Crystallization and purification equipment for producing o-chlorobenzyl cyanide and operation method of crystallization and purification equipment

Abstract

The invention discloses crystallization and purification equipment for production of o-chlorobenzyl cyanide and an operation method of the crystallization and purification equipment, and relates to the technical field of production of o-chlorobenzyl cyanide. The device comprises a supporting assembly, an I-shaped frame, a vertical plate fixed to the middle position of the upper end of the I-shaped frame, an annular heater located on one side edge of the vertical plate and fixedly connected with the upper end face of the I-shaped frame, a crystallization purification assembly, a dissolving assembly and a proportioning assembly. The mounting ring is fixed to the upper end face of the dissolving tank, the proportioning column and the graduated drum are located on the periphery of the dissolving tank and arranged on the upper end face of the mounting ring, an electronic scale is arranged in a conical groove, an operation barrel is arranged on the outer wall of the proportioning column, and an electromagnet is fixed in the operation barrel located below a pushing rod. The metering proportion is controlled through the proportioning assembly, it is guaranteed that o-chlorobenzyl cyanide is fully dissolved in the diethyl ether solution, meanwhile, through siphon work between the dissolving tank and the crystallization purification tank, extraction of the solution cannot be automatically controlled, and comprehensive extraction of the solution is guaranteed.

Description

Technical Field

[0001] The invention belongs to the technical field of o-chlorobenzyl cyanide production, and particularly relates to a crystallization purification device for o-chlorobenzyl cyanide production and an operation method thereof. Background Art

[0002] Used in the production of o-chlorobenzyl cyanide, o-chlorobenzyl alcohol, synthetic dyes, pharmaceuticals, etc. o-chlorobenzyl cyanide is an intermediate of the herbicide isothiocarbamide and also an intermediate of the pharmaceutical enzyme inhibitor. Organic synthetic raw materials, used in the pharmaceutical industry to make stimulant enzyme inhibitors, etc. During the production of o-chlorobenzyl cyanide, it is necessary to wear appropriate protective equipment such as gloves and goggles when using it. It should be stored in a dry and cool place, away from fire and flammable substances. In the process of waste treatment, relevant environmental protection laws and regulations must be observed to avoid pollution to the environment. It can be seen that most of the equipment for producing o-chlorobenzyl cyanide uses automated equipment to reduce the operation of workers.

[0003] Therefore, in order to be able to crystallize and purify o-chlorobenzyl cyanide, o-chlorobenzyl cyanide and the solution are fully dissolved. During the dissolution process, the insoluble substances in o-chlorobenzyl cyanide will remain in the equipment. When the existing equipment separates the solid and liquid therein, the solution is poured into the filter bottle from top to bottom, wherein the solution permeates from the filter paper, and the solid-liquid structure is blocked. When the solid-liquid filtration is performed in this way, it is mostly necessary to control the rotation of the equipment to pour out the solution. However, the excessive operation of the equipment and the small particles of o-chlorobenzyl cyanide will produce even smaller impurities after the dissolution, and the solution When flowing, impurities will be driven out, and there will be a problem that it is impossible to filter comprehensively, and it is impossible to ensure that the solution is poured out accurately. At the same time, when dissolving o-chlorobenzyl cyanide, most of the o-chlorobenzyl cyanide and the solution are poured in order and stirred. In the crystallization and purification process, it is necessary to ensure that o-chlorobenzyl cyanide is fully dissolved. The existing method is to gradually add o-chlorobenzyl cyanide or the solution during the stirring process to achieve the full dissolution of o-chlorobenzyl cyanide. Since it does not have the function of allocating o-chlorobenzyl cyanide and the solution at the first time, this method increases the crystallization and purification process and time, and reduces the efficiency. To this end, we provide a crystallization and purification device for the production of o-chlorobenzyl cyanide and its operation method to solve the above problems. Summary of the invention

[0004] The object of the present invention is to provide a crystallization purification device for the production of o-chlorobenzyl cyanide and an operation method thereof, wherein the metering ratio is controlled by a proportioning component to ensure that o-chlorobenzyl cyanide is fully dissolved in an ether solution, and at the same time, through the siphon work between a dissolving tank and a crystallization purification tank, the extraction of the solution cannot be automatically controlled, thereby ensuring that the extraction of the solution is comprehensive.

