A device for purifying thymol by melt crystallization and its use method

Abstract

The invention discloses an apparatus for purifying thymol by melt crystallization and a method for using the apparatus, comprising a reactor and a stirring device, wherein the stirring device is installed in the reactor and partially extends from the reactor, the stirring device comprises a stirring main rod which can be driven to rotate axially, the interior of the stirring main rod is penetrated up and down to form a material taking channel, the inner side wall of the material taking channel is connected to an auxiliary silk pattern plate through a connecting piece, the auxiliary silk pattern plate is rotatably connected to an adjusting ring frame, and the adjusting ring frame can move vertically, an injection piece is installed at the bottom end of the stirring main rod, the injection piece comprises a cylindrical sleeve, an injection head, a lower plug and a pressure plate, the cylindrical sleeve is upwardly connected to the material taking channel, an upper portion of the outer circumference of the injection head is provided with a discharge port, and the lower portion penetrates the bottom plate of the cylindrical sleeve, the lower plug is installed at the opening of the lower end of the injection head, the pressure plate is connected to a spring on the bottom surface of the cylindrical sleeve, and is connected to the lower plug, and when sampling the melt crystallization, the sampler can be directly used in conjunction with the rotating stirring device to perform sampling and detection on the reactor.

Description

Technical Field

[0001] The present invention relates to the technical field related to melt crystallization, and in particular to a device for purifying thymol by melt crystallization and a method for using the device. Background Art

[0002] p-Thymol (3-methyl-4-isopropylphenol), with a melting point of 112°C and a boiling point of 244°C, occurs as white, needle-shaped crystals and is an important cosmetic ingredient. With its antibacterial, antiperspirant, and deodorant properties, p-thymol is widely used in shampoo, soap, hand sanitizer, toothpaste, and other personal hygiene products and cosmetics. It is a promising alternative to older antiseptics, offering safety, low toxicity, skin-friendly properties, easy degradation, and minimal environmental impact. p-thymol is now widely adopted by major cosmetics companies, with its scope of use and usage increasing year by year. However, obtaining high-purity p-thymol remains a challenge in product development and promotion.

[0003] Separation operations are common in the chemical, food, pharmaceutical, and materials industries. Conventional separation methods include distillation, extraction, and solution crystallization. With increasing demands for purity and the emergence of difficult-to-separate systems, conventional separation methods are unable to purify and separate these systems. Melt crystallization plays a unique role in temperature-sensitive systems or when the separation system cannot tolerate the presence of solvents.

[0004] Melt crystallization is a novel chemical separation technology widely used in the refining and purification of chemical intermediates, pharmaceutical intermediates, and biochemical products. Compared with conventional chemical separation methods (absorption, distillation, extraction) and some novel separation technologies (supercritical extraction, adsorption separation, chromatography, membrane separation), this technology offers the following advantages: it can isolate high-purity products (purity of products processed by melt crystallization can reach over 99.9% or even 99.99%); it is suitable for specialized systems such as materials with similar boiling points, isomers, chiral substances, heat-sensitive substances, dilute solutions, and substances with very high boiling points; melt crystallization is generally performed at atmospheric pressure and low temperature, making it simple and safe to operate, with minimal equipment requirements, thus reducing costs and equipment investment; melt crystallization does not require drying to remove solvents, thus reducing the drying step and avoiding the increased costs, environmental pollution, and low-temperature freezing caused by solvent incorporation; and the energy consumption of melt crystallization is generally only 10%-30% of that of distillation.

[0005] In the production process of thymol synthesized from m-cresol, the crude product contains thymol, m-thymol (3-methyl-5-isopropylphenol), p-thymol, 3-methyl-2,6-diisopropylphenol and 3-methyl-4,6-diisopropylphenol. High-purity p-thymol can be purified from the crude thymol using the melt crystallization method.

[0006] When using the melt crystallization method to purify thymol, it is necessary to sample the material in the reactor after the material is melted to measure the crystallization point of the mixture and the content of thymol, so as to better control the subsequent crystallization temperature. Most of the existing technologies are to open a sampling port on the side wall of the reactor to sample the material. This sampling method not only damages the reactor, but also may affect the movement of the stirring paddle when the sampling head is inserted into the reactor for sampling; some sampling methods are to insert a sampling tube extending into the reactor from the top of the reactor, and use a vacuum extraction method to extract a small amount of material for sampling during sampling. However, due to the large depth of the reactor, a large amount of material will adhere to the inner wall of the sampling tube after sampling, which will not only cause material waste, but also the material adhered to the inner wall of the sampling tube will be mixed into the sample during the next sampling, affecting the accuracy of the test results. Summary of the Invention

[0007] In order to purify high-purity p-thymol from crude products, the present invention provides a device for purifying p-thymol by melt crystallization and a method for using the device.

