A triethylamine hydrochloride freezing crystallization device and process

Abstract

The invention discloses a triethylamine hydrochloride freezing crystallization device and process, and relates to the technical field of triethylamine hydrochloride preparation. The invention comprises a solution processing component, comprising a processing tank and a tank cover located at an upper port position of the processing tank and flange-connected thereto, a crystallization component, comprising a crystallization tank located inside the processing tank and a stirring motor fixed at an upper end surface position of the tank cover, a distinguishing linkage component, comprising a distinguishing column sliding inside a transverse cylinder and a linkage column located inside the processing tank and arranged parallel to the distinguishing column at the same height, a circulation reflux component, and a freezing and recycling component. The invention realizes that the size of the crystals inside the crystallization tank can be distinguished by sliding the distinguishing column inside the transverse cylinder, thereby moving the curved hole and the vertical hole to the position directly below the lower port of the crystallization tank in different time periods, and small crystals are transported to a heating box through a screw rod, and the recovered small crystals are melted and recrystallized, so as to realize the work of achieving recrystallization by utilizing the waste heat.

Description

Technical Field

[0001] The invention belongs to the technical field of triethylamine hydrochloride preparation, and particularly relates to triethylamine hydrochloride freezing crystallization equipment and a process. Background Art

[0002] Triethylamine hydrochloride is often used as a base catalyst in organic synthesis, for example, in reactions such as esterification, etherification, and alkylation. It is hygroscopic and corrosive, and should be handled in a well-ventilated place and avoid contact with the skin and eyes. At the same time, triethylamine is an organic base, and reacts with hydrochloric acid to form triethylamine hydrochloride, that is, its hydrochloride form. This salt may usually have a high solubility in water, but the solubility will decrease when the temperature decreases. According to the existing public document CN118787979B, when preparing crystallization of triethylamine hydrochloride, frozen crystallization is also a preparation method.

[0003] However, at present, when using freezing crystallization equipment to crystallize the solution, the size of the crystal cannot be controlled, and there will be crystals of different sizes, and the smaller crystals need to be further washed and processed to purify them. However, since the equipment does not have the ability to distinguish crystals of different sizes, it is impossible to recycle and recrystallize the smaller crystals, so the crystals will be uniformly transported to the next step, affecting the purity of the product. At the same time, during the freezing crystallization process, a large amount of hot steam will be generated in the heat exchange process, and each time the smaller crystals are recrystallized, the small crystals need to be melted again, and each melting work needs to be heated separately. Since there is no function of reusing the hot steam, it will lead to the loss of heat energy, which will increase the energy consumption of the equipment and cause energy waste. To this end, we provide a triethylamine hydrochloride freezing crystallization equipment and process to solve the above problems. Summary of the invention

[0004] The purpose of the present invention is to provide a triethylamine hydrochloride freezing crystallization device and process. By sliding a distinguishing column inside a transverse cylinder, a curved hole and a vertical hole are respectively moved to a position directly below a lower port of a crystallizer in different time periods, so that the size of crystals inside the crystallizer can be distinguished and processed, and small crystals can be recovered. At the same time, the small crystals are transported to a heating box through a screw rod, and the steam in the condensation process is reused to melt and recrystallize the recovered small crystals, so that the recrystallization work is achieved by utilizing the waste heat.

[0005] In order to solve the above technical problems, the present invention is achieved through the following technical solutions:

[0006] The invention provides a triethylamine hydrochloride freezing crystallization device, comprising a solution processing component, comprising a processing tank and a tank cover located at an upper port position of the processing tank and flange-connected therewith, a crystallization component, comprising a crystallization tank located inside the processing tank and a stirring motor fixed at an upper end surface position of the tank cover, a transverse cylinder fixed at a lower end position of the crystallization tank, a differentiation linkage component, comprising a differentiation column sliding inside the transverse cylinder and a linkage column located inside the processing tank and arranged in parallel with the differentiation column at the same height, independent cavity pistons at both ends of the linkage column are provided with pressure plugs, a curved hole and a vertical hole symmetrically arranged are opened on the surface side of the differentiation column located inside the transverse cylinder, a circulation reflux component, comprising a circulation box and a heating box located inside the processing tank, a vertically arranged spiral rod inside the circulation box, and a freezing and recycling component, comprising a condensation ring group fixed at a lower position on the surface side of the processing tank and a heating ring group fixed at a lower position on the surface side of the heating box, and a steam pipe fixedly connected between the condensation ring group and the heating ring group.

