A method for preparing industrial turpentine musk

Abstract

This invention discloses a method for preparing industrial-grade musk, relating to the field of musk synthesis technology. The method utilizes an industrial-grade musk preparation device, which includes a washing mechanism. A separating mechanism is located at the top of the washing mechanism's inner cavity, forming a first annular storage chamber and a second annular storage chamber at the top of the inner cavity. The first annular storage chamber is positioned above the second annular storage chamber. A driving mechanism is jointly provided at the bottom and inside of the washing mechanism. A stirring and discharging mechanism and a lifting and dispensing mechanism are sequentially connected from bottom to top to the outside of the driving mechanism. This invention can more quickly complete the washing of organic layer A and organic layer B, and allows for vacuum distillation without transferring the products, thus significantly improving the efficiency of musk preparation and making it more suitable for industrial production.

Description

Technical Field

[0001] This invention relates to the field of musk synthesis technology, and in particular to a method for preparing industrially produced musk. Background Technology

[0002] Tuna Musk is a daily-use fragrance, belonging to the bicyclic naphthyl musk class. It has a strong powdery aroma, excellent fragrance quality, elegant fragrance, and long-lasting scent. This product has strong diffusion and good compatibility. It is stable in acidic and alkaline media, does not easily change color, and has strong adhesion to fibers. It is suitable for high-end cosmetics such as soaps and face powders.

[0003] The invention patent with authorization announcement number CN 102050715 B discloses a method for preparing industrial turpentine musk. Using p-isopropyltoluene and 2,3-dimethyl-1-butene as raw materials and tert-butyl chloride as a hydrogen absorber, an intermediate 1,1,3,4,4,6-hexamethyltetrahydronaphthalene is synthesized via Friedel-Crafts alkylation. Then, the intermediate is used as a raw material to undergo Friedel-Crafts acylation with acetyl chloride in dichloromethane solvent to obtain the product turpentine musk. Compared with existing methods and technologies, this method is simple to operate, has a fast reaction rate, and the product purification only requires thermal dissolution of the pigment with anhydrous ethanol, eliminating the need for distillation and fractionation, and achieving high yield, thus realizing industrial production.

[0004] After separating the organic layers in reactant A and reactant B, the above preparation method requires multiple washings with saturated sodium chloride for the organic layer in reactant A, and multiple washings with unsaturated sodium carbonate followed by multiple washings with saturated sodium chloride for the organic layer in reactant B. In this process, due to the large volume of organic layers processed in industrial production, a large amount of unsaturated sodium carbonate and saturated sodium chloride are required. After each washing, a long feeding time is needed before the next washing can be completed. This consumes a significant amount of time in practical applications, thus reducing the efficiency of organic layer processing.

[0005] Therefore, it is necessary to invent an industrial method for preparing musk to solve the above problems. Summary of the Invention

[0006] The purpose of this invention is to provide a method for preparing industrial turpentine musk to solve the problems mentioned in the background art.

[0007] To achieve the above objectives, the present invention provides the following technical solution: a method for preparing industrial turbid musk, wherein the method for preparing industrial turbid musk is implemented using an industrial turbid musk preparation device, the industrial turbid musk preparation device includes a washing mechanism, and a separating mechanism is provided at the top of the inner cavity of the washing mechanism. The separating mechanism forms a first annular liquid storage cavity and a second annular liquid storage cavity at the top of the inner cavity of the washing mechanism, wherein the first annular liquid storage cavity is located above the second annular liquid storage cavity;

[0008] The washing mechanism is provided with a drive mechanism at the bottom and inside the washing mechanism. The outside of the drive mechanism is connected to a stirring and discharging mechanism and a lifting liquid supply mechanism in sequence from bottom to top. The stirring and discharging mechanism is provided with a trigger mechanism at the top. The lifting liquid supply mechanism is provided with two closed auxiliary mechanisms at the bottom inside.

[0009] The washing mechanism includes a washing shell, a filter plate, a feed pipe, a liquid outlet pipe, a discharge pipe, a negative pressure pipe, and an electric heating element;

[0010] The filter plate is fixedly installed at the bottom of the inner cavity of the washing shell. The feed pipe and the liquid outlet pipe are fixedly installed through the left side of the washing shell from top to bottom. The discharge pipe and the negative pressure pipe are fixedly installed through the right side of the washing shell from bottom to top. The electric heating element is fixedly sleeved at the bottom of the outer side of the washing shell.

[0011] The separation mechanism includes a first separation plate, a second separation plate, an annular guide platform, a first liquid inlet pipe, a second liquid inlet pipe, and a pressure equalization pipe;

[0012] The first partition plate and the second partition plate are fixedly installed on the top inner side of the washing shell from top to bottom. There are two annular flow guides, which are fixedly installed on the top of the first partition plate and the second partition plate respectively. The first liquid inlet pipe and the second liquid inlet pipe are fixedly installed through the top left side of the washing shell from top to bottom. There are two pressure equalization pipes, which are fixedly installed through the top right side of the washing shell.

[0013] Preferably, the drive mechanism includes a drive motor, a drive shaft, and a reciprocating screw;

[0014] The drive motor is fixedly installed at the bottom of the washing housing. The drive shaft is located inside the washing housing and is connected to the drive motor for transmission. The reciprocating screw is connected to the top of the drive shaft through an overrunning clutch. The top of the reciprocating screw penetrates the inner wall of the washing housing and extends to the outer side of the washing housing. The reciprocating screw is rotatably connected to the washing housing through a bearing.

