Method for preparing carvacrol from p-cymene
By using technical means such as dual drive mechanisms and rotary dispersion disks in the reactor, the contact area between air and mixed materials is increased, and the problem of low oxidation reaction rate in the prior art is solved, and efficient carvacrol production is achieved.
Patent Information
- Application Number
- CN202411652829.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-19
- Publication Date
- 2025-02-14
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
In the prior art, due to the large input amount of compressed air and the fast flow rate, the mixed material inside the reactor flows away from the outlet position under the push of the air flow, forming a limited contact area, reducing the oxidation reaction rate, and increasing production time and cost.
The dual driving mechanism is used to drive the compressed air dispersion mechanism and the bubble forming mechanism to move downward synchronously, and the contact area between the air and the mixed material is increased by rotating the dispersion disk and the bubble forming mechanism, thereby increasing the oxidation reaction rate.
By increasing the contact area between air and mixed materials, the oxidation reaction rate is significantly improved, the compressed air input time is shortened, the production efficiency of carvacrol products is improved, and the production cost is reduced.
Smart Images

Figure CN119425538A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of carvacrol preparation, and in particular to a method for preparing carvacrol from p-cymene. Background Art
[0002] Carvacrol is a colorless to light yellow thick oily liquid with the smell of thymol. It can be used in the production of spices, food additives, antioxidants, sanitary disinfectants, insect repellents, deodorants and pharmaceutical intermediates.
[0003] The invention patent with the authorization announcement number CN115448819B discloses a method for preparing carvacrol from p-cymene, which comprises: dissolving p-cymene with a solvent, adding a self-made copper catalyst, then adding a tetramethylpiperidinium oxide catalyst, stirring, and introducing compressed air as an oxidant to oxidize p-cymene to carvacrol. After the reaction is completed, a 10% sodium bicarbonate solution is added for quenching. The reaction is allowed to stand until the oil phase and the water phase are separated, and the solvent in the oil phase is distilled out after the oil phase is separated to obtain a crude carvacrol product after the solvent is removed, and the crude carvacrol product enters a distillation tower for purification to obtain a finished carvacrol product.
[0004] This invention innovatively oxidizes para-cymene into carvacrol by directly introducing air into the air under the action of a catalyst. This process is simple and has the characteristics of easy industrial production, high production efficiency and large product profit margin.
[0005] However, after actual application by technicians skilled in the art, it was found that the above preparation method still has some shortcomings. The most obvious one is that due to the large amount of compressed air input and the fast flow rate, when it is input into the mixed material, since the gas outlet position is single and fixed in one place, the mixed material inside the reactor will flow away from the gas outlet position under the push of the airflow and accumulate, which will lead to the limitation of the contact area between the compressed air and the mixed material, which has a great impact on the oxidation reaction rate.
[0006] Therefore, it takes a long time for the compressed air to be input to complete the reaction, which reduces production efficiency and increases production costs.
[0007] Therefore, it is necessary to invent a method for preparing carvacrol from p-cymene to solve the above problems. Summary of the invention
[0008] The object of the present invention is to provide a method for preparing carvacrol from para-cymene, wherein a dual driving mechanism is used to drive a compressed air dispersion mechanism and a bubble forming mechanism to move downward synchronously, and the compressed air dispersion mechanism rotates due to the driving of the dual driving mechanism during the descent process, and the compressed air dispersion mechanism drives multiple groups of bubble forming mechanisms to rotate synchronously when rotating, thereby mixing the mixed material, and after the compressed air dispersion mechanism arrives at the reaction station at the bottom of the inner cavity of the reactor, the compressed air input mechanism inputs a compressed air flow into the compressed air dispersion mechanism, and at this time, the compressed air flow forms multiple air columns and enters the mixed material, and at this time, due to the rotation of the bubble forming mechanism, the rising air column is continuously divided and forms a large number of bubbles, so as to increase the mixing of air and the mixed material. In addition, the subsequent dual-drive mechanism can also trigger the bubble forming mechanism, so that it can rotate while revolving, so as to increase the bubble generation rate, so as to solve the problem raised in the above background technology that due to the large amount of compressed air input and the fast flow rate, when it is input into the mixed material, since the gas outlet position is single and fixed in one place, the mixed material inside the reactor will flow away from the gas outlet position under the push of the airflow and accumulate, which will lead to the limitation of the contact area between the compressed air and the mixed material, which has a great influence on the oxidation reaction rate. Therefore, it takes a long time for the compressed air to input to complete the reaction, which reduces the production efficiency and also causes the problem of increased production cost.
