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

Abstract

The invention discloses an ultrasonic crystallization device for preparing high-purity ethyl maltol and a process thereof, relating to the technical field of ethyl maltol preparation. The device comprises an installation stand and a reactor body, wherein a rotating plate is rotatably installed on the top of the reactor body, and further comprises a grinding component, a stirring component and an ultrasonic oscillation component. The device can refine powder in a grinding area to avoid agglomeration. On the other hand, when a subsequent hydraulic rod moves downward, it can drive a sealing ring plug to move downward, thereby allowing a portion of air in an inner grinding cylinder to pass into an annular cavity through a one-way air outlet valve, and finally to be diverted through multiple oblique branches and blown into a drop hole on the rotating plate, thereby promoting the falling of the powder. At the same time, another portion of air in the inner grinding cylinder is aerated into the reactor body through a bottom through-pipe and the one-way air outlet valve, thereby achieving the effects of assisting material dissolution and promoting subsequent crystallization.

Description

Technical Field

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

[0002] As an important food additive and flavoring ingredient, the production of high-purity ethyl maltol requires extremely high efficiency and quality in the crystallization process. In the prior art, the preparation of ethyl maltol typically involves key steps such as raw material dissolution, solution concentration, and crystallization. The uniformity and efficiency of the raw material dissolution stage directly impact the crystal form, purity, and yield of the subsequent crystallization process. However, the dissolution process currently used in industry has significant drawbacks and is in urgent need of improvement.

[0003] Specifically, during the raw material dissolution process, when powdered ethyl maltol or its precursor material is added to a solvent (such as ethanol or a water-ethanol mixed solution), it is very easy to agglomerate and clump due to the hydrophilicity of the material or surface electrostatic effects. The formation of these agglomerates not only leads to a significant reduction in the contact area between the material and the solvent, but also prolongs the dissolution time, and even requires additional increases in the solvent temperature or extended mechanical stirring time to promote dispersion. Although traditional dissolution equipment is usually equipped with a mechanical stirring unit (such as a paddle or magnetic stirrer), the stirring method that relies solely on shear force and convection has limited improvement on the agglomeration problem of micron-sized powders, especially in the initial stage of material feeding or in high-concentration systems. It is difficult for stirring to quickly penetrate and disperse dense agglomerates. In addition, excessive reliance on stirring may lead to local temperature unevenness or the introduction of bubbles, further affecting the dissolution efficiency and solution stability.

[0004] The problem of insufficient dissolution will be directly transmitted to the subsequent crystallization process. Incompletely dissolved microparticles may become heterogeneous crystal nuclei, resulting in inconsistent crystal growth rates, mixed crystal forms or impurities, and ultimately reducing product purity and yield. Although the existing technology attempts to alleviate the agglomeration problem by optimizing stirring parameters (such as rotation speed, blade shape), these methods often increase 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 micro-jet action, but there is no special device design for the ethyl maltol dissolution-crystallization process in existing patents and literature. In particular, how to efficiently couple ultrasonic energy to the dissolution stage to simultaneously inhibit agglomeration, accelerate dissolution, and synergistically improve the crystallization effect is still a blank. Summary of the Invention

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

[0006] The technical solution of the present invention is: an ultrasonic crystallization device for preparing high-purity ethyl maltol, comprising a mounting stand and a reaction kettle body, wherein a rotating plate is rotatably mounted on the top of the reaction kettle body, and further comprising a grinding component, a stirring component, and an ultrasonic oscillation component;

[0007] The grinding assembly includes a bearing seat fixedly mounted on the top of the reactor body, the bearing seat and the rotating plate are coaxially arranged, a grinding bucket is rotatably mounted in the bearing seat, a coaxially arranged grinding inner cylinder is fixedly mounted on the surface of the rotating plate, the outer side of the grinding inner cylinder and the grinding bucket constitute a grinding area, the rotating plate is provided with evenly distributed blanking holes near the edge, the grinding inner cylinder is provided with an annular cavity near the bottom, the bottom of the grinding inner cylinder is provided with multiple groups of oblique branches connected to the annular cavity, the inner wall of the grinding inner cylinder is provided with multiple mounting ports connected to the annular cavity, and a one-way air outlet valve 1 is fixedly installed inside each mounting port, a multiple bottom through-tubes distributed at equal distances are fixedly passed through the position of the rotating plate near the grinding inner cylinder, and a one-way air outlet valve 2 is fixedly installed at the bottom end of each bottom through-tube;