[0008] In order to achieve the above object, the present invention adopts the following technical solutions:

[0009] A device for purifying thymol by melt crystallization comprises a reactor and a stirring device, wherein the stirring device is installed inside the reactor and partially extends outward from the reactor, and is characterized in that:

[0010] The stirring device includes a stirring main rod that can be driven to rotate axially. The stirring main rod has a material taking channel that runs vertically through it. The inner side wall of the material taking channel is connected to the auxiliary wire pattern plate through a connecting piece. The auxiliary wire pattern plate is rotatably connected to the adjustment ring frame, and the adjustment ring frame can move vertically.

[0011] An injection part is installed at the bottom end of the stirring main rod, and the injection part includes a cylindrical sleeve, an injection head, a lower plug and a pressure plate. The cylindrical sleeve is connected to the material collection channel, and a sampler can be placed in the material collection channel, and the sampler can fall into the cylindrical sleeve. A discharge port is opened on the upper part of the outer peripheral side of the injection head, and the lower part passes through the bottom plate of the cylindrical sleeve. The lower plug is installed at the opening at the lower end of the injection head. The pressure plate is connected to the spring of the bottom surface of the cylindrical sleeve and is connected to the lower plug.

[0012] Preferably, the sampler includes a sampling tank, a pressure piece and a sealing cover. The bottom of the sampling tank is provided with an injection channel that allows the injection head to be inserted. The sealing cover covers the upper opening of the injection channel. The pressure piece is fixed in the sampling tank and is spring-connected to the sealing cover in the vertical direction.

[0013] Preferably, the injection head is installed at the center of the bottom surface of the cylindrical sleeve, and the outer peripheral surface of the cylindrical sleeve is connected to the stirring main rod bearing.

[0014] Preferably, the adjustment ring frame has a ring guide groove, the auxiliary silk pattern plate includes a silk pattern arc plate, an outer guide rod and a guide wheel, the outer guide rod is connected to the silk pattern arc plate and extends from the material taking channel, the guide wheel is installed on the end of the outer guide rod extending to the outside and is stuck in the ring guide groove, and the width of the ring guide groove is greater than the guide wheel.

[0015] Preferably, a limiting column is further provided on the bottom surface of the cylindrical sleeve, and the limiting column extends vertically upward from the stirring main rod. After extending out of the stirring main rod, the limiting column bends downward and is connected to the top plate of the reactor.

[0016] Preferably, the outer circumference of the sampling tank has a limiting groove that allows the limiting column to be placed, and the outer circumference of the sampling tank also has a silk pattern corresponding to the silk pattern arc plate.

[0017] A method for using a device for purifying thymol by melt crystallization comprises the following steps:

[0018] S1: placing a material containing thymol, m-thymol (3-methyl-5-isopropylphenol), p-thymol, 3-methyl-2,6-diisopropylphenol and 3-methyl-4,6-diisopropylphenol into a reaction chamber, heating the reactor and starting a stirring device to melt the material;

[0019] S2: vertically insert the sampler into the material collection channel with the material injection channel facing downward and the limit groove and the limit column engaged, and the sampler presses down the pressure plate to allow part of the melted material in the reactor to enter the sampler;

[0020] S3: Lift the adjustment ring frame so that the wire arc plate is close to the sampling tank, wait for a while and then take the sampler sent by the wire arc plate to the opening on the stirring main rod;

[0021] S4: measuring the crystallization point T of the material in S3 and performing chromatographic analysis on the thymol content in the material;

[0022] S5: Cool the reactor to T+10°C and add seed crystals;

[0023] S6: Cool the reactor in a stepwise manner of 1°C / 10min to 0°C, discharge the material and centrifuge.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] 1. The melt crystallization method is used to purify thymol. Compared with conventional separation methods such as distillation, extraction, and solution crystallization, the purified product has higher purity and lower purification cost;

[0026] 2. During melt crystallization, the sampler can be directly placed in the stirring main rod. After the sampler falls into the stirring main rod and completes the sampling, it can be rotated with the silk arc plate to rise and discharge the material, thereby completing the sampling work. The reactor does not need to open a separate sampling port, and the sampling is convenient and fast, with good applicability.