[0009] To achieve the above-mentioned object, the present invention provides the following technical scheme: a method for preparing carvacrol from p-cymene, wherein the method for preparing carvacrol from p-cymene is implemented by a carvacrol preparation device, wherein the carvacrol preparation device comprises a reactor, wherein a heating resistor is arranged inside the reactor, a dual driving mechanism is arranged at the top of the inner cavity of the reactor, a compressed air dispersion mechanism is arranged at the bottom end of the dual driving mechanism, a plurality of groups of bubble forming mechanisms are evenly arranged at the top edge of the compressed air dispersion mechanism, and a compressed air input mechanism is arranged at the top of the outer side of the compressed air dispersion mechanism; The dual drive mechanism drives the compressed air dispersion mechanism and the bubble forming mechanism to move downward synchronously to reach the reaction station at the bottom of the inner cavity of the reactor. The compressed air input mechanism inputs compressed air flow into the compressed air dispersion mechanism. The dual drive mechanism drives the compressed air dispersion mechanism to rotate continuously so that the compressed air flow forms multiple air columns and enters into the mixed material. The compressed air dispersion mechanism drives the bubble forming mechanism to rotate synchronously to divide the rising air columns to form bubbles. The dual drive mechanism triggers the bubble forming mechanism to make it rotate while revolving.
[0010] Preferably, the dual drive mechanism comprises a reciprocating screw, a drive motor, a square slide, an outer sleeve, a return spring and an inner sleeve; The reciprocating screw penetrates the top of the reactor and extends into the interior of the reactor and is rotationally connected to the reactor through a bearing. The driving motor is fixedly arranged on the top of the reactor and is transmission-connected to the reciprocating screw. The square slide groove is opened at the bottom end of the reciprocating screw. The outer sleeve, the return spring and the inner sleeve are sequentially sleeved on the outside of the reciprocating screw from top to bottom. The outer sleeve is transmission-connected to the reciprocating screw. The return spring is fixedly connected between the outer sleeve and the inner sleeve. The inner sleeve is slidably connected to the reciprocating screw and is slidably nested in the inner side of the outer sleeve along the vertical direction.
[0011] Preferably, the dual drive mechanism further comprises an outer sleeve plate, a drive ring and a threaded hole; The outer sleeve plate is fixedly sleeved on the outer bottom of the outer sleeve, and the drive ring is rotatably sleeved on the outer side of the outer sleeve plate through a bearing. There are multiple threaded holes, and the multiple threaded holes are evenly penetrated and arranged on the top of the drive ring.
[0012] Preferably, the compressed air dispersion mechanism comprises a square slide bar, a connecting tube, an air inlet, a dispersion disk, a dispersion hole and a rotating base; The square slide bar is slidably arranged on the inner side of the square slide groove along the vertical direction, the connecting tube is fixedly arranged on the bottom of the square slide bar and is rotatably connected to the inner sleeve through a bearing, two air inlet holes are arranged, and the two air inlet holes are respectively opened on the top of both sides of the connecting tube, the dispersion disk is fixedly sleeved and arranged on the outer bottom of the connecting tube, and a plurality of dispersion holes are arranged, and the plurality of dispersion holes are evenly opened on the outer side of the bottom of the dispersion disk, and the rotating base is rotatably arranged at the bottom center of the dispersion disk through a bearing.
[0013] Preferably, the bubble forming mechanism comprises a unidirectional screw, a stirring plate and a cutting knife; The one-way screw is rotatably nested at the top edge of the dispersion disk through a bearing, the one-way screw is located inside the threaded hole and is threadedly connected to the threaded hole, two stirring plates are provided, and four cutting knives are provided. The two stirring plates are respectively fixed at the bottom of both sides of the one-way screw, and the four cutting knives are respectively fixed at the two side surfaces of the two stirring plates.
[0014] Preferably, the compressed air input mechanism comprises a sealing cover, an inner air intake pipe and an outer air intake pipe; The sealing cover is rotatably sleeved on the outer top of the connecting tube through a bearing, the inner air intake pipe is fixedly penetrated on the side of the sealing cover, the outer air intake pipe is fixedly penetrated on the top of the reactor and slidably sleeved on the outer side of the inner air intake pipe along the vertical direction, and the input end of the outer air intake pipe is connected to a compressed air source.
