Ultrasonic crystallization device and technology for preparing high-purity ethyl maltol

Abstract

The invention discloses an ultrasonic crystallization device for preparing high-purity ethyl maltol and a process thereof, and relates to the technical field of ethyl maltol preparation, the ultrasonic crystallization device comprises a mounting vertical frame and a reaction kettle body, the top end of the reaction kettle body is rotatably provided with a rotating plate, and the ultrasonic crystallization device further comprises a grinding assembly, a stirring assembly and an ultrasonic oscillation assembly; according to the powder grinding device, powder can be refined in the grinding area, and the caking condition is avoided; on the other hand, when a follow-up hydraulic rod moves downwards, a sealing ring plug can be driven to move downwards, so that a part of air in the grinding inner cylinder is introduced into a ring cavity through a one-way air outlet valve I, and finally, the air is shunted through a plurality of inclined branch ports and is blown into a blanking hole in a rotating plate, so that the powder is promoted to fall off; meanwhile, the other part of air in the grinding inner cylinder is aerated into the reaction kettle body through a bottom through pipe and a one-way air outlet valve II, so that the effects of assisting material dissolution and promoting subsequent crystallization are achieved.

Description

Technical Field

[0001] The present invention relates to the technical field of ethyl maltol preparation, and in particular to an ultrasonic crystallization device and process for preparing high-purity ethyl maltol. Background Art

[0002] As an important food additive and flavor ingredient, the preparation of high-purity ethyl maltol products has extremely high requirements for the efficiency and quality of the crystallization process. In the prior art, the preparation of ethyl maltol usually undergoes key steps such as raw material dissolution, solution concentration, and crystallization. Among them, the uniformity and efficiency of the raw material dissolution stage directly affect the crystal form, purity, and yield of the subsequent crystallization process. However, the dissolution processes commonly used in industry at present have significant defects and need to be improved urgently.

[0003] Specifically, during the raw material dissolution process, when powdered ethyl maltol or its precursor materials are put into a solvent (such as ethanol or a water-ethanol mixed solution), due to the hydrophilicity or surface electrostatic effect of the materials, agglomeration and caking are very likely to occur. The formation of these cakes not only greatly reduces the contact area between the materials and the solvent, but also prolongs the dissolution time, and even requires additional elevation of the solvent temperature or extension of the mechanical stirring duration to promote dispersion. Although traditional dissolution devices usually are equipped with mechanical stirring units (such as paddle or magnetic stirrers), the stirring method relying solely on shear force and convection has limited improvement on the caking problem of micron-sized powders. Especially in the initial stage of material feeding or in a high-concentration system, it is difficult for stirring to quickly penetrate and disperse dense agglomerates. In addition, excessive reliance on stirring may lead to uneven local temperature or the introduction of bubbles, further affecting the dissolution efficiency and solution stability.

[0004] The problem of insufficient dissolution will directly affect the subsequent crystallization process. Undissolved fine particles may become heterogeneous crystal nuclei, resulting in inconsistent crystal growth rates, mixed crystal forms, or entrapment of impurities, ultimately reducing the product purity and yield. Although attempts have been made in the prior art to alleviate the caking problem by optimizing stirring parameters (such as rotation speed, blade shape), these methods often increase the process complexity and have limited effects. In recent years, ultrasonic-assisted technology has shown potential in the field of chemical dispersion due to its cavitation effect and microjet action. However, there is no dedicated device design for the ethyl maltol dissolution-crystallization combined process in existing patents and literature. In particular, there is still a blank in the technical solution of how to efficiently couple ultrasonic energy into the dissolution stage to simultaneously inhibit caking, accelerate dissolution, and synergistically improve the crystallization effect. Summary of the Invention

[0005] The purpose of the present invention is to provide an ultrasonic crystallization device and process for preparing high-purity ethyl maltol to solve the problems raised in the above background art.

