A racemic catalyst preparation device and method

Abstract

The invention discloses a racemic catalyst preparation device, comprising a fixed outer frame and a reactor, the reactor can be flipped and installed on the fixed outer frame, the reactor comprises a sealing cover and a reaction box, the inner side of the sealing cover is covered with a heating plate, the interior of the reaction box is spherical and bowl-shaped and recessed, the interior of the reaction box is provided with a leak-proof plate, a heating arc plate and a screen plate from the outside to the inside, the leak-proof plate is connected to the inner bottom surface of the reaction box by a plurality of springs, a through cylinder is installed at the bottom center of the screen plate, a driving rod is vertically provided in the reactor, the driving rod is driven to move vertically and rotate axially, a stirring assembly is axially rotatably provided on the outside of the driving rod, the driving rod can respectively drive the stirring assembly and the screen plate to rotate, a liquid outlet pipe is provided at the bottom end of the driving rod, a plurality of drainage ports connected to the liquid outlet pipe are provided on the outer peripheral surface of the bottom end of the driving rod, the bottom center of the leak-proof plate is penetrated by the liquid outlet pipe, and a through outlet is provided at the bottom center of the reaction box.

Description

Technical Field

[0001] The present invention relates to the technical field of catalyst preparation, and in particular to a racemization catalyst preparation device and a method thereof. Background Art

[0002] L-Menthol, also known as L-menthol and natural menthol, is a colorless, needle-shaped crystal with a refreshing minty aroma. It is soluble in organic solvents such as ethanol, acetone, ether, chloroform, and benzene, and slightly soluble in water. It is relatively stable and can evaporate with steam. L-Menthol is mostly produced in the leaves, where it is the main component of peppermint oil. It is a type of cyclic monoterpenoid. It is a highly volatile essential oil produced by plants, primarily composed of hemiterpenes, monoterpenes, and sesquiterpenes, and its production is particularly high in warm climates. Some important plant pigments are terpenoids or compounds containing terpenoid groups.

[0003] L-menthol can be used as a flavoring agent in toothpaste, perfume, beverages, and candies. It is used medicinally as a stimulant, acting on the skin or mucous membranes to provide a cooling and antipruritic effect. It can also be taken internally as a carminative for headaches and inflammation of the nose, throat, and throat. Its esters are used in fragrances and medicines.

[0004] Due to limited natural resources, the quality and quantity of L-menthol extraction are also affected by various factors, which has led to a gradual increase in the cost of naturally extracted L-menthol. With the development of organic synthetic chemistry technology, chemical synthesis of L-menthol has gradually become the mainstream.

[0005] There is a chemical synthesis process for L-menthol: thymol is hydrogenated to DL-menthol, which is then separated by splitting to produce L-menthol. This process produces approximately 50% D-menthol, making its reuse a top priority.

[0006] D-menthol is racemized into DL-menthol under the action of a catalyst, and then L-menthol can be obtained by reusing the splitting process. On the one hand, this increases the production capacity of L-menthol, and on the other hand, it reduces the generation of by-products.

[0007] Currently, there is an urgent need for a D-menthol racemization catalyst with high catalytic activity, simple preparation, long service life, and easy regeneration for industrial synthesis of racemic menthol. Summary of the Invention

[0008] In order to solve the problems mentioned in the above background technology, the present invention provides a D-menthol racemization catalyst with good catalytic performance, simple preparation, stable catalytic performance, high activity, low cost, continuous production and easy regeneration, as well as its preparation equipment and method.

[0009] In order to achieve the above object, the present invention adopts the following technical solutions:

[0010] A racemization catalyst preparation device includes a fixed outer frame and a reactor. The reactor is reversibly mounted within the fixed outer frame. The reactor includes a sealing cover and a reaction box. The inner side of the sealing cover is covered with a heating plate. The interior of the reaction box is concave in the shape of a spherical bowl bottom. The interior of the reaction box is sequentially provided with a leak-proof plate, a heating arc plate, and a sieve plate from the outside to the inside. The leak-proof plate is connected to the inner bottom surface of the reaction box by a plurality of springs. A through-tube is installed at the center of the bottom of the sieve plate.

