An apparatus and method for preparing benzoyl Corey lactone

Abstract

The present invention discloses a preparation device and method for benzoyl Corey lactone. The device includes: a reaction device, which includes a reaction housing. Inside the reaction housing, there is a reaction inner cylinder. A cooling space is formed between the reaction inner cylinder and the reaction housing. And a heating component is preset in the reaction inner cylinder and is uniformly arranged, and the inside of the reaction inner cylinder forms a reaction chamber; a pushing piston is arranged in the reaction chamber, and one end of the pushing piston is connected to a push rod, and the push rod is arranged on a pushing cylinder; at the inner end of the reaction chamber and embedded in the lower part of the reaction inner cylinder is a pressure control valve, and at the inner end of the reaction chamber and embedded in the upper part of the reaction inner cylinder is an exhaust valve, and the exhaust valve is connected to a reflux cooling device; on the upper surface of the reaction housing, there is a multi-way joint assembly, and a plurality of electromagnetic valves are embedded in the joint housing. Each electromagnetic valve is connected to a feeding tank through a corresponding feeding pipeline and a meter arranged on the feeding pipeline.

Description

Technical Field

[0001] The present invention relates to the technical field of the preparation of benzoyl Corey lactone, and particularly relates to a preparation device and method for benzoyl Corey lactone. Background Art

[0002] Currently, benzoyl Corey lactone is basically prepared by laboratory methods. Although there are also technologies for large-scale production in the publicly disclosed technologies, the main synthetic route is still based on the laboratory preparation idea for reaction, filtration, and evaporation to obtain. For example, the publication number: "CN109096320A" discloses a preparation method for benzoyl Corey lactone. 17.2 kg of (-)-Corey Lactone is put into a 500 L reaction kettle, 130 kg of dichloromethane is added, and they are stirred and mixed. 25.3 kg of diisopropylethylamine is added at room temperature. Under stirring, the temperature is lowered to 20 °C, and 16.6 kg (1.1 eq) of triethylchlorosilane is slowly added dropwise. The reaction is carried out at 20 - 30 °C for 2 hours. 18.3 kg of benzoic acid is added, 26.9 kg of EDCI and 0.7 kg of DMAP are added, and the reaction is carried out at room temperature for 20 hours. After cooling to 10 °C, 150 kg of 10% hydrochloric acid is added, and the reaction is carried out with heat preservation and stirring for 6 - 12 hours. After liquid separation, the dichloromethane layer is dried with anhydrous sodium sulfate, filtered, the filtrate is evaporated to dryness, and 50 L of petroleum ether is added for crystallization to obtain 24 kg of (-)-Corey Lactone benzoate, with a yield of 86.9%, a purity of 99.8%, and an ee of 99.97%. Summary of the Invention

[0003] In order to solve the problems of the prior art, the present invention provides a preparation device for benzoyl Corey lactone, including: a reaction device, which includes a reaction housing, and a reaction inner cylinder is arranged inside the reaction housing. A cooling space is formed between the reaction inner cylinder and the reaction housing, and a uniformly arranged heating component is preset inside the reaction inner cylinder, and a reaction cavity is formed inside the reaction inner cylinder;

[0004] A pushing piston is arranged in the reaction cavity, and one end of the pushing piston is connected to a push rod, and the push rod is arranged on a pushing cylinder;

[0005] A pressure control valve is embedded at the inner end of the reaction cavity and at the lower part of the reaction inner cylinder. The pressure control valve passes through the cooling space and the reaction housing and is fixed to one end of a connecting pipe arranged outside the reaction housing. The other end of the connecting pipe is fixed to the inlet of a filtering valve, and the filtering valve is embedded inside a filter cylinder;

[0006] An exhaust valve is embedded at the inner end of the reaction chamber and above the reaction inner cylinder. The exhaust valve passes through the cooling space and the reaction housing and is connected to one end of an exhaust valve joint arranged outside the reaction housing. The other end of the exhaust valve joint is connected to an exhaust pipe, and the exhaust pipe is connected to a reflux cooling device;

[0007] A multi-way joint assembly is arranged on the upper surface of the reaction housing. The multi-way joint assembly includes a joint housing and a plurality of solenoid valves embedded inside the joint housing. Each solenoid valve is connected to a feeding tank through a corresponding feeding pipeline and a meter arranged on the feeding pipeline;

[0008] A control device is connected to the pushing cylinder, the pressure control valve, the exhaust valve, the multi-way joint assembly and the heating assembly.

[0009] Furthermore, an inlet pipe for adding a cooling medium and a reflux pipe for the cooling medium to flow out are arranged on the reaction housing. The inlet pipe is connected to a cooling water tank through an inlet water pipeline and an inlet end switching valve arranged on the inlet water pipeline. The reflux pipe is connected to a return water tank through a reflux pipeline and a reflux switching valve arranged on the reflux pipeline.

[0010] Furthermore, the filter cartridge seals and fixes the filter valve, the connecting pipe and the extended section of the pressure control valve outside the reaction housing together outside the reaction housing.

[0011] Furthermore, the reflux cooling device is a three-stage cooling device, including a first-stage condensate component with a multi-stage composite membrane arranged inside; a second-stage gas-venting and guiding component connected to the first-stage condensate component and a third-stage gas-venting and guiding component connected to the second-stage gas-venting and guiding component; the end of the third-stage gas-venting and guiding component is connected to a liquid collection tank through a guiding pipeline, and the liquid collection tank is connected to a reflux feeding port through a reflux pipeline and a reflux valve.

[0012] Furthermore, the first-stage condensate component, the second-stage gas-venting and guiding component and the third-stage gas-venting and guiding component are three independent units connected in sequence;

[0013] Among them, the first-stage condensate component includes: a first-stage condensation outer shell and a first-stage condensation inner pipe. A closed first cooling channel is formed between the first-stage condensation outer shell and the first-stage condensation inner pipe. A first inlet and a first outlet are arranged on the first-stage condensation outer shell. The first inlet is connected to a cold water tank through a first flow control valve and a first inlet water pipeline, and the first outlet is connected to a recovery water tank through a second flow control valve and a first reflux pipeline;

[0014] And the replacement speed of the cooling water in the first cooling channel is controlled by setting the opening degrees of the first flow control valve and the second flow control valve to achieve controlling the cooling degree of the first-stage condensate component on the air flow;

[0015] Moreover, the air flow of the multi-stage composite membrane disposed in the first-stage condensation inner tube undergoes wire mesh condensation during the condensation process. After condensing into droplets, it accelerates through the multi-stage composite membrane under the action of the gas and enters the second-stage air venting and guiding component. Among them, the gas freely passes through the multi-stage composite membrane and enters the interior of the second-stage air venting and guiding component;