[0007] The present invention is further configured such that a stirring rod with an upper end passing through the upper end surface of the crystallization tank is provided inside the crystallization tank, a main tooth plate is fixed to the rotating shaft end of the stirring motor inside the processing tank, and a slave tooth plate meshing with the main tooth plate is fixed to the upper end surface of the stirring rod. Through the linkage work of the main tooth plate and the slave tooth plate, it can be ensured that the stirring motor drives the rotation of the stirring rod, and the solution inside the crystallization tank can be stirred at all times.

[0008] The present invention is further configured such that a limit plate is provided between the stirring rod located above the crystallization tank and the rotating shaft of the stirring motor, the stirring rod and the rotating shaft of the stirring motor are both rotatably connected to the limit plate, a solution tube is provided on the upper end surface of the tank cover, and the lower end of the solution tube passes through the tank cover and is plugged into the interior of the crystallization tank, the stirring rod and the rotating shaft of the stirring motor are matched through the limit plate to ensure stable meshing of the main tooth plate and the slave tooth plate, and at the same time the solution tube is connected to an external solution device, so that the solution tube can enter the crystallization tank in a regular and quantitative manner.

[0009] The present invention is further configured such that a discharge pipe whose upper and lower positions are consistent with those of the lower port of the crystallizer is connected to the middle of the lower surface side of the transverse tube, and an inclined tube whose port is inclined downward is fixedly connected to the middle of the surface side of the transverse tube between the discharge pipe and the crystallizer, and the discharge pipe passes through the bottom position of the crystallizer, so that after the vertical hole and the discharge pipe are consistent in upper and lower positions, the crystals inside the crystallizer will be directly discharged from the positions of the vertical hole and the discharge pipe.

[0010] The present invention is further configured such that the surface side wall of the circulation box is fixedly connected with a bellows whose port is inclined upward and sealedly connected to the inclined pipe, the upper part of the surface side of the circulation box is fixedly connected with an inclined curved pipe connected to the inside of the heating box, the surface side wall of the crystallizer is fixed with a connecting pipe, and the lower end of the heating box is fixed with a reflux pipe connected to the connecting pipe. Due to the inclined coordination of the inclined pipe and the bellows, the crystals inside the crystallizer can accurately and completely slide into the circulation box, and the end of the inclined curved pipe close to the circulation box is at a high position, while the end of the inclined curved pipe close to the crystallizer is at a low position, so that small crystals can slide from the position of the inclined curved pipe into the heating box.

[0011] The present invention is further configured such that a bevel gear 1 is fixed on the lower end face of the spiral rod passing through the circulation box, a progressive motor is fixed on the outer wall of the processing tank, a bevel gear 2 meshing with the bevel gear 1 is fixed on the shaft end of the progressive motor rotating through the circulation box, and a screen is fixed on the upper end of the curved hole. Through the cooperation of the bevel gear 1 and the bevel gear 2, the spiral rod is driven to work in a spiral progressive manner inside the circulation box. At the same time, the crystals inside the crystallization tank are distinguished by size through the screen, and the small crystals are recovered.

[0012] The present invention is further configured such that linkage plates are fixed at both ends of the distinguishing column outside the transverse cylinder, linkage rods are fixed between the linkage plates and the adjacent pressure plug blocks, and two L-shaped tubes are fixed on the surface side walls of the linkage column, which are respectively connected to the inside of the independent cavities at both ends of the linkage column, and the other ends of the two L-shaped tubes pass through the surface wall of the processing tank. The L-shaped tube outside the processing tank is arranged parallel to the surface wall of the processing tank. At the same time, when the pressure plug blocks slide in the two independent cavities at both ends of the linkage column, they will drive the linkage rod to follow the movement, and thereby control the linkage plate to drive the distinguishing column to move synchronously inside the transverse cylinder.

[0013] The present invention is further configured such that racks passing through the upper ports of the L-shaped tubes are arranged inside the two L-shaped tubes outside the processing tank, and a piston block arranged inside the L-shaped tube is fixed on the lower end surface of the rack. When the rack is driven by the tooth plate to slide up and down, the rack will drive the piston block to move in the L-shaped tube, thereby compressing the gas inside the L-shaped tube, thereby promoting the movement of the compressed plug block.