[0015] Preferably, the method specifically comprises the following steps: S1, adding solvent acetonitrile, p-cymene, copper catalyst and co-catalyst into the reactor in sequence to form a mixed material, starting a heating resistor, and heating the mixed material with the heating resistor; S2, start the driving motor, after the driving motor is started, it drives the reciprocating screw to rotate, and when the reciprocating screw rotates, it drives the guided outer sleeve to move downward continuously, and when the outer sleeve moves downward, it drives the inner sleeve to move downward through the reset spring, and drives the driving ring to move downward through the outer sleeve plate, and when the inner sleeve moves downward, it drives the dispersion plate to move downward synchronously through the connecting tube, so that the dispersion plate moves to the bottom of the inner cavity of the reactor, and when the reciprocating screw rotates, it drives the square slide rod to rotate through the square slide groove, and the square slide rod drives the dispersion plate to rotate through the connecting tube, and when the dispersion plate rotates, it drives multiple groups of bubble forming mechanisms to rotate synchronously; S3, when the outer sleeve descends to a first threshold, the dispersion disk drives the bubble forming mechanism to enter the mixed material. At this time, as the dispersion disk and the multiple groups of bubble forming mechanisms continue to rotate, the mixed material is continuously mixed; S4, when the outer sleeve descends to a second threshold, the bottom of the rotating base contacts the bottom of the inner cavity of the reactor. At this time, the dispersion plate is in the reaction position. At the same time, due to the obstruction of the inner wall of the reactor, the dispersion plate cannot continue to descend. Subsequently, as the outer sleeve continues to descend, the return spring is compressed by the inner sleeve that also cannot descend. At the same time, the outer sleeve continues to drive the driving ring to descend through the outer sleeve plate; S5, the compressed air source inputs compressed air into the inner part of the air inlet outer tube, the compressed air enters into the sealing cover through the air inlet inner tube, then enters into the connecting tube through the air inlet hole, and finally enters into the dispersion disk and is ejected through multiple dispersion holes. The compressed air is ejected through the dispersion holes to form an air column, which displaces the mixed material at the bottom of the inner cavity of the reactor, and then continues to rise inside the mixed material. During the rising process, the compressed air is intercepted by the continuously rotating bubble forming mechanism, thereby forming bubbles; S6. During the descent of the driving ring, the one-way screw in the orbiting state is driven to continuously rotate. When the one-way screw rotates, the four cutters are driven to rotate synchronously through the two stirring plates, thereby continuously cutting off the rising air column while stirring the mixed material; S7, when the outer sleeve descends to a third threshold, the outer sleeve moves to the bottom of the reciprocating thread on the outer side of the reciprocating screw, and then as the reciprocating screw continues to rotate, the outer sleeve moves upward and resets; S8, when the upward movement distance of the outer sleeve reaches the fourth threshold value, the compressed reset spring is reset, and the reaction of the mixed material is completed at this time, and the input of compressed air is stopped. Subsequently, as the outer sleeve continues to move upward, the compressed air dispersion mechanism and the bubble formation mechanism are gradually removed from the reacted mixed material; S9, during the upward movement of the compressed air dispersion mechanism and the bubble forming mechanism, sodium hydroxide solution is added to the interior of the reactor through a pipeline for quenching, and during the addition of the sodium hydroxide solution, the dual driving mechanism, the compressed air dispersion mechanism and the bubble forming mechanism are flushed, so that the mixed material attached to the surfaces of the dual driving mechanism, the compressed air dispersion mechanism and the bubble forming mechanism is dropped and recovered; S10, when the upward movement distance of the outer sleeve reaches the fifth threshold, the outer sleeve arrives at the initial position, that is, the top of the reciprocating thread on the outer side of the reciprocating screw, and the drive motor is stopped at this time; S11, the quenched mixed material is allowed to stand, and after the standing, the oil phase floats above the solvent, and the solvent and the oil phase are successively output through a pipeline, and the oil phase is distilled after being output to obtain a carvacrol product.
[0016] Technical effects and advantages of the present invention: The present invention is provided with a dual driving mechanism, a compressed air dispersion mechanism, a bubble forming mechanism and a compressed air input mechanism, so that the dual driving mechanism drives the compressed air dispersion mechanism and the bubble forming mechanism to move downward synchronously. During the descending process of the compressed air dispersion mechanism, it is driven by the dual driving mechanism to rotate. When the compressed air dispersion mechanism rotates, it drives multiple groups of bubble forming mechanisms to rotate synchronously, thereby mixing the mixed materials. After the compressed air dispersion mechanism reaches the reaction station at the bottom of the inner cavity of the reactor, the compressed air input mechanism inputs compressed air into the compressed air dispersion mechanism. At this time, the compressed air forms multiple air columns and enters the mixed materials. At this time, due to the rotation of the bubble forming mechanism, the rising The air column is continuously divided and forms a large number of bubbles to increase the contact area between the air and the mixed material. In addition, the subsequent dual drive mechanism can also trigger the bubble forming mechanism, so that it can rotate while revolving to increase the bubble generation rate. Compared with the same type of devices and methods in the prior art, the present invention uses a large number of bubbles evenly dispersed in the mixed material to replace the huge air column formed by a single air inlet position in the prior art, effectively increasing the contact area between the airflow and the reaction material, thereby increasing the oxidation reaction rate. At the same time, due to the increase in the reaction rate, the compressed air input time can be effectively shortened, thereby improving the production efficiency of the carvacrol finished product and reducing the production cost of the carvacrol finished product. The present invention adds sodium hydroxide solution for quenching during the upward resetting process of the compressed air dispersion mechanism and the bubble forming mechanism, so that the sodium hydroxide solution can clean and recover the residual materials on the surfaces of the dual driving mechanism, the compressed air dispersion mechanism and the bubble forming mechanism. At the same time, the centrifugal force generated when the compressed air dispersion mechanism and the bubble forming mechanism rotate can also throw off the residual sodium hydroxide solution, thereby reducing the residual materials. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Figure 1 It is a schematic diagram of the overall structure of the present invention.
