Method for preparing high-purity carvacrol from o-cresol

Abstract

The invention discloses a method for preparing high-purity carvacrol by using o-cresol, and relates to the technical field of carvacrol preparation, the method for preparing high-purity carvacrol by using o-cresol is realized through carvacrol preparation equipment, and the carvacrol preparation equipment comprises a reaction mechanism, a driving mechanism is arranged at the top and in the reaction mechanism, and a uniform suction mechanism, a screening and stirring mechanism and a throwing and blocking mechanism are sequentially arranged on the outer side of the driving mechanism from top to bottom; and the driving mechanism synchronously drives the uniform suction mechanism, the screening and stirring mechanism and the throwing and plugging mechanism. According to the present invention, the reaction product cooling operation and the catalyst filtration operation can be synchronously performed so as to effectively improve the carvacrol crude product preparation efficiency, and the catalyst filtration can be performed without the transfer so as to improve the product yield by reducing the transfer frequency.

Description

Technical Field

[0001] The invention relates to the technical field of carvacrol preparation, and in particular to a method for preparing high-purity carvacrol by utilizing o-cresol. Background Art

[0002] Carvacrol has a bactericidal effect and is mainly found in the essential oils of thyme plants. Due to its broad-spectrum antibacterial properties and extremely low residues in animals, it is widely used in the treatment of diarrhea and anticoccidial diseases in animals such as chickens and piglets.

[0003] The invention patent of the L-shaped stirring rod 43 with the authorization announcement number CN1133047 discloses a method for preparing high-purity carvacrol using o-cresol. The invention first prepares a Ce and Al co-doped porous nano ZrO2 active catalyst. Due to the porous structure of the nano catalyst and the synergistic effect of Ce and Al co-doping, and in the catalytic reaction of preparing carvacrol from o-cresol, the auxiliary effect of microwaves is used, and no toxic solvent is required, so that o-cresol can have a high conversion rate and a high selectivity for carvacrol, thereby ensuring the yield and purity of carvacrol.

[0004] However, after actual application by technicians skilled in the art, it was found that the above method still has some shortcomings. The most obvious one is that in the preparation process of crude carvacrol, the operator needs to cool the reaction product first, then transfer the cooled reaction product to a filtering device, and finally remove the catalyst from the reaction product through the filtering device. The operation is cumbersome and time-consuming, and the cooling and catalyst filtering operations cannot be performed simultaneously, which has a great impact on the preparation efficiency of crude carvacrol. In addition, there will inevitably be residues in the transfer process of the reaction product, and an increase in the number of transfers will also lead to a decrease in the yield of the reaction product.

[0005] Therefore, it is necessary to invent a method for preparing high-purity carvacrol using o-cresol to solve the above problems. Summary of the invention

[0006] The object of the present invention is to provide a method for preparing high-purity carvacrol by using o-cresol, wherein a driving mechanism, a suction uniform mechanism, a screening and stirring mechanism and a throwing and blocking mechanism are provided, so that the suction uniform mechanism is used to continuously circulate the mixed material, thereby making the active catalyst more evenly distributed in the mixed material to improve the reaction rate. In addition, after the reaction of the mixed material is completed, the throwing and blocking mechanism blocks the bottom of the screening and stirring mechanism to form an annular filtering chamber, and at this time, the reaction product outputted from the suction uniform mechanism to the top of the throwing and blocking mechanism is continuously filtered by the screening and stirring mechanism, and the active catalyst is continuously The reaction product is cooled down rapidly during the centrifugal throwing process to solve the problem that in the preparation process of crude carvacrol proposed in the above background technology, the operator needs to cool the reaction product first, then transfer the cooled reaction product to the filtering equipment, and finally remove the catalyst from the reaction product through the filtering equipment. The operation is cumbersome and time-consuming, and the cooling and catalyst filtering operations cannot be performed simultaneously, which has a great impact on the preparation efficiency of crude carvacrol. In addition, there will inevitably be residues in the transfer process of the reaction product, and the increase in the number of transfers will also lead to a decrease in the yield of the reaction product.

[0007] To achieve the above object, the present invention provides the following technical solution: a method for preparing high-purity carvacrol using o-cresol, wherein the method for preparing high-purity carvacrol using o-cresol is implemented by a carvacrol preparation device, wherein the carvacrol preparation device comprises a reaction mechanism, wherein a driving mechanism is provided on the top and inside of the reaction mechanism, and a suction uniformity mechanism, a screening and stirring mechanism, and a throwing and blocking mechanism are provided on the outside of the driving mechanism in sequence from top to bottom; The driving mechanism drives the suction and uniformizing mechanism, the screening and stirring mechanism and the spreading and blocking mechanism synchronously; the suction and uniformizing mechanism sucks the mixed material containing more catalyst at the bottom of the inner cavity of the reaction mechanism and inputs it to the top of the spreading and blocking mechanism; the screening and stirring mechanism mixes the mixed material; the spreading and blocking mechanism spreads the mixed material falling on the top thereof; after the spreading and blocking mechanism seals the bottom of the screening and stirring mechanism, the screening and stirring mechanism filters out the catalyst in the reaction product.