[0006] The technical solution of the present invention is: an ultrasonic crystallization device for preparing high-purity ethyl maltol, including an installation vertical frame and a reaction kettle body. A rotating plate is rotatably installed at the top of the reaction kettle body, and further includes a grinding component, a stirring component, and an ultrasonic oscillation component; The grinding component includes a bearing seat fixedly installed at the top of the reaction kettle body. The bearing seat is coaxially arranged with the rotating plate. A grinding hopper is rotatably installed in the bearing seat. A grinding inner cylinder arranged coaxially is fixedly installed on the surface of the rotating plate. A grinding area is formed between the outer side of the grinding inner cylinder and the grinding hopper. Uniformly distributed blanking holes are formed near the edge of the rotating plate. An annular cavity is formed near the bottom position of the grinding inner cylinder. A plurality of inclined branch ports communicating with the annular cavity are formed at the bottom of the grinding inner cylinder. A plurality of installation ports communicating with the annular cavity are formed on the inner wall of the grinding inner cylinder, and a one-way air outlet valve I is fixedly installed inside each installation port. A plurality of bottom through pipes distributed at equal distances are fixedly penetrated through the position of the rotating plate close to the grinding inner cylinder, and a one-way air outlet valve II is fixedly installed at the bottom end of each bottom through pipe; The ultrasonic oscillation component includes a top vertical frame fixedly installed at the top of the reaction kettle body. A hydraulic rod is fixedly installed on one side of the top vertical frame. An extension column is fixed to the output shaft of the hydraulic rod, and an ultrasonic oscillator is fixedly installed at the end of the extension column. A sealing ring plug slidably matched with the grinding inner cylinder is fixedly installed at one end of the extension column.

[0007] Preferably, a plurality of air inlets are formed on the sealing ring plug, and a one-way air inlet valve is fixedly installed inside each air inlet. A pair of hoop frames are fixedly installed between the installation vertical frame and the reaction kettle body. A frame-shaped top frame is fixedly installed between the top vertical frame and the installation vertical frame.

[0008] Preferably, a top ring is rotatably installed on the inner wall of the top of the reaction kettle body, and a plurality of pairs of side rods are fixedly installed on the outer side wall of the top ring. The bottom end of each pair of side rods is fixedly installed with a U-shaped bottom frame. A valve-equipped liquid supply pipe is fixedly communicated with one side of the reaction kettle body near the top, and a valve-equipped discharge pipe is fixedly communicated with the bottom end of the reaction kettle body.

[0009] Preferably, the stirring component includes an L-shaped end rod rotatably installed at one end of the U-shaped bottom frame. A plurality of hook-shaped cavity blocks are fixedly installed at a position near the bottom end of the L-shaped end rod. Each hook-shaped cavity block has a structure that is narrow at the top and wide at the bottom. An oval notch is formed at the end of each L-shaped end rod. A ring rod is jointly movably installed through the oval notches of the plurality of L-shaped end rods. A pair of abutting ring pieces are fixedly installed at the position of the ring rod close to the oval notch.

[0010] Preferably, the stirring component further includes a plurality of bottom connecting rods fixedly installed at the bottom of the top ring. One end of the extension column is rotatably installed with a convex key cylinder and a collar through bearings. The convex key cylinder is fixedly connected with the collar. The convex key cylinder is slidably connected with the rotating plate in the vertical direction. A plurality of connecting ribs are fixedly connected between the collar and the ring rod.

[0011] Preferably, a connecting ring block is fixedly installed at the ends of the plurality of bottom connecting rods together, and the connecting ring block is rotatably connected to the convex key cylinder in the vertical direction. The convex key cylinder forms a key connection with the rotating plate and the connecting ring block. A conical panel is fixedly installed at the bottom end of the connecting ring block, and a plurality of arc-shaped grooves are arranged at equal distances on the surface of the conical panel. All the bottom through pipes fixedly penetrate through the collar.

[0012] Preferably, multiple groups of vertical rods are fixedly installed on each connecting rib, and a bottom plate is fixedly installed at the bottom ends of each group of vertical rods together. A plurality of X-shaped notches are formed on each bottom plate.

[0013] Preferably, a mounting plate is fixed at the top of the reaction kettle body, and a driving motor is fixedly installed on one side of the mounting plate. The output shaft of the driving motor is fixed with a transmission rod that movably penetrates through the reaction kettle body. A first transmission gear and a second transmission gear are fixedly installed on the transmission rod. An external tooth ring is fixedly installed on the outer wall of the grinding hopper, and the external tooth ring meshes with the first transmission gear.

[0014] Preferably, uniformly distributed convex teeth are fixedly installed on the inner peripheral wall of the top ring, and the second transmission gear meshes with the convex teeth.

[0015] The present invention also discloses an ultrasonic crystallization process for the preparation of high-purity ethyl maltol, which specifically includes the following steps: Step 1, Dissolution: Place ethyl maltol in the reaction kettle body and dissolve it in ethanol to obtain an ethyl maltol solution. The dissolution temperature is 40 - 45 °C; Step 2, Control the temperature of the reaction kettle body to drop to 25 °C, the frequency of the ultrasonic oscillator to be 30 KHz, and the treatment time to be 2 - 3 h to induce the precipitation of fine impurities; Step 3, Introduce the liquid obtained in Step 2 into a filter for filtration to remove fine impurity crystals; then introduce it into a decolorizer to remove trace impurities dissolved in the ethyl maltol clear liquid to obtain a refined ethyl maltol solution; Step 4, Place the refined ethyl maltol solution in the reaction kettle body again, control the refined ethyl maltol solution to cool down slowly to 0 °C for cooling crystallization, and then obtain high-purity ethyl maltol after separation and drying.

