A retinol crystallization separation and purification device

Abstract

The application discloses a retinol crystallization separation and purification device, in particular to the technical field of recrystallization, which comprises a recrystallization tank, a closely-fitted heat exchange sleeve is arranged on the recrystallization tank, and a spiral heat exchange pipe is embedded in the heat exchange sleeve; the two ends of the heat exchange pipe are connected with the circulation loop of a semiconductor temperature control assembly; the semiconductor temperature control assembly is provided with a heat circulation loop and a cold circulation loop which can be switched with each other; a connecting seat is connected with the bottom of the recrystallization tank; an electromagnetic valve is arranged in the pipeline between the connecting seat and the recrystallization tank; a one-way air inlet valve is arranged on the top of the recrystallization tank and is communicated with the inner cavity of the recrystallization tank; a filter bottle is connected with the bottom of the connecting seat; a hole plate is arranged on the annular protrusion of the inner wall of the top of the filter bottle; a filter paper is arranged on the top of the hole plate and covers the hole plate completely; and a filter tube is arranged on the middle of the filter bottle. The semiconductor temperature control assembly is arranged to heat and cool the substance in the recrystallization tank, the energy consumption of refrigeration is saved, and the experimental steps are simplified.

Description

Technical Field

[0001] This utility model belongs to the field of recrystallization technology, specifically relating to a retinol crystallization separation and purification device. Background Technology

[0002] The crystallization and purification of retinol (vitamin A alcohol) is a sophisticated chemical process aimed at obtaining high-purity crystals that meet pharmaceutical or food-grade standards from mixtures such as crude crystals, reaction solutions, or concentrates. Its core principle is to utilize the differences in retinol's solubility in different solvents and at different temperatures to achieve separation and purification.

[0003] Traditional recrystallization processes require heating and then cooling the retinol-containing solution. These two steps are independent and both consume energy, requiring different equipment and making the process cumbersome. Therefore, a novel retinol crystallization and purification device is needed. Utility Model Content

[0004] To address the aforementioned problems, this utility model discloses a retinol crystallization separation and purification device.

[0005] To achieve the above objectives, the technical solution of this utility model is as follows:

[0006] A retinol crystallization separation and purification device includes a recrystallization tank. The recrystallization tank is fitted with a heat exchange jacket that fits tightly, and a spiral heat exchange tube is embedded in the heat exchange jacket. The two ends of the heat exchange tube are connected to the circulation loop of a semiconductor temperature control component, and the semiconductor temperature control component is provided with a switchable hot circulation loop and a cold circulation loop. The bottom of the recrystallization tank is connected to a connecting seat, and a solenoid valve is installed in the pipeline between the connecting seat and the recrystallization tank. A one-way air inlet valve is installed on the top of the recrystallization tank and communicates with its inner cavity. A filtration flask is connected to the bottom of the connecting seat. A perforated plate is placed on the annular protrusion on the top inner wall of the filtration flask, and filter paper that completely covers the perforated plate is placed on top of the perforated plate. A filtration tube extends from the middle of the filtration flask.

[0007] As a preferred embodiment of this utility model, the semiconductor temperature control component includes a temperature control box. The inner cavity of the temperature control box is equipped with semiconductor cooling chips that divide the inner cavity equally. A three-way valve is installed at the top and bottom of the temperature control box, and the two three-way valves are respectively connected to both ends of the heat exchange tube. Each three-way valve is simultaneously connected to both compartments of the temperature control box, and each three-way valve is equipped with an electromagnetic switch for switching the connection between the heat exchange tube and the two compartments. A delivery pump is installed at the two inlets of the bottom three-way valve in each of the two compartments of the temperature control box.

[0008] As a preferred embodiment of this invention, heat exchange fins are attached to both the cold and hot ends of the semiconductor refrigeration chip.

[0009] As a preferred embodiment of this utility model, the top of the temperature control box extends into two circular tubes that communicate with its compartments, and the top of the circular tubes is covered with a top cover.

[0010] As a preferred embodiment of this utility model, both compartments of the temperature control box are equipped with temperature sensors.