[0008] Preferably, the reaction mechanism comprises a reaction kettle, a base, a microwave heating assembly and a blocking sleeve; The base is fixedly arranged at the bottom of the reaction kettle, the microwave heating component is fixedly arranged at the outside of the reaction kettle, and the microwave heating component is fixedly arranged at the bottom of the inner cavity of the reaction kettle.

[0009] Preferably, the driving mechanism comprises a driving motor, a first reciprocating screw and a second reciprocating screw; The driving motor is fixedly arranged on the top of the reactor, the first reciprocating screw penetrates the top of the reactor and extends into the interior of the reactor, the first reciprocating screw is rotationally connected to the reactor through a bearing and is transmission-connected to the driving motor, and the second reciprocating screw is fixedly connected to the bottom end of the first reciprocating screw and its bottom end is rotationally connected to the inner wall of the reactor through a bearing.

[0010] Preferably, the uniform suction mechanism comprises a piston cylinder, a connecting rod, a suction pipe, an output pipe, a valve, a piston plate and a first guide rod; The piston cylinder is fixedly sleeved on the outside of the first reciprocating screw, the connecting rod is fixedly arranged on the top of the piston cylinder and fixedly connected to the inner wall of the reactor, the suction pipe is fixedly penetrated at the bottom of the outside of the piston cylinder, a one-way valve is arranged on the suction pipe, the output pipe is fixedly penetrated at the bottom of the piston cylinder, the valve is fixedly arranged at the bottom end of the output pipe, the piston plate transmission sleeve is arranged on the outside of the first reciprocating screw and is slidably arranged on the inside of the piston cylinder along the vertical direction, the first guide rod slides through the top of the reactor and extends to the inside of the reactor and is fixedly connected to the piston plate.

[0011] Preferably, the screening and stirring mechanism comprises an extension plate, an annular filter screen, an L-shaped stirring rod, a bottom scraper, an inner scraper and an outer scraper; The extension plate is fixedly sleeved on the outer top of the second reciprocating screw, the annular filter is fixedly sleeved on the outer side of the extension plate, the L-shaped stirring rod is fixedly set on the outer bottom of the annular filter, the bottom scraper is fixedly set on the bottom end of the L-shaped stirring rod, and the inner scraper and the outer scraper are respectively fixedly set on the inner end and the outer end of the top of the bottom scraper.

[0012] Preferably, the spill blocking mechanism comprises a spill plate, a movable ring, a return spring, a lifting plate and a second guide rod; The spreading plate is slidably nested in the vertical direction on the outside of the second reciprocating screw, the movable ring, the reset spring and the lifting plate are sequentially sleeved on the outside of the second reciprocating screw from top to bottom, the movable ring is rotatably arranged at the bottom of the spreading plate through a bearing, the reset spring is fixedly connected between the movable ring and the lifting plate, the lifting plate is transmission-connected to the second reciprocating screw, and the second guide rod slides through the bottom of the reactor and extends to the inside of the reactor and is fixedly connected to the lifting plate.

