquid entrained in the gas and improve the product yield.

[0033] Further, in this embodiment, spray trays 22 communicating with the spray liquid inlets are provided at the tops of the water spray tower 12 and the alkali spray tower 11; at least one porous liquid distribution plate 23 is provided below the spray trays 22 in the water spray tower 12 and the alkali spray tower 11. The setting of the spray trays 22 enables the spray liquid to uniformly enter the water spray tower 12 and the alkali spray tower 11 and fully contact the gas, improving the spray absorption efficiency; the setting of the porous liquid distribution plates 23 enables the gas to contact the spray liquid more fully, and further improves the gas absorption efficiency.

[0034] Further, in this embodiment, a second stirring device is provided in the drying tank 13. The second stirring device includes a second stirring motor 24, a hollow second stirring shaft 25 connected to the output shaft of the second stirring motor 24, and a plurality of hollow second stirring blades 26 communicating with the hollow second stirring shaft 25; the bottom end of the hollow second stirring shaft 25 is connected to a steam storage tank 27 through a rotary joint (not shown in the figure). Steam is introduced into the hollow second stirring shaft 25 and the hollow second stirring blades 26 through the steam storage tank 27. During the stirring process, the heated hollow second stirring shaft 25 and the hollow second stirring blades 26 are in full contact with the material, improving the drying efficiency.

[0035] Further, in this embodiment, a plurality of porous flow disturbance plates 28 are provided on the inner wall of the second condenser 16; the plurality of porous flow disturbance plates 28 are arranged in a staggered manner. The setting of the porous flow disturbance plates 28 can effectively improve the gas condensation efficiency.

[0036] It should be noted that for those of ordinary skill in the art, without departing from the principle of the present utility model, several improvements and modifications can still be made to the present utility model, and these improvements and modifications also fall within the scope of protection of the claims of the present utility model. The scope of protection of the present utility model patent is defined by the claims and may include other embodiments that can be conceived by those skilled in the art. If these other embodiments have structural elements similar to the literal description of the claims, or if they include equivalent structural elements that have no substantial difference from the literal description of the claims, then these other embodiments should also be included within the scope of the claims.

Claims

1. An apparatus for producing o-fluoronitrobenzene and recovering a catalyst, characterized in that: It includes a connected reactor, a cooling kettle, a plate and frame filter, a distillation column, and a finished product storage tank; The reactor is connected to a DMF metering tank, an o-chloronitrobenzene metering tank, and a potassium fluoride metering tank. A catalyst addition port is also provided on the reactor; the gas outlet of the reactor is connected to a first condenser through a reflux pipeline, and the liquid outlet of the first condenser is connected to the reactor; the gas outlet of the first condenser is successively connected to an alkali spray tower and a water spray tower; the solid outlet of the plate and frame filter is connected to a drying tank and a catalyst recovery tank; the filtrate outlet of the plate and frame filter is connected to the distillation column; the gas outlet of the distillation column is connected to a solvent recovery tank and a finished product storage tank through a second condenser.

2. The device for producing o-fluoronitrobenzene and recovering the catalyst according to claim 1, wherein: A porous filter plate is provided at the gas outlet of the first condenser.

3. The device for producing o-fluoronitrobenzene and recovering the catalyst according to claim 1, characterized in that: A cooling coil is provided in the cooling kettle.

4. An apparatus for producing o-fluoronitrobenzene and recovering a catalyst according to claim 3, characterized in that: A first stirring device is provided in the cooling kettle. The first stirring device includes a first stirring motor and a first stirring shaft connected to the output shaft of the first stirring motor. A plurality of first stirring blades are provided on the first stirring shaft; the cooling coil is sleeved outside the first stirring shaft and the first stirring blades.

5. The device for producing o-fluoronitrobenzene and recovering the catalyst according to claim 1, characterized in that: Spray trays communicated with the spray liquid inlet are provided at the tops of the water spray tower and the alkali spray tower.

6. The device for producing o-fluoronitrobenzene and recovering the catalyst according to claim 5, characterized in that: At least one porous liquid distribution plate is provided below the spray trays in the water spray tower and the alkali liquid spray tower.

7. An apparatus for producing o-fluoronitrobenzene and recovering a catalyst according to claim 1, characterized in that: A second stirring device is provided in the drying tank. The second stirring device includes a second stirring motor, a hollow second stirring shaft connected to the output shaft of the second stirring motor, and a plurality of hollow second stirring blades communicated with the hollow second stirring shaft; the bottom end of the hollow second stirring shaft is connected to a steam storage tank through a rotary joint.

8. The device for producing o-fluoronitrobenzene and recovering the catalyst according to claim 1, wherein: A plurality of porous flow disturbance plates are provided on the inner wall of the second condenser; the plurality of porous flow disturbance plates are arranged alternately.

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