[0005] In order to solve the above technical problems, the present invention is achieved through the following technical solutions: The invention provides a crystallization purification device for producing o-chlorobenzyl cyanide, comprising a supporting assembly, comprising a work-shaped frame, a vertical plate fixed at the middle position of the upper end of the work-shaped frame, and an annular heater located on one side of the vertical plate and fixedly connected to the upper end surface of the work-shaped frame; a crystallization purification assembly, comprising a crystallization purification tank connected to the upper end surface of the annular heater, a condensation box and a water tank located on the other side of the vertical plate and fixed to the upper end surface of the work-shaped frame, a vacuum pump is arranged in the middle cavity of the work-shaped frame on the same side as the condensation box, a dissolving assembly, comprising a dissolving tank located on the same side as the condensation box, a filter tube is fixed on the side wall of the vertical plate above the dissolving tank, and one end of the filter tube is connected to the dissolving tank. A siphon short tube connected to the inner bottom, the other end of the filter tube is connected to a siphon long tube, a proportioning assembly, including a mounting ring fixed on the side wall of the vertical plate and slidably connected to the upper surface of the dissolving tank, and a proportioning column and a scale cylinder located on the periphery of the dissolving tank and arranged on the upper end surface of the mounting ring, a tilting tube with a valve is fixed to the lower end of the scale cylinder, a proportioning port is provided on the upper end surface of the proportioning column, a conical groove is provided inside the proportioning column below the proportioning port, an electronic scale is arranged inside the conical groove, an operating cylinder is provided on the outer wall of the proportioning column, a pushing rod for adjusting the inclination angle of the electronic scale is provided inside the operating cylinder, and an electromagnet is fixed inside the operating cylinder below the pushing rod.

[0006] The present invention is further configured such that a gear ring is fixed to the lower part of the surface wall of the dissolving tank, a motor is fixed to the side wall of the vertical plate below the filter tube, and a gear plate meshing with the gear ring is fixed to the rotating shaft end of the motor.

[0007] The present invention is further configured such that a condenser pipe connected to the interior of the crystallization purification tank and the condensation tank is provided between the crystallization purification tank and the condensation tank, the water pump inside the water tank is connected to the interior of the crystallization purification tank through a pipeline, and the port of the vacuum pump is connected to the interior of the crystallization purification tank through a fixed air pipe.

[0008] The present invention is further configured such that a sealing plate is provided on the upper end surface of the crystallization purification tank, the bottom end of the long siphon tube passes through the middle of the sealing plate, frames for supporting the crystallization purification tank and the dissolution tank are fixed on both sides of the vertical plate, and the two frames are arranged in upper and lower positions, the upper end surface of the crystallization purification tank is lower than the bottom of the dissolution tank, and a plug-in tube connected to the bottom of the crystallization purification tank is fixed at the bottom of the short siphon tube, and a plurality of leakage holes distributed in a circular array are opened through the surface side of the plug-in tube.

[0009] The present invention is further configured such that a discharge pipe with a solenoid valve is fixed to the bottom of the crystallization purification tank, and the discharge pipe passes through the hollow position of the annular heater and the upper end surface position of the I-shaped frame in sequence.

[0010] The present invention is further configured such that the proportioning port and the tapered groove are connected via a through hole provided inside the proportioning column, an electrically controlled ball valve is fixed at the position of the through hole, a special-shaped port is provided on the side wall of the proportioning column on the same side as the operating cylinder, a rotating column used in conjunction with the special-shaped port is fixed at the end of the electronic scale, a linkage plate passing through the position of the special-shaped port is fixed on the side wall of the rotating column, and the linkage plate abuts against the upper end face of the operating cylinder, a sliding tube connected to the inside of the tapered groove is fixed to the lower end face of the proportioning column, and a mounting frame bolted to the mounting ring is fixed to the lower end face of the proportioning column.

[0011] The present invention is further configured such that the inner side wall of the matching column located inside the special-shaped mouth is provided with two axial holes arranged symmetrically in front and back, an axial rod rotating in the position inside the axial hole is fixed on the side wall of the rotating column, and an arc spring abutting against the side wall of the matching column is fixed on the upper end surface of the linkage plate.

[0012] The present invention is further configured such that a telescopic hole with a smaller diameter than the inner diameter of the operating cylinder is opened on the upper end surface of the operating cylinder, the upper end surface of the pushing rod slides in the telescopic hole, a circular plate sliding in the inner position of the operating cylinder is fixed on the lower end surface of the pushing rod, and a metal rod adsorbed by the electromagnet is fixed on the lower end surface of the circular plate.

[0013] The present invention is further configured such that a positioning ring is fixed in the middle position inside the operating cylinder, a pushing spring abutting against the end face of the positioning ring is fixed at the lower end of the circular plate, the surface side of the operating cylinder is connected to the proportioning column bolt through a fixed locking plate, and a remote control switch electrically connected to the electromagnet and the electronic scale is fixed to the surface wall of the operating cylinder.

