Grignard reagent reaction device with pneumatic diaphragm pump

Abstract

The utility model relates to a Grignard reagent reaction device with a pneumatic diaphragm pump, which comprises the pneumatic diaphragm pump, a feed port of the pneumatic diaphragm pump is connected with a halogenated hydrocarbon storage tank through a feed pipe, a discharge port of the pneumatic diaphragm pump is connected with a reaction kettle through a discharge pipe, flow control valves are arranged on the feed pipe and the discharge pipe, a temperature sensor is arranged in the reaction kettle, and the pneumatic diaphragm pump is connected with the reaction kettle. A jacket is arranged outside the reaction kettle, a refrigerant inlet pipe is arranged at the top end of the left side of the jacket, a refrigerant outlet pipe is arranged at the bottom end of the right side of the jacket, a heating medium inlet pipe is arranged at the bottom end of the left side of the jacket, a heating medium outlet pipe is arranged at the top end of the right side of the jacket, and the refrigerant inlet pipe, the refrigerant outlet pipe, the heating medium inlet pipe and the heating medium outlet pipe are all provided with electromagnetic valves; and the flow control valve, the temperature sensor and the electromagnetic valve are respectively connected with the PLC. The Grignard reagent reaction device disclosed by the utility model can be used for controlling the adding amount of halogenated hydrocarbon to avoid side reaction caused by instantaneous increase of the temperature in the reaction kettle, and can be used for ensuring that the reaction temperature is controlled within a certain range and improving the purity of the Grignard reagent.

Description

Technical Field

[0001] This utility model belongs to the technical field of chemical reaction apparatus, specifically relating to a Grignard reagent reaction apparatus equipped with a pneumatic diaphragm pump. Background Technology

[0002] The principle behind the preparation of Grignard reagents is that magnesium atoms are directly bonded to carbon chains, and under the influence of polarization, the carbon atoms exhibit negative charge. As a traditional organic synthesis reagent, Grignard reagents have wide applications and play an important role in the fields of pharmaceuticals, chemical engineering, and even the entire field of organic synthesis.

[0003] The preparation of Grignard reagents involves a large amount of heat release within the reaction vessel, which can easily lead to coupling reactions. Therefore, strict control of the amount of reactants added and the reaction temperature within the vessel is necessary. Furthermore, throughout the entire preparation process, the reaction vessel must be kept dry and under nitrogen protection.

[0004] CN212882392U discloses a continuous production apparatus for preparing Grignard reagents from halogenated hydrocarbons. The apparatus includes a first feed pump connected to a raw material premixing tank and a distributor, the distributor being positioned at the top of the reaction bed. A magnesium powder solvent storage tank is connected to a second feed pump, which extends into the reaction bed through a pipeline equipped with valves and check valves. The reaction bed is equipped with a pressure gauge and an upper thermometer. Cooling coils, located outside the reaction bed, are positioned inside the reaction bed. A plate-type sight glass is installed in the upper middle part of the reaction bed. A lower thermometer and a filter sintering mesh are located at the bottom of the reaction bed. The bottom outlet of the reaction bed is connected to a transfer tank, which is equipped with a sampling pipe and a discharge pipe. A delivery pump connected to the discharge pipe is connected to the raw material premixing tank and a storage tank with a vent pipe through a pipeline equipped with valves. In this patent, the halogenated hydrocarbons directly enter the reaction bed via the first feed pump, the raw material premixing tank, and the distributor, making it impossible to control the amount of halogenated hydrocarbons added and prone to coupling reactions. Summary of the Invention

[0005] The purpose of this invention is to provide a Grignard reagent reaction apparatus equipped with a pneumatic diaphragm pump, which can control the amount of haloalkanes added to avoid the side reactions caused by the instantaneous increase in temperature inside the reactor, and can ensure that the reaction temperature is controlled within a certain range, thereby improving the purity of the final Grignard reagent.

[0006] The technical solution adopted by this utility model to solve the above problems is as follows: a Grignard reagent reaction device with a pneumatic diaphragm pump, including a pneumatic diaphragm pump connected to an air compressor, the inlet of the pneumatic diaphragm pump connected to a halogenated hydrocarbon storage tank, the outlet of the pneumatic diaphragm pump connected to a reaction vessel, a temperature sensor installed inside the reaction vessel, a jacket installed outside the reaction vessel, a refrigerant inlet pipe at the top left side of the jacket, a refrigerant outlet pipe at the bottom right side of the jacket, a heat medium inlet pipe at the bottom left side of the jacket, and a heat medium outlet pipe at the top right side of the jacket. Each of the refrigerant inlet pipe, refrigerant outlet pipe, heat medium inlet pipe, and heat medium outlet pipe is equipped with a solenoid valve; the temperature sensor and the solenoid valves are respectively connected to a PLC controller.

[0007] Preferably, the reactor is also connected to a nitrogen storage tank via a nitrogen pipe.

[0008] Preferably, the Grignard reagent reaction apparatus further includes a magnesium particle storage tank, which is connected to the reaction vessel via a magnesium particle conveying pipe.

