A reaction device for Grignard reaction

Abstract

The utility model relates to a reaction device for Grignard reaction, which comprises: a Grignard reagent batching kettle; a Grignard reactor, wherein the Grignard reactor comprises a reactor body, a second jacket formed on the outer wall of the reactor body, a second agitator rotatably mounted in the reactor body and extending to the outside thereof, a second motor mounted on the top of the reactor body and connected to the second agitator, a plurality of second feed ports opened on the top of the reactor body, and a second discharge valve mounted on the bottom of the reactor body; a feed delivery component, wherein the feed delivery component comprises a feed delivery pipe connecting the first discharge valve and any of the second feed ports, a first flow meter mounted on the feed delivery pipe, and a first regulating valve mounted on the feed delivery pipe and located downstream of the first flow meter. In this way, the problems of overheating (i.e., energy accumulation) and spraying that may exist when a single reactor is used can be avoided.

Description

Technical Field

[0001] The utility model belongs to the field of chemical equipment and relates to a reaction device, in particular to a reaction device for Grignard reaction. Background Art

[0002] The reaction device is a container that can carry out physical or chemical reactions. Through the structural design and parameter configuration of the container, the heating, evaporation, cooling and low-speed mixing functions required by the process are realized. The reaction device is widely used in the fields of petroleum, chemical industry, rubber, pesticide, dye, medicine and food. It is a container used to complete the process of vulcanization, nitration, hydrogenation, hydrocarbonization, polymerization, condensation, etc. It can include structures such as reactors, reaction pots, decomposition pots and polymerization kettles.

[0003] The Grignard reaction (also known as the Grignard reaction) is one of the most basic and important carbon-carbon bond forming reactions in organic chemistry. It was discovered by the French chemist Victor Grignard, hence the name. The essence of the Grignard reaction is to generate new carbon-carbon bonds through the addition reaction of the Grignard reagent (an organic magnesium halide) with various common electrophilic reagents such as aldehydes, ketones, imines, esters, epoxides, carbon dioxide, etc. This reaction plays a vital role in organic synthesis and drug synthesis.

[0004] The Grignard reaction has the processes of heating, initiation, dripping, and heat preservation. Since there is energy accumulation in the reaction, accidents may occur, so it must be initiated first; traditional initiation is completed manually using a quantitative initiation tank (fixed liquid level or quantity), and then manually judge whether the initiation is successful, and then decide whether to drip; the dripping process cannot be too fast, otherwise it will cause accumulation, and then rush and explode. The Chinese utility model patent with the authorization announcement number CN220573475U discloses a reaction device of phenyl magnesium chloride, including a reactor with a stirring device, a plurality of inlets are provided on the reactor, an initiator feed pipe, a magnesium chip feeding hopper, a first stock liquid metering tank and a second stock liquid metering tank are respectively connected to the corresponding inlets for feeding, a circulating discharge port and a circulating feed port are provided at the bottom of the reactor, and the circulating discharge port, an external circulating pump and a circulating feed port are connected by a pipeline, and the reaction liquid is circulated by the circulating pump to facilitate the reaction, and a tank jet mixer is provided on the reactor inside the circulating feed port, and the outlet connecting pipe of the external circulating pump is connected to the inlet of the built-in tank jet mixer. This application also accurately measures various raw materials of phenylmagnesium chloride and feeds them into a single reactor, which cannot solve the problem of energy accumulation. Summary of the invention

[0005] The utility model aims to provide a reaction device for Grignard reaction in order to overcome the shortcomings of the prior art.

