Intelligent extraction method and equipment for metaraminol bitartrate

Abstract

The invention relates to the technical field of tartrate continuous crystallization control, in particular to an intelligent extraction method and equipment for metaraminol bitartrate, crystals are separated out of a solution through a physical means, a low-pressure state is maintained in a crystallizing tank through a pressure adjusting device in the extraction process, the distillation temperature of the solution can be reduced, and the extraction efficiency is improved. Necessary heat energy is provided for the solution through the heating device, low-temperature distillation is promoted, and cooling precipitation of crystals can be further promoted through low-temperature distillation. The liquid level sensor monitors the liquid level in the crystallizing tank and cooperates with the first switch device to control the opening and closing of the feeding pipe, so that the accuracy of the feeding time and the feeding amount of materials is ensured; the pressure sensor monitors the pressure in the crystallizing tank and cooperates with the pressure adjusting device to maintain the low-pressure environment in the tank, so that the low-temperature distillation process is facilitated; the weight of crystals in the discharging pipe is monitored through a weighing sensor, and the crystals are regularly guided out through cooperation with a second switch device; and the stability of the product quality is ensured through continuous cooling crystallization.

Description

Technical Field

[0001] The invention relates to the technical field of continuous crystallization control of bitartrate, and in particular to an intelligent extraction method and equipment for meta-hydroxylamine bitartrate. Background Art

[0002] As an important pharmaceutical intermediate, metahydroxylamine bitartrate is widely used in the synthesis of cardiovascular drugs. Metahydroxylamine is first synthesized and then converted into bitartrate; wherein, purified metahydroxylamine is mixed with excess tartaric acid in a solvent, and the pH value is adjusted to form bitartrate, and then the formed salt is cooled and crystallized, and finally filtered and dried to obtain the product; therefore, the crystallization process in the production process of metahydroxylamine bitartrate has a significant impact on the purity and yield of the product.

[0003] At present, the crystallization production of metaryl tartrate mainly adopts batch operation. Due to the fluctuation of operating conditions and the lack of effective monitoring and feedback mechanism in the batch crystallization process, the product quality varies greatly between different batches, affecting the stability of the product; in each batch of crystallization process, the control of key parameters such as production temperature and pressure in the container often depends entirely on the operator's experience and manual adjustment, lacking precise automatic control methods; the monitoring of the crystallization process also depends on the operator's regular sampling and offline analysis, which has a certain lag. Therefore, it is difficult to maintain the optimal crystallization conditions in the production process of metaryl tartrate, which affects the quality and yield of the crystallization. Summary of the invention

[0004] The invention provides an intelligent extraction method and equipment for meta-hydroxylamine bitartrate, which can effectively solve the problems in the background technology.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is:

[0006] An intelligent extraction method for meta-hydroxylamine bitartrate comprises the following steps:

[0007] Setting material delivery parameters and cooperating with the first monitoring device to inject solution into the crystallization tank, setting product export parameters and cooperating with the second monitoring device to export crystals to the collection box, setting container pressure parameters and cooperating with the third monitoring device to adjust the pressure value in the crystallization tank;

[0008] The control unit controls the feed pipe to inject the solution into the crystallization tank to the set value of the material delivery parameter based on the collected data of the first monitoring device;

[0009] The internal pressure of the crystallization tank after the solution is injected is adjusted to the set value of the container pressure parameter by a pressure regulating device;

[0010] The solution in the crystallization tank is heated by a heating device, and the steam is discharged from the crystallization tank by a blower;

[0011] The solution near the discharge pipe is cooled and crystallized by a cooling device. When the weight of the crystals reaches the set value of the product export parameter, the control unit controls the discharge pipe to discharge the precipitated crystals into the collection box.

[0012] Further, the blower and the feed pipe are both located at the top of the crystallization tank, the heating device is located in the middle of the crystallization tank, and the cooling device and the discharge pipe are both located at the bottom of the crystallization tank;

[0013] The control unit starts and stops the solution injection by controlling a first switch device provided in the crystallization tank corresponding to the outlet of the feed pipe;

[0014] The control unit controls the second switch device in the discharge pipe to discharge the crystals accumulated in the discharge pipe and introduce them into the collection box.

[0015] Furthermore, the first monitoring device includes a liquid level sensor disposed in the crystallization tank, and the setting value of the material delivery parameter is greater than the installation height value of the heating device;

[0016] The second monitoring device includes a weighing sensor corresponding to the second switch device, which is used to detect the weight of the crystals accumulated in the discharge pipe;

[0017] The third monitoring device includes a pressure sensor disposed in the crystallization tank, which cooperates with the pressure regulating device to adjust the interior of the crystallization tank to a low pressure environment.

[0018] Furthermore, the control unit sets a warning liquid level value, a warning weight value and a warning pressure value respectively based on the first monitoring device, the second monitoring device and the third monitoring device;

[0019] When any feedback data from the first monitoring device, the second monitoring device and the third monitoring device exceeds the warning liquid level value, the warning weight value or the warning pressure value, the control unit triggers the warning device.

