Multistage continuous fractionation device for synthesizing vitamin B6 intermediate

Abstract

The utility model provides a multi-stage continuous fractionation device for synthesizing a vitamin B6 intermediate, and belongs to the technical field of compound synthesis equipment. Comprising a hollow rotating drum, an inner drum coaxial with the rotating drum is arranged in the rotating drum, the inner drum and the rotating drum are integrally formed, a rotating shaft is fixedly arranged in the inner drum, a spiral partition plate located in the rotating drum is arranged outside the inner drum, an intermittent feeding structure is arranged at one end of the rotating drum, at least one intermittent discharging structure is arranged outside the rotating drum in a spaced mode, and the rotating shaft is connected with a power source. The rotating drum is rotationally connected to a rack, the liquid level height in the rotating drum is larger than the difference between the outer diameter of the inner drum and the inner diameter of the outer drum, and the liquid level height in the rotating drum is smaller than the radius of the rotating drum; the intermittent discharging structure comprises a sleeve rotationally connected to the outer wall of the rotary drum, the sleeve is fixedly connected with the rack, the top of the sleeve is provided with an exhaust connecting pipe, the bottom of the sleeve is provided with a liquid discharging connecting pipe, the rotary drum is provided with discharging holes, and the discharging holes can be intermittently communicated with the exhaust connecting pipe and the liquid discharging connecting pipe. The device has the advantages of high efficiency and the like.

Description

Technical Field

[0001] The utility model belongs to the technical field of compound synthesis equipment and relates to a multi-stage continuous fractionation device for synthesizing a vitamin B6 intermediate. Background Art

[0002] The production process of vitamin B6 intermediate N-ethoxyoxalyl-L-alanine ethyl ester requires the fractionation of ethanol and diethyl oxalate one by one, and the mixed material in the reactor needs to be heated and pressure-controlled twice, and then the bottom material is discharged and refilled. In order to reduce the frequency of filling, improve heat utilization and maintain pressure, the single filling should not be too little, and more materials will inevitably lead to low distillation purity and low distillation efficiency.

[0003] At the same time, in the synthesis of other compounds, there are also situations where substances with different boiling points are separated one by one, and this scheme can also be applied. Utility Model Content

[0004] The purpose of the utility model is to provide a multi-stage continuous distillation device for synthesizing a vitamin B6 intermediate in view of the above-mentioned problems existing in the prior art. The technical problem to be solved by the utility model is how to realize continuous multi-stage distillation.

[0005] The purpose of the utility model can be achieved through the following technical solutions: a multi-stage continuous fractionation device for synthesizing vitamin B6 intermediates, characterized in that it includes a hollow rotating drum, an inner drum coaxial with the rotating drum is provided in the rotating drum, the inner drum and the rotating drum are integrally formed, a rotating shaft is fixedly arranged in the inner drum, a spiral partition plate is provided outside the inner drum and located in the rotating drum, one end of the rotating drum has an intermittent feeding structure, at least one intermittent discharging structure is alternately arranged outside the rotating drum, the rotating shaft is connected to a power source, the rotating drum is rotatably connected to a frame, the rotating drum is horizontally placed, the liquid level in the rotating drum is higher than the difference between the outer diameter of the inner drum and the inner diameter of the outer drum, and the liquid level in the rotating drum is lower than the radius of the rotating drum; the intermittent discharging structure includes a sleeve rotatably connected to the outer wall of the rotating drum, the sleeve is fixedly connected to the frame, the top of the sleeve has an exhaust pipe, the bottom of the sleeve has a drainage pipe, and the rotating drum has a discharge hole, and the discharge hole can be intermittently connected to the exhaust pipe and the drainage pipe.

[0006] Furthermore, the intermittent feeding structure is a feeding pump.

[0007] As another option, the intermittent feeding structure includes a material box fixed on the frame, the rotating drum is rotatably connected to the material box, the material box is provided with a material pipe, a temporary storage tube is slidably connected to the material tube along the radial direction of the rotating drum, the top of the temporary storage tube is sealed, the side wall of the temporary storage tube is provided with a feeding hole, the lower end of the temporary storage tube is provided with a one-way valve, the rotating drum is provided with a guide ring eccentric to the rotating drum, the lowest point of the guide ring is provided with a feeding port connected to the inner cavity of the rotating drum, and the valve block of the one-way valve is against the outer peripheral surface of the guide ring.

[0008] The essence of this scheme is that a liquid storage area is formed between adjacent circles of the partition plates in the rotating drum, and adjacent liquid storage areas are separated under the treatment of the liquid level setting. Specifically, the liquid level is higher than the bottom of the inner drum and lower than the top of the inner drum, so that the outer peripheral surface of the inner drum and the spiral partition plate complete the isolation of each liquid storage area, and the mixed material to be distilled is spread in small quantities and multiple areas. In addition, this scheme is positive pressure distillation, and the pressure is generated because the volatile substances in each liquid storage area exist above the liquid surface. Therefore, it is not difficult to see that compared with the traditional distillation method, this scheme distributes the material, increases the heating surface and the bubble escape surface, and also realizes continuous feeding and discharging. For positive pressure distillation, no pressure source is required, and the positive pressure distillation is realized by utilizing the principle that the gas storage space between adjacent liquid storage areas is separated and the gas pressure increases after heating. BRIEF DESCRIPTION OF THE DRAWINGS

[0009] Figure 1 It is a structural schematic diagram of the multi-stage continuous distillation device.

[0010] Figure 2 yes Figