Gradient cooling crystallization device for alcohol precipitation process of belladonna extract

Abstract

The invention relates to the technical field of extraction of alkaloid drugs, in particular to a gradient cooling crystallization device for an alcohol precipitation process of belladonna extractum, which comprises a crystallization tank, a precipitation tank and a recovery tank which are sequentially stacked from top to bottom, drain valves are respectively arranged at the bottoms of the crystallization tank, the precipitation tank and the recovery tank, and a top cover is in threaded connection with a tank opening at the top end of the crystallization tank. A dynamic stirring mechanism is arranged at the bottom end of the top cover, and a temperature sensor, an electrical bar and a liquid level sensor are arranged at the middle end of the inner wall of one side of the crystallizing tank; on the basis of efficiently mixing materials, the liquid level change in the tank is monitored through the liquid level sensor, and the position and stirring strength of the stirrer are dynamically adjusted, so that crystals are effectively prevented from being adhered and agglomerated at the bottom of the tank body, the overall crystallization efficiency and quality are improved, and meanwhile, by combining the feedback temperature of the temperature sensor, the crystallization efficiency is improved. And gradient cooling adjustment is performed on the tank body, so that the crystallization condition is further optimized, and the purity and quality of a final crystallized product are improved.

Description

Technical Field

[0001] The invention relates to the technical field of alkaloid drug extraction, in particular to a gradient cooling crystallization device for an alcohol precipitation process of a belladonna extract. Background Art

[0002] Belladonna extract is a key raw material for alkaloid drugs. The alcohol precipitation and crystallization steps in the production process play a vital role in the purity and yield of the product. For details, please refer to the stirred crystallization tank in the CN213555461U patent.

[0003] Common clean mixing tanks can achieve clean mixing of materials. However, for the alcohol precipitation and crystallization process of belladonna extract, since the fixed blades cannot adjust the stirring intensity according to the liquid level changes, insufficient mixing intensity is likely to occur in the low liquid level area, which will cause a large number of crystals to adhere to the bottom of the tank and cause crystal agglomeration, resulting in low crystallization efficiency and reduced crystal quality. Summary of the Invention

[0004] The purpose of the present invention is to monitor the changes in the liquid level in the tank through a liquid level sensor on the basis of efficient mixing of materials, and dynamically adjust the position and stirring intensity of the agitator to effectively avoid the adhesion and agglomeration of crystals at the bottom of the tank, thereby improving the overall crystallization efficiency and quality. At the same time, combined with the feedback temperature of the temperature sensor, the tank is gradually cooled to further optimize the crystallization conditions and improve the purity and quality of the final crystallized product.

[0005] The object of the present invention can be achieved by the following technical scheme: a gradient cooling crystallization device for the alcohol precipitation process of belladonna extract, comprising a crystallization tank, a precipitation tank and a recovery tank stacked in sequence from top to bottom, and a drain valve is provided at the bottom of each of the three tanks, a top cover is threadedly connected to the top filling port of the crystallization tank, and a dynamic mixing mechanism is provided at the bottom end of the top cover, a temperature sensor, an electric heating rod and a liquid level sensor are provided at the middle end of the inner wall of one side of the crystallization tank, and a feeding pipe is provided at the inner wall of the other side of the crystallization tank, a detachable filter is provided at the top end of the precipitation tank, and a coil-type condenser is provided inside the recovery tank;

[0006] Among them, the dynamic mixing mechanism includes a single-axis motor arranged on the top surface of the crystallization tank cover, and the bottom output end of the single-axis motor is fixedly installed with a double-concave limit frame with an I-shaped cross-section, and an inner groove is opened in the center of the double-concave limit frame, and a double-axis motor is arranged at the center of the inner groove.

[0007] Furthermore, the output shafts at both ends of the dual-axis motor extend to the inner walls of the grooves on both sides of the double-concave limit frame and are fixedly installed with discs, and the two groups of discs are fixedly installed with circular shafts at the upper center position away from each other.