[0018] Figure 2 It is a schematic diagram of the overall cross-sectional structure of the present invention.
[0019] Figure 3 It is a schematic cross-sectional structural diagram of the dual drive mechanism of the present invention.
[0020] Figure 4 It is a schematic cross-sectional structure diagram of a part of the compressed air dispersion mechanism and the bubble forming mechanism of the present invention.
[0021] Figure 5 It is a schematic cross-sectional structural diagram of a part of the compressed air dispersion mechanism and the compressed air input mechanism of the present invention.
[0022] In the figure: 1. Reactor; 2. Double drive mechanism; 21. Reciprocating screw; 22. Drive motor; 23. Square slide; 24. Outer sleeve; 25. Return spring; 26. Inner sleeve; 27. Outer plate; 28. Drive ring; 29. Threaded hole; 3. Compressed air dispersion mechanism; 31. Square slide rod; 32. Connecting tube; 33. Air inlet hole; 34. Dispersion disk; 35. Dispersion hole; 36. Rotating base; 4. Bubble forming mechanism; 41. One-way screw; 42. Stirring plate; 43. Cutter; 5. Compressed air input mechanism; 51. Sealing cover; 52. Inner air inlet pipe; 53. Outer air inlet pipe. DETAILED DESCRIPTION
[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions 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 creative work are within the scope of protection of the present invention.
[0024] Example 1
[0025] The present invention provides Figure 1-Figure 5 A method for preparing carvacrol from para-cymene is shown, and the method for preparing carvacrol from para-cymene is implemented by a carvacrol preparation device, and the carvacrol preparation device comprises a reactor 1, a heating resistor is arranged inside the reactor 1, a dual driving mechanism 2 is arranged at the top of the inner cavity of the reactor 1, a compressed air dispersion mechanism 3 is arranged at the bottom of the dual driving mechanism 2, a plurality of groups of bubble forming mechanisms 4 are evenly arranged at the top edge of the compressed air dispersion mechanism 3, and a compressed air input mechanism 5 is arranged at the top of the outer side of the compressed air dispersion mechanism 3; The dual drive mechanism 2 drives the compressed air dispersion mechanism 3 and the bubble forming mechanism 4 to move downward synchronously to reach the reaction station at the bottom of the inner cavity of the reactor 1. The compressed air input mechanism 5 inputs compressed air flow into the compressed air dispersion mechanism 3. The dual drive mechanism 2 drives the compressed air dispersion mechanism 3 to rotate continuously, so that the compressed air flow forms multiple air columns and enters the mixed material. The compressed air dispersion mechanism 3 drives the bubble forming mechanism 4 to rotate synchronously, divides the rising air column to form bubbles, and the dual drive mechanism 2 triggers the bubble forming mechanism 4 to make it rotate while revolving.
[0026] like Figure 3 As shown, the dual drive mechanism 2 includes a reciprocating screw 21, a driving motor 22, a square slide 23, an outer sleeve 24, a return spring 25, an inner sleeve 26, an outer sleeve plate 27, a drive ring 28 and a threaded hole 29, wherein the reciprocating screw 21 passes through the top of the reactor 1 and extends to the inside of the reactor 1 and is rotatably connected to the reactor 1 through a bearing, the driving motor 22 is fixedly arranged on the top of the reactor 1 and is transmission-connected to the reciprocating screw 21, the square slide 23 is opened at the bottom end of the reciprocating screw 21, the outer sleeve 24, the return spring 25 and the inner sleeve 26 are connected from the top to the bottom of the reciprocating screw 21, and the outer sleeve 24, the return spring 25 and the inner sleeve 26 are connected from the top to the bottom of the reciprocating screw 21. The outer sleeve 24 is transmission-connected to the reciprocating screw 21, the return spring 25 is fixedly connected between the outer sleeve 24 and the inner sleeve 26, the inner sleeve 26 is slidingly connected to the reciprocating screw 21 and is slidably nested on the inner side of the outer sleeve 24 along the vertical direction, the outer sleeve plate 27 is fixedly sleeved on the outer bottom of the outer sleeve 24, the drive ring 28 is rotatably sleeved on the outer side of the outer sleeve plate 27 through a bearing, and a plurality of threaded holes 29 are provided, and a plurality of the threaded holes 29 are evenly penetrated through the top of the drive ring 28.
[0027] By setting the above structure, the drive motor 22 can drive the reciprocating screw 21 to rotate after it is started. When the reciprocating screw 21 rotates, it drives the guided outer sleeve 24 to move downward continuously. When the outer sleeve 24 moves downward, the return spring 25 drives the inner sleeve 26 to move downward, and the outer sleeve plate 27 drives the drive ring 28 to move downward.
