Reaction device for Grignard reaction

Abstract

The utility model relates to a reaction device for Grignard reaction, which comprises a reaction kettle, an inlet of the reaction kettle is connected with a diaphragm pump, the reaction kettle is further connected with a nitrogen storage tank through a nitrogen pipe, the nitrogen storage tank is further connected with a material pressing device through a nitrogen pipe, the material pressing device is arranged on a Grignard reagent barrel, and the material pressing device comprises a disc. A liquid phase pipe and a gas phase pipe penetrate through the disc, and the material pressing device is further connected with an inlet of the reaction kettle through a feeding valve and a pneumatic control valve. According to the reaction device for the Grignard reaction, disclosed by the utility model, a Grignard reagent is prevented from being in contact with air in a conveying process, is added into the reaction kettle in a nitrogen atmosphere and reacts in the nitrogen atmosphere, so that the Grignard reagent is prevented from being decomposed.

Description

Technical Field

[0001] This utility model belongs to the field of chemical equipment technology, and specifically relates to a reaction device for Grignard reactions. Background Technology

[0002] The Grignard reaction (also known as the Grignard reaction) is one of the most fundamental and important carbon-carbon bond formation reactions in organic chemistry. It was discovered by the French chemist Victor Grignard, hence its name. Essentially, the Grignard reaction involves the addition reaction of Grignard reagents with various common electrophilic reagents such as aldehydes, ketones, imines, esters, epoxides, and carbon dioxide, resulting in the formation of new carbon-carbon bonds. This reaction plays a crucial role in organic synthesis and pharmaceutical synthesis.

[0003] Grignard reagents are organomagnesium halides with the general formula RMgX, where R is an aliphatic or aromatic hydrocarbon group and X is a halogen (Cl, Br, or I). Grignard reagents are important organic synthesis reagents. As covalent compounds, the magnesium atom is directly bonded to carbon to form a polar covalent bond, with carbon as the negatively charged end. Therefore, Grignard reagents are extremely strong Lewis bases, capable of abstracting protons from water and other Lewis acids. Thus, Grignard reagents cannot come into contact with water or carbon dioxide and must be used under anhydrous, air-free conditions. Currently, the methods of transporting Grignard reagents in Grignard reactions are insufficient to meet the requirement of avoiding contact with air during transport. For example, using ordinary pumps may result in air mixing during transport, and the feed rate is difficult to control.

[0004] Chinese patent CN222739179U discloses a Grignard reaction apparatus, comprising: a Grignard reagent mixing vessel; a Grignard reaction vessel, the Grignard reaction vessel including a reaction vessel body, a second jacket formed on the outer wall of the reaction vessel body, a second stirrer rotatably mounted inside the reaction vessel body and extending to its exterior, a second motor mounted on the top of the reaction vessel body and connected to the second stirrer, a plurality of second feeding ports opened on the top of the reaction vessel body, and a second discharge valve mounted on the bottom of the reaction vessel body; and a conveying assembly, the conveying assembly including a conveying pipe connecting the first discharge valve and any of the second feeding ports, a first flow meter mounted on the conveying pipe, and a first regulating valve mounted on the conveying pipe and located downstream of the first flow meter. In this patent, the Grignard reagent enters the reaction apparatus via the conveying assembly, and air may be mixed in during the conveying process, thus affecting the Grignard reaction efficiency.

[0005] Therefore, there is a need for a reaction apparatus that can effectively prevent Grignard reaction raw materials from coming into contact with air and can safely and efficiently add Grignard reagents dropwise into the reaction vessel. Summary of the Invention

[0006] The purpose of this invention is to provide a reaction apparatus for Grignard reactions, which prevents the Grignard reagent from coming into contact with air during transport, adds it to the reaction vessel in a nitrogen atmosphere, and reacts in a nitrogen atmosphere to avoid the decomposition of the Grignard reagent.

[0007] The technical solution adopted by this utility model to solve the above problems is as follows: a reaction device for Grignard reaction, including a reaction vessel, the inlet of which is connected to a diaphragm pump, the reaction vessel is also connected to a nitrogen storage tank via a nitrogen pipe, the nitrogen storage tank is also connected to a pressing device via a nitrogen pipe, the pressing device is installed on a Grignard reagent barrel, the pressing device includes a disc, the disc is penetrated by a liquid phase pipe and a gas phase pipe, and the pressing device is also connected to the inlet of the reaction vessel via a feed valve and a pneumatic regulating valve.

[0008] Preferably, the reaction vessel is equipped with a temperature sensor, which is connected to a PLC controller.

[0009] Preferably, the reactor is provided with a jacket that allows refrigerant to flow through it, with the refrigerant inlet of the jacket located at the lower part of the reactor and the refrigerant outlet of the jacket located at the upper part of the reactor.