[0015] Preferably, the mixing and discharging mechanism includes a fixing collar, an arc-shaped guide plate, and multiple mixing components, wherein the mixing components include a mixing main rod, a mixing support rod, and a limiting collar.

[0016] Preferably, the fixing collar is fixedly sleeved on the top outer side of the drive shaft, multiple arc-shaped guide plates are provided, and the multiple arc-shaped guide plates are evenly fixedly provided on the outer side of the fixing collar, multiple sets of stirring components are rotatably provided on the top of the multiple arc-shaped guide plates, the bottom end of the stirring main rod is rotatably nested on the top of the arc-shaped guide plate through a bearing, multiple stirring support rods are provided, and the multiple stirring support rods are evenly fixedly provided on both sides of the stirring main rod, and the limiting collar is fixedly sleeved on the middle outer side of the stirring main rod.

[0017] Preferably, the triggering mechanism includes a mounting collar, an inner annular sleeve, a first spring, an outer annular sleeve, and a threaded sleeve;

[0018] The mounting collar is rotatably sleeved on the bottom outer side of the reciprocating screw via a bearing. The inner annular sleeve is slidably sleeved on the middle outer side of the reciprocating screw. The first spring is sleeved on the outer side of the reciprocating screw and located between the mounting collar and the inner annular sleeve. The outer annular sleeve is rotatably sleeved on the outer side of the inner annular sleeve via a bearing. Multiple threaded sleeves are provided, and multiple threaded sleeves are uniformly fixed and penetrated through the top of the outer annular sleeve and respectively sleeved on the outer side of multiple stirring main rods.

[0019] Preferably, the lifting liquid supply mechanism includes a lifting cylinder, a lifting collar, and a connecting rod;

[0020] The lifting cylinder is slidably nested inside the first partition plate and the second partition plate. A strip slider is fixedly installed on both sides of the lifting cylinder. A limit groove is provided on the inner side of the first partition plate and the second partition plate. The strip slider is slidably installed inside the limit groove. The lifting collar is sleeved on the outside of the reciprocating screw and is connected to the reciprocating screw through a reciprocating thread. Multiple connecting rods are provided. The multiple connecting rods are evenly fixedly installed on the outside of the lifting collar and are all fixedly connected to the inner wall of the lifting cylinder.

[0021] Preferably, the enclosed auxiliary mechanism includes a mounting plate, a support rod, an end plate, and a second spring;

[0022] The mounting plate is fixedly connected to the inner wall of the lifting cylinder, the support rod passes through the mounting plate and is slidably connected to the mounting plate, the end plate is fixedly installed at the top of the support rod, the second spring is sleeved on the outside of the support rod, one end of the second spring is fixedly connected to the mounting plate and the other end is fixedly connected to the end plate.

[0023] Preferably, the preparation method of the industrial turpentine musk specifically includes the following steps:

[0024] S1. Using p-isopropyltoluene, 2,3-dimethyl-1-butene, and tert-butyl chloride as raw materials, a reaction solution A is formed. Using anhydrous aluminum trichloride, concentrated sulfuric acid, hydrochloric acid, and cyclohexane as raw materials, a reaction mixture A is formed. The reaction solution A is added dropwise to the reaction mixture A to form reactant A. The reactant is added to brine and stirred continuously to form a mixed liquid A. The mixed liquid A is added into the washing shell through the feed pipe. The mixed liquid A falls to the bottom of the inner cavity of the washing shell and is filtered by the filter plate to obtain organic layer A.

[0025] S2. While performing the above operation, saturated sodium chloride is added to the second annular storage chamber through the second inlet pipe. After the mixed liquid A is filtered, the addition of saturated sodium chloride is completed.

[0026] S3. Start the drive motor so that the drive motor drives the drive shaft to rotate clockwise. At this time, the drive shaft drives the reciprocating screw to rotate synchronously. When the reciprocating screw rotates, it drives the lifting cylinder to descend synchronously through the lifting collar and connecting rod. As the lifting cylinder continues to descend, the saturated sodium chloride in the second annular liquid storage chamber enters the interior of the lifting cylinder through the opening at the top of the lifting cylinder, and then falls to the top of the organic layer A, thus completing one saturated sodium chloride output.

[0027] S4. Switch the drive direction of the drive motor so that the drive motor drives the drive shaft to rotate counterclockwise. At this time, due to the limitation of the overrunning clutch, the reciprocating screw does not rotate. When the drive motor rotates, it drives the arc-shaped guide plate to rotate through the fixed collar. At the same time, the arc-shaped guide plate drives multiple stirring support rods to rotate through the stirring main rod, thereby stirring the organic layer A mixed with saturated sodium chloride, thus completing the first washing of the organic layer A.

[0028] S5. Repeatedly switch the drive direction of the drive motor multiple times to complete multiple washes of the organic layer A. At the same time, as the lifting drum continues to descend, when the descent distance of the lifting drum reaches the first threshold, the lifting drum drives the support rod to push the inner annular sleeve plate. The inner annular sleeve plate drives the threaded sleeve to descend through the outer annular sleeve plate. When the threaded sleeve descends, it drives the stirring main rod to rotate. When the stirring main rod rotates, it drives multiple stirring support rods to rotate around the stirring main rod as the axis, thereby better stirring the organic layer being washed.

[0029] S6. When the lifting cylinder descends to the second threshold, the inner annular sleeve drives the threaded sleeve to descend to the top of the limiting sleeve. At this time, the inner annular sleeve can no longer descend. Then, driven by the lifting cylinder, the support rod is pushed upward. When the lifting cylinder descends to the third threshold, the bottom of the lifting cylinder contacts the top of the inner annular sleeve, and the inner annular sleeve closes the bottom opening of the lifting cylinder. At the same time, the lifting sleeve moves to the lowest end of the reciprocating thread on the outside of the reciprocating screw.