[0011] As a preferred technical solution of this utility model, the connecting seat and the filtration bottle are connected by threads, and the filtration bottle has a polygonal outer contour at the connection.

[0012] As a preferred embodiment of this utility model, the heat exchange jacket is fixedly connected to a bracket, and the heat exchange jacket, the semiconductor temperature control component, and the connecting seat are all fixedly connected to the branch at the top of the bracket.

[0013] As a preferred embodiment of the present invention, a conical plug is inserted into the top feed inlet of the recrystallization tank, and the feed inlet is configured as a conical opening adapted to the conical plug.

[0014] The beneficial effects of this utility model are as follows:

[0015] 1. This application is equipped with a semiconductor temperature control component to heat and cool the substance in the recrystallization tank. When the heat exchange tube is connected to the hot circulation loop of the semiconductor temperature control component, the liquid in the hot end compartment is heated and transported to the heat exchange tube for circulation backflow, while the liquid in the cold end compartment is cooled. When the heat exchange tube needs to be connected to the cold circulation loop of the semiconductor temperature control component, only a small amount of cooling of the liquid in the cold end compartment by the semiconductor cooling chip is required to meet the cooling needs of the cold circulation loop, saving energy consumption for cooling. At the same time, the same experimental equipment is used for heating and cooling, without the need to change the equipment, simplifying the experimental steps.

[0016] Second, after recrystallization is completed, the newly precipitated retinol crystals can be quickly separated from the solution by vacuum filtration, which can reduce the solution temperature rise caused by slow operation and the redissolution of retinol crystals, thereby improving the yield of retinol recrystallization. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the overall structure of an embodiment of the present utility model;

[0018] Figure 2 This is an exploded view of the recrystallization tank, heat exchange tube, connecting seat, solenoid valve, vacuum filtration flask, orifice plate, filter paper, conical plug, and one-way air inlet valve according to an embodiment of the present invention.

[0019] Figure 3 This is a cross-sectional view of a semiconductor temperature control component according to an embodiment of the present invention.

[0020] List of identifiers in attached diagrams:

[0021] 1. Recrystallization tank; 2. Heat exchange jacket; 3. Heat exchange tubes;

[0022] 4. Semiconductor temperature control assembly; 401. Temperature control box; 402. Semiconductor refrigeration chip; 403. Heat exchange fins; 404. Three-way valve; 405. Transfer pump; 406. Top cover;

[0023] 5. Connecting seat; 6. Solenoid valve; 7. Filter bottle; 8. Orifice plate; 9. Filter paper; 10. Conical plug; 11. One-way air inlet valve; 12. Support. Detailed Implementation

[0024] The present invention will be further explained below with reference to the accompanying drawings and specific embodiments. It should be understood that the following specific embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention.

[0025] Please see Figure 1-3 A retinol crystallization separation and purification device includes a recrystallization tank 1, which is fitted with a heat exchange jacket 2, and a spiral heat exchange tube 3 is embedded in the heat exchange jacket 2. The recrystallization tank 1, the heat exchange jacket 2, and the spiral heat exchange tube 3 are made of a thermally conductive material. The two ends of the heat exchange tube 3 are connected to the circulation loop of a semiconductor temperature control component 4. The semiconductor temperature control component 4 is provided with a hot circulation loop and a cold-hot circulation loop, and the heat exchange tube 3 can switch between the hot circulation loop and the cold-hot circulation loop. A connecting seat 5 is connected to the bottom of the recrystallization tank 1, and a solenoid valve 6 is installed in the pipeline between the connecting seat 5 and the recrystallization tank 1. A one-way air inlet valve 11 is installed on the top of the recrystallization tank 1 and communicates with its inner cavity. A filtration flask 7 is connected to the bottom of the connecting seat 5, and a filtration tube extends from the middle of the filtration flask 7. The filtration tube of the filtration flask 7 is connected to a vacuum pump for vacuuming during operation via a hose. A perforated plate 8 is placed on the annular protrusion on the top inner wall of the filtration flask 7, and filter paper 9 is placed on top of the perforated plate 8 to completely cover the perforated plate 8.

