An ethylene glycol crude product purification device

Abstract

The utility model discloses a kind of glycolide crude product purification equipment, including spherical reaction kettle and reaction kettle base;The spherical reaction kettle is rotatably connected in the reaction kettle base;The stirring assembly of stirring material is provided in the spherical reaction kettle interior;The spherical reaction kettle includes upper half, the liquid inlet for liquid inlet is opened in the upper half top, and the first liquid discharge port for liquid discharge is opened in side wall.The spherical reaction kettle further includes lower half, the lower half is located in the reaction kettle base inboard, the lower half and the upper half butt joint, connect by fixing part.The stirring assembly includes second transmission shaft and stirring paddle, the upper end of the second transmission shaft is connected drive source by penetrating the upper half, and lower end is located in the spherical reaction kettle interior and connects the stirring paddle.The utility model aims at overcoming existing defects and provides a kind of glycolide crude product purification equipment, simple structure, easy operation, and guarantee cleaning quality.

Description

Technical Field

[0001] This utility model relates to a purification device for crude glycolide. Background Technology

[0002] Polyglycolic acid (PGA) and its polymers are important biodegradable polymers for medical applications. High molecular weight PGA can be prepared by ring-opening polymerization of glycolide. The purity of glycolide has a significant impact on the molecular weight and other properties of PGA.

[0003] In the prior art, patent document CN 119771261 A discloses a lactide purification system and method. The lactide purification system includes a first stirred tank, a second stirred tank, a feeding component, a discharging component, a solvent adding component, and a central control platform. The feeding component, discharging component, and solvent adding component are all connected to the first and second stirred tanks. The central control platform controls the working status of the feeding component, discharging component, and solvent adding component. The mass ratio of solvent to crude lactide is 1:(1.2~1.4). In this patent, when the feed amount of crude lactide reaches a preset value, the central control platform automatically adjusts the status of the relevant components, switches the crude lactide conveying process to another stirred tank, and automatically adds solvent to the corresponding stirred tank. This achieves automated control of the crude lactide and solvent mixing process, ensuring the accuracy of the mass ratio between crude lactide and solvent and preventing product quality defects caused by mixing deviations.

[0004] However, in actual operation, the equipment is complex, and residues of crude glycolide and solvent remain in the pipeline, which has a significant impact on the final purity of glycolide.

[0005] Therefore, a crude glycolide purification device is proposed to address the above problems. Utility Model Content

[0006] The purpose of this invention is to overcome the existing defects and provide a crude glycolide purification device with simple structure, convenient operation, and guaranteed cleaning quality.

[0007] To achieve the above objectives, this utility model provides the following technical solution: a crude glycolide purification device, comprising a spherical reactor and a reactor base; the spherical reactor is rotatably connected inside the reactor base; a stirring assembly for stirring materials is provided inside the spherical reactor;

[0008] The spherical reactor includes an upper body, with an inlet for liquid inlet on the upper body and a first outlet for liquid outlet on the side wall.

[0009] Preferably, the spherical reactor further includes a lower half, which is located inside the reactor base and is connected to the upper half by a fastener.

[0010] Preferably, the stirring assembly includes a second drive shaft and a stirring paddle. The upper end of the second drive shaft passes through the upper body and is connected to a drive source, while the lower end is located inside the spherical reactor and is connected to the stirring paddle.

[0011] Preferably, it further includes a metal filter screen, with the lower outer wall of the second drive shaft connected to the horizontally arranged first drive shaft, and the metal filter screen connected to the outer wall of the first drive shaft.

[0012] Preferably, it also includes liquid cooling and heating pipelines, which are connected to the outer wall of the reactor base for heating or cooling the internal spherical reactor.

[0013] Preferably, a second drain port is provided at the bottom of the reactor base.

[0014] Preferably, a temperature sensor for detecting the temperature of the spherical reactor is provided on the inner wall of the reactor base.

[0015] Preferably, the bottom of the reactor base is connected to multiple support columns for support.

[0016] Compared with the prior art, the beneficial effects of this utility model are: This crude glycolide purification equipment includes a spherical reactor and a reactor base; the spherical reactor is rotatably connected inside the reactor base; the spherical reactor is equipped with a stirring component for stirring materials; the structure is simple, the operation is convenient, the cleaning quality is guaranteed, and the purification of crude glycolide is achieved in the same reactor, avoiding the residue of crude glycolide and solvent during pipeline transportation, which would affect the purity of the final product. Attached Figure Description

[0017] The accompanying drawings are provided to further illustrate the present invention and form part of the specification. They are used together with the embodiments of the present invention to explain the present invention, but do not constitute a limitation thereof. In the drawings:

[0018] Figure 1 This is an isometric view of the crude glycolide purification equipment of this utility model;

[0019] Figure 2 This is an isometric view of the crude glycolide purification equipment of this utility model from another perspective;

[0020] Figure 3 This is a detailed drawing of the spherical reactor of this utility model;

[0021] Figure 4 This is a detailed internal view of the spherical reactor of this utility model.