[0008] Furthermore, the grooves on both sides of the double-concave limit frame are slidably connected to the limit long frame at adjacent positions of the disc, and the circular shafts are slidably connected to the frame grooves of the corresponding limit long frames. Several groups of vertical frames are hinged at equal distances at the bottom end of each group of the limit long frames, and vertical card slots are provided inside the vertical frames.

[0009] Furthermore, a rectangular positioning frame is connected to the bottom center of the double-concave limit frame through a telescopic rod, and a spiral rotating rod 1 and a spiral rotating rod 2 are provided at the front and rear ends of the bottom inner wall of the positioning frame. A dual-axis motor 2 is commonly provided between the two adjacent groups of spiral rotating rods 1 and spiral rotating rods 2 near the front end of the bottom inner wall of the positioning frame, and the two adjacent groups of spiral rotating rods 1 and spiral rotating rods 2 located at the rear end of the bottom inner wall of the positioning frame are fixedly connected by a connecting rod, and the spiral rotating rod 1 and spiral rotating rod 2 are arranged in opposite thread structures.

[0010] Furthermore, the ends of the spiral rod 1 and the spiral rod 2 close to each other are respectively fixedly installed with transmission wheels, and the two adjacent groups of transmission wheels on the same side are commonly connected with a transmission belt, and the ends of the spiral rod 1 and the spiral rod 2 close to the transmission wheel are respectively movably connected with a spiral frame.

[0011] Furthermore, the two groups of spiral sleeve frames on the front and rear sides of the same side are fixedly connected with a support rod, and the support rods respectively pass through the vertical slots of the vertical frames arranged on the same side.

[0012] The present invention also provides an operating method of a gradient cooling crystallization device for the alcohol precipitation process of belladonna extract, comprising the following steps:

[0013] Step 1: During the alcohol precipitation stage, the belladonna extract and ethanol are added to the crystallization tank through the feeding tube, and then stirred and dissolved using a dynamic mixing mechanism at a constant temperature of 50°C to form a uniform solution;

[0014] Step 2: Gradient cooling stage, the temperature inside the crystallization tank is adjusted to a gradient lowering level according to the temperature feedback from the temperature sensor. In the first stage, the temperature is lowered to 30°C at 2°C / h to induce the formation of a small number of crystal nuclei; in the second stage, the temperature is lowered to 15°C at 1°C / h to promote the growth of the target component; in the third stage, the temperature is lowered to 5°C at 0.5°C / h to complete the final crystallization;

[0015] Step 3: During the crystal growth and separation phase, according to the liquid level inside the crystallizer fed back by the liquid level sensor, the dynamic mixing mechanism position is adjusted and constant temperature stirring is performed again for 1-2 hours to reduce the crystal deposition at the bottom of the crystallizer. Then, stirring is stopped and the mixed liquid is poured into a sedimentation tank for static filtration;

[0016] Step 4: In the solvent recovery stage, the mother liquor is introduced into the recovery tank, condensed by the condenser to recover ethanol and recycled.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] The present invention realizes uniform stirring of the belladonna extract solution, avoids the situation where the local concentration of the solution is too high or too low during the cooling process, and improves the crystallization efficiency and crystallization quality. At the same time, the opposite thread structures of the spiral rotating rod 1 and the spiral rotating rod 2 are set, so that the push rod can drive the spiral sleeve to move left and right on the spiral rotating rod, further realizing all-round stirring of the solution. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] To facilitate understanding by those skilled in the art, the present invention is further described below with reference to the accompanying drawings.

[0020] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0021] Figure 2 It is a side sectional view of the overall structure of the present invention;

[0022] Figure 3 This is a schematic diagram of the overall structure of the dynamic mixing mechanism of the present invention;

[0023] Figure 4 This is a cross-sectional view of the bottom of the crystallization tank of the present invention;

[0024] Figure 5 It is a cross-sectional view of a crystallization tank of the present invention;

[0025] Figure 6 It is a schematic diagram of the three-dimensional structure of the positioning frame of the present invention.

[0026] In the figure: 1. Crystallization tank; 2. Sedimentation tank; 3. Recovery tank; 4. Dynamic mixing mechanism; 41. Single-axis motor; 42. Double-concave limit frame; 43. Double-axis motor 1; 44. Disc; 45. Circular shaft; 46. Limit long frame; 47. Vertical frame; 48. Positioning frame; 49. Screw rod 1; 410. Screw rod 2; 411. Double-axis motor 2; 412. Transmission wheel; 413. Spiral sleeve frame; 414. Push rod; 5. Filter. DETAILED DESCRIPTION

[0027] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0028] Example 1: Please refer to Figure 1-Figure 5As shown, a gradient cooling crystallization device for the alcohol precipitation process of belladonna extract includes a crystallization tank 1, a precipitation tank 2, and a recovery tank 3 stacked in sequence from top to bottom, and a drain valve is provided at the bottom of each of the three tanks. A top cover is threadedly connected to the top filling port of the crystallization tank 1, and a dynamic mixing mechanism 4 is provided at the bottom of the top cover.

[0029] A temperature sensor, a heating rod, and a liquid level sensor are installed at the middle end of the inner wall of one side of the crystallizer 1. The temperature sensor model is Parker Balston PT100 ClassA, which collects and sends feedback on the temperature data inside the crystallizer 1 in real time to trigger the start and stop of the heating rod. The liquid level sensor model is Endress+Hauser Prosonic FMU30, which collects and monitors the liquid level of the crystallizer in real time.

[0030] A feeding pipe is provided on the inner wall of the other side of the crystallization tank 1, a detachable filter screen 5 is provided at the top of the precipitation tank 2, and a coil-type condenser is provided inside the recovery tank 3;

[0031] Among them, the dynamic mixing mechanism 4 includes a single-axis motor 41 arranged on the top surface of the top cover of the crystallization tank 1, and a double-concave limit frame 42 with an I-shaped cross-section is fixedly installed at the bottom output end of the single-axis motor 41, and an inner groove is provided in the center of the double-concave limit frame 42. A double-axis motor 1 43 is provided in the center of the inner groove. The output shafts at both ends of the double-axis motor 1 43 extend to the inner walls of the grooves on both sides of the double-concave limit frame 42 and are fixedly installed with discs 44. A circular shaft 45 is fixedly installed at the upper position of the center of the two sets of discs 44 away from each other.

[0032] The inner grooves on both sides of the double concave limit frame 42 and adjacent to the disc 44 are slidably connected to the limit long frame 46, and the circular shaft 45 is slidably connected to the inner grooves of the corresponding limit long frame 46. Several groups of vertical frames 47 are hinged at equal distances at the bottom end of each group of limit long frames 46, and vertical card slots are provided inside the vertical frames 47.

[0033] The feeding pipe sequentially adds belladonna extract and ethanol into the crystallizer 1 through the feeding pipe, heats the interior of the crystallizer 1 through the electric heating rod, and monitors the temperature inside the crystallizer 1 in real time through the temperature sensor and sends the temperature to the external controller. When the preset temperature reaches 50 degrees, the controller generates a stop signal to control the electric heating rod to stop heating, and then starts the single-axis motor 41 to drive the double concave limit frame 42 to rotate, and the bottom of the plurality of assembly frames 47 stirs the liquid mixture in multiple directions to stir and dissolve the liquid to form a uniform solution;

[0034] During the rotation and stirring process, according to the initial liquid level in the crystallization tank 1 fed back by the liquid level sensor and the liquid level change caused by continuous heating and evaporation, the specific adjustment process includes: the dual-axis motor 43 drives the two sets of discs 44 to rotate simultaneously, forcing the circular shaft 45 to slide inside the frame groove of the limit long frame 46 while pulling the limit long frame 46 to move up and down. The lifting and lowering of the limit long frame 46 pulls the synchronous lifting and lowering of several sets of vertical frames 47 at its bottom until the bottom end of the vertical frame 47 is inserted into the mixed liquid at a suitable height, thereby further improving the quality of solid crystallization.

[0035] At the same time, the liquid level height inside the crystallizer 1 is monitored in real time by a liquid level sensor and sent to an external controller. When the liquid level height drops to a preset value, the controller generates a control signal to immediately open the drain valve to discharge the liquid inside the crystallizer 1 into the sedimentation tank 2. The solid crystals are separated from the liquid through the filtering effect of the filter 5, and the liquid continues to flow into the recovery tank 3, and the liquid is condensed and recovered through the condenser.

[0036] Example 2: Please refer to Figure 3-Figure 6 As shown, a rectangular positioning frame 48 is connected to the bottom center of the double-concave limit frame 42 via a telescopic rod, and a spiral rotating rod 1 49 and a spiral rotating rod 2 410 are provided at the front and rear ends of the bottom inner wall of the positioning frame 48. A dual-axis motor 2 411 is provided between two adjacent groups of spiral rotating rods 1 49 and spiral rotating rods 2 410 near the front end of the bottom inner wall of the positioning frame 48. The two adjacent groups of spiral rotating rods 1 49 and spiral rotating rods 2 410 located at the rear end of the bottom inner wall of the positioning frame 48 are fixedly connected by a connecting rod, and the spiral rotating rod 1 49 and the spiral rotating rod 2 410 are arranged in opposite thread structures.

[0037] A transmission wheel 412 is fixedly installed on the ends of the spiral rotating rod 1 49 and the spiral rotating rod 2 410 close to each other, and a transmission belt is commonly connected between the two adjacent sets of transmission wheels 412 on the same side. A spiral sleeve 413 is movably connected to the ends of the spiral rotating rod 1 49 and the spiral rotating rod 2 410 close to the transmission wheel 412, and a support rod 414 is commonly fixedly connected between the two sets of spiral sleeves 413 on the same side, and the support rod 414 passes through the vertical slots of the vertical frames 47 arranged on the same side.

[0038] After the rotation and stirring is completed, the adjacent spiral rotating rods 1 49 and 2 410 are driven to rotate in the same direction by the dual-axis motor 2 411. Since the spiral rotating rods 1 49 and 2 410 adopt opposite thread structure designs, the adjacent spiral sleeves 413 on the same side will move towards each other under the action of the push rod 414.

[0039] At the same time, during the rotation of the spiral rod 1 49 and the spiral rod 2 410, the other set of spiral rods 1 49 and the spiral rod 2 410 rotate synchronously through the cooperation of the transmission wheel 412 and the transmission belt, thereby simultaneously driving the two sets of spiral sleeves 413. The two sets of spiral sleeves 413 on the same side jointly pull the same push rod 414 to move linearly. During this process, each set of push rods 414 will simultaneously press several vertical frames 47, forcing the vertical frames 47 to tilt and deflect, and the bottom ends of the vertical frames 47 will stir the materials along the bottom of the crystallization tank 1 to prevent the crystals from settling and agglomerating at the bottom.

[0040] Similarly, as the liquid level continues to decrease, the bottom end of the vertical frame 47 can be forced to contact the bottom of the crystallization tank 1 through the above-mentioned lifting method, thereby achieving dynamic adjustment.