[0027] 3. When sampling, the sampler will not contact the stirring paddle, which will not affect the normal operation of the stirring device, nor will it affect the melting and crystallization of the materials in the reactor.

[0028] 4. The material in the reactor is directly injected into the sampler and sent upward, which will not cause material adhesion and waste, and can also ensure that the sample taken out is pure material in the reactor, ensuring the accuracy of sample detection. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0030] Figure 1 The figure is a schematic diagram of the structure of the equipment for purifying thymol by melt crystallization according to the present invention.

[0031] Figure 2 for Figure 1 Enlarged structural diagram at point A in the middle.

[0032] Figure 3 This is a top view of the equipment for purifying thymol by melt crystallization described in the present invention.

[0033] Figure 4 for Figure 3 Enlarged structural diagram at point B in the middle.

[0034] Figure 5 The present invention provides a schematic diagram of the upper portion of a reactor for the purification of thymol by melt crystallization.

[0035] Figure 6 This is a cross-sectional view of the bottom end structure of the stirring main rod according to the present invention.

[0036] Figure 7 This is an independent side sectional view of the injection molding according to the present invention.

[0037] Figure 8 This is an independent side sectional view of the sampler described in the present invention.

[0038] Figure 9 It is a top view of the sampler of the structural schematic diagram of the present invention.

[0039] In the figure: 1, reactor; 101, reaction chamber; 2, stirring device; 21, motor; 22, stirring main rod; 2201, material taking channel; 221, tooth ring; 23, auxiliary wire plate; 231, wire arc plate; 232, outer guide rod; 233, guide wheel; 24, adjustment ring frame; 2401, ring guide groove; 241, adjustment support rod; 242, circular ring frame; 25, connecting piece; 25 1. Short rod; 252. Connecting block; 26. Injection piece; 2601. Insertion cavity; 261. Cylindrical sleeve; 262. Injection head; 26201. Discharge port; 263. Lower plug; 264. Pressure plate; 265. Limiting column; 3. Sampler; 31. Sampling tank; 3101. Injection channel; 3102. Limiting groove; 32. Sealing cover; 33. Pressing piece; 34. Sealing cover. DETAILED DESCRIPTION

[0040] To make the objectives, technical solutions, and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings 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 making creative efforts shall fall within the scope of protection of the present invention.

[0041] Reference Figure 1-9 , a device for purifying thymol by melt crystallization and a method for using the same will be described in detail below.

[0042] A device for purifying thymol by melt crystallization comprises: a reactor 1, a stirring device 2 and a sampler 3. The stirring device 2 is installed inside the reactor 1 and partially extends outward from the reactor 1. The sampler 3 can be placed in the stirring device 2 to remove part of the material in the reactor 1.

[0043] The reactor 1 has a reaction chamber 101 inside for materials to react. The stirring device 2 includes a motor 21, a stirring main rod 22, an auxiliary wire plate 23 and an adjustment ring frame 24. The stirring main rod 22 is inserted vertically downward from the outside of the reactor 1 into the reaction chamber 101. A stirring paddle is installed on the outer peripheral surface of the stirring main rod 22 inserted into the reaction chamber 101.

[0044] The outer circumference of the stirring rod 22 extending from the reactor 1 is provided with a toothed ring 221. The motor 21 is in driving connection with the toothed ring 221 to drive the stirring rod 22 to rotate axially. The axial rotation of the stirring rod 22 drives the stirring paddle mounted on the outer circumference to effectively stir the material in the reactor 1, causing the material to melt or crystallize rapidly.

[0045] The interior of the stirring main rod 22 is passed from bottom to top to form a material collection channel 2201. Two auxiliary silk pattern plates 23 are provided, symmetrically arranged in the material collection channel 2201. The auxiliary silk pattern plates 23 include a silk pattern arc plate 231, an outer guide rod 232 and a guide wheel 233. The inner wall of the concave side of the silk pattern arc plate 231 has silk patterns, and the outer wall of the convex side of the silk pattern arc plate 231 is installed with a connecting member 25. The connecting member 25 includes a short rod 251 and two connecting blocks 252 respectively hingedly connected to the two ends of the short rod 251. The two connecting blocks 252 are respectively connected to the outer wall of the convex side of the silk pattern arc plate 231 and the inner wall of the material collection channel 2201, so that the auxiliary silk pattern plates 23 can rotate together with the stirring main rod 22.

[0046] The adjusting ring frame 24 includes an adjusting support rod 241 and a circular frame 242. The circular frame 242 is coaxially mounted on the outside of the stirring main rod 22 by the adjusting support rod 241. The length of the adjusting support rod 241 is adjustable. The extension and retraction of the adjusting support rod 241 can drive the circular frame 242 to move vertically.

[0047] The adjusting ring frame 24 has an annular guide groove 2401. The outer guide rod 232 is connected to the wire pattern arc plate 231 and extends from the material collection channel 2201. The guide wheel 233 is mounted on the end of the outer guide rod 232 that extends outward and is engaged with the annular guide groove 2401. When the auxiliary wire pattern plate 23 rotates axially together with the stirring main rod 22, the guide wheel 233 can move in a circular motion using the annular guide groove 2401 as a track. When the annular frame 242 moves vertically, it can drive the rotating guide wheel 233 to move vertically synchronously, thereby driving the rotating wire pattern arc plate 231 to move vertically.

[0048] Because the patterned arc plate 231 is connected to the stirring main rod 22 via the connecting member 25, and the length of the short rod 251 is constant, when the patterned arc plate 231 moves up and down, the short rod 251 is driven to rotate, driving the patterned arc plate 231 to move horizontally at the same time. The width of the annular guide groove 2401 is greater than the diameter of the guide wheel 233, allowing the guide wheel 233 to move horizontally with the patterned arc plate 231.

[0049] The auxiliary silk pattern plate 23 falls into the material taking channel 2201 under the influence of its own gravity. At this time, the short rod 251 is tilted downward. When the auxiliary silk pattern plate 23 is pulled up by the adjustment ring frame 24, the short rod 251 will rotate and push the silk pattern arc plate 231 close to the central axis of the material taking channel 2201.

[0050] An injection piece 26 is installed at the bottom end of the stirring main rod 22. The lower end of the injection piece 26 directly contacts the material in the reaction chamber 101. The injection piece 26 is set at the same position as the central axis of the stirring main rod 22. The outer peripheral surface of the injection piece 26 is connected to the bearing of the stirring main rod 22. When the stirring main rod 22 rotates axially, the injection piece 26 can remain stationary.

[0051] The injection piece 26 includes a cylindrical sleeve 261, an injection head 262, a lower plug 263 and a pressure plate 264. The cylindrical sleeve 261 has a plug cavity 2601 with an inner diameter smaller than the material collection channel 2201. The plug cavity 2601 is upwardly connected to the material collection channel 2201. The injection head 262 is installed at the center of the bottom surface of the plug cavity 2601. The lower part of the injection head 262 passes through the bottom plate of the cylindrical sleeve 261 so that the material in the reaction chamber 101 can enter the injection head 262. The upper part of the outer peripheral side of the injection head 262 is provided with a discharge port 26201 so that the material in the injection head 262 can enter the plug cavity 2601. The lower plug 263 is installed at the lower end opening of the injection head 262 to seal the lower end opening of the injection head 262 to prevent the material from entering the plug cavity 2601. The pressure plate 264 is connected to the cylindrical sleeve 261 by a spring, and the pressure plate 264 is connected to the lower plug 263. When not under pressure, the pressure plate 264 is pushed upward by the spring and pulls the lower plug 263 to plug the lower end opening of the injection head 262. After being subjected to a certain pressure, the pressure plate 264 will move downward and drive the lower plug 263 away from the bottom surface of the cylindrical sleeve 261, thereby opening the lower end opening of the injection head 262 and allowing the material to enter the insert cavity 2601.

[0052] The bottom surface of the cylindrical sleeve 261 is also provided with a limiting post 265. The limiting post 265 extends vertically upward and protrudes from the stirring rod 22. After extending from the stirring rod 22, the limiting post 265 bends downward and connects to the top plate of the reactor 1. The cylindrical sleeve 261 is fixed in a fixed position within the material extraction channel 2201 by means of the limiting post 265, while the stirring rod 22 can rotate axially outside the cylindrical sleeve 261. The path of the limiting post 265 connecting to the reactor 1 avoids the rotation path of the outer guide rod 232 and the vertical movement range of the annular frame 242, thereby preventing the fixed limiting post 265 from obstructing the rotation of the outer guide rod 232 and the vertical movement of the annular frame 242.