[0010] Preferably, the reactor is equipped with a stirring mechanism, which includes a stirring shaft and stirring blades connected to the stirring shaft, and the stirring blades are provided in three or five pieces.

[0011] Preferably, the nitrogen pipe is equipped with a nitrogen regulating valve, the nitrogen storage tank is equipped with a pressure sensor, and both the nitrogen regulating valve and the pressure sensor are connected to a PLC controller.

[0012] Preferably, the pressing device is installed on the Grignard reagent container via a threaded connection.

[0013] Preferably, the Grignard reagent container is placed on an electronic scale for precise control of the amount of Grignard reagent added to the reaction vessel.

[0014] Preferably, the liquid phase tube extends to the bottom of the Grignard reagent container, and the gas phase tube extends downward to above the liquid surface of the Grignard reagent container.

[0015] Preferably, the nitrogen storage tank is also connected to the gas phase pipe in the pressing device via a nitrogen pipe, and the liquid phase pipe in the pressing device is also connected to the inlet of the reactor via a feed valve and a pneumatic regulating valve.

[0016] Compared with the prior art, the advantages of this utility model are:

[0017] The reaction apparatus for Grignard reactions of this invention includes a reaction vessel, an inlet connected to a diaphragm pump, and a nitrogen storage tank connected to the reaction vessel via a nitrogen pipe. The nitrogen storage tank is also connected to the gas phase pipe of a pressing device installed on a Grignard reagent container, and the liquid phase pipe of the pressing device is connected to the reaction vessel. This prevents the Grignard reagent from contacting air during transportation, allowing it to be added to the reaction vessel in a nitrogen atmosphere and react in the nitrogen atmosphere, thus preventing the decomposition of the Grignard reagent. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the reaction apparatus used for Grignard reaction in an embodiment of this utility model.

[0019] Figure 2 This is a schematic diagram of the pressing device in the reaction apparatus used for Grignard reaction in an embodiment of this utility model.

[0020] Among them: 1 is the reaction vessel, 2 is the diaphragm pump, 3 is the nitrogen pipe, 4 is the nitrogen storage tank, 5 is the pressing device, 5.1 is the disc, 5.2 is the liquid phase pipe, 5.3 is the gas phase pipe, 6 is the Grignard reagent container, 7 is the feed valve, 8 is the pneumatic regulating valve, 9 is the temperature sensor, 10 is the nitrogen regulating valve, 11 is the pressure sensor, and 12 is the electronic scale. Detailed Implementation

[0021] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments.

[0022] like Figure 1 The diagram shown is a schematic representation of the reaction apparatus used for the Grignard reaction in this embodiment.

[0023] A reaction apparatus for a Grignard reaction includes a reaction vessel 1, with a diaphragm pump 2 connected to the inlet of the reaction vessel 1. The reaction vessel 1 is also connected to a nitrogen storage tank 4 via a nitrogen pipe 3. The nitrogen storage tank 4 is further connected to a pressing device 5 via a nitrogen pipe 3. The pressing device 5 is threadedly mounted on a Grignard reagent container 6. The pressing device 5 includes a disc 5.1, through which a liquid phase pipe 5.2 and a gas phase pipe 5.3 pass. The pressing device 5 is also connected to the reaction vessel via a feed valve 7 and a pneumatic regulating valve 8. The inlet of reactor 1 is specifically as follows: the nitrogen storage tank 4 is also connected to the gas phase pipe 5.3 in the pressing device 5 via a nitrogen pipe 3; the liquid phase pipe 5.2 in the pressing device 5 is also connected to the inlet of reactor 1 via a feed valve 7 and a pneumatic regulating valve 8; the liquid phase pipe 5.2 extends to the bottom of the liquid surface in the Grignard reagent container 6, and the gas phase pipe 5.3 extends downward to above the liquid surface in the Grignard reagent container 6; the Grignard reagent container 6 is placed on an electronic scale 12 for precise control of the amount of Grignard reagent added to reactor 1.

[0024] The reactor 1 is equipped with a temperature sensor 9, which is connected to a PLC controller. The reactor 1 is also equipped with a stirring mechanism, which includes a stirring shaft and stirring blades connected to the stirring shaft. There are three stirring blades. The reactor 1 is equipped with a jacket that allows refrigerant to flow through it. The refrigerant inlet of the jacket is located at the lower part of the reactor 1, and the refrigerant outlet of the jacket is located at the upper part of the reactor 1.

[0025] In addition, a nitrogen regulating valve 10 is provided on the nitrogen pipe 3, and a pressure sensor 11 is provided in the nitrogen storage tank 4. Both the nitrogen regulating valve 10 and the pressure sensor 11 are connected to a PLC controller. This configuration ensures that the pressure in the nitrogen storage tank is between 0.02 and 0.03 MPa, providing a stable nitrogen source.