[0030] S7. Subsequently, anhydrous sodium sulfate is manually added to the inside of the washing shell to dry the washed organic layer A. Then, the electric heating element is activated, and air inside the washing shell is drawn in through the negative pressure tube. At this time, the bottom of the inner cavity of the washing shell is under negative pressure, and the organic layer A is distilled under reduced pressure to obtain intermediate 1,1,3,4,4,6-hexamethyltetrahydronaphthalene.

[0031] S8. The drive motor drives the drive shaft to rotate counterclockwise, which in turn causes the fixed collar to rotate multiple arc-shaped guide plates. The arc-shaped guide plates push the intermediate 1,1,3,4,4,6-hexamethyltetrahydronaphthalene, so that it is output through the discharge pipe.

[0032] S9. Using 1,1,3,4,4,6-hexamethyltetrahydronaphthalene and acetyl chloride as raw materials, a reaction solution B is formed. Using anhydrous aluminum trichloride and dichloromethane as raw materials, a reaction mixture B is formed. The reaction solution B is added dropwise to the reaction mixture B to form reactant B. The reactant is added to brine and stirred continuously to form a mixed liquid B. The mixed liquid B is added into the washing shell through the feed pipe. The mixed liquid A falls to the bottom of the inner cavity of the washing shell and is filtered by the filter plate to obtain the organic layer B.

[0033] S10. When performing the above operation, unsaturated sodium carbonate and saturated sodium chloride are added to the first annular storage chamber and the second annular storage chamber through the first liquid inlet pipe and the second liquid inlet pipe, respectively. After the mixture liquid B is filtered, the addition of unsaturated sodium carbonate and saturated sodium chloride is completed.

[0034] S11. Repeat S3-S7 above to obtain crude 7-acetyl-1,1,3,4,4,6-hexamethyltetrahydronaphthalene. Mix the crude 7-acetyl-1,1,3,4,4,6-hexamethyltetrahydronaphthalene with anhydrous ethanol and let stand until solid precipitates. Then filter to obtain tuna musk.

[0035] The technical effects and advantages of this invention are as follows:

[0036] This invention incorporates a separating mechanism, a driving mechanism, a stirring and discharging mechanism, a triggering mechanism, a lifting liquid supply mechanism, and a sealing auxiliary mechanism. The driving mechanism intermittently drives the lifting liquid supply mechanism, causing the separating mechanism to intermittently supply saturated sodium chloride and unsaturated sodium carbonate to the bottom of the washing shell cavity via the lifting liquid supply mechanism. This rapidly completes the washing of organic layers A and B. Simultaneously, as the lifting liquid supply mechanism is continuously driven, it further drives the stirring and discharging mechanism through the sealing auxiliary mechanism and the triggering mechanism, enhancing the stirring effect. Finally, with the continuous movement of the lifting liquid supply mechanism, the sealing auxiliary mechanism is eventually triggered, sealing the bottom of the lifting liquid supply mechanism and creating a closed environment at the bottom of the washing shell cavity. This provides conditions for subsequent vacuum distillation. Compared to similar devices or methods in the prior art, this invention can complete the washing of organic layers A and B more quickly, and vacuum distillation can be performed without transferring the products, thus significantly improving the efficiency of musk preparation and making it more suitable for industrial production. Attached Figure Description

[0037] Figure 1 This is a schematic diagram of the overall front view of the washing housing of the present invention after it has been cut open.

[0038] Figure 2 This is a schematic diagram of the overall front cross-sectional structure of the present invention.

[0039] Figure 3 This is a front cross-sectional view of the drive mechanism, stirring and discharging mechanism, and triggering mechanism of the present invention.

[0040] Figure 4 This is a front cross-sectional view of the separation mechanism, lifting liquid supply mechanism, and sealing auxiliary mechanism of the present invention.

[0041] In the diagram: 1. Washing mechanism; 11. Washing shell; 12. Filter plate; 13. Feed pipe; 14. Liquid outlet pipe; 15. Discharge pipe; 16. Negative pressure pipe; 17. Heating element; 2. Separating mechanism; 21. First separator plate; 22. Second separator plate; 23. Annular guide platform; 24. First liquid inlet pipe; 25. Second liquid inlet pipe; 26. Pressure equalizing pipe; 3. Drive mechanism; 31. Drive motor; 32. Drive shaft; 33. Reciprocating screw; 4. Stirring and discharging mechanism; 41. Fixing collar; 42. Arc-shaped guide plate; 43. Stirring main rod; 44. Stirring support rod; 45. Limiting collar; 5. Triggering mechanism; 51. Mounting collar; 52. Inner annular sleeve; 53. First spring; 54. Outer annular sleeve; 55. Threaded sleeve; 6. Lifting liquid supply mechanism; 61. Lifting cylinder; 62. Lifting collar; 63. Connecting rod; 7. Sealing auxiliary mechanism; 71. Mounting plate; 72. Support rod; 73. End plate; 74. Second spring. Detailed Implementation

[0042] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0043] Example 1

[0044] This invention provides, for example Figure 1-4 The present invention discloses a method for preparing industrial musk, wherein the method is implemented using an industrial musk preparation device, the industrial musk preparation device includes a washing mechanism 1, and a separating mechanism 2 is provided at the top of the inner cavity of the washing mechanism 1. The separating mechanism 2 forms a first annular liquid storage cavity and a second annular liquid storage cavity at the top of the inner cavity of the washing mechanism 1, wherein the first annular liquid storage cavity is located above the second annular liquid storage cavity.

[0045] The washing mechanism 1 is provided with a drive mechanism 3 at its bottom and inside. The drive mechanism 3 is connected to a stirring and discharging mechanism 4 and a lifting liquid supply mechanism 6 from bottom to top on its outer side. The stirring and discharging mechanism 4 is provided with a trigger mechanism 5 at its top. The lifting liquid supply mechanism 6 is provided with two closed auxiliary mechanisms 7 at its inner bottom.

[0046] like Figure 2 As shown, the washing mechanism 1 includes a washing housing 11, a filter plate 12, a feed pipe 13, a liquid outlet pipe 14, a discharge pipe 15, a negative pressure pipe 16, and an electric heating element 17. The filter plate 12 is fixedly disposed at the bottom of the inner cavity of the washing housing 11. The feed pipe 13 and the liquid outlet pipe 14 are fixedly disposed through the left side of the washing housing 11 from top to bottom. The discharge pipe 15 and the negative pressure pipe 16 are fixedly disposed through the right side of the washing housing 11 from bottom to top. The electric heating element 17 is fixedly sleeved on the bottom outer side of the washing housing 11.

[0047] like Figure 2 and Figure 4As shown, the separating mechanism 2 includes a first separating plate 21, a second separating plate 22, an annular guide platform 23, a first liquid inlet pipe 24, a second liquid inlet pipe 25, and a pressure equalizing pipe 26. The first separating plate 21 and the second separating plate 22 are fixedly arranged on the top inner side of the washing housing 11 from top to bottom. There are two annular guide platforms 23, which are respectively fixedly arranged on the top of the first separating plate 21 and the second separating plate 22. The first liquid inlet pipe 24 and the second liquid inlet pipe 25 are fixedly arranged through the top left side of the washing housing 11 from top to bottom. There are two pressure equalizing pipes 26, which are both fixedly arranged through the top right side of the washing housing 11.

[0048] By setting up the above structure, unsaturated sodium carbonate and saturated sodium chloride can be added to the first annular storage chamber and the second annular storage chamber through the first liquid inlet pipe 24 and the second liquid inlet pipe 25.

[0049] like Figure 3 As shown, the drive mechanism 3 includes a drive motor 31, a drive shaft 32, and a reciprocating screw 33. The drive motor 31 is fixedly mounted on the bottom of the washing housing 11. The drive shaft 32 is located inside the washing housing 11 and is connected to the drive motor 31 in a transmission manner. The reciprocating screw 33 is connected to the top of the drive shaft 32 through an overrunning clutch. The top of the reciprocating screw 33 penetrates the inner wall of the washing housing 11 and extends to the outer side of the washing housing 11. The reciprocating screw 33 is rotatably connected to the washing housing 11 through a bearing.

[0050] By setting the above structure, the drive motor 31 drives the drive shaft 32 to rotate clockwise, and the reciprocating screw 33 rotates synchronously. When the drive motor 31 drives the drive shaft 32 to rotate counterclockwise, the reciprocating screw 33 does not rotate due to the limitation of the overrunning clutch.

[0051] like Figure 3 As shown, the mixing and discharging mechanism 4 includes a fixed collar 41, an arc-shaped guide plate 42, and multiple sets of mixing components. Each mixing component includes a mixing main rod 43, mixing support rods 44, and a limiting collar 45. The fixed collar 41 is fixedly sleeved on the top outer side of the drive shaft 32. Multiple arc-shaped guide plates 42 are provided and are evenly fixedly arranged on the outer side of the fixed collar 41. Multiple sets of mixing components are rotatably arranged on the top of the multiple arc-shaped guide plates 42. The bottom end of the mixing main rod 43 is rotatably nested on the top of the arc-shaped guide plate 42 through a bearing. Multiple mixing support rods 44 are provided and are evenly fixedly arranged on both sides of the mixing main rod 43. The limiting collar 45 is fixedly sleeved on the middle outer side of the mixing main rod 43.

[0052] By setting the above structure, when the drive motor 31 rotates, it drives the arc-shaped guide plate 42 to rotate through the fixed collar 41. At the same time, the arc-shaped guide plate 42 drives multiple stirring support rods 44 to rotate through the stirring main rod 43, thereby stirring the organic layer A mixed with saturated sodium chloride, the organic layer B mixed with saturated sodium chloride, or the organic layer B mixed with unsaturated sodium carbonate.

[0053] like Figure 3 As shown, the triggering mechanism 5 includes a mounting collar 51, an inner annular sleeve 52, a first spring 53, an outer annular sleeve 54, and a threaded sleeve 55. The mounting collar 51 is rotatably sleeved on the bottom outer side of the reciprocating screw 33 via a bearing. The inner annular sleeve 52 is slidably sleeved on the middle outer side of the reciprocating screw 33. The first spring 53 is sleeved on the outer side of the reciprocating screw 33 and located between the mounting collar 51 and the inner annular sleeve 52. The outer annular sleeve 54 is rotatably sleeved on the outer side of the inner annular sleeve 52 via a bearing. Multiple threaded sleeves 55 are provided, and multiple threaded sleeves 55 are uniformly fixedly and penetrate through the top of the outer annular sleeve 54 and are respectively sleeved on the outer side of multiple stirring rods 43.

[0054] By setting up the above structure, when the inner annular sleeve 52 is pressed down, the inner annular sleeve 52 drives the threaded sleeve 55 to descend through the outer annular sleeve 54. When the threaded sleeve 55 descends, it drives the stirring main rod 43 to rotate. When the stirring main rod 43 rotates, it drives multiple stirring support rods 44 to rotate around the stirring main rod 43 as the axis, thereby better stirring the organic layer being washed.

[0055] like Figure 4 As shown, the lifting liquid supply mechanism 6 includes a lifting cylinder 61, a lifting collar 62, and connecting rods 63. The lifting cylinder 61 is slidably nested inside the first partition plate 21 and the second partition plate 22. Strip-shaped sliders are fixedly provided on both sides of the lifting cylinder 61. Limiting grooves are provided on the inner sides of the first partition plate 21 and the second partition plate 22. The strip-shaped sliders are slidably disposed inside the limiting grooves. The lifting collar 62 is sleeved on the outer side of the reciprocating screw 33 and is connected to the reciprocating screw 33 through a reciprocating thread. Multiple connecting rods 63 are provided, and the multiple connecting rods 63 are evenly fixedly disposed on the outer side of the lifting collar 62 and are all fixedly connected to the inner wall of the lifting cylinder 61.

[0056] By setting the above structure, after the lifting collar 62 is driven by the reciprocating screw 33, the lifting collar 62 drives the lifting cylinder 61 to descend intermittently through the connecting rod 63, thereby causing the saturated sodium chloride in the second annular liquid storage chamber or the unsaturated sodium carbonate in the first annular liquid storage chamber and the saturated sodium chloride in the second annular liquid storage chamber to be intermittently input into the bottom of the inner cavity of the washing shell 11.

[0057] like Figure 4 As shown, the closed auxiliary mechanism 7 includes a mounting plate 71, a support rod 72, an end plate 73, and a second spring 74. The mounting plate 71 is fixedly connected to the inner wall of the lifting cylinder 61. The support rod 72 passes through the mounting plate 71 and is slidably connected to the mounting plate 71. The end plate 73 is fixedly disposed on the top end of the support rod 72. The second spring 74 is sleeved on the outside of the support rod 72. One end of the second spring 74 is fixedly connected to the mounting plate 71, and the other end is fixedly connected to the end plate 73.

[0058] By setting up the above structure, when the inner annular sleeve 52 can no longer descend, the support rod 72 is compressed and rises, and then pulls the second spring 74 through the end plate 73. As the support rod 72 continues to rise, the inner annular sleeve 52 seals the bottom of the lifting cylinder 61, thereby forming a closed environment at the bottom of the inner cavity of the washing shell 11, providing conditions for subsequent vacuum distillation.

[0059] Example 2

[0060] The preparation method of the industrial musk specifically includes the following steps:

[0061] S1. Using p-isopropyltoluene, 2,3-dimethyl-1-butene, and tert-butyl chloride as raw materials, a reaction solution A is formed by mixing them. Using anhydrous aluminum trichloride, concentrated sulfuric acid, hydrochloric acid, and cyclohexane as raw materials, a reaction mixture A is formed by mixing them. The reaction solution A is added dropwise to the reaction mixture A to form reactant A. The reactant is added to brine and stirred continuously to form a mixed liquid A. The mixed liquid A is added into the washing shell 11 through the feed pipe 13. The mixed liquid A falls to the bottom of the inner cavity of the washing shell 11 and is filtered by the filter plate 12 to obtain an organic layer A.

[0062] S2. While performing the above operation, saturated sodium chloride is added to the second annular storage chamber through the second liquid inlet pipe 25. The addition of saturated sodium chloride is completed after the mixed liquid A is filtered.

[0063] S3. Start the drive motor 31, which drives the drive shaft 32 to rotate clockwise. At this time, the drive shaft 32 drives the reciprocating screw 33 to rotate synchronously. When the reciprocating screw 33 rotates, it drives the lifting cylinder 61 to descend synchronously through the lifting collar 62 and the connecting rod 63. As the lifting cylinder 61 continues to descend, the saturated sodium chloride in the second annular liquid storage chamber enters the interior of the lifting cylinder 61 through the top opening of the lifting cylinder 61, and then falls to the top of the organic layer A, thus completing one saturated sodium chloride output.

[0064] S4. Switch the drive direction of the drive motor 31 so that the drive motor 31 drives the drive shaft 32 to rotate counterclockwise. At this time, due to the limitation of the overrunning clutch, the reciprocating screw 33 does not rotate. When the drive motor 31 rotates, it drives the arc-shaped guide plate 42 to rotate through the fixed collar 41. At the same time, the arc-shaped guide plate 42 drives multiple stirring support rods 44 to rotate through the stirring main rod 43, thereby stirring the organic layer A mixed with saturated sodium chloride, thus completing the first washing of the organic layer A.

[0065] S5. Repeatedly switch the drive direction of the drive motor 31 multiple times to complete multiple washes of the organic layer A. At the same time, as the lifting drum 61 continues to descend, when the descent distance of the lifting drum 61 reaches the first threshold, the lifting drum 61 drives the support rod 72 to push the inner annular sleeve 52. The inner annular sleeve 52 drives the threaded sleeve 55 to descend through the outer annular sleeve 54. When the threaded sleeve 55 descends, it drives the stirring main rod 43 to rotate. When the stirring main rod 43 rotates, it drives multiple stirring support rods 44 to rotate around the stirring main rod 43 as the axis, thereby better stirring the organic layer being washed.

[0066] S6. When the lifting cylinder 61 descends to the second threshold, the inner annular sleeve 52 drives the threaded sleeve 55 to descend to the top of the limiting sleeve 45. At this time, the inner annular sleeve 52 can no longer descend. Then, driven by the lifting cylinder 61, the support rod 72 is pushed upward. When the lifting cylinder 61 descends to the third threshold, the bottom of the lifting cylinder 61 contacts the top of the inner annular sleeve 52. The inner annular sleeve 52 closes the bottom opening of the lifting cylinder 61. At the same time, the lifting sleeve 62 moves to the lowest end of the reciprocating thread on the outside of the reciprocating screw 33.

[0067] S7. Subsequently, anhydrous sodium sulfate is manually added to the inside of the washing shell 11 to dry the washed organic layer A. Then, the heating element 17 is activated, and the air inside the washing shell 11 is drawn through the negative pressure pipe 16. At this time, the bottom of the inner cavity of the washing shell 11 is under negative pressure, and the organic layer A is distilled under reduced pressure to obtain the intermediate 1,1,3,4,4,6-hexamethyltetrahydronaphthalene.

[0068] S8. Drive the drive motor 31 to drive the drive shaft 32 to rotate counterclockwise, which in turn causes the fixed collar 41 to drive multiple arc-shaped guide plates 42 to rotate. The arc-shaped guide plates 42 push the intermediate 1,1,3,4,4,6-hexamethyltetrahydronaphthalene, so that it is output through the discharge pipe 15.

[0069] S9. Using 1,1,3,4,4,6-hexamethyltetrahydronaphthalene and acetyl chloride as raw materials, a reaction solution B is formed by mixing them. Anhydrous aluminum trichloride and dichloromethane are used as raw materials to form a reaction mixture B. The reaction solution B is added dropwise to the reaction mixture B to form reactant B. The reactant is added to brine and stirred continuously to form a mixed liquid B. The mixed liquid B is added into the washing shell 11 through the feed pipe 13. The mixed liquid A falls to the bottom of the inner cavity of the washing shell 11 and is filtered by the filter plate 12 to obtain the organic layer B.

[0070] S10. When performing the above operation, unsaturated sodium carbonate and saturated sodium chloride are added to the first annular storage chamber and the second annular storage chamber through the first liquid inlet pipe 24 and the second liquid inlet pipe 25 respectively. After the mixture liquid B is filtered, the addition of unsaturated sodium carbonate and saturated sodium chloride is completed.

[0071] S11. Repeat S3-S7 above to obtain crude 7-acetyl-1,1,3,4,4,6-hexamethyltetrahydronaphthalene. Mix the crude 7-acetyl-1,1,3,4,4,6-hexamethyltetrahydronaphthalene with anhydrous ethanol and let stand until solid precipitates. Then filter to obtain tuna musk.

[0072] This invention incorporates a separating mechanism 2, a driving mechanism 3, a stirring and discharging mechanism 4, a triggering mechanism 5, a lifting liquid supply mechanism 6, and a sealing auxiliary mechanism 7. The driving mechanism 3 intermittently drives the lifting liquid supply mechanism 6, thereby causing the separating mechanism 2 to intermittently supply saturated sodium chloride and unsaturated sodium carbonate to the bottom of the washing housing 11 via the lifting liquid supply mechanism 6, rapidly completing the washing of organic layers A and B. Simultaneously, as the lifting liquid supply mechanism 6 is continuously driven, it, through the sealing auxiliary mechanism 7 and the triggering mechanism 5, performs secondary stirring and discharging on the stirring and discharging mechanism 4. The driving mechanism enhances the stirring effect of the stirring and discharging mechanism 4. Simultaneously, as the lifting liquid supply mechanism 6 moves continuously, the sealing auxiliary mechanism 7 is eventually triggered, causing the triggering mechanism 5 to seal the bottom of the lifting liquid supply mechanism 6. This creates a closed environment at the bottom of the inner cavity of the washing shell 11, providing conditions for subsequent vacuum distillation. Compared with similar devices or methods in the prior art, this invention can complete the washing of organic layer A and organic layer B more quickly, and can perform vacuum distillation without transferring the product, thereby significantly improving the preparation efficiency of musk and making it more suitable for industrial production.

[0073] Finally, it should be noted that the above description 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 foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A process for the preparation of industrial tonal musk, characterized in that: The preparation method of the industrial tonal musk is realized by using an industrial tonal musk preparation device, which comprises a washing mechanism (1), a separation mechanism (2) arranged at the top of the inner cavity of the washing mechanism (1), and a first annular liquid storage cavity and a second annular liquid storage cavity formed by the separation mechanism (2) at the top of the inner cavity of the washing mechanism (1), wherein the first annular liquid storage cavity is located above the second annular liquid storage cavity; The bottom of the washing mechanism (1) and the inside of the washing mechanism (1) are jointly provided with a driving mechanism (3), the outer side of the driving mechanism (3) is sequentially connected with a stirring and discharging mechanism (4) and a lifting liquid feeding mechanism (6) from bottom to top, the top of the stirring and discharging mechanism (4) is provided with a triggering mechanism (5), and the inner side of the lifting liquid feeding mechanism (6) is provided with two closed auxiliary mechanisms (7) at the bottom. The washing mechanism (1) comprises a washing shell (11), a filter plate (12), a feeding pipe (13), a liquid outlet pipe (14), a discharging pipe (15), a negative pressure pipe (16) and an electric heating element (17). The filter plate (12) is fixedly arranged at the bottom of the inner cavity of the washing shell (11), the feeding pipe (13) and the liquid outlet pipe (14) are sequentially fixedly and penetratively arranged on the left side of the washing shell (11) from top to bottom, the discharging pipe (15) and the negative pressure pipe (16) are sequentially fixedly and penetratively arranged on the right side of the washing shell (11) from bottom to top, and the electric heating element (17) is fixedly and sleevedly arranged at the bottom of the outer side of the washing shell (11). The separation mechanism (2) comprises a first separation plate (21), a second separation plate (22), an annular flow guide table (23), a first liquid inlet pipe (24), a second liquid inlet pipe (25) and an equalizing pipe (26). The first separation plate (21) and the second separation plate (22) are sequentially fixedly arranged on the top of the inner side of the washing shell (11) from top to bottom, the annular flow guide table (23) is provided with two annular flow guide tables (23) fixedly arranged on the top of the first separation plate (21) and the second separation plate (22), respectively, the first liquid inlet pipe (24) and the second liquid inlet pipe (25) are sequentially fixedly and penetratively arranged on the top of the left side of the washing shell (11) from top to bottom, and the equalizing pipe (26) is provided with two equalizing pipes (26) fixedly and penetratively arranged on the top of the right side of the washing shell (11).