[0011] The reactor is vertically provided with a driving rod, which can be driven to move vertically and rotate axially. A stirring assembly is axially rotatably provided on the outside of the driving rod. The driving rod can drive the stirring assembly and the filter plate to rotate respectively. A liquid outlet pipe is provided at the bottom end of the driving rod. Several drainage ports connected to the liquid outlet pipe are provided on the outer peripheral surface of the bottom end of the driving rod. The liquid outlet pipe penetrates the center position of the bottom of the leak-proof plate, and a through outlet is provided at the center position of the bottom of the reaction box.

[0012] Preferably, the leakage-proof plate is made of a material that does not allow solids and liquids to pass through, the heating arc plate and the sieve plate are made of a material that only allows liquids to pass through, the upper portion of the heating arc plate is detachably connected to the heating plate, and the heating arc plate is made of a heat-conducting material.

[0013] Preferably, a lifting accessory is installed at the center position of the inner side of the sealing cover, and the stirring assembly includes a lifting ring, an expansion ring, an extension rod and a stirring paddle. The lifting accessory has a matching groove inside to allow the lifting ring to be installed therein, and the lower end of the expansion ring has at least one first docking notch, and a first docking ear is provided at a position on the outer peripheral surface of the drive rod corresponding to the first docking notch.

[0014] Preferably, at least one second docking notch is provided through the opening of the upper end of the cylinder, and a second docking ear is provided at a position on the outer circumference of the lower end of the driving rod corresponding to the second docking notch.

[0015] A method for using a racemization catalyst preparation device comprises the following steps:

[0016] S1: CO(CH3COO)2, Mo(CH3COO)2, and Ba(CH3COO)2 are mixed in a mass ratio of 187:37:1 to form reagent A, and K2CO3 is added to the solvent to form reagent B;

[0017] S2: The reactor is kept in a state where the sealing cover is upward, and the lifting and rotating motor is controlled to lift up so that the first docking ear is placed in the first docking notch. The driving rod drives the stirring assembly to rotate at a stirring speed of 250 to 500 rpm. Reagent A and reagent B are added dropwise to the reaction chamber through the feed port. The heating plate is energized to increase the temperature of the heating arc plate, and the material in the reaction chamber is controlled to maintain at 50°C to 60°C.

[0018] S3: Measure the pH value of the material solution in the reaction chamber with a pH meter. Stop stirring when the material solution satisfies 8 < pH < 9, and keep it still and warm for one hour.

[0019] S4: Control the lifting and rotating motor to lower, so that the driving rod presses down the leak-proof plate, drain the liquid material in the reaction chamber, make the driving rod drive the sieve filter plate to rotate at high speed, and carry out centrifugal dehydration on the solid material on the surface of the sieve filter plate. After the sieve filter plate rotates for 10 minutes, reduce the speed, inject deionized water for washing through the feed port, monitor the conductivity and pH value of the centrifugally drained mother liquor, and stop centrifugation and washing when the pH value is lower than 9 and the conductivity is less than 1000 us / cm.

[0020] S5: Flip the reactor to spread the centrifugally washed material on the heating plate, power on the heating plate, and make the temperature in the reaction chamber reach and remain at 200 °C (±3 °C) for 6 hours of drying.

[0021] S6: Put the catalyst obtained by drying in S5 into a muffle furnace for calcination, raise the temperature from room temperature 25 °C (±10 °C) to 400 °C (±10 °C), and keep it at 425 °C for 2 hours to obtain the finished catalyst.

[0022] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0023] 1. The present invention uses metal oxides to obtain a porous catalyst structure through roasting; the raw materials for preparing the catalyst are easy to obtain, the price is low, and the preparation method is simple; the obtained catalyst is in solid form, which is convenient for the catalyst to be reused, significantly reduces the production cost of L-menthol, and is suitable for industrial production applications.

[0024] 2. The catalyst prepared by the present invention reduces the molar ratio of recycle hydrogen to D-menthol, greatly reduces the generation of by-products such as low-boiling oligomers, improves the life and stability of the catalytic performance of the catalyst, and is suitable for industrial production applications.

