A method for purifying corilagin diol

Abstract

The present invention discloses a method for purifying kolidinol diol, comprising the following steps: 1) adding 20 Kg of crude product into the reaction chamber, then gradually adding 22 L of methanol into the reaction chamber, and simultaneously gradually adding 0.6 - 1 L of concentrated hydrochloric acid to form a premixed material; 2) heating the reaction chamber to keep the premixed material in the reaction chamber boiling, and using the method of heating under reflux to completely dissolve the crude product to form a reaction solution; 3) maintaining the temperature in the reaction chamber between -1 and 1 °C, and then adding saturated sodium bicarbonate solution into the reaction chamber to neutralize the reaction solution; 4) controlling the temperature of the reaction chamber to be 100 - 105 °C to complete vacuum concentration. After the concentration is completed, adding chloroform into the reaction chamber, setting the temperature of the reaction chamber to 70 - 85 °C for heating and dissolving. When all is dissolved, controlling the discharge valve at the discharge port provided on the reaction chamber to open, and filtering at a temperature not lower than 60 °C inside the filtering device, and inputting the filtrate into the precipitation device, and cooling and crystallizing in the precipitation device.

Description

Technical Field

[0001] The present invention relates to the technical field of the preparation of corilagin diol, and particularly relates to a purification method of corilagin diol. Background Art

[0002] Currently, the corilagin diol is basically prepared by laboratory methods. The purity of the corilagin diol prepared in the laboratory is not high and it cannot be directly used as a pharmaceutical raw material. It must be purified to improve the purity of the crude product. In the existing publicly available technologies, there is no literature on the purification technology of corilagin diol. Through the research on the synthesis route of corilagin diol, it is found that the main reason for the low purity is that the impurities in the later stage of the reaction cannot be completely removed in the laboratory preparation method. Summary of the Invention

[0003] In order to solve the problems of the prior art, the present invention provides a purification method of corilagin diol, which comprises the following steps:

[0004] 1) Add 20 Kg of the crude product of corilagin diol into the reaction chamber arranged in the reaction device, then gradually add 22 L of methanol into the reaction chamber, and at the same time gradually add 0.6 - 1 L of concentrated hydrochloric acid. While adding, start the control device to open the pushing cylinder, and under the action of the pushing cylinder, gently push the piston in the reaction chamber to drive the crude product in the reaction chamber to be gradually mixed with methanol and concentrated hydrochloric acid until evenly mixed to form a premixed material;

[0005] 2) Control the heating wire to heat the reaction chamber through the control device and heat it to 100 - 105 °C, keep the premixed material in the reaction chamber boiling, then control the control device to open the exhaust valve, and use the method of heating and refluxing to pass the formed vapor through the reflux cooling device to carry out netting, cooling, condensation and recovery to the recovery tank under the premise of controlling the replacement speed of cooling water, and then introduce it from the recovery tank into the interior of the reaction chamber to completely dissolve the crude product to form a reaction solution;

[0006] 3) The control device opens the gas cooler, and the cooled nitrogen gas is input into the cooling space through the intake valve and the intake valve path by the gas cooler. The reaction chamber is cooled through the cooling space. When the temperature in the reaction chamber drops to 0 °C, at the same time open the reflux gas valve on the outlet pipe, and control the opening degrees of the intake valve and the reflux gas valve to be the same to maintain the temperature in the reaction chamber between -1 and 1 °C, and then add saturated sodium bicarbonate solution into the reaction chamber to neutralize the reaction solution and make the pH = 4.2 - 4.6;

