Preparation kettle for 2, 6-diethylaniline catalyst

Abstract

The utility model discloses a 2, 6-diethylaniline catalyst preparation kettle which comprises a preparation kettle, a stirrer and an aluminum powder metering tank, the preparation kettle comprises a kettle body and a kettle cover, the stirrer is rotatably installed on the kettle cover and is driven by a motor installed above the kettle cover to rotate, the kettle cover is provided with an eyepiece, a feed port I and a feed port II, and the eyepiece is connected with the feed port I and the feed port II. The eyepiece is used for observing the internal condition of the preparation kettle; the feeding port I is connected with an aniline storage tank through a feeding pipeline, a flow meter is arranged in the feeding pipeline, the feeding port II is connected with an aluminum powder metering tank through a charging pipeline, a stop valve is arranged in the charging pipeline, and a weight sensor is arranged at the bottom of the aluminum powder metering tank; compared with the prior art, the preparation kettle disclosed by the utility model is simple in overall structure, the addition amount of aluminum powder can be accurately controlled according to the amount of aniline, and agglomeration in the stirring process can be effectively avoided by adopting the ultrasonic generator, so that a product is uniformly dispersed and stable in performance.

Description

TECHNICAL FIELD

[0001] The utility model relates to chemical equipment technical field, concretely is a kind of 2.6-diethyl aniline catalyst preparation kettle. BACKGROUND

[0002] 2.6-diethyl aniline is an important pesticide, dye and pharmaceutical intermediate, is the production raw material of amide herbicide amide, butachlor and propachlor. Meanwhile, 2.6-diethyl aniline can also be used as polymer catalyst, plasticizer, flame retardant and antioxidant etc. In 2.6-diethyl aniline synthesis process, can use p-hydroxyacetophenone as raw material, and ethanol and ammonia are reacted, then after rearrangement, product is obtained by refining etc.;Also can use o-nitrobenzene as raw material, through reduction, amination, rearrangement etc. to obtain product. The steps of the above two methods are complicated, product yield is low, and cost is relatively high. Another process is that aniline and aluminum powder are reacted to produce aniline aluminum catalyst complex, then carry out alkylation reaction and hydrolysis reaction to obtain product. The above method is relatively simple, yield is high, cost is low, and has become the mainstream process in industry.

[0003] But the above process in 2.6-diethyl aniline catalyst complex preparation process, due to aniline and aluminum powder are solid-liquid reaction, in the reaction process, easy to produce agglomeration, product is not evenly dispersed, and performance is unstable, and then affect the conversion rate and yield of subsequent alkylation reaction, thereby make cost increase. In addition, if the amount of aluminum powder and aniline cannot be accurately controlled, it will also cause low aniline conversion rate, increase subsequent separation cost, for this purpose, the utility model provides a kind of 2.6-diethyl aniline catalyst preparation kettle. UTILITY MODEL CONTENT

[0004] The utility model aims at providing a kind of 2.6-diethyl aniline catalyst preparation kettle to solve the problems raised in the above background technology.

[0005] To achieve the above object, the utility model provides the following technical scheme: a kind of 2.6-diethyl aniline catalyst preparation kettle, including preparation kettle, agitator, aluminum powder metering tank, the preparation kettle includes kettle body and kettle cover, the agitator is rotatably installed on kettle cover, and agitator is driven to rotate by motor installed above kettle cover, be equipped with ocular lens, feed inlet I and feed inlet II on the kettle cover, the ocular lens is used to observe the inside situation of preparation kettle;

[0006] The feed inlet I is connected with aniline storage tank by feed pipe, flowmeter is arranged in the feed pipe, the feed inlet II is connected with aluminum powder metering tank by feeding pipe, cut-off valve is arranged in the feeding pipe, the bottom of the aluminum powder metering tank is provided with weight sensor, the flowmeter and weight sensor are electrically connected with the cut-off valve by controller;For controlling the flow of aluminum powder flowing into preparation kettle.