[0014] The present invention is further configured such that a linkage motor is provided on the surface wall of the processing tank located between the two racks, and the linkage motor is bolted to the processing tank via a mounting plate fixed on the surface side, and a linkage tooth plate meshing with the two racks is fixed on the rotating shaft end of the linkage motor.

[0015] The present invention also provides a freezing crystallization process of triethylamine hydrochloride, which is implemented by the following steps:

[0016] S1: transporting the solution from the inside of the solution tube to allow the triethylamine hydrochloride solution to enter the crystallization tank, and controlling the temperature inside the crystallization tank in the condensation ring group to control the inside of the triethylamine hydrochloride solution to perform freezing crystallization;

[0017] S2: After the crystallizer has been working for a certain period of time, the linkage motor is controlled to work in the forward direction, thereby controlling the curved hole to move to the position directly below the lower port of the crystallizer. At this time, the smaller crystals inside the crystallizer will slide from the curved hole into the circulation box;

[0018] S3: The crystals are then transported to the heating box through the work of the screw rod, and the hot gas exchanged between the condensate and the high-temperature gas in the condensation ring group will enter the heating box, and the cooling gas will cool the inside of the crystallizer. At the same time, the hot steam heats and evaporates the crystals in the heating box. After a period of time, the solution produced will flow back to the crystallizer from the bottom of the heating box;

[0019] S4: At the same time, after the linkage motor is controlled to reverse, the vertical hole will be controlled to move to a position directly below the lower port of the crystallizer, and then the remaining crystals in the crystallizer will be discharged from the inside of the vertical hole.

[0020] The present invention has the following beneficial effects:

[0021] Drive the distinguishing column to slide in the internal position of the horizontal cylinder. First, it is necessary to control the curved hole to move to the position just below the lower port of the crystallizer, and open the solenoid valve at the lower port of the crystallizer, so that the crystals inside the crystallizer will fall onto the screen, and the small crystals will be separated from the curved hole into the circulation box through the screen. Then, the distinguishing column is controlled to move in the opposite direction, and the vertical hole is moved to the position just below the lower port of the crystallizer, so that the remaining crystals inside the crystallizer will be directly discharged from the vertical hole, so that the crystals inside the crystallizer can be distinguished by size and processed to ensure that the small crystals can be recycled.

[0022] The spiral rod will spirally transport the small crystals inside the circulation box upward, and the pipes installed inside the heating ring group will fit the surface wall of the heating box, so that the high-temperature steam will gradually increase the temperature inside the heating box. At the same time, the corresponding condenser is installed inside the condenser ring group used. The condensate inside the condenser is connected with the high-temperature gas, and the generated steam will enter the steam pipe, thereby heating the inside of the heating box, so as to melt the crystals in the heating box and reflux them into the crystallization tank, realizing recrystallization by utilizing the waste heat.

[0023] 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

[0024] 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.

[0025] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0026] Figure 2 This is a structural combination diagram of the crystallization tank, stirring motor, separation column and circulation box in the present invention.

[0027] Figure 3 It is a schematic diagram of the internal structure of the linkage plate, linkage column, rack and linkage motor in the present invention.

[0028] Figure 4 It is a structural diagram of the linkage plate, linkage column, rack and toothed plate in the present invention.

[0029] Figure 5 The figure is a structural combination diagram of the crystallization tank, the stirring motor, the solution tank, the limit plate and the stirring rod in the present invention.

[0030] Figure 6 This is a diagram of the internal structure of the crystallization component of the present invention.

[0031] Figure 7 This is a structural combination diagram of the circulation box, heating box, spiral rod and progressive motor in the present invention.

[0032] Figure 8 It is a structural combination diagram of the condensing ring group and the heating ring group in the present invention.

[0033] Fig. 9 It is an external schematic diagram of the overall structure of the present invention.

[0034] Fig.10 It is a structural diagram of the crystallization tank, the separation column and the linkage column in the present invention.

[0035] Fig.11 It is a structural combination diagram of the circulation box, heating box and progressive motor in the present invention.