[0007] 4) When the pH = 4.2 - 4.6, the control device closes the gas cooler, and at the same time closes the intake valve. Set the opening degree of the reflux gas valve to full opening. After all the nitrogen gas is refluxed to the buffer tank, close the reflux gas valve. Then control the heating wire to heat and set the temperature of the heating wire to 100 - 105 °C. Control the pushing cylinder to retreat at a set speed to form a decompression environment and complete decompression concentration. After the concentration is completed, add chloroform to the reaction chamber, set the temperature of the reaction chamber to 70 - 85 °C for heating and dissolution. When all is dissolved, control the discharge valve at the discharge port set on the reaction chamber to open, and at the same time control the discharge switch valve to open. Transfer all the materials inside the reaction chamber to the filtering device, and complete the filtration inside the filtering device at a temperature not lower than 60 °C. Open the precipitation end switch valve, input the filtrate into the precipitation device, and cool and crystallize in the precipitation device. After the crystals are completely precipitated, use the filtration valve set at the bottom of the precipitation device to statically filter out the liquid. After that, set the temperature of the precipitation device to 40 °C and dry for 2 - 4 hours to obtain purified corilagin diol.

[0008] In the above, the set flow ratio of methanol to concentrated hydrochloric acid added is 20 - 25:1.

[0009] In the above, the control device controls the pushing cylinder to drive the pushing piston to move forward through the push rod within a set first range. Under the action of the pushing cylinder, the pushing piston is gently reciprocally pushed within a set first range in the reaction chamber, so that the methanol and concentrated hydrochloric acid inside the reaction chamber form a back-and-forth swimming motion to mix with the crude product.

[0010] In the above, the gas cooler is used to cool nitrogen gas to -3 °C. The gas cooler inputs the cooled nitrogen gas into the cooling space through the intake valve and the intake valve path, and cools the reaction chamber through the cooling space. When the temperature inside the reaction chamber drops to 0 °C, simultaneously open the reflux gas valve on the outlet gas pipeline, and control the opening degrees of the intake valve and the reflux gas valve to be the same to maintain the temperature inside the reaction chamber at 0 °C.

[0011] In the above, a control device is also provided inside the reaction device;

[0012] A storage module is provided inside the control device. The storage module has a plurality of storage units, and each storage unit is used to store the corresponding set control instructions;

[0013] The control device loads the control instructions in the storage unit. Based on the control instructions, the control device controls the pushing cylinder to drive the pushing piston to move forward through the push rod within a set first range. Under the action of the pushing cylinder, the pushing piston is gently reciprocally pushed within a set first range in the reaction chamber, so that the methanol and concentrated hydrochloric acid inside the reaction chamber form a back-and-forth swimming motion to mix with the crude product;

[0014] Alternatively, based on the control instruction, the control device controls the exhaust valve to open, and uses the method of heating and refluxing to heat the material in the reaction chamber and boil it. The formed vapor passes through the reflux cooling device and is subjected to wire hanging, cooling, condensation and recovery into the recovery tank under the premise of controlling the replacement speed of the cooling water, and then is introduced from the recovery tank into the reaction chamber to completely dissolve the crude product;

[0015] Alternatively, based on the control instruction, the control device controls the heating wire and the pushing cylinder to act simultaneously to complete the concentration by means of reduced pressure concentration.

[0016] In the above, a temperature sensor, a pressure sensor and a pH value detection sensor are arranged in the reaction chamber.

[0017] This application designs a method for industrial purification of colilactone diol. The main idea is to completely dissolve the crude product, remove the impurities in the crude product, and then perform crystallization, and achieve the method of purifying the purity of colilactone diol through re-crystallization. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] 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 the description of the embodiments. 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 be obtained based on these drawings.

[0019] Figure 1 is a flowchart of the method provided by the present invention;

[0020] Figure 2 is a schematic structural diagram of the device provided by the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0021] 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.

[0022] Example 1, referring to Figure 2 , the present invention provides a purification device for colilactone diol, including: a reaction device, which has a reaction housing 4 and a reaction assembly 42 arranged inside the reaction housing 4;

[0023] The reaction assembly 42 includes an inner cavity and an insulating housing, and heating wires are arranged in a uniformly arranged manner between the inner cavity and the insulating housing; and the heating wires are arranged along the outer wall of the inner cavity.

