CN117024452B - A kind of preparation process of phenylmagnesium chloride - Google Patents

Abstract

The invention discloses a preparation process of phenyl magnesium chloride. In the preparation process, chlorobenzene or a mixed solution of chlorobenzene, a solvent A and a solvent B is used as a first stock solution, a mixed solution of the solvent A and the solvent B is used as a second stock solution, and magnesium chips and an initiator are mixed as a third stock solution; firstly, part of the first stock solution is put into a reaction kettle to be mixed with the third stock solution, the reaction is initiated at a certain temperature, part of the first stock solution and the second stock solution are simultaneously dripped at 90-110 ℃, then the rest of the first stock solution and the second stock solution are simultaneously dripped at 85-95 ℃ for 2-3 hours, and the heat preservation reaction is carried out to obtain the product phenylmagnesium chloride solution with high yield. The invention is beneficial to control the side reaction for generating biphenyl by adopting limited feed liquid and reaction, thereby improving the yield of the phenylmagnesium chloride, being more energy-saving, and the conversion rate of the chlorobenzene reaches more than 99.5 percent, and the yield of the phenylmagnesium chloride reaches more than 98.8 percent.

Description

A kind of preparation process of phenylmagnesium chloride

Technical Field

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation process of phenylmagnesium chloride with high yield.

Background technique

Phenyl magnesium chloride is an intermediate for the preparation of triphenylphosphine, which is the basic raw material for rhodium phosphine complex catalysts and has a wide range of uses in petrochemicals. Triphenylphosphine is also used in the pharmaceutical industry, organic synthesis, analysis and other fields. It can also be used to prepare Wittig reagents, as a brightener for dye technology, an antioxidant for polymer polymerization and color film development, a stabilizer for polyepoxidation, and an analytical reagent.

Phenylmagnesium chloride is usually synthesized by Grignard reaction of chlorobenzene and magnesium in a mixed solvent of toluene (or benzene) and tetrahydrofuran (or 2-methyltetrahydrofuran). The reaction equation is:

The main side reaction is the reaction of phenylmagnesium chloride with chlorobenzene to form biphenyl, and the reaction equation is:

,

Moreover, generally, an increase in the reaction temperature is more conducive to the side reaction of generating biphenyl.

Chinese patent CN102887919B mentions a method for synthesizing phenylmagnesium chloride with chlorobenzene and magnesium in a mixed solvent of toluene and tetrahydrofuran, wherein toluene (80-120 parts), tetrahydrofuran (26-35 parts), and magnesium (6-8.5 parts) are all put into a reactor, and then chlorobenzene (220-260 parts) is added dropwise in stages. In the first stage, 1/4-1/2 chlorobenzene is added dropwise at 80±5°C, and then the temperature is raised to 100-105°C for 30 minutes, and then the temperature is lowered to 80±5°C and the remaining chlorobenzene is added dropwise, and then the temperature is raised to 100-105°C and the remaining chlorobenzene is added dropwise. In this process, chlorobenzene is in large excess relative to magnesium, and the temperature is raised to 100°C-105°C twice, which is not conducive to controlling the occurrence of biphenyl side reactions, and the yield of the product phenylmagnesium chloride is low.

Chinese patent CN108084225A mentions a method for synthesizing phenylmagnesium chloride with chlorobenzene and magnesium in a mixed solvent of toluene and tetrahydrofuran. After mixing chlorobenzene, toluene and tetrahydrofuran, about 10% of the mixed solution is first added to the reactor and mixed with magnesium chips, the reaction is initiated at 50-60°C, and then the remaining chlorobenzene and the mixed solution of the solvent are slowly added dropwise at 100-110°C for 4.5-5.5h, and the reaction is terminated by keeping warm at 100-110°C for 4.5-5.5h. This process also controls the excess of chlorobenzene relative to magnesium, does not control the amount of biphenyl generated, and extracts biphenyl as a by-product in the separation stage of the final product triphenylphosphine. The economic value of the biphenyl product is low. It takes two molecules of chlorobenzene and one molecule of magnesium to obtain one molecule of biphenyl. The value of the raw material has greatly exceeded the value of the product. The practice of sacrificing the yield of phenylmagnesium chloride is not worth the loss and has poor practicality.