[0053] The sampler 3 includes a sampling tank 31, a sealing cover 32, a pressing piece 33 and a blocking cover 34. The interior of the sampling tank 31 is hollow and passes upward to the outside. The sealing cover 32 is removably and sealedly installed on the upper opening of the sampling tank 31. The sealing cover 32 can seal the sampling tank 31. After the sampling tank 31 completes sampling, the sealing cover 32 can be removed to pour out the material in the sampling tank 31.

[0054] The sampling tank 31 is provided with an injection channel 3101 at the bottom. The inner diameter of the injection channel 3101 is larger than the outer diameter of the injection head 262 to allow the injection head 262 to be inserted. The blocking cover 34 covers the upper opening of the injection channel 3101. The pressing member 33 is fixedly installed inside the sampling tank 31 and is connected to the blocking cover 34 in the vertical direction by a spring. The spring presses the blocking cover 34 downward at its normal length to seal the injection channel 3101. After the sampler 3 falls into the insertion cavity 2601, it can press the pressure plate 264 downward to allow the material to enter the injection head 262. At the same time, the injection head 262 will also be inserted into the injection channel 3101 and push up the blocking cover 34. The discharge port 26201 extends into the sampling tank 31, and the material in the injection head 262 can be injected into the sampling tank 31 to complete the sampling.

[0055] The sampling tank 31 has a limiting groove 3102 on its outer peripheral surface. When the sampling tank 31 is placed in the material collection channel 2201 , the limiting column 265 can be clamped into the limiting groove 3102 , so that after the sampling tank 31 falls into the material collection channel 2201 , it is restricted by the limiting column 265 and cannot rotate axially.

[0056] The outer peripheral surface of the sampling tank 31 also has a silk pattern corresponding to the silk pattern arc plate 231. Under normal circumstances, the silk pattern arc plate 231 droops due to its own weight. At this time, the silk pattern arc plate 231 has an inner concave surface with silk patterns away from the sampling tank 31; after being pulled up, the silk pattern arc plate 231 will move and fit tightly against the outer wall of the sampling tank 31, thereby engaging with the silk pattern of the sampling tank 31. After the sampling of the sampling tank 31 is completed, the silk arc plate 231 can be pulled up and lifted to cooperate with the silk pattern of the sampling tank 31. At this time, the silk arc plate 231 rotating together with the stirring main rod 22 can gradually lift the sampling tank 31 that originally fell into the bottom of the material collection channel 2201. The silk pattern of the silk arc plate 231 is distributed upward until it approaches the opening on the stirring main rod 22, so that the sampling tank 31 can be lifted to the opening on the stirring main rod 22 for easy removal. The sampling tank 31 taken out of the stirring main rod 22 can remove the sealing cover 32 and pour out the sample for subsequent testing.

[0057] A method for purifying thymol by melt crystallization, comprising the following steps;

[0058] S1: placing a material containing thymol, m-thymol (3-methyl-5-isopropylphenol), p-thymol, 3-methyl-2,6-diisopropylphenol and 3-methyl-4,6-diisopropylphenol into a reaction chamber 101, heating the reactor 1 and starting the stirring device 2 to melt the material;

[0059] S2: The sampler 3 is vertically inserted into the material extraction channel 2201 with the injection channel 3101 facing downward and the limiting groove 3102 engaging with the limiting column 265. The sampler 3 presses down the pressure plate 264 to allow part of the melted material in the reactor 1 to enter the sampler 3;

[0060] S3: Lift the adjustment ring frame 24 so that the wire arc plate 231 is close to the sampling tank 31, wait for a while and then take the sampler 3 sent by the wire arc plate 231 to the opening on the stirring main rod 22;

[0061] S4: measuring the crystallization point T of the material in S3 and performing chromatographic analysis on the thymol content in the material;

[0062] S5: Cool the reactor 1 to T+10°C and add seed crystals;

[0063] S6: Cool the reactor 1 in a stepwise manner of 1°C / 10min to 0°C, discharge the contents and centrifuge.

[0064] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like to indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0065] In the present invention, unless otherwise expressly specified or limited, terms such as "disposed," "installed," "connected," "connected," and "fixed" should be understood in a broad sense. For example, they may refer to fixed connections, detachable connections, or integration; they may refer to mechanical connections, direct connections, or indirect connections through an intermediate medium; they may refer to internal communication between two elements or interaction between two elements. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0066] The control method of the present invention is automatic control through a controller. The control circuit of the controller can be implemented by simple programming by a person skilled in the art. The provision of power is also common knowledge in the art. The present invention is mainly used to protect mechanical devices, so the control method and circuit connection are not explained in detail in the present invention.