[0016] The present invention provides an ultrasonic crystallization device and its process for the preparation of high-purity ethyl maltol through improvement. Compared with the prior art, it has the following improvements and advantages: First: During the actual use of the present invention, powder materials can be added into the grinding hopper, and by using the relative rotation between the grinding hopper and the inner grinding cylinder, the powder materials can be refined in the grinding area to avoid caking. On the other hand, when the subsequent hydraulic rod moves downward, it can drive the sealing ring plug to move downward, so that a part of the air in the inner grinding cylinder can be introduced into the ring cavity through the one-way air outlet valve, and finally, after being shunted through multiple inclined branch ports, it is blown into the blanking holes on the rotating plate, thereby promoting the falling of the powder materials. At the same time, another part of the air in the inner grinding cylinder is aerated into the reaction kettle body through the bottom pipe and the second one-way air outlet valve, so as to achieve the effects of assisting the dissolution of materials and promoting subsequent crystallization. Second: When multiple L-shaped end rods rotate around the center of the reaction kettle body, the arranged hook-shaped cavity blocks can stir the materials. At the same time, since the hook-shaped cavity blocks are narrower at the top and wider at the bottom, the materials can enter from the wide opening at the bottom of the hook-shaped cavity blocks and then be output from the narrow opening at the top. During this process, by using the pipe narrowing effect, the flow rate of the materials is increased, thereby promoting the mixing between the materials. When the hydraulic rod operates, it can drive the convex key cylinder and the collar to move vertically, and then drive the ring rod to move synchronously through the connecting ribs. When the ring rod moves vertically, it can cooperate with the long oval notch to drive the L-shaped end rod to flip along the connection with the U-shaped bottom frame, thereby adjusting the stirring angle and range to achieve the purpose of improving the mixing effect and promoting the dissolution of materials. Third: When the bottom connecting rod drives the connecting ring block to rotate, it can synchronously drive the conical panel to rotate. Cooperating with the arranged multiple arc-shaped grooves, it can further shunt the materials falling from the rotating plate, realizing more uniform addition of the powder materials, which is beneficial to the dissolution of the materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings required for use in the description of the specific embodiments or the prior art. Obviously, the following drawings are some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0018] Figure 1 is the overall three-dimensional structure schematic diagram of the present invention; Figure 2 is the internal structure schematic diagram of the reaction kettle body of the present invention; Figure 3 is the sectional structure schematic diagram of the reaction kettle body of the present invention; Figure 4 is of the present invention Figure 3 magnified structure schematic diagram at A in; Figure 5 is the three-dimensional structure schematic diagram of the hook-shaped cavity block of the present invention; Figure 6 Schematic diagram of the plane structure of the extension column of the present invention; Figure 7 For the Figure 6 Enlarged structure diagram at position B in the present invention; Figure 8 Schematic three-dimensional structure diagram of the top ring and the grinding hopper of the present invention; Figure 9 Schematic three-dimensional structure diagram of the ring rod and the rotating plate of the present invention; Figure 10 Schematic three-dimensional structure diagram of the conical panel, the inner grinding cylinder and the convex key cylinder of the present invention; Figure 11 For the Figure 6 Enlarged structure diagram at position C in the present invention.

[0019] Reference numerals: 1, reaction kettle body; 101, liquid supply pipe with valve; 102, discharge pipe with valve; 103, installation vertical frame; 104, hoop frame; 105, frame-shaped top frame; 2, top vertical frame; 201, hydraulic rod; 202, sealing ring plug; 3, drive motor; 301, transmission rod; 302, first transmission gear; 303, second transmission gear; 4, grinding hopper; 401, external tooth ring; 402, inner grinding cylinder; 5, top ring; 501, convex tooth; 6, rotating plate; 601, blanking hole; 7, extension column; 701, ultrasonic oscillator; 8, convex key cylinder; 9, side rod; 901, U-shaped bottom frame; 902, L-shaped end rod; 903, hook-shaped cavity block; 904, long oval notch; 10, bottom through pipe; 11, check valve II for air outlet; 12, ring rod; 121, abutting ring piece; 122, connecting rib; 123, sleeve ring; 13, ring cavity; 14, inclined support port; 15, bottom connecting rod; 151, connecting ring block; 16, conical panel; 161, arc groove; 17, vertical rod; 171, bottom plate; 172, X-shaped notch; 18, bearing seat; 19, air inlet; 20, check valve for air inlet; 21, check valve I for air outlet. Detailed implementation manners