[0020] An intelligent extraction device for meta-hydroxylamine bitartrate, using the above-mentioned intelligent extraction method, comprises a crystallizer and a feed pipe, a discharge pipe, a blower and a pressure regulating device arranged thereon, wherein the feed pipe and the blower are both arranged at the top of the crystallizer, and the discharge pipe and the pressure regulating device are both arranged at the bottom of the crystallizer;

[0021] A first switch device is provided at the outlet of the feed pipe, and the liquid level value and the pressure value in the crystallization tank are respectively monitored by the first monitoring device and the second monitoring device. A second switch device is provided in the discharge pipe, and a third monitoring device is provided corresponding to the second switch device, for monitoring the weight value of the crystals in the discharge pipe;

[0022] A heating device is arranged in the middle of the crystallizer, and a cooling device is arranged at the bottom of the crystallizer near the discharge pipe. The discharge pipe is arranged vertically and communicated with a collecting box located below the crystallizer.

[0023] Further, the pressure regulating device includes a piston seat, a compression spring and a lifting mechanism, wherein the piston seat is arranged at the bottom of the crystallization tank and can move in the vertical direction, the lifting mechanism is located below the piston seat and is connected to the piston seat through the compression spring, the piston seat is located at one side inside the crystallization tank and is provided with a conical groove, and one end of the discharge pipe is arranged at the bottom of the conical groove;

[0024] The lifting mechanism includes a fixed seat, a screw rod and a driving assembly arranged thereon, the fixed seat is fixedly connected to the crystallization tank, the screw rod is vertically arranged and the top end of the screw rod is connected to the compression spring, the screw rod is threadedly connected to the fixed seat and driven to rotate by the driving assembly, and a locking structure is arranged between the driving assembly and the fixed seat.

[0025] Further, the fixing seat includes a first fixing plate and a second fixing plate arranged in parallel, the driving assembly includes a sleeve and a rotating seat sleeved thereon, the screw is threadedly connected to the first fixing plate, and the sleeve is rotatably connected to the second fixing plate through a shaft sleeve arranged at one end thereof;

[0026] A slide groove is provided on the screw rod along its length direction, a slider is provided on the inner wall of the sleeve corresponding to the slide groove, the sleeve is slidably connected with the slide groove through the slider, the rotating seat rotates coaxially with the sleeve, and is slidably connected with the limiting groove of the side wall of the sleeve through its upper limit ring;

[0027] The rotating seat is also connected to the sleeve through a leaf spring, and abuts against the second fixed plate under the action of the leaf spring. The locking structure includes a clamping block arranged on the rotating seat, and a clamping slot is opened on the second fixed plate. The clamping block and the clamping slot are both correspondingly arranged in multiple numbers along the circumferential direction.

[0028] Furthermore, the discharge pipe comprises a first tube body, a second tube body and a third tube body, one end of the first tube body and the third tube body are respectively fixedly connected to the piston seat and the collecting box, and the other end is respectively slidably connected to the two ends of the second tube body;

[0029] The second switch device comprises a disc arranged in the second tube body, the disc is adapted to the inner diameter of the second tube body, and is driven by the first motor to flip along the horizontal axis;

[0030] The second monitoring device includes a weighing scale fixed to the bottom surface of the piston seat, a detection head of the weighing scale is connected to the second tube body via a connecting plate, and the first motor is arranged on the connecting plate.

[0031] Furthermore, the material collection box is connected to the crystallization tank through a constant pressure pipe, the constant pressure pipe and the discharge pipe are both connected to the top surface of the material collection box, and a movable baffle is provided on the inner wall of the top of the material collection box corresponding to the constant pressure pipe and the discharge pipe;

[0032] A filter plate is arranged inside the material collection box, a door plate is arranged on the side of the material collection box, the filter plate is arranged obliquely corresponding to the door plate, and a drainage pipe is arranged at the bottom of the material collection box.

[0033] Further, the blower includes a housing and a rotating disk arranged therein, the housing is provided with an air intake pipe and an air exhaust pipe, the rotating disk is driven to rotate by a second motor, a plurality of blades are arranged along the circumference of the rotating disk, the blades are all slidably connected to the rotating disk and can extend or retract to the surface of the rotating disk in its radial direction;

[0034] The shell comprises a first arc surface and a second arc surface which are arranged relatively between the air intake pipe and the air exhaust pipe, the first arc surface covers the outer ring of the rotating disk, and the second arc surface has a diameter larger than the first arc surface;

[0035] A first inclined surface and a second inclined surface are respectively arranged in the shell near the air intake pipe and the air exhaust pipe and corresponding to the fan blades. The first inclined surface and the second inclined surface are respectively used for the transition of extending or retracting the fan blades.

[0036] The beneficial effects of the present invention are:

[0037] The present invention realizes the precipitation of crystals from the solution by physical means. During the extraction process, a low pressure state is maintained in the crystallization tank by a pressure regulating device, which can reduce the distillation temperature of the solution. The necessary heat energy is provided to the solution by a heating device to promote low-temperature distillation, and low-temperature distillation can further promote the cooling and precipitation of crystals.