[0008] The ultrasonic oscillator assembly includes a top stand fixedly mounted on the top of the reactor body, and a hydraulic rod is fixedly mounted on one side of the top stand, an extension column is fixed on the output shaft of the hydraulic rod, and an ultrasonic oscillator is fixedly mounted on the end of the extension column, and a sealing ring plug that slides with the grinding inner cylinder is fixedly mounted on one end of the extension column.

[0009] Preferably, the sealing ring plug is provided with a plurality of air inlets, and a one-way air inlet valve is fixedly installed in each air inlet, a pair of hoops are fixedly installed between the mounting stand and the reactor body, and a frame-type top frame is fixedly installed between the top stand and the mounting stand.

[0010] Preferably, a top ring is rotatably mounted on the top inner wall of the reactor body, and multiple pairs of side rods are fixedly mounted on the outer side wall of the top ring, and a U-shaped base frame is fixedly mounted on the bottom end of each pair of side rods. A liquid supply pipe with a valve is fixedly connected to one side of the reactor body close to the top, and a discharge pipe with a valve is fixedly connected to the bottom end of the reactor body.

[0011] Preferably, the stirring assembly includes an L-shaped end rod rotatably mounted on one end of the U-shaped base frame, and a plurality of hook-shaped cavity blocks are fixedly mounted near the bottom end of the L-shaped end rod, each of the hook-shaped cavity blocks is narrow at the top and wide at the bottom, and an oblong groove is provided at the end of each of the L-shaped end rods, and a ring rod is movably mounted together through the oblong groove, and a pair of abutment ring plates are fixedly mounted on the ring rod near the oblong groove.

[0012] Preferably, the stirring assembly also includes a plurality of bottom connecting rods fixedly mounted on the bottom of the top ring, and a convex key cylinder and a sleeve are rotatably mounted on one end of the extension column through a bearing, the convex key cylinder is fixedly connected to the sleeve, and the convex key cylinder is slidably connected to the rotating plate in the vertical direction, and a plurality of connecting ribs are fixedly connected between the sleeve and the ring rod.

[0013] Preferably, the ends of the plurality of bottom connecting rods are commonly fixedly mounted with a connecting ring block, 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, the bottom end of the connecting ring block is fixedly mounted with a conical panel, and the surface of the conical panel is provided with a plurality of equally spaced arc grooves, and the plurality of bottom through pipes are fixedly passed through the sleeve.

[0014] Preferably, a plurality of groups of vertical rods are fixedly mounted on each of the connecting bars, and a bottom plate is fixedly mounted on the bottom end of each group of vertical rods, and a plurality of X-shaped slots are provided on each of the bottom plates.

[0015] Preferably, a mounting plate is fixed on the top of the reactor body, and a drive motor is fixedly mounted on one side of the mounting plate, and a transmission rod that movably passes through the reactor body is fixed on the output shaft of the drive motor, and transmission gear 1 and transmission gear 2 are fixedly mounted on the transmission rod, and an outer gear ring is fixedly mounted on the outer wall of the grinding bucket, and the outer gear ring is meshed with transmission gear 1.

[0016] Preferably, evenly distributed convex teeth are fixedly mounted on the inner peripheral wall of the top ring, and the second transmission gear is engaged with the convex teeth.

[0017] The present invention also discloses an ultrasonic crystallization process for preparing high-purity ethyl maltol, which specifically comprises the following steps:

[0018] Step 1: Dissolving: placing ethyl maltol in a reaction vessel and dissolving it in ethanol to obtain an ethyl maltol solution at a dissolving temperature of 40-45°C;

[0019] Step 2: Control the temperature of the reactor to 25°C, the frequency of the ultrasonic oscillator to 30 kHz, and the treatment time to 2-3 hours to induce the precipitation of fine impurities;

[0020] 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 solution to obtain a refined ethyl maltol solution;

[0021] Step 4: placing the refined ethyl maltol solution in the reactor 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.