[0041] As an embodiment of the present invention, there is also disclosed a method for operating a gradient cooling crystallization device for the alcohol precipitation process of belladonna extract, comprising the following steps:

[0042] Step 1: Alcohol precipitation stage: After belladonna extract and ethanol are added to the crystallizer 1 through the feeding pipe, the electric heating rod heats the inside of the crystallizer 1, and the temperature inside the crystallizer 1 is monitored in real time by a temperature sensor. When the preset temperature reaches 50 degrees, the electric heating rod stops heating. Under the condition of a constant temperature of 50 degrees, the double-concave limit frame 42 is driven to rotate by a single-axis motor 41, and the bottom ends of several groups of vertical frames 47 stir the liquid mixture in multiple directions. The position of the vertical frames 47 is dynamically adjusted to ensure that the bottom ends of the vertical frames 47 are inserted into the mixed liquid, and the liquid is stirred and dissolved to form a uniform solution;

[0043] Step 2: Gradient cooling stage, the temperature inside the crystallization tank 1 is adjusted to a gradient lowering level according to the temperature feedback from the temperature sensor. In the first stage, the temperature is lowered to 30°C at 2°C / h to induce the formation of a small amount of crystal nuclei; in the second stage, the temperature is lowered to 15°C at 1°C / h to promote the growth of the target component; in the third stage, the temperature is lowered to 5°C at 0.5°C / h to complete the final crystallization;

[0044] Step 3: During the crystal growth and separation phase, the position of the dynamic mixing mechanism 4 is adjusted according to the liquid level inside the crystallization tank 1 as fed back by the liquid level sensor, and constant temperature stirring is performed again for 1-2 hours. The adjacent spiral rotating rods 1 49 and 2 410 are driven to rotate in the same direction by the dual-axis motor 2 411, and the adjacent spiral sleeves 413 on the same side move in opposite directions.

[0045] At the same time, during the rotation of the spiral rotating rod 1 49 and the spiral rotating rod 2 410, through the cooperation of the transmission wheel 412 and the transmission belt, the other set of spiral rotating rods 1 49 and the spiral rotating rod 2 410 rotate synchronously, realizing the simultaneous driving of the two sets of spiral sleeve frames 413. The two sets of spiral sleeve frames 413 on the same side jointly pull the same push rod 414 to move in a straight line. During this process, each set of push rods 414 will simultaneously press a number of vertical frames 47, forcing the vertical frames 47 to tilt and deflect, and the bottom end of the vertical frame 47 is stirred along the bottom of the crystallization tank 1 to prevent the crystals from depositing and agglomerating at the bottom and reduce the situation of crystals depositing at the bottom of the crystallization tank 1. Then, the stirring is stopped, and the mixed liquid is poured into the precipitation tank 1 for static filtration;

[0046] Step 4: In the solvent recovery stage, the mother liquor is introduced into the recovery tank 3, condensed by the condenser to recover ethanol and recycled.

[0047] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to specific embodiments. Obviously, many modifications and variations are possible based on the contents of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A gradient cooling crystallization device for the alcohol precipitation process of belladonna extract, comprising a crystallization tank (1), a precipitation tank (2) and a recovery tank (3) stacked in sequence from top to bottom, and a drain valve is provided at the bottom of each of the three tanks, characterized in that: The top of the crystallizer (1) is threadedly connected to a top cover, and a dynamic mixing mechanism (4) is provided at the bottom of the top cover; a temperature sensor, an electric heating rod and a liquid level sensor are provided at the middle end of the inner wall of one side of the crystallizer (1); and a feeding pipe is provided at the inner wall of the other side of the crystallizer (1); a detachable filter screen (5) is provided at the top end of the precipitation tank (2); and a coil-type condenser is provided inside the recovery tank (3); The dynamic material mixing mechanism (4) comprises a single-axis motor (41) arranged on the top surface of the top cover of the crystallization tank (1), a double-concave limit frame (42) with an I-shaped cross-section is fixedly installed at the bottom output end of the single-axis motor (41), and an inner groove is provided at the center of the inner center of the double-concave limit frame (42), and a double-axis motor (43) is provided at the center of the inner groove.