[0038] By controlling the continuous crystallization production process of the intelligent extraction equipment, the differences between batches are reduced, the stability of product quality is ensured, and key parameters such as liquid level, pressure and crystal weight are monitored in real time during the production process to ensure accurate control of the production process; abnormal situations are discovered and handled in a timely manner through the early warning mechanism, reducing production risks. The intelligent extraction equipment realizes the automation and intelligence of the production process by integrating an adaptive control system, improving production efficiency. The automated production process reduces manual intervention, reduces production costs and operational risks. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0040] Figure 1 The figure is a schematic flow chart of the intelligent extraction method of meta-hydroxylamine bitartrate in the present invention;

[0041] Figure 2 It is a structural schematic diagram of the intelligent extraction device in the present invention;

[0042] Figure 3 It is a schematic diagram of the cross-sectional structure of the intelligent extraction device in the present invention;

[0043] Figure 4 It is a structural schematic diagram of the pressure regulating device in the present invention;

[0044] Figure 5 It is a structural schematic diagram of the lifting mechanism in the present invention;

[0045] Figure 6 for Figure 5 A magnified view of the local structure at point A in the middle;

[0046] Figure 7 It is a schematic cross-sectional structure diagram of the pressure regulating device in the present invention;

[0047] Figure 8 It is a schematic diagram of the internal structure of the aggregate box in the present invention;

[0048] Fig. 9 It is a schematic diagram of the internal structure of the blower in the present invention.

[0049] Figure numerals: 1, crystallization tank; 11, feed pipe; 12, discharge pipe; 121, first tube body; 122, second tube body; 123, third tube body; 13, first switch device; 14, second switch device; 141, disc; 142, first motor; 21, first monitoring device; 211, liquid level sensor; 22, second monitoring device; 221, weighing scale; 222, connecting plate; 23, third monitoring device; 231, pressure sensor; 3, pressure regulating device; 31, piston seat; 311, conical groove; 32, compression spring; 33, lifting mechanism; 34, fixed seat; 341, first fixed plate; 342, second fixed plate; 342a, slot; 35, screw Rod; 351, slide; 36, drive assembly; 361, sleeve; 361a, slider; 361b, limit slot slide; 361c, sleeve; 362, rotating seat; 362a, limit ring; 362b, block; 363, locking structure; 363a, leaf spring; 4, blower; 41, shell; 411, first arc surface; 412, second arc surface; 413, first inclined surface; 414, second inclined surface; 42, suction pipe; 43, exhaust pipe; 44, turntable; 441, fan blade; 45, second motor; 5, heating device; 6, cooling device; 7, collection box; 71, constant pressure pipe; 72, movable baffle; 73, filter plate; 74, door panel; 75, drain pipe. DETAILED DESCRIPTION

[0050] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0051] It should be noted that when an element is referred to as being "fixed to" another element, it may be directly on the other element or there may be a central element. When an element is considered to be "connected to" another element, it may be directly connected to the other element or there may be a central element at the same time. The terms "vertical", "horizontal", "left", "right" and similar expressions used herein are for illustrative purposes only and do not represent the only implementation method.

[0052] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used herein in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more related listed items.

[0053] The present invention discloses an intelligent extraction method for meta-hydroxylamine bitartrate, which is used in conjunction with production equipment with an integrated adaptive control system to achieve efficient and continuous crystallization production of meta-hydroxylamine bitartrate. Figure 1 As shown, the specific steps include:

[0054] Set the material delivery parameters and cooperate with the first monitoring device 21 to inject the solution into the crystallization tank 1, set the product export parameters and cooperate with the second monitoring device 22 to export the crystals to the collecting box 7, set the container pressure parameters and cooperate with the third monitoring device 23 to adjust the pressure value in the crystallization tank 1.

[0055] Based on the collected data of the first monitoring device 21, the control unit controls the feed pipe 11 to inject the solution into the crystallizer 1 to the set value of the material delivery parameter; adjusts the internal pressure of the crystallizer 1 after the solution is injected to the set value of the container pressure parameter through the pressure regulating device 3; heats the solution in the crystallizer 1 through the heating device 5, and cooperates with the blower 4 to discharge the steam from the crystallizer 1; cools and crystallizes the solution near the discharge pipe 12 through the cooling device 6, and when the crystal weight reaches the set value of the product export parameter, the control unit controls the discharge pipe 12 to discharge the precipitated crystals to the collecting box 7.

[0056] Among them, the blower 4 and the feed pipe 11 are both located at the top of the crystallization tank 1, the heating device 5 is located in the middle of the crystallization tank 1, and the cooling device 6 and the discharge pipe 12 are both located at the bottom of the crystallization tank 1; the control unit starts and stops the solution injection by controlling the first switch device 13 set at the outlet of the feed pipe 11 in the crystallization tank 1; the control unit discharges the crystals accumulated in the discharge pipe 12 and introduces them into the collecting box 7 by controlling the second switch device 14 in the discharge pipe 12.