[0014] The present invention also provides an operating method of a crystallization purification device for producing o-chlorobenzyl cyanide, which is implemented by the following steps: S1: First, pour the ether solvent into the graduated cylinder, and pour the o-chlorobenzyl cyanide powder into the proportioning port, and set the weighing value on the electronic scale. At this time, according to the capacity of the ether solvent in the graduated cylinder, control the electric control ball valve to open, so that the o-chlorobenzyl cyanide powder falls onto the electronic scale; S2: When the o-chlorobenzyl cyanide powder on the electronic scale reaches the set weighing value, the electromagnet electrically controlled ball valve is closed, the electromagnet is powered off, and the pushing rod moves upward, pushing the linkage plate to rotate upward, thereby the linkage plate drives the electronic scale to rotate downward, so that the o-chlorobenzyl cyanide powder on the electronic scale slides into the dissolving tank; S3: Pour the ether solvent in the graduated cylinder into the dissolving tank at the same time, so that the ether solvent and the o-chlorocyanobenzyl powder are fully dissolved; S4: At this time, the water in the water tank is pumped into the crystallization purification tank, so that the water level in the crystallization purification tank is higher than the height of the plug-in pipe, and the vacuum tank is controlled to vacuum the interior of the crystallization purification tank, thereby siphoning occurs between the crystallization purification tank and the dissolution tank, so that all the dissolved liquid enters the crystallization purification tank; S5: reducing the pressure in the crystallization purification tank by a vacuum pump to reduce the boiling point of the liquid therein, and controlling the operation of the ring heater to perform evaporation treatment on the inside of the crystallization purification tank to recrystallize the dissolved o-chlorobenzyl cyanide; S6: The evaporated water and ether solution are cooled and recovered from the inside of the condenser, and the crystallized o-chlorobenzyl cyanide is discharged through the discharge pipe.

[0015] The present invention has the following beneficial effects: The weight of o-chlorobenzyl cyanide is accurately measured by an electronic scale to match the o-chlorobenzyl cyanide with the ether solvent, and the electromagnet is controlled to be powered off, so that the pushing rod is reset and moves upward, and the electronic scale is pushed to rotate downward, so that the o-chlorobenzyl cyanide on the electronic scale will slide directly into the dissolution tank, thereby achieving accurate material feeding and ensuring that the o-chlorobenzyl cyanide and the ether solution can be fully dissolved.

[0016] The water tank is controlled to pump pure water into the crystallization purification tank so that the lower port in the siphon short tube is in the water. At this time, the interior of the crystallization purification tank is evacuated to reduce the pressure inside the crystallization purification tank. At the same time, the crystallization purification tank is located below the dissolution tank, and a siphon reaction occurs between the dissolution tank and the crystallization purification tank. The solution inside the dissolution tank will be pumped into the crystallization purification tank. Since the filter tube is located between the long siphon tube and the short siphon tube, the filter tube is used to filter the solution flowing between the long siphon tube and the short siphon tube to avoid the flow of impurities, thereby realizing automatic control of the extraction of the solution and ensuring comprehensive extraction.

[0017] Of course, any product implementing the present invention does not necessarily need to achieve all of the above advantages at the same time. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings required for describing the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without paying creative work.

[0019] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0020] Figure 2 It is a schematic diagram of the structure of the dissolving component in the present invention.

[0021] Figure 3 It is a structural schematic diagram of the proportioning component in the present invention.

[0022] Figure 4 It is a structural combination diagram of the proportioning column, operating cylinder, electronic scale and installation device in the present invention.

[0023] Figure 5 This is a structural combination diagram of the operating cylinder, electromagnet and metal rod in the present invention.

[0024] Figure 6 It is a structural schematic diagram of the electronic scale in the present invention.

[0025] Figure 7 It is a schematic diagram of the structure of the support assembly in the present invention.

[0026] Figure 8 It is a structural cross-sectional view of the proportioning column in the present invention.

[0027] Fig. 9 It is a structural diagram of the dissolving tank in the present invention.

[0028] Fig.10 It is a structural diagram of the operating cylinder in the present invention.

[0029] Fig.11 It is a structural combination diagram of the filter tube, crystallization purification tank and dissolution tank in the present invention.

[0030] Fig.12 It is a structural combination diagram of the filter tube in the present invention.

[0031] In the accompanying drawings, the components represented by the reference numerals are listed as follows: 100-support assembly, 101-work frame, 102-vertical plate, 103-filter tube, 103a-siphon long tube, 103b-siphon short tube, 103b-1-plug tube, 103b-2-leak hole, 104-motor, 104a-tooth plate, 105-ring heater, 106-support frame, 200-crystallization purification assembly, 201-crystallization purification tank, 201a-discharge pipe, 201b-sealing plate, 202-vacuum pump, 203-condensation box, 204-water tank, 205-condensation tube, 300-dissolution assembly, 301-dissolution tank, 302-tooth ring, 400-proportioning assembly, 401-proportioning column, 401a-proportioning Ratio port, 401a-1-through hole, 401b-electrically controlled ball valve, 401c-conical groove, 401d-sliding tube, 401e-special-shaped port, 401f-axial hole, 402-scale cylinder, 402a-tilt tube, 403-mounting ring, 404-operating cylinder, 404a-locking plate, 404b-positioning ring, 404c-telescopic hole, 405-electronic scale, 405a-rotating column, 405a-1-axial rod, 405b-linkage plate, 405c-arc spring, 406-mounting frame, 407-electromagnet, 408-metal rod, 408a-round plate, 408b-pushing rod, 408c-pushing spring, 409-remote control switch. DETAILED DESCRIPTION