[0020] The present invention will be described in detail below. The technical solutions in the embodiments of the present invention are clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0021] The present invention provides a high-purity ethyl maltol preparation ultrasonic crystallization device and its process by improvement. The technical solution of the present invention is: As Figures 1 to 11As shown in the figure, an ultrasonic crystallization device for preparing high-purity ethyl maltol according to an embodiment of the present invention includes an installation vertical frame 103 and a reaction kettle body 1. A rotating plate 6 is rotatably installed at the top of the reaction kettle body 1. The device further includes a grinding component, a stirring component, and an ultrasonic oscillation component. The provided grinding component is used to put and grind the powder materials to achieve uniform addition of the powder materials. It should be noted that in this application, the reaction kettle body 1 has a temperature adjustment function, which belongs to the prior art. Therefore, the temperature adjustment principle and its related structure will not be described herein.

[0022] The grinding component includes a bearing seat 18 fixedly installed at the top of the reaction kettle body 1. The bearing seat 18 is coaxially arranged with the rotating plate 6. A grinding hopper 4 is rotatably installed in the bearing seat 18. A grinding inner cylinder 402 arranged coaxially is fixedly installed on the surface of the rotating plate 6. A grinding area is formed between the outer side of the grinding inner cylinder 402 and the grinding hopper 4. Uniformly distributed blanking holes 601 are formed near the edge of the rotating plate 6. An annular cavity 13 is formed near the bottom of the grinding inner cylinder 402. A plurality of inclined branch ports 14 communicating with the annular cavity 13 are formed at the bottom of the grinding inner cylinder 402. A plurality of installation ports communicating with the annular cavity 13 are formed on the inner wall of the grinding inner cylinder 402, and a one-way air outlet valve I 21 is fixedly installed inside each installation port. A plurality of bottom through pipes 10 distributed at equal distances are fixedly penetrated through the position of the rotating plate 6 near the grinding inner cylinder 402, and a one-way air outlet valve II 11 is fixedly installed at the bottom end of each bottom through pipe 10. Through the above structure, during actual use, the powder materials can be added into the grinding hopper 4, and the relative rotation between the grinding hopper 4 and the grinding inner cylinder 402 is utilized to refine the powder materials in the grinding area, avoiding caking. On the other hand, when the subsequent hydraulic rod 201 moves downward, it can drive the sealing ring plug 202 to move downward, so that a part of the air in the grinding inner cylinder 402 is introduced into the annular cavity 13 through the one-way air outlet valve I 21, and finally is split through a plurality of inclined branch ports 14 and blown into the blanking holes 601 on the rotating plate 6, thereby promoting the falling of the powder materials. At the same time, another part of the air in the grinding inner cylinder 402 is aerated into the reaction kettle body 1 through the bottom through pipes 10 and the one-way air outlet valve II 11, thereby achieving the effects of assisting the dissolution of the materials and promoting subsequent crystallization.

[0023] The ultrasonic oscillation component includes a top-mounted vertical frame 2 fixedly installed at the top of the reaction kettle body 1. A hydraulic rod 201 is fixedly installed on one side of the top-mounted vertical frame 2. An extension column 7 is fixed to the output shaft of the hydraulic rod 201, and an ultrasonic oscillator 701 is fixedly installed at the end of the extension column 7. A sealing ring plug 202 slidably matched with the grinding inner cylinder 402 is fixedly installed at one end of the extension column 7. Through the above structure, by using the provided hydraulic rod 201, the height of the ultrasonic oscillator 701 can be adjusted in cooperation with the extension column 7, and thus the dynamic oscillation of the materials in the reaction kettle body 1 can be realized, further improving the dissolution and crystallization effects of the materials.

[0024] Furthermore, a plurality of air inlets 19 are formed in the sealing ring plug 202, and a one-way air inlet valve 20 is fixedly installed in each air inlet 19. A pair of hoop frames 104 are fixedly installed between the installation stand 103 and the reaction kettle body 1, and a frame-shaped top frame 105 is fixedly installed between the top installation stand 2 and the installation stand 103; it should be noted that a filter sheet can be arranged at the opening of the one-way air inlet valve 20. With the above structure, when the hydraulic rod 201 drives the extension column 7 to move upward, under the negative pressure, the air in the dust-free workshop can be filtered through the filter sheet and then introduced into the inner side of the grinding inner cylinder 402 to maintain air pressure balance.