[0026] The semiconductor temperature control assembly 4 includes a temperature control box 401, the inner cavity of which is equipped with semiconductor cooling chips 402 that divide the inner cavity equally. A three-way valve 404 is installed at the top and bottom of the temperature control box 401, and the two three-way valves 404 are respectively connected to both ends of the heat exchange tube 3. Each three-way valve 404 is simultaneously connected to both chambers of the temperature control box 401, and each three-way valve 404 is equipped with an electromagnetic switch for switching the connection between the heat exchange tube 3 and the two chambers. In each of the two chambers of the temperature control box 401, a delivery pump 405 is installed at both inlet ports of the bottom three-way valve 404. When the heat exchange tube 3 is connected to the hot circulation loop, the two three-way valves 404 control the heat exchange tube 3 to only be connected to the hot end compartment of the semiconductor cooling chip 402 through the electromagnetic switch. The hot end compartment delivery pump 405 delivers the liquid in the hot end compartment to the heat exchange tube 3 for circulation backflow. The heat exchange tube 3 heats the material inside the recrystallization tank 1 through the recrystallization tank 1 and the heat exchange jacket 2. The same applies when the heat exchange tube 3 is connected to the cold circulation loop.

[0027] Both the cold and hot ends of the thermoelectric cooler 402 are fitted with heat exchange fins 403. The heat exchange fins 403 enable rapid heat exchange between the cold and hot ends of the thermoelectric cooler 402 and the liquid inside the temperature control chamber 401. The liquid inside the temperature control chamber 401 can remain liquid over a wide temperature range, such as kerosene, which can remain liquid from -40 degrees Celsius to 150 degrees Celsius.

[0028] Two circular tubes extend from the top of the temperature control box 401, communicating with its respective chamber, and the top of the circular tubes is covered with a top cover 406. After long-term use, the liquid inside the temperature control box 401 will be lost, which can be replenished by opening the top cover 406.

[0029] Temperature sensors are installed in both compartments of the temperature control box 401. The temperature sensors are used to detect whether the circulating liquid has reached the required temperature, thereby controlling the working state of the semiconductor cooling chip 402.

[0030] The connecting seat 5 and the filtration bottle 7 are connected by threads, and the filtration bottle 7 has a polygonal outer contour at the connection point, which makes it easy to tighten by hand or disassemble with a wrench.

[0031] The heat exchange jacket 2 is fixedly connected to the bracket 12, and the heat exchange jacket 2, the semiconductor temperature control component 4, and the connecting seat 5 are all fixedly connected to the branch at the top of the bracket 12. The bottom of the filtration bottle 7 is suspended after installation.

[0032] A conical plug 10 is inserted into the top feed inlet of the recrystallization tank 1, and the feed inlet is configured as a conical opening that matches the conical plug 10. The conical fit can enhance the sealing of the top feed inlet of the recrystallization tank 1.

[0033] Working principle:

[0034] In use, an ethanol-water (volume ratio 8:2) mixture is added to recrystallization tank 1 as a solvent. Then, retinol crystals are added to recrystallization tank 1. The heat exchange tube 3 is connected to the thermal circulation loop of the semiconductor temperature control component 4 to heat recrystallization tank 1 (heating the solution to 60 degrees Celsius) so that the retinol crystals are completely dissolved to form a saturated retinol solution. Then, the heat exchange tube 3 is connected to the cold circulation loop of the semiconductor temperature control component 4 to cool recrystallization tank 1 (slowly cooling to 0 to 5 degrees Celsius and growing crystals at this temperature for 4 to 12 hours). During the cooling process, new retinol crystals precipitate from the solution. Then, the solenoid valve 6 is opened, and the suction tube of the suction flask 7 is connected to the vacuum pump through the hose to draw a vacuum (air is introduced through the one-way air inlet valve 11), so that the solid-liquid mixture in recrystallization tank 1 is filtered through the filter paper 9. The newly precipitated retinol crystals remain on the filter paper 9, and the solution flows into the bottom of the suction flask 7. Finally, the suction flask 7 can be unscrewed to remove the retinol crystals on the filter paper 9.