[0028] like Figure 4 and Figure 5As shown, the compressed air dispersion mechanism 3 includes a square slide bar 31, a connecting tube 32, an air inlet 33, a dispersion disk 34, a dispersion hole 35 and a rotating base 36, wherein the square slide bar 31 is slidably arranged on the inner side of the square slide groove 23 along the vertical direction, the connecting tube 32 is fixedly arranged at the bottom of the square slide bar 31 and is rotatably connected to the inner sleeve 26 through a bearing, two air inlet holes 33 are provided, and the two air inlet holes 33 are respectively opened at the top of both sides of the connecting tube 32, the dispersion disk 34 is fixedly sleeved and arranged at the outer bottom of the connecting tube 32, a plurality of dispersion holes 35 are provided, and a plurality of dispersion holes 35 are evenly opened on the outer side of the bottom of the dispersion disk 34, and the rotating base 36 is rotatably arranged at the bottom center of the dispersion disk 34 through a bearing.
[0029] By setting the above structure, when the inner sleeve 26 moves downward, the dispersion plate 34 is driven to move downward synchronously through the connecting tube 32, so that the dispersion plate 34 moves to the bottom of the inner cavity of the reactor 1. In addition, when the reciprocating screw 21 rotates, the square slide rod 31 is driven to rotate through the square slide groove 23, and the square slide rod 31 drives the dispersion plate 34 to rotate through the connecting tube 32. When the dispersion plate 34 rotates, it drives multiple groups of bubble forming mechanisms 4 to rotate synchronously.
[0030] like Figure 4 As shown, the bubble forming mechanism 4 includes a one-way screw 41, a stirring plate 42 and a cutter 43, wherein the one-way screw 41 is rotatably nested at the top edge of the dispersion disk 34 through a bearing, the one-way screw 41 is located on the inner side of the threaded hole 29 and is threadedly connected to the threaded hole 29, two stirring plates 42 are provided, and four cutters 43 are provided. The two stirring plates 42 are respectively fixedly provided at the bottom of both sides of the one-way screw 41, and the four cutters 43 are respectively fixedly provided at the two side surfaces of the two stirring plates 42.
[0031] By setting the above structure, the bubble forming mechanism 4 is driven to rotate synchronously when the dispersion disk 34 rotates, thereby completing the mixing of the mixed material and the cutting off of the columnar airflow in succession. When the subsequent driving ring 28 descends, the one-way screw 41 in the orbital state is driven to rotate continuously. When the one-way screw 41 rotates, the four cutters 43 are driven to rotate synchronously through the two stirring plates 42, thereby accelerating the stirring efficiency of the mixed material and the cutting off efficiency of the rising air column, so that a large number of bubbles are generated.
[0032] like Figure 5 As shown, the compressed air input mechanism 5 includes a sealing cover 51, an air intake inner tube 52 and an air intake outer tube 53, wherein the sealing cover 51 is rotatably sleeved on the outer top of the connecting tube 32 through a bearing, the air intake inner tube 52 is fixedly penetrated on the side of the sealing cover 51, the air intake outer tube 53 is fixedly penetrated on the top of the reactor 1 and slidably sleeved on the outer side of the air intake inner tube 52 along the vertical direction, and the input end of the air intake outer tube 53 is connected to a compressed air source.
[0033] By setting the above structure, when the connecting tube 32 is raised or lowered, the sealing cover 51 and the intake inner tube 52 can be raised or lowered synchronously with the connecting tube 32, and when the intake inner tube 52 is raised or lowered, it is also raised or lowered synchronously inside the intake outer tube 53, so that the connecting tube 32 can continue to maintain a connected state with the intake outer tube 53 during the raising or lowering process.
[0034] When the subsequent compressed air source inputs compressed air into the inner part of the air inlet outer tube 53, the compressed air enters into the sealing cover 51 through the air inlet inner tube 52, then enters into the connecting tube 32 through the air inlet hole 33, and finally enters into the dispersion disk 34 and is ejected through multiple dispersion holes 35. After being ejected through the dispersion holes 35, the compressed air forms an air column, which displaces the mixed material at the bottom of the inner cavity of the reactor 1, and then continues to rise inside the mixed material. During the rising process, it is intercepted by the continuously rotating bubble forming mechanism 4, thereby forming bubbles.