[0025] Furthermore, a top ring 5 is rotatably installed on the inner wall of the top of the reaction kettle body 1, and a plurality of pairs of side rods 9 are fixedly installed on the outer side wall of the top ring 5. The bottom end of each pair of side rods 9 is fixedly installed with a U-shaped bottom frame 901. A valve-equipped liquid supply pipe 101 is fixedly connected to one side of the reaction kettle body 1 near the top, and a valve-equipped discharge pipe 102 is fixedly connected to the bottom end of the reaction kettle body 1; the provided valve-equipped liquid supply pipe 101 is used to add liquid materials into the reaction kettle body 1; and the provided valve-equipped discharge pipe 102 is used to discharge the materials after stirring is completed.

[0026] As a further solution of the present invention, the stirring assembly includes an L-shaped end rod 902 rotatably installed at one end of the U-shaped bottom frame 901, and a plurality of hook-shaped cavity blocks 903 are fixedly installed at a position near the bottom end of the L-shaped end rod 902. Each hook-shaped cavity block 903 has a structure that is narrow at the top and wide at the bottom. An oval slot 904 is formed at the end of each L-shaped end rod 902. A ring rod 12 is movably installed through the oval slots 904 by a plurality of L-shaped end rods 902. A pair of abutting ring pieces 121 are fixedly installed at positions of the ring rod 12 near the oval slots 904; with the above structure, when a plurality of L-shaped end rods 902 rotate around the center of the reaction kettle body 1, the provided hook-shaped cavity blocks 903 can stir the materials. At the same time, since the hook-shaped cavity blocks 903 are narrow at the top and wide at the bottom, the materials can enter from the wide opening at the bottom end of the hook-shaped cavity blocks 903 and then output from the narrow opening at the top end. During this process, the flow rate of the materials is increased by using the venturi effect, thereby promoting the mixing between the materials.

[0027] As a further solution of the present invention, the stirring assembly further includes a plurality of bottom connecting rods 15 fixedly installed at the bottom of the top ring 5. One end of the extension column 7 is rotatably installed with a convex key cylinder 8 and a collar 123 through bearings. The convex key cylinder 8 is fixedly connected to the collar 123. The convex key cylinder 8 is slidably connected to the rotating plate 6 in the vertical direction. A plurality of connecting ribs 122 are fixedly connected between the collar 123 and the ring rod 12; with the above structure, when the top ring 5 rotates, it can drive the connecting ring block 151 to rotate through the provided bottom connecting rods 15, and drive the convex key cylinder 8 and the collar 123 to rotate by using the connecting ring block 151; When the top ring 5 rotates, it can cooperate with the side rod 9 and the U-shaped chassis 901 to drive the L-shaped end rod 902 to rotate. Moreover, the collar 123 can cooperate with the connecting rib 122 to drive the ring rod 12 to rotate. With the arranged abutting ring piece 121, synchronously, a rotational driving force is applied to the L-shaped end rod 902, enabling multiple L-shaped end rods 902 to drive the hook-shaped cavity block 903 to rotate stably. On the other hand, when the hydraulic rod 201 operates, it can drive the convex key cylinder 8 and the collar 123 to move vertically. Furthermore, it can cooperate with the connecting rib 122 to drive the ring rod 12 to move synchronously. When the ring rod 12 moves vertically, it can cooperate with the oblong notch 904 to drive the L-shaped end rod 902 to flip along the connection with the U-shaped chassis 901, thereby adjusting the stirring angle and range to achieve the purpose of improving the mixing effect and promoting the dissolution of the materials.

[0028] Furthermore, a connecting ring block 151 is fixedly installed at the ends of multiple bottom connecting rods 15 together. And the connecting ring block 151 is rotatably connected to the convex key cylinder 8 in the vertical direction. The convex key cylinder 8 forms a key connection with the rotating plate 6 and the connecting ring block 151. A conical panel 16 is fixedly installed at the bottom end of the connecting ring block 151. And a plurality of arc-shaped grooves 161 are arranged at equal distances on the surface of the conical panel 16. Multiple bottom through pipes 10 are all fixedly penetrated through the collar 123. Through the above structure, when the bottom connecting rod 15 drives the connecting ring block 151 to rotate, it can synchronously drive the conical panel 16 to rotate. With the arranged multiple arc-shaped grooves 161, it can further divide the materials falling from the rotating plate 6, realizing more uniform addition of the powder materials, which is beneficial to the dissolution of the materials.

[0029] As a further solution of the present invention, as Figures 9 - 10 shown, multiple groups of vertical rods 17 are fixedly installed on each connecting rib 122. And a bottom plate 171 is fixedly installed at the bottom ends of each group of vertical rods 17 together. A plurality of X-shaped notches 172 are opened on each bottom plate 171. When the ring rod 12 moves vertically, it can cooperate with the vertical rods 17 to drive the bottom plate 171 to move vertically. With the arranged X-shaped notches 172, the mixing effect is further improved.