Chinese patent CN111454292A mentions a method for synthesizing phenylmagnesium chloride using chlorobenzene and magnesium in a mixed solvent of benzene and 2-methyltetrahydrofuran, wherein chlorobenzene, benzene and 2-methyltetrahydrofuran are mixed in a mass ratio of 1:2:(1.3-2) as a first reaction stock solution, magnesium and a catalyst are mixed as a second reaction stock solution, the mass ratio of chlorobenzene to magnesium is (4-7):1, the second reaction stock solution is heated to 50-100°C, and then the first reaction stock solution is added dropwise to react, and the temperature is maintained for 2 hours to obtain phenylmagnesium chloride. In this process, chlorobenzene is in large excess relative to magnesium, which is not conducive to the inhibition of biphenyl side reactions, and the yield of phenylmagnesium chloride is low.

Summary of the invention

The purpose of the present invention is to overcome the deficiencies of the prior art and provide a process for preparing phenylmagnesium chloride with high yield, which can effectively inhibit the side reaction of biphenyl, improve the conversion rate of chlorobenzene and the selectivity of the main reaction.

To achieve the above object, the present invention provides the following technical solution: a preparation process of phenylmagnesium chloride, specifically comprising the following steps:

1) Chlorobenzene or a mixture of chlorobenzene, solvent A and solvent B is used as the first stock solution, a mixture of solvent A and solvent B is used as the second stock solution, and a mixture of magnesium chips and an initiator is used as the third stock solution, solvent A is toluene or benzene, and solvent B is tetrahydrofuran or 2-methyltetrahydrofuran;

2) The third stock solution is heated to 65-90° C. in a reaction kettle, 2-20 wt% of the first stock solution is added into the reaction kettle to initiate a reaction, and then 40-60 wt% of the remaining first stock solution and 60-100 wt% of the second stock solution are simultaneously added dropwise at 90-110° C. within 3-6 hours, and then the remaining first stock solution and the second stock solution are continuously added dropwise at 85-95° C. within 2-3 hours. After the addition is completed, the reaction is carried out at 80-90° C. for 2-5 hours to obtain a high-yield product phenylmagnesium chloride solution.

Furthermore, the present invention defines the total mass ratio of solvent A to solvent B in the first stock solution and the second stock solution as 4-6.5:6-3.5; the total mass of solvent A and solvent B in the first stock solution accounts for 0-30% of the total mass of solvent A and solvent B in the first stock solution and the second stock solution; the molar ratio of chlorobenzene to the total amount of solvent B in the first stock solution and the second stock solution is 1:1.9-3.0; the molar ratio of chlorobenzene to magnesium chips is 1:1.0-1.4.

Furthermore, the present invention defines that the initiator is a mixed solution of solvent A and solvent B containing phenylmagnesium chloride. The mixed solution as the initiator can be either externally added to the kettle or a residual product of the previous batch reaction.

Furthermore, the present invention stipulates that in the initiation reaction stage, in addition to adding 2-20wt% of the first stock solution, 2-15wt% of the second stock solution can also be added.

Furthermore, the present invention defines the stage of dropwise addition of the remaining first stock solution and the second stock solution and the heat preservation reaction stage after the dropwise addition, and the stirring speed of the reactor is 125rpm-250rpm; and in the heat preservation reaction stage, the liquid in the reactor is circulated by an external circulation pump to enhance the mixing of the liquid in the reactor.

Furthermore, the present invention stipulates that during the heat preservation reaction stage, the liquid in the reactor is circulated by an external circulation pump to enhance the mixing of the liquid in the reactor, and the pipe mouth of the external circulation pump circulating into the reactor is located below the liquid level in the reactor.

Furthermore, the present invention defines that a tank jet mixer is provided in the reactor, a pipe opening for circulating into the reactor is inserted into the reactor and connected to the tank jet mixer, and the feed liquid is circulated through the tank jet mixer.

In order to better control the reaction, the present invention can also be provided with baffles in the reactor, the number of the baffles is 3-8, and the baffles are evenly distributed along the wall of the reactor.