[0057] Specifically, the first monitoring device 21 includes a liquid level sensor 211 arranged in the crystallization tank 1, and the set value of the material delivery parameter is greater than the installation height value of the heating device 5; the second monitoring device 22 includes a weighing sensor corresponding to the second switch device 14, which is used to detect the weight of the crystals accumulated in the discharge pipe 12; the third monitoring device 23 includes a pressure sensor 231 arranged in the crystallization tank 1, which cooperates with the pressure regulating device 3 to adjust the inside of the crystallization tank 1 to a low pressure environment.

[0058] Before the extraction operation, the material delivery parameters, product export parameters and container pressure parameters are first set as standard values ​​for a stable continuous crystallization production process; in the specific implementation process, the liquid level data in the tank collected by the first monitoring device 21 is compared with the material delivery parameters to determine whether to replenish the solution; the weight of the crystals precipitated in the discharge pipe 12 collected by the second monitoring device 22 is compared with the product export parameters to determine whether to discharge the crystals from the collecting box 7; the tank pressure data collected by the third monitoring device 23 is compared with the container pressure parameters to determine whether it is necessary to adjust the tank pressure through the pressure regulating device 3.

[0059] During the extraction crystallization process, a low-pressure environment is formed in the crystallization tank 1 through the pressure regulating device 3, which is beneficial to the low-temperature distillation of the solution. Specifically, a heating device 5 arranged on the crystallization tank 1 provides heat energy for the low-temperature distillation, and a blower 4 is used to discharge steam from the crystallization tank 1, which is also beneficial to maintaining the low-pressure environment in the tank, and the solution is easier to cool and crystallize after low-temperature distillation.

[0060] Furthermore, the control unit sets a warning liquid level value, a warning weight value and a warning pressure value based on the first monitoring device 21, the second monitoring device 22 and the third monitoring device 23 respectively; when any feedback data from the first monitoring device 21, the second monitoring device 22 and the third monitoring device 23 exceeds the warning liquid level value, the warning weight value or the warning pressure value, the control unit triggers the warning device.

[0061] In the present invention, material delivery parameters, product export parameters and container pressure parameters are set, and real-time monitoring is performed in conjunction with the liquid level sensor 211, the weighing sensor and the pressure sensor 231 respectively. During the crystallization extraction process, the solution is heated by the heating device 5, and low-temperature distillation helps the cooling and crystallization process of the solution; the cooling device 6 is located at the bottom of the crystallization tank 1, and cools and crystallizes the solution near the discharge pipe 12, so that the crystals precipitated in the solution are accumulated in the discharge pipe 12.

[0062] In the specific implementation process; the control unit controls the feed pipe 11 to inject the solution into the crystallizer 1 based on the data of the liquid level sensor 211. When the liquid level reaches the set value, the first switch device 13 is driven to close the feed pipe 11. If the first switch device 13 fails, the liquid level exceeds the warning value, and the warning device is triggered. The pressure regulating device 3 adjusts the pressure in the crystallizer 1 to the set value according to the data of the pressure sensor 231. The blower 4 is located at the top of the crystallizer 1 to discharge steam and maintain a low-pressure environment. When the pressure abnormally rises to the warning value, the warning device is triggered. When the weight of the crystals in the discharge pipe 12 reaches the set value, the control unit drives the second switch device 14 to open the discharge pipe 12, so that the crystals are discharged into the collection box 7 for the convenience of the operator to take out; if the second switch device 14 fails, the weight of the crystals fed back to the control unit exceeds the warning value, and the warning device is triggered.

[0063] The intelligent extraction method for meta-hydroxylamine bitartrate disclosed in the present invention realizes automatic adjustment and control of the production process through real-time monitoring and feedback mechanism, ensures the continuity of crystallization and improves the crystallization efficiency. In the extraction method, the stability of continuous production is achieved by accurately controlling key parameters such as liquid level, pressure and crystal weight, avoiding the problem of large product quality differences in batch operation; and the automated and intelligent production process is realized through adaptive control program to reduce manual intervention and waiting time, thereby improving production efficiency. Real-time monitoring and fault warning mechanism in the production process can timely discover and deal with safety hazards, ensuring the safety of the production process.

[0064] like Figures 2 to 9 The present invention further discloses an intelligent extraction device for meta-hydroxylamine bitartrate, which adopts the above-mentioned intelligent extraction method, including a crystallizer 1 and a feed pipe 11, a discharge pipe 12, a blower 4 and a pressure regulating device 3 arranged thereon, wherein the feed pipe 11 and the blower 4 are both arranged at the top of the crystallizer 1, and the discharge pipe 12 and the pressure regulating device 3 are both arranged at the bottom of the crystallizer 1; a first switch device 13 is arranged at the outlet of the feed pipe 11, and the liquid level value and the pressure value in the crystallizer 1 are respectively monitored by the first monitoring device 21 and the second monitoring device 22, a second switch device 14 is arranged in the discharge pipe 12, and a third monitoring device 23 is arranged corresponding to the second switch device 14, which is used to monitor the crystal weight value in the discharge pipe 12; a heating device 5 is arranged in the middle position of the crystallizer 1, and a cooling device 6 is arranged at the bottom of the crystallizer 1 near the discharge pipe 12, and the discharge pipe 12 is vertically arranged and communicated with a collecting box 7 located below the crystallizer 1.