[0022] The present invention provides an ultrasonic crystallization device and process for preparing high-purity ethyl maltol through improvement, which has the following improvements and advantages compared with the prior art:

[0023] Firstly, when the present invention is actually used, powder can be added to the grinding hopper, and the grinding hopper and the grinding inner cylinder can rotate in opposite directions to refine the powder in the grinding area, thereby avoiding agglomeration. Secondly, when the hydraulic rod moves downward, it can drive the sealing ring plug to move downward, thereby allowing a portion of the air in the grinding inner cylinder to pass into the annular cavity through the one-way air outlet valve, and finally to be diverted through multiple oblique branches and blown into the drop holes on the rotating plate, thereby promoting the falling of the powder. At the same time, another portion of the air in the grinding inner cylinder is aerated into the reactor body through the bottom through-pipe and the one-way air outlet valve, thereby achieving the effect of assisting the dissolution of the material and promoting subsequent crystallization.

[0024] Secondly, when the multiple L-shaped end rods of the present invention rotate with the center of the reactor body as the center of the circle, the hook-shaped cavity block provided can stir the material. At the same time, since the hook-shaped cavity block is narrow at the top and wide at the bottom, the material can enter from the wide opening at the bottom end of the hook-shaped cavity block and then be discharged from the narrow opening at the top. In this process, the narrow tube effect is utilized to increase the flow rate of the material, thereby promoting the mixing between the materials. When the hydraulic rod is running, it can drive the convex key cylinder and the sleeve ring to move vertically, and then cooperate with the connecting reinforcement to drive the ring rod to move synchronously. When the ring rod moves vertically, it can cooperate with the oblong groove to drive the L-shaped end rod to flip along the connection with the U-shaped base frame, thereby adjusting the stirring angle and range to achieve the purpose of improving the mixing effect, thereby promoting the dissolution of the material.

[0025] Thirdly, when the bottom connecting rod drives the connecting ring block to rotate, the conical panel can be driven to rotate synchronously. The multiple arc grooves provided in combination can further divert the material falling from the rotating plate, thereby achieving more uniform addition of the powder, which is beneficial to the dissolution of the material. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the specific embodiments or the description of the prior art. Obviously, the drawings described below are 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.

[0027] Figure 1 It is a schematic diagram of the overall three-dimensional structure of the present invention;

[0028] Figure 2 This is a schematic diagram of the internal structure of the reactor body of the present invention;

[0029] Figure 3 This is a schematic diagram of the cross-sectional structure of the reactor body of the present invention;

[0030] Figure 4 For the present invention Figure 3 A in the middle is an enlarged structural diagram;

[0031] Figure 5 This is a schematic diagram of the three-dimensional structure of the hook-shaped cavity block of the present invention;

[0032] Figure 6 This is a schematic diagram of the planar structure of the extension column of the present invention;

[0033] Figure 7 For the present invention Figure 6 The enlarged structural diagram at B in the middle;

[0034] Figure 8 This is a schematic diagram of the three-dimensional structure of the top ring and grinding bucket of the present invention;

[0035] Figure 9 Schematic diagram of the three-dimensional structure of the ring rod and the rotating plate of the present invention;

[0036] Figure 10 It is a schematic diagram of the three-dimensional structure of the cone plate, the grinding inner cylinder and the convex key cylinder of the present invention;

[0037] Figure 11 For the present invention Figure 6 Enlarged structural diagram at point C in the middle.