[0024] The interior of the inner chamber forms a reaction chamber 41. A pushing piston 3 is arranged in the reaction chamber 41 and on the left side of the reaction chamber 41. A push rod 2 is arranged on the left side of the pushing piston 3, and the push rod 2 is fixed on a pushing cylinder 1;

[0025] A joint assembly 7 is arranged on the reaction shell. A plurality of switching valves are integrated in the joint assembly 7. The bottom of each switching valve is connected to the inside of the reaction chamber 41 through a feed pipe 70, and the upper part of the switching valve is connected to a feed tank 72 through a feed pipeline and a metering valve 71 on the feed pipeline;

[0026] An exhaust valve 60 is embedded at the inner end of the reaction chamber 41 and in the upper part of the inner chamber. The exhaust valve 60 passes through the cooling space 40 and the reaction shell and is connected to one end of an exhaust valve joint 61 arranged outside the reaction shell. The other end of the exhaust valve joint 61 is connected to an exhaust pipe 62. The exhaust pipe 62 is connected to a reflux cooling device. The reflux cooling device is connected to a liquid collection tank 74 through a liquid collection control valve 66 and a liquid collection pipeline, and a liquid collection switch control valve 69 is arranged on the liquid collection pipeline. The liquid collection tank 74 is connected to the joint assembly 7 through a reflux pipeline and is connected to one of the switching valves; and a reflux liquid control valve 73 is arranged on the reflux pipeline;

[0027] A discharge port 11 is embedded in the reaction chamber 41 and in the lower part of the inner chamber. A discharge valve 12 is arranged at the discharge port 11. The discharge valve 12 is connected to a filtering device 14 through a discharge pipeline, and the filtering device 14 is connected to a precipitation device 16.

[0028] Further, a cooling space 40 is formed between the reaction shell and the reaction assembly 42. An air inlet pipe 81 is arranged at the upper left side of the reaction shell. The air inlet pipe 81 is communicated with the cooling space 40, and the air inlet pipe 81 is connected to a gas cooler 8 through an air inlet pipeline and an air inlet valve switching valve 80 on the air inlet pipeline;

[0029] An air outlet pipe 91 is arranged at the lower left side of the reaction shell. The air outlet pipe 91 is communicated with the cooling space 40, and the air outlet pipe 91 is connected to a buffer tank 9 through an air outlet pipe 91 road and an air outlet valve 90 on the air outlet pipe 91 road. The buffer tank 9 is connected to the gas cooler 8 through a circulation pipeline and a circulation control valve 10 arranged on the circulation pipeline.

[0030] Further, the gas cooler 8 is used to cool nitrogen to -3°C. The gas cooler 8 inputs the cooled nitrogen into the cooling space 40 through the air inlet pipe 81 and the air inlet pipe 81 road, and cools the reaction chamber 41 through the cooling space 40. When the temperature in the reaction chamber 41 drops to 0°C, the reflux gas valve on the air outlet pipe 91 road is opened simultaneously, and the opening degrees of the air inlet pipe 81 and the reflux gas valve are controlled to be the same to maintain the temperature in the reaction chamber 41 at 0°C.

[0031] Furthermore, a control device is also provided inside the reaction device;

[0032] A storage module is provided inside the control device. The storage module has a plurality of storage units, and each storage unit is used to store corresponding set control instructions;

[0033] The control device loads the control instructions in the storage unit. Based on the control instructions, the control device controls the pushing cylinder 1 to drive the pushing piston 3 forward through the push rod 2, and the forward movement stroke is within a set first range. Under the action of the pushing cylinder 1, the pushing piston 3 is gently reciprocally pushed within a set first range in the reaction chamber 41, so that methanol and concentrated hydrochloric acid inside the reaction chamber 41 form a back-and-forth movement to mix with the crude product;

[0034] Or, based on the control instructions, the control device controls the exhaust valve 60 to open, and uses the method of heating and refluxing to heat the material in the reaction chamber 41. When the formed vapor during boiling passes through the reflux cooling device, under the premise of controlling the replacement speed of cooling water, it is netted, cooled, condensed and recovered into the recovery tank, and then introduced from the recovery tank into the inside of the reaction chamber 41, so that the crude product is completely dissolved;

[0035] Or, based on the control instructions, the control device controls the heating wire and the pushing cylinder to act simultaneously to complete the concentration by means of reduced pressure concentration.