[0032] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Example 1

[0033] See also Figure 1 , Figure 2 and Figure 3 , which is the first embodiment of the present invention, provides a crystallization and purification device for the production of o-chlorobenzyl cyanide. The metering ratio is controlled by the proportioning component 400 to ensure that o-chlorobenzyl cyanide is fully dissolved in the ether solution. At the same time, through the siphon work between the dissolution tank 301 and the crystallization and purification tank 201, the extraction of the solution cannot be automatically controlled, ensuring that the extraction of the solution is comprehensive.

[0034] Specifically, the support assembly 100 includes a work frame 101, a vertical plate 102 fixed to the middle of the upper end of the work frame 101, and a ring heater 105 located on one side of the vertical plate 102 and fixedly connected to the upper end surface of the work frame 101; the crystallization purification assembly 200 includes a crystallization purification tank 201 connected to the upper end surface of the ring heater 105, a condensation box 203 and a water tank 204 located on the other side of the vertical plate 102 and fixed to the upper end surface of the work frame 101, and a dissolution assembly 300. , including a dissolving tank 301 on the same side as the condensation tank 203, a proportioning assembly 400, including a mounting ring 403 fixed to the side wall of the vertical plate 102 and slidably connected to the upper surface of the dissolving tank 301, and a proportioning column 401 and a scale cylinder 402 located at the periphery of the dissolving tank 301 and arranged at the upper end surface of the mounting ring 403. When the dissolving tank 301 rotates, the dissolving tank 301 will not drive the mounting ring 403 to rotate, thereby ensuring the position stability of the proportioning assembly 400 structure; By setting and using the above-mentioned structure, through the use of the proportioning column 401 and the graduated cylinder 402, the dosage of o-chlorobenzyl cyanide and the ether solvent is controlled, so that the two can be fully dissolved, and the impurities in the o-chlorobenzyl cyanide that cannot be dissolved by the ether solvent will be precipitated in the dissolution tank 301. At the same time, through the cooperation between the crystallization purification tank 201 and the dissolution tank 301, the dissolved liquid is siphoned into the crystallization purification tank 201, and the solution inside the crystallization purification tank 201 is evaporated by the annular heater 105, so that the o-chlorobenzyl cyanide is recrystallized and purified.

[0035] according to Figure 2 , Figure 4 , Figure 8 and Fig.11A filter tube 103 is fixed on the side wall of the vertical plate 102 above the dissolving tank 301. One end of the filter tube 103 is connected to a siphon short tube 103b connected to the bottom of the dissolving tank 301. The other end of the filter tube 103 is connected to a siphon long tube 103a. A vacuum pump 202 is arranged in the middle cavity of the I-shaped frame 101 on the same side as the condensation tank 203. An inclined tube 402a with a valve is fixed to the lower end of the graduated cylinder 402. The proportioning column 403 is provided with a vacuum pump 202a. A proportioning port 401a is provided on the upper end surface of the proportioning column 401, a conical groove 401c is provided inside the proportioning column 401 below the proportioning port 401a, an electronic scale 405 is provided inside the conical groove 401c, an operating cylinder 404 is provided on the outer wall of the proportioning column 401, a pushing rod 408b for adjusting the tilt angle of the electronic scale 405 is provided inside the operating cylinder 404, and an electromagnet 407 is fixed inside the operating cylinder 404 below the pushing rod 408b; When the above-mentioned structure is used, after the dosage of o-chlorobenzyl cyanide and ether solvent is controlled, the weight of o-chlorobenzyl cyanide can be measured on the electronic scale 405, so as to control the electromagnet 407 to be powered off, and then the pushing rod 408b is reset to move upward, and the electronic scale 405 is pushed to rotate downward, so that the o-chlorobenzyl cyanide on the electronic scale 405 will directly slide into the dissolution tank 301, so as to achieve accurate feeding, ensure that the o-chlorobenzyl cyanide and the ether solution can be fully dissolved, and at the same time, the dissolution tank 301 and the crystallization purification tank 201 are connected through the siphon short tube 103b and the siphon long tube 103a, and the water tank 204 is controlled to pump pure water into the crystallization purification tank 201, so that the siphon short tube 103 The lower port in b is in water, and at this time, the interior of the crystallization purification tank 201 is evacuated to reduce the pressure inside the crystallization purification tank 201. At the same time, the crystallization purification tank 201 is located below the dissolution tank 301, and a siphon reaction occurs between the dissolution tank 301 and the crystallization purification tank 201, and the solution inside the dissolution tank 301 is drawn into the crystallization purification tank 201. Since the filter tube 103 is located between the long siphon tube 103a and the short siphon tube 103b, the filter tube 103 filters the solution flowing between the long siphon tube 103a and the short siphon tube 103b to avoid the flow of impurities, thereby achieving the inability to automatically control the extraction of the solution and achieving comprehensive extraction.

