Lipoic acid preparation device

Abstract

The utility model discloses a lipoic acid preparation device, which relates to the technical field of synthesis and comprises a cold medium inlet, a cold medium outlet, a paddle and a reaction kettle, a jacket is sleeved outside the reaction kettle, the top of one end of the jacket is communicated with the cold medium inlet, and the top of the other end of the jacket is communicated with the cold medium outlet. A vacuum valve is arranged on one side of the cold medium inlet, air can be discharged out of a reaction system by ventilating the reaction kettle, and a reducing gas sulfur dioxide is added, so that the generation of impurities can be reduced, and a by-product ethyl 1, 2, 3-trithiahexane-4-valerate can be directly reduced into lipoic acid in the reaction process. According to the method, the reaction steps are greatly simplified, the yield and the purity of the product are improved, the reaction can be completed at a lower temperature in a short time (within 1 hour) through the ball-milling reaction in combination with a cooling environment, and the generation of by-products can be reduced due to the low temperature.

Description

Technical Field

[0001] The utility model relates to the technical field of synthesis, in particular to a device for preparing thioctic acid. Background Art

[0002] Lipoic acid, due to its disulfide five-membered ring structure, possesses significant electrophilicity and free radical-attacking abilities, enabling it to directly eliminate harmful hydroxyl and hydrogen radicals in aqueous solution. Consequently, lipoic acid plays a crucial role in various biochemical processes, including the treatment of liver dysfunction, subacute necrotizing encephalopathy, neurological diseases, radiation damage, and heavy metal poisoning such as arsenic, cadmium, and mercury. It is known as a "universal antioxidant." Furthermore, lipoic acid is widely used in biological research, cosmetics, and photography. Its synthesis is attracting increasing attention.

[0003] The main industrial preparation method for lipoic acid today is the adipic acid method, which uses adipic acid to prepare 6,8-dichlorooctanoic acid ethyl ester. This is then reacted at high temperature for a long time using toluene as a solvent and Na2S / S as a sulfiding agent to obtain lipoic acid ethyl ester. However, this process presents many problems, such as the large amount of toluene added, the long reaction time (over 5 hours), and low production efficiency. During the reaction, a byproduct, 1,2,3-trithiane-4-pentanoic acid ethyl ester, is produced. Therefore, after the reaction is completed, sodium sulfite must be added for further impurity removal, which is a cumbersome step and affects product yield. The presence of oxygen can also lead to the appearance of other impurities in the reaction, affecting product quality.

[0004] Therefore, for the problems referred to above, a kind of thioctic acid preparation device is proposed Utility Model Content

[0005] In view of the deficiencies in the prior art, the present invention provides a device for preparing lipoic acid, which solves the problems raised in the background technology.

[0006] To achieve the above objectives, the present invention is implemented through the following technical solutions: a thioctic acid preparation device, comprising a cold medium inlet, a cold medium outlet, a paddle and a reactor, the reactor being externally sheathed with a jacket, the top of one end of the jacket being connected to the cold medium inlet, and the top of the other end of the jacket being connected to the cold medium outlet, a vacuum valve being provided on one side of the cold medium inlet, the bottom of the vacuum valve being connected to the interior of the reactor, a toluene valve being provided on one side of the vacuum valve, the toluene valve being connected to the ethyl dichlorooctanoate valve and the interior of the reactor respectively, a solid feeding valve being provided on one side of the ethyl dichlorooctanoate valve, the bottom of the solid feeding valve being connected to the interior of the reactor, a sulfur dioxide valve being provided on one side of the solid feeding valve, the sulfur dioxide valve being connected to the hot air valve and the interior of the reactor respectively, and the bottom of the reactor being connected to the bottom valve.

[0007] Preferably, a motor is installed at one end of the reactor by screws, a main shaft is mounted on the outside of the motor output end, paddles are distributed on the outside of the main shaft, and a plurality of grinding balls are arranged at the bottom end of the reactor. The grinding balls are driven by the paddles to move in the reactor, which is conducive to improving the reaction efficiency.

[0008] Preferably, an arc-shaped groove is provided at the bottom of the reactor, and a perforated plate is welded on the top of the arc-shaped groove at the bottom of the reactor. The perforated plate is arc-shaped. When air enters the groove at the bottom of the reactor, it will pass through the perforated plate and rise inside the reactor, thereby performing aeration, which is beneficial to further improve the reaction efficiency.

[0009] Preferably, one side of the bottom of the reactor is connected to one end of the bottom of the connecting pipe, one end of the top of the connecting pipe is connected to the air pump, one end of the bottom of the air pump is connected to the top of the air tank, and the bottom of the air tank is connected to the top of the reactor. After rising inside the reactor, the air will enter the air tank and then be pumped into the bottom of the reactor again through the air pump and the connecting pipe, thereby performing continuous aeration and greatly improving the reaction rate.