[0030] Furthermore, an installation plate is fixed at the top of the reaction kettle body 1. And a driving motor 3 is fixedly installed on one side of the installation plate. The output shaft of the driving motor 3 is fixed with a transmission rod 301 that movably penetrates through the reaction kettle body 1. A first transmission gear 302 and a second transmission gear 303 are fixedly installed on the transmission rod 301. An external tooth ring 401 is fixedly installed on the outer wall of the grinding hopper 4. And the external tooth ring 401 meshes with the first transmission gear 302. Through the above structure, when the driving motor 3 operates, it can drive the top ring 5 to rotate through the cooperation of the second transmission gear 303 and the subsequent convex teeth 501. At the same time, when the top ring 5 rotates, it can drive the rotating plate 6 to rotate through the convex key cylinder 8, and the rotating plate 6 drives the grinding inner cylinder 402 to rotate. On the other hand, when the driving motor 3 operates, it can drive the grinding hopper 4 to rotate through the transmission of the first transmission gear 302 and the external tooth ring 401. At this time, the grinding hopper 4 and the inner grinding cylinder 402 rotate towards each other to complete the grinding and feeding operations.

[0031] Furthermore, evenly distributed convex teeth 501 are fixedly installed on the inner peripheral wall of the top ring 5, and the second transmission gear 303 meshes with the convex teeth 501; through the above structure, the second transmission gear 303 can form a transmission cooperation with the convex teeth 501. The specific working method is as follows: during use, the liquid material is introduced into the reaction kettle body 1 through the liquid supply pipe 101 with a valve, and the proportioned powder material is added into the grinding hopper 4. Under the action of gravity, the powder material enters the grinding area between the grinding hopper 4 and the inner grinding cylinder 402. Start the driving motor 3. Through the cooperation of the second transmission gear 303 and the subsequent convex teeth 501, drive the top ring 5 to rotate; at the same time, when the top ring 5 rotates, it can drive the rotating plate 6 to rotate through the convex key cylinder 8, and the rotating plate 6 drives the inner grinding cylinder 402 to rotate; on the other hand, when the driving motor 3 operates, it can drive the grinding hopper 4 to rotate through the transmission of the first transmission gear 302 and the external tooth ring 401. At this time, the grinding hopper 4 and the inner grinding cylinder 402 rotate towards each other to complete the grinding process, so that the powder material is refined in the grinding area to avoid caking. On the other hand, when the subsequent hydraulic rod 201 moves downward, it can drive the sealing ring plug 202 to move downward, thereby discharging a part of the air in the inner grinding cylinder 402 into the annular cavity 13 through the one-way air outlet valve 21, and finally shunting through a plurality of inclined branch ports 14 and blowing into the material dropping holes 601 on the rotating plate 6, thereby promoting the falling of the powder material; at the same time, another part of the air in the inner grinding cylinder 402 is aerated into the reaction kettle body 1 through the bottom through pipe 10 and the one-way air outlet valve 11, so as to achieve the effect of assisting the dissolution of the material and promoting subsequent crystallization; by using the provided hydraulic rod 201, it can cooperate with the extension column 7 to adjust the height of the ultrasonic oscillator 701, and further realize the dynamic oscillation of the material in the reaction kettle body 1, further improving the dissolution and crystallization effects of the material. When the hydraulic rod 201 drives the extension column 7 to move upward, under the action of negative pressure, the air in the dust-free workshop can be filtered through the filter element and introduced into the inner side of the inner grinding cylinder 402 to maintain air pressure balance. When multiple L-shaped end rods 902 rotate around the center of the reaction kettle body 1, the provided hook-shaped cavity block 903 can stir the materials. At the same time, since the hook-shaped cavity block 903 is narrow at the top and wide at the bottom, the materials can enter from the wide opening at the bottom end of the hook-shaped cavity block 903 and then output from the narrow opening at the top end. During this process, using the venturi effect, the flow rate of the materials is increased, thereby promoting the mixing between the materials; when the top ring 5 rotates, it can drive the connecting ring block 151 to rotate through the provided bottom connecting rod 15, and drive the convex key cylinder 8 and the collar 123 to rotate by using the connecting ring block 151; when the top ring 5 rotates, it can cooperate with the side rod 9 and the U-shaped bottom frame 901 to drive the L-shaped end rod 902 to rotate. Moreover, the collar 123 can cooperate with the connecting ribs 122 to drive the ring rod 12 to rotate, and cooperate with the provided abutting ring piece 121 to synchronously apply a rotational driving force to the L-shaped end rod 902, so that multiple L-shaped end rods 902 can drive the hook-shaped cavity block 903 to rotate stably; on the other hand, when the hydraulic rod 201 operates, it can drive the convex key cylinder 8 and the collar 123 to move vertically, and then cooperate with the connecting ribs 122 to drive the ring rod 12 to move synchronously. When the ring rod 12 moves vertically, it can cooperate with the long circular notch 904 to drive the L-shaped end rod 902 to flip along the connection with the U-shaped bottom frame 901, thereby adjusting the stirring angle and range to achieve the purpose of improving the mixing effect, so as to promote the dissolution of the materials; when the ring rod 12 moves vertically, it can cooperate with the vertical rod 17 to drive the bottom plate 171 to move vertically, and cooperate with the provided X-shaped notch 172 to further improve the mixing effect; after the mixing of the materials is completed, control the temperature of the reaction kettle body 1 to drop to 25°C, the frequency of the ultrasonic oscillator 701 to be 30 KHz, and the treatment time to be 2 - 3 h to induce the precipitation of fine impurities; Open the valve-equipped discharge pipe 102, introduce the liquid into the filter for filtration to remove fine impurity crystals; then introduce it into the decolorizer to remove trace impurities dissolved in the ethyl maltol clear liquid to obtain a refined ethyl maltol solution; finally, place the refined ethyl maltol solution back into the reaction kettle body 1, use the reaction kettle body 1 to control the refined ethyl maltol solution to cool slowly to 0°C for cooling crystallization, and then through separation and drying, high-purity ethyl maltol is obtained.