2. The gradient cooling crystallization device for the alcohol precipitation process of belladonna extract according to claim 1, characterized in that: The output shafts at both ends of the dual-axis motor (43) extend to the inner walls of the grooves on both sides of the double-concave limit frame (42) and are fixedly mounted with discs (44). A circular shaft (45) is fixedly mounted at the upper center position of the two sets of discs (44) away from each other.

3. The gradient cooling crystallization device for the alcohol precipitation process of belladonna extract according to claim 1, characterized in that: The inner grooves on both sides of the double concave limit frame (42) and adjacent to the circular disc (44) are slidably connected to the limit long frame (46), and the circular shaft (45) is slidably connected to the inner grooves of the corresponding limit long frame (46). The bottom end of each group of the limit long frame (46) is hinged with a plurality of groups of vertical frames (47) at equal distances, and the vertical frames (47) are provided with vertical slots inside.

4. The gradient cooling crystallization device for the alcohol precipitation process of belladonna extract according to claim 1, characterized in that: The center of the bottom of the double-concave limit frame (42) is connected to a rectangular positioning frame (48) through a telescopic rod, and a spiral rotating rod 1 (49) and a spiral rotating rod 2 (410) are provided at the front and rear ends of the bottom inner wall of the positioning frame (48), and a double-axis motor 2 (411) is provided between two adjacent groups of spiral rotating rods 1 (49) and spiral rotating rods 2 (410) near the front end of the bottom inner wall of the positioning frame (48). The two adjacent groups of spiral rotating rods 1 (49) and spiral rotating rods 2 (410) located at the rear end of the bottom inner wall of the positioning frame (48) are fixedly connected by a connecting rod, and the spiral rotating rods 1 (49) and spiral rotating rods 2 (410) are provided with opposite thread structures.

5. The gradient cooling crystallization device for the alcohol precipitation process of belladonna extract according to claim 4, characterized in that: The ends of the spiral rotating rod 1 (49) and the spiral rotating rod 2 (410) close to each other are respectively fixedly mounted with a transmission wheel (412), and the two sets of transmission wheels (412) adjacent to each other on the same side are commonly sleeved with a transmission belt, and the ends of the spiral rotating rod 1 (49) and the spiral rotating rod 2 (410) close to the transmission wheel (412) are respectively movably sleeved with a spiral sleeve frame (413).

6. The gradient cooling crystallization device for the alcohol precipitation process of belladonna extract according to claim 5, characterized in that: The two groups of spiral sleeve frames (413) on the same side are fixedly connected with a support rod (414), and the support rod (414) respectively passes through the vertical slots of the vertical frames (47) arranged on the same side.

7. The method for operating a gradient cooling crystallization device for alcohol precipitation of belladonna extract according to any one of claims 1 to 6, characterized in that: The following steps are involved: Step 1: Alcohol precipitation stage, after adding belladonna extract and ethanol into the crystallization tank (1) through the feeding pipe, stirring and dissolving them by using the dynamic mixing mechanism (4) at a constant temperature of 50°C to form a uniform solution; Step 2: Gradient cooling stage, the temperature inside the crystallization tank (1) is adjusted to a gradient lowering adjustment according to the temperature feedback from the temperature sensor. In the first stage, the temperature is lowered to 30°C at 2°C / h to induce the formation of a small amount of crystal nuclei; in the second stage, the temperature is lowered to 15°C at 1°C / h to promote the growth of the target component; in the third stage, the temperature is lowered to 5°C at 0.5°C / h to complete the final crystallization; Step 3: In the crystal growth and separation stage, according to the liquid level height inside the crystallization tank (1) fed back by the liquid level sensor, the position of the dynamic mixing mechanism (4) is adjusted and constant temperature stirring is performed again for 1-2 hours to reduce the crystal deposition at the bottom of the crystallization tank (1), and then the stirring is stopped and the mixed liquid is poured into the precipitation tank (1) and allowed to stand for filtration; Step 4: In the solvent recovery stage, the mother liquor is introduced into the recovery tank (3), condensed by the condenser to recover ethanol and recycled.

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