[0036] Further, according to Figure 2 and Fig.11 It can be seen that a discharge pipe 201a with a solenoid valve is fixed to the bottom of the crystallization purification tank 201, and the discharge pipe 201a passes through the hollow position of the annular heater 105 and the upper end surface of the I-shaped frame 101 in sequence. After the solution inside the crystallization purification tank 201 evaporates, the crystals produced will be precipitated at the bottom of the crystallization purification tank 201. At this time, the solenoid valve on the discharge pipe 201a can be opened, so that the crystals can be discharged from the inside of the discharge pipe 201a.

[0037] It should be noted that the electronic structures used are all powered by an external power supply, and the electronic structures used are linked and controlled by an external control center. When collecting the o-chlorobenzyl cyanide after crystallization and purification, the collection box can be set in the internal position of the I-shaped frame 101 directly below the crystallization purification tank 201, so it is convenient to collect the crystallized o-chlorobenzyl cyanide. Example 2

[0038] See also Figure 7 , Fig. 9 and Fig.11 On the basis of Example 1, this example drives the dissolution tank 301 to rotate by the motor 104, so that the solution can flow, thereby improving the rapid dissolution rate of o-chlorobenzyl cyanide in the ether solvent.

[0039] Specifically, a gear ring 302 is fixed to the lower part of the surface wall of the dissolving tank 301, a motor 104 is fixed to the side wall of the vertical plate 102 located below the filter tube 103, and a gear plate 104a meshing with the gear ring 302 is fixed to the rotating shaft end of the motor 104; By setting and using the above-mentioned structure, after the control motor 104 is working, the motor 104 will drive the gear ring 302 to rotate through the gear plate 104a. Therefore, after the o-chlorobenzyl cyanide and ether solution are poured into the dissolving tank 301, the dissolving tank 301 will drive the solution therein to shake, so as to make the solution flow, thereby improving the rapid dissolution speed of o-chlorobenzyl cyanide in the ether solvent. Example 3

[0040] See also Figure 2 , Fig.11 and Fig.12 On the basis of Example 1, this embodiment installs a plug-in tube 103b-1 at the bottom of the siphon short tube 103b, and penetrates a plurality of leak holes 103b-2 at different heights on the plug-in tube 103b-1, so as to avoid the situation where the port of the plug-in tube 103b-1 is blocked due to excessive impurities in the dissolution tank 301.

[0041] Specifically, a condenser pipe 205 connected to the interior of the crystallization purification tank 201 and the condensation tank 203 is arranged between the crystallization purification tank 201 and the condensation tank 203, a water pump in the water tank 204 is connected to the interior of the crystallization purification tank 201 through a pipeline, a port of the vacuum pump 202 is connected to the interior of the crystallization purification tank 201 through a fixed air pipe, a sealing plate 201b is arranged on the upper end surface of the crystallization purification tank 201, the bottom end of the siphon long tube 103a passes through the middle of the sealing plate 201b, a support frame 106 for supporting the crystallization purification tank 201 and the dissolution tank 301 is fixed on both sides of the vertical plate 102, and the two support frames 106 are arranged in an upper and lower position, the upper end surface of the crystallization purification tank 201 is lower than the bottom of the dissolution tank 301, a plug-in pipe 103b-1 connected to the bottom of the crystallization purification tank 201 is fixed at the bottom of the siphon short tube 103b, and a plurality of leak holes 103b-2 distributed in a ring array are opened through the surface side of the plug-in pipe 103b-1; By setting and using the above-mentioned structure, when all the solution inside the dissolving tank 301 flows into the internal position of the crystallization purification tank 201, the annular heater 105 is turned on at this time, so the steam generated inside the crystallization purification tank 201 flows into the condenser 205, and after the cooling treatment of the condenser 205, the ether solution and water are stored in the condensation box 203, and because the bottom of the siphon short tube 103b is fixed with the plug-in tube 103b-1, after the siphon short tube 103b is inserted into the dissolving tank 301, the plug-in tube 103b-1 will be located at the bottom position of the dissolving tank 301, and at the same time, the side wall of the plug-in tube 103b-1 passes through the leakage hole 103b-2, and the leakage hole 103b-2 is at different heights, so that solutions at different heights can be sucked into the plug-in tube 103b-1, avoiding the situation where the port of the plug-in tube 103b-1 is blocked due to excessive impurities in the dissolving tank 301. Example 4

[0042] See also Figure 4 , Figure 6 and Figure 8 On the basis of Example 1, this embodiment facilitates the reset activity of the electronic scale 405 by compressing the arc spring 405c and pushing the linkage plate 405b.