By adopting the above technology, compared with the prior art, the beneficial effects of the present invention are as follows:

1) The present invention achieves flexible suppression of the biphenyl side reaction according to the progress of the reaction by adding chlorobenzene and a mixed solvent separately and dropwise into the reactor in batches, and ensures a high concentration of magnesium chips and a low concentration of chlorobenzene in the reaction system in the early stage of the reaction, and ensures a relatively high reaction temperature, so that the main reaction of generating phenylmagnesium chloride proceeds rapidly, and suppresses the side reaction of chlorobenzene and phenylmagnesium chloride; as the reaction proceeds, the concentration of phenylmagnesium chloride in the system increases and the concentration of magnesium chips decreases, and by adding more solvent to dilute the concentration of phenylmagnesium chloride and lowering the reaction temperature, the side reaction of biphenyl is suppressed, and the yield of the main reaction is guaranteed;

2) The present invention provides a baffle in the reactor and, in the later stage of the reaction, strengthens the stirring, increases the external circulation and builds in a jet mixer to strengthen the contact between the residual magnesium chips and chlorobenzene in the system, thereby continuing to promote the main reaction and ensuring the yield of the main reaction;

3) The present invention controls the excess of magnesium relative to chlorobenzene, which is beneficial to controlling the side reaction of generating biphenyl, and the unreacted magnesium can be retained in the kettle by static separation for the production of the next batch of phenylmagnesium chloride; the background patent uses an excess of chlorobenzene relative to magnesium, which is not conducive to controlling the side reaction of biphenyl, and the conversion rate of chlorobenzene is low, and the subsequent process needs to consume more energy to recover the unreacted chlorobenzene through distillation or rectification. The present invention can not only improve the yield of phenylmagnesium chloride, but also be more energy-efficient.

4) The process provided by the present invention can achieve a high conversion rate of chlorobenzene and a high yield of phenylmagnesium chloride, the conversion rate of chlorobenzene reaches more than 99.5%, and the yield of phenylmagnesium chloride reaches more than 98.8%.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG1 is a schematic structural diagram of a reaction device of the present invention.

In the figure: 1 - reactor; 2 - magnesium chips feeding hopper; 3 - first stock liquid metering tank; 4 - second stock liquid metering tank; 5 - external circulation pump; 6 - baffle; 7 - tank jet mixer.

Detailed ways

The present invention is further defined below in conjunction with the embodiments, but the protection scope of the present invention is not limited thereto.

The process for preparing phenyl magnesium chloride of the present invention adopts a device for preparing phenyl magnesium chloride with a limited high yield, and its structure is shown in FIG1. The device comprises a reactor 1, a magnesium chip feeding hopper 2, an external circulation pump 5, a first stock solution metering tank 3 and a second stock solution metering tank 4; the reactor 1 is provided with a plurality of inlets; the outlet of the magnesium chip feeding hopper 2 is connected to the magnesium chip inlet arranged on the reactor 1, the bottom and the side wall of the reactor 1 are provided with circulating liquid outlets, the side wall of the reactor is provided with a circulating liquid inlet, a tank jet mixer 7 is provided at the inlet end in the reactor, the circulating liquid outlet is connected to the inlet of the external circulation pump 5, and the outlet of the external circulation pump 5 is connected to the inlet of the built-in tank jet mixer 7; the outlet of the first stock solution metering tank 3 is connected to the first stock solution inlet arranged on the reactor 1 for feeding the first stock solution, and the outlet of the second stock solution metering tank 4 is connected to the second stock solution inlet arranged on the reactor 1 for feeding the second stock solution.

In order to improve the liquid circulation effect, the present invention provides circulating liquid outlets at the bottom and side walls of the reactor respectively, and the circulating liquid outlets are connected to the inlet of an external circulating pump 5 through a pipeline.

The circulating liquid inlet of the side wall of the reactor 1 is located below the side wall of the reactor 1 or at any position of the lower head except the bottom outlet.

In order to further control the reaction, the present invention further provides baffles 6 inside the reactor 1 , wherein the number of baffles is 3-8 and they are evenly distributed along the wall of the reactor 1 .

In order to facilitate the feeding of the initiator, the present invention provides an initiator inlet on the reaction kettle 1 .

Example 1

1) Chlorobenzene is used as the first stock solution, and a mixture of toluene and tetrahydrofuran in a mass ratio of 5:5 is used as the second stock solution, and the molar ratio of chlorobenzene in the first stock solution to tetrahydrofuran in the second stock solution is 1:2.1; magnesium chips and an initiator are mixed as the third stock solution, and the molar ratio of magnesium chips to chlorobenzene in the first stock solution is 1.05:1, and the initiator is a toluene and tetrahydrofuran solution of phenylmagnesium chloride, and the amount used is 20% of the volume of the first stock solution, wherein the mass concentration of phenylmagnesium chloride is 25%, and the mass ratio of toluene and tetrahydrofuran is 5:5;