[0035] Example 2
[0036] The method specifically comprises the following steps: S1, adding solvent acetonitrile, para-cymene, copper catalyst and co-catalyst into the reactor 1 in sequence to form a mixed material, starting a heating resistor, and heating the mixed material with the heating resistor; S2, start the driving motor 22. After the driving motor 22 is started, it drives the reciprocating screw 21 to rotate. When the reciprocating screw 21 rotates, it drives the guided outer sleeve 24 to move downward continuously. When the outer sleeve 24 moves downward, it drives the inner sleeve 26 to move downward through the return spring 25, and drives the driving ring 28 to move downward through the outer sleeve plate 27. When the inner sleeve 26 moves downward, it drives the dispersion plate 34 to move downward synchronously through the connecting tube 32, so that the dispersion plate 34 moves toward the bottom of the inner cavity of the reactor 1. In addition, when the reciprocating screw 21 rotates, it drives the square slide bar 31 to rotate through the square slide groove 23, and the square slide bar 31 drives the dispersion plate 34 to rotate through the connecting tube 32. When the dispersion plate 34 rotates, it drives multiple groups of bubble forming mechanisms 4 to rotate synchronously; S3, when the outer sleeve 24 descends to a first threshold, the dispersion disc 34 drives the bubble forming mechanism 4 to enter the mixed material. At this time, as the dispersion disc 34 and the plurality of bubble forming mechanisms 4 continue to rotate, the mixed material is continuously mixed; S4, when the outer sleeve 24 descends to a second threshold, the bottom of the rotating base 36 contacts the bottom of the inner cavity of the reactor 1, and the dispersion plate 34 is at the reaction position. At the same time, due to the obstruction of the inner wall of the reactor 1, the dispersion plate 34 cannot continue to descend. Subsequently, as the outer sleeve 24 continues to descend, the return spring 25 is compressed by the inner sleeve 26 which also cannot descend, and at the same time, the outer sleeve 24 continues to drive the driving ring 28 to descend through the outer sleeve plate 27; S5, the compressed air source inputs compressed air into the inner part of the air inlet outer tube 53, the compressed air enters into the sealing cover 51 through the air inlet inner tube 52, then enters into the connecting tube 32 through the air inlet hole 33, and finally enters into the dispersion plate 34 and is ejected through the plurality of dispersion holes 35. After being ejected through the dispersion holes 35, the compressed air forms an air column, which displaces the mixed material at the bottom of the inner cavity of the reactor 1, and then continues to rise inside the mixed material. During the rising process, the compressed air is intercepted by the continuously rotating bubble forming mechanism 4, thereby forming bubbles; S6, during the descent of the driving ring 28, the one-way screw 41 in the orbiting state is driven to continuously rotate. When the one-way screw 41 rotates, the four cutters 43 are driven to rotate synchronously through the two stirring plates 42, thereby continuously cutting off the rising air column while stirring the mixed material; S7, when the outer sleeve 24 descends to a third threshold, the outer sleeve 24 moves to the bottom of the reciprocating thread on the outer side of the reciprocating screw 21, and then as the reciprocating screw 21 continues to rotate, the outer sleeve 24 moves upward and resets; S8, when the upward movement distance of the outer sleeve 24 reaches the fourth threshold, the compressed return spring 25 is reset, and the reaction of the mixed material is completed at this time, and the input of compressed air is stopped. Subsequently, as the outer sleeve 24 continues to move upward, the compressed air dispersion mechanism 3 and the bubble formation mechanism 4 are gradually removed from the reacted mixed material; S9, during the upward movement of the compressed air dispersion mechanism 3 and the bubble forming mechanism 4, sodium hydroxide solution is added to the interior of the reactor 1 through the pipeline for quenching. During the addition of the sodium hydroxide solution, the dual driving mechanism 2, the compressed air dispersion mechanism 3 and the bubble forming mechanism 4 are flushed, so that the mixed material attached to the surfaces of the dual driving mechanism 2, the compressed air dispersion mechanism 3 and the bubble forming mechanism 4 is dropped and recovered; S10, when the upward movement distance of the outer sleeve 24 reaches the fifth threshold, the outer sleeve 24 reaches the initial position, that is, the top of the reciprocating thread on the outer side of the reciprocating screw 21, and the driving motor 22 is stopped at this time; S11, the quenched mixed material is allowed to stand, and after the standing, the oil phase floats above the solvent, and the solvent and the oil phase are successively output through a pipeline, and the oil phase is distilled after being output to obtain a carvacrol product.
[0037] Example 3
[0038] It should also be noted that the first threshold, the second threshold and the third threshold increase in sequence, and the fourth threshold and the fifth threshold increase in sequence. At the same time, the first threshold, the second threshold, the third threshold, the fourth threshold and the fifth threshold are recorded for the convenience of accurately describing the actual working conditions of the scheme; When the solution of the present application is actually produced, according to the actual specifications of the outer sleeve 24, the first threshold value, the second threshold value, the third threshold value, the fourth threshold value and the fifth threshold value are all specific values.