[0043] Specifically, the proportioning port 401a is connected to the tapered groove 401c through a through hole 401a-1 provided inside the proportioning column 401, an electrically controlled ball valve 401b is fixed at the position of the through hole 401a-1, a special-shaped port 401e is provided on the side wall of the proportioning column 401 on the same side as the operating cylinder 404, a rotating column 405a used in conjunction with the special-shaped port 401e is fixed at the end of the electronic scale 405, a linkage plate 405b passing through the position of the special-shaped port 401e is fixed on the side wall of the rotating column 405a, and the linkage plate 405b is connected to the operating cylinder 404. The upper end faces are abutted, the lower end face of the proportioning column 401 is fixed with a sliding tube 401d connected with the inside of the conical groove 401c, the lower end face of the proportioning column 401 is fixed with a mounting frame 406 bolted with the mounting ring 403, the inner side wall of the proportioning column 401 located inside the special-shaped opening 401e is provided with two shaft holes 401f arranged symmetrically in the front and back, the side wall of the rotating column 405a is fixed with a shaft rod 405a-1 rotating in the position inside the shaft hole 401f, and the upper end face of the linkage plate 405b is fixed with an arc spring 405c abutting against the side wall of the proportioning column 401; By setting and using the above-mentioned structure, when the linkage plate 405b is pushed by the pushing rod 408b, the linkage plate 405b will rotate upward and compress the arc spring 405c, so that the rotating column 405a rotates inside the special-shaped mouth 401e and controls the electronic scale 405 to rotate in the conical groove 401c, so that the o-chlorobenzyl cyanide on the surface of the electronic scale 405 can slide off. At the same time, after the pushing rod 408b is reset and contracted, the arc spring 405c will push the linkage plate 405b to rotate downward and drive the electronic scale 405 to fit with the lower end of the through hole 401a-1 again. Example 5

[0044] See also Figure 4 , Figure 5 and Fig.10 On the basis of Example 1, this embodiment controls the on and off operation of the electromagnet 407 to ensure automatic control of the rotation of the electronic scale 405.

[0045] Specifically, the upper end surface of the operating cylinder 404 is provided with a telescopic hole 404c whose aperture is smaller than the inner diameter of the operating cylinder 404, the upper end surface of the pushing rod 408b slides in the telescopic hole 404c, the lower end surface of the pushing rod 408b is fixed with a circular plate 408a which slides in the internal position of the operating cylinder 404, the lower end surface of the circular plate 408a is fixed with a metal rod 408 which is attracted to the electromagnet 407, a positioning ring 404b is fixed at the middle position inside the operating cylinder 404, the lower end of the circular plate 408a is fixed with a pushing spring 408c which abuts against the end surface of the positioning ring 404b, the surface side of the operating cylinder 404 is bolted to the proportioning column 401 through a fixed locking plate 404a, and the surface wall of the operating cylinder 404 is fixed with a remote control switch 409 which is electrically connected to the electromagnet 407 and the electronic scale 405; By setting and using the above structure, when the electromagnet 407 is powered off, the electromagnet 407 stops adsorbing the metal rod 408, and then the pushing spring 408c will push the circular plate 408a to move upward inside the operating cylinder 404, and then the circular plate 408a will control the pushing rod 408b to push the linkage plate 405b to rotate upward. When the electromagnet 407 is powered on, the electromagnet 407 will adsorb the metal rod 408, so that the metal rod 408 moves downward, and then the metal rod 408 drives the circular plate 408a to compress the pushing spring 408c, so as to ensure the automatic control of the rotation of the electronic scale 405; It should be noted that the elastic force of the pushing spring 408c used is greater than the elastic force of the arc spring 405c and the gravity of the linkage plate 405b, thereby ensuring that the linkage plate 405b can be pushed. Example 6

[0046] The present invention also provides an operating method of a crystallization purification device for producing o-chlorobenzyl cyanide, which is implemented by the following steps: S1: First, pour the ether solvent into the graduated cylinder 402, and pour the o-chlorobenzyl cyanide powder into the proportioning port 401a, and set the weighing value on the electronic scale 405. At this time, according to the capacity of the ether solvent in the graduated cylinder 402, control the electric control ball valve 401b to open, so that the o-chlorobenzyl cyanide powder falls onto the electronic scale 405; S2: After the o-chlorobenzyl cyanide powder on the electronic scale 405 reaches the set weighing value, the electromagnet 407 electrically controlled ball valve 401b is closed, the electromagnet 407 is powered off, and the pushing rod 408b moves upward, pushing the linkage plate 405b to rotate upward, thereby the linkage plate 405b drives the electronic scale 405 to rotate downward, so that the o-chlorobenzyl cyanide powder on the electronic scale 405 slides into the dissolving tank 301; S3: Pour the ether solvent in the graduated cylinder 402 into the dissolving tank 301 at the same time, so that the ether solvent and the o-chlorocyanobenzyl powder are fully dissolved; S4: At this time, the water in the water tank 204 is pumped into the crystallization purification tank 201, so that the water level in the crystallization purification tank 201 is higher than the height of the plug-in pipe 103b-1, and the vacuum tank is controlled to vacuum the interior of the crystallization purification tank 201, thereby siphoning occurs between the crystallization purification tank 201 and the dissolution tank 301, so that all the dissolved liquid enters the crystallization purification tank 201; S5: reducing the pressure in the crystallization purification tank 201 by the vacuum pump 202 to reduce the boiling point of the liquid therein, and controlling the ring heater 105 to evaporate the inside of the crystallization purification tank 201 to recrystallize the dissolved o-chlorobenzyl cyanide; S6: The evaporated water liquid and ether solution are cooled and recovered from the inside of the condenser 205, and the crystallized o-chlorobenzyl cyanide is discharged through the discharge pipe 201a.