[0065] The crystallizer 1, as the core reaction vessel of the intelligent extraction equipment, realizes the precipitation of crystals from the solution by physical means; during the extraction process, the pressure regulating device 3 is used to maintain the low pressure state in the crystallizer 1, which can reduce the distillation temperature of the solution, and the heating device 5 provides the necessary heat energy for the solution to promote low-temperature distillation, and low-temperature distillation can further promote the cooling and precipitation of crystals. Specifically, the liquid level in the crystallizer 1 is monitored by the first monitoring device 21 (i.e., the liquid level sensor 211), and the opening and closing of the feed pipe 11 is controlled in cooperation with the first switch device 13 to ensure the accuracy of the timing and amount of material delivery; the pressure in the crystallizer 1 is monitored by the second monitoring device 22 (i.e., the pressure sensor 231), and the pressure regulating device 3 is coordinated to maintain the low-pressure environment in the tank, which is conducive to the low-temperature distillation process; the weight of the crystals in the discharge pipe 12 is monitored by the third monitoring device 23 (i.e., the weighing sensor), and the crystals are regularly derived in cooperation with the second switch device 14, wherein the discharge pipe 12 is vertically arranged to facilitate the natural discharge of the crystals under the influence of gravity, reducing the risk of blockage.

[0066] The present invention reduces the difference between batches by controlling the continuous crystallization production process of the intelligent extraction equipment, ensures the stability of product quality, monitors key parameters such as liquid level, pressure and crystal weight in real time during the production process, ensures accurate control of the production process; and timely discovers and handles abnormal situations through an early warning mechanism, thereby reducing production risks. The intelligent extraction equipment realizes the automation and intelligence of the production process by integrating an adaptive control system, and improves production efficiency. The automated production process reduces manual intervention, reduces production costs and operational risks.

[0067] In this embodiment, if Figure 3 and Figure 4 The pressure regulating device 3 includes a piston seat 31, a compression spring 32 and a lifting mechanism 33. The piston seat 31 is arranged at the bottom of the crystallization tank 1 and can move in the vertical direction. The lifting mechanism 33 is located below the piston seat 31 and is connected to the piston seat 31 through the compression spring 32. The piston seat 31 is located on one side inside the crystallization tank 1 and is provided with a tapered groove 311. One end of the discharge pipe 12 is arranged at the bottom of the tapered groove 311; the lifting mechanism 33 includes a fixed seat 34 and a screw 35 and a driving assembly 36 arranged thereon. The fixed seat 34 is fixedly connected to the crystallization tank 1, the screw 35 is vertically arranged and its top end is connected to the compression spring 32, the screw 35 is screwed to the fixed seat 34 and driven to rotate by the driving assembly 36, and a locking structure 363 is arranged between the driving assembly 36 and the fixed seat 34.

[0068] When the pressure in the crystallizer 1 needs to be adjusted, the driving assembly 36 is started to drive the screw 35 to rotate; at this time, since the screw 35 is screwed to the fixed seat 34, the rotation of the screw 35 will be converted into vertical displacement and transmitted to the piston seat 31 through the compression spring 32. The movement of the piston seat 31 in the vertical direction will change the volume inside the crystallizer 1, thereby adjusting the pressure inside the tank; specifically, by moving the piston seat 31 downward, the volume inside the crystallizer 1 is increased, the pressure is reduced, and the piston seat 31 will also have a tendency to move downward under the action of the gravity of the solution in the crystallizer 1; after the adjustment is completed, the position of the screw 35 is locked by the locking structure 363 to ensure the stability after the pressure adjustment.

[0069] Precise control of the pressure in the crystallization tank 1 by the driving component 36 helps to optimize the crystallization process, improve the crystallization speed and crystallization quality, and thus improve production efficiency; the setting of the locking structure 363 ensures the stability of the pressure after adjustment, reducing fluctuations and uncertainties in the production process.