[0036] Furthermore, a temperature sensor, a pressure sensor and a pH value detection sensor are provided inside the reaction chamber 41. Among them, the temperature sensor is used to measure the temperature data inside the reaction chamber 41 in real time and transmit the temperature data to the control device. The pressure sensor is used to collect the pressure signal inside the reaction chamber 41 in real time and feedback the collected pressure signal to the control device. The control device judges whether the pressure inside the reaction chamber 41 is within the set range based on the pressure signal. The pH value detection sensor is used to detect the pH value of the reaction material inside the reaction chamber 41 and transmit the detected pH value to the control device.

[0037] Furthermore, the filtering device 14 is used to filter the material at a temperature not lower than 60 °C. After the filtering is completed, the precipitation end switching valve is opened, and the filtrate is input into the precipitation device 16. In the precipitation device 16, cooling crystallization is carried out. After the crystals are completely precipitated, the filtering valve provided at the bottom of the precipitation device 16 is used to statically filter the liquid. After that, the temperature of the precipitation device 16 is set to 40 °C and dried for 2 - 4 hours to obtain purified corilagin diol.

[0038] In the above, the joint assembly 7 is integrated with six switch valves, one of which is used to dock with the crude product feeding tank for adding the crude product into the reaction chamber 41; one of the switch valves is used to dock with the methanol feeding tank for adding methanol into the reaction chamber 41; one of the switch valves is used to dock with the concentrated hydrochloric acid feeding tank for adding concentrated hydrochloric acid into the reaction chamber 41; one of the switch valves is used to dock with the saturated sodium bicarbonate solution feeding tank for adding saturated sodium bicarbonate solution into the reaction chamber 41; one of the switch valves is used to dock with the chloroform feeding tank for adding chloroform into the reaction chamber 41; and one of the switch valves is used to dock with the liquid collecting tank for reflux of the liquid during heating reflux.

[0039] In the above, the reflux cooling device includes a cooling shell and a collecting pipe, a cooling trough 64 is formed between the cooling shell and the collecting pipe, a plurality of staggered filter screens are arranged inside the collecting pipe, and the filter holes on adjacent filter screens are also staggered, a cold air inlet is opened at the upper part of the cooling shell, and a cooling outlet is arranged at the lower part of the cooling shell, wherein the cold air inlet is connected to the cold supply tank 68 through a cold air pipeline and a cold air control valve 67 arranged on the cold air pipeline, and the cold supply tank 68 is connected to the gas cooler 8, the cooling outlet is connected to the reflux tank 63 through the reflux cooling pipeline and the reflux control valve 65 on the reflux cooling pipeline, the reflux tank 63 is connected to the gas cooler 8, and a switch valve is arranged on the connecting pipeline between the reflux tank 63, the cold supply tank 68 and the gas cooler 8. When reflux cooling is performed, the control device controls the switch valves provided on the connecting pipelines between the reflux tank 63, the cold supply tank 68 and the gas cooler 8 to be closed, and the cold air control valve 67 and the reflux control valve 65 are opened at the same time, and the opening of the cold air control valve 67 is set to 20% of the full opening, and the reflux control valve 65 is set to 5% of the full opening, so as to provide cooled nitrogen to the cooling tank 64. The cooled nitrogen quickly cools the collecting pipe, so that the temperature of the steam flowing through the inside is quickly reduced, and condenses on the filter screen to achieve hanging and condensation. In order to facilitate the downward flow of the condensed liquid, the reflux cooling device in the present application is arranged to be tilted downward, preferably, tilted downward by 10°. When the gas in the cooling tank 64 reaches a certain amount (which can be controlled by setting the cold air supply time), the openings of the cold air control valve 67 and the reflux control valve 65 are both set to 5% of the full opening to keep the temperature of the cooling tank 64 constant. At the same time, after the cooling tank 68 has provided cooling for a set time, the switch valves provided on the connecting pipelines between the reflux tank 63, the cooling tank 68 and the gas cooler 8 are opened respectively to realize the cooling cycle.