2. A process for the preparation of industrial tonal musk as claimed in claim 1, wherein: The driving mechanism (3) comprises a driving motor (31), a driving shaft (32) and a reciprocating screw (33). The driving motor (31) is fixedly arranged at the bottom of the washing shell (11), the driving shaft (32) is located in the inside of the washing shell (11) and is in transmission connection with the driving motor (31), the reciprocating screw (33) is connected to the top end of the driving shaft (32) through an overrunning clutch, the top end of the reciprocating screw (33) penetrates the inner wall of the washing shell (11) and extends to the outside of the washing shell (11), and the reciprocating screw (33) is rotationally connected with the washing shell (11) through a bearing.

3. A process for the preparation of industrial tonal musk as claimed in claim 2, wherein: The stirring discharging mechanism (4) comprises a fixed collar (41), an arc-shaped guide plate (42) and a plurality of stirring assemblies, wherein the stirring assembly comprises a stirring main rod (43), a stirring branch rod (44) and a limiting collar (45).

4. A process for the preparation of industrial tonal musk as claimed in claim 3, wherein: The fixed collar (41) is fixedly sleeved on the top of the outer side of the driving shaft (32), the arc-shaped guide plate (42) is provided in plurality, the plurality of arc-shaped guide plates (42) are uniformly fixedly arranged on the outer side of the fixed collar (41), the plurality of stirring assemblies are rotatably arranged on the top of the plurality of arc-shaped guide plates (42), respectively, the stirring main rod (43) is rotatably and nested on the top of the arc-shaped guide plate (42) through a bearing, the stirring branch rod (44) is provided in plurality, the plurality of stirring branch rods (44) are uniformly fixedly arranged on the two sides of the stirring main rod (43), and the limiting collar (45) is fixedly sleeved on the middle of the outer side of the stirring main rod (43).

5. A process for the preparation of industrial tonal musk as claimed in claim 4 wherein: The trigger mechanism (5) comprises a mounting collar (51), an inner annular sleeve plate (52), a first spring (53), an outer annular sleeve plate (54) and a threaded sleeve (55). The mounting collar (51) is rotatably and sleeved on the bottom of the outer side of the reciprocating screw rod (33) through a bearing, the inner annular sleeve plate (52) is slidably and sleeved on the middle of the outer side of the reciprocating screw rod (33), the first spring (53) is sleeved on the outer side of the reciprocating screw rod (33) and located between the mounting collar (51) and the inner annular sleeve plate (52), the outer annular sleeve plate (54) is rotatably and sleeved on the outer side of the inner annular sleeve plate (52) through a bearing, and the threaded sleeve (55) is provided in plurality, the plurality of threaded sleeves are uniformly and fixedly arranged on the top of the outer annular sleeve plate (54) and are sleeved on the outer sides of the plurality of stirring main rods (43), respectively.

6. A process for the preparation of industrial tonal musk as claimed in claim 5 wherein: The lifting type liquid feeding mechanism (6) comprises a lifting cylinder (61), a lifting collar (62) and a connecting rod (63). The lifting cylinder (61) is slidably and nested on the inner sides of the first partition plate (21) and the second partition plate (22), the lifting cylinder (61) is fixedly provided with a strip-shaped sliding block on the two sides, the inner sides of the first partition plate (21) and the second partition plate (22) are provided with limiting sliding grooves, the strip-shaped sliding blocks are slidably arranged on the inner sides of the limiting sliding grooves, the lifting collar (62) is sleeved on the outer side of the reciprocating screw rod (33) and is drivingly connected with the reciprocating screw rod (33) through a reciprocating thread, and the connecting rod (63) is provided in plurality, the plurality of connecting rods (63) are uniformly fixedly arranged on the outer side of the lifting collar (62) and are fixedly connected with the inner wall of the lifting cylinder (61).

7. A process for the preparation of industrial tonal musk as claimed in claim 6 wherein: The closing auxiliary mechanism (7) comprises a mounting plate (71), a supporting rod (72), an end plate (73) and a second spring (74). The mounting plate (71) is fixedly connected with the inner wall of the lifting cylinder (61), the supporting rod (72) penetrates through the mounting plate (71) and is in sliding connection with the mounting plate (71), the end plate (73) is fixedly arranged at the top end of the supporting rod (72), the second spring (74) is sleeved and arranged outside the supporting rod (72), one end of the second spring (74) is fixedly connected with the mounting plate (71), and the other end is fixedly connected with the end plate (73).