[0070] In this embodiment, see further Figures 5 to 7As shown, the fixing seat 34 includes a first fixing plate 341 and a second fixing plate 342 arranged in parallel, the driving assembly 36 includes a sleeve 361 and a rotating seat 362 sleeved thereon, the screw 35 is threadedly connected to the first fixing plate 341, and the sleeve 361 is rotatably connected to the second fixing plate 342 through a shaft sleeve 361c arranged at one end thereof; a slide groove 351 is opened on the screw 35 along its length direction, and a slider 361a is arranged on the inner wall of the sleeve 361 corresponding to the slide groove 351, and the sleeve 361 is connected to the slide groove 351 through the slider 361a. The rotating seat 362 is slidingly connected to the sleeve 361 and coaxially rotates, and is slidably connected to the limiting groove 361b on the side wall of the sleeve 361 through its upper limit ring 362a; the rotating seat 362 is also connected to the sleeve 361 through a leaf spring 363a, and abuts against the second fixed plate 342 under the action of the leaf spring 363a, and the locking structure 363 includes a block 362b arranged on the rotating seat 362, and a slot 342a is opened on the second fixed plate 342, and there are multiple corresponding blocks 362b and slots 342a along the circumferential direction.

[0071] In the specific implementation process, the rotating seat is first pulled downward to release the locking state of the block 362b and the slot 342a, and the rotating seat 362 is driven to rotate by external power, and the rotating seat 362 drives the sleeve 361 to rotate together; because the slider 361a on the inner wall of the sleeve 361 cooperates with the slide groove 351 on the screw 35, the rotation of the sleeve 361 will be converted into the axial movement of the screw 35. When the required pressure is reached, the rotating seat 362 is rotated to make the block 362b snap into the slot 342a, and the leaf spring 363a maintains the abutment state of the rotating seat 362 and the second fixed plate 342, ensuring the reliability of the mutual locking between the block 362b and the slot 342a.

[0072] Among them, the parallel arranged first fixed plate 341 and the second fixed plate 342 provide a stable supporting foundation for the driving assembly 36 and the screw 35. The sleeve 361 is rotatably connected to the second fixed plate 342 through the shaft sleeve 361c, which provides guidance and support for the rotation of the screw 35. The rotating seat is slidably connected to the limiting groove 361b on the side wall of the sleeve 361 through the limiting ring 362a, which facilitates the locking operation of the rotating seat and also ensures the stability of the rotating seat 362 during the rotation process; the leaf spring 363a not only provides the elastic force for the rotating seat 362 to reset after adjustment, but also ensures that the rotating seat 362 can remain in a locked state when not subject to external force, thereby preventing the screw 35 from moving under non-operating conditions.

[0073] In this embodiment, if Figure 5 and Figure 8As shown, the discharge pipe 12 includes a first tube body 121, a second tube body 122 and a third tube body 123, one end of the first tube body 121 and the third tube body 123 are respectively fixedly connected to the piston seat 31 and the collecting box 7, and the other ends are respectively slidably connected to the two ends of the second tube body 122; the second switch device 14 includes a disc 141 arranged in the second tube body 122, the disc 141 is adapted to the inner diameter of the second tube body 122, and is driven to flip along the horizontal axis by the first motor 142; the second monitoring device 22 includes a weighing scale 221 fixed on the bottom surface of the piston seat 31, the detection head of the weighing scale 221 is connected to the second tube body 122 through a connecting plate 222, and the first motor 142 is arranged on the connecting plate 222.

[0074] The crystals are accumulated in the discharge pipe 12 and the weight is borne by the disc 141. The weighing scale 221 monitors the weight of the material in the discharge pipe 12 in real time and feeds the data back to the control system. When the preset discharge amount is reached, the first motor 142 drives the disc 141 to flip to a position parallel to the axis of the second tube body 122, and the discharge pipe 12 is opened, so that the crystals flow into the collection box 7 along the discharge pipe 12 under the action of gravity.

[0075] Among them, the discharge pipe 12 adopts a three-section design, and the second tube body 122 is slidably connected to the first tube body 121 and the third tube body 123 as the middle section, so as to facilitate the adjustment of the overall length of the discharge pipe 12. The second tube body 122 is connected to the detection head of the weighing scale 221 through the connecting plate 222. When the disc 141 arranged in the second tube body 122 carries the crystallization, the second tube body 122 drives the inner disc 141 to move downward and the weighing scale 221 reads the weight data on the disc 141.

[0076] In this embodiment, if Figure 8 As shown, the aggregate box 7 is connected to the crystallization tank 1 through a constant pressure tube 71, the constant pressure tube 71 and the discharge pipe 12 are both connected to the top surface of the aggregate box 7, and a movable baffle 72 is provided on the inner wall of the top of the aggregate box 7 corresponding to the constant pressure tube 71 and the discharge pipe 12; a filter plate 73 is provided inside the aggregate box 7, a door plate 74 is provided on the side of the aggregate box 7, the filter plate 73 is inclined corresponding to the door plate 74, and a drainage pipe 75 is provided at the bottom of the aggregate box 7.

[0077] The constant pressure tube 71 is connected to the crystallization tank 1 to ensure that the pressure in the collection box 7 is consistent with the pressure in the crystallization tank 1, thereby preventing the crystals in the discharge pipe 12 from being unable to flow normally to the collection box 7 after the second switch device 14 is opened due to the pressure difference; when the crystals in the collection box 7 need to be taken out, the constant pressure tube 71 and the discharge pipe 12 are first blocked by the movable baffle 72, and the filtered liquid is then discharged through the drain pipe 75, and finally the door panel 74 is opened to clean or replace the filter plate 73, and the crystals thereon are taken out at the same time.