[0016] The second-stage air venting and guiding component includes: a second-stage condensation outer shell and a second-stage condensation inner tube. The second-stage condensation inner tube is set with a first groove whose bottom is inclined downward. The first groove conveys condensed water to the third-stage air venting and guiding component. The upper part of the second-stage condensation inner tube is set with a first guiding groove that collects gas into a gas collection tank; a second cooling channel is formed between the second-stage condensation outer shell and the second-stage condensation inner tube. A second inlet and a second outlet are provided on the second-stage condensation outer shell. The second inlet is connected to a cold water tank through a third flow control valve and a second water inlet pipeline. The second outlet is connected to a recovery tank through a fourth flow control valve and a second return pipeline; and by setting the opening degrees of the third flow control valve and the fourth flow control valve, the replacement speed of the cooling water in the second cooling channel is controlled to achieve the control of the cooling degree of the second-stage condensation component on the air flow;

[0017] The third-stage air venting and guiding component includes: a third-stage condensation outer shell and a third-stage condensation inner tube. The third-stage condensation inner tube is set with a second groove whose bottom is inclined downward. The second groove conveys condensed water to the end of the third-stage condensation inner tube. The upper part of the third-stage condensation inner tube is set with a second guiding groove that collects gas into a gas collection tank; a third cooling channel is formed between the third-stage condensation outer shell and the third-stage condensation inner tube. A third inlet and a third outlet are provided on the third-stage condensation outer shell. The third inlet is connected to a cold water tank through a fifth flow control valve and a third water inlet pipeline. The third outlet is connected to a recovery tank through a sixth flow control valve and a third return pipeline; and by setting the opening degrees of the fifth flow control valve and the sixth flow control valve, the replacement speed of the cooling water in the third cooling channel is controlled to achieve the control of the cooling degree of the third-stage condensation component on the air flow; wherein, the inclination degrees of the first groove and the second groove are the same, and the first groove and the second groove are connected end to end.

[0018] Furthermore, a temperature sensor, a pressure sensor, and a pH value detection sensor are disposed in the reaction chamber; and the temperature sensor, the pressure sensor, and the pH value detection sensor are respectively connected to a control device.

[0019] The present invention also provides a preparation method of benzoyl Corey lactone, including the preparation device of benzoyl Corey lactone described above, and is characterized by including the following steps:

[0020] 1) Add 40 L of pyridine into the reaction chamber, and then add 4 kg of Corey lactone diol. The control device drives the push rod according to the set first instruction to drive the push piston to perform a slow reciprocating motion in the reaction chamber within the first set period, so as to drive the mixture of Corey lactone diol and pyridine to surge in the reaction chamber along with the movement of the push piston and complete the mixing. After mixing, control the push cylinder to stop moving, and add 7 kg of triphenylmethyl chloride into the reaction chamber to obtain a primary reaction mixture;

[0021] 2) Control the temperature in the reaction chamber to be maintained at 15 - 20 °C. The control device drives the push rod according to the set second instruction to drive the push piston to perform a slow reciprocating motion in the reaction chamber within the second set period, so as to drive the primary reaction mixture to surge in the reaction chamber along with the movement of the push piston and complete the complete reaction to obtain a first mixture;

[0022] 3) Control the temperature in the reaction chamber to be maintained at 18 - 22 °C, and gradually add 5 L of benzoyl chloride into the reaction chamber. At the same time, the control device drives the push rod according to the set third instruction to drive the push piston to perform a slow reciprocating motion in the reaction chamber within the third set period, so as to drive the first mixture and benzoyl chloride to surge in the reaction chamber along with the movement of the push piston and complete the complete reaction to obtain a second mixture;

[0023] 4) Keep the temperature at 18 - 22 °C, and add 50 L of pure water into the reaction chamber. At the same time, the control device controls the push cylinder to drive the push rod to drive the push piston to perform a reciprocating motion in the reaction chamber within the set period according to the set periodic control instruction set. And within the set period, the pushing stroke of the push piston in the reaction chamber gradually increases, so that the second mixture and pure water in the reaction chamber are mixed in a cyclic manner multiple times during the reciprocating motion of the push piston to form a suspension. And when the pushing stroke gradually increases, it promotes the pressure environment in the reaction chamber to gradually increase. The gradually increasing pressure environment accelerates the formation of the suspension. When at the end of the execution of the set period, the pushing stroke of the push piston gradually reaches the maximum, the pressure in the reaction chamber reaches the upper limit value triggered by the pressure control valve. At this time, the pressure control valve is opened, and the suspension in the reaction chamber is pressure-filtered to obtain a third mixture. The control device controls the push cylinder to retract;

[0024] 5) Add 45 L of methanol into the reaction chamber, control the heating component to heat the inside of the reaction chamber, and maintain the temperature at 150 - 180 °C. The control device controls the feeding cylinder to push the push rod according to the set fourth instruction to drive the feeding piston to reciprocate in the reaction chamber, so as to drive the fourth mixture and methanol to mix in the reaction chamber with the movement of the feeding piston. After mixing, stop the operation of the feeding cylinder, then open the exhaust valve, carry out heating reflux for 3 - 4 hours, and then close the exhaust valve and the heating component to reduce the temperature in the reaction chamber to room temperature;

[0025] 6) The control device controls the feeding cylinder to push the push rod according to the set fifth instruction to drive the feeding piston to move forward in the reaction chamber with the maximum stroke. The pressure in the reaction chamber reaches the upper limit value triggered by the pressure control valve. At this time, the pressure control valve is opened to filter the liquid in the reaction chamber to obtain solid powder, and then the control device controls the feeding cylinder to retract; Add 48 L of acetonitrile into the reaction chamber; Then gradually add 55 L of hydrochloric acid aqueous solution with a concentration of 1 - 2 mol / L into the reaction chamber to form the fifth mixture; The control device controls the heating component to heat the reaction chamber to 32 - 35 °C, and at the same time, the control device controls the feeding cylinder to push the push rod according to the set sixth instruction to drive the feeding piston to reciprocate slowly in the reaction chamber to drive the fifth mixture to react fully in the reaction chamber with the movement of the feeding piston to obtain the sixth mixture, and then the control device controls the feeding cylinder to stop working;

[0026] 7) Control the temperature in the reaction chamber to be maintained at 18 - 22 °C, gradually add saturated sodium bicarbonate aqueous solution into the reaction chamber for neutralization reaction, and at the same time, the control device controls the feeding cylinder to push the push rod according to the set seventh instruction to drive the feeding piston to reciprocate slowly in the reaction chamber to drive the sixth mixture and saturated sodium bicarbonate aqueous solution to mix and react fully in the reaction chamber until pH = 7 to obtain the seventh reactant, and then the control device controls the feeding cylinder to stop working;