[0013] Preferably, the method specifically comprises the following steps: S1. Add o-cresol, isopropanol and an active catalyst into the reactor. The o-cresol, isopropanol and the active catalyst fall into the annular chamber formed by the inner wall of the reactor and the outer wall of the blocking sleeve under the action of gravity to form a mixed material. Start the microwave heating component, and the microwave heating component continuously heats the mixed material at the bottom of the inner cavity of the reactor. S2, start the driving motor, after the driving motor is started, the first reciprocating screw and the second reciprocating screw are driven to rotate, and the first reciprocating screw drives the piston plate guided by the first guide rod to continuously move upward when rotating, and negative pressure is generated inside the piston cylinder during the upward movement of the piston plate, and the negative pressure sucks the mixed material at the bottom of the inner cavity of the reactor through the suction tube, and in addition, the first reciprocating screw drives the piston cylinder to continuously rotate when rotating, and the two suction tubes are driven to rotate synchronously when the piston cylinder rotates, so as to suck the mixed material at different positions; S3, when the second reciprocating screw rotates, the annular filter screen is driven to rotate through the extension plate, and when the annular filter screen rotates, the L-shaped stirring rod, the bottom scraper, the inner scraper and the outer scraper are driven to rotate synchronously, and when the L-shaped stirring rod, the bottom scraper, the inner scraper and the outer scraper rotate, the mixed material is continuously stirred, so that the o-cresol and the isopropanol react rapidly under the catalysis of the active catalyst; S4, when the second reciprocating screw rotates, it drives the lifting plate guided by the second guide rod to move downward continuously, and drives the spreading plate nested and arranged outside the lifting plate in a vertical direction to rotate continuously. When the lifting plate moves downward, the spreading plate is driven to move downward continuously through the reset spring and the movable ring; S5. When the piston plate moves up to the first threshold, the piston plate moves to the top of the reciprocating thread on the outer side of the first reciprocating screw. Subsequently, as the first reciprocating screw continues to rotate, the piston plate moves down and resets. During the downward movement of the piston plate, due to the obstruction of the one-way valve on the suction pipe, the mixed material inside the piston cylinder enters the output pipe and breaks the valve and falls on the top of the spreading plate. During the rotation and upward movement of the spreading plate, the mixed material falling on the top is sprinkled, so that this part of the mixed material falls evenly on the top layer of the mixed material at the bottom of the inner cavity of the reactor; S6, when the downward movement distance of the piston plate reaches the second threshold, the piston plate arrives at the initial position, that is, the bottom end of the reciprocating thread outside the first reciprocating screw, and then as the first reciprocating screw continues to rotate, the piston plate moves up again for suction; S7, when the downward movement distance of the lifting plate reaches the third threshold, the lifting plate moves to the bottom of the reciprocating thread outside the second reciprocating screw, and then as the second reciprocating screw continues to rotate, the lifting plate moves upward and resets; S8, when the lifting plate moves up to the fourth threshold, the bottom of the spreading plate seals the bottom of the annular filter screen, and the spreading plate and the annular filter screen form an annular filter chamber. At this time, the mixed material reacts to generate reaction products. At the same time, due to the obstruction of the annular filter screen, the spreading plate cannot continue to rise. Subsequently, as the lifting plate continues to rise, the reset spring is continuously compressed; S9, stopping the heating of the microwave heating assembly, and when the subsequent suction uniformity mechanism outputs the reaction product, the reaction product falls into the annular filter chamber, and as the annular filter screen continues to rotate, the reaction product passes through the annular filter screen under the action of centrifugal force and is output, and the active catalyst remains inside the annular filter screen; S10, when the upward movement distance of the lifting plate reaches the fifth threshold, the lifting plate moves to the top of the reciprocating thread on the outer side of the second reciprocating screw, at which time the active catalyst has been filtered out, and the reaction product at the bottom of the inner cavity of the reactor is output to obtain a crude carvacrol product, and subsequently, as the second reciprocating screw continues to rotate, the lifting plate moves downward and resets; S11, when the downward movement distance of the lifting plate reaches the sixth threshold, the compressed reset spring is reset, and the reaction product has been outputted. Subsequently, as the lifting plate continues to move downward, the throwing plate releases the blockage of the bottom of the annular filter. At this time, the active catalyst located on the top of the throwing plate is evenly thrown to the bottom of the inner cavity of the reactor under the action of centrifugal force; S12: When the downward movement distance of the lifting plate reaches the seventh threshold, the lifting plate arrives at the initial working position, and the driving motor is stopped at this time.

[0014] Technical effects and advantages of the present invention: The present invention is provided with a driving mechanism, a suction uniformity mechanism, a screening and stirring mechanism and a throwing and sealing mechanism, so that the suction uniformity mechanism can be used to continuously circulate the mixed material, thereby making the active catalyst more evenly distributed in the mixed material to increase the reaction rate. In addition, after the reaction of the mixed material is completed, the throwing and sealing mechanism blocks the bottom of the screening and stirring mechanism to form an annular filter chamber. At this time, the reaction product output by the suction uniformity mechanism to the top of the throwing and sealing mechanism is continuously filtered by the screening and stirring mechanism, and the active catalyst is continuously filtered out. The reaction product is accelerated to cool down during the centrifugal throwing process. Compared with the same type of devices and methods in the prior art, the present invention can simultaneously perform reaction product cooling and catalyst filtering operations, thereby effectively improving the preparation efficiency of crude carvacrol. In addition, there is no need to transfer to achieve catalyst filtering, thereby improving the product yield by reducing the number of transfers. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0016] Figure 2 It is a schematic diagram of the overall cross-sectional structure of the present invention.

[0017] Figure 3 It is a schematic cross-sectional structural diagram of the reaction mechanism of the present invention.

[0018] Figure 4 It is a schematic cross-sectional view of the uniform suction mechanism of the present invention.

[0019] Figure 5 It is a schematic cross-sectional structure diagram of the screening and stirring mechanism and the spreading and blocking mechanism of the present invention.

[0020] Figure 6 It is a schematic diagram of the partial structure of the spreading and blocking mechanism of the present invention.

[0021] In the figure: 1. reaction mechanism; 11. reaction kettle; 12. base; 13. microwave heating assembly; 14. blocking sleeve; 2. driving mechanism; 21. driving motor; 22. first reciprocating screw; 23. second reciprocating screw; 3. suction uniformity mechanism; 31. piston cylinder; 32. connecting rod; 33. suction pipe; 34. output pipe; 35. valve; 36. piston plate; 37. first guide rod; 4. screening and stirring mechanism; 41. extension plate; 42. annular filter; 43. L-shaped stirring rod; 44. bottom scraper; 45. inner scraper; 46. outer scraper; 5. spreading and blocking mechanism; 51. spreading plate; 52. movable ring; 53. reset spring; 54. lifting plate; 55. second guide rod. DETAILED DESCRIPTION

[0022] 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.

[0023] Example 1

[0024] The present invention provides Figure 1-Figure 6 A method for preparing high-purity carvacrol using o-cresol is shown, and the method for preparing high-purity carvacrol using o-cresol is implemented by a carvacrol preparation device, and the carvacrol preparation device includes a reaction mechanism 1, and a driving mechanism 2 is provided on the top and inside of the reaction mechanism 1, and a suction uniformity mechanism 3, a screening and stirring mechanism 4, and a throwing and blocking mechanism 5 are sequentially provided on the outside of the driving mechanism 2 from top to bottom; The driving mechanism 2 drives the suction and uniformizing mechanism 3, the screening and stirring mechanism 4 and the throwing and blocking mechanism 5 synchronously; the suction and uniformizing mechanism 3 sucks the mixed material containing more catalyst at the bottom of the inner cavity of the reaction mechanism 1 and inputs it to the top of the throwing and blocking mechanism 5; the screening and stirring mechanism 4 mixes the mixed material; the throwing and blocking mechanism 5 throws the mixed material falling on the top thereof; after the throwing and blocking mechanism 5 seals the bottom of the screening and stirring mechanism 4, the screening and stirring mechanism 4 filters out the catalyst in the reaction product.

[0025] like Figure 3 As shown, the reaction mechanism 1 includes a reactor 11, a base 12, a microwave heating component 13 and a blocking sleeve 14, wherein the base 12 is fixedly arranged at the bottom of the reactor 11, the microwave heating component 13 is fixedly arranged at the outside of the reactor 11, and the microwave heating component 13 is fixedly arranged at the bottom of the inner cavity of the reactor 11.

[0026] By setting the above structure, it is convenient to add o-cresol, isopropanol and active catalyst into the reactor 11. Under the action of gravity, o-cresol, isopropanol and active catalyst fall into the annular chamber formed by the inner wall of the reactor 11 and the outer wall of the blocking sleeve 14 to form a mixed material. The microwave heating component 13 is started, and the microwave heating component 13 continuously heats the mixed material at the bottom of the inner cavity of the reactor 11.

[0027] like Figure 4 and Figure 5 As shown, the driving mechanism 2 includes a driving motor 21, a first reciprocating screw 22 and a second reciprocating screw 23, wherein the driving motor 21 is fixedly arranged on the top of the reactor 11, the first reciprocating screw 22 passes through the top of the reactor 11 and extends into the interior of the reactor 11, the first reciprocating screw 22 is rotationally connected to the reactor 11 through a bearing and is transmission-connected to the driving motor 21, and the second reciprocating screw 23 is fixedly connected to the bottom end of the first reciprocating screw 22 and its bottom end is rotationally connected to the inner wall of the reactor 11 through a bearing.

[0028] By providing the above structure, it is convenient to start the driving motor 21. After the driving motor 21 is started, it drives the first reciprocating screw 22 and the second reciprocating screw 23 to rotate.

[0029] like Figure 4 As shown, the uniform suction mechanism 3 includes a piston cylinder 31, a connecting rod 32, a suction pipe 33, an output pipe 34, a valve 35, a piston plate 36 and a first guide rod 37, wherein the piston cylinder 31 is fixedly sleeved on the outside of the first reciprocating screw 22, the connecting rod 32 is fixedly arranged on the top of the piston cylinder 31 and is fixedly connected to the inner wall of the reactor 11, the suction pipe 33 is fixedly penetrated and arranged at the bottom of the outer side of the piston cylinder 31, a one-way valve is arranged on the suction pipe 33, the output pipe 34 is fixedly penetrated and arranged at the bottom of the piston cylinder 31, the valve 35 is fixedly arranged at the bottom end of the output pipe 34, the piston plate 36 is transmission sleeved and arranged on the outside of the first reciprocating screw 22 and is slidably arranged on the inner side of the piston cylinder 31 along the vertical direction, and the first guide rod 37 slides through the top of the reactor 11 and extends to the inside of the reactor 11 and is fixedly connected to the piston plate 36.

[0030] By setting the above structure, when the first reciprocating screw 22 rotates, it drives the piston plate 36 guided by the first guide rod 37 to continuously move upward. During the upward movement of the piston plate 36, negative pressure is generated inside the piston cylinder 31. The negative pressure sucks the mixed material at the bottom of the inner cavity of the reactor 11 through the suction pipe 33. In addition, when the first reciprocating screw 22 rotates, it drives the piston cylinder 31 to continuously rotate. When the piston cylinder 31 rotates, it drives the two suction pipes 33 to rotate synchronously, thereby sucking the mixed material at different positions. After the piston plate 36 moves to the top of the reciprocating thread on the outside of the first reciprocating screw 22, as the first reciprocating screw 22 continues to rotate, the piston plate 36 moves down and resets. During the downward movement of the piston plate 36, due to the obstruction of the one-way valve on the suction pipe 33, the mixed material inside the piston cylinder 31 enters the output pipe 34 and breaks open the valve 35 to fall on the top of the throwing and blocking mechanism 5. During the rotation and upward process of the throwing and blocking mechanism 5, the mixed material falling on the top is thrown, so that this part of the mixed material falls evenly on the top layer of the mixed material at the bottom of the inner cavity of the reactor 11, thereby making the active catalyst more evenly distributed in the mixed material to increase the reaction rate.

[0031] like Figure 5 and Figure 6 As shown, the screening and stirring mechanism 4 includes an extension plate 41, an annular filter 42, an L-shaped stirring rod 43, a bottom scraper 44, an inner scraper 45 and an outer scraper 46, wherein the extension plate 41 is fixedly sleeved on the outer top of the second reciprocating screw 23, the annular filter 42 is fixedly sleeved on the outer side of the extension plate 41, the L-shaped stirring rod 43 is fixedly set on the outer bottom of the annular filter 42, the bottom scraper 44 is fixedly set on the bottom end of the L-shaped stirring rod 43, and the inner scraper 45 and the outer scraper 46 are respectively fixedly set on the inner end and the outer end of the top of the bottom scraper 44.

[0032] By setting the above structure, when the second reciprocating screw 23 rotates, the annular filter screen 42 is driven to rotate through the extension plate 41, and when the annular filter screen 42 rotates, the L-shaped stirring rod 43, the bottom scraper 44, the inner scraper 45 and the outer scraper 46 are driven to rotate synchronously. When the L-shaped stirring rod 43, the bottom scraper 44, the inner scraper 45 and the outer scraper 46 rotate, the mixed material is continuously stirred, so that the o-cresol and the isopropanol react quickly under the catalysis of the active catalyst; After the bottom of the subsequent extension plate 41 is blocked by the throwing and blocking mechanism 5, an annular filter chamber is formed inside the annular filter screen 42. When the subsequent suction uniformity mechanism 3 outputs the reaction product, the reaction product falls into the annular filter chamber. As the annular filter screen 42 continues to rotate, the reaction product passes through the annular filter screen 42 under the action of centrifugal force and is output, while the active catalyst remains inside the annular filter screen 42.

[0033] like Figure 5As shown, the spreading and blocking mechanism 5 includes a spreading plate 51, a movable ring 52, a reset spring 53, a lifting plate 54 and a second guide rod 55, wherein the spreading plate 51 is slidably nested in the vertical direction on the outside of the second reciprocating screw 23, the movable ring 52, the reset spring 53 and the lifting plate 54 are sequentially sleeved from top to bottom on the outside of the second reciprocating screw 23, the movable ring 52 is rotatably arranged at the bottom of the spreading plate 51 through a bearing, the reset spring 53 is fixedly connected between the movable ring 52 and the lifting plate 54, the lifting plate 54 is transmission-connected to the second reciprocating screw 23, and the second guide rod 55 slides through the bottom of the reactor 11 and extends to the inside of the reactor 11 and is fixedly connected to the lifting plate 54.

[0034] By setting the above structure, when the second reciprocating screw 23 rotates, the lifting plate 54 guided by the second guide rod 55 is driven to move downward continuously, and the throwing plate 51 slidably nested and arranged on the outside thereof in the vertical direction is driven to rotate continuously. When the lifting plate 54 moves downward, the throwing plate 51 is driven to move downward continuously by the reset spring 53 and the movable ring 52. After the lifting plate 54 moves to the bottom of the reciprocating thread on the outside of the second reciprocating screw 23, as the second reciprocating screw 23 continues to rotate, the lifting plate 54 moves up and resets until the bottom of the throwing plate 51 seals the bottom of the annular filter screen 42. At this time, the throwing plate 51 and the annular filter screen 42 form an annular filter chamber, and the mixed material reacts to generate reaction products. At the same time, due to the obstruction of the annular filter screen 42, the throwing plate 51 cannot continue to rise. Subsequently, as the lifting plate 54 continues to rise, the reset spring 53 is continuously compressed until the lifting plate 54 moves to the top of the reciprocating thread on the outside of the second reciprocating screw 23. At this time, the active catalyst has been filtered out. Subsequently, as the second reciprocating screw 23 continues to rotate, the lifting plate 54 moves down and resets, and gradually drives the compressed reset spring 53 to reset. As the lifting plate 54 continues to move downward, the spreading plate 51 releases the blockage of the bottom of the annular filter 42. At this time, the active catalyst located on the top of the spreading plate 51 is evenly thrown to the bottom of the inner cavity of the reactor 11 under the action of centrifugal force to wait for the next preparation operation. When the lifting plate 54 arrives at the initial workstation, the drive motor 21 is shut down.

[0035] Example 2

[0036] The method specifically comprises the following steps: S1, adding o-cresol, isopropanol and an active catalyst into the reactor 11, the o-cresol, isopropanol and the active catalyst fall into the annular chamber formed by the inner wall of the reactor 11 and the outer wall of the blocking sleeve 14 under the action of gravity to form a mixed material, starting the microwave heating component 13, and the microwave heating component 13 continuously heats the mixed material at the bottom of the inner cavity of the reactor 11; S2, start the drive motor 21. After the drive motor 21 is started, it drives the first reciprocating screw 22 and the second reciprocating screw 23 to rotate. When the first reciprocating screw 22 rotates, it drives the piston plate 36 guided by the first guide rod 37 to continuously move upward. During the upward movement of the piston plate 36, negative pressure is generated inside the piston cylinder 31. The negative pressure sucks the mixed material at the bottom of the inner cavity of the reactor 11 through the suction pipe 33. In addition, when the first reciprocating screw 22 rotates, it drives the piston cylinder 31 to continuously rotate. When the piston cylinder 31 rotates, it drives the two suction pipes 33 to rotate synchronously, thereby sucking the mixed material at different positions; S3, when the second reciprocating screw 23 rotates, the annular filter screen 42 is driven to rotate through the extension plate 41, and when the annular filter screen 42 rotates, the L-shaped stirring rod 43, the bottom scraper 44, the inner scraper 45 and the outer scraper 46 are driven to rotate synchronously, and when the L-shaped stirring rod 43, the bottom scraper 44, the inner scraper 45 and the outer scraper 46 rotate, the mixed material is continuously stirred, so that the o-cresol and the isopropanol react rapidly under the catalysis of the active catalyst; S4, when the second reciprocating screw 23 rotates, it drives the lifting plate 54 guided by the second guide rod 55 to continuously move downward, and drives the spreading plate 51 slidably nested and arranged outside the lifting plate 54 to continuously rotate. When the lifting plate 54 moves downward, the restoring spring 53 and the movable ring 52 drive the spreading plate 51 to continuously move downward; S5, when the upward movement distance of the piston plate 36 reaches the first threshold, the piston plate 36 moves to the top of the reciprocating thread on the outer side of the first reciprocating screw 22, and then as the first reciprocating screw 22 continues to rotate, the piston plate 36 moves down and resets. During the downward movement of the piston plate 36, due to the obstruction of the one-way valve on the suction pipe 33, the mixed material inside the piston cylinder 31 enters the output pipe 34 and breaks the valve 35 and falls on the top of the throwing plate 51. During the rotation and upward process of the throwing plate 51, the mixed material falling on the top is thrown, so that this part of the mixed material falls evenly on the top layer of the mixed material at the bottom of the inner cavity of the reactor 11; S6, when the downward movement distance of the piston plate 36 reaches the second threshold, the piston plate 36 arrives at the initial position, that is, the bottom end of the outer reciprocating thread of the first reciprocating screw 22, and then as the first reciprocating screw 22 continues to rotate, the piston plate 36 moves up again to perform suction; S7, when the downward movement distance of the lifting plate 54 reaches the third threshold, the lifting plate 54 moves to the bottom of the outer reciprocating thread of the second reciprocating screw 23, and then as the second reciprocating screw 23 continues to rotate, the lifting plate 54 moves upward and resets; S8, when the lifting plate 54 moves up to the fourth threshold, the bottom of the spreading plate 51 seals the bottom of the annular filter screen 42, and the spreading plate 51 and the annular filter screen 42 form an annular filter chamber. At this time, the mixed material reacts to generate reaction products. At the same time, due to the obstruction of the annular filter screen 42, the spreading plate 51 cannot continue to rise. Subsequently, as the lifting plate 54 continues to rise, the return spring 53 is continuously compressed; S9, stopping the heating of the microwave heating assembly 13, and when the subsequent suction uniform mechanism 3 outputs the reaction product, the reaction product falls into the annular filter chamber, and as the annular filter screen 42 continues to rotate, the reaction product passes through the annular filter screen 42 under the action of centrifugal force and is output, and the active catalyst remains inside the annular filter screen 42; S10, when the upward movement distance of the lifting plate 54 reaches the fifth threshold, the lifting plate 54 moves to the top of the reciprocating thread on the outside of the second reciprocating screw 23. At this time, the active catalyst has been filtered out, and the reaction product at the bottom of the inner cavity of the reactor 11 is output to obtain the crude carvacrol. Subsequently, as the second reciprocating screw 23 continues to rotate, the lifting plate 54 moves down and resets. S11, when the downward movement distance of the lifting plate 54 reaches the sixth threshold, the compressed reset spring 53 is reset, and the reaction product has been outputted. Subsequently, as the lifting plate 54 continues to move downward, the throwing plate 51 releases the blockage of the bottom of the annular filter 42. At this time, the active catalyst located on the top of the throwing plate 51 is evenly thrown to the bottom of the inner cavity of the reactor 11 under the action of centrifugal force; S12, when the downward movement distance of the lifting plate 54 reaches the seventh threshold, the lifting plate 54 arrives at the initial working position, and the driving motor 21 is stopped at this time.