[0007] As a preferred technical solution of this utility model, the stirrer is configured as an anchor frame stirrer, and the distance between the bottom of the anchor frame stirrer and the bottom of the preparation vessel is 1 / 6 to 2 / 6 of the height of the preparation vessel.

[0008] As a preferred technical solution of this utility model, an ultrasonic generator is provided on the inner wall of the vessel.

[0009] As a preferred technical solution of this utility model, a discharge port is provided at the bottom of the vessel body, and a switch control valve is provided at the discharge port.

[0010] As a preferred technical solution of this utility model, the top of the preparation vessel is also provided with a steam riser, which is connected to a condensation reflux component through a pipe, and a hydrogen buffer tank is connected to the end of the condensation reflux component away from the steam riser.

[0011] As a preferred technical solution of this utility model, the hydrogen buffer tank is equipped with a pressure self-control instrument circuit.

[0012] As a preferred technical solution of this utility model, the outer periphery of the vessel body is covered with a jacket layer, the bottom of the jacket layer is provided with an oil inlet, the upper end of the jacket layer is provided with an oil outlet, and the oil outlet is connected to the oil inlet in sequence through a temperature-controlled oil tank and a circulating pump.

[0013] Compared with the prior art, the beneficial effects of this utility model are:

[0014] 1. This utility model uses a flow meter installed in the feed pipe connected to the feed inlet I of the preparation vessel to measure the amount of aniline entering the preparation vessel. By installing a weight sensor at the bottom of the aluminum powder metering tank, the flow meter transmits the detected aniline flow rate and the real-time aluminum powder addition signal detected by the weight sensor to the controller. The controller controls the opening and closing of the shut-off valve according to the ratio between aniline and aluminum powder. When the weight change of the weight sensor and the data detected by the flow meter reach the set value, the shut-off valve closes, stopping the feeding into the preparation vessel, thus improving the accuracy of the ratio and maintaining the stability of product performance.

[0015] 2. This utility model, by incorporating a pressure self-control instrument circuit within the hydrogen buffer tank, can maintain stable pressure, which is beneficial to the operational safety of the reaction.

[0016] 3. This invention, by installing an ultrasonic generator on the inner wall of the preparation vessel, prevents the mixture from agglomerating during stirring, ensuring uniform product dispersion and stable performance. The stirrer is an anchor-frame type, which provides more thorough mixing, further improving product quality.

[0017] In conclusion, the preparation kettle has simple overall structure, can accurately control the adding amount of aluminum powder according to the amount of aniline, and can effectively avoid agglomeration in the stirring process by using the ultrasonic generator, so that the product is uniformly dispersed and has stable performance.

[0018] Other features and advantages of the present application will be described in detail in the following specific embodiments. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 It is an overall structure schematic diagram of the present application;

[0020] In the figure: 1. Preparation kettle, 2. Stirrer, 3. Aluminum powder metering tank, 4. Kettle cover, 5. Eyepiece, 6. Inlet I, 7. Inlet II, 8. Aniline storage tank, 9. Flow meter, 10. Shut-off valve, 11. Weight sensor, 12. Kettle body, 13. Ultrasonic generator, 14. Discharge port, 15. Steam inlet, 16. Condensation reflux part, 17. Hydrogen buffer tank, 18. Jacket layer, 19. Oil inlet, 20. Oil outlet, 21. Temperature control oil tank, 22. Circulating pump. DETAILED DESCRIPTION

[0021] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0022] In the description of the present application, it should be pointed out that the orientations or positional relationships indicated by the terms "vertical", "upper", "lower", "horizontal" and the like are based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and therefore cannot be understood as indicating or implying that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application.