[0025] 3. The equipment for preparing the catalyst in the present invention completes the stirring, mixing reaction, dehydration washing and drying of the catalyst in a single reactor. The reactor has a reasonable structure and convenient operation, which is conducive to improving the production efficiency of the catalyst. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0027] Figure 1This is a schematic diagram of the external structure of a racemization catalyst preparation device described in the present invention.

[0028] Figure 2 This is a top view of a racemization catalyst preparation device according to the present invention.

[0029] Figure 3 This is a side sectional view in one direction of a racemization catalyst preparation device according to the present invention when the reactor is upright.

[0030] Figure 4 It is a side sectional view in another direction when the reactor of the racemization catalyst preparation equipment described in the present invention is inverted.

[0031] Figure 5 This is an independent side sectional view of a reactor of a racemization catalyst preparation equipment according to the present invention.

[0032] Figure 6 for Figure 5 Enlarged structural diagram at point A in the middle.

[0033] Figure 7 for Figure 5 Enlarged structural diagram at point B in the middle.

[0034] Figure 8 This is a partial cross-sectional view of the sealing cover of the racemization catalyst preparation equipment described in the present invention.

[0035] Figure 9 This is a schematic structural diagram of a stirring assembly of a racemization catalyst preparation device according to the present invention.

[0036] Figure 10 This is a schematic diagram of the sieve plate structure of a racemization catalyst preparation equipment described in the present invention.

[0037] Figure 11 This is a schematic diagram of the driving rod structure of a racemization catalyst preparation device described in the present invention.

[0038] Figure 12 This is a schematic diagram of the cross-sectional structure of the bottom end of a driving rod of a racemization catalyst preparation device described in the present invention.

[0039] In the figure: 1. Fixed outer frame; 2. Reactor; 201. Reaction chamber; 202. Through outlet; 21. Sealing cover; 2101. Feed port; 2102. Limiting groove; 22. Reaction box; 23. Heating plate; 24. Leak-proof plate; 2401. Docking hole; 25. Spring; 26. Heating arc plate; 27. Screen plate; 28. Through-tube; 2801. Second docking slot; 3. Rotating rod; 4. Control motor; 5. Lifting accessories; 501. Matching slot; 6. Stirring assembly; 601. First docking slot; 61. Lifting ring; 62. Extension ring; 63. Extension rod; 64. Stirring paddle; 7. Driving rod; 701. Discharge port; 71. First docking ear; 72. Second docking ear; 73. Liquid outlet pipe; 8. Lifting and rotating motor; 9. Movable seal; 91. Sealing cover; 92. Hook. DETAILED DESCRIPTION

[0040] To make the objectives, technical solutions, and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings 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 making creative efforts shall fall within the scope of protection of the present invention.

[0041] Reference Figure 1-12 A racemization catalyst preparation device includes a fixed outer frame 1 and a reactor 2. The fixed outer frame 1 is through-hole, and the reactor 2 is mounted inside the fixed outer frame 1 with the aid of rotating rods 3 installed on both sides. A control motor 4 is mounted on the outside of the fixed outer frame 1, which can drive the rotating rods 3 to rotate axially and maintain them in a specified rotational position, thereby controlling the reactor 2 to flip and maintain its position.

[0042] The reactor 2 includes a sealing cover 21 and a reaction box 22. The sealing cover 21 is removably fastened to the reaction box 22 to form a sealed reaction chamber 201 within the reactor 2. The inner side of the sealing cover 21 is covered with a heating plate 23, which is electrically connected to an external control unit. By passing different currents through the heating plate 23, the heating plate 23 can reach any temperature between 50°C and 250°C.

[0043] The reaction box 22 has a spherical, bowl-shaped, recessed interior to accommodate a spherical, bowl-shaped leak-proof plate 24, made of a material impermeable to solids and liquids. Several springs 25 are mounted on the bottom of the reaction box 22. Each spring 25 connects the bottom of the reaction box 22 to the leak-proof plate 24 at its ends, lifting the plate 24 away from the bottom.

[0044] A hanging fitting 5 is mounted at the center of the inner side of the sealing cover 21. A stirring assembly 6 is axially and rotatably mounted on the lower end of the hanging fitting 5. The stirring assembly 6 comprises a hanging ring 61, an expansion ring 62, an extension rod 63, and a stirring paddle 64. A mating groove 501 is defined within the hanging fitting 5 to allow the hanging ring 61 to be inserted therein. The hanging ring 61 is disposed within the mating groove 501 and can rotate axially but cannot move up and down to disengage, thereby allowing the entire stirring assembly 6 to be smoothly mounted on the lower end of the hanging fitting 5.

[0045] The expansion ring 62 extends vertically and has at least one first docking notch 601 at its lower end. The extension rods 63 are symmetrically distributed at the lower end of the expansion ring 62. Each extension rod 63 is externally mounted with a stirring paddle 64. When the stirring assembly 6 rotates axially, the stirring paddles 64 stir the material within the reaction chamber 201.

[0046] A drive rod 7 is mounted within the reaction chamber 201. The drive rod 7 is axially rotatably disposed within the suspension fitting 5 and the stirring assembly 6 and extends downward until it is inserted into a docking hole 2401 formed at the bottom of the leak-proof plate 24. The upper end of the drive rod 7 is connected to a lifting and rotating motor 8 mounted on the exterior of the sealing cover 21. The lifting and rotating motor 8 can be moved toward or away from the sealing cover 21 and can drive the drive rod 7 to axially rotate.

[0047] A first docking ear 71 is provided on the outer surface of the driving rod 7 at a position corresponding to the first docking slot 601. The lifting and rotating motor 8 drives the driving rod 7 to move to a position where the first docking ear 71 is inserted into the first docking slot 601. At this time, the axially rotating driving rod 7 can drive the stirring assembly 6 to rotate synchronously, thereby achieving stirring of the material in the reaction chamber 201.

[0048] A heating arc plate 26 is installed within the leak-proof plate 24. The upper portion of the heating arc plate 26 is removably connected to the heating plate 23. The heating arc plate 26 is made of a heat-conducting material that only allows the passage of liquids. When the heating arc plate 26 is connected to the heating plate 23, heat emitted by the heating plate 23 is rapidly transferred to the heating arc plate 26, thereby raising the temperature of the heating arc plate 26. As the materials in the reaction chamber 201 undergo a stirring reaction, the heating plate 23 utilizes heat transfer from the heating arc plate 26 to continuously heat the materials, ensuring that the materials react at the appropriate temperature.

[0049] The upper surface of the heating arc plate 26 is detachably covered with a sieve plate 27, which is made of a material that only allows liquid to pass through. A through-tube 28 is installed at the center of the bottom of the sieve plate 27, and the through-tube 28 just allows the drive rod 7 to be inserted therein. The upper end opening of the through-tube 28 is provided with at least one second docking slot 2801, and the outer peripheral surface of the lower end of the drive rod 7 is provided with a second docking ear 72 at a position corresponding to the second docking slot 2801. When the lifting and rotating motor 8 drives the drive rod 7 to move to the position where the second docking ear 72 is placed in the second docking slot 2801, the axially rotating drive rod 7 can drive the through-tube 28 to rotate synchronously, thereby driving the entire sieve plate 27 to rotate axially, thereby realizing centrifugal treatment of the material on the surface of the sieve plate 27.

[0050] It is worth mentioning that the vertical distance between the first docking ear 71 and the second docking ear 72 is smaller than the vertical distance from the first docking slot 601 to the second docking slot 2801, so that the first docking ear 71 and the second docking ear 72 cannot be placed in the first docking slot 601 and the second docking slot 2801 respectively at the same time, thereby avoiding the simultaneous rotation of the sieve plate 27 and the stirring assembly 6 and interference with each other.

[0051] The bottom end of the drive rod 7 is provided with a liquid outlet pipe 73, which has a smaller diameter than the drive rod 7. The liquid outlet pipe 73 penetrates the center of the bottom of the leak-proof plate 24. As the drive rod 7 moves downward, the second docking lug 72 is positioned within the second docking notch 2801, simultaneously pressing the leak-proof plate 24 downward. The heating arc plate 26 connected to the heating plate 23 remains in its original vertical position along with the sieve plate 27. When the leak-proof plate 24 descends, a gap is created between the heating arc plate 26 and the heating arc plate 26. Some liquid within the reaction chamber 201 will permeate the sieve plate 27 and heating arc plate 26 and enter the gap.

[0052] The outer circumferential surface at the bottom end of the drive rod 7 is provided with a plurality of drainage ports 701, which are connected to the liquid outlet pipe 73. The portion of the drive rod 7 with the drainage ports 701 is normally enclosed by the through-tube 28. However, when the drive rod 7 presses down on the leak-proof plate 24, the drainage ports 701 move downward, away from the through-tube 28, and into the gap between the leak-proof plate 24 and the heating arc plate 26. A through-port 202 is provided at the center of the bottom of the reaction box 22. When the drive rod 7 moves downward, the liquid outlet pipe 73 is inserted into the through-port 202. Liquid in the gap between the leak-proof plate 24 and the heating arc plate 26 can flow through the drainage ports 701 into the liquid outlet pipe 73 and ultimately out through the through-port 202. After all the liquid in the reaction chamber 201 has flowed out, any water-containing solids will adhere to the sieve plate 27. At this point, the drive rod 7 drives the sieve plate 27 to rotate at high speed, further centrifugally dehydrating the solids adhered to the sieve plate 27. After centrifugal dehydration, the control motor 4 can control the reactor 2 to flip as a whole, and the dehydrated solid material on the screen plate 27 will fall onto the heating plate 23. At this time, the heating plate 23 can be heated to 200°C to dry the material, and the water vapor dried out will escape and be discharged through the outlet 202.

[0053] The sealing cover 21 is provided with two feed ports 2101, through which the raw materials are added into the reaction chamber 201. A limiting groove 2102 is provided on the inner wall of the feed port 2101, and a movable plug 9 is provided upside down below the feed port 2101 with the aid of the limiting groove 2102. The movable plug 9 includes a cover 91 and a hook 92, wherein the upper end of the hook 92 is hung in the limiting groove 2102 and the lower end is connected to the cover 91, so that the cover 91 can move vertically within the range limited by the limiting groove 2102. After the reactor 2 is turned over, the cover 91 can block the feed port 2101 to prevent the material from leaking.

[0054] A pH meter and a thermometer are also inserted into the reaction chamber 201 to monitor the physical and chemical indicators of the material in the reaction chamber 201 .

[0055] Example 1:

[0056] A method for preparing a racemization catalyst using a racemization catalyst preparation device comprises the following steps:

[0057] S1: CO(CH3COO)2, Mo(CH3COO)2, and Ba(CH3COO)2 are mixed in a mass ratio of 187:37:1 to form reagent A, and K2CO3 is added to the solvent to form reagent B;

[0058] S2: Keep the reactor 2 in the state with the sealing cover 21 facing upward, control the lifting and rotating motor 8 to lift so that the first docking ear 71 is placed into the first docking notch 601, make the driving rod 7 drive the stirring component 6 to rotate at a stirring speed of 250 - 500 revolutions per minute, drip reagent A and reagent B into the reaction chamber 201 through the feed port 2101, energize the heating plate 23 to heat up the heating arc plate 26, and control the material in the reaction chamber 201 to be maintained at 50°C - 60°C;

[0059] S3: Measure the pH value of the material solution in the reaction chamber 201 with a pH meter. When the material solution satisfies 8 < pH < 9, stop stirring and keep it warm for one hour;

[0060] S4: Control the lifting and rotating motor 8 to lower so that the driving rod 7 presses down the leak - proof plate 24, discharge the liquid material in the reaction chamber 201, make the driving rod 7 drive the sieve filter plate 27 to rotate at a high speed, perform centrifugal dehydration on the solid material on the surface of the sieve filter plate 27. After the sieve filter plate 27 rotates for 10 minutes, reduce the speed and inject deionized water for washing through the feed port 2101, monitor the conductivity and pH value of the centrifugally discharged mother liquor, and stop centrifuging and washing when the pH value is lower than 9 and the conductivity is less than 1000 us / cm;

[0061] S5: Flip the reactor 2 to spread the centrifugally washed material on the heating plate 23, energize the heating plate 23, make the temperature in the reaction chamber 201 reach and be maintained at 200°C (±3°C), and dry for 6 hours;

[0062] S6: Put the catalyst obtained by drying in S5 into a muffle furnace for calcination, raise the temperature from room temperature 25°C (±10°C) to 400°C (±10°C), and keep it at 425°C for 2 hours to obtain the finished catalyst product.