[0039] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for preparing carvacrol from p-cymene, characterized in that: The method for preparing carvacrol from para-cymene is implemented by a carvacrol preparation device, the carvacrol preparation device comprising a reactor (1), a heating resistor is arranged inside the reactor (1), a dual drive mechanism (2) is arranged at the top of the inner cavity of the reactor (1), a compressed air dispersion mechanism (3) is arranged at the bottom of the dual drive mechanism (2), a plurality of groups of bubble forming mechanisms (4) are evenly arranged at the top edge of the compressed air dispersion mechanism (3), and a compressed air input mechanism (5) is arranged at the top of the outer side of the compressed air dispersion mechanism (3); The dual drive mechanism (2) drives the compressed air dispersion mechanism (3) and the bubble forming mechanism (4) to move downward synchronously to reach the reaction station at the bottom of the inner cavity of the reactor (1); the compressed air input mechanism (5) inputs compressed air into the compressed air dispersion mechanism (3); the dual drive mechanism (2) drives the compressed air dispersion mechanism (3) to rotate continuously, so that the compressed air forms a plurality of air columns and enters the mixed material; the compressed air dispersion mechanism (3) drives the bubble forming mechanism (4) to rotate synchronously, divides the rising air columns, and forms bubbles; the dual drive mechanism (2) triggers the bubble forming mechanism (4) to rotate while orbiting.
2. The method for preparing carvacrol from p-cymene according to claim 1, characterized in that: The dual drive mechanism (2) comprises a reciprocating screw (21), a drive motor (22), a square slide groove (23), an outer sleeve (24), a return spring (25) and an inner sleeve (26); The reciprocating screw (21) passes through the top of the reactor (1) and extends into the interior of the reactor (1) and is rotationally connected to the reactor (1) via a bearing. The driving motor (22) is fixedly arranged at the top of the reactor (1) and is transmission-connected to the reciprocating screw (21). The square slide groove (23) is opened at the bottom of the reciprocating screw (21). The outer sleeve (24), the return spring (25) and the inner sleeve (26) are sequentially sleeved and arranged on the outside of the reciprocating screw (21) from top to bottom. The outer sleeve (24) is transmission-connected to the reciprocating screw (21). The return spring (25) is fixedly connected between the outer sleeve (24) and the inner sleeve (26). The inner sleeve (26) is slidably connected to the reciprocating screw (21) and is slidably nested and arranged on the inside of the outer sleeve (24) in a vertical direction.
3. The method for preparing carvacrol from p-cymene according to claim 2, characterized in that: The dual drive mechanism (2) further comprises an outer sleeve plate (27), a drive ring (28) and a threaded hole (29); The outer sleeve (27) is fixedly sleeved on the outer bottom of the outer sleeve (24), and the drive ring (28) is rotatably sleeved on the outer side of the outer sleeve (27) via a bearing. A plurality of threaded holes (29) are provided, and the plurality of threaded holes (29) are evenly penetrated through the top of the drive ring (28).
4. The method for preparing carvacrol from p-cymene according to claim 3, characterized in that: The compressed air dispersion mechanism (3) comprises a square sliding rod (31), a connecting tube (32), an air inlet (33), a dispersion disk (34), a dispersion hole (35) and a rotating base (36); The square slide bar (31) is slidably arranged on the inner side of the square slide groove (23) along the vertical direction, the connecting tube (32) is fixedly arranged on the bottom of the square slide bar (31) and is rotatably connected to the inner sleeve (26) via a bearing, two air inlet holes (33) are arranged, and the two air inlet holes (33) are respectively opened on the top of both sides of the connecting tube (32), the dispersion plate (34) is fixedly sleeved and arranged on the outer bottom of the connecting tube (32), a plurality of dispersion holes (35) are arranged, and the plurality of dispersion holes (35) are evenly opened on the outer side of the bottom of the dispersion plate (34), and the rotating base (36) is rotatably arranged at the center of the bottom of the dispersion plate (34) via a bearing.
5. The method for preparing carvacrol from p-cymene according to claim 4, characterized in that: The bubble forming mechanism (4) comprises a unidirectional screw (41), a stirring plate (42) and a cutting knife (43); The one-way screw (41) is rotatably nested at the top edge of the dispersion plate (34) via a bearing. The one-way screw (41) is located inside the threaded hole (29) and is threadedly connected to the threaded hole (29). Two stirring plates (42) are provided. Four cutting knives (43) are provided. The two stirring plates (42) are respectively fixedly provided at the bottom of both sides of the one-way screw (41). The four cutting knives (43) are respectively fixedly provided at both sides of the two stirring plates (42).
6. The method for preparing carvacrol from p-cymene according to claim 5, characterized in that: The compressed air input mechanism (5) comprises a sealing cover (51), an inner air intake pipe (52) and an outer air intake pipe (53); The sealing cover (51) is rotatably sleeved on the outer top of the connecting tube (32) via a bearing, the air intake inner tube (52) is fixedly penetrated on the side of the sealing cover (51), the air intake outer tube (53) is fixedly penetrated on the top of the reaction kettle (1) and slidably sleeved on the outer side of the air intake inner tube (52) in a vertical direction, and the input end of the air intake outer tube (53) is connected to a compressed air source.
