A high-purity galaxolone refining device and method

Abstract

The invention discloses a high-purity galaxolone refining device and method. The refining device comprises a main tank body, a blocking component and a filter press component. Both the blocking component and the filter press component are installed in the main tank body. The interior of the main tank body is divided into a mixing chamber, a guide chamber and a filter press chamber from top to bottom in sequence. A blocking component is installed at the junction of the mixing chamber and the guide chamber. The blocking component comprises a lifting seat and a plurality of stacking plates. The lifting seat can be moved vertically up and down. A plurality of stacking plates are installed around the outer periphery of the lifting seat to form an annular cover plate. The filter press chamber is sealed by a sealing cover and an opening and closing plate. The filter press component is installed in the filter press chamber. The filter press component comprises an extrusion piece and a filter press plate. The extrusion piece can push the filter press plate to one side of the filter press chamber. The galaxolone stock solution is dissolved in a solvent. The galaxolone is purified by a method of heating dissolution and cooling crystallization. The crystals are then filter-pressed and dried. The invention is suitable for industrial large-scale preparation of high-purity galaxolone finished products.

Description

Technical Field

[0001] The invention relates to the technical field of galaxolide production and processing, and in particular to a method for refining high-purity galaxolide. Background Art

[0002] Musk fragrance has a high aroma value. Natural musk has been cherished since ancient times as a precious spice and medicinal material. Synthetic musk, as a substitute for natural musk, has been widely used in the formulation of various flavors. IFF's chemists were the first to successfully synthesize galaxolide. Galaxolide has a strong aroma, good stability, is not absorbed by the human body, can even be taken orally, and is low in price, so it is deeply loved by perfumers.

[0003] At present, the industrial synthesis of galaxol generally adopts a three-step process. First, α-methylstyrene and isopentene are reacted under acidic catalytic conditions to generate pentamethylindane; then, pentamethylindane and propylene oxide are condensed under AlCl3 catalysis to generate hexamethylindanol; finally, hexamethylindanol is condensed with formaldehyde under acidic catalyst to perform cyclization reaction to obtain galaxol. The galaxol produced by this process will produce isomers at the same time, with similar structures and boiling points. It is difficult to obtain high-purity galaxol with existing distillation equipment. Summary of the invention

[0004] Aiming at the problem that a large amount of galaxolone isomers are produced in the existing production process, the separation degree of equipment is poor in the distillation process, and high-purity galaxolone cannot be produced on a large scale, the present invention proposes a method for refining high-purity galaxolone, and the GC purity of galaxolone can reach more than 95%.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] A high-purity galaxolone refining device comprises a main tank body, a blocking component and a filter press component, wherein the blocking component and the filter press component are both installed in the main tank body, the interior of the main tank body is sequentially divided into a mixing chamber, a guide chamber and a filter press chamber from top to bottom, a blocking component is installed at the junction of the mixing chamber and the guide chamber, the blocking component comprises a lifting seat and a plurality of stacking plates, the lifting seat can be moved vertically up and down, and a plurality of stacking plates are installed around the outer periphery of the lifting seat to form a circular ring cover plate;

[0007] The filter press chamber is sealed by a sealing cover and an opening and closing plate. The filter press assembly is installed in the filter press chamber. The filter press assembly includes an extrusion piece and a filter press plate. The extrusion piece can push the filter press plate to one side of the filter press chamber.

[0008] Preferably, the mixing chamber is a cylindrical cavity, a stirring device is installed inside the mixing chamber, and a circulating heat exchange chamber is provided on the side wall of the mixing chamber.

[0009] Preferably, a control device is fixedly installed in the guide cavity, the control device comprises a fixed platform, a control motor and a hydraulic rod, the fixed platform is fixedly installed in the guide cavity, and there is a certain distance between the fixed platform and the inner wall of the guide cavity.

[0010] Preferably, the lifting seat includes a connecting seat, a surrounding seat, a top cover and a clamping ring. The connecting seat is fixedly installed on the upper end of the hydraulic rod, the surrounding seat can be movably surrounded by the outside of the connecting seat, the top cover is installed above the connecting seat and connected to the surrounding seat, and the clamping ring is surrounded and arranged outside the surrounding seat, and the clamping ring is connected to the surrounding seat through a connecting ring sheet.

[0011] Preferably, the stacking plate includes a main plate and a connecting buckle, one side of the main plate has a stacking groove, the connecting buckle has a round groove and an insertion groove, the round groove can be wrapped around the outside of the clamping ring, and the width of the insertion groove is greater than the thickness of the connecting ring piece.

[0012] Preferably, when the lifting seat is lowered to the lowest point, the stacking plate is placed horizontally on the fixed table, and a sealing plate is also installed on the upper end of the connecting seat. When the lifting seat is lowered to the lowest point, the outer edge of the sealing plate is tightly fitted with the inner side of each main plate.

[0013] Preferably, the filter press plate is liquid permeable.

[0014] A method for refining high-purity galaxolide comprises the following steps:

[0015] S1: The crude galaxolide product is subjected to refined galaxolide distillation to obtain a galaxolide stock solution, the galaxolide stock solution is injected into a mixing chamber, and a solvent selected from any one or a combination of two of n-heptane, n-hexane, petroleum ether, ethyl acetate, dichloromethane, and butyl acetate is added, wherein the added volume of the solvent is 1-10 times the volume of the galaxolide stock solution;

[0016] S2: raising the temperature of the galaxolide stock solution to 50° C., and stirring the galaxolide stock solution and the solvent to form a uniform phase;

[0017] S3: cooling the galaxolide mixed solution, keeping it at -5~5°C and stirring it for crystallization for 1-10 hours to generate a large amount of solid;

[0018] S4: The stirred mixture is discharged into a filter press chamber, and the filter press assembly separates the mixture into solid and liquid phases and discharges them separately, wherein the solid phase is a high-purity pure product of galaxolone.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] 1. The present invention dissolves the galaxolide stock solution in a solvent, purifies the galaxolide by heating dissolution and cooling crystallization, and then performs filter pressing and drying on the crystals. The method is easy to operate, has low equipment requirements, and is suitable for industrial large-scale preparation of high-purity galaxolide finished products.

[0021] 2. The present invention integrates the dissolution, crystallization and filtration of galaxolide in the same device for processing, and the refining process is centralized and continuous, with high production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0023] Figure 1 It is a schematic overall cross-sectional view of a high-purity galaxolone refining device according to the present invention;

[0024] Figure 2 for Figure 1 Enlarged view of point A in the middle;

[0025] Figure 3 It is a schematic diagram of the structure of the lifting seat part of the present invention;

[0026] Figure 4 This is a schematic diagram of the sealing disc and connecting seat structure of the present invention;

[0027] Figure 5 It is a schematic diagram of the structure of the multiple stacked plate circles after being spread out according to the present invention;

[0028] Figure 6 for Figure 5 Enlarged view of point B in the middle;

[0029] Figure 7 This is a schematic diagram of the structure of a single stacked plate according to the present invention.

[0030] In the figure: 1. main tank body; 101. mixing chamber; 102. guiding chamber; 103. filter press chamber; 104. circulating heat exchange chamber; 105. drain port; 2. blocking assembly; 21. lifting seat; 211. connecting seat; 212. surrounding seat; 213. top cover; 214. snap ring; 215. connecting ring piece; 216. sealing disk; 22. stacking plate; 2201. stacking groove; 2202. round bag groove; 2203. insertion groove; 221. main plate; 222. connecting buckle; 3. filter press assembly; 31. extrusion piece; 32. filter press plate; 4. stirring device; 5. control device; 51. fixing table; 52. control motor; 53. hydraulic rod; 6. sealing ring; 7. sealing cover; 8. partition; 9. opening and closing plate. DETAILED DESCRIPTION

[0031] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are 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.

[0032] Reference Figure 1-7 A high-purity galaxolone refining device comprises a main tank body 1, a blocking component 2 and a filter press component 3, wherein the blocking component 2 and the filter press component 3 are both installed in the main tank body 1.

[0033] The main tank body 1 is hollow inside, and is divided into a mixing chamber 101, a guide chamber 102 and a filter press chamber 103 from top to bottom. The mixing chamber 101 is a cylindrical cavity, and a stirring device 4 is installed inside the mixing chamber 101. The side wall of the mixing chamber 101 has a circulating heat exchange chamber 104. The galaxol concentrate and the diluent can be injected into the mixing chamber 101 and stirred and mixed by the stirring device 4. While the feed liquid is being mixed, heat exchange liquid of different temperatures can be circulated into the circulating heat exchange chamber 104 to change the temperature of the feed liquid in the mixing chamber 101.

[0034] A control device 5 is fixedly installed in the guide chamber 102, and the control device 5 includes a fixed platform 51, a control motor 52 and two hydraulic rods 53. The fixed platform 51 is fixedly installed in the guide chamber 102, and there is a certain distance between the fixed platform 51 and the inner wall of the guide chamber 102 to allow the liquid in the mixing chamber 101 to flow down into the guide chamber 102. The control motor 52 is installed inside the fixed platform 51, and the two hydraulic rods 53 are respectively installed at the upper and lower ends of the control motor 52. The hydraulic rods 53 extend outside the fixed platform 51, and the control motor 52 can drive each hydraulic rod 53 to independently extend and retract.

[0035] The blocking assembly 2 includes a lifting seat 21 and a plurality of stacking plates 22. The lifting seat 21 is fixedly mounted on the upper end of the hydraulic rod 53. A plurality of stacking plates 22 are mounted around the outer periphery of the lifting seat 21. The stacking plates 22 surround the outside of the lifting seat 21 in a circumference to form an annular cover plate. The outer portion of the annular cover plate formed by the stacking plates 22 is in close contact with the inner wall of the mixing chamber 101 to block the mixing chamber 101 from the guiding chamber 102, so that the liquid in the mixing chamber 101 cannot enter the guiding chamber 102.

[0036] The lifting seat 21 includes a connecting seat 211, a surrounding seat 212, a top cover 213 and a clamping ring 214. The connecting seat 211 is fixedly mounted on the upper end of the hydraulic rod 53. The connecting seat 211 is lifted and lowered as the hydraulic rod 53 is extended and retracted. The surrounding seat 212 is movably surrounded by the outside of the connecting seat 211. The top cover 213 is mounted above the connecting seat 211 and connected to the surrounding seat 212. After the hydraulic rod 53 is extended, the connecting seat 211 can be lifted up. After the connecting seat 211 is lifted up, the top cover 213 and the surrounding seat 212 can be pulled up together. The clamping ring 214 is arranged to surround the outside of the surrounding seat 212, and the clamping ring 214 is connected to the surrounding seat 212 through a connecting ring sheet 215.

[0037] The stacking plate 22 includes a main plate 221 and a connecting buckle 222. One side of the main plate 221 has a stacking groove 2201. The stacking groove 2201 is in the shape of a right-angled trapezoid. The right-angle side of the stacking groove 2201 extends to one side of the main plate 221, and the depth of the stacking groove 2201 gradually increases from the short bottom side to the long bottom side. The length of the long bottom side of the stacking groove 2201 is less than the length of the bottom surface of the main plate 221, and the free space is used to install the connecting buckle 222.

[0038] The connecting buckle 222 has a round groove 2202 and an insertion groove 2203. The round groove 2202 can be wrapped around the outside of the snap ring 214. The insertion groove 2203 is arranged on the side of the connecting buckle 222 away from the main plate 221. The width of the insertion groove 2203 is greater than the thickness of the connecting ring piece 215, so as to allow the connecting buckle 222 to swing and rotate to a certain extent after being snap-fitted on the outside of the snap ring 214.

[0039] When the connecting buckle 222 is installed outside the clamping ring 214, the main plate 221 is in an inclined state, and a plurality of the main plates 221 are stacked and tilted to surround the outside of the lifting seat 21 to form a circular cover.

[0040] It can be understood that, when one of the main plates 221 is set, it is placed in the stacking groove 2201 of a main plate 221 adjacent to it, and another main plate 221 adjacent to it is set in the stacking groove 2201 of this main plate 221. The stacking groove 2201 can make the stacked main plates 221 on the same horizontal plane, ensuring the integrity of the circular cover plate formed by the stacked main plates 221; the upper surface of each main plate 221 is tightly attached to the bottom surface of the stacking groove 2201, ensuring the sealing of the circular cover plate formed by the stacked main plates 221.

[0041] When the lifting seat 21 is lowered to the lowest position, the stacking plate 22 is placed horizontally on the fixed platform 51. A sealing disk 216 is also installed on the upper end of the connecting seat 211. When the lifting seat 21 is lowered to the lowest position, the outer edge of the sealing disk 216 is tightly fitted with the inner side of each main plate 221 to prevent the liquid from flowing down from the gaps of each connecting buckle 222. The inner wall of the mixing chamber 101 is also provided with a sealing ring 6 that can be tightly fitted with the outer edge of each stacking plate 22 after the stacking plate 22 is placed horizontally. The sealing ring 6 and the sealing disk 216 can further fit and seal the inner ring and outer ring of the circular cover formed by the stacking plates 22, so that the liquid can be stored intact in the mixing chamber 101 when the stacking plates 22 are placed horizontally.

[0042] After the liquid feed is stirred and solids are precipitated in the mixing chamber 101, the lifting seat 21 can be lifted to pull up the end of the stacking plate 22 close to the lifting seat 21, and the main plates 221 originally stacked horizontally around will be tilted to form a truncated cone. The edge of the stacking plate 22 that was originally tightly attached to the inner wall of the mixing chamber 101 will have a gap with the inner wall of the mixing chamber 101 due to the tilt of the stacking plate 22, and the liquid feed will be guided by the tilted stacking plate 22 to flow into the guide chamber 102.

[0043] It is worth mentioning that the stacking groove 2201 leaves gaps between each tightly stacked stacking plate 22, so that the stacking plates 22 can be tilted smoothly, avoiding the stacking plates 22 from being squeezed against each other and getting stuck when tilting.

[0044] The lower end of the guide chamber 102 is connected to the filter press chamber 103, and the feed liquid flowing into the guide chamber 102 will eventually enter the filter press chamber 103. A sealing cover 7 is provided under the fixed platform 51, and the hydraulic rod 53 is connected to the sealing cover 7. The shape of the sealing cover 7 corresponds to the upper end opening of the filter press chamber 103. After the feed liquid is injected into the filter press chamber 103, the hydraulic rod 53 can be extended so that the sealing cover 7 covers the sealed filter press chamber 103.

[0045] A partition 8 is provided in the filter press chamber 103, and a filter press assembly 3 is provided on each side of the partition 8. The filter press assembly 3 includes an extrusion member 31 and a filter press plate 32. The extrusion member 31 can push the filter press plate 32 toward the partition 8. The filter press plate 32 is provided parallel to the partition 8, and the upper end of the filter press plate 32 can be in close contact with the sealing cover 7. The filter press plate 32 allows liquid to pass through, while the partition 8 does not allow liquid and solid to pass through. Before the feed liquid is injected into the filter press chamber 103, the filter press plate 32 is in close contact with the side wall of the filter press chamber 103. After the feed liquid is injected into the filter press chamber 103, the filter press plate 32 gradually moves toward the partition 8. The liquid substance will pass through the filter press plate 32 and remain on the side of the filter press plate 32 facing the side wall of the filter press chamber 103, while the solid substance will remain on the side of the filter press plate 32 facing the partition 8.

[0046] The lower end of the filter press chamber 103 is sealed by an opening and closing plate 9, and a drain port 105 is provided near the side wall of the lower part of the filter press chamber 103. After solid-liquid separation, the liquid part of the feed liquid is first discharged through the drain port 105, and then the opening and closing plate 9 is opened to discharge the residual solid in the filter press chamber 103.

[0047] The present invention also provides a method for refining high-purity galaxolide, comprising the following steps:

[0048] S1: The galaxol crude product is refined and distilled to obtain a galaxol stock solution, the galaxol stock solution is injected into the mixing chamber 101, and a solvent composed of any one or a combination of two of n-heptane, n-hexane, petroleum ether, ethyl acetate, dichloromethane, and butyl acetate is added, and the added volume of the solvent is 1-10 times the volume of the galaxol stock solution;

[0049] S2: Inject circulating hot water into the circulating heat exchange chamber 104 to raise the temperature of the galaxolide stock solution to 50° C., and start the stirring device 4 to stir the galaxolide stock solution and the solvent into a uniform phase;

[0050] S3: injecting circulating cooling water into the circulating heat exchange chamber 104 to cool the galaxolide mixed solution, and stirring and crystallizing at -5~5°C for 1-10 hours to generate a large amount of solids;

[0051] S4: the stirred mixture is discharged into the filter press chamber 103, and the filter press assembly 3 separates the mixture into solid and liquid phases and discharges them separately, wherein the solid phase is a high-purity pure galaxolide.

[0052] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0053] In the present invention, unless otherwise clearly specified and limited, the terms "set", "install", "connect", "connect", "fix" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral one; it can be a mechanical connection, a direct connection, or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0054] The control method of the present invention is automatic control through a controller. The control circuit of the controller can be implemented by simple programming by technicians in this field. The provision of power is also common knowledge in this field. The present invention is mainly used to protect mechanical devices, so the present invention will no longer explain the control method and circuit connection in detail.