[0038] Reference numerals:

[0039] 1. Reactor body; 101. Liquid supply pipe with valve; 102. Discharge pipe with valve; 103. Mounting stand; 104. Hoop frame; 105. Frame-type top frame; 2. Top stand; 201. Hydraulic rod; 202. Sealing ring plug; 3. Drive motor; 301. Transmission rod; 302. Transmission gear 1; 303. Transmission gear 2; 4. Grinding bucket; 401. Outer gear ring; 402. Grinding inner cylinder; 5. Top ring; 501. Protruding teeth; 6. Rotating plate; 601. Dropping hole; 7. Extension column; 701. Ultrasonic oscillator; 8. Protruding key cylinder; 9. , side rod; 901, U-shaped base frame; 902, L-shaped end rod; 903, hook-shaped cavity block; 904, oblong notch; 10, bottom through pipe; 11, one-way air outlet valve 2; 12, ring rod; 121, abutment ring; 122, connecting rib; 123, sleeve ring; 13, ring cavity; 14, oblique branch; 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, one-way air inlet valve; 21, one-way air outlet valve 1. DETAILED DESCRIPTION

[0040] The present invention is described in detail below, clearly and completely describing the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0041] The present invention provides an ultrasonic crystallization device and process for preparing high-purity ethyl maltol through improvement. The technical solution of the present invention is:

[0042] like Figures 1 to 11 As shown, an embodiment of the present invention provides an ultrasonic crystallization device for preparing high-purity ethyl maltol, including a mounting stand 103 and a reactor body 1, a rotating plate 6 is rotatably mounted on the top of the reactor body 1, and further includes a grinding component, a stirring component and an ultrasonic oscillation component; the grinding component is provided for feeding and grinding the powder to achieve uniform addition of the powder; it should be noted that, in the present application, the reactor body 1 has a temperature regulation function, which belongs to the prior art, so its temperature regulation principle and related structure are no longer described.

[0043] The grinding assembly includes a bearing seat 18 fixedly mounted on the top of the reactor body 1, the bearing seat 18 and the rotating plate 6 are coaxially arranged, a grinding bucket 4 is rotatably mounted in the bearing seat 18, a coaxially arranged grinding inner cylinder 402 is fixedly mounted on the surface of the rotating plate 6, the outer side of the grinding inner cylinder 402 and the grinding bucket 4 form a grinding area, the rotating plate 6 is provided with evenly distributed drop holes 601 near the edge, the grinding inner cylinder 402 is provided with an annular cavity 13 near the bottom, the bottom of the grinding inner cylinder 402 is provided with multiple groups of oblique branches 14 connected to the annular cavity 13, and the grinding inner cylinder 402 is provided with a plurality of oblique branches 14 connected to the annular cavity 13. The inner wall is provided with a plurality of mounting openings communicating 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-tubes 10 distributed at equal distances are fixedly passed through the rotating plate 6 near the grinding inner cylinder 402, and a one-way air outlet valve 11 is fixedly installed at the bottom end of each bottom through-tube 10. With the above structure, in actual use, powder can be added to the grinding hopper 4, and the grinding hopper 4 and the grinding inner cylinder 402 are rotated in opposite directions to refine the powder in the grinding zone, thereby avoiding agglomeration.

[0044] On the other hand, when the subsequent hydraulic rod 201 moves downward, it can drive the sealing ring plug 202 to move downward, thereby allowing a portion of the air in the grinding inner cylinder 402 to pass into the annular cavity 13 through the one-way air outlet valve 21, and finally be diverted through multiple oblique branches 14 and blown into the drop hole 601 on the rotating plate 6, thereby promoting the falling of the powder; at the same time, another portion of the air in the grinding inner cylinder 402 is aerated into the reactor body 1 through the bottom through pipe 10 and the one-way air outlet valve 2 11, thereby achieving the effect of assisting the dissolution of the material and promoting subsequent crystallization.

[0045] The ultrasonic oscillation component includes a top stand 2 fixedly mounted on the top of the reactor 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 slides with the grinding inner cylinder 402 is fixedly mounted on one end of the extension column 7; through the above structure, the hydraulic rod 201 is arranged to cooperate with the extension column 7 to adjust the height of the ultrasonic oscillator 701, thereby realizing dynamic oscillation of the material in the reactor body 1, further improving the material dissolution and crystallization effects.

[0046] Furthermore, a plurality of air inlets 19 are provided on 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 mounting stand 103 and the reactor body 1, and a frame-type top frame 105 is fixedly installed between the top stand 2 and the mounting stand 103; it should be noted that a filter plate can be provided at the opening of the one-way air inlet valve 20. Through the above structure, 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 plate and passed into the inner side of the grinding inner cylinder 402 to maintain air pressure balance.