[0006] In order to achieve the above object, the technical solution adopted by the utility model is: a reaction device for Grignard reaction, which comprises:

[0007] A Grignard reagent batching kettle, the Grignard reagent batching kettle comprising a batching kettle body, a first jacket formed on the inner wall of the batching kettle body, a first agitator rotatably mounted in the batching kettle body and extending to the outside thereof, a first motor mounted on the top of the batching kettle body and connected to the first agitator, a plurality of first feeding ports provided on the top of the batching kettle body, and a first discharge valve mounted on the bottom of the batching kettle body;

[0008] A Grignard reactor, comprising a reactor body, a second jacket formed on the inner wall of the reactor body, a second agitator rotatably mounted in the reactor body and extending to the outside thereof, a second motor mounted on the top of the reactor body and connected to the second agitator, a plurality of second feed ports provided on the top of the reactor body, and a second discharge valve mounted on the bottom of the reactor body;

[0009] A material delivery component, the material delivery component includes a material delivery pipe connecting the first discharge valve and any of the second feed ports, a first flow meter installed on the material delivery pipe, and a first regulating valve installed on the material delivery pipe and located downstream of the first flow meter.

[0010] Optimally, the material delivery assembly further comprises a material delivery branch pipe which is in communication with the material delivery pipe and connected in parallel with the first regulating valve, and a third regulating valve is installed on the material delivery branch pipe.

[0011] Furthermore, the material delivery assembly also includes two second regulating valves installed on the material delivery pipe and located upstream and downstream of the first regulating valve, and the two second regulating valves are both located downstream of the first flow meter.

[0012] Furthermore, the two second regulating valves are connected in parallel with the third regulating valve.

[0013] Optimally, the Grignard reactor further comprises a temperature sensor disposed in the reactor body and an alarm temperature control circuit connected to the temperature sensor and the second motor.

[0014] Furthermore, it also includes:

[0015] a control module, the control module comprising a stirring sensor for detecting the state of the second stirrer and a control unit communicating with the stirring sensor and connected to the alarm temperature control loop,

[0016] The control unit is also connected to the first discharge valve, the first regulating valve and the first flow meter respectively.

[0017] Furthermore, the Grignard reactor further comprises a flow indicating interlocking flow meter connected to the first flow meter, and the control unit is connected to the first flow meter via the flow indicating interlocking flow meter.

[0018] Furthermore, the first jacket and the second jacket are independently provided with a temperature control TCU unit, and the control unit is connected to the temperature control TCU unit.

[0019] Due to the application of the above technical scheme, the utility model has the following advantages compared with the prior art: the reaction device of the Grignard reaction of the utility model, by adding a Grignard reagent batching kettle and using a material feeding component with a specific structure to connect the Grignard reagent batching kettle and the Grignard reactor, can avoid the problems of overheating (i.e., energy accumulation) and material spraying that may exist when using a single reactor; and can timely cut off the connection between the Grignard reagent batching kettle and the Grignard reactor to avoid danger. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a structural schematic diagram of a reaction device for Grignard reaction of the utility model. DETAILED DESCRIPTION

[0021] The utility model is further described below in conjunction with the embodiments shown in the accompanying drawings.

[0022] like Figure 1 The reaction device of the Grignard reaction shown mainly includes a Grignard reagent batching kettle 1, a Grignard reaction kettle 2, a material feeding component 3, etc.

[0023] The Grignard reagent batching kettle 1 comprises a batching kettle body 11, a first jacket 12 formed on the outer wall of the batching kettle body 11 (for example, a cooling medium is introduced into the first jacket 12 to reduce the temperature of the batching kettle body 11), a first agitator 10 rotatably mounted in the batching kettle body 11 and extending to the outside thereof (for example, a bearing is mounted at the contact point between the first agitator 10 and the batching kettle body 11, and a conventional sealing method (such as a liquid seal, an air seal or other conventional structural seal) is used to ensure that they are in a sealed state), and a first agitator 10 mounted on the top of the batching kettle body 11 and connected to the first agitator 10. A motor 13 (when the first motor 13 is working, it can drive the first agitator 10 to rotate; the connection between the first motor 13 and the first agitator 10 can be achieved by a coupling or a reducer, etc.), a plurality of first feeding ports 14 opened on the top of the batching kettle body 11 (the specific number of the first feeding ports 14 is usually greater than the types of raw materials for the Grignard reaction, so that the redundant first feeding ports 14 can be used to install some necessary detection instruments, such as temperature sensors, etc.; the amount of raw materials added can be accurately controlled by a conventional metering instrument) and a first discharge valve 15 installed at the bottom of the batching kettle body 11.