[0036] In the accompanying drawings, the components represented by the reference numerals are listed as follows:

[0037] 100-solution processing assembly, 101-processing tank, 102-tank cover, 200-crystallization assembly, 201-crystallization tank, 201a-transverse cylinder, 201b-discharge pipe, 201c-connecting pipe, 201d-inclined pipe, 202-stirring motor, 202a-main tooth plate, 203-solution pipe, 204-limiting plate, 205-stirring rod, 205a-slave tooth plate, 300-differentiation linkage assembly, 301-differentiation column, 301a-vertical hole, 301b-bent hole, 301c-screen, 302-linkage plate, 302a-pressure plug, 302b -linking rod, 303-linking column, 303a-L-shaped tube, 304-rack, 304a-piston block, 305-linking motor, 305a-mounting plate, 305b-linking gear plate, 400-circulation reflux assembly, 401-circulation box, 401a-inclined curved pipe, 401b-bellows, 402-heating box, 402a-reflux pipe, 403-screw rod, 403a-bevel gear one, 404-progressive motor, 404a-bevel gear two, 500-refrigeration reuse assembly, 501-condensation ring group, 501a-steam pipe, 502-heating ring group. DETAILED DESCRIPTION

[0038] 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

[0039] See also Figure 1 , Figure 2 , Figure 7 , Figure 8 and Fig. 9 , which is the first embodiment of the present invention, provides a triethylamine hydrochloride freezing crystallization device, through the sliding of the distinguishing column 301 inside the horizontal cylinder 201a, the curved hole 301b and the vertical hole 301a are moved to the position directly below the lower port of the crystallization tank 201 at different time periods, so that the crystals inside the crystallization tank 201 can be distinguished by size, ensuring that small crystals can be recovered, and at the same time, the small crystals are transported to the heating box 402 through the spiral rod 403, and the steam in the condensation process is reused to melt and recrystallize the recovered small crystals, thereby achieving recrystallization by utilizing the waste heat.

[0040] Specifically, the solution processing component 100 includes a processing tank 101 and a tank cover 102 located at an upper port position of the processing tank 101 and flange-connected thereto; the crystallization component 200 includes a crystallization tank 201 located inside the processing tank 101 and a stirring motor 202 fixed on an upper end surface position of the tank cover 102; the differentiation linkage component 300 includes a differentiation column 301 sliding inside a transverse cylinder 201a and a linkage column 303 located inside the processing tank 101 and arranged parallel to the differentiation column 301 at the same height; the circulation reflux component 400 includes a circulation box 401 and a heating box 402 located inside the processing tank 101; the freezing and recycling component 500 includes a condensation ring group 501 fixed at a lower portion of the surface side of the processing tank 101 and a heating ring group 502 fixed at a lower portion of the surface side of the heating box 402;

[0041] By setting and using the above-mentioned structure, the triethylamine hydrochloride solution is poured into the crystallizer 201, and the high-temperature gas is sent in through an external compressor, and refrigerated through the condensing ring group 501, so as to freeze the inside of the crystallizer 201, and control the solution inside the crystallizer 201 to gradually crystallize, and at the same time, the generated steam will enter the heating ring group 502 to heat the inside of the heating box 402, so when the crystals are screened, the small crystals generated will enter the heating box 402, and the crystals will be melted by the high temperature inside the heating box 402, and when the solution reaches a certain height inside the heating box 402, the fixed liquid level device inside the heating box 402 will control the signal data to open the valve on the reflux pipe 402a, so that the solution enters the crystallizer 201.

[0042] according to Figure 3 , Figure 5 , Figure 7 and Fig.10 A transverse cylinder 201a is fixed at the lower port of the crystallization tank 201, and pistons in independent cavities at both ends of the linkage column 303 are provided with pressure plugs 302a. A curved hole 301b and a vertical hole 301a are symmetrically arranged on the surface side of the distinguishing column 301 inside the transverse cylinder 201a. A vertically arranged spiral rod 403 is arranged inside the circulation box 401. A steam pipe 501a is fixedly connected between the condensing ring group 501 and the heating ring group 502, and a screen 301c is fixed on the upper end of the curved hole 301b.