[0037] Example 3

[0038] It should also be noted that the first threshold and the second threshold are equal, the third threshold, the fourth threshold and the fifth threshold increase successively, and the sixth threshold and the seventh threshold increase successively. At the same time, the first threshold, the second threshold, the third threshold, the fourth threshold, the fifth threshold, the sixth threshold and the seventh 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 first reciprocating screw 22 and the second reciprocating screw 23, the first threshold, the second threshold, the third threshold, the fourth threshold, the fifth threshold, the sixth threshold and the seventh threshold 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 high-purity carvacrol using o-cresol, characterized in that: The method for preparing high-purity carvacrol using o-cresol is achieved by a carvacrol preparation device, the carvacrol preparation device comprising a reaction mechanism (1), a driving mechanism (2) being provided on the top and inside of the reaction mechanism (1), and a suction uniformity mechanism (3), a screening and stirring mechanism (4) and a throwing and blocking mechanism (5) being provided on the outside of the driving mechanism (2) in order from top to bottom; The driving mechanism (2) drives the suction and uniformizing mechanism (3), the screening and stirring mechanism (4) and the throwing and blocking mechanism (5) synchronously; the suction and uniformizing mechanism (3) sucks the mixed material containing a large amount of catalyst at the bottom of the inner cavity of the reaction mechanism (1) and inputs it to the top of the throwing and blocking mechanism (5); the screening and stirring mechanism (4) mixes the mixed material; the throwing and blocking mechanism (5) throws the mixed material falling on the top of the mixing mechanism (5); after the throwing and blocking mechanism (5) seals the bottom of the screening and stirring mechanism (4), the screening and stirring mechanism (4) filters out the catalyst in the reaction product.

2. The method for preparing high-purity carvacrol using o-cresol according to claim 1, characterized in that: The reaction mechanism (1) comprises a reaction vessel (11), a base (12), a microwave heating component (13) and a blocking sleeve (14); The base (12) is fixedly arranged at the bottom of the reaction kettle (11), the microwave heating component (13) is fixedly arranged at the outside of the reaction kettle (11), and the microwave heating component (13) is fixedly arranged at the bottom of the inner cavity of the reaction kettle (11).

3. The method for preparing high-purity carvacrol using o-cresol according to claim 2, characterized in that: The driving mechanism (2) comprises a driving motor (21), a first reciprocating screw (22) and a second reciprocating screw (23); The driving motor (21) is fixedly arranged on the top of the reactor (11); the first reciprocating screw (22) penetrates the top of the reactor (11) and extends into the interior of the reactor (11); the first reciprocating screw (22) is rotationally connected to the reactor (11) via a bearing and is transmission-connected to the driving motor (21); the second reciprocating screw (23) is fixedly connected to the bottom end of the first reciprocating screw (22) and the bottom end thereof is rotationally connected to the inner wall of the reactor (11) via a bearing.

4. The method for preparing high-purity carvacrol using o-cresol according to claim 3, characterized in that: The uniform suction mechanism (3) comprises a piston cylinder (31), a connecting rod (32), a suction pipe (33), an output pipe (34), a valve (35), a piston plate (36) and a first guide rod (37); The piston cylinder (31) is fixedly sleeved and arranged on the outside of the first reciprocating screw (22); the connecting rod (32) is fixedly arranged on the top of the piston cylinder (31) and is fixedly connected to the inner wall of the reaction kettle (11); the suction pipe (33) is fixedly arranged through the bottom of the outside of the piston cylinder (31); a one-way valve is arranged on the suction pipe (33); the output pipe (34) is fixedly arranged through the bottom of the piston cylinder (31); the valve (35) is fixedly arranged at the bottom end of the output pipe (34); the piston plate (36) is transmission sleeved and arranged on the outside of the first reciprocating screw (22) and is slidably arranged on the inside of the piston cylinder (31) in the vertical direction; the first guide rod (37) slidably penetrates the top of the reaction kettle (11) and extends to the inside of the reaction kettle (11) and is fixedly connected to the piston plate (36).

5. The method for preparing high-purity carvacrol using o-cresol according to claim 4, characterized in that: The screening and stirring mechanism (4) comprises an extension plate (41), an annular filter screen (42), an L-shaped stirring rod (43), a bottom scraper (44), an inner scraper (45) and an outer scraper (46); The extension plate (41) is fixedly sleeved on the outer top of the second reciprocating screw (23), the annular filter (42) is fixedly sleeved on the outer side of the extension plate (41), the L-shaped stirring rod (43) is fixedly arranged on the outer bottom of the annular filter (42), the bottom scraper (44) is fixedly arranged on the bottom end of the L-shaped stirring rod (43), and the inner scraper (45) and the outer scraper (46) are fixedly arranged on the inner end and the outer end of the top of the bottom scraper (44), respectively.

6. The method for preparing high-purity carvacrol using o-cresol according to claim 5, characterized in that: The spill blocking mechanism (5) comprises a spill plate (51), a movable ring (52), a return spring (53), a lifting plate (54) and a second guide rod (55); The spreading plate (51) is slidably nested along the vertical direction on the outside of the second reciprocating screw (23); the movable ring (52), the return spring (53) and the lifting plate (54) are sequentially sleeved on the outside of the second reciprocating screw (23) from top to bottom; the movable ring (52) is rotatably arranged at the bottom of the spreading plate (51) via a bearing; the return spring (53) is fixedly connected between the movable ring (52) and the lifting plate (54); the lifting plate (54) is transmission-connected to the second reciprocating screw (23); and the second guide rod (55) slides through the bottom of the reactor (11) and extends to the inside of the reactor (11) and is fixedly connected to the lifting plate (54).