8. A process for the preparation of industrial tonal musk as claimed in claim 7 wherein, The preparation method of the industrial tonal musk specifically comprises the following steps: S1, with p-cymene, 2,3-dimethyl-1-butene and tert-butyl chloride as raw materials, a material reaction liquid A is formed, with anhydrous aluminum chloride, concentrated sulfuric acid, hydrochloric acid and cyclohexane as raw materials, a reaction mixture A is formed, the material reaction liquid A is added dropwise into the reaction mixture A to form a reactant A, the reactant is added into the brine and continuously stirred to form a mixed liquid A, the mixed liquid A is added into the inside of the washing shell (11) through the feeding pipe (13), the mixed liquid A falls on the filter plate (12) at the bottom of the inside cavity of the washing shell (11) and is filtered to obtain an organic layer A; S2, when the above operation is performed, saturated sodium chloride is added into the second annular liquid storage cavity through the second liquid inlet pipe (25) at the same time, and after the filtering of the mixed liquid A is completed, the addition of the saturated sodium chloride is completed; S3, the driving motor (31) is started, so that the driving motor (31) drives the driving shaft (32) to rotate clockwise, at this time, the driving shaft (32) drives the reciprocating screw (33) to rotate synchronously, and when the reciprocating screw (33) rotates, the lifting sleeve ring (62) and the connecting rod (63) drive the lifting cylinder (61) to descend synchronously, with the continuous descent of the lifting cylinder (61), the saturated sodium chloride in the second annular liquid storage cavity enters into the inside of the lifting cylinder (61) through the top opening of the lifting cylinder (61), and then falls on the top of the organic layer A, and then the output of the saturated sodium chloride is completed once; S4, the driving direction of the driving motor (31) is switched, so that the driving motor (31) drives the driving shaft (32) to rotate counterclockwise, at this time, due to the limitation of the overrunning clutch, the reciprocating screw (33) does not rotate, and when the driving motor (31) rotates, the fixed sleeve ring (41) drives the arc-shaped guide plate (42) to rotate, and at the same time, the arc-shaped guide plate (42) drives the plurality of stirring branch rods (44) to rotate through the stirring main rod (43), so as to stir the organic layer A mixed with the saturated sodium chloride, and then the washing of the organic layer A is completed once. S5, repeatedly switch the driving direction of the motor (31) multiple times, thereby completing multiple washing of the organic layer A, and as the lifting cylinder (61) continues to descend, when the descending distance of the lifting cylinder (61) reaches a first threshold value, the lifting cylinder (61) drives the support rod (72) to push the inner annular sleeve plate (52), the inner annular sleeve plate (52) drives the threaded sleeve (55) to descend through the outer annular sleeve plate (54), the threaded sleeve (55) drives the stirring main rod (43) to rotate when descending, the stirring main rod (43) drives multiple stirring branch rods (44) to rotate around the stirring main rod (43) when rotating, thereby better stirring the washed organic layer; S6, when the descending distance of the lifting cylinder (61) reaches a second threshold value, the inner annular sleeve plate (52) drives the threaded sleeve (55) to descend to the top of the limiting sleeve ring (45), at this time the inner annular sleeve plate (52) cannot continue to descend, then under the driving of the lifting cylinder (61), the support rod (72) is pushed upward, when the descending distance of the lifting cylinder (61) reaches a third threshold value, the bottom of the lifting cylinder (61) contacts the top of the inner annular sleeve plate (52), the inner annular sleeve plate (52) closes the opening at the bottom of the lifting cylinder (61), and at the same time the lifting sleeve ring (62) moves to the outer side of the reciprocating screw (33) to the lowermost end of the reciprocating thread; S7, then add anhydrous sodium sulfate into the inside of the washing shell (11) by hand, thereby drying the washed organic layer A, then start the heating element (17), and at the same time, the air inside the washing shell (11) is sucked through the negative pressure pipe (16), at this time the bottom of the inner cavity of the washing shell (11) is in a negative pressure state, the organic layer A is distilled under reduced pressure to obtain intermediate 1,1,3,4,4,6-hexamethyltetralin; S8, drive the motor (31) to rotate the drive shaft (32) counterclockwise, thereby driving the fixed sleeve ring (41) to rotate the multiple arc-shaped guide plates (42), the arc-shaped guide plates (42) push the intermediate 1,1,3,4,4,6-hexamethyltetralin to pass through the discharge pipe (15) and be output; S9, using 1,1,3,4,4,6-hexamethyltetralin and acetyl chloride as raw materials, mixing to form a material reaction liquid B, using anhydrous aluminum chloride and dichloromethane as raw materials, mixing to form a reaction mixture B, adding the material reaction liquid B dropwise into the reaction mixture B to form a reactant B, adding the reactant into the brine and continuously stirring to form a mixed liquid B, adding the mixed liquid B into the inside of the washing shell (11) through the feeding pipe (13), and filtering the mixed liquid A falling on the bottom of the inner cavity of the washing shell (11) by the filter plate (12) to obtain an organic layer B; S10, when the above operations are performed, unsaturated sodium carbonate and saturated sodium chloride are respectively added into the first annular liquid storage cavity and the second annular liquid storage cavity through the first liquid inlet pipe (24) and the second liquid inlet pipe (25) at the same time, after the filtering of the mixed liquid B is completed, the addition of unsaturated sodium carbonate and saturated sodium chloride is completed. S11, repeat S3-S7 above to produce 7-acetyl-1,1,3,4,4,6-hexamethyltetralin crude product, mix 7-acetyl-1,1,3,4,4,6-hexamethyltetralin crude product with anhydrous ethanol, stand until solid precipitates, then perform suction filtration to produce tonal musk.

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