[0027] 8) Control the heating component to heat the inside of the reaction chamber and maintain the temperature at 100 - 120 °C. At the same time, open the exhaust valve to evaporate all the acetonitrile in the seventh reactant to obtain the crude product. After evaporation, reduce the temperature in the reaction chamber to 60 °C. The control device controls the feeding cylinder to push the push rod according to the set eighth instruction to drive the feeding piston to move forward in the reaction chamber with the maximum stroke. The pressure in the reaction chamber reaches the upper limit value triggered by the pressure control valve. At this time, the pressure control valve is opened to filter the liquid in the crude product in the reaction chamber, and then the control device controls the feeding cylinder to retract;

[0028] 9) Add 25 L of isopropyl ether into the reaction chamber. The control device controls the pusher cylinder to push the push rod according to the set ninth instruction within the ninth set period, so as to drive the pusher piston to perform a slow reciprocating motion in the reaction chamber, so as to drive the crude product to be completely mixed with isopropyl ether. After uniform mixing, a primary refined product is formed. Then, close the pusher cylinder, control the heating component to heat the inside of the reaction chamber, and maintain the temperature at 150 - 180 °C. At the same time, open the exhaust valve and carry out heating reflux for 2 - 3 hours. Then, close the exhaust valve. The control device controls the pusher cylinder to push the push rod according to the set tenth instruction to drive the pusher piston to move forward in the reaction chamber with the maximum stroke. The pressure in the reaction chamber reaches the upper limit value triggered by the pressure control valve. At this time, the pressure control valve is opened, and the liquid in the primary refined product in the reaction chamber is pressure-filtered. After the pressure filtration is completed, the control device controls the pusher cylinder to retract the pusher piston, and then controls the temperature of the heating component to be 40 - 50 °C, and dry for 1 - 3 hours at 40 - 50 °C to obtain benzoyl Corey lactone.

[0029] This application designs a device for industrial preparation of benzoyl Corey lactone. Compared with the traditional laboratory preparation method, this application can be continuously produced and can complete large-scale production.

[0030] This application uses a way similar to surging to evenly mix the materials. Compared with the stirring method, the surging method makes the distribution of solids more uniform when the solid-liquid is suspended. When stirring, it is easy for the solids to gather in the central vortex of the stirring, which is not conducive to the uniform distribution of solids. And through the piston propulsion, the pressure in the reaction chamber gradually increases, and the increasing pressure also accelerates the uniform mixing. Brief Description of the Drawings

[0031] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following will briefly introduce the drawings required for use in the embodiment descriptions. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0032] Figure 1 It is a schematic structural diagram of the device provided by the present invention;

[0033] Figure 2 It is a schematic structural diagram of the reflux cooling device provided by the present invention. Detailed Embodiments

[0034] To make the purpose, technical solutions and advantages of the present invention clearer, the following will further describe the embodiments of the present invention in detail with reference to the drawings.

[0035] Example 1, refer to Figure 1 and Figure 2, the present invention provides a preparation device for benzoyl Corey lactone, comprising: a reaction device, which includes a reaction housing 4. Inside the reaction housing 4, a reaction inner cylinder 41 is provided. A cooling space 40 is formed between the reaction inner cylinder 41 and the reaction housing 4. And a heating component is preset in the reaction inner cylinder 41 and uniformly arranged, and a reaction chamber 42 is formed inside the reaction inner cylinder 41;

[0036] A pushing piston 3 is arranged in the reaction chamber 42. One end of the pushing piston 3 is connected to a push rod 2, and the push rod 2 is arranged on a pushing cylinder 1;

[0037] At the inner end of the reaction chamber 42 and at the lower part of the reaction inner cylinder 41, a pressure control valve 50 is embedded. The pressure control valve 50 passes through the cooling space 40 and the reaction housing 4 and is fixed to one end of a connecting pipe arranged outside the reaction housing 4. The other end of the connecting pipe is fixed to the inlet of a filtering valve 52, and the filtering valve 52 is embedded inside a filter cylinder 5;

[0038] At the inner end of the reaction chamber 42 and at the upper part of the reaction inner cylinder 41, an exhaust valve 60 is embedded. The exhaust valve 60 passes through the cooling space 40 and the reaction housing 4 and is connected to one end of an exhaust valve joint 61 arranged outside the reaction housing 4. The other end of the exhaust valve joint 61 is connected to an exhaust pipe 62, and the exhaust pipe 62 is connected to a reflux cooling device 6;

[0039] On the upper surface of the reaction housing 4, a multi-way joint component 7 is provided. The multi-way joint component 7 includes a joint housing and a plurality of solenoid valves embedded inside the joint housing. Each solenoid valve is connected to a feeding tank 71 through a corresponding feeding pipeline and a meter 72 arranged on the feeding pipeline. Among them, the solenoid valve is arranged on the feeding pipeline, and the feeding pipeline is arranged inside the joint housing and communicated with the reaction chamber.

[0040] A control device is connected to the pushing cylinder 1, the pressure control valve 50, the exhaust valve 60, the multi-way joint component 7 and the heating component.

[0041] Further, an inlet pipe 81 for adding a cooling medium and a reflux pipe 91 for the cooling medium to flow out are provided on the reaction housing 4. Among them, the inlet pipe 81 is connected to a cooling water tank 8 through an inlet water pipeline and an inlet end switching valve 80 arranged on the inlet water pipeline. The reflux pipe 91 is connected to a return water tank 9 through a reflux pipeline and a reflux switching valve 89 arranged on the reflux pipeline.

[0042] Further, the filter cylinder 5 seals and fixes the filtering valve 52, the connecting pipe and the extended section of the pressure control valve 50 outside the reaction housing 4 together on the outside of the reaction housing 4.

[0043] Further, the reflux cooling device 6 is a three-stage cooling device, including a first-stage condensate component provided with a multi-stage composite membrane 65 therein; a second-stage gas-venting and guiding component connected to the first-stage condensate component; and a third-stage gas-venting and guiding component connected to the second-stage gas-venting and guiding component; the end of the third-stage gas-venting and guiding component is connected to the liquid collection tank 300 through a guiding pipeline, a guiding valve 690 is arranged on the guiding pipeline, and the liquid collection tank 300 is connected to the reflux material port through a reflux pipeline and a reflux valve.