[0063] Example 2:

[0064] A method for preparing a racemization catalyst by a racemization catalyst preparation device, the difference from Example 1 is only that in S6, the catalyst in the muffle furnace is first calcined at 条件下焙烧2h,再450℃煅烧,得到催化剂成品。 [[ID=二十]]

[0065] Example 3:

[0066] A method for preparing a racemization catalyst by a racemization catalyst preparation device, the difference from Example 2 is only that in S6, the catalyst in the muffle furnace is calcined at 450°C for 2h to obtain the finished catalyst product.

[0067] It should be noted that there is an unclear part in the original text of "再450℃煅烧,得到催化剂成品。" in Example 2, which may need to be further clarified for a more accurate translation. I have translated it as best as possible according to the context. Also, in the translation of Example 2, there is an unclear part in the original text "在S6中马弗炉内的催化剂先在425℃条件下焙烧2h,再450℃煅烧,得到催化剂成品。" which should be more clearly expressed in the original Chinese for a more accurate translation. Here, I translated it based on the overall understanding, but there may be some inaccuracies due to the unclear expression in the original.800g of the finished catalyst prepared by the aforementioned method was sieved into 3mm-long particles and then loaded into the constant temperature section of a fixed-bed reactor. A hydrogen atmosphere was introduced, and the reaction system was heated to 200-230°C. D-menthol was then introduced into the reaction system using a mass pump. The catalytic reaction was carried out at a reaction pressure of 8 MPa. The crude reaction product flowed through a pipeline into a gas-liquid separator for gas-liquid separation. The liquid was collected from the lower end of the separator. After two hours of continuous reaction, samples were collected and analyzed by gas chromatography and polarimetry. The menthane content and specific rotation of the reaction solution (a key indicator of successful racemization) are listed in Table 1.

[0068] Example Catalyst No. catalyst Menthane content (%) Specific rotation of reaction solution (°) 1 CAT-1 Calcination at 425℃ 20.53 2.3 2 CAT-2 Calcination at 425℃ + 450℃ 2.06 1.6 3 CAT-3 450℃ 0.51 0.68

[0069] Table 1

[0070] As shown in Table 1, the catalysts prepared in Examples 1-3 of the present invention can effectively catalyze the racemization of D-menthol.

[0071] 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 to 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, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0072] In the present invention, unless otherwise expressly specified or limited, terms such as "disposed," "installed," "connected," "connected," and "fixed" should be understood in a broad sense. For example, they may refer to fixed connections, detachable connections, or integration; they may refer to mechanical connections, direct connections, or indirect connections through an intermediate medium; they may refer to internal communication between two elements or interaction between two elements. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0073] 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 a person skilled in the art. The provision of power is also common knowledge in the art. The present invention is mainly used to protect mechanical devices, so the control method and circuit connection are not explained in detail in the present invention.

[0074] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A racemization catalyst preparation device, comprising a fixed outer frame (1) and a reactor (2), characterized in that: The reactor (2) is reversibly mounted in a fixed outer frame (1). The reactor (2) comprises a sealing cover (21) and a reaction box (22). The inner side of the sealing cover (21) is covered with a heating plate (23). The interior of the reaction box (22) is concave in the shape of a spherical bowl bottom. The interior of the reaction box (22) is provided with a leak-proof plate (24), a heating arc plate (26) and a sieve plate (27) in sequence from the outside to the inside. The leak-proof plate (24) is connected to the inner bottom surface of the reaction box (22) by a plurality of springs (25). A through-tube (28) is installed at the center of the bottom of the sieve plate (27). The reactor (2) is vertically provided with a driving rod (7), and the driving rod (7) is driven to move vertically and rotate axially. A stirring assembly (6) is axially rotatably provided on the outside of the driving rod (7), and the driving rod (7) can respectively drive the stirring assembly (6) and the screen plate (27) to rotate. A liquid outlet pipe (73) is provided at the bottom end of the driving rod (7), and a plurality of liquid discharge ports (701) connected to the liquid outlet pipe (73) are provided on the outer peripheral surface of the bottom end of the driving rod (7). The liquid outlet pipe (73) penetrates the center position of the bottom of the leak-proof plate (24), and a through outlet (202) is provided at the center position of the bottom of the reaction box (22).

