Recrystallization device for synthesizing hydroxyl pinacolone retinoate

Abstract

The utility model discloses a recrystallization device for synthesizing hydroxyl pinacolone retinoate, which is characterized in that a filter base, a conical filter plate of the filter base and an annular scraper are arranged at the bottom of a kettle body, so that the filter efficiency is improved, and the yield is increased; the discharging device is matched with the filtering base, and the discharging device and the filtering base are matched for use, so that the efficiency can be improved while the yield is improved, and the operation is simple.

Description

TECHNICAL FIELD

[0001] The utility model relates to synthetic device technical field, concretely is a kind of for hydroxyl pinacolone retinol synthesis's recrystallization device. BACKGROUND

[0002] Hydroxyl pinacolone retinol, it belongs to vitamin A ester derivative, is a new generation of esterification of retinoic acid, unlike other retinoic acid derivatives, it can directly produce effect without conversion, and principle is similar to all-trans A acid.Compared with retinoic acid, the irritability of hydroxyl pinacolone retinol is reduced a lot, and it is more safe to use around eye, and transdermal rate is more excellent.

[0003] For the synthesis of hydroxyl pinacolone retinol, raw material is acylated, esterified, and crude product is obtained, and finished product is obtained by refining crystallization.The specific steps of refining crystallization are that crude product is added to recrystallization solvent, and then cooling crystallization is carried out to obtain final product.In the synthesis of hydroxyl pinacolone retinol, the utilization rate of the used equipment is high, material transfer is reduced, the purity of product has great influence, and excellent basic production conditions are provided for large-scale industrial production.

[0004] Recrystallization is the process of dissolving crystal in solvent or melting, and then crystallizing from solution or melt again.Recrystallization can purify impure substances or separate substances mixed together.Hydroxyl pinacolone retinol needs recrystallization to obtain product with higher purity, so the used recrystallization device is particularly important.In existing recrystallization device, crystal may adhere to side wall, and it is difficult to pour out, and other defects exist, and the crystallized product cannot be completely taken out, so yield and production efficiency are reduced. SUMMARY

[0005] The utility model aims at providing a kind of recrystallization device for hydroxyl pinacolone retinol synthesis to solve the problems raised in the above background.

[0006] To achieve the above object, the utility model provides the following technical scheme:

[0007] The utility model provides a kind of recrystallization device for hydroxyl pinacolone retinol synthesis, including kettle body, kettle cover, filter base, discharging device, kettle body is provided with cooling layer outside, kettle cover is set up on kettle body, motor is set up on kettle cover, motor connects stirring shaft, stirring shaft bottom penetrates kettle cover and suspends in kettle body, stirring shaft bottom is provided with multiple paddles, filter base is set up at kettle body bottom, filter base is bolted and sealed with kettle body, and filter base bottom is connected with discharging device by lifting mechanism.

[0008] Further, positioning plate is set up on cooling layer, and the crystallization device is placed on support frame by positioning plate, to facilitate the discharge of bottom discharging device.

[0009] Further, the filter base comprises a ring-shaped sealing plate, an inner edge of the sealing plate is provided with a cylindrical flange arranged upward, an upper edge of the flange is fixedly connected with a conical filter plate, and a lower end surface of the sealing plate is designed with a cylindrical baffle downward, the baffle is provided with a reverse conical discharge port inside, and the discharge port is connected with a discharge pipe.

[0010] Further, the upper end of the flange is further fixedly connected with a support rod, one, two or more ring-shaped scrapers are fixedly connected on the support rod, the ring-shaped scrapers are arranged to scrape the product adhered to the wall during discharging, and residual products are removed at the same time.

[0011] Further, the discharge device comprises a discharge tank, a cylindrical solvent tank is arranged in the discharge tank, a lifting rod is arranged in the wall of the solvent tank, the lifting rod is fixedly connected to the lower surface of the filter base through a support block, after crystallization is completed, the mixed solution of solvent and product is filtered through the conical filter plate after the discharge pipe is opened, the solvent is discharged to the solvent tank through the discharge pipe, the crystallization product is on the conical filter plate, after the mixed solution is completely discharged, the bolt between the filter base and the kettle body is opened, the lifting rod is lowered to drive the filter base to descend, so that the ring-shaped scraper is driven to move downward to scrape the wall, and the ring-shaped scraper slides along the conical filter plate to the discharge tank.