[0044] Further, the first-stage condensate component, the second-stage gas-venting and guiding component, and the third-stage gas-venting and guiding component are three independent units connected in sequence;

[0045] Among them, the first-stage condensate component includes: a first-stage condensation outer shell and a first-stage condensation inner pipe. A closed first cooling channel 64 is formed between the first-stage condensation outer shell and the first-stage condensation inner pipe. A first inlet 201 and a first outlet 106 are opened on the first-stage condensation outer shell. The first inlet 201 is connected to the cold water tank 200 through a first flow control valve 202 and a first water inlet pipeline, and the first outlet 106 is connected to the recovery water tank 100 through a second flow control valve 105 and a first reflux pipeline;

[0046] And by setting the opening degrees of the first flow control valve 202 and the second flow control valve 105 to control the replacement speed of the cooling water in the first cooling channel 64, so as to control the cooling degree of the first-stage condensate component on the air flow;

[0047] And the air flow passing through the multi-stage composite membrane 65 arranged in the first-stage condensation inner pipe is subjected to netting condensation during the condensation process. After condensing into liquid droplets, it penetrates through the multi-stage composite membrane and enters the second-stage gas-venting and guiding component. Among them, the gas freely passes through the multi-stage composite membrane and enters the interior of the second-stage gas-venting and guiding component; the first-stage condensation inner pipe is connected to the exhaust pipe 62 through a butt joint pipe 63.

[0048] The second-stage gas-venting and guiding component includes: a second-stage condensation outer shell and a second-stage condensation inner pipe 67. The second-stage condensation inner pipe 67 is arranged with a first groove with a downward slope at the bottom, and the first groove is used to convey the condensed water to the third-stage gas-venting and guiding component. The upper part of the second-stage condensation inner pipe is arranged with a first guiding groove with an upward slope, and the gas is collected into the gas collection tank 400 through the first guiding groove; a second cooling channel 66 is formed between the second-stage condensation outer shell and the second-stage condensation inner pipe. A second inlet 203 and a second outlet 103 are opened on the second-stage condensation outer shell. The second inlet 203 is connected to the cold water tank through a third flow control valve 204 and a second water inlet pipeline, and the second outlet 103 is connected to the recovery water tank 100 through a fourth flow control valve 104 and a second reflux pipeline; and by setting the opening degrees of the third flow control valve 204 and the fourth flow control valve 104 to control the replacement speed of the cooling water in the second cooling channel, so as to control the cooling degree of the second-stage condensate component on the air flow;

[0049] The three-stage air evacuation and diversion assembly includes: a three-stage condensation outer shell and a three-stage condensation inner tube. The three-stage condensation inner tube is configured to have a second groove with a downward inclination at the bottom. The second groove is used to transport condensed water to the end of the three-stage condensation inner tube. The upper part of the three-stage condensation inner tube is configured to have a second diversion groove with an upward inclination, and the gas is collected into the gas collection tank through the second diversion groove; a third cooling channel 68 is formed between the three-stage condensation outer shell and the three-stage condensation inner tube, and a third inlet 206 and a third outlet 102 are provided on the three-stage condensation outer shell. The third inlet is connected to the cold water tank through the fifth flow control valve 205 and the third water inlet pipeline, and the third outlet is connected to the recovery water tank through the sixth flow control valve 101 and the third return pipeline; and the replacement speed of the cooling water in the third cooling channel is controlled by setting the opening of the fifth flow control valve and the sixth flow control valve to achieve the control of the cooling degree of the airflow by the three-stage condensation assembly; wherein, the inclination of the first groove and the second groove is the same, and the first groove and the second groove are connected end to end.

[0050] Furthermore, the reaction chamber 42 is equipped with a temperature sensor, a pressure sensor, and a pH value detection sensor; and the temperature sensor, the pressure sensor, and the pH value detection sensor are connected to the control device respectively.

[0051] Example 2

[0052] The present invention also provides a method for preparing benzoylcorine lactone, comprising the following steps:

[0053] 1) The control device opens the first solenoid valve connected to the first feeding tank and embedded in the joint housing, and opens the first metering device, and adds 40L of pyridine from the first feeding tank through the first feeding line, the first metering device, and the first solenoid valve into the reaction chamber 42; after the addition is completed, the control device opens the second solenoid valve connected to the second feeding tank and embedded in the joint housing, and opens the second metering device, and adds 4kg of corianol diol from the second feeding tank through the second feeding line, the second metering device, and the second solenoid valve into the reaction chamber 42; the control device controls the push according to the set first instruction The cylinder 1 pushes the push rod 2 within a first set period to drive the push piston 3 to perform a slowed reciprocating motion within the reaction chamber 42, thereby causing the mixture of corianolactone diol and pyridine to surge within the reaction chamber 42 along with the movement of the push piston 3, thereby completing mixing. After mixing, the push cylinder 1 is controlled to stop, and a third solenoid valve connected to the third feeding tank and embedded in the joint housing is opened by the control device, and the third meter is opened. 7 kg of triphenylmethane is added from the third feeding tank into the reaction chamber 42 through the third feeding line, the third meter, and the third solenoid valve to obtain a primary reaction mixture.

[0054] 2) The control device opens the inlet end switch valve, adds cooling water into the cooling space 40 until it is full, then controls the reflux switch valve to open, and sets the opening degrees of the inlet end switch valve and the reflux switch valve to be the same, both being 20% of the full opening degree, so as to keep the temperature in the reaction chamber 42 at 15 - 20 °C. The control device controls the pusher cylinder 1 to push the push rod 2 within the second set period according to the set second instruction, so as to drive the pusher piston 3 to perform a slow reciprocating motion in the reaction chamber 42, so as to drive the primary reaction mixture to surge in the reaction chamber 42 along with the movement of the pusher piston 3 and thus complete the complete reaction to obtain the first mixture. The control device controls the pusher cylinder 1 to stop working;

[0055] 3) The control device sets the opening degrees of the inlet end switch valve and the reflux switch valve to 15% of the full opening degree, so as to keep the temperature in the reaction chamber 42 at 18 - 22 °C. The control device opens the fourth solenoid valve connected to the fourth charging tank and embedded on the joint housing, and opens the fourth meter. 5 L of benzoyl chloride is gradually added into the reaction chamber 42 from the fourth charging tank through the fourth charging pipeline, the fourth meter and the fourth solenoid valve. At the same time, the control device controls the pusher cylinder 1 to push the push rod 2 within the third set period according to the set third instruction, so as to drive the pusher piston 3 to perform a slow reciprocating motion in the reaction chamber 42, so as to drive the first mixture and benzoyl chloride to surge in the reaction chamber 42 along with the movement of the pusher piston 3 and thus complete the complete reaction to obtain the second mixture. The control device controls the pusher cylinder 1 to stop working;