[0010] Preferably, the blades are distributed in an annular shape at equal intervals outside the main shaft, and one end of the blade is L-shaped, and one end of the blade is in contact with the grinding ball, which is conducive to the blade driving the grinding ball to move while stirring the material.

[0011] In this scheme, ethyl dichlorooctanoate is ethyl 6,8-dichlorooctanoate

[0012] The utility model provides a device for preparing lipoic acid, which has the following beneficial effects:

[0013] (1) The thioctic acid preparation device can exhaust air from the reaction system by ventilating the reactor and adding reducing gas sulfur dioxide to reduce the generation of impurities. During the reaction process, the by-product, 1,2,3-trithiahexane-4-pentanoic acid ethyl ester, can be directly reduced to thioctic acid, which greatly simplifies the reaction steps and improves the yield and purity of the product.

[0014] (2) The lipoic acid preparation device can complete the reaction in a short time (within 1 hour) at a relatively low temperature through ball milling reaction and in combination with a cooling environment. Due to the low temperature, the generation of by-products can also be reduced. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 This is a schematic diagram of the overall structure of the utility model;

[0016] Figure 2 This is a schematic diagram of the internal structure of the utility model;

[0017] Figure 3This is a schematic diagram of the orifice plate structure of the utility model;

[0018] Figure 4 This is a schematic diagram of the top view of the structure of the utility model;

[0019] Figure 5 It is a side view structural diagram of the utility model.

[0020] In the figure, 1. cold medium inlet; 2. jacket; 3. vacuum valve; 4. toluene valve; 5. ethyl dichlorooctanoate valve; 6. solid feeding valve; 7. sulfur dioxide valve; 8. hot air valve; 9. cold medium outlet; 10. motor; 11. main shaft; 12. paddle; 13. grinding ball; 14. bottom valve; 15. air chamber; 16. air pump; 17. connecting pipe; 18. reactor; 19. orifice plate. DETAILED DESCRIPTION

[0021] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described 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 are within the scope of protection of the present invention.

[0022] Example 1:

[0023] See also Figure 1-5 A thioctic acid preparation device includes a cold medium inlet 1, a cold medium outlet 9, a paddle 12 and a reactor 18. The reactor 18 is externally covered with a jacket 2. The top of one end of the jacket 2 is connected to the cold medium inlet 1, and the top of the other end of the jacket 2 is connected to the cold medium outlet 9. A vacuum valve 3 is provided on one side of the cold medium inlet 1. The bottom of the vacuum valve 3 is connected to the interior of the reactor 18. A toluene valve 4 is provided on one side of the vacuum valve 3. The toluene valve 4 is connected to the ethyl dichlorooctanoate valve 5 and the interior of the reactor 18 respectively. A solid feeding valve 6 is provided on one side of the ethyl dichlorooctanoate valve 5. 6 is connected to the interior of the reactor 18, and a sulfur dioxide valve 7 is provided on one side of the solid feeding valve 6. The sulfur dioxide valve 7 is connected to the hot air valve 8 and the interior of the reactor 18 respectively. The bottom of the reactor 18 is connected to the bottom valve 14. By ventilating the reactor 18, air can be discharged from the reaction system, and the reducing gas sulfur dioxide is added to reduce the generation of impurities. During the reaction process, the by-product - 1,2,3-trithiahexane-4-pentanoic acid ethyl ester can be directly reduced to lipoic acid, which greatly simplifies the reaction steps and improves the yield and purity of the product.

[0024] Example 2:

[0025] The blades 12 are distributed in a circular shape with equal intervals outside the main shaft 11, and one end of the blade 12 is L-shaped, and one end of the blade 12 is in contact with the grinding ball 13. A motor 10 is installed at one end of the reactor 18 by screws, and the main shaft 11 is mounted on the outside of the output end of the motor 10. The blades 12 are distributed on the outside of the main shaft 11. A plurality of grinding balls 13 are provided at the bottom end of the reactor 18. The main shaft 11 is driven to rotate by the motor 10, which is conducive to the blades 12 driving the grinding balls 13 to move while stirring the material. Through the reaction of the grinding balls 13 and in combination with the cooling environment, the reaction can be completed at a lower temperature in a short time (within 1 hour). Due to the low temperature, the generation of by-products can also be reduced.

[0026] Example 3:

[0027] An arc-shaped groove is provided at the bottom of the reactor 18, and a orifice plate 19 is welded to the top of the arc-shaped groove at the bottom of the reactor 18. The orifice plate 19 is arc-shaped. One side of the bottom of the reactor 18 is connected to one end of the bottom of the connecting pipe 17, and one end of the top of the connecting pipe 17 is connected to the air pump 16. One end of the bottom of the air pump 16 is connected to the top of the air tank 15, and the bottom of the air tank 15 is connected to the top of the reactor 18. When the air enters the groove at the bottom of the reactor 18, it will pass through the orifice plate 19 and rise inside the reactor 18, thereby performing aeration, which is beneficial to further improve the reaction efficiency. After rising inside the reactor 18, the air will enter the air tank 15, and then be pumped into the bottom of the reactor 18 again through the air pump 16 and the connecting pipe 17, thereby performing continuous aeration, which greatly improves the reaction rate.

[0028] Working Principle: By ventilating the reactor 18, air can be discharged from the reaction system, and the addition of reducing gas sulfur dioxide can reduce the generation of impurities. During the reaction process, the by-product, 1,2,3-trithiahexane-4-pentanoic acid ethyl ester, can be directly reduced to lipoic acid, which greatly simplifies the reaction steps and improves the yield and purity of the product. The motor 10 drives the main shaft 11 to rotate, which is conducive to enabling the blades 12 to drive the grinding balls 13 to move while stirring the materials. Through the reaction of the grinding balls 13, combined with the cooling environment, the reaction can be completed at a relatively low temperature in a short time (within 1 hour). Due to the low temperature, the generation of by-products can also be reduced. When the air enters the groove at the bottom of the reactor 18, it will pass through the orifice plate 19 and rise inside the reactor 18, thereby aerating, which is conducive to further improving the reaction efficiency. After rising inside the reactor 18, the air will enter the air chamber 15 and then be pumped back to the bottom of the reactor 18 through the air pump 16 and the connecting pipe 17, thereby continuously aerating, greatly improving the reaction rate.

[0029] The components of the utility model, 1. cold medium inlet; 2. jacket; 3. vacuum valve; 4. toluene valve; 5. ethyl dichlorooctanoate valve; 6. solid feeding valve; 7. sulfur dioxide valve; 8. hot air valve; 9. cold medium outlet; 10. motor; 11. main shaft; 12. paddle; 13. grinding ball; 14. bottom valve; 15. gas chamber; 16. air pump; 17. connecting pipe; 18. reactor; 19. orifice plate, are all universal standard parts or components 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.

[0030] The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention. For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and that the present invention can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention. Therefore, no matter from which point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, it is intended that all changes that fall within the meaning and range of equivalents of the claims are included in the present invention. Any reference signs in the claims should not be construed as limiting the claim to which they relate.

[0031] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method 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 can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A thioctic acid preparation device, characterized in that: The invention comprises a cold medium inlet (1), a cold medium outlet (9), a paddle (12) and a reaction kettle (18); the reaction kettle (18) is externally provided with a jacket (2); the top of one end of the jacket (2) is connected to the cold medium inlet (1); the top of the other end of the jacket (2) is connected to the cold medium outlet (9); a vacuum valve (3) is arranged on one side of the cold medium inlet (1); the bottom of the vacuum valve (3) is connected to the inside of the reaction kettle (18); a toluene valve (4) is arranged on one side of the vacuum valve (3); The toluene valve (4) is communicated with the (6), (8)-ethyl dichlorooctanoate valve (5) and the interior of the reactor (18) respectively; a solid feeding valve (6) is arranged on one side of the ethyl dichlorooctanoate valve (5); the bottom of the solid feeding valve (6) is communicated with the interior of the reactor (18); a sulfur dioxide valve (7) is arranged on one side of the solid feeding valve (6); the sulfur dioxide valve (7) is communicated with the hot air valve (8) and the interior of the reactor (18) respectively; the bottom of the reactor (18) is communicated with the bottom valve (14).

2. A thioctic acid preparation device according to claim 1, characterized in that: A motor (10) is mounted on one end of the reactor (18) by means of screws, a main shaft (11) is mounted on the outside of the output end of the motor (10), blades (12) are distributed on the outside of the main shaft (11), and a plurality of grinding balls (13) are arranged at the bottom of the reactor (18).

3. A thioctic acid preparation device according to claim 1, characterized in that: The bottom of the reaction kettle (18) is provided with an arc-shaped groove, and a perforated plate (19) is welded on the top of the arc-shaped groove at the bottom of the reaction kettle (18), and the perforated plate (19) is in an arc shape.

4. A thioctic acid preparation device according to claim 1, characterized in that: One side of the bottom of the reaction kettle (18) is connected to one end of the bottom of the connecting pipe (17), one end of the top of the connecting pipe (17) is connected to the air pump (16), one end of the bottom of the air pump (16) is connected to the top of the air bin (15), and the bottom of the air bin (15) is connected to the top of the reaction kettle (18).

5. A thioctic acid preparation device according to claim 1, characterized in that: The blades (12) are distributed outside the main shaft (11) in an annular shape with equal spacing, and one end of the blade (12) is in an L-shaped structure, and one end of the blade (12) is in contact with the grinding ball (13).

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