[0035] When the heat exchange tube 3 is connected to the hot circulation loop of the semiconductor temperature control component 4, the liquid in the hot end compartment is heated and transported to the heat exchange tube 3 for circulation and return. At the same time, the liquid in the cold end compartment is cooled. When the heat exchange tube 3 needs to be connected to the cold circulation loop of the semiconductor temperature control component 4, only a small amount of cooling of the liquid in the cold end compartment by the semiconductor cooling chip 402 is needed to meet the cooling needs of the cold circulation loop. (When the heat exchange tube 3 is initially connected to the cold circulation loop, the liquid in the cold end compartment will mix with the liquid with a higher temperature in the heat exchange tube 3, making it difficult to generate a low temperature that exceeds the cooling requirement. If a low temperature that exceeds the cooling requirement is generated, the temperature can be increased by switching between the hot circulation loop and the cold circulation loop multiple times.)

[0036] It should be noted that the above content merely illustrates the technical concept of this utility model and cannot be used to limit the scope of protection of this utility model. For those skilled in the art, several improvements and modifications can be made without departing from the principle of this utility model, and all such improvements and modifications fall within the scope of protection of the claims of this utility model.

Claims

1. A retinol crystallization separation and purification apparatus, comprising a recrystallization tank (1), characterized in that, The recrystallization tank (1) is fitted with a heat exchange jacket (2) that fits tightly, and the heat exchange jacket (2) is embedded with a spiral heat exchange tube (3). The two ends of the heat exchange tube (3) are connected to the circulation loop of the semiconductor temperature control component (4), and the semiconductor temperature control component (4) is provided with a hot circulation loop and a cold circulation loop that can be switched between each other. The bottom of the recrystallization tank (1) is connected to a connecting seat (5), and a solenoid valve (6) is provided in the pipeline between the connecting seat (5) and the recrystallization tank (1). The top of the recrystallization tank (1) is equipped with a one-way air inlet valve (11) that communicates with its inner cavity. The bottom of the connecting seat (5) is connected to a suction flask (7). A perforated plate (8) is placed on the annular protrusion on the top inner wall of the suction flask (7), and a filter paper (9) that completely covers the perforated plate (8) is placed on the top of the perforated plate (8). A suction tube extends from the middle of the suction flask (7).

2. The retinol crystallization separation and purification apparatus according to claim 1, characterized in that, The semiconductor temperature control assembly (4) includes a temperature control box (401). The inner cavity of the temperature control box (401) is equipped with semiconductor cooling chips (402) that divide the inner cavity equally. A three-way valve (404) is installed at the top and bottom of the temperature control box (401), and the two three-way valves (404) are respectively connected to both ends of the heat exchange tube (3). Each three-way valve (404) is simultaneously connected to the two compartments of the temperature control box (401), and each three-way valve (404) is equipped with an electromagnetic switch for switching the heat exchange tube (3) to the two compartments. In the two compartments of the temperature control box (401), a delivery pump (405) is installed at the two inlets of the bottom three-way valve (404).

3. The retinol crystallization separation and purification apparatus according to claim 2, characterized in that, The semiconductor cooling chip (402) has heat exchange fins (403) attached to both its cold and hot ends.

4. The retinol crystallization separation and purification apparatus according to claim 2, characterized in that, The top of the temperature control box (401) extends two circular tubes that communicate with its compartments, and the top of the circular tubes is covered with a top cover (406).

5. The retinol crystallization separation and purification apparatus according to claim 2, characterized in that, Temperature sensors are installed in both compartments of the temperature control box (401).

6. The retinol crystallization separation and purification apparatus according to claim 1, characterized in that, The connecting seat (5) and the filtration bottle (7) are connected by threads, and the filtration bottle (7) has a polygonal outer contour at the connection.

7. The retinol crystallization separation and purification apparatus according to claim 1, characterized in that, The heat exchange jacket (2) is fixedly connected to the bracket (12), and the heat exchange jacket (2), the semiconductor temperature control component (4), and the connecting seat (5) are all fixedly connected to the branch at the top of the bracket (12).

8. The retinol crystallization separation and purification apparatus according to claim 1, characterized in that, The top inlet of the recrystallization tank (1) is fitted with a conical plug (10), and the inlet is configured as a conical opening adapted to the conical plug (10).

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