2) The third stock solution was heated to 75°C in the reactor, 10wt% of the first stock solution was added into the reactor to initiate the reaction, and then 50wt% of the remaining first stock solution and 60wt% of the second stock solution were added dropwise at a reactor speed of 100rpm, a reactor temperature of 100°C, and a time of 5h. Then the stirring speed of the reactor was adjusted to 125rpm, and the remaining first stock solution and the second stock solution were continued to be added dropwise at 95°C for 2h. After the addition was completed, an external circulation pump was started for circulation, and the mouth of the circulation pipe entered below the liquid level in the reactor, and a tank jet mixer was provided at the mouth of the pipe. The reaction was kept warm at 85°C for 2h to obtain a high-yield phenylmagnesium chloride solution, which was sampled and sent for inspection. According to the test results, the chlorobenzene conversion rate was 99.89%, and the phenylmagnesium chloride yield was 99.26%.

Example 2

1) Benzene and tetrahydrofuran are mixed in a mass ratio of 5:5, 20% of which is mixed with chlorobenzene as the first stock solution, and the remaining 80% is the second stock solution, and the molar ratio of chlorobenzene to all tetrahydrofuran in the first stock solution and the second stock solution is 1:2.2; magnesium chips and an initiator are mixed as the third stock solution, the molar ratio of magnesium chips to chlorobenzene in the first stock solution is 1.3:1, and the initiator is a benzene and tetrahydrofuran solution of phenylmagnesium chloride, the amount of which is 15% of the volume of the first stock solution, wherein the mass concentration of phenylmagnesium chloride is 25%, and the mass ratio of benzene to tetrahydrofuran is 5:5;

2) The third stock solution was heated to 85°C in a reactor, 20wt% of the first stock solution was added into the reactor to initiate the reaction, and then 40wt% of the remaining first stock solution and 80wt% of the second stock solution were added dropwise at a reactor speed of 90rpm, a reactor temperature of 110°C, and a time of 3h. Then the stirring speed of the reactor was adjusted to 150rpm, and the remaining first stock solution and the second stock solution were continued to be added dropwise at 90°C for 3h. After the addition was completed, an external circulation pump was started for circulation, and the mouth of the circulation pipe entered below the liquid level in the reactor, and a tank jet mixer was provided at the mouth of the pipe. The reaction was kept warm at 85°C for 4h to obtain a high-yield phenylmagnesium chloride solution, which was sampled and sent for inspection. According to the test results, the chlorobenzene conversion rate was 99.93%, and the phenylmagnesium chloride yield was 99.37%.

Example 3

1) Toluene and 2-methyltetrahydrofuran are mixed in a mass ratio of 5:5, 15% of which is mixed with chlorobenzene as the first stock solution, and the remaining 85% is the second stock solution, and the molar ratio of chlorobenzene to all 2-methyltetrahydrofuran in the first stock solution and the second stock solution is 1:2.4; the part of the product remaining in the reactor from the above batch reaction is the initiator, and magnesium chips are put into the reactor and mixed with the initiator to form the third stock solution, the molar ratio of magnesium chips to chlorobenzene in the first stock solution is 1.2:1, and the initiator is a toluene and 2-methyltetrahydrofuran solution of phenylmagnesium chloride, and the amount used is 15% of the volume of the first stock solution, wherein the mass concentration of phenylmagnesium chloride is 25%, and the mass ratio of toluene and 2-methyltetrahydrofuran is 5:5;

2) The third stock solution was heated to 80°C in a reactor, 15wt% of the first stock solution was added into the reactor to initiate the reaction, and then 50wt% of the remaining first stock solution and 70wt% of the second stock solution were added dropwise at a reactor speed of 90rpm, a reactor temperature of 95°C, and a time of 5h. Then the stirring speed of the reactor was adjusted to 140rpm, and the remaining first stock solution and the second stock solution were continued to be added dropwise at 85°C for 3h. After the addition was completed, an external circulation pump was started for circulation, and the mouth of the circulation pipe entered below the liquid level in the reactor, and a tank jet mixer was provided at the mouth of the pipe. The reaction was kept warm at 80°C for 3h to obtain a high-yield phenylmagnesium chloride solution, which was sampled and sent for inspection. According to the test results, the chlorobenzene conversion rate was 99.91%, and the phenylmagnesium chloride yield was 99.34%.