[0009] Preferably, the reactor includes a stirring mechanism, which includes a stirring shaft. One end of the stirring shaft is connected to a drive motor, and the other end is connected to a stirring paddle. The stirring paddle includes three stirring blades evenly arranged circumferentially.

[0010] Preferably, a feed pipe is provided between the feed inlet of the pneumatic diaphragm pump and the halogenated hydrocarbon storage tank, and a discharge pipe is provided between the discharge outlet of the pneumatic diaphragm pump and the reaction vessel.

[0011] More preferably, one end of the feed pipe is connected to the feed port of the pneumatic diaphragm pump, and the other end of the feed pipe extends into the lower end of the halogenated hydrocarbon storage tank through the inlet of the halogenated hydrocarbon storage tank.

[0012] More preferably, one end of the discharge pipe is connected to the discharge port of the pneumatic diaphragm pump, and the other end of the discharge pipe extends into the top of the reactor through the feed port of the reactor.

[0013] More preferably, both the feed pipe and the discharge pipe are equipped with flow control valves, and the flow control valves are connected to the PLC controller.

[0014] Preferably, the lower end of the reactor is also provided with a discharge port.

[0015] Compared with the prior art, the advantages of this utility model are:

[0016] The Grignard reagent reaction apparatus of this invention includes a pneumatic diaphragm pump. The inlet of the pneumatic diaphragm pump is connected to a halogenated hydrocarbon storage tank via a feed pipe, and the outlet of the pneumatic diaphragm pump is connected to a reaction vessel via a discharge pipe. Both the feed pipe and the discharge pipe are equipped with flow control valves. A temperature sensor is installed inside the reaction vessel, and a jacket is installed outside the reaction vessel. The jacket is equipped with a refrigerant inlet pipe, a refrigerant outlet pipe, a hot medium inlet pipe, and a hot medium outlet pipe. Each of the refrigerant inlet pipe, refrigerant outlet pipe, hot medium inlet pipe, and hot medium outlet pipe is equipped with a solenoid valve. The temperature sensor, solenoid valves, and flow control valves are connected to a PLC controller. This configuration can control the amount of halogenated hydrocarbon added to prevent the temperature inside the reaction vessel from rising suddenly and causing side reactions, and can ensure that the reaction temperature is controlled within a certain range, thereby improving the purity of the final Grignard reagent. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the Grignard reagent reaction device with a pneumatic diaphragm pump in an embodiment of this utility model.

[0018] Among them: 1 is a pneumatic diaphragm pump, 2 is an air compressor, 3 is a halogenated hydrocarbon storage tank, 4 is a reaction vessel, 5 is a temperature sensor, 6 is a jacket, 7.1 is a refrigerant inlet pipe, 7.2 is a refrigerant outlet pipe, 8.1 is a heat medium inlet pipe, 8.2 is a heat medium outlet pipe, 9 is a solenoid valve, 10 is a nitrogen pipe, 11 is a nitrogen storage tank, 12 is a magnesium granule storage tank, 13 is a magnesium granule conveying pipe, 14 is a feed pipe, 15 is a discharge pipe, and 16 is a flow control valve. Detailed Implementation

[0019] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments.

[0020] like Figure 1 The diagram shown is a schematic representation of the Grignard reagent reaction apparatus with a pneumatic diaphragm pump in this embodiment.

[0021] A Grignard reagent reaction apparatus with a pneumatic diaphragm pump includes a pneumatic diaphragm pump 1 connected to an air compressor 2. The inlet of the pneumatic diaphragm pump 1 is connected to a halogenated hydrocarbon storage tank 3, and the outlet of the pneumatic diaphragm pump 1 is connected to a reaction vessel 4. A feed pipe 14 is provided between the inlet of the pneumatic diaphragm pump 1 and the halogenated hydrocarbon storage tank 3, and a discharge pipe 15 is provided between the outlet of the pneumatic diaphragm pump 1 and the reaction vessel 4. One end of the feed pipe 14 is connected to the inlet of the pneumatic diaphragm pump 1. The other end of the feed pipe 14 extends into the lower end of the halogenated hydrocarbon storage tank 3 through the inlet of the halogenated hydrocarbon storage tank 3. One end of the discharge pipe 15 is connected to the discharge port of the pneumatic diaphragm pump 1, and the other end of the discharge pipe 15 extends into the top of the reactor 4 through the feed port of the reactor 4. Both the feed pipe 14 and the discharge pipe 15 are equipped with flow control valves 16, which are connected to a PLC controller. The reactor 4 is also connected to the nitrogen storage tank 11 via a nitrogen pipe 10, and the lower end of the reactor 4 is also equipped with a discharge port.

[0022] The reaction vessel 4 is equipped with a temperature sensor 5 and a stirring mechanism. The stirring mechanism includes a stirring shaft, one end of which is connected to a drive motor and the other end is connected to a stirring paddle. The stirring paddle includes three stirring blades evenly arranged circumferentially.