[0043] When using the structure set as above, the pressure plug 302a is controlled to move in the independent cavities at both ends of the linkage column 303, thereby driving the distinguishing column 301 to slide in the internal position of the horizontal cylinder 201a. First, the curved hole 301b needs to be controlled to move to the position directly below the lower port of the crystallizer 201, and the solenoid valve at the lower port of the crystallizer 201 is opened, so that the crystals inside the crystallizer 201 will fall onto the screen 301c, and the small crystals will be separated from the position of the curved hole 301b to the circulation box 401 through the screen 301c, and then the distinguishing column 301 is controlled to move in the opposite direction, and the vertical hole 301a is moved to the position directly below the lower port of the crystallizer 201 ... The remaining crystals will be directly discharged from the vertical hole 301a, and when the spiral rod 403 in the circulation box 401 is working, the spiral rod 403 will spirally transport the small crystals inside the circulation box 401 upward, and the pipe installed inside the heating ring group 502 will fit the surface wall of the heating box 402, so that the high-temperature steam gradually increases the temperature inside the heating box 402. At the same time, the corresponding condensing tube is installed inside the condensing ring group 501 used. The condensate inside the condensing tube is connected with the high-temperature gas, and the generated steam will enter the steam pipe 501a, so as to heat the inside of the heating box 402, so as to melt the crystals in the heating box 402 and return them to the crystallization tank 201;

[0044] In summary, the steam pipe 501a used and the condenser in the condensation ring group 501 are in a state of mutual connection. Therefore, after the condensate in the condenser absorbs heat and vaporizes, the generated gas floats upward in the condenser, thereby entering the steam pipe 501a, and enters the pipeline in the heating ring group 502 through the steam pipe 501a, continuously heating the heating box 402, and at the same time, the liquid or gas formed by the gas in the heating ring group 502 after cooling will flow away from the position of the external pipe of the heating ring group 502, and the condensation ring group is not connected with the crystallization tank 201 and the interior of the transverse tube 201a.

[0045] Further, according to Figure 7 It can be seen that the spiral rod 403 passes through the lower end face of the circulation box 401 and is fixed with a bevel gear 1 403a, and the outer wall of the processing tank 101 is fixed with a progressive motor 404. The progressive motor 404 rotates and passes through the circulation box 401, and a bevel gear 2 404a meshing with the bevel gear 1 403a is fixed on the axial end, so as to control the progressive motor 404 to work. The progressive motor 404 will drive the bevel gear 2 404a to rotate, and thereby drive the bevel gear 1 403a to work, so that the bevel gear 1 403a will directly drive the spiral rod 403 to rotate inside the rotating box, thereby controlling the small crystals inside the circulation box 401 to be transported upward.

[0046] It should be noted that the refrigerant is compressed into a high-temperature and high-pressure gas by an external compressor and transported to the condensation ring group 501, and the condensate is circulated through the condenser tube in the condensation ring group 501 through an external condensate device to reflux, thereby generating high-temperature steam, which enters the steam pipe. At the same time, the surface walls of the heating box 402 and the crystallization tank 201 are wrapped with thermal insulation cotton to reduce the temperature loss efficiency inside the heating box 402 and the crystallization tank 201. Example 2

[0047] See also Figure 5 and Figure 6 On the basis of Example 1, this embodiment constantly stirs the interior of the crystallization tank 201 by means of a stirring rod 205 to ensure that the solute in the crystallization tank 201 is prevented from accumulating at the bottom of the container, thereby ensuring that the solute in the solution is evenly dissolved.

[0048] Specifically, the interior of the crystallizer 201 is provided with a stirring rod 205 whose upper end passes through the upper end surface of the crystallizer 201, a main tooth plate 202a is fixed to the rotating shaft end of the stirring motor 202 located inside the processing tank 101, and a slave tooth plate 205a meshing with the main tooth plate 202a is fixed to the upper end surface of the stirring rod 205, a limit plate 204 is arranged between the stirring rod 205 located above the crystallizer 201 and the rotating shaft of the stirring motor 202, the stirring rod 205 and the rotating shaft of the stirring motor 202 are both rotatably connected to the limit plate 204, a solution tube 203 is arranged on the upper end surface of the tank cover 102, and the lower end of the solution tube 203 passes through the tank cover 102 and is plugged into the interior of the crystallizer 201;

[0049] By setting and using the above-mentioned structure, before the triethylamine hydrochloride solution in the crystallizer 201 is crystallized, it is necessary to control the stirring motor 202 to work, so as to drive the slave tooth plate 205a to rotate through the main tooth plate 202a, and control the stirring rod 205 to rotate inside the crystallizer 201, so as to evenly stir the triethylamine hydrochloride solution in the crystallizer 201, so as to ensure that the solute in the crystallizer 201 is prevented from accumulating at the bottom of the container and ensure that the solute in the solution is evenly dissolved. At the same time, the limit plate 204 is rotationally connected with the stirring rod 205 and the rotating shaft of the stirring motor 202 to ensure that the limit plate 204 does not rotate and the stirring motor 202 can drive the stirring rod 205 to rotate synchronously. Example 3

[0050] See also Figure 6 , Figure 7 and Fig.11On the basis of Example 1, this embodiment realizes the connection between the interior of the heating box 402, the circulation box 401 and the crystallization tank 201 in a reflux phase connection by connecting the inclined tube 201d and the bellows 401b, and connecting the reflux pipe 402a and the connecting pipe 201c, thereby ensuring the stable operation of the melting and recrystallization of small crystals.