[0024] The structure of the Grignard reactor 2 is basically the same as that of the Grignard reagent batching reactor 1. Specifically, the Grignard reactor 2 includes a reactor body 21, a second jacket 22 formed on the outer wall of the reactor body 21, a second agitator 20 rotatably mounted in the reactor body 21 and extending to the outside thereof, a second motor 23 mounted on the top of the reactor body 21 and connected to the second agitator 20, a plurality of second feed ports 24 opened on the top of the reactor body 21, and a second discharge valve 25 mounted on the bottom of the reactor body 21; since the reaction raw materials have been preliminarily mixed in the Grignard reagent batching reactor 1, the number of the second feed ports 24 can be appropriately reduced.

[0025] The material delivery component 3 includes a material delivery pipe 31 connected to the first discharge valve 15 and any second feed port 24, a first flow meter 32 installed on the material delivery pipe 31, and a first regulating valve 33 installed on the material delivery pipe 31 and located downstream of the first flow meter 32, so that the mixed material obtained by the Grignard reaction can be delivered from the Grignard reagent batching kettle 1 to the Grignard reactor 2 through the material delivery component 3, and the intensity of the Grignard reaction can be controlled to a certain extent through the first flow meter 32 and the first regulating valve 33. In this way, the problems of overheating (i.e., energy accumulation) and material spraying that may exist when using a single reactor can be avoided; and the connection between the Grignard reagent batching kettle 1 and the Grignard reactor 2 can be cut off in time to avoid danger.

[0026] In this embodiment, the feed assembly 3 also includes a feed branch pipe connected to the feed pipe 31 and connected in parallel with the first regulating valve 33, and a third regulating valve 35 is installed on the feed branch pipe; in this way, when the feed pipe 31 cannot work due to the blockage of the first regulating valve 33, the feed branch pipe can still be used to maintain the normal operation of the entire reaction device. The feed assembly 3 also includes two second regulating valves 34 installed on the feed pipe 31 and located upstream and downstream of the first regulating valve 33. The two second regulating valves 34 are both located downstream of the first flow meter 32, so that the two second regulating valves 34 are connected in parallel with the third regulating valve 35, which is conducive to extending the service life of the first regulating valve 33.

[0027] In this embodiment, in order to improve the degree of automation of the reaction device, the Grignard reactor 2 also includes a temperature sensor 27 (for measuring the temperature in the reactor body 21) arranged in the reactor body 21 and an alarm temperature control loop 26 (i.e., a temperature control loop with an alarm, abbreviated as TICAS) connected to the temperature sensor 27 and the second motor 23; the TICAS can be conventionally used to receive signals (usually electrical signals, such as H signals, LL signals, etc.) sent by the second motor 23 and the temperature sensor 27. Specifically, the Grignard reaction device also includes a control module, which includes a stirring sensor for detecting the state of the second stirrer 20 (when the second stirrer 20 fails, the stirring sensor generates a corresponding fault signal) and a control unit 4 (using a commercially available HollySys and Li Shi ETM100 programmable control system PLC module) communicating with the stirring sensor and connected to the alarm temperature control loop 26. At this time, the control unit 4 can receive the aforementioned stirring sensor signal and the alarm temperature control loop 26 signal. The control unit 4 is also connected to the first discharge valve 15, the first regulating valve 33 and the first flowmeter 32 respectively, so as to control the first discharge valve 15, the first regulating valve 33 and the first flowmeter 32 (usually the opening degree control) according to the aforementioned received signal. In this embodiment, the Grignard reactor 2 also includes a flow indicating interlocking flowmeter 36 connected to the first flowmeter 32, and the control unit 4 is connected to the first flowmeter 32 through the flow indicating interlocking flowmeter 36, so as to realize the control of the first flowmeter 32 through the flow indicating interlocking flowmeter 36. The first jacket 12 and the second jacket 22 are also independently provided with a temperature control TCU unit 41, and the control unit 4 is connected to the temperature control TCU unit 41, so that the control unit 4 can also receive the signal of the temperature control TCU unit 41 and then control the first discharge valve 15, the first regulating valve 33 and the first flowmeter 32.