[0012] Further, the outer diameter of the solvent tank is smaller than the inner diameter of the baffle, the baffle is sleeved outside the solvent tank during discharging, and the product is prevented from entering the solvent tank during discharging.

[0013] Further, a cover is arranged on the solvent tank to prevent solvent volatilization.

[0014] Further, a pipeline is arranged at the bottom of the solvent tank to communicate with the discharge tank outside, so that the solvent can be recycled.

[0015] Compared with the prior art, the beneficial effects of the present application are:

[0016] The present application discloses a kind of heavy crystallization devices for hydroxyl pinakon retinol synthesis, kettle bottom is provided with filter base, the conical filter plate of filter base, ring-shaped scraper, improve the filtering efficiency and improve yield;With the discharge device matched with filter base, the two are used in cooperation, improve yield while also improving efficiency, and simple operation. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 It is a kind of heavy crystallization devices for hydroxyl pinakon retinol synthesis of the utility model's three-dimensional structure schematic diagram;

[0018] Figure 2 It is a kind of heavy crystallization devices for hydroxyl pinakon retinol synthesis of the utility model's internal structure schematic diagram;

[0019] Figure 3 It is a three-dimensional structure schematic view of the filter base of the utility model.

[0020] Mark explanation

[0021] In the figure: 1, kettle body; 2, kettle cover; 3, cooling layer; 4, positioning plate; 5, filter base; 6, discharge pool; 7, motor; 8, feed inlet; 9, baffle; 10, solvent pool; 11, lifting rod; 12, discharge pipe; 13, stirring shaft; 14, paddle; 15, annular scraper; 16, support rod; 17, conical filter plate; 18, sealing plate. Specific implementation

[0022] The technical solutions in the embodiments of the utility model will be clearly and completely described below with reference to the drawings in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by those skilled in the art without creative labor belong to the protection scope of the utility model. Embodiment 1

[0023] A kind of recrystallization device for hydroxyl pinakon retinol ester synthesis, including kettle body 1, kettle cover 2, filter base 5, discharge device, kettle body 1 outside is provided with cooling layer 3, kettle body 1 upper end portion is also equipped with feed inlet 8, kettle body 1 is provided kettle cover 2, kettle cover 2 is provided with motor 7, motor 7 connects stirring shaft 13, stirring shaft 13 bottom penetrates kettle cover 2 and is suspended in kettle body 1, stirring shaft 13 bottom is provided with multiple paddles 14, kettle body 1 bottom is provided with filter base 5, filter base 5 is bolted and sealed with kettle body 1, filter base 5 bottom is connected with discharge device by lifting mechanism.

[0024] Cooling layer 3 is provided with positioning plate 4, and the crystallization device is placed on the support frame by positioning plate 4.

[0025] Filter base 5 includes annular sealing plate 18, the inner edge of sealing plate 18 is provided with a cylindrical flange upward, the upper edge of the flange is fixedly connected with a conical filter plate 17, the lower end surface of the sealing plate 18 is designed downward with a cylindrical baffle 9, the baffle 9 is provided with an inverted conical discharge port, and the discharge port is connected with a discharge pipe 12. The upper end of the flange is also fixedly connected with a support rod 16, and the support rod 16 is fixedly connected with two annular scrapers 15, and the annular scrapers 15 are arranged to scrape the wall-stuck product during discharge.

[0026] The discharging device comprises a discharging tank 6, a cylindrical solvent tank 10 is arranged in the discharging tank 6, a lifting rod 11 is arranged on the wall of the solvent tank 10, the lifting rod 11 is fixedly connected to the lower surface of the filter base 5 through a supporting block; the outer diameter of the solvent tank 10 is smaller than the inner diameter of the baffle 9, the baffle 9 is sleeved outside the solvent tank 10 during discharging; a cover is arranged on the solvent tank 10. A pipeline is arranged at the bottom of the solvent tank 10 and is communicated with the discharging tank 6.