7. The method for preparing high-purity carvacrol using o-cresol according to claim 6, characterized in that: The method specifically comprises the following steps: S1, adding o-cresol, isopropanol and an active catalyst into the reactor (11), wherein the o-cresol, isopropanol and the active catalyst fall into an annular chamber formed by the inner wall of the reactor (11) and the outer wall of the blocking sleeve (14) under the action of gravity to form a mixed material, and starting the microwave heating component (13), wherein the microwave heating component (13) continuously heats the mixed material at the bottom of the inner cavity of the reactor (11); S2, starting the driving motor (21). After the driving motor (21) is started, it drives the first reciprocating screw (22) and the second reciprocating screw (23) to rotate. When the first reciprocating screw (22) rotates, it drives the piston plate (36) guided by the first guide rod (37) to continuously move upward. During the upward movement of the piston plate (36), negative pressure is generated inside the piston cylinder (31). The negative pressure sucks the mixed material at the bottom of the inner cavity of the reactor (11) through the suction pipe (33). In addition, when the first reciprocating screw (22) rotates, it drives the piston cylinder (31) to continuously rotate. When the piston cylinder (31) rotates, it drives the two suction pipes (33) to rotate synchronously, thereby sucking the mixed material at different positions; S3, when the second reciprocating screw (23) rotates, the annular filter screen (42) is driven to rotate via the extension plate (41), and when the annular filter screen (42) rotates, the L-shaped stirring rod (43), the bottom scraper (44), the inner scraper (45) and the outer scraper (46) are driven to rotate synchronously, and when the L-shaped stirring rod (43), the bottom scraper (44), the inner scraper (45) and the outer scraper (46) rotate, the mixed material is continuously stirred, so that the o-cresol and the isopropanol react rapidly under the catalysis of the active catalyst; S4, when the second reciprocating screw (23) rotates, it drives the lifting plate (54) guided by the second guide rod (55) to continuously move downward, and drives the spreading plate (51) slidably nested and arranged outside the lifting plate (54) in the vertical direction to continuously rotate. When the lifting plate (54) moves downward, the restoring spring (53) and the movable ring (52) drive the spreading plate (51) to continuously move downward; S5. When the upward movement distance of the piston plate (36) reaches a first threshold value, the piston plate (36) moves to the top of the reciprocating thread on the outside of the first reciprocating screw (22). Subsequently, as the first reciprocating screw (22) continues to rotate, the piston plate (36) moves downward and resets. During the downward movement of the piston plate (36), due to the obstruction of the one-way valve on the suction pipe (33), the mixed material inside the piston cylinder (31) enters the inside of the output pipe (34) and breaks open the valve (35) to fall on the top of the spreading plate (51). During the upward rotation of the spreading plate (51), the mixed material falling on the top is spread, so that the mixed material falls evenly on the top layer of the mixed material at the bottom of the inner cavity of the reactor (11); S6, when the downward movement distance of the piston plate (36) reaches a second threshold value, the piston plate (36) arrives at the initial position, that is, the bottom end of the outer reciprocating thread of the first reciprocating screw (22), and subsequently, as the first reciprocating screw (22) continues to rotate, the piston plate (36) moves upward again to perform suction; S7, when the downward movement distance of the lifting plate (54) reaches a third threshold value, the lifting plate (54) moves to the bottom end of the outer reciprocating thread of the second reciprocating screw (23), and then as the second reciprocating screw (23) continues to rotate, the lifting plate (54) moves upward and resets; S8, when the upward movement distance of the lifting plate (54) reaches a fourth threshold value, the bottom of the spreading plate (51) seals the bottom of the annular filter screen (42), and the spreading plate (51) and the annular filter screen (42) form an annular filter chamber. At this time, the mixed material reacts to generate a reaction product. At the same time, due to the obstruction of the annular filter screen (42), the spreading plate (51) cannot continue to rise. Subsequently, as the lifting plate (54) continues to rise, the return spring (53) is continuously compressed; S9, stopping the heating of the microwave heating component (13), and when the subsequent suction uniformity mechanism (3) outputs the reaction product, the reaction product falls into the annular filter chamber, and as the annular filter screen (42) continues to rotate, the reaction product passes through the annular filter screen (42) under the action of centrifugal force and is output, while the active catalyst remains inside the annular filter screen (42); S10, when the upward movement distance of the lifting plate (54) reaches the fifth threshold value, the lifting plate (54) moves to the top of the reciprocating thread on the outside of the second reciprocating screw (23), at which time the active catalyst has been filtered out, and the reaction product at the bottom of the inner cavity of the reactor (11) is discharged to obtain a crude carvacrol product. Subsequently, as the second reciprocating screw (23) continues to rotate, the lifting plate (54) moves downward and resets; S11, when the downward movement distance of the lifting plate (54) reaches a sixth threshold value, the compressed reset spring (53) is reset, and at this time, the reaction product has been completely discharged. Subsequently, as the lifting plate (54) continues to move downward, the throwing plate (51) releases the blockage of the bottom of the annular filter (42), and at this time, the active catalyst located on the top of the throwing plate (51) is evenly thrown to the bottom of the inner cavity of the reactor (11) under the action of centrifugal force; S12: When the downward movement distance of the lifting plate (54) reaches the seventh threshold value, the lifting plate (54) arrives at the initial working position, and the driving motor (21) is stopped at this time.

Images