Example 4

1) Chlorobenzene is used as the first stock solution, and a mixture of toluene and tetrahydrofuran in a mass ratio of 5:5 is used as the second stock solution, and the molar ratio of chlorobenzene in the first stock solution to tetrahydrofuran in the second stock solution is 1:2.1; magnesium chips and an initiator are mixed as the third stock solution, and the molar ratio of magnesium chips to chlorobenzene in the first stock solution is 1.2:1, and the initiator is a toluene and tetrahydrofuran solution of phenylmagnesium chloride, and the amount used is 20% of the volume of the first stock solution, wherein the mass concentration of phenylmagnesium chloride is 25%, and the mass ratio of toluene and tetrahydrofuran is 5:5;

2) The third stock solution was heated to 75°C in a reactor, 10wt% of the first stock solution and 10wt% of the second stock solution were added into the reactor to initiate the reaction, and then 50wt% of the remaining first stock solution and 60wt% of the second stock solution were added dropwise at a reactor speed of 100rpm, a reactor temperature of 100°C, and a time of 5h. Then the stirring speed of the reactor was adjusted to 125rpm, and the remaining first stock solution and the second stock solution were continued to be added dropwise at 95°C for 2h. After the addition was completed, an external circulation pump was started for circulation, the mouth of the circulation pipe entered below the liquid level in the reactor, and a tank jet mixer was provided at the mouth of the pipe. The reaction was kept warm at 85°C for 2h to obtain a high-yield phenylmagnesium chloride solution, which was sampled and sent for inspection. According to the test results, the chlorobenzene conversion rate was 99.93%, and the phenylmagnesium chloride yield was 99.42%.

Example 5

1) Chlorobenzene is used as the first stock solution, and a mixture of toluene and tetrahydrofuran in a mass ratio of 4:6 is used as the second stock solution, and the molar ratio of chlorobenzene in the first stock solution to tetrahydrofuran in the second stock solution is 1:2.8; the part of the product remaining in the reactor from the above batch reaction is used as the initiator, and magnesium chips are put into the reactor and mixed with the initiator to form the third stock solution, and the molar ratio of magnesium chips to chlorobenzene in the first stock solution is 1.4:1, and the initiator is a toluene and tetrahydrofuran solution of phenylmagnesium chloride, and the amount used is 20% of the volume of the first stock solution, wherein the mass concentration of phenylmagnesium chloride is 25%, and the mass ratio of toluene and tetrahydrofuran is 4:6;

2) The third stock solution was heated to 90°C in a reactor, 10wt% of the first stock solution and 10wt% of the second stock solution were added into the reactor to initiate the reaction, and then 40wt% of the remaining first stock solution and 80wt% of the second stock solution were added dropwise at a reactor speed of 100rpm, a reactor temperature of 110°C, and a time of 4h. Then the stirring speed of the reactor was adjusted to 130rpm, and the remaining first stock solution and the second stock solution were continued to be added dropwise at 90°C for 2h. After the addition was completed, an external circulation pump was started for circulation, the mouth of the circulation pipe entered below the liquid level in the reactor, and a tank jet mixer was provided at the mouth of the pipe. The reaction was kept warm at 85°C for 2h to obtain a high-yield phenylmagnesium chloride solution, which was sampled and sent for inspection. According to the test results, the chlorobenzene conversion rate was 99.53%, and the phenylmagnesium chloride yield was 99.02%.

Example 6

1) Toluene and 2-methyltetrahydrofuran are mixed in a mass ratio of 6:4, 10% of which is mixed with chlorobenzene as the first stock solution, and the remaining 90% is the second stock solution, and the molar ratio of chlorobenzene in the first stock solution to 2-methyltetrahydrofuran in the second stock solution is 1:3; magnesium chips and an initiator are mixed as the third stock solution, the molar ratio of magnesium chips to chlorobenzene in the first stock solution is 1.3:1, and the initiator is a toluene and 2-methyltetrahydrofuran solution of phenylmagnesium chloride, and the amount used is 20% of the volume of the first stock solution, wherein the mass concentration of phenylmagnesium chloride is 25%, and the mass ratio of toluene and 2-methyltetrahydrofuran is 6:4;

2) The third stock solution was heated to 80°C in a reactor, 5wt% of the first stock solution and 10wt% of the second stock solution were added into the reactor to initiate the reaction, and then 40wt% of the remaining first stock solution and 80wt% of the second stock solution were added dropwise at a reactor speed of 100rpm, a reactor temperature of 110°C, and a time of 4h. Then the stirring speed of the reactor was adjusted to 128rpm, and the remaining first stock solution and the second stock solution were continued to be added dropwise at 90°C for 2h. After the addition was completed, an external circulation pump was started for circulation, and the mouth of the circulation pipe entered below the liquid level in the reactor, and a tank jet mixer was provided at the mouth of the pipe. The reaction was kept warm at 85°C for 2h to obtain a high-yield phenylmagnesium chloride solution, which was sampled and sent for inspection. According to the test results, the chlorobenzene conversion rate was 99.83%, and the phenylmagnesium chloride yield was 99.62%.