[0047] Furthermore, a top ring 5 is rotatably installed on the top inner wall of the reactor body 1, and a plurality of pairs of side rods 9 are fixedly installed on the outer wall of the top ring 5, and a U-shaped base frame 901 is fixedly installed on the bottom end of each pair of side rods 9. A valved liquid supply pipe 101 is fixedly connected to the side of the reactor body 1 close to the top, and a valved discharge pipe 102 is fixedly connected to the bottom end of the reactor body 1; the valved liquid supply pipe 101 is provided for adding liquid material into the reactor body 1; and the valved discharge pipe 102 is provided for unloading the material after stirring is completed.

[0048] As a further solution of the present invention, the stirring assembly includes an L-shaped end rod 902 rotatably mounted on one end of the U-shaped base frame 901, and a plurality of hook-shaped cavity blocks 903 are fixedly mounted near the bottom end of the L-shaped end rod 902, each hook-shaped cavity block 903 is narrow at the top and wide at the bottom, and an oblong slot 904 is opened at the end of each L-shaped end rod 902, and a plurality of L-shaped end rods 902 are movably mounted with a ring rod 12 through the oblong slot 904, and a pair of abutment ring pieces 121 are fixedly mounted on the ring rod 12 near the oblong slot 904; through the above structure, when the plurality of L-shaped end rods 902 rotate with the center of the reactor body 1 as the center of the circle, the set hook-shaped cavity block 903 can stir the material, and at the same time, since the hook-shaped cavity block 903 is narrow at the top and wide at the bottom, the material can enter from the wide mouth at the bottom end of the hook-shaped cavity block 903 and then be discharged from the narrow mouth at the top. In this process, the narrow tube effect is utilized to increase the flow rate of the material, thereby promoting the mixing between the materials.

[0049] As a further embodiment of the present invention, 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 collar 123 are rotatably mounted on one end of the extension column 7 through a bearing. 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. Through the above structure, when the top ring 5 rotates, the bottom connecting rods 15 can drive the connecting ring block 151 to rotate, and the connecting ring block 151 can drive the convex key cylinder 8 and the collar 123 to rotate.

[0050] When the top ring 5 rotates, it can cooperate with the side rods 9 and the U-shaped base frame 901 to drive the L-shaped end rods 902 to rotate. In addition, the collar 123 can cooperate with the connecting rib 122 to drive the ring rod 12 to rotate, and cooperate with the provided abutment ring piece 121 to synchronously apply a rotational driving force to the L-shaped end rods 902, so that the multiple L-shaped end rods 902 can drive the hook-shaped cavity block 903 to rotate stably.

[0051] On the other hand, when the hydraulic rod 201 is running, it can drive the convex key cylinder 8 and the ring 123 to move vertically, and then 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 groove 904 to drive the L-shaped end rod 902 to flip along the connection with the U-shaped base frame 901, and then adjust the stirring angle and range to achieve the purpose of improving the mixing effect, thereby promoting the dissolution of the material.

[0052] Furthermore, the ends of the multiple bottom connecting rods 15 are commonly fixedly installed with a connecting ring block 151, 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. The bottom end of the connecting ring block 151 is fixedly installed with a conical panel 16, and the surface of the conical panel 16 is provided with a plurality of equally distributed arc grooves 161, and a plurality of bottom through-tubes 10 are fixedly passed through the sleeve 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, and the multiple arc grooves 161 provided in conjunction with the provided can further divert the material falling from the rotating plate 6, achieve more uniform addition of the powder, and thus facilitate the dissolution of the material.

[0053] As a further embodiment of the present invention, Figure 9-10 As shown, multiple groups of vertical rods 17 are fixedly installed on each connecting rib 122, and a bottom plate 171 is fixedly installed on the bottom end of each group of vertical rods 17. Each bottom plate 171 is provided with multiple X-shaped slots 172; when the ring rod 12 moves vertically, it can cooperate with the vertical rods 17 to drive the bottom plate 171 to move vertically, and the X-shaped slots 172 provided can further improve the mixing effect.

