Lipoic acid melt refining device

Abstract

The utility model discloses a lipoic acid melting refining device, which relates to the technical field of crystallization, and comprises a crystallizing tank, a filter screen, a sweating melting tank, a condenser pipe and a cold medium inlet II, one end of the crystallizing tank is communicated with a pulse nitrogen valve, the top of one end of the crystallizing tank is communicated with a feed valve, a jacket I is sleeved outside the crystallizing tank, and the condenser pipe is sleeved outside the jacket I; one end of the jacket I is communicated with the cold medium inlet I, the other end of the jacket I is communicated with the cold medium outlet I, a filter screen is welded inside the other end of the crystallizing tank, and the end part of the other end of the crystallizing tank is communicated with the residual liquid outlet valve. The whole device can be used for continuous crystallization, the production efficiency is greatly improved, the sweating link that pulse nitrogen is used for material transportation and hot nitrogen is used for melt crystallization is adopted, it is effectively guaranteed that a product does not make contact with oxygen to be deteriorated in the refining process, and the purity of the product is greatly improved.

Description

Technical Field

[0001] The utility model relates to the technical field of crystallization, in particular to a thioctic acid melting and refining device. Background Art

[0002] Lipoic acid is also known as α-lipoic acid, and its chemical name is 1,2-dithiolane-3-pentanoic acid. It is a coenzyme that exists in mitochondria. Due to its unique antioxidant properties, it can remove active oxygen components that cause skin aging. It also has good water solubility and fat solubility, and is easily absorbed by the skin. It is widely used in beauty and anti-aging drugs, skin care products, and health care products. In addition, it also has a good therapeutic effect on liver disease, diabetes, multiple sclerosis, acute infarction and other diseases. Therefore, its synthesis and refinement have become the focus and hotspot of research.

[0003] Existing industrial technology is to use 6,8-dichlorooctanoic acid ethyl ester and sulfur powder, sodium disulfide cyclization to generate thioctic acid ethyl ester, then hydrolyze to obtain thioctic acid crude product, and then use organic solvent (such as petroleum ether, n-hexane, isopropyl ether, cyclohexane, etc.) to refine to obtain thioctic acid (US3223712, EP0593896, US5455264,). However, there are some problems with these refining methods. Since the solvent itself carries a part of impurities, new impurities are generated in the product precipitated by recrystallization; the presence of oxygen in the air may cause impurities to be generated during product recrystallization; during recrystallization, the use of a large amount of organic solvents, and all of them are mixed solvents, makes it difficult to recycle solvents, reduce yields, and may also affect the environment. Therefore, a thioctic acid melting refining device is proposed for the above problems. Utility Model Content

[0004] In view of the deficiencies in the prior art, the utility model provides a lipoic acid melting refining device, which solves the problems raised in the background technology.

[0005] To achieve the above objectives, the utility model is implemented through the following technical solutions: a thioctic acid melting and refining device, comprising a crystallizer, a filter, a sweating melting tank, a condenser and a cold medium inlet II, one end of the crystallizer is connected to a pulse nitrogen valve, the top of one end of the crystallizer is connected to a feed valve, a jacket I is mounted on the outside of the crystallizer, one end of the jacket I is connected to a cold medium inlet I, the other end of the jacket I is connected to a cold medium outlet I, a filter is welded inside the other end of the crystallizer, and the other end of the crystallizer is connected to a residual liquid outlet valve, a movable plate is arranged below the filter, the movable plate is mounted on the outside of the output end of the first motor, the first motor is fixed to the outside of one side of the jacket I by screws, the movable plate is located at the top of the sweating melting tank, the top of the sweating melting tank is connected to the inside of the crystallizer, the bottom of the sweating melting tank is respectively connected to a hot nitrogen valve and a product outlet valve, the sweating melting tank is mounted on the outside of the sweating melting tank, and the top and bottom sides of the jacket II are respectively connected to a hot medium outlet and a hot medium inlet.