7. The method for preparing carvacrol from p-cymene according to claim 6, characterized in that: The method specifically comprises the following steps: S1, adding solvent acetonitrile, para-cymene, a copper-based catalyst and a co-catalyst into the reactor (1) in sequence to form a mixed material, starting a heating resistor, and heating the mixed material with the heating resistor; S2, starting the driving motor (22). After the driving motor (22) is started, it drives the reciprocating screw (21) to rotate. When the reciprocating screw (21) rotates, it drives the guided outer sleeve (24) to continuously move downward. When the outer sleeve (24) moves downward, it drives the inner sleeve (26) to move downward through the return spring (25), and drives the driving ring (28) to move downward through the outer sleeve plate (27). When the inner sleeve (26) moves downward, it drives the dispersion plate (34) to move downward synchronously through the connecting tube (32), thereby causing the dispersion plate (34) to move toward the bottom of the inner cavity of the reactor (1). In addition, when the reciprocating screw (21) rotates, it drives the square slide bar (31) to rotate through the square slide groove (23), and the square slide bar (31) drives the dispersion plate (34) to rotate through the connecting tube (32). When the dispersion plate (34) rotates, it drives the multiple groups of bubble forming mechanisms (4) to rotate synchronously; S3, when the outer sleeve (24) descends a distance reaching a first threshold, the dispersion disc (34) drives the bubble forming mechanism (4) to enter the mixed material, and at this time, as the dispersion disc (34) and the plurality of bubble forming mechanisms (4) continue to rotate, the mixed material is continuously mixed; S4, when the outer sleeve (24) reaches a second threshold value after the lowering distance, the bottom of the rotating base (36) contacts the bottom of the inner cavity of the reactor (1), and the dispersion plate (34) is at the reaction position. At the same time, due to the obstruction of the inner wall of the reactor (1), the dispersion plate (34) cannot continue to descend. Subsequently, as the outer sleeve (24) continues to descend, the return spring (25) is compressed by the inner sleeve (26) which is also unable to descend, and at the same time, the outer sleeve (24) continues to drive the driving ring (28) to descend through the outer sleeve plate (27); S5, allowing the compressed air source to input compressed air into the inner part of the air inlet outer tube (53), the compressed air entering the inner part of the sealing cover (51) through the air inlet inner tube (52), then entering the inner part of the connecting tube (32) through the air inlet hole (33), and finally entering the inner part of the dispersion plate (34) and being ejected through the plurality of dispersion holes (35), the compressed air being ejected through the dispersion holes (35) to form an air column, which displaces the mixed material at the bottom of the inner cavity of the reaction kettle (1), then continuously rises inside the mixed material, and is intercepted by the continuously rotating bubble forming mechanism (4) during the rising process, thereby forming bubbles; S6, during the descending process of the driving ring (28), the one-way screw (41) in the orbiting state is driven to continuously rotate. When the one-way screw (41) rotates, the four cutters (43) are driven to rotate synchronously through the two stirring plates (42), thereby continuously cutting off the rising air column while stirring the mixed material; S7, when the outer sleeve (24) reaches a third threshold value after the descending distance, the outer sleeve (24) moves to the bottom end of the reciprocating thread on the outer side of the reciprocating screw (21), and then as the reciprocating screw (21) continues to rotate, the outer sleeve (24) moves upward and resets; S8, when the upward movement distance of the outer sleeve (24) reaches a fourth threshold value, the compressed return spring (25) is reset, and at this time the reaction of the mixed material is completed, and the input of compressed air is stopped. Subsequently, as the outer sleeve (24) continues to move upward, the compressed air dispersion mechanism (3) and the bubble formation mechanism (4) are gradually removed from the reacted mixed material; S9, during the upward movement of the compressed air dispersion mechanism (3) and the bubble formation mechanism (4), sodium hydroxide solution is added to the interior of the reaction kettle (1) through a pipeline for quenching. During the addition of the sodium hydroxide solution, the dual drive mechanism (2), the compressed air dispersion mechanism (3) and the bubble formation mechanism (4) are flushed, so that the mixed material attached to the surfaces of the dual drive mechanism (2), the compressed air dispersion mechanism (3) and the bubble formation mechanism (4) falls down and is recovered; S10, when the upward movement distance of the outer sleeve (24) reaches the fifth threshold value, the outer sleeve (24) reaches the initial position, that is, the topmost point of the reciprocating thread on the outer side of the reciprocating screw (21), and the driving motor (22) is stopped at this time; S11, the quenched mixed material is allowed to stand, and after the standing, the oil phase floats above the solvent, and the solvent and the oil phase are successively output through a pipeline, and the oil phase is distilled after being output to obtain a carvacrol product.
Citation Information
Patent Citations
A method for preparing carvacrol from cymene
CN115448819B