[0056] 4) Keep the temperature at 18 - 22 °C. The control device opens the fifth solenoid valve connected to the fifth charging tank and embedded on the joint housing, and opens the fifth meter. 50 L of pure water is added into the reaction chamber 42 from the fifth charging tank through the fifth charging pipeline, the fifth meter and the fifth solenoid valve. At the same time, the control device controls the pusher cylinder 1 to push the push rod 2 within the set period according to the set periodic control instruction set, so as to drive the pusher piston 3 to perform a reciprocating motion in the reaction chamber 42. And within the set period, the pushing stroke of the pusher piston 3 in the reaction chamber 42 gradually increases, so that the second mixture and pure water in the reaction chamber 42 are mixed in a cyclic manner multiple times during the reciprocating motion of the pusher piston 3 to form a suspension. And when the pushing stroke gradually increases, it promotes the pressure environment in the reaction chamber 42 to gradually increase. The gradually increasing pressure environment accelerates the formation of the suspension. When at the end of the execution of the set period, the pushing stroke of the pusher piston 3 gradually reaches the maximum, the pressure in the reaction chamber 42 reaches the upper limit value triggered by the pressure control valve 50. At this time, the pressure control valve 50 is opened, and the suspension in the reaction chamber 42 is pressure-filtered to obtain the third mixture. The control device controls the pusher cylinder 1 to retract;

[0057] 5) The control device opens the sixth solenoid valve connected to the sixth charging tank and embedded in the joint housing, and opens the sixth meter. 45 L of methanol is added into the reaction chamber 42 from the sixth charging tank through the sixth charging pipeline, the sixth meter, and the sixth solenoid valve. The control device closes the inlet end switch valve, then sets the opening degree of the reflux switch valve to the full opening degree, returns all the cooling water in the cooling space 40 to the return water tank, then closes the reflux switch valve. The control device heats the interior of the reaction chamber 42 by controlling the heating component and maintains the temperature at 150 - 180 °C. The control device controls the pushing cylinder 1 to push the push rod 2 to drive the push piston 3 to reciprocate in the reaction chamber 42 according to the set fourth instruction within the fourth set period, so as to drive the fourth mixture and methanol to mix in the reaction chamber 42 with the movement of the push piston 3. After mixing, the work of the pushing cylinder 1 is stopped, then the exhaust valve 60 is opened, and heating reflux is carried out for 3 - 4 hours. Then the exhaust valve 60 and the heating component are closed. The control device opens the inlet end switch valve, adds cooling water into the cooling space 40 and fills it up. Then the control device opens the reflux switch valve and sets the opening degrees of the inlet end switch valve and the reflux switch valve to be the same, both being 30% of the full opening degree. When the temperature in the reaction chamber 42 drops to room temperature, the control device closes the inlet end switch valve, then sets the opening degree of the reflux switch valve to the full opening degree, returns all the cooling water in the cooling space 40 to the return water tank, and then closes the reflux switch valve;

[0058] 6) The control device controls the pushing cylinder 1 to push the push rod 2 to drive the push piston 3 to move forward with the maximum stroke in the reaction chamber 42 according to the set fifth instruction. The pressure in the reaction chamber 42 reaches the upper limit value triggered by the pressure control valve 50. At this time, the pressure control valve 50 is opened, and the liquid in the reaction chamber 42 is pressure-filtered to obtain solid powder. Then the control device controls the pushing cylinder 1 to retract; The control device opens the seventh solenoid valve connected to the seventh charging tank and embedded in the joint housing, and opens the seventh meter. 48 L of acetonitrile is added into the reaction chamber 42 from the seventh charging tank through the seventh charging pipeline, the seventh meter, and the seventh solenoid valve; Then, the control device opens the eighth solenoid valve connected to the eighth charging tank and embedded in the joint housing, and opens the eighth meter. 55 L of hydrochloric acid aqueous solution with a concentration of 1 - 2 mol / L is gradually added into the reaction chamber 42 from the eighth charging tank through the eighth charging pipeline, the eighth meter, and the eighth solenoid valve to form the fifth mixture; The control device controls the heating component to heat the reaction chamber 42 to 32 - 35 °C. At the same time, the control device controls the pushing cylinder 1 to push the push rod 2 to drive the push piston 3 to reciprocate slowly in the reaction chamber 42 according to the set sixth instruction within the sixth set period, so as to drive the fifth mixture to fully react in the reaction chamber 42 with the movement of the push piston 3 to obtain the sixth mixture. Then the control device controls the pushing cylinder 1 to stop working;

[0059] 7) The control device opens the inlet end switch valve, adds cooling water into the cooling space 40 until it is full, then controls the reflux switch valve to open, and sets the opening degrees of the inlet end switch valve and the reflux switch valve to be the same, both being 15% of the full opening degree, so as to keep the temperature in the reaction chamber 42 at 18 - 22 °C. The control device opens the ninth electromagnetic valve connected to the ninth feeding tank and embedded on the joint housing, and opens the ninth meter. The saturated sodium bicarbonate aqueous solution is gradually added from the ninth feeding tank into the reaction chamber 42 through the ninth feeding pipeline, the ninth meter, and the ninth electromagnetic valve for neutralization reaction. At the same time, the control device controls the pushing cylinder 1 to push the push rod 2 within the seventh set period according to the set seventh instruction, so as to drive the pushing piston 3 to perform a slow reciprocating motion in the reaction chamber 42, so as to drive the sixth mixture and the saturated sodium bicarbonate aqueous solution to fully mix and react in the reaction chamber 42 until pH = 7, obtaining the seventh reactant. Then the control device controls the pushing cylinder 1 to stop working;

[0060] 8) The control device closes the inlet end switch valve, then sets the opening degree of the reflux switch valve to the full opening degree, returns all the cooling water in the cooling space 40 to the return water tank, then closes the reflux switch valve, controls the heating component to heat the inside of the reaction chamber 42, and keeps the temperature at 100 - 120 °C. At the same time, the exhaust valve 60 is opened to evaporate all the acetonitrile in the seventh reactant, obtaining the crude product. After the evaporation is completed, the control device opens the inlet end switch valve, adds cooling water into the cooling space 40 until it is full, then controls the reflux switch valve to open, and sets the opening degrees of the inlet end switch valve and the reflux switch valve to be the same, both being 30% of the full opening degree. When the temperature in the reaction chamber 42 is reduced to 60 °C, the control device closes the inlet end switch valve, then sets the opening degree of the reflux switch valve to the full opening degree, returns all the cooling water in the cooling space 40 to the return water tank, and then closes the reflux switch valve; the control device controls the pushing cylinder 1 to push the push rod 2 to drive the pushing piston 3 to move forward with the maximum stroke in the reaction chamber 42 according to the set eighth instruction. The pressure in the reaction chamber 42 reaches the upper limit value triggered by the pressure control valve 50. At this time, the pressure control valve 50 is opened to filter the liquid in the crude product in the reaction chamber 42, and then the control device controls the pushing cylinder 1 to retract;