[0040] Example 2

[0041] Reference Figure 2 The present application also provides a method for purifying corilactone diol, comprising the following steps:

[0042] 1) Add 20 Kg of the crude product of corilagin diol into the reaction chamber 41 set in the reaction device, then gradually add 22 L of methanol into the reaction chamber 41, and at the same time gradually add 0.6 - 1 L of concentrated hydrochloric acid. While adding, activate the control device to turn on the feeding cylinder 1. Under the action of the feeding cylinder 1, gently push the piston in the reaction chamber 41 to drive the crude product in the reaction chamber 41 to be gradually mixed with methanol and concentrated hydrochloric acid until evenly mixed to form a premixed material;

[0043] 2) Control the heating wire to heat the reaction chamber 41 through the control device and heat it to 100 - 105 °C, keep the premixed material in the reaction chamber 41 boiling, then control the control device to open the exhaust valve 60, and use the method of heating reflux to make the formed vapor be netted, cooled, condensed and recycled to the recovery tank through the reflux cooling device under the premise of controlling the replacement speed of cooling water, and then introduced from the recovery tank into the interior of the reaction chamber 41 to completely dissolve the crude product to form a reaction solution;

[0044] 3) The control device turns on the gas cooler 8, and the cooled nitrogen is input into the cooling space 40 through the intake pipe 81 and the intake pipe 81 path by the gas cooler 8, and the reaction chamber 41 is cooled through the cooling space 40. When the temperature in the reaction chamber 41 drops to 0 °C, simultaneously open the reflux gas valve on the outlet pipe 91 path, and control the opening degrees of the intake pipe 81 and the reflux gas valve to be the same to maintain the temperature in the reaction chamber 41 between -1 and 1 °C. Then add saturated sodium bicarbonate solution into the reaction chamber 41 to neutralize the reaction solution and make the pH = 4.2 - 4.6;

[0045] 4) When the pH = 4.2 - 4.6, the control device closes the gas cooler 8, simultaneously closes the intake pipe 81, sets the opening degree of the reflux gas valve to the full opening degree, after all the nitrogen is refluxed to the buffer tank, closes the reflux gas valve, then controls the heating wire to heat and sets the temperature of the heating wire to 100 - 105 °C, and controls the feeding cylinder 1 to retreat at a set speed to form a reduced-pressure environment to complete reduced-pressure concentration. After concentration is completed, add chloroform into the reaction chamber 41, set the temperature of the reaction chamber 41 to 70 - 85 °C for heating and dissolution. When all is dissolved, open the discharge valve 12 at the discharge port 11 set on the reaction chamber 41, and at the same time control the discharge switch valve 13 to open, transfer all the materials inside the reaction chamber 41 to the filtering device 14, complete filtration in the filtering device 14 at not less than 60 °C, open the precipitation end switch valve, input the filtrate into the precipitation device 16, cool and crystallize in the precipitation device 16. After the crystals are completely precipitated, use the filtering valve set at the bottom of the precipitation device 16 to statically filter and remove the liquid, and the filtered liquid enters the liquid tank 17 set at the bottom of the precipitation device 16; After that, set the temperature of the precipitation device 16 to 40 °C and dry for 2 - 4 hours to obtain purified corilagin diol.

[0046] In the above, when filtering, the temperature is maintained not lower than 60 °C. Otherwise, when the temperature is too low, crystallization will occur. Therefore, this step is regarded as the hot filtration stage.