[0028] The above embodiments are only for illustrating the technical concept and features of the utility model, and their purpose is to enable people familiar with the technology to understand the content of the utility model and implement it accordingly, and they cannot be used to limit the protection scope of the utility model. Any equivalent changes or modifications made according to the spirit of the utility model should be included in the protection scope of the utility model.

Claims

1. A reaction apparatus for a Grignard reaction, characterized in that: It includes: A Grignard reagent batching kettle (1), the Grignard reagent batching kettle (1) comprising a batching kettle body (11), a first jacket (12) formed on the outer wall of the batching kettle body (11), a first stirrer (10) rotatably mounted in the batching kettle body (11) and extending to the outside thereof, a first motor (13) mounted on the top of the batching kettle body (11) and connected to the first stirrer (10), a plurality of first feed ports (14) provided on the top of the batching kettle body (11), and a first discharge valve (15) mounted on the bottom of the batching kettle body (11); A Grignard reactor (2), the Grignard reactor (2) comprising a reactor body (21), a second jacket (22) formed on the outer wall of the reactor body (21), a second stirrer (20) rotatably mounted in the reactor body (21) and extending to the outside thereof, a second motor (23) mounted on the top of the reactor body (21) and connected to the second stirrer (20), a plurality of second feed ports (24) provided on the top of the reactor body (21), and a second discharge valve (25) mounted on the bottom of the reactor body (21); A material delivery component (3), the material delivery component (3) comprising a material delivery pipe (31) connected to the first discharge valve (15) and any one of the second feed ports (24), a first flow meter (32) installed on the material delivery pipe (31), and a first regulating valve (33) installed on the material delivery pipe (31) and located downstream of the first flow meter (32).

2. The reaction device for the Grignard reaction according to claim 1, characterized in that: The material delivery assembly (3) further comprises a material delivery branch pipe which is in communication with the material delivery pipe (31) and connected in parallel with the first regulating valve (33); a third regulating valve (35) is installed on the material delivery branch pipe.

3. The reaction device for the Grignard reaction according to claim 2, characterized in that: The material delivery assembly (3) further comprises two second regulating valves (34) installed on the material delivery pipe (31) and located upstream and downstream of the first regulating valve (33); the two second regulating valves (34) are both located downstream of the first flow meter (32).

4. The reaction device for the Grignard reaction according to claim 3, characterized in that: The two second regulating valves (34) are connected in parallel with the third regulating valve (35).

5. The reaction device for the Grignard reaction according to claim 1, characterized in that: The Grignard reactor (2) further comprises a temperature sensor (27) disposed in the reactor body (21) and an alarm temperature control circuit (26) connected to the temperature sensor (27) and the second motor (23).

6. The reaction device for the Grignard reaction according to claim 5, characterized in that: It also includes: a control module, the control module comprising a stirring sensor for detecting the state of the second stirrer (20) and a control unit (4) communicating with the stirring sensor and connected to the alarm temperature control circuit (26), The control unit (4) is also respectively connected to the first discharge valve (15), the first regulating valve (33) and the first flow meter (32).

7. The reaction device for the Grignard reaction according to claim 6, characterized in that: The Grignard reactor (2) further comprises a flow indicating interlocking flow meter (36) connected to the first flow meter (32), and the control unit (4) is connected to the first flow meter (32) via the flow indicating interlocking flow meter (36).

8. The reaction device for the Grignard reaction according to claim 6, characterized in that: The first jacket (12) and the second jacket (22) are independently provided with a temperature control TCU unit (41), and the control unit (4) is connected to the temperature control TCU unit (41).

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