Comparative Example 1 (according to patent CN108084225A, the amount of magnesium chips was modified to be excessive compared to chlorobenzene)

Prepare a mixed solution of chlorobenzene, toluene and tetrahydrofuran in a mass ratio of 1:2:3.1, add magnesium chips into the reactor, the molar ratio of magnesium chips to chlorobenzene is 1.15:1, add 1/10 of the above mixed solution of chlorobenzene, toluene and tetrahydrofuran into the reactor, add toluene and tetrahydrofuran solutions of phenylmagnesium chloride as initiators, heat to 60°C to initiate Grignard reaction, then heat to 110°C, slowly add the remaining mixed solution dropwise through an overhead tank within 5.5 hours at this temperature, keep the reaction at 110°C for 5.5 hours after the addition is completed, and obtain phenylmagnesium chloride solution, take samples for inspection, and calculate the chlorobenzene conversion rate and phenylmagnesium chloride yield according to the test results to be 94.33%, and 86.45%.

Claims (8)

1. A preparation process for phenylmagnesium chloride, characterized in that it comprises the following steps: 1) Chlorobenzene or a mixture of chlorobenzene, solvent A and solvent B is used as the first stock solution, a mixture of solvent A and solvent B is used as the second stock solution, and a mixture of magnesium chips and an initiator is used as the third stock solution, solvent A is toluene or benzene, solvent B is tetrahydrofuran or 2-methyltetrahydrofuran, and the molar ratio of chlorobenzene to magnesium chips is 1:1.0-1.4; 2) The third stock solution is heated to 65-90° C. in a reaction kettle, 2-20 wt% of the first stock solution is added into the reaction kettle to initiate a reaction, and then 40-60 wt% of the remaining first stock solution and 60-100 wt% of the second stock solution are simultaneously added dropwise at 90-110° C. within 3-6 hours, and then the remaining first stock solution and the second stock solution are continuously added dropwise at 85-95° C. within 2-3 hours. After the addition is completed, the reaction is carried out at 80-90° C. for 2-5 hours to obtain a high-yield product phenylmagnesium chloride solution. 2. A preparation process for phenylmagnesium chloride according to claim 1, characterized in that the total mass ratio of solvent A to solvent B in the first stock solution and the second stock solution is 4-6.5:6-3.5; the sum of the masses of solvent A and solvent B in the first stock solution accounts for 0-30% of the total mass of solvent A and solvent B in the first stock solution and the second stock solution; the molar ratio of chlorobenzene to the total amount of solvent B in the first stock solution and the second stock solution is 1:1.9-3.0. 3. A preparation technology for phenylmagnesium chloride according to claim 1, characterized in that the initiator is a mixed solution of solvent A and solvent B of phenylmagnesium chloride. 4. A process for preparing phenylmagnesium chloride according to claim 1, characterized in that in the initiation reaction stage, in addition to inputting 2-20wt% of the first stock solution, 2-15wt% of the second stock solution can also be input. 5. A process for preparing phenylmagnesium chloride according to claim 1, characterized in that during the dropwise addition of the remaining first stock solution and the second stock solution and the heat preservation reaction stage after the dropwise addition, the stirring speed of the reactor is 125rpm-250rpm; and during the heat preservation reaction stage, the feed liquid in the reactor is circulated by an external circulating pump to enhance the mixing of the feed liquid in the reactor. 6. A process for preparing phenylmagnesium chloride according to any one of claims 1 to 5, characterized in that in the insulation reaction stage, the feed liquid in the reactor is circulated by an external circulating pump to strengthen the mixing of the feed liquid in the reactor, and the nozzle of the external circulating pump circulating into the reactor is located below the liquid level in the reactor. 7. A preparation process for phenylmagnesium chloride according to claim 6, characterized in that a tank jet mixer is provided in the reactor, a nozzle for circulating into the reactor is inserted into the reactor and connected to the tank jet mixer, and liquid circulation is carried out through the tank jet mixer. 8. A process for preparing phenylmagnesium chloride according to any one of claims 1 to 5, characterized in that baffles are provided inside the reactor, the number of the baffles being 3 to 8, uniformly distributed along the reactor wall.