[0047] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0048] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A crystallization and purification device for the production of o-chlorobenzyl cyanide, characterized in that: include, A support assembly (100) comprising an I-shaped frame (101), a vertical plate (102) fixed to the middle of the upper end of the I-shaped frame (101), and an annular heater (105) located on one side of the vertical plate (102) and fixedly connected to the upper end surface of the I-shaped frame (101); A crystallization purification assembly (200) comprises a crystallization purification tank (201) connected to the upper end surface of the annular heater (105), a condensation box (203) and a water tank (204) located on the other side of the vertical plate (102) and fixed to the upper end surface of the I-shaped frame (101), and a vacuum pump (202) is arranged in the middle cavity of the I-shaped frame (101) on the same side as the condensation box (203); A dissolution assembly (300) comprises a dissolution tank (301) located on the same side as the condensation tank (203), a filter tube (103) being fixed on the side wall of the vertical plate (102) located above the dissolution tank (301), one end of the filter tube (103) being connected to a short siphon tube (103b) connected to the bottom of the dissolution tank (301), and the other end of the filter tube (103) being connected to a long siphon tube (103a); and, A proportioning assembly (400) comprises a mounting ring (403) fixed to a side wall of a vertical plate (102) and slidably connected to an upper surface of a dissolving tank (301), a proportioning column (401) and a graduated cylinder (402) located at the periphery of the dissolving tank (301) and arranged at an upper end surface of the mounting ring (403), wherein an inclined tube (402a) with a valve is fixed to a lower end of the graduated cylinder (402), a proportioning port (401a) is provided on an upper end surface of the proportioning column (401), a conical groove (401c) is provided inside the proportioning column (401) below the proportioning port (401a), and an electronic scale (405) is provided inside the conical groove (401c); An operating cylinder (404) is provided on the outer wall of the proportioning column (401), a pushing rod (408b) for adjusting the tilt angle of the electronic scale (405) is provided inside the operating cylinder (404), and an electromagnet (407) is fixed inside the operating cylinder (404) below the pushing rod (408b).

2. A crystallization and purification equipment for the production of o-chlorobenzyl cyanide according to claim 1, characterized in that: A gear ring (302) is fixed to the lower portion of the surface wall of the dissolving tank (301), a motor (104) is fixed to the side wall of the vertical plate (102) below the filter tube (103), and a gear plate (104a) meshing with the gear ring (302) is fixed to the end of the rotating shaft of the motor (104).

3. A crystallization and purification equipment for the production of o-chlorobenzyl cyanide according to claim 1, characterized in that: A condenser pipe (205) connected to the interior of the crystallization purification tank (201) and the condensation tank (203) is provided between the crystallization purification tank (201) and the condensation tank (203). The water pump inside the water tank (204) is connected to the interior of the crystallization purification tank (201) through a pipeline. The port of the vacuum pump (202) is connected to the interior of the crystallization purification tank (201) through a fixed air pipe.

4. A crystallization and purification equipment for the production of o-chlorobenzyl cyanide according to claim 3, characterized in that: The upper end surface of the crystallization purification tank (201) is provided with a sealing plate (201b), and the bottom end of the long siphon tube (103a) passes through the middle of the sealing plate (201b); Support frames (106) for supporting the crystallization purification tank (201) and the dissolution tank (301) are fixed on both sides of the vertical plate (102), and the two support frames (106) are arranged in upper and lower positions, and the upper end surface of the crystallization purification tank (201) is lower than the bottom of the dissolution tank (301); A plug-in pipe (103b-1) connected to the bottom of the crystallization purification tank (201) is fixed at the bottom of the siphon short tube (103b), and a plurality of leak holes (103b-2) distributed in a ring array are penetrated through the surface of the plug-in pipe (103b-1).

5. A crystallization and purification equipment for the production of o-chlorobenzyl cyanide according to claim 1, characterized in that: A discharge pipe (201a) with a solenoid valve is fixed to the bottom of the crystallization purification tank (201), and the discharge pipe (201a) passes through the hollow position of the annular heater (105) and the upper end surface of the I-shaped frame (101) in sequence.