[0022] In the diagram: 1. Spherical reactor; 2. Liquid inlet; 3. Stirring paddle; 4. First drain outlet; 5. Metal filter screen; 6. First drive shaft; 8. Fixing component; 9. Reactor base; 10. Second drain outlet; 11. Liquid cooling and heating pipeline; 12. Central control platform; 13. Upper body; 14. Lower body; 15. Second drive shaft; 16. Support column. Detailed Implementation

[0023] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0024] like Figure 1-4 As shown, a crude glycolide purification device includes a spherical reactor 1 and a reactor base 9. The spherical reactor 1 is rotatably connected to the reactor base 9. A stirring assembly for stirring materials is installed inside the spherical reactor 1. The spherical reactor 1 includes an upper body 13, with a liquid inlet 2 at the top and a first drain outlet 4 on the side wall for draining. The spherical reactor 1 also includes a lower body 14, located inside the reactor base 9, which is connected to the upper body 13 via a fastener 8. A second drain outlet 10 is located at the bottom of the reactor base 9.

[0025] Specifically, the stirring assembly includes a second drive shaft 15 and a stirring paddle 3. The upper end of the second drive shaft 15 passes through the upper half 13 and is connected to the drive source, while the lower end is located inside the spherical reactor 1 and connected to the stirring paddle 3. It also includes a metal filter screen 5. The lower outer wall of the second drive shaft 15 is connected to a horizontally arranged first drive shaft 6, and the metal filter screen 5 is connected to the outer wall of the first drive shaft 6.

[0026] Specifically, the metal filter screen has a pore size of 80-120μm and a thickness of not less than 1mm; the outer end of the filter screen has a layer of fluororubber on both the upper and lower layers for sealing with the upper and lower layers of the spherical reactor.

[0027] Specifically, the thickness of the three blades of the agitator is not less than 2mm, and the agitator is driven by an external motor with a speed of not less than 6000rpm.

[0028] Specifically, it also includes liquid cooling and heating pipelines 11, which are connected to the outer wall of the reactor base 9 and used for heating or cooling the internal spherical reactor 1. The liquid cooling and heating pipelines 11 can provide a temperature of 0-100℃ to the spherical reactor.

[0029] Specifically, the thickness of the spherical reactor 1 shall not be less than 1 mm.

[0030] Specifically, the thickness of the reactor base 9 shall not be less than 3mm.

[0031] Specifically, a temperature sensor for detecting the temperature of the spherical reactor 1 is installed on the inner wall of the reactor base 9.

[0032] Specifically, the bottom of the reactor base 9 is connected to multiple support columns 16 for support. The support columns 16 are stainless steel pipes.

[0033] Specifically, the first drive shaft 6, the second drive shaft 15, the agitator 3, the spherical reactor 1, and the metal filter screen 5 are all made of stainless steel (304 stainless steel). The first drive shaft 6 and the metal filter screen 5 are welded together. The metal filter screen 5 is located in the middle of the spherical reactor 1, and both the upper and lower parts of the spherical reactor 1 are separable. The agitator 3 passes through the top of the spherical reactor and is controlled to rotate by an external motor. The liquid inlet 3 and the first liquid outlet 4 at the upper end of the spherical reactor can be opened or closed as needed. The central control platform 12 can control the rotation of the spherical reactor 1 to rotate at any angle by controlling the rotating shaft; it can also display the temperature inside the reactor and control the temperature inside the spherical reactor through the liquid cooling and heating pipes 11.