[0023] In the description of the present application, it should be pointed out that, unless otherwise explicitly specified and limited, the terms "arrangement", "installation", "connection", "connection" should be broadly understood, for example, it can be fixedly connected, or it can be detachably connected, or integrally connected; it can be mechanically connected, or it can be electrically connected; it can be directly connected, or it can be indirectly connected through an intermediate medium, or it can be connected inside two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0024] Please refer to Figure 1In the embodiment, a 2.6-diethyl aniline catalyst preparation kettle is provided, which comprises a preparation kettle 1, a stirrer 2, and an aluminum powder metering tank 3. The preparation kettle 1 comprises a kettle body 12 and a kettle cover 4. The stirrer 2 is rotatably installed on the kettle cover 4 and is driven to rotate by a motor installed above the kettle cover 4. The kettle cover 4 is provided with an ocular lens 5, a feeding port I 6, and a feeding port II 7. The ocular lens 5 is used to observe the internal condition of the preparation kettle. The outer periphery of the kettle body 12 is wrapped with a jacket layer 18. The bottom of the jacket layer 18 is provided with an oil inlet 19. The upper end of the jacket layer 18 is provided with an oil outlet 20. The oil outlet 20 is connected with the oil inlet 19 in sequence through a temperature control oil tank 21 and a circulating pump 22. The feeding port I 6 is connected with an aniline storage tank 8 through a feeding pipeline. A flow meter 9 is arranged in the feeding pipeline. The feeding port II 7 is connected with the aluminum powder metering tank 3 through a feeding pipeline. A shut-off valve 10 is arranged in the feeding pipeline. The bottom of the aluminum powder metering tank 3 is provided with a weight sensor 11. The flow meter 9 and the weight sensor 11 are electrically connected with the shut-off valve 10 through a controller. The controller is used to control the flow of the aluminum powder flowing into the preparation kettle 1. The bottom of the kettle body 12 is provided with a discharge port 14. A switch control valve is arranged at the discharge port 14. An ultrasonic generator 13 is arranged on the inner wall of the kettle body 12. The ultrasonic generator can be independently controlled. The working frequency is 10-80 KHz, and the power is 300-3000 W. After the aniline and the aluminum powder enter the kettle body 12, the stirrer 2 and the ultrasonic generator 13 are started. After the stirring of the stirrer 2 is stopped, the ultrasonic wave is continuously used for 5-20 min. The use of the ultrasonic wave can prevent the agglomeration during the stirring process. The product is uniformly dispersed, and the performance is stable. After the ultrasonic wave is stopped, the catalyst complex can be discharged by opening the switch control valve of the discharge port 14. The controller can be set as a PLC control unit. The flow meter 9 transmits the flow of the aniline detected and the addition amount signal of the aluminum powder detected by the weight sensor 11 to the controller. The controller controls the on-off of the shut-off valve according to the ratio of the aniline and the aluminum powder. When the weight change of the weight sensor and the data detected by the flow meter reach the set value, the shut-off valve is closed, and the feeding into the preparation kettle is stopped. The accuracy of the ratio is improved, and the stability of the product performance can be maintained.

[0025] In the embodiment, the stirrer 2 is an anchor frame stirrer. The distance between the bottom of the anchor frame stirrer and the bottom end of the preparation kettle 1 is 1 / 6 to 2 / 6 of the height of the preparation kettle 1. The anchor frame stirrer has a relatively solid structure and can stir a large amount of material. The anchor frame stirrer is particularly suitable for materials with large viscosity and large processing capacity, especially materials containing solids, so that the reactants can be fully mixed.

[0026] In the embodiment, the top of the preparation kettle 1 is further provided with a steam outlet 15 connected with a condensing reflux component 16 through a pipeline, the end of the condensing reflux component 16 away from the steam outlet 15 is connected with a hydrogen buffer tank 17, the boiling aniline is refluxed through the condensing reflux component 16 above the preparation kettle, the generated hydrogen enters the hydrogen buffer tank 17 after passing through the condensing reflux component 16, the condensing reflux component 16 is a common condensing reflux device, a reflux container component is connected with the hydrogen buffer tank 17 through a pipeline, and the hydrogen buffer tank 17 is provided with a pressure self-control instrument circuit, so that the pressure can be kept stable, and the operation safety of the reaction is favorable.