[0047] In the above,

[0048] In the above, the set flow ratio of methanol to concentrated hydrochloric acid added is 20 - 25:1.

[0049] In the above, the control device controls the pushing cylinder 1 to drive the pushing piston 3 forward through the push rod 2, and the forward movement stroke is within a set first range. Under the action of the pushing cylinder 1, the pushing piston 3 is gently reciprocated within the set first range in the reaction chamber 41, so that the methanol and concentrated hydrochloric acid inside the reaction chamber 41 form a back-and-forth swimming motion to mix with the crude product.

[0050] In the above, the gas cooler 8 is used to cool nitrogen to -3 °C. The gas cooler 8 inputs the cooled nitrogen into the cooling space 40 through the inlet pipe 81 and the inlet pipe 81 path, and cools the reaction chamber 41 through the cooling space 40. When the temperature in the reaction chamber 41 drops to 0 °C, the reflux gas valve on the outlet pipe 91 path is opened simultaneously, and the opening degrees of the inlet pipe 81 and the reflux gas valve are controlled to be the same to maintain the temperature in the reaction chamber 41 at 0 °C.

[0051] In the above, a control device is also provided in the reaction device;

[0052] A storage module is provided in the control device. The storage module has a plurality of storage units, and each storage unit is used to store the corresponding set control instructions;

[0053] The control device loads the control instructions in the storage unit. Based on the control instructions, the control device controls the pushing cylinder 1 to drive the pushing piston 3 forward through the push rod 2, and the forward movement stroke is within a set first range. Under the action of the pushing cylinder 1, the pushing piston 3 is gently reciprocated within the set first range in the reaction chamber 41, so that the methanol and concentrated hydrochloric acid inside the reaction chamber 41 form a back-and-forth swimming motion to mix with the crude product;

[0054] Or, based on the control instructions, the control device controls the exhaust valve 60 to open, and the vapor formed when heating and boiling the materials in the reaction chamber 41 by the method of heating reflux is passed through the reflux cooling device and is netted, cooled, condensed and recovered into the recovery tank under the premise of controlling the replacement speed of cooling water, and then is introduced into the reaction chamber 41 from the recovery tank to completely dissolve the crude product;

[0055] Or, based on the control instructions, the control device controls the heating wire and the pushing cylinder to act simultaneously to complete the concentration by the method of reduced pressure concentration.

[0056] In the above, a temperature sensor, a pressure sensor and a pH value detection sensor are arranged in the reaction chamber 41.

[0057] The present application designs a method for industrially purifying colilactone diol. The main idea is to completely dissolve the crude product, remove the impurities in the crude product, and then perform crystallization, and achieve the method for purifying the purity of colilactone diol by performing crystallization again.