[0061] 9) Open the tenth solenoid valve connected to the tenth feeding tank and embedded on the joint housing through the control device, and open the tenth meter. Add 25L of saturated isopropyl ether into the reaction chamber 42 from the tenth feeding tank through the tenth feeding pipeline, the tenth meter, and the tenth solenoid valve. The control device controls the pushing cylinder 1 to drive the push rod 2 to drive the push piston 3 to perform a slow reciprocating motion in the reaction chamber 42 according to the set ninth instruction within the ninth set period, so as to drive the crude product to be completely mixed with isopropyl ether. After being evenly mixed, a primary refined product is formed. Then, close the pushing cylinder 1, control the heating component to heat the inside of the reaction chamber 42, and maintain the temperature at 150 - 180 °C. At the same time, open the exhaust valve 60 and carry out heating reflux for 2 - 3 hours. Then, close the exhaust valve 60. The control device controls the pushing cylinder 1 to drive the push rod 2 to drive the push piston 3 to move forward in the reaction chamber 42 with the maximum stroke according to the set tenth instruction. The pressure in the reaction chamber 42 reaches the upper limit value triggered by the pressure control valve 50. At this time, the pressure control valve 50 is opened, and the liquid in the primary refined product in the reaction chamber 42 is pressure-filtered. After the pressure filtration is completed, the control device controls the pushing cylinder 1 to retract the push piston 3, then controls the temperature of the heating component to be 40 - 50 °C, and then opens the water inlet end switch valve through the control device, adds cooling water into the cooling space 40 and fills it up. Then, control the reflux switch valve to open, and set the opening degrees of the water inlet end switch valve and the reflux switch valve to be the same, and both are 30% of the full opening degree, so that when the temperature in the reaction chamber 42 is kept reduced to 60 °C, then close the water inlet end switch valve through the control device, then set the opening degree of the reflux switch valve to be the full opening degree, return all the cooling water in the cooling space 40 to the return water tank, and then close the reflux switch valve, so that the temperature of the reaction chamber 42 gradually drops to 40 - 50 °C, and dry for 1 - 3 hours at 40 - 50 °C to obtain benzoyl Corey lactone.

[0062] In the above, set the upper limit value triggered by the pressure control valve 50 (for example, set it to 5 - 15 Kpa); among them, the upper limit value triggered by the pressure control valve 50 only needs to be set once before starting the machine. The pressure control valve 50 can be realized by the following methods. One is to set a group of pressure sensors on the inner wall of the reaction chamber 42, collect the pressure in the reaction chamber 42 in real time through the pressure sensors, and transmit the collected pressure data to the control device. The control device receives the pressure data and compares it with the set upper limit value triggered by the pressure control valve 50 to judge whether it exceeds. If it exceeds, control the pressure control valve 50 to open. If it does not exceed, control the pressure control valve 50 to remain closed. The pressure control valve 50 adopts an intelligent control type solenoid valve and is connected to the control device. Another scheme is to adopt an adaptive pressure regulating valve for automatic control.

[0063] In the above, the set of periodic control instructions refers to the same as the above-set period (circulating once every 30 minutes). That is to say, the set of control instructions also circulates once every 30 minutes, and the execution of the instructions for one cycle is completed within 30 minutes. The set of control instructions is a set of instructions for controlling the pusher cylinder 1. For example, one instruction is executed every 3 minutes. In the first 3 minutes, the maximum stroke of the pusher cylinder 1 pushing the pusher piston 3 forward through the push rod 2 is 5 unit amounts (which can be actually converted into a specific distance). In 3 minutes, the pusher piston 3 is driven to reciprocate in the reaction chamber 42. When the pusher piston 3 reciprocates in the reaction chamber 42, the material in the corresponding reaction chamber 42 is uniformly mixed in a form similar to surging back and forth (simulating the ebb and flow of the tide). When the pusher piston 3 is pushed forward, the pressure in the reaction chamber 42 gradually increases, and the increase in pressure also accelerates the uniform mixing of the material. In the second 3 minutes, the maximum stroke of the pusher cylinder 1 pushing the pusher piston 3 forward through the push rod 2 is 10 unit amounts, and so on. Until the 10th 3 minutes, the maximum stroke of the pusher cylinder 1 pushing the pusher piston 3 forward through the push rod 2 is 50 unit amounts. At this time, the pushing stroke is the largest and reaches the upper limit value for triggering the pressure control valve 50 to trigger.

[0064] This application uses a way similar to surging to uniformly mix the material. Compared with the stirring method, the surging method makes the distribution of solids more uniform when the solid-liquid is suspended. When stirring, it is easy for the solids to gather in the central vortex of the stirring, which is not conducive to the uniform distribution of solids. And through the piston propulsion, the pressure in the reaction chamber 42 gradually increases, and the increase in pressure also accelerates the uniform mixing.

[0065] In step 5), during the reflux cooling, the replacement speed of the cooling water in the first cooling channel is controlled by setting the opening degrees of the first flow control valve and the second flow control valve to achieve the control of the cooling degree of the gas flow by the first-stage condensate component; and the gas flow of the multi-stage composite membrane arranged in the first-stage condensate inner tube is subjected to net condensation during the condensation process, and after condensing into liquid droplets, it penetrates through the multi-stage composite membrane and enters the second-stage gas drainage and diversion component; the replacement speed of the cooling water in the second cooling channel is controlled by setting the opening degrees of the third flow control valve and the fourth flow control valve to achieve the control of the cooling degree of the gas flow by the second-stage condensate component; the replacement speed of the cooling water in the third cooling channel is controlled by setting the opening degrees of the fifth flow control valve and the sixth flow control valve to achieve the control of the cooling degree of the gas flow by the third-stage condensate component.

[0066] In step 8), during evaporation, without using the reflux cooling method, directly open the first diversion valve 403 at the first diversion groove 404 and the second diversion valve 402 at the second diversion groove 401, and close the collection reflux valve 69 at the end of the three-stage condensation component. When the acetonitrile vapor encounters the multi-stage composite membrane without cooling, it does not form a network but is directly collected into the recovery tank through the first diversion groove, the first diversion valve, the second diversion groove, and the second diversion valve.

[0067] The heating reflux in step 9) is the same as that in step 5).

[0068] It should be noted that in the above, a storage module is provided in the control device. This storage module is used to store various instructions set by the control device. At the same time, when pressure filtration is not involved, the pushing stroke of the pushing cylinder 1 in any state is set according to the requirements of mixing or reaction, but it will not reach the upper limit value of the pressure setting of the pressure control valve 50. In this application, the pressure filtration valve is the same as the common filtration valve 52, allowing liquid to pass through, while suspended substances and solids are blocked and not pressure-filtered out.

[0069] It should also be noted that the capacity of the reaction inner cylinder 41 in this application reaches 350 - 600L. Without considering pressure filtration, the materials in the entire reaction cavity cannot reach the same height as the exhaust valve. At the same time, during the evaporation operation and the heating reflux operation, the pushing cylinder is not used synchronously to ensure that no materials flow out of the exhaust valve during the entire process.

[0070] It should also be noted that the filter cartridge in this application is also provided with a discharge port for recovering the process materials generated during the pressure filtration process.