[0027] In summary, the preparation kettle has simple overall structure, the addition amount of the aluminum powder can be accurately controlled according to the amount of the aniline, the pressure self-control instrument circuit is arranged in the hydrogen buffer tank, so that the pressure can be kept stable, and the operation safety of the reaction is favorable, the ultrasonic wave is adopted, so that no agglomeration and bubbles are generated in the stirring process, the product is uniformly dispersed, and the performance is stable.

[0028] The basic principle and main features of the utility model and the advantages of the utility model are shown and described above. It should be understood by the person skilled in the art that the utility model is not limited by the above-mentioned embodiments, the above-mentioned embodiments and the description in the specification only illustrate the principle of the utility model, various changes and improvements of the utility model can be made without departing from the spirit and scope of the utility model, and these changes and improvements all fall within the scope of the utility model claimed. The protection scope of the utility model is defined by the appended claims and equivalents thereof.

Claims

1. A reactor for preparing a 2,6-diethylaniline catalyst, characterized in that, The equipment includes a preparation vessel (1), a stirrer (2), and an aluminum powder metering tank (3). The preparation vessel (1) includes a vessel body (12) and a vessel lid (4). The stirrer (2) is rotatably mounted on the vessel lid (4) and is driven to rotate by a motor mounted above the vessel lid (4). The vessel lid (4) is provided with an eyepiece (5), a feed inlet I (6), and a feed inlet II (7). The eyepiece (5) is used to observe the internal condition of the preparation vessel. The feed inlet I (6) is connected to the aniline storage tank (8) through the feed pipe. A flow meter (9) is installed in the feed pipe. The feed inlet II (7) is connected to the aluminum powder metering tank (3) through the feeding pipe. A shut-off valve (10) is installed in the feeding pipe. A weight sensor (11) is installed at the bottom of the aluminum powder metering tank (3). The flow meter (9) and the weight sensor (11) are electrically connected to the shut-off valve (10) through a controller. This is used to control the flow rate of aluminum powder flowing into the preparation vessel (1).

2. The reactor for preparing 2,6-diethylaniline catalyst according to claim 1, characterized in that, The stirrer (2) is configured as an anchor frame stirrer, and the distance between the bottom of the anchor frame stirrer and the bottom of the preparation vessel (1) is 1 / 6 to 2 / 6 of the height of the preparation vessel (1).

3. The reactor for preparing 2,6-diethylaniline catalyst according to claim 1, characterized in that, An ultrasonic generator (13) is provided on the inner wall of the vessel body (12).

4. The reactor for preparing 2,6-diethylaniline catalyst according to claim 1, characterized in that, The bottom of the vessel body (12) is provided with a discharge port (14), and a switch control valve is provided at the discharge port (14).

5. The reactor for preparing 2,6-diethylaniline catalyst according to claim 1, characterized in that, The top of the preparation vessel (1) is also provided with a steam riser (15), which is connected to a condensation reflux component (16) through a pipe. The end of the condensation reflux component (16) away from the steam riser (15) is connected to a hydrogen buffer tank (17).

6. The reactor for preparing 2,6-diethylaniline catalyst according to claim 5, characterized in that, The hydrogen buffer tank (17) is equipped with a pressure self-control instrument circuit.

7. The reactor for preparing 2,6-diethylaniline catalyst according to claim 1, characterized in that, The outer periphery of the vessel body (12) is covered with a jacket layer (18). An oil inlet (19) is provided at the bottom of the jacket layer (18), and an oil outlet (20) is provided at the upper end of the jacket layer (18). The oil outlet (20) is connected to the oil inlet (19) in sequence through a temperature-controlled oil tank (21) and a circulating pump (22).

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