[0006] Preferably, a second motor is embedded in the bottom of the sweating melting tank, and the top output end of the second motor is externally connected to a stirring paddle through a shaft. The stirring paddle is arranged inside the sweating melting tank, and the stirring paddle is driven to rotate by the second motor, so that the solid can be stirred and heated uniformly.

[0007] Preferably, one side of the top of the sweating and melting tank is connected to a hot steam outlet valve, the hot steam outlet valve is connected to one end of the condenser, and the other end of the condenser is connected to a waste liquid tank. The steam inside the sweating and melting tank can enter the condenser through the hot steam outlet valve, thereby allowing the steam inside the condenser to cool down and become condensed water that flows into the waste liquid tank for collection.

[0008] Preferably, the condenser is arranged in an inclined shape, and a jacket III is mounted on the outside of the condenser. The two ends of the jacket III are respectively connected to the cold medium outlet II and the cold medium inlet II. The cold medium is introduced into the jacket III through the cold medium inlet II, so that the temperature of the condenser can be further reduced, and the steam inside the condenser is accelerated to become condensed water.

[0009] Preferably, a plurality of scrapers are provided at the bottom of the filter, one end of the scraper is sleeved on the outside of the output end of the third motor, the third motor is installed on the outside of the jacket I by screws, and adjacent scrapers are connected to each other by a transmission belt, and the scraper is driven to rotate by the third motor, and the scraper can clean the bottom of the filter while rotating.

[0010] Compared with the prior art, the beneficial effects of the utility model are:

[0011] 1. By adopting the melt crystallization method, the solvent impurities brought to lipoic acid by conventional recrystallization are effectively overcome. The entire device can perform continuous crystallization, greatly improving production efficiency;

[0012] 2. By using pulse nitrogen for material transportation and using hot nitrogen for the sweating process of melt crystallization, it is effectively ensured that the product will not be exposed to oxygen and deteriorate during the refining process, which greatly improves the purity of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 It is a schematic diagram of the overall structure of the utility model;

[0014] Figure 2 This is a schematic diagram of the cross-sectional structure of the utility model;

[0015] Figure 3 This is a schematic diagram of the scraper structure of the utility model;

[0016] Figure 4 This is a schematic diagram of the top view structure of the utility model;

[0017] Figure 5 It is a side structural schematic diagram of the utility model.

[0018] In the figure, 1. pulse nitrogen valve; 2. feed valve; 3. jacket Ⅰ; 4. crystallization tank; 5. cold medium inlet Ⅰ; 6. filter screen; 7. residual liquid outlet valve; 8. scraper; 9. movable plate; 10. first motor; 11. stirring paddle; 12. hot medium outlet; 13. jacket Ⅱ; 14. sweating melting tank; 15. hot nitrogen valve; 16. second motor; 17. product outlet valve; 18. hot medium inlet; 19. cold medium outlet Ⅰ; 20. hot steam outlet valve; 21. cold medium outlet Ⅱ; 22. jacket Ⅲ; 23. condenser; 24. cold medium inlet Ⅱ; 25. waste liquid tank; 26. third motor. DETAILED DESCRIPTION

[0019] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0020] Embodiment 1:

[0021] See also Figure 1-5A lipoic acid melting and refining device comprises a crystallizer 4, a filter screen 6, a sweating melting tank 14, a condenser 23 and a cold medium inlet II 24, one end of the crystallizer 4 is connected to a pulse nitrogen valve 1, the top of one end of the crystallizer 4 is connected to a feed valve 2, a jacket I 3 is mounted on the outside of the crystallizer 4, one end of the jacket I 3 is connected to a cold medium inlet I 5, the other end of the jacket I 3 is connected to a cold medium outlet I 19, a filter screen 6 is welded inside the other end of the crystallizer 4, and the other end of the crystallizer 4 is connected to a residual liquid outlet valve 7, a movable plate 9 is arranged below the filter screen 6, and the movable plate 9 is mounted on the outside of the output end of the first motor 10, and the first motor 1 0 is fixed to the outside of one side of the jacket Ⅰ3 by screws, the movable plate 9 is located at the top of the sweating melting tank 14, the top of the sweating melting tank 14 is connected with the inside of the crystallization tank 4, the bottom of the sweating melting tank 14 is respectively connected with the hot nitrogen valve 15 and the product outlet valve 17, the sweating melting tank 14 is externally sleeved with a jacket Ⅱ 13, the top and bottom sides of the jacket Ⅱ 13 are respectively connected with the hot medium outlet 12 and the hot medium inlet 18, the cold medium is introduced into the jacket Ⅰ3 to cool the crystallization tank 4, the hot medium is introduced into the jacket Ⅱ 13 to heat the sweating melting tank 14, the cold medium is introduced into the jacket Ⅲ 22 to condense the condenser 23. The molten crude lipoic acid product enters the crystallization tank 4 through the feed valve 2, the pulse nitrogen valve 1 is opened to push the material forward, the residual liquid outlet valve 7 is opened, the material is filtered through the filter screen 6, and the filtrate is discharged out of the crystallization device through the residual liquid outlet valve 7, which effectively overcomes the solvent impurities brought to lipoic acid by conventional recrystallization, and the entire device can perform continuous crystallization, greatly improving the production efficiency.

[0022] Embodiment 2:

[0023] A second motor 16 is embedded at the bottom of the sweating melting tank 14. The top output end of the second motor 16 is externally connected to a stirring paddle through a shaft. The stirring paddle 11 is arranged inside the sweating melting tank 14. The stirring paddle 11 is driven to rotate by the second motor 16, so that the solid can be stirred and heated uniformly.

[0024] Embodiment 3:

[0025] One side of the top of the sweating melting tank 14 is connected to the hot steam outlet valve 20, the hot steam outlet valve 20 is connected to one end of the condenser 23, the other end of the condenser 23 is connected to the waste liquid tank 25, the condenser 23 is arranged in an inclined shape, and the outer part of the condenser 23 is provided with a jacket III 22, and the two ends of the jacket III 22 are respectively connected to the cold medium outlet II 21 and the cold medium inlet II 24, and the steam inside the sweating melting tank 14 can enter the condenser 23 through the hot steam outlet valve 20, so that the steam inside the condenser 23 can be cooled and turned into condensed water to flow to the waste liquid tank 25 is collected inside, and cold medium is introduced into the jacket III 22 through the cold medium inlet II 24, so that the temperature of the condenser 23 can be further reduced, and the steam inside the condenser is accelerated to become condensed water; a plurality of scrapers 8 are arranged at the bottom of the filter screen 6, one end of the scraper is sleeved on the outside of the output end of the third motor 26, the third motor 26 is installed on the outside of the jacket I3 by screws, and adjacent scrapers 8 are connected to each other by transmission belt transmission, and the scrapers are driven to rotate by the third motor, and the scrapers can clean the fixings at the bottom of the filter screen while rotating.

[0026] Working principle: first close all valves, pass cold medium into jacket Ⅰ3 to cool the crystallizer 4, pass hot medium into jacket Ⅱ13 to heat the sweating melting tank 14, pass cold medium into jacket Ⅲ22 to condense the condenser 23, let the molten crude lipoic acid product enter the crystallizer 4 through the feed valve 2, open the pulse nitrogen valve 1 to push the material forward, open the residual liquid outlet valve 7, the material is filtered through the filter screen 6, and the filtrate is discharged to the outside of the crystallizer through the residual liquid outlet valve 7. When this batch of materials is filtered, the first motor 10 opens the movable plate 9 to put the filter cake into the sweating melting tank 14, at this time, the scraper 8 is driven to rotate by the third motor 26 to scrape the solid product remaining on the filter screen 6 into the sweating melting tank 14. At the same time, the second motor 16 is started to drive the stirring paddle 11 to stir and heat the solid evenly. The hot nitrogen valve 15 is opened to introduce hot nitrogen to carry the impurity vapor of crystallized sweating upward. At the same time, the hot steam outlet valve 20 is started to carry the impurity vapor out of the sweating melting tank 14, condense it through the condenser 23, and discharge it into the waste liquid tank 25. When no condensate is discharged, the product outlet valve 17 is opened to discharge the liquid purified product from the device, and condense to obtain a pure product.