[0027] Working principle: the recrystallized substance and the crystallization solvent are added into the kettle body 1 from the feeding port 8, the motor 7 and the cooling layer 3 are started, the stirring shaft 13 is driven to stir and mix, the cooling layer 3 cools and crystallizes the system in the kettle, after the crystallization is completed, the discharging pipe 12 switch is opened, the mixed solution of the solvent and the product is filtered through the conical filter plate 17, the solvent is discharged to the solvent tank 10 through the discharging pipe 12, the crystallized product is on the conical filter plate 17, after the mixed solution is completely discharged, the bolt between the filter base 5 and the kettle body 1 is opened, the lifting rod 11 is lowered to drive the filter base 5 to descend, so as to drive the annular scraper 15 to move downward and scrape the wall, and then the annular scraper 15 slides along the conical filter plate 17 to the discharging tank 6, and the discharging is completed.

[0028] It should be noted that the relational terms such as first and second and the like in this text are merely used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply that there is any such actual relationship or order between these entities or operations. Moreover, the terms "include", "contain" or any other variants thereof are intended to cover non-exclusive inclusion, so that the process, method, article or equipment including a series of elements not only includes those elements, but also includes other elements not explicitly listed or inherent to such process, method, article or equipment.

[0029] It should be noted that the above only illustrates the technical thought of the present application, and cannot limit the protection scope of the present application. For ordinary skilled persons in the technical field, some improvements and refinements can be made without departing from the principle of the present application, and these improvements and refinements all fall within the protection scope of the present application.

Claims

1. A recrystallization apparatus for the synthesis of hydroxypinazone retinate, characterized in that, The device includes a vessel body, a vessel lid, a filter base, and a discharge device. A cooling layer is installed outside the vessel body. The vessel lid is installed on the vessel body, and a motor is installed on the vessel lid. The motor is connected to a stirring shaft. The bottom of the stirring shaft passes through the vessel lid and is suspended inside the vessel body. Multiple blades are installed at the bottom of the stirring shaft. A filter base is installed at the bottom of the vessel body. The filter base is bolted to the vessel body. The bottom of the filter base is connected to the discharge device through a lifting mechanism.

2. The recrystallization apparatus for the synthesis of hydroxypinazone retinate according to claim 1, characterized in that, A positioning plate is provided on the cooling layer.

3. The recrystallization apparatus for the synthesis of hydroxypinazone retinate according to claim 1, characterized in that, The filter base includes an annular sealing plate. A cylindrical flange is provided on the inner edge of the sealing plate, and a conical filter plate is fixedly connected to the upper edge of the flange. A cylindrical baffle is designed on the lower end of the sealing plate, and an inverted conical discharge port is provided inside the baffle. The discharge port is connected to a discharge pipe.

4. The recrystallization apparatus for the synthesis of hydroxypinazone retinate according to claim 3, characterized in that, A support rod is also fixedly connected to the upper end of the flange, and one, two or more annular scrapers are fixedly connected to the support rod.

5. The recrystallization apparatus for the synthesis of hydroxypinazone retinate according to claim 3, characterized in that, The discharge device includes a discharge pool, inside which is a cylindrical solvent pool. A lifting rod is installed inside the solvent pool wall, and the lifting rod is fixedly connected to the lower surface of the filter base by a support block.

6. The recrystallization apparatus for the synthesis of hydroxypinazone retinate according to claim 5, characterized in that, The outer diameter of the solvent pool is smaller than the inner diameter of the baffle.

7. The recrystallization apparatus for the synthesis of hydroxypinazone retinate according to claim 5, characterized in that, A cover is provided on the solvent pool.

8. The recrystallization apparatus for the synthesis of hydroxypinazone retinate according to claim 5, characterized in that, The solvent tank is connected to the outside of the discharge tank by a pipe at the bottom.

Images