[0032] An ultrasonic crystallization process for preparing high-purity ethyl maltol specifically includes the following steps: Step 1, Dissolution: Place ethyl maltol in the reaction kettle body 1 and dissolve it in ethanol to obtain an ethyl maltol solution, and the dissolution temperature is 40 - 45°C; Step 2, Control the temperature of the reaction kettle body 1 to drop to 25°C, the frequency of the ultrasonic oscillator 701 to be 30 KHz, and the treatment time to be 2 - 3 h to induce the precipitation of fine impurities; Step 3: Introduce the liquid obtained in Step 2 into a filter for filtration to remove fine impurity crystals; then introduce it into a decolorizer to remove trace impurities dissolved in the ethyl maltol clear liquid, obtaining a refined ethyl maltol solution. Step 4: Place the refined ethyl maltol solution in the reactor body 1 again, control the refined ethyl maltol solution to slowly cool down to 0 °C for cooling crystallization, and then after separation and drying, high-purity ethyl maltol is obtained.

[0033] The above description enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be obvious to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to these embodiments shown herein, but rather will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. An ultrasonic crystallization device for preparing high-purity ethyl maltol, comprising a mounting stand (103) and a reaction kettle body (1), characterized in that: The top of the reaction kettle body (1) is rotatably mounted with a rotating plate (6), and further comprises a grinding component, a stirring component and an ultrasonic oscillation component; The grinding assembly comprises a bearing seat (18) fixedly mounted on the top of the reaction kettle body (1), the bearing seat (18) and the rotating plate (6) being coaxially arranged, a grinding bucket (4) being rotatably mounted in the bearing seat (18), a coaxially arranged grinding inner cylinder (402) being fixedly mounted on the surface of the rotating plate (6), the outer side of the grinding inner cylinder (402) and the grinding bucket (4) forming a grinding area, the rotating plate (6) having evenly distributed drop holes (601) near the edge, and the grinding inner cylinder (402) having a bottom portion thereof. an annular cavity (13), the bottom of the grinding inner cylinder (402) is provided with a plurality of oblique branch openings (14) in communication with the annular cavity (13), the inner wall of the grinding inner cylinder (402) is provided with a plurality of mounting openings in communication with the annular cavity (13), and a one-way air outlet valve (21) is fixedly installed inside each mounting opening, a plurality of bottom through pipes (10) distributed at equal distances are fixedly penetrated at a position of the rotating plate (6) close to the grinding inner cylinder (402), and a one-way air outlet valve (11) is fixedly installed at the bottom end of each bottom through pipe (10); The ultrasonic oscillator assembly comprises a top stand (2) fixedly mounted on the top of the reaction kettle body (1), and a hydraulic rod (201) is fixedly mounted on one side of the top stand (2), an extension column (7) is fixedly mounted on the output shaft of the hydraulic rod (201), and an ultrasonic oscillator (701) is fixedly mounted on the end of the extension column (7), and a sealing ring plug (202) that slidably cooperates with the grinding inner cylinder (402) is fixedly mounted on one end of the extension column (7).

2. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 1, characterized in that: The sealing ring plug (202) is provided with a plurality of air inlets (19), and a one-way air inlet valve (20) is fixedly installed in each air inlet (19); a pair of hoop frames (104) are fixedly installed between the mounting frame (103) and the reactor body (1); and a frame-type top frame (105) is fixedly installed between the top frame (2) and the mounting frame (103).

3. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 1, characterized in that: A top ring (5) is rotatably mounted on the inner wall of the top of the reactor body (1), and a plurality of pairs of side rods (9) are fixedly mounted on the outer wall of the top ring (5), and a U-shaped bottom frame (901) is fixedly mounted on the bottom end of each pair of side rods (9). A liquid supply pipe (101) with a valve is fixedly connected to one side of the reactor body (1) close to the top, and a discharge pipe (102) with a valve is fixedly connected to the bottom end of the reactor body (1).

4. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 3, characterized in that: The stirring assembly comprises an L-shaped end rod (902) rotatably mounted on one end of a U-shaped base frame (901), and a plurality of hook-shaped cavity blocks (903) are fixedly mounted near the bottom of the L-shaped end rod (902), each of the hook-shaped cavity blocks (903) being narrow at the top and wide at the bottom, and an oblong notch (904) is formed at the end of each L-shaped end rod (902), and a ring rod (12) is movably mounted on the plurality of L-shaped end rods (902) through the oblong notch (904), and a pair of abutment ring sheets (121) are fixedly mounted on the ring rod (12) near the oblong notch (904).

5. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 4, characterized in that: The stirring assembly further comprises a plurality of bottom connecting rods (15) fixedly mounted on the bottom of the top ring (5); a convex key cylinder (8) and a sleeve ring (123) are rotatably mounted on one end of the extension column (7) via a bearing; the convex key cylinder (8) and the sleeve ring (123) are fixedly connected; the convex key cylinder (8) is slidably connected to the rotating plate (6) in the vertical direction; and a plurality of connecting ribs (122) are fixedly connected between the sleeve ring (123) and the ring rod (12).

6. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 5, characterized in that: A connecting ring block (151) is fixedly mounted on the ends of the plurality of bottom connecting rods (15), and the connecting ring block (151) is rotatably connected to the convex key cylinder (8) in the vertical direction. The convex key cylinder (8) forms a key connection with the rotating plate (6) and the connecting ring block (151). A cone panel (16) is fixedly mounted on the bottom end of the connecting ring block (151), and a plurality of arc grooves (161) distributed at equal distances are formed on the surface of the cone panel (16). The plurality of bottom through pipes (10) are fixedly passed through the sleeve ring (123).

7. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 5, characterized in that: A plurality of groups of vertical rods (17) are fixedly mounted on each of the connecting bars (122), and a bottom plate (171) is fixedly mounted on the bottom end of each group of vertical rods (17), and a plurality of X-shaped notches (172) are formed on each of the bottom plates (171).

8. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 3, characterized in that: A mounting plate is fixed on the top of the reactor body (1), and a driving motor (3) is fixedly mounted on one side of the mounting plate, and a transmission rod (301) that movably penetrates the reactor body (1) is fixed to the output shaft of the driving motor (3), a transmission gear 1 (302) and a transmission gear 2 (303) are fixedly mounted on the transmission rod (301), and an outer gear ring (401) is fixedly mounted on the outer wall of the grinding bucket (4), and the outer gear ring (401) is meshed with the transmission gear 1 (302).

9. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 8, characterized in that: Evenly distributed convex teeth (501) are fixedly mounted on the inner peripheral wall of the top ring (5), and the second transmission gear (303) meshes with the convex teeth (501).

10. An ultrasonic crystallization process for preparing high-purity ethyl maltol, which is applied to the ultrasonic crystallization device for preparing high-purity ethyl maltol according to any one of claims 1 to 9, characterized in that: The specific steps include: Step 1, dissolving: placing ethyl maltol in a reaction kettle (1) and dissolving it in ethanol to obtain an ethyl maltol solution, the dissolving temperature of which is 40-45° C.; Step 2: Control the temperature of the reactor (1) to 25°C, the frequency of the ultrasonic oscillator (701) to 30KHz, and the treatment time to 2-3h to induce the precipitation of fine impurities; Step 3, introducing the liquid obtained in step 2 into a filter to filter and remove fine impurity crystals; then introducing the liquid into a decolorizer to remove trace impurities dissolved in the ethyl maltol clear liquid, and obtaining a refined ethyl maltol solution; Step 4: placing the refined ethyl maltol solution in the reaction vessel (1) again, controlling the refined ethyl maltol solution to slowly cool to 0°C, performing cooling crystallization, and then separating and drying to obtain high-purity ethyl maltol.

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