[0027] The components of the utility model, 1, pulse nitrogen valve; 2, feed valve; 3, jacket I; 4, crystallization tank; 5, cold medium inlet I; 6, filter screen; 7, residual liquid outlet valve; 8, scraper; 9, movable plate; 10, first motor; 11, stirring paddle; 12, hot medium outlet; 13, jacket II; 14, sweating melting tank; 15, hot nitrogen valve; 16, second motor; 17, product outlet valve; 18, hot medium inlet; 19, cold medium outlet I; 20, hot steam outlet valve; 21, cold medium outlet II; 22, jacket III; 23, condenser; 24, cold medium inlet II; 25, waste liquid tank; 26, third motor, are all general standard parts or parts known to those skilled in the art, and their structures and principles can be known to those skilled in the art through technical manuals or conventional experimental methods.

[0028] The above shows and describes the basic principles and main features of the utility model and the advantages of the utility model. For those skilled in the art, it is obvious that the utility model is not limited to the details of the above exemplary embodiments, and can be implemented in other specific forms without departing from the spirit or basic features of the utility model. Therefore, no matter from which point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the utility model is defined by the attached claims rather than the above description, and it is intended to include all changes within the meaning and scope of the equivalent elements of the claims. Any figure mark in the claims should not be regarded as limiting the claims involved.

[0029] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A thioctic acid melting refining device, characterized in that: The invention comprises a crystallization tank (4), a filter screen (6), a sweating melting tank (14), a condenser (23) and a cold medium inlet II (24), wherein one end of the crystallization tank (4) is connected to a pulse nitrogen valve (1), the top of one end of the crystallization tank (4) is connected to a feed valve (2), a jacket I (3) is mounted on the outside of the crystallization tank (4), one end of the jacket I (3) is connected to a cold medium inlet I (5), the other end of the jacket I (3) is connected to a cold medium outlet I (19), a filter screen (6) is welded inside the other end of the crystallization tank (4), and the other end of the crystallization tank (4) is connected to a residual liquid outlet valve (7), and the filter screen (6) is below the bottom. A movable plate (9) is provided, the movable plate (9) being sleeved on the outside of the output end of the first motor (10), the first motor (10) being fixed to the outside of one side of the jacket I (3) by means of screws, the movable plate (9) being located at the top of the sweating melting tank (14), the top of the sweating melting tank (14) being connected to the inside of the crystallization tank (4), the bottom of the sweating melting tank (14) being respectively connected to the hot nitrogen valve (15) and the product outlet valve (17), the sweating melting tank (14) being sleeved on the outside with a jacket II (13), the top and bottom sides of the jacket II (13) being respectively connected to the heat medium outlet (12) and the heat medium inlet (18).

2. A thioctic acid melting and refining device according to claim 1, characterized in that: A second motor (16) is embedded at the bottom of the sweating melting tank (14); the top output end of the second motor (16) is externally connected to a stirring paddle via a shaft; and the stirring paddle (11) is arranged inside the sweating melting tank (14).

3. A thioctic acid melting and refining device according to claim 1, characterized in that: One side of the top of the sweating melting tank (14) is connected to the hot steam outlet valve (20), the hot steam outlet valve (20) is connected to one end of the condenser (23), and the other end of the condenser (23) is connected to the waste liquid tank (25).

4. A thioctic acid melting and refining device according to claim 1, characterized in that: The condenser (23) is arranged in an inclined shape, and a jacket III (22) is mounted on the outside of the condenser (23). The two ends of the jacket III (22) are respectively connected to the cold medium outlet II (21) and the cold medium inlet II (24).

5. A thioctic acid melting and refining device according to claim 1, characterized in that: A plurality of scrapers (8) are arranged at the bottom of the filter screen (6), one end of each scraper is sleeved on the outside of the output end of the third motor (26), the third motor (26) is mounted on the outside of the jacket I (3) by means of screws, and adjacent scrapers (8) are connected to each other by means of a transmission belt.

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