[0078] In this embodiment, if Fig. 9As shown, the blower 4 includes a shell 41 and a turntable 44 arranged therein, an air intake pipe 42 and an air exhaust pipe 43 are arranged on the shell 41, the turntable 44 is driven to rotate by a second motor 45, and a plurality of blades 441 are arranged along the circumference of the turntable 44, the blades 441 are all slidably connected with the turntable 44 and can be extended or retracted along the radial direction of the turntable 44 surface; the shell 41 includes a first arc surface 411 and a second arc surface 412 which are relatively arranged between the air intake pipe 42 and the air exhaust pipe 43, the first arc surface 411 is covered on the outer ring of the turntable 44, and the diameter of the second arc surface 412 is larger than the first arc surface 411; a first inclined surface 413 and a second inclined surface 414 are respectively arranged in the shell 41 near the air intake pipe 42 and the air exhaust pipe 43, and corresponding to the blades 441, and the first inclined surface 413 and the second inclined surface 414 are respectively used for the transition of the blades 441 extending or retracting.

[0079] In the specific implementation process, the second motor 45 drives the turntable 44 to rotate, and the fan blade 441 on the turntable 44 retreats to the inside of the turntable 44 in the space of the housing 41 located at the first arc surface 411, and the fan blade 441 extends out of the turntable 44 surface in the space of the housing 41 located at the second arc surface 412 and slides along the inner wall of the second arc surface 412. When the fan blade 441 located in the first arc surface 411 moves to the first inclined surface 413, it gradually extends to abut against the inner wall of the second arc surface 412. At this time, as the turntable 44 rotates, the space between the fan blade 441 and the first inclined surface 413 increases, so that the suction pipe 42 extracts gas from the crystallization tank 1, until the fan blade 441 moves along the second arc surface 412 to the second inclined surface 414 and discharges the extracted gas from the exhaust pipe 43. In this cycle, as the fan blade 441 periodically extends and retreats between the first arc surface 411 and the second arc surface 412, continuous suction, transportation and discharge of gas are achieved. By adjusting the rotation speed of the turntable 44, the air volume and air pressure of the blower 4 can be flexibly adjusted to meet the needs under different working conditions.

[0080] Those skilled in the art should understand that the present invention is not limited to the above embodiments, and the above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, and these changes and improvements fall within the scope of the present invention to be protected. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. An intelligent extraction method for meta-hydroxylamine bitartrate, characterized in that: The following steps are involved: Setting material delivery parameters and cooperating with the first monitoring device to inject solution into the crystallization tank, setting product export parameters and cooperating with the second monitoring device to export crystals to the collection box, setting container pressure parameters and cooperating with the third monitoring device to adjust the pressure value in the crystallization tank; The control unit controls the feed pipe to inject the solution into the crystallization tank to the set value of the material delivery parameter based on the collected data of the first monitoring device; The internal pressure of the crystallization tank after the solution is injected is adjusted to the set value of the container pressure parameter by a pressure regulating device; The solution in the crystallization tank is heated by a heating device, and the steam is discharged from the crystallization tank by a blower; The solution near the discharge pipe is cooled and crystallized by a cooling device. When the weight of the crystals reaches the set value of the product export parameter, the control unit controls the discharge pipe to discharge the precipitated crystals into the collection box.

2. The intelligent extraction method for meta-hydroxylamine bitartrate according to claim 1, characterized in that: The blower and the feed pipe are both located at the top of the crystallizer, the heating device is located in the middle of the crystallizer, and the cooling device and the discharge pipe are both located at the bottom of the crystallizer; The control unit starts and stops the solution injection by controlling a first switch device provided in the crystallization tank corresponding to the outlet of the feed pipe; The control unit controls the second switch device in the discharge pipe to discharge the crystals accumulated in the discharge pipe and introduce them into the collection box.

3. The intelligent extraction method for meta-hydroxylamine bitartrate according to claim 2, characterized in that: The first monitoring device includes a liquid level sensor disposed in the crystallization tank, and the setting value of the material delivery parameter is greater than the installation height value of the heating device; The second monitoring device includes a weighing sensor corresponding to the second switch device, which is used to detect the weight of the crystals accumulated in the discharge pipe; The third monitoring device includes a pressure sensor disposed in the crystallization tank, which cooperates with the pressure regulating device to adjust the interior of the crystallization tank to a low pressure environment.

4. The intelligent extraction method for meta-hydroxylamine bitartrate according to claim 3, characterized in that: The control unit is respectively set with a warning liquid level value, a warning weight value and a warning pressure value based on the first monitoring device, the second monitoring device and the third monitoring device; When any feedback data from the first monitoring device, the second monitoring device and the third monitoring device exceeds the warning liquid level value, the warning weight value or the warning pressure value, the control unit triggers the warning device.