[0058] 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 principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A method for purifying corilagin diol, characterized in that, It includes the following steps: 1) Add 20 Kg of the crude product of corilagin diol into the reaction chamber set in the reaction device, then gradually add 22 L of methanol into the reaction chamber, and at the same time gradually add 0.6 - 1 L of concentrated hydrochloric acid. While adding, activate the control device to start the feeding cylinder, and under the action of the feeding cylinder, gently push the piston in the reaction chamber to drive the crude product in the reaction chamber to be gradually mixed with methanol and concentrated hydrochloric acid until evenly mixed to form a premixed material; 2) Control the heating wire to heat the reaction chamber through the control device, and heat it to 100 - 105 °C to keep the premixed material in the reaction chamber boiling. Then, the control device controls the exhaust valve to open, and uses the method of heating reflux to pass the formed vapor through the reflux cooling device to carry out netting, cooling, condensation and recovery into the recovery tank under the premise of controlling the replacement speed of cooling water, and then introduce it from the recovery tank into the interior of the reaction chamber to completely dissolve the crude product to form a reaction solution; 3) The control device opens the gas cooler, and the cooled nitrogen is input into the cooling space through the intake valve and the intake valve path by the gas cooler. The reaction chamber is cooled through the cooling space. When the temperature in the reaction chamber drops to 0 °C, at the same time open the reflux gas valve on the outlet pipeline, and control the opening degrees of the intake valve and the reflux gas valve to be the same to maintain the temperature in the reaction chamber between -1 and 1 °C. Then add saturated sodium bicarbonate solution into the reaction chamber to neutralize the reaction solution and make the pH = 4.2 - 4.6; 4) When the pH = 4.2 - 4.6, the control device closes the gas cooler, and at the same time closes the intake valve. Set the opening degree of the reflux gas valve to the full opening degree. After all the nitrogen is refluxed to the buffer tank, close the reflux gas valve. Then control the heating wire to heat and set the temperature of the heating wire to 100 - 105 °C, and control the feeding cylinder to retreat at a set speed to form a reduced pressure environment to complete reduced pressure concentration. After concentration, add chloroform into the reaction chamber, set the temperature of the reaction chamber to 70 - 85 °C for heating and dissolving. When all is dissolved, open the discharge valve at the discharge port set on the reaction chamber, and at the same time control the discharge switch valve to open, transfer all the materials inside the reaction chamber to the filtering device, complete the filtration in the filtering device at a temperature not lower than 60 °C, open the precipitation end switch valve, input the filtrate into the precipitation device, cool and crystallize in the precipitation device. After the crystals are completely precipitated, use the filtration valve set at the bottom of the precipitation device to statically filter out the liquid. After that, set the temperature of the precipitation device to 40 °C and dry for 2 - 4 hours to obtain the purified corilagin diol; In step 1), the control device controls the feeding cylinder to drive the feeding piston to move forward through the push rod within a set first range, and under the action of the feeding cylinder, gently reciprocate the feeding piston within the set first range in the reaction chamber so that the methanol and concentrated hydrochloric acid inside the reaction chamber form a back-and-forth movement to be mixed with the crude product; A control device is also set in the reaction device; A storage module is set in the control device, and the storage module has a plurality of storage units, and each storage unit is used to store the corresponding set control instructions; The control device loads the control instructions in the storage unit. Based on the control instructions, the control device controls the pusher cylinder to drive the pusher piston forward through the push rod, and the forward movement stroke is within a set first range. Under the action of the pusher cylinder, the pusher piston is gently reciprocated within the set first range in the reaction chamber, so that methanol and concentrated hydrochloric acid in the reaction chamber form a back-and-forth movement to mix with the crude product. Alternatively, based on the control instructions, the control device controls the exhaust valve to open, and uses the method of heating and refluxing to heat the materials in the reaction chamber. When the formed vapor during boiling passes through the reflux cooling device, under the premise of controlling the replacement speed of cooling water, it is netted, cooled, condensed and recovered into the recovery tank, and then introduced into the reaction chamber from the recovery tank, so that the crude product is completely dissolved. Alternatively, based on the control instructions, the control device controls the heating wire and the pushing cylinder to act simultaneously to complete the concentration by means of vacuum concentration.

2. The purification method of corilagin diol according to claim 1, characterized in that, In step 1), the set flow ratio of methanol to concentrated hydrochloric acid added is 20 - 25:

1.

3. The purification method of koliolide diol according to claim 1, characterized in that, The gas cooler is used to cool nitrogen to -3°C. The gas cooler inputs the cooled nitrogen into the cooling space through the intake valve and the intake valve path, and cools the reaction chamber through the cooling space. When the temperature in the reaction chamber drops to 0°C, the reflux gas valve on the outlet pipe is opened simultaneously, and the opening degrees of the intake valve and the reflux gas valve are controlled to be the same to maintain the temperature in the reaction chamber at 0°C.

4. The purification method of corilagin diol according to claim 1, characterized in that, A temperature sensor, a pressure sensor and a pH value detection sensor are arranged in the reaction chamber.

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