[0055] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A high-purity galaxolone refining device, comprising a main tank body (1), a barrier assembly (2) and a filter press assembly (3), wherein the barrier assembly (2) and the filter press assembly (3) are both installed in the main tank body (1), characterized in that: The interior of the main tank body (1) is divided into a mixing chamber (101), a guide chamber (102) and a filter press chamber (103) in order from top to bottom; a blocking component (2) is installed at the junction of the mixing chamber (101) and the guide chamber (102); the blocking component (2) comprises a lifting seat (21) and a plurality of stacking plates (22); the lifting seat (21) can move vertically up and down; a plurality of stacking plates (22) are installed around the outer periphery of the lifting seat (21) to form a circular cover plate; the outer portion of the circular cover plate formed by the stacking plates (22) is in close contact with the inner wall of the mixing chamber (101); A control device (5) is fixedly installed in the guide cavity (102), the control device (5) comprising a fixed platform (51), a control motor (52) and a hydraulic rod (53), the fixed platform (51) is fixedly installed in the guide cavity (102), and a certain distance exists between the fixed platform (51) and the inner wall of the guide cavity (102); The lifting seat (21) comprises a connecting seat (211), an enclosing seat (212), a top cover (213) and a clamping ring (214); the connecting seat (211) is fixedly mounted on the upper end of the hydraulic rod (53); the enclosing seat (212) is movably enclosed outside the connecting seat (211); the top cover (213) is mounted above the connecting seat (211) and is connected to the enclosing seat (212); the clamping ring (214) is enclosed outside the enclosing seat (212); and the clamping ring (214) is connected to the enclosing seat (212) via a connecting ring sheet (215); The stacking plate (22) comprises a main plate (221) and a connecting buckle (222); one side of the main plate (221) has a stacking groove (2201); the connecting buckle (222) has a round groove (2202) and an insertion groove (2203); the round groove (2202) can be wrapped around the outside of the clamping ring (214); the width of the insertion groove (2203) is greater than the thickness of the connecting ring (215); When the lifting seat (21) is lowered to the lowest position, the stacking plate (22) is placed horizontally on the fixed platform (51), and a sealing plate (216) is installed on the upper end of the connecting seat (211). When the lifting seat (21) is lowered to the lowest position, the outer edge of the sealing plate (216) is tightly fitted with the inner side of each main plate (221). The lifting seat (21) can be lifted to pull up one end of the stacking plate (22) close to the lifting seat (21), and the main plates (221) originally stacked horizontally around each other will be tilted to form a circular table; The filter press chamber (103) is sealed by means of a sealing cover (7) and an opening and closing plate (9); the filter press assembly (3) is installed in the filter press chamber (103); the filter press assembly (3) comprises an extrusion member (31) and a filter press plate (32); the extrusion member (31) can push the filter press plate (32) toward one side of the filter press chamber (103).

2. A high-purity galaxolide refining device according to claim 1, characterized in that: The mixing chamber (101) is a cylindrical cavity, a stirring device (4) is installed inside the mixing chamber (101), and a circulating heat exchange chamber (104) is provided on the side wall of the mixing chamber (101).

3. A high-purity galaxolide refining device according to claim 1, characterized in that: The filter press plate (32) allows liquid to permeate.

4. A refining method of a high-purity galaxolide refining device according to any one of claims 1 to 3, characterized in that: The following steps are involved: S1: The crude galaxolide product is subjected to refined galaxolide distillation to obtain a galaxolide stock solution, the galaxolide stock solution is injected into a mixing chamber (101), and a solvent selected from any one of n-heptane, n-hexane, petroleum ether, ethyl acetate, dichloromethane, and butyl acetate or a combination of two thereof is added, wherein the added volume of the solvent is 1 to 10 times the volume of the galaxolide stock solution; S2: raising the temperature of the galaxolide stock solution to 50° C., and stirring the galaxolide stock solution and the solvent to form a uniform phase; S3: cooling the galaxolide mixed solution, keeping it at -5-5°C with stirring for crystallization for 1-10 hours, and generating a large amount of solid; S4: the stirred mixture is discharged into the filter press chamber (103), and the filter press component (3) separates the mixture into solid and liquid phases and discharges them separately, wherein the solid phase is a high-purity pure galaxolone product.

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