[0026] The working process of this embodiment will be described in detail below with reference to the accompanying drawings:

[0027] First, the electrophilic reagent is pumped into the reactor 1 via diaphragm pump 2. Nitrogen gas from nitrogen storage tank 4 enters the reactor 1 through nitrogen pipe 3, filling the reactor 1 with a nitrogen atmosphere. Coolant enters the jacket outside the reactor 1 through the coolant inlet and exits through the coolant outlet. Cooling medium is circulated through the jacket of reactor 1 to cool the temperature inside the reactor 1 to -10~0℃. Then, nitrogen gas from nitrogen storage tank 4 enters the Grignard reagent container 6 through nitrogen pipe and gas phase pipe 5.3 in the pressing device 5, filling the Grignard reagent container 6 with a nitrogen atmosphere. Finally, the feed valve 7 and pneumatic regulating valve 8 are opened, and the Grignard reagent enters the reaction vessel through liquid phase pipe 5.2. The reaction takes place inside reactor 1. During the reaction, temperature sensor 9 inside reactor 1 monitors the temperature of reactor 1 in real time and transmits the temperature detection results to the PLC controller. When the temperature of the material inside reactor 1 is greater than 0℃, the PLC controller controls the pneumatic regulating valve 8 to close. When the temperature of the material inside reactor 1 is less than -10℃, the PLC controller controls the pneumatic regulating valve 8 to open and close, allowing Grignard reagent to be added to reactor 1. Through the interaction of temperature sensor 9, PLC controller, and pneumatic regulating valve 8, the temperature of the reaction system is ensured to be between -10℃ and 0℃, thus improving product quality and yield.

[0028] In addition to the above embodiments, this utility model also includes other implementation methods. All technical solutions formed by equivalent transformation or equivalent substitution should fall within the protection scope of the claims of this utility model.

Claims

1. A reaction apparatus for a Grignard reaction, characterized in that: The reactor includes a reactor (1), the inlet of which is connected to a diaphragm pump (2). The reactor (1) is also connected to a nitrogen storage tank (4) via a nitrogen pipe (3). The nitrogen storage tank (4) is also connected to a pressing device (5) via a nitrogen pipe (3). The pressing device (5) is installed on a Grignard reagent container (6). The pressing device (5) includes a disc (5.1). The disc (5.1) is through which a liquid phase pipe (5.2) and a gas phase pipe (5.3) pass. The pressing device (5) is also connected to the inlet of the reactor (1) via a feed valve (7) and a pneumatic regulating valve (8).

2. The reaction apparatus for a Grignard reaction according to claim 1, characterized in that: The reactor (1) is equipped with a temperature sensor (9), which is connected to a PLC controller.

3. The reaction apparatus for a Grignard reaction according to claim 1, characterized in that: The reactor (1) is provided with a jacket that allows refrigerant to pass through. The refrigerant inlet of the jacket is located at the lower part of the reactor (1), and the refrigerant outlet of the jacket is located at the upper part of the reactor (1).

4. The reaction apparatus for a Grignard reaction according to claim 1, characterized in that: The reactor (1) is equipped with a stirring mechanism, which includes a stirring shaft and stirring blades connected to the stirring shaft.

5. The reaction apparatus for a Grignard reaction according to claim 1, characterized in that: The nitrogen pipe (3) is equipped with a nitrogen regulating valve (10), and the nitrogen storage tank (4) is equipped with a pressure sensor (11). Both the nitrogen regulating valve (10) and the pressure sensor (11) are connected to a PLC controller.

6. The reaction apparatus for a Grignard reaction according to claim 1, characterized in that: The pressing device (5) is installed on the Grignard reagent container (6) via a threaded connection.

7. The reaction apparatus for a Grignard reaction according to claim 1, characterized in that: The Grignard reagent container (6) is placed on an electronic scale (12) for precise control of the amount of Grignard reagent added to the reaction vessel (1).

8. The reaction apparatus for a Grignard reaction according to claim 1, characterized in that: The liquid phase tube (5.2) extends to the bottom of the liquid surface in the Grignard reagent container (6), and the gas phase tube (5.3) extends downward to above the liquid surface in the Grignard reagent container (6).

9. The reaction apparatus for a Grignard reaction according to claim 1, characterized in that: The nitrogen storage tank (4) is also connected to the gas phase pipe (5.3) in the pressing device (5) via a nitrogen pipe (3), and the liquid phase pipe (5.2) in the pressing device (5) is also connected to the inlet of the reactor (1) via a feed valve (7) and a pneumatic regulating valve (8).

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