[0067] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A device for purifying thymol by melt crystallization, comprising a reactor (1) and a stirring device (2), wherein the stirring device (2) is installed inside the reactor (1) and partially extends outward from the reactor (1), and is characterized in that: The stirring device (2) includes a stirring main rod (22) that can be driven to rotate axially, and a material collection channel (2201) is provided inside the stirring main rod (22) and is connected to the auxiliary wire pattern plate (23) via a connecting piece (25). The auxiliary wire pattern plate (23) is rotatably connected to an adjustment ring frame (24), and the adjustment ring frame (24) can move vertically. The bottom end of the stirring main rod (22) is equipped with an injection piece (26), and the injection piece (26) includes a cylindrical sleeve (261), an injection head (262), a lower plug (263) and a pressure plate (264). The cylindrical sleeve (261) is connected to the material collection channel (2201), and a sampler (3) can be placed in the material collection channel (2201). The sampler (3) can fall into the cylindrical sleeve (261). The upper part of the outer peripheral side of the injection head (262) is provided with a discharge port (26201), and the lower part passes through the bottom plate of the cylindrical sleeve (261). The lower plug (263) is installed at the lower end opening of the injection head (262). The pressure plate (264) is connected to the bottom spring of the cylindrical sleeve (261) and is connected to the lower plug (263).

2. The device for purifying thymol by melt crystallization according to claim 1, wherein: The sampler (3) comprises a sampling tank (31), a pressing member (33) and a blocking cover (34). The bottom of the sampling tank (31) is provided with an injection channel (3101) for allowing the injection head (262) to be inserted. The blocking cover (34) covers the upper opening of the injection channel (3101). The pressing member (33) is fixed in the sampling tank (31) and is connected to the blocking cover (34) in a vertical direction by a spring.

3. The device for purifying thymol by melt crystallization according to claim 1, wherein: The injection head (262) is installed at the center of the bottom surface of the cylindrical sleeve (261), and the outer peripheral surface of the cylindrical sleeve (261) is connected to the bearing of the stirring main rod (22).

4. The device for purifying thymol by melt crystallization according to claim 1, wherein: The adjusting ring frame (24) has a ring guide groove (2401), and the auxiliary silk pattern plate (23) includes a silk pattern arc plate (231), an outer guide rod (232) and a guide wheel (233). The outer guide rod (232) is connected to the silk pattern arc plate (231) and extends from the material taking channel (2201). The guide wheel (233) is installed on the end of the outer guide rod (232) extending to the outside and is clamped in the ring guide groove (2401). The width of the ring guide groove (2401) is greater than that of the guide wheel (233).

5. The device for purifying thymol by melt crystallization according to claim 1, wherein: A limiting column (265) is further provided on the bottom surface of the cylindrical sleeve (261). The limiting column (265) extends vertically upward from the stirring main rod (22). After extending from the stirring main rod (22), the limiting column (265) bends downward and is connected to the top plate of the reactor (1).

6. The device for purifying thymol by melt crystallization according to claim 2, characterized in that: The outer circumference of the sampling tank (31) has a limiting groove (3102) that allows the limiting column (265) to be placed therein, and the outer circumference of the sampling tank (31) also has a silk pattern corresponding to the silk pattern arc plate (231).

7. A method for using the apparatus for melt crystallization purification of thymol according to any one of claims 1 to 6, characterized in that: The following steps are involved: S1: placing a material containing thymol, m-thymol (3-methyl-5-isopropylphenol), p-thymol, 3-methyl-2,6-diisopropylphenol, and 3-methyl-4,6-diisopropylphenol into a reaction chamber (101), heating the reactor (1) and starting a stirring device (2) to melt the material; S2: The sampler (3) is vertically inserted into the material extraction channel (2201) with the injection channel (3101) facing downward and the limiting groove (3102) engaging with the limiting column (265). The sampler (3) presses down the pressure plate (264) so ​​that part of the melted material in the reactor (1) enters the sampler (3); S3: Lift the adjustment ring frame (24) so ​​that the wire arc plate (231) is close to the sampling tank (31), wait for a while and then take the sampler (3) sent by the wire arc plate (231) to the upper opening of the stirring main rod (22); S4: measuring the crystallization point T of the material in S3 and performing chromatographic analysis on the thymol content in the material; S5: Cool the reactor (1) to T+10°C and add seed crystals; S6: The temperature of the reactor (1) is lowered in a stepwise manner by 1°C / 10min to 0°C, and the contents are discharged and centrifuged.

Images