[0054] Furthermore, a mounting plate is fixed to the top of the reactor body 1, and a drive motor 3 is fixedly mounted on one side of the mounting plate. A transmission rod 301 that movably penetrates the reactor body 1 is fixed to the output shaft of the drive motor 3. A transmission gear 1 302 and a transmission gear 2 303 are fixedly mounted on the transmission rod 301. 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. Through the above structure, when the drive motor 3 is in operation, it can drive the top ring 5 to rotate through the cooperation of the transmission gear 2 303 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.

[0055] On the other hand, when the driving motor 3 is running, the grinding bucket 4 can be driven to rotate through the transmission gear 1 302 and the outer gear ring 401. At this time, the grinding bucket 4 and the grinding inner cylinder 402 rotate towards each other to complete the grinding and feeding operations.

[0056] Furthermore, evenly distributed protruding teeth 501 are fixedly mounted on the inner circumference of the top ring 5, and the second transmission gear 303 meshes with the protruding teeth 501. Through the above structure, the second transmission gear 303 can form a transmission cooperation with the protruding teeth 501. The specific working method is as follows: during use, liquid material is introduced into the interior of the reactor body 1 through the valved liquid supply pipe 101, and the well-proportioned powder material is added to the grinding hopper 4. Under the action of gravity, the powder material enters the grinding area between the grinding hopper 4 and the grinding inner cylinder 402.

[0057] The drive motor 3 is started, and the top ring 5 is driven to rotate through the cooperation of the transmission gear 2 303 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 drive motor 3 is running, it can drive the grinding bucket 4 to rotate through the transmission action of the transmission gear 1 302 and the outer gear ring 401. At this time, the grinding bucket 4 and the grinding inner cylinder 402 rotate in opposite directions to complete the grinding process, so that the powder is refined in the grinding zone and agglomeration is avoided.

[0058] On the other hand, when the subsequent hydraulic rod 201 moves downward, it can drive the sealing ring plug 202 to move downward, thereby allowing a portion of the air in the grinding inner cylinder 402 to pass into the annular cavity 13 through the one-way air outlet valve 1 21, and finally be diverted through multiple oblique branches 14 and blown into the drop hole 601 on the rotating plate 6, thereby promoting the falling of the powder; at the same time, another portion of the air in the grinding inner cylinder 402 is aerated into the reactor body 1 through the bottom through-tube 10 and the one-way air outlet valve 2 11, thereby achieving the effect of assisting the dissolution of the material and promoting subsequent crystallization; the provided hydraulic rod 201 can be used in conjunction with the extension column 7 to adjust the height of the ultrasonic oscillator 701, thereby achieving dynamic oscillation of the material in the reactor body 1, further improving the material dissolution and crystallization effects;

[0059] 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 and then passed into the inner side of the grinding inner cylinder 402 to maintain the air pressure balance;

[0060] When the multiple L-shaped end rods 902 rotate with the center of the reactor body 1 as the center of the circle, the hook-shaped cavity block 903 provided can stir the material. At the same time, since the hook-shaped cavity block 903 is narrow at the top and wide at the bottom, the material can enter from the wide opening at the bottom end of the hook-shaped cavity block 903 and then be discharged from the narrow opening at the top. In this process, the narrow tube effect is used to increase the flow rate of the material, 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 use the connecting ring block 151 to drive the convex key cylinder 8 and the sleeve ring 123 to rotate. When the top ring 5 rotates, it can cooperate with the side rod 9 and the U-shaped base frame 901 to drive the L-shaped end rod 902 to rotate, and the sleeve ring 123 can cooperate with the connecting rib 122 to drive the ring rod 12 to rotate, and cooperate with the provided abutment 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 is running, it can drive the convex key cylinder 8 and the collar 123 to move vertically, and then 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 base frame 901, thereby adjusting the stirring angle and range to achieve the purpose of improving the mixing effect, thereby promoting the dissolution of the material; 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 materials are mixed, the temperature of the reactor body 1 is controlled to drop to 25°C, the frequency of the ultrasonic oscillator 701 is 30KHz, and the processing time is 2-3h to induce the precipitation of fine impurities;

[0061] The valved discharge pipe 102 is opened, and the liquid is introduced into a filter for filtration to remove fine impurity crystals; the liquid is then introduced into a decolorizer to remove trace impurities dissolved in the ethyl maltol clear liquid to obtain a refined ethyl maltol solution; finally, the refined ethyl maltol solution is placed back into the reactor body 1, and the reactor body 1 is used to control the refined ethyl maltol solution to slowly cool to 0°C for cooling crystallization, and then separated and dried to obtain high-purity ethyl maltol.