6. A crystallization and purification equipment for the production of o-chlorobenzyl cyanide according to claim 1, characterized in that: The proportioning port (401a) and the tapered groove (401c) are connected via a through hole (401a-1) provided inside the proportioning column (401); an electrically controlled ball valve (401b) is fixed at the position of the through hole (401a-1); a special-shaped port (401e) is provided on the side wall of the proportioning column (401) on the same side as the operating cylinder (404); a rotating column (405a) used in conjunction with the special-shaped port (401e) is fixed at the end of the electronic scale (405); a linkage plate (405b) passing through the position of the special-shaped port (401e) is fixed on the side wall of the rotating column (405a); and the linkage plate (405b) is in contact with the upper end surface of the operating cylinder (404); A sliding tube (401d) connected to the inside of the conical groove (401c) is fixed to the lower end surface of the proportioning column (401), and a mounting frame (406) bolted to the mounting ring (403) is fixed to the lower end surface of the proportioning column (401).

7. A crystallization and purification equipment for the production of o-chlorobenzyl cyanide according to claim 6, characterized in that: The inner side wall of the proportioning column (401) located inside the special-shaped opening (401e) is provided with two axial holes (401f) arranged symmetrically in the front and rear directions; a shaft (405a-1) rotating inside the axial hole (401f) is fixed on the side wall of the rotating column (405a); and an arc spring (405c) abutting against the side wall of the proportioning column (401) is fixed on the upper end surface of the linkage plate (405b).

8. A crystallization and purification equipment for the production of o-chlorobenzyl cyanide according to claim 1, characterized in that: The upper end surface of the operating cylinder (404) is provided with a telescopic hole (404c) whose diameter is smaller than the inner diameter of the operating cylinder (404); the upper end surface of the pushing rod (408b) slides in the telescopic hole (404c); the lower end surface of the pushing rod (408b) is fixed with a circular plate (408a) that slides inside the operating cylinder (404); and the lower end surface of the circular plate (408a) is fixed with a metal rod (408) that is attracted to the electromagnet (407).

9. A crystallization and purification device for the production of o-chlorobenzyl cyanide according to claim 8, characterized in that: A positioning ring (404b) is fixed at the middle position inside the operating cylinder (404), and a pushing spring (408c) abutting against the end surface of the positioning ring (404b) is fixed at the lower end of the circular plate (408a); The surface side of the operating cylinder (404) is bolted to the proportioning column (401) via a fixed locking plate (404a), and a remote control switch (409) electrically connected to the electromagnet (407) and the electronic scale (405) is fixed to the surface wall of the operating cylinder (404).

10. An operating method for a crystallization purification device for producing o-chlorobenzyl cyanide, characterized in that: The crystallization purification device for producing o-chlorobenzyl cyanide according to any one of claims 1 to 6 is implemented by the following steps: S1: First, pour the ether solvent into the graduated cylinder (402), and pour the o-chlorobenzyl cyanide powder into the proportioning port (401a), and set the weighing value on the electronic scale (405). At this time, according to the capacity of the ether solvent inside the graduated cylinder (402), control the electric control ball valve (401b) to open, so that the o-chlorobenzyl cyanide powder falls onto the electronic scale (405); S2: After the o-chlorobenzyl cyanide powder on the electronic scale (405) reaches a set weighing value, the electromagnet (407) and the electric-controlled ball valve (401b) are closed, the electromagnet (407) is powered off, and the pushing rod (408b) moves upward, pushing the linkage plate (405b) to rotate upward, whereby the linkage plate (405b) drives the electronic scale (405) to rotate downward, so that the o-chlorobenzyl cyanide powder on the electronic scale (405) slides into the dissolving tank (301); S3: simultaneously pouring the ether solvent in the graduated cylinder (402) into the dissolving tank (301) to fully dissolve the ether solvent and the o-chlorobenzyl cyanide powder; S4: at this time, the water in the water tank (204) is pumped into the crystallization purification tank (201), so that the water level in the crystallization purification tank (201) is higher than the height of the plug-in tube (103b-1), and the vacuum tank is controlled to perform vacuum treatment on the inside of the crystallization purification tank (201), thereby generating a siphon between the crystallization purification tank (201) and the dissolution tank (301), so that all the dissolved liquid enters the crystallization purification tank (201); S5: reducing the pressure in the crystallization purification tank (201) by means of the vacuum pump (202) to reduce the boiling point of the liquid therein, and controlling the ring heater (105) to operate to perform an evaporation treatment on the inside of the crystallization purification tank (201) to recrystallize the dissolved o-chlorobenzyl cyanide; S6: The evaporated water liquid and ether solution are cooled and recovered from the inside of the condenser (205), and the crystallized o-chlorobenzyl cyanide is discharged through the discharge pipe (201a).

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