[0023] The reactor 4 is equipped with a jacket 6. The top left side of the jacket 6 is provided with a refrigerant inlet pipe 7.1, the bottom right side of the jacket 6 is provided with a refrigerant outlet pipe 7.2, the bottom left side of the jacket 6 is provided with a heat medium inlet pipe 8.1, and the top right side of the jacket 6 is provided with a heat medium outlet pipe 8.2. All three pipes are equipped with solenoid valves 9.

[0024] The temperature sensor 5 and solenoid valve 9 mentioned above are connected to the PLC controller.

[0025] The Grignard reagent reaction apparatus also includes a magnesium particle storage tank 12, which is connected to the reaction vessel 4 via a magnesium particle conveying pipe 13.

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

[0027] First, nitrogen from nitrogen storage tank 11 enters reactor 4 via a nitrogen pipe. Under nitrogen-filled conditions, magnesium particles from magnesium particle storage tank 12 enter reactor 4 via magnesium particle conveying pipe 13. Then, air compressor 2 and pneumatic diaphragm pump 1 are turned on. Air compressor 2 drives pneumatic diaphragm pump 1 to add halogenated hydrocarbons from halogenated hydrocarbon storage tank 3 into reactor 4 sequentially via feed pipe 14 and discharge pipe 15 for reaction. During the reaction, temperature sensor 5 transmits the temperature to the PLC controller in real time. If the temperature is lower than the reaction temperature range, the PLC controller controls the heat transfer medium inlet pipe 8.1 and heat transfer medium outlet pipe. The solenoid valve 9 on pipe 8.2 opens to increase the temperature inside the reactor 4. Once the temperature reaches the reaction temperature range, the PLC controller controls the solenoid valve 9 to close. If the temperature exceeds the reaction temperature range, the PLC controller controls the solenoid valves 9 on the refrigerant inlet pipe 7.1 and refrigerant outlet pipe 7.2 to open to decrease the temperature inside the reactor 4. At the same time, the PLC controller controls the flow control valves 16 on the feed pipe 14 and discharge pipe 15 to slow down the dripping rate of the halogenated hydrocarbons entering the reactor 4. Once the temperature reaches the reaction temperature range, the PLC controller controls the solenoid valve 9 to close.

[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 Grignard reagent reaction apparatus with a pneumatic diaphragm pump, characterized by: The system includes a pneumatic diaphragm pump (1), the inlet of which is connected to a halogenated hydrocarbon storage tank (3) via a feed pipe (14), and the outlet of which is connected to a reactor (4) via a discharge pipe (15). Both the feed pipe (14) and the discharge pipe (15) are equipped with flow control valves (16). The reactor (4) is equipped with a temperature sensor (5), and the reactor (4) is equipped with a jacket (6). The top left side of the jacket (6) is equipped with a refrigerant inlet pipe (7.1). The jacket (6) has a refrigerant outlet pipe (7.2) at the bottom right side, a heat medium inlet pipe (8.1) at the bottom left side, and a heat medium outlet pipe (8.2) at the top right side. The refrigerant inlet pipe (7.1), refrigerant outlet pipe (7.2), heat medium inlet pipe (8.1), and heat medium outlet pipe (8.2) are all equipped with solenoid valves (9). The temperature sensor (5), solenoid valve (9), and flow control valve (16) are respectively connected to the PLC controller.

2. Grignard reagent reaction apparatus with a pneumatic diaphragm pump according to claim 1, characterized in that: The pneumatic diaphragm pump (1) is connected to the air compressor (2).

3. Grignard reagent reaction apparatus with pneumatic diaphragm pump according to claim 1, characterized in that: The reactor (4) is also connected to the nitrogen storage tank (11) via a nitrogen pipe (10).

4. Grignard reagent reaction apparatus with pneumatic diaphragm pump according to claim 1, characterized in that: The Grignard reagent reaction apparatus also includes a magnesium particle storage tank (12), which is connected to the reaction vessel (4) via a magnesium particle conveying pipe (13).

5. Grignard reagent reaction apparatus with pneumatic diaphragm pump according to claim 1, characterized in that: The reactor (4) includes a stirring mechanism, which includes a stirring shaft. One end of the stirring shaft is connected to a drive motor, and the other end is connected to a stirring paddle. The stirring paddle includes three stirring blades evenly arranged in the circumferential direction.

6. Grignard reagent reaction apparatus with pneumatic diaphragm pump according to claim 1, characterized in that: One end of the feed pipe (14) is connected to the feed port of the pneumatic diaphragm pump (1), and the other end of the feed pipe (14) extends into the lower end of the halogenated hydrocarbon storage tank (3) through the inlet of the halogenated hydrocarbon storage tank (3).

7. Grignard reagent reaction apparatus with pneumatic diaphragm pump according to claim 1, characterized in that: One end of the discharge pipe (15) is connected to the discharge port of the pneumatic diaphragm pump (1), and the other end of the discharge pipe (15) extends into the top of the reactor (4) through the feed port of the reactor (4).

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