[0062] An ultrasonic crystallization process for preparing high-purity ethyl maltol specifically comprises the following steps:

[0063] Step 1, dissolving: placing ethyl maltol in the reaction vessel 1 and dissolving it in ethanol to obtain an ethyl maltol solution at a dissolution temperature of 40-45°C;

[0064] Step 2: Control the temperature of the reactor 1 to 25°C, set the frequency of the ultrasonic oscillator 701 to 30 kHz, and process for 2-3 hours to induce the precipitation of fine impurities;

[0065] 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 solution to obtain a refined ethyl maltol solution;

[0066] Step 4: Place the refined ethyl maltol solution in the reactor body 1 again, control the refined ethyl maltol solution to slowly cool to 0° C., perform cooling crystallization, and then separate and dry to obtain high-purity ethyl maltol.

[0067] The above description is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to 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 reactor body (1), characterized in that: The top of the reactor 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 reactor body (1), the bearing seat (18) and the rotating plate (6) are coaxially arranged, a grinding bucket (4) is rotatably mounted in the bearing seat (18), a coaxially arranged grinding inner cylinder (402) is fixedly mounted on the surface of the rotating plate (6), the outer side of the grinding inner cylinder (402) and the grinding bucket (4) form a grinding area, the rotating plate (6) is provided with evenly distributed drop holes (601) near the edge, and the grinding inner cylinder (402) is provided with a plurality of holes (601) near the bottom. The grinding inner cylinder (402) has a plurality of oblique branches (14) in communication with the annular cavity (13), and the inner wall of the grinding inner cylinder (402) has 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-tubes (10) distributed at equal distances are fixedly passed through the rotating plate (6) at a position 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-tube (10); The ultrasonic oscillator assembly comprises a top stand (2) fixedly mounted on the top of the reactor 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 is slidably matched with the grinding inner cylinder (402) is fixedly mounted on one end of the extension column (7); 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 stand (103) and the reactor body (1); and a frame-type top frame (105) is fixedly installed between the top stand (2) and the mounting stand (103); 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 base 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) near the top, and a discharge pipe (102) with a valve is fixedly connected to the bottom end of the reactor body (1); 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 provided 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 pieces (121) are fixedly mounted on the ring rod (12) near the oblong notch (904).

2. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 1, wherein: 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 collar (123) are rotatably mounted on one end of the extension column (7) via a bearing; 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); The ends of the plurality of bottom connecting rods (15) are commonly fixedly mounted with a connecting ring block (151), 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). The bottom end of the connecting ring block (151) is fixedly mounted with a cone panel (16), and the surface of the cone panel (16) is provided with a plurality of equally spaced arc grooves (161). The plurality of bottom through pipes (10) are all fixedly passed through the collar (123).

3. A high-purity ethyl maltol preparation ultrasonic crystallization device according to claim 2, characterized in that: A plurality of groups of vertical rods (17) are fixedly mounted on each connecting rib (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 bottom plate (171).

4. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 2, wherein: 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. 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). 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).

5. The ultrasonic crystallization device for preparing high-purity ethyl maltol according to claim 4, wherein: Evenly distributed convex teeth (501) are fixedly mounted on the inner peripheral wall of the top ring (5), and the second transmission gear (303) is meshed with the convex teeth (501).

6. 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 5, characterized in that: The specific steps include: Step 1, dissolving: placing ethyl maltol in a reaction vessel (1) and dissolving it in ethanol to obtain an ethyl maltol solution at a dissolution temperature of 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 solution to obtain 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 to 0°C, perform cooling crystallization, and then separate and dry to obtain high-purity ethyl maltol.

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