2. The racemization catalyst preparation device according to claim 1, characterized in that: The anti-leakage plate (24) is made of a material that does not allow solids and liquids to pass through, the heating arc plate (26) and the sieve plate (27) are made of a material that only allows liquids to pass through, the upper part of the heating arc plate (26) is detachably connected to the heating plate (23), and the heating arc plate (26) is made of a heat-conducting material.

3. The racemization catalyst preparation device according to claim 1, characterized in that: A hanging accessory (5) is installed at the center position of the inner side of the sealing cover (21), and the stirring assembly (6) includes a hanging ring (61), an expansion ring (62), an extension rod (63) and a stirring paddle (64). The hanging accessory (5) has a matching groove (501) inside to allow the hanging ring (61) to be installed therein, and the lower end opening of the expansion ring (62) has at least one first docking notch (601), and a first docking ear (71) is provided at a position on the outer peripheral surface of the driving rod (7) corresponding to the first docking notch (601).

4. The racemization catalyst preparation device according to claim 1, characterized in that: The upper opening of the through-tube (28) is provided with at least one second docking notch (2801), and the outer peripheral surface of the lower end of the driving rod (7) is provided with a second docking ear (72) at a position corresponding to the second docking notch (2801).

5. The method for using the racemization catalyst preparation device according to any one of claims 1 to 4, characterized in that: The following steps are involved: S1: CO(CH3COO)2, Mo(CH3COO)2, and Ba(CH3COO)2 are mixed in a mass ratio of 187:37:1 to form reagent A, and K2CO3 is added to the solvent to form reagent B; S2: The reactor (2) is kept in a state where the sealing cover (21) is upward, the driving rod (7) drives the stirring assembly (6) to rotate at a stirring speed of 250 to 500 rpm, reagents A and B are added dropwise to the reactor (2), and the heating plate (23) is energized to increase the temperature of the heating arc plate (26), and the material in the reaction chamber (201) is controlled to be maintained at 50°C to 60°C; S3: Measure the pH value of the material solution in the reactor (2) with a pH meter. Stop stirring when the material solution satisfies 8 < pH < 9, and keep it static and warm for one hour. S4: Control the driving rod (7) to press down the leak-proof plate (24) to discharge the liquid material in the reactor (2). The driving rod (7) drives the sieve filter plate (27) to rotate at a high speed to centrifugally dehydrate the solid material on the surface of the sieve filter plate (27). After the sieve filter plate (27) rotates for 10 minutes, reduce the rotation speed and inject deionized water for washing. Monitor the conductivity and pH value of the centrifugally discharged mother liquor. Stop centrifugation and washing when the pH value is lower than 9 and the conductivity is less than 1000 us / cm. S5: Flip the reactor (2) to spread the centrifugally washed material on the heating plate (23). Apply power to the heating plate (23) to make the temperature in the reactor (2) reach and remain at 200 °C (±3 °C) for 6 hours of drying. S6: Put the catalyst obtained by drying in S5 into a muffle furnace for calcination. Raise the temperature from room temperature 25 °C (±10 °C) to 400 °C (±10 °C), and maintain it at 425 °C for 2 hours to obtain the finished catalyst product.

6. The method for using the racemization catalyst preparation device according to claim 5, characterized in that: In S6, the catalyst in the muffle furnace is first calcined at 425 °C for 2 h, and then calcined at 450 °C to obtain the finished catalyst product.

7. The method for using the racemization catalyst preparation device according to claim 5, characterized in that: In S6, the catalyst in the muffle furnace is calcined at 450 °C for 2 h to obtain the finished catalyst product.

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