[0051] Specifically, the middle part of the lower surface side of the transverse tube 201a is connected with a discharge pipe 201b which is consistent with the position of the lower port of the crystallizer 201, and the middle part of the surface side of the transverse tube 201a between the discharge pipe 201b and the crystallizer 201 is fixedly connected with an inclined pipe 201d whose port is inclined downward, and the surface side wall of the circulation box 401 is fixedly connected with a bellows 401b whose port is inclined upward and sealedly connected with the inclined pipe 201d, and the upper part of the surface side of the circulation box 401 is fixedly connected with an inclined curved pipe 401a connected with the inside of the heating box 402, and the surface side wall of the crystallizer 201 is fixed with a connecting pipe 201c, and the lower end of the heating box 402 is fixed with a reflux pipe 402a connected with the connecting pipe 201c.

[0052] By setting and using the above structure, the control column 301 slides inside the horizontal tube 201a, and after the vertical hole 301a is moved to the position just below the lower port of the crystallizer 201, the vertical hole 301a is connected to the inner part of the discharge pipe 201b, so that the crystals inside the crystallizer 201 are directly discharged from the inner part of the discharge pipe 201b, and when the curved hole 301b is moved to the position just below the lower port of the crystallizer 201, the small crystals screened therein enter the inclined tube 201d from the position of the curved hole 301b, thereby being discharged from the corrugated tube. The position of 401b slides into the circulation box 401, and the inclined curved pipe 401a is used at the same time. Therefore, after the spiral rod 403 transports the small crystals to the position directly above the circulation box 401, the small crystals will enter the inclined curved pipe 401a, and then the small crystals will be discharged into the heating box 402. The crystals are melted by the heating box, and the reflux pipe 402a is connected to the connecting pipe 201c, so the melted solution will pass through the reflux pipe 402a and the connecting pipe 201c into the crystallization tank 201, so as to recrystallize it. Example 4

[0053] See also Figure 3 , Figure 4 and Fig.10 On the basis of Example 1, this embodiment drives the two racks 304 to slide up and down through the linkage motor 305, so as to drive the distinguishing column 301 to slide back and forth in both directions inside the horizontal cylinder 201a, so that the curved hole 301b and the vertical hole 301a can be moved to the position directly below the lower port of the crystallization tank 201 respectively, so as to distinguish the crystals.

[0054] Specifically, linkage plates 302 are fixed at both ends of the distinguishing column 301 outside the transverse cylinder 201a, and linkage rods 302b are fixed between the linkage plates 302 and the adjacent pressure plugs 302a. Two L-shaped tubes 303a are fixed to the surface side wall of the linkage column 303, which are respectively connected to the independent cavities at both ends of the linkage column 303, and the other ends of the two L-shaped tubes 303a pass through the surface wall of the processing tank 101. The two L-shaped tubes 303a outside the processing tank 101 are both provided with A rack 304 is provided passing through the upper end of the L-shaped tube 303a, a piston block 304a having a piston arranged inside the L-shaped tube 303a is fixed to the lower end surface of the rack 304, a linkage motor 305 is provided on the surface wall of the processing tank 101 between the two racks 304, and the linkage motor 305 is bolted to the processing tank 101 through a mounting plate 305a fixed on the surface side, and a linkage tooth plate 305b meshing with the two racks 304 is fixed to the rotating shaft end of the linkage motor 305;

[0055] Through the arrangement and use of the above-mentioned structure, when it is necessary to control the back-and-forth cyclic movement of the curved hole 301b and the vertical hole 301a, it is necessary to control the linkage motor 305 to work forward and reversely. After the linkage motor 305 is controlled to work forwardly, the two racks 304 will be driven to move up and down respectively through the linkage tooth plate 305b, so as to control the piston block 304a to compress and suck the two independent L-shaped tubes 303a, thereby driving the compressed plug blocks 302a inside the two inner cavities of the linkage column 303 to move in the same direction, thereby controlling the distinguishing column 301 to move unidirectionally inside the horizontal cylinder 201a, and driving the curved hole 301b to move to a position directly below the lower port of the crystallization tank 201. At the same time, after the linkage motor 305 is controlled to work in reverse, it will work in the directions of the above-mentioned structures, so as to drive the distinguishing column 301 to slide in the opposite direction inside the horizontal cylinder 201a, and drive the vertical hole 301a to move to a position directly below the lower port of the crystallization tank 201, thereby realizing the distinction of crystals. Example 5