[0071] During the heating reflux operation process, it should also be noted that this application also provides a pressurizing pipe at the docking pipe 63 that is inclined towards the one-stage cooling channel. This pressurizing pipe is connected to the gas tank through a pressurizing valve and a pressurizing pump, and an inert gas is introduced into the one-stage cooling channel through the pressurizing pipe to accelerate the liquid penetration through the multi-stage composite filtration membrane. When using inert gas pressurization, synchronously open the first diversion valve 403 at the first diversion groove 404 and the second diversion valve 402 at the second diversion groove 401 for the recovery of the inert gas. It should be noted that in the design of this application, the acetonitrile vapor is also recovered using the above method, but after both have completed the recovery and use, that is, when the recovery tank is completely recovered, the next step can be carried out. The two cannot be mixed together.

[0072] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included within the protection scope of the present invention.

Claims

1. A preparation device for benzoylcorine lactone, characterized in that, include: A reaction device, comprising a reaction shell, an inner reaction cylinder disposed inside the reaction shell, a cooling space formed between the inner reaction cylinder and the reaction shell, and uniformly arranged heating components pre-set inside the inner reaction cylinder, the interior of the inner reaction cylinder forming a reaction chamber; A push piston is disposed in the reaction chamber, and one end of the push piston is connected to a push rod, which is disposed on a push cylinder. The push cylinder pushes the push rod to drive the push piston to perform a slow reciprocating motion in the reaction chamber, thereby achieving mixing of the reaction materials in the reaction chamber. A pressure control valve is embedded at the inner end of the reaction chamber and at the lower part of the reaction inner cylinder. The pressure control valve passes through the cooling space and the reaction shell and is fixed to one end of a connecting pipe arranged outside the reaction shell. The other end of the connecting pipe is fixed to the inlet of the filter valve, and the filter valve is embedded in the filter cartridge. An exhaust valve is embedded at the inner end of the reaction chamber and located on the upper part of the reaction inner cylinder. The exhaust valve passes through the cooling space and the reaction shell and is connected to one end of an exhaust valve connector provided outside the reaction shell. The other end of the exhaust valve connector is connected to an exhaust pipe, and the exhaust pipe is connected to a reflux cooling device. A multi-way connector assembly is provided on the upper surface of the reaction shell, the multi-way connector assembly comprising a connector shell, a plurality of solenoid valves embedded in the connector shell, each solenoid valve being connected to a feeding tank via a corresponding feeding pipeline and a meter provided on the feeding pipeline; A control device, connecting the push cylinder, the pressure control valve, the exhaust valve, the multi-way joint assembly and the heating assembly; The reflux cooling device is a three-stage cooling device, including a first-stage condensing component in which a multi-stage composite membrane is arranged, a second-stage air drainage and diversion component connected to the first-stage condensing component, and a third-stage air drainage and diversion component connected to the second-stage air drainage and diversion component. The ends of the three-stage air drainage and diversion components are connected to the liquid collecting tank through the diversion pipeline, and the liquid collecting tank is connected to the reflux material port through the reflux pipeline and the reflux valve.

2. The preparation device of benzoylcorine lactone according to claim 1, wherein An inlet pipe for adding a cooling medium and a return pipe for discharging the cooling medium are provided on the reaction shell, wherein the inlet pipe is connected to the cooling water tank through an inlet pipe and a water inlet end switch valve on the inlet pipe, and the return pipe is connected to the return water tank through a return pipe and a return switch valve provided on the return pipe.

3. The preparation device of benzoylcorine lactone according to claim 1, wherein The filter cartridge seals the filter valve, the connecting pipe and the pressure control valve together at an extension section outside the reaction shell and fixes them outside the reaction shell.

4. The preparation device of benzoylcorine lactone according to claim 1, wherein The first stage condensing assembly, the second stage evacuation and diversion assembly, and the third stage evacuation and diversion assembly are three independent units connected in sequence; The first stage condensing assembly includes: a condensing outer shell and a condensing inner tube, a closed first cooling channel is formed between the condensing outer shell and the condensing inner tube, and a first inlet and a first outlet are opened on the condensing outer shell, the first inlet is connected to the cold water tank through a first flow control valve and a first water inlet pipeline, and the first outlet is connected to the recovery water tank through a second flow control valve and a first return pipeline; The replacement speed of the cooling water in the first cooling channel is controlled by setting the opening of the first flow control valve and the second flow control valve, so as to control the cooling degree of the air flow by the first condensing component; The airflow passing through the multi-stage composite membrane disposed in the first-stage condensation inner tube is subjected to mesh condensation during the condensation process. After condensation into droplets, the droplets penetrate the multi-stage composite membrane and enter the second-stage gas drainage and diversion assembly. The gas freely passes through the multi-stage composite membrane and enters the interior of the second-stage gas drainage and diversion assembly. The two-stage air evacuation and diversion assembly includes: a two-stage condensation outer shell and a two-stage condensation inner tube, the two-stage condensation inner tube is configured to have a first groove with a downward inclination at the bottom, the first groove is used to transport condensed water to the three-stage air evacuation and diversion assembly, and the upper part of the two-stage condensation inner tube is configured to have a first diversion groove with an upward inclination, and the gas is collected into the gas collection tank through the first diversion groove; a second cooling channel is formed between the two-stage condensation outer shell and the two-stage condensation inner tube, a second inlet and a second outlet are opened on the two-stage condensation outer shell, the second inlet is connected to the cold water tank through a third flow control valve and a second water inlet pipe, and the second outlet is connected to the recovery water tank through a fourth flow control valve and a second return pipe; and the replacement speed of the cooling water in the second cooling channel is controlled by setting the opening of the third flow control valve and the fourth flow control valve, so as to achieve the control of the cooling degree of the air flow by the two-stage air evacuation and diversion assembly; The three-section air evacuation and diversion assembly includes: a three-section condensation outer shell and a three-section condensation inner tube. The three-section condensation inner tube is configured to have a second groove with a downward inclination at the bottom, and the second groove is used to transport condensed water to the end of the three-section condensation inner tube. The upper part of the three-section condensation inner tube is configured to have a second diversion groove with an upward inclination, and the gas is collected into the gas collection tank through the second diversion groove; a third cooling channel is formed between the three-section condensation outer shell and the three-section condensation inner tube, and a third inlet and a third outlet are opened on the three-section condensation outer shell. The third inlet is connected to the cold water tank through the fifth flow control valve and the third water inlet pipe, and the third outlet is connected to the recovery water tank through the sixth flow control valve and the third return pipe; and the replacement speed of the cooling water in the third cooling channel is controlled by setting the opening of the fifth flow control valve and the sixth flow control valve to achieve the control of the cooling degree of the airflow by the three-section air evacuation and diversion assembly; wherein, the inclination of the first groove and the second groove is the same, and the first groove and the second groove are connected end to end.