5. An intelligent extraction device for meta-hydroxylamine bitartrate, characterized in that: The intelligent extraction method according to any one of claims 1 to 4 above comprises a crystallization tank and a feed pipe, a discharge pipe, a blower and a pressure regulating device arranged thereon, wherein the feed pipe and the blower are both arranged at the top of the crystallization tank, and the discharge pipe and the pressure regulating device are both arranged at the bottom of the crystallization tank; A first switch device is provided at the outlet of the feed pipe, and the liquid level value and the pressure value in the crystallization tank are respectively monitored by the first monitoring device and the second monitoring device. A second switch device is provided in the discharge pipe, and a third monitoring device is provided corresponding to the second switch device, for monitoring the weight value of the crystals in the discharge pipe; A heating device is arranged in the middle of the crystallizer, and a cooling device is arranged at the bottom of the crystallizer near the discharge pipe. The discharge pipe is arranged vertically and communicated with a collecting box located below the crystallizer.

6. The intelligent extraction equipment for meta-hydroxylamine bitartrate according to claim 5, characterized in that: The pressure regulating device comprises a piston seat, a compression spring and a lifting mechanism, wherein the piston seat is arranged at the bottom of the crystallization tank and can move in the vertical direction, the lifting mechanism is located below the piston seat and is connected to the piston seat through the compression spring, the piston seat is located at one side inside the crystallization tank and is provided with a conical groove, and one end of the discharge pipe is arranged at the bottom of the conical groove; The lifting mechanism includes a fixed seat, a screw rod and a driving assembly arranged thereon, the fixed seat is fixedly connected to the crystallization tank, the screw rod is vertically arranged and the top end of the screw rod is connected to the compression spring, the screw rod is threadedly connected to the fixed seat and driven to rotate by the driving assembly, and a locking structure is arranged between the driving assembly and the fixed seat.

7. The intelligent extraction equipment for meta-hydroxylamine bitartrate according to claim 6, characterized in that: The fixing seat comprises a first fixing plate and a second fixing plate arranged in parallel, the driving assembly comprises a sleeve and a rotating seat sleeved thereon, the screw is threadedly connected to the first fixing plate, and the sleeve is rotatably connected to the second fixing plate via a shaft sleeve arranged at one end thereof; A slide groove is provided on the screw rod along its length direction, a slider is provided on the inner wall of the sleeve corresponding to the slide groove, the sleeve is slidably connected with the slide groove through the slider, the rotating seat rotates coaxially with the sleeve, and is slidably connected with the limiting groove of the side wall of the sleeve through its upper limit ring; The rotating seat is also connected to the sleeve through a leaf spring, and abuts against the second fixed plate under the action of the leaf spring. The locking structure includes a clamping block arranged on the rotating seat, and a clamping slot is opened on the second fixed plate. The clamping block and the clamping slot are both correspondingly arranged in multiple numbers along the circumferential direction.

8. The intelligent extraction equipment for meta-hydroxylamine bitartrate according to claim 6, characterized in that: The discharge pipe comprises a first tube body, a second tube body and a third tube body, one end of the first tube body and the third tube body are respectively fixedly connected to the piston seat and the collecting box, and the other end is respectively slidably connected to the two ends of the second tube body; The second switch device comprises a disc arranged in the second tube body, the disc is adapted to the inner diameter of the second tube body, and is driven by the first motor to flip along the horizontal axis; The second monitoring device includes a weighing scale fixed to the bottom surface of the piston seat, a detection head of the weighing scale is connected to the second tube body via a connecting plate, and the first motor is arranged on the connecting plate.

9. The intelligent extraction equipment for meta-hydroxylamine bitartrate according to claim 5, characterized in that: The material collection box is connected to the crystallization tank through a constant pressure pipe, the constant pressure pipe and the discharge pipe are both connected to the top surface of the material collection box, and a movable baffle is provided on the inner wall of the top of the material collection box corresponding to the constant pressure pipe and the discharge pipe; A filter plate is arranged inside the material collection box, a door plate is arranged on the side of the material collection box, the filter plate is arranged obliquely corresponding to the door plate, and a drainage pipe is arranged at the bottom of the material collection box.

10. The intelligent extraction equipment for meta-hydroxylamine bitartrate according to claim 5, characterized in that: The blower comprises a housing and a rotating disk arranged therein, an air intake pipe and an air discharge pipe are arranged on the housing, the rotating disk is driven to rotate by a second motor, a plurality of blades are arranged along the circumference of the rotating disk, the blades are all slidably connected to the rotating disk and can extend or retract from the rotating disk surface in the radial direction thereof; The shell comprises a first arc surface and a second arc surface which are arranged relatively between the air intake pipe and the air exhaust pipe, the first arc surface covers the outer ring of the rotating disk, and the second arc surface has a diameter larger than the first arc surface; A first inclined surface and a second inclined surface are respectively arranged in the shell near the air intake pipe and the air exhaust pipe and corresponding to the fan blades. The first inclined surface and the second inclined surface are respectively used for the transition of extending or retracting the fan blades.

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