[0056] A freezing crystallization process of triethylamine hydrochloride is implemented by the following steps:

[0057] S1: transporting the solution from the inside of the solution pipe 203 to allow the triethylamine hydrochloride solution to enter the crystallization tank 201, and controlling the temperature inside the crystallization tank 201 in the condensation ring group 501, so as to control the inside of the triethylamine hydrochloride solution to perform freezing crystallization;

[0058] S2: After the crystallizer 201 has been working for a certain period of time, the linkage motor 305 is controlled to work in the forward direction, thereby controlling the curved hole 301b to move to a position directly below the lower port of the crystallizer 201. At this time, the smaller crystals inside the crystallizer 201 will slide from the curved hole 301b to the circulation box 401;

[0059] S3: The crystals are then transported to the heating box 402 through the operation of the screw rod 403, and the hot gas exchanged between the condensate in the condensation ring group 501 and the high-temperature gas will enter the heating box 402, and the cooling gas will cool the inside of the crystallizer, while the hot steam heats and evaporates the crystals in the heating box 402, and after a period of time, the resulting solution will flow back from the bottom of the heating box 402 to the crystallizer 201;

[0060] S4: At the same time, after the linkage motor 305 is controlled to reverse, the vertical hole 301a is controlled to move to a position directly below the lower port of the crystallization tank 201, and then the remaining crystals in the crystallization tank 201 are discharged from the inside of the vertical hole 301a.

[0061] 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.

[0062] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only specific implementation methods. 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 triethylamine hydrochloride freezing crystallization equipment, characterized in that: include, A solution processing assembly (100) comprises a processing tank (101) and a tank cover (102) located at an upper port of the processing tank (101) and flange-connected thereto; A crystallization assembly (200) comprises a crystallization tank (201) located inside the processing tank (101) and a stirring motor (202) fixed to the upper end surface of the tank cover (102), wherein a transverse cylinder (201a) is fixed to the lower end of the crystallization tank (201); A distinguishing linkage assembly (300) comprises a distinguishing column (301) slidingly arranged inside a transverse cylinder (201a) and a linkage column (303) located inside a processing tank (101) and arranged parallel to and at the same height as the distinguishing column (301), wherein pistons in independent cavities at both ends of the linkage column (303) are provided with pressure plugs (302a), and a curved hole (301b) and a vertical hole (301a) are symmetrically arranged on the surface side of the distinguishing column (301) located inside the transverse cylinder (201a); A circulation reflux assembly (400) comprises a circulation box (401) and a heating box (402) located inside the processing tank (101), wherein a vertically arranged spiral rod (403) is provided inside the circulation box (401); and, The freezing and recycling assembly (500) includes a condensing ring assembly (501) fixed to the lower portion of the surface side of the processing tank (101) and a heating ring assembly (502) fixed to the lower portion of the surface side of the heating box (402), wherein a steam pipe (501a) is fixedly connected between the condensing ring assembly (501) and the heating ring assembly (502).

2. A triethylamine hydrochloride freezing and crystallization equipment according to claim 1, characterized in that, The crystallization tank (201) is provided with a stirring rod (205) whose upper end passes through the upper end surface of the crystallization tank (201); a main tooth plate (202a) is fixed to the rotating shaft end of the stirring motor (202) inside the processing tank (101); and a secondary tooth plate (205a) meshing with the main tooth plate (202a) is fixed to the upper end surface of the stirring rod (205).

3. a kind of triethylamine hydrochloride freezing crystallization equipment according to claim 2, is characterized in that, A limit plate (204) is provided between a stirring rod (205) located above the crystallization tank (201) and a rotating shaft of a stirring motor (202); the stirring rod (205) and the rotating shaft of the stirring motor (202) are both rotatably connected to the limit plate (204); a solution tube (203) is provided on the upper end surface of the tank cover (102); and a lower end of the solution tube (203) passes through the tank cover (102) and is plugged into the interior of the crystallization tank (201).