[0034] Specifically, the solid-liquid mixture of crude glycolide is added to the lower spherical reactor 1, with a volume not exceeding 1 / 3 of the reactor 1's volume. A metal filter screen 5 and the upper half 13 of the spherical reactor 1 are then placed in sequence, and the reactor 1 is sealed closed using fasteners 8. The first drain port 4 is closed, and anhydrous ethanol is added into the spherical reactor 1 through the inlet port 2, with the liquid level between 1 / 3 and 1 / 2 of the reactor 1's volume. The stirring paddle 3 is driven by an external motor to stir the mixture at a speed between 6000 and 8000 rpm for 3 to 5 minutes. The motor is removed, and the spherical reactor 1 is rotated via the central control platform 12 until the first drain port 4 aligns with the second drain port 10. The first drain port 4 is then opened, and the waste liquid is discharged through the second drain port 10. The first drain port 4 is closed, and the spherical reactor 1 is reset via the central control platform 12. Anhydrous ethanol is then added again, and the above steps are repeated twice. After the final evacuation of the waste liquid, close the first drain port 4, reset the spherical reactor 1, and connect an external vacuum gauge and vacuum pump to the inlet 2 to maintain the pressure inside the spherical reactor 1 below -0.1 MPa. Control the temperature inside the spherical reactor 1 at 44–46°C using the central control platform 12, and continue heating for 7–9 hours. Turn off the heating and remove the external vacuum equipment. Weigh the crude glycolide (m) inside the spherical reactor 1. Add ethyl acetate through the inlet 2, with a volume equal to 130–200% of the crude glycolide mass (m). Install a reflux condenser pipe at the inlet 2. Control the temperature inside the spherical reactor 1 to 68–74°C using the central control platform 12. Use an external motor to stir the mixture via a stirrer 3 at a speed between 500–800 rpm for 0.5–2 hours. Then remove the reflux condenser pipe and the external motor, close the inlet 2, and control the temperature inside the spherical reactor 1 to 0–15°C using the central control platform 12, maintaining this temperature for 2–3 hours. Controlling the spherical reactor 1 via the central control platform 12, rotate the first drain port 4 to align with the second drain port 10, opening the first drain port 4 to discharge waste liquid. Then, control the spherical reactor 1 to reset and close the first drain port 4. Open the inlet port 2 and add ethyl acetate, adding 70-90% of the previous volume. Install a reflux condenser pipe on the inlet port 2. Control the temperature inside the spherical reactor 1 to 68-74℃ via the central control platform 12. Use an external motor to stir via the agitator 3 at a speed between 500-800 rpm for 0.5-2 hours. Then, remove the reflux condenser pipe and the external motor, close the inlet port 2, and turn off the temperature heating via the central control platform 12, maintaining this temperature for 16-20 hours. Controlling the spherical reactor 1 via the central control platform 12, rotate the first drain port 4 to align with the second drain port 10, opening the first drain port 4 to discharge waste liquid. Then, close the first drain port 4 and control the spherical reactor 1 to reset. A vacuum gauge and vacuum pump are connected to the liquid inlet 2 to keep the pressure inside the spherical reactor 1 < -0.1 MPa. The temperature inside the spherical reactor 1 is controlled at 44-46℃ by the central control platform 12. After continuous heating for 7-9 hours, purified glycolide can be obtained.

[0035] This crude glycolide purification equipment consists of a spherical reactor 1 and a reactor base 9. The spherical reactor 1 is rotatably connected to the reactor base 9. The spherical reactor 1 is equipped with a stirring component for stirring materials. The equipment has a simple structure, is easy to operate, ensures the quality of cleaning, and achieves the purification of crude glycolide in the same reactor. This avoids the residue of crude glycolide and solvent during pipeline transportation, which would affect the purity of the final product.

[0036] Finally, it should be noted that the above are merely preferred embodiments of this utility model and are not intended to limit the utility model. Although the utility model 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 this utility model should be included within the protection scope of this utility model.

Claims

1. An ethylene glycol crude purification apparatus, characterized by, It includes a spherical reactor (1) and a reactor base (9); the spherical reactor (1) is rotatably connected inside the reactor base (9); the spherical reactor (1) is equipped with a stirring assembly for stirring materials. The spherical reactor (1) includes an upper body (13), with an inlet (2) for liquid inlet on the upper body (13) and a first drain (4) for liquid outlet on the side wall.

2. The crude glycolide purification apparatus of claim 1, wherein, The spherical reactor (1) also includes a lower half (14), which is located inside the reactor base (9). The lower half (14) and the upper half (13) are connected by a fastener (8).

3. The crude glycolide purification apparatus of claim 1, wherein, The stirring assembly includes a second drive shaft (15) and a stirring paddle (3). The upper end of the second drive shaft (15) passes through the upper half (13) and is connected to the drive source, while the lower end is located inside the spherical reactor (1) and is connected to the stirring paddle (3).

4. The crude glycolide purification apparatus of claim 3, wherein, It also includes a metal filter screen (5), and the lower end of the outer wall of the second drive shaft (15) is connected to the first drive shaft (6) which is arranged horizontally. The metal filter screen (5) is connected to the outer wall of the first drive shaft (6).

5. The crude glycolide purification apparatus of claim 1, wherein, It also includes liquid cooling and heating pipelines (11), which are connected to the outer wall of the reactor base (9) for heating or cooling the internal spherical reactor (1).

6. The crude glycolide purification apparatus of claim 1, wherein, The bottom of the reactor base (9) has a second drain port (10).

7. The glycolide crude purification apparatus according to claim 1, wherein, A temperature sensor for detecting the temperature of the spherical reactor (1) is provided on the inner wall of the reactor base (9).

8. The glycolide crude purification apparatus according to claim 1, wherein, The bottom of the reactor base (9) is connected to multiple support columns (16) for support.

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