5. The preparation device of benzoylcorine lactone according to claim 1, characterized in that, The reaction chamber is equipped with a temperature sensor, a pressure sensor, and a pH value detection sensor; and the temperature sensor, the pressure sensor, and the pH value detection sensor are respectively connected to the control device.

6. A method for preparing benzoylcorine lactone, comprising the preparation device for benzoylcorine lactone according to any one of claims 1 to 5, characterized in that: The steps include: 1) 40 L of pyridine is added to the reaction chamber, followed by 4 kg of corrylactone diol. The control device, in accordance with a set first instruction, controls the push cylinder to push the push rod within a first set period, thereby driving the push piston to slowly reciprocate within the reaction chamber, thereby causing the mixture of corrylactone diol and pyridine to surge within the reaction chamber along with the movement of the push piston, thereby achieving mixing. After mixing, the push cylinder is controlled to stop, and 7 kg of triphenylmethane chloride is added to the reaction chamber to obtain a primary reaction mixture. 2) The temperature in the reaction chamber is controlled to maintain at 15-20° C. The control device controls the push cylinder to push the push rod within a second set period according to the set second instruction, thereby driving the push piston to perform slow reciprocating motion in the reaction chamber, thereby driving the primary reaction mixture to surge in the reaction chamber along with the movement of the push piston to complete the reaction and obtain a first mixture; 3) The temperature in the reaction chamber is maintained at 18-22° C., and 5 L of benzoyl chloride is gradually added to the reaction chamber. Simultaneously, the control device controls the push cylinder to push the push rod within a third set period according to the set third instruction, thereby driving the push piston to slowly reciprocate within the reaction chamber, thereby driving the first mixture and benzoyl chloride to surge within the reaction chamber along with the movement of the push piston, thereby completing a complete reaction and obtaining a second mixture; 4) Maintaining the temperature at 18-22°C, 50L of pure water is added to the reaction chamber. At the same time, the control device controls the push cylinder to push the push rod within the set period to drive the push piston to reciprocate in the reaction chamber according to the set periodic control instruction set, and within the set period, the pushing stroke of the push piston in the reaction chamber gradually increases, so that the second mixture in the reaction chamber and the pure water are mixed in a cyclic manner for multiple times during the reciprocating motion of the push piston to form a suspension, and when the pushing stroke gradually increases, the pressure in the reaction chamber is also gradually increased, and the gradual increase in pressure accelerates the formation of the suspension. When the pushing stroke of the push piston gradually reaches the maximum at the end of the execution of the set period, the pressure in the reaction chamber reaches the upper limit value triggered by the pressure control valve. At this time, the pressure control valve is opened to filter the suspension in the reaction chamber to obtain the third mixture, and the control device controls the push cylinder to retreat; 5) 45 L of methanol is added to the reaction chamber, and the heating assembly is controlled to heat the interior of the reaction chamber and maintain the temperature at 150-180° C. The control device controls the push cylinder to push the push rod within a fourth set period according to the set fourth instruction, thereby driving the push piston to reciprocate within the reaction chamber, thereby driving the fourth mixture and methanol to mix within the reaction chamber as the push piston moves. After mixing, the push cylinder is stopped, and the exhaust valve is opened. Heating and reflux are performed for 3-4 hours, and then the exhaust valve and the heating assembly are closed to reduce the temperature within the reaction chamber to room temperature. 6) The control device controls the push cylinder to push the push rod according to the set fifth instruction to drive the push piston to move forward at the maximum stroke in the reaction chamber. The pressure in the reaction chamber reaches the upper limit value triggered by the pressure control valve. At this time, the pressure control valve is opened, and the liquid in the reaction chamber is filtered to obtain solid powder. Then the control device controls the push cylinder to retreat; 48L of acetonitrile is added to the reaction chamber; then 55L of a hydrochloric acid aqueous solution with a concentration of 1-2mol / L is gradually added to the reaction chamber to form a fifth mixture; the control device controls the heating component to heat the reaction chamber to 32-35°C through the control device. At the same time, the control device controls the push cylinder to push the push rod according to the set sixth instruction within a sixth set period to drive the push piston to perform slow reciprocating motion in the reaction chamber, so as to drive the fifth mixture to fully react in the reaction chamber with the movement of the push piston to obtain a sixth mixture. Then the control device controls the push cylinder to stop working; 7) The temperature in the reaction chamber is maintained at 18-22° C., and a saturated sodium bicarbonate aqueous solution is gradually added to the reaction chamber for a neutralization reaction. Simultaneously, the control device controls the push cylinder to push the push rod within a seventh set period according to the set seventh instruction, thereby driving the push piston to perform a slow reciprocating motion within the reaction chamber, thereby driving the sixth mixture and the saturated sodium bicarbonate aqueous solution to be fully mixed and reacted within the reaction chamber with the movement of the push piston until the pH reaches 7, thereby obtaining a seventh reactant. The control device then controls the push cylinder to stop operating. 8) Controlling the heating assembly to heat the interior of the reaction chamber and maintaining the temperature at 100-120° C., while simultaneously opening the exhaust valve to evaporate all acetonitrile in the seventh reactant to obtain a crude product. After the evaporation is complete, the temperature in the reaction chamber is lowered to 60° C. The control device controls the push cylinder to push the push rod according to the set eighth instruction, thereby driving the push piston to move forward within the reaction chamber at its maximum stroke. When the pressure within the reaction chamber reaches the upper limit of the pressure control valve, the pressure control valve is opened, and the liquid in the crude product in the reaction chamber is filtered by pressure. The control device then controls the push cylinder to retract. 9) 25 L of saturated isopropyl ether is added to the reaction chamber. The control device controls the push cylinder to push the push rod within a ninth set period according to the ninth set instruction, thereby driving the push piston to slowly reciprocate within the reaction chamber to completely mix the crude product with the isopropyl ether. After uniform mixing, a primary refined product is formed. The push cylinder is closed, and the heating component is controlled to heat the interior of the reaction chamber and maintain the temperature at 150-180° C. The exhaust valve is opened, and heating and reflux are performed for 2-3 hours. The exhaust valve is then closed. The control device controls the push cylinder to push the push rod within the reaction chamber according to the tenth set instruction, thereby driving the push piston to move forward within the reaction chamber at its maximum stroke. The pressure within the reaction chamber reaches the upper limit of the pressure control valve. At this time, the pressure control valve is opened, and the liquid in the primary refined product within the reaction chamber is subjected to pressure filtration. After the pressure filtration is completed, the control device controls the push cylinder to retract the push piston, and then controls the temperature of the heating component to 40-50° C. The product is dried at 40-50° C. for 1-3 hours to obtain benzoylcorine lactone.

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