4. a kind of triethylamine hydrochloride freezing crystallization equipment according to claim 1, is characterized in that, The middle portion of the lower surface side of the transverse tube (201a) is connected to a discharge pipe (201b) whose position is aligned with the lower port of the crystallization tank (201) in vertical direction, and the middle portion of the upper surface side of the transverse tube (201a) between the discharge pipe (201b) and the crystallization tank (201) is fixedly connected to an inclined tube (201d) whose port is inclined downward.

5. a kind of triethylamine hydrochloride freezing crystallization equipment according to claim 4, is characterized in that, The surface side wall of the circulation box (401) is fixedly connected with a bellows (401b) whose port is inclined upward and sealed to the inclined pipe (201d); the upper portion of the surface side of the circulation box (401) is fixedly connected with an inclined curved pipe (401a) connected to the interior of the heating box (402); the surface side wall of the crystallization tank (201) is fixed with a connecting pipe (201c); and the lower end of the heating box (402) is fixed with a reflux pipe (402a) connected to the connecting pipe (201c).

6. A triethylamine hydrochloride freezing crystallization equipment according to claim 1, characterized in that, The spiral rod (403) passes through the lower end surface of the circulation box (401) and is fixed with a bevel gear 1 (403a); the outer wall of the processing tank (101) is fixed with a progressive motor (404); the axial end of the progressive motor (404) that rotates and passes through the circulation box (401) is fixed with a bevel gear 2 (404a) that meshes with the bevel gear 1 (403a); and the upper end of the curved hole (301b) is fixed with a screen (301c).

7. A triethylamine hydrochloride freezing crystallization equipment according to claim 1, characterized in that, Linkage plates (302) are fixed at both ends of the dividing column (301) outside the transverse cylinder (201a), and linkage rods (302b) are fixed between the linkage plates (302) and the adjacent pressure plugs (302a). Two L-shaped tubes (303a) are fixed to the surface side wall of the linkage column (303), which are respectively connected to the inside of the independent cavities at both ends of the linkage column (303), and the other ends of the two L-shaped tubes (303a) pass through the surface wall of the processing tank (101).

8. A triethylamine hydrochloride freezing crystallization equipment according to claim 7, characterized in that, Racks (304) passing through the upper ports of the L-shaped tubes (303a) are arranged inside the two L-shaped tubes (303a) outside the processing tank (101), and piston blocks (304a) arranged inside the L-shaped tubes (303a) are fixed to the lower end surfaces of the racks (304).

9. A triethylamine hydrochloride freezing crystallization equipment according to claim 8, characterized in that, A linkage motor (305) is provided on the surface wall of the processing tank (101) between the two racks (304), and the linkage motor (305) is bolted to the processing tank (101) via a mounting plate (305a) fixed on the surface side, and a linkage tooth plate (305b) meshing with the two racks (304) is fixed to the rotating shaft end of the linkage motor (305).

10. A freezing crystallization process for triethylamine hydrochloride, characterized in that: The triethylamine hydrochloride freezing crystallization device described in claim 9 is implemented by the following steps: S1: transporting the solution from the inside of the solution pipe (203) to allow the triethylamine hydrochloride solution to enter the crystallization tank (201), and controlling the temperature inside the crystallization tank (201) in the condensation ring group (501) to control the inside of the triethylamine hydrochloride solution to perform freezing crystallization; S2: After the crystallization tank (201) has been working for a certain period of time, the linkage motor (305) is controlled to work in the forward direction, thereby controlling the curved hole (301b) to move to a position directly below the lower port of the crystallization tank (201), and at this time, the smaller crystals inside the crystallization tank (201) will slide from the position of the curved hole (301b) into the circulation box (401); S3: The crystals are then transported to the heating box (402) through the operation of the screw rod (403), and the hot gas exchanged between the condensate in the condensation ring group (501) and the high-temperature gas will enter the heating box (402), and the cooled gas will cool the interior of the crystallization tank (201), while the hot steam heats and evaporates the crystals in the heating box (402), and after a period of time, the generated solution will flow back from the bottom of the heating box (402) to the crystallization tank (201); S4: At the same time, after the linkage motor (305) is controlled to reverse, the vertical hole (301a) is controlled to move to a position directly below the lower port of the crystallization tank (201), and the remaining crystals in the crystallization tank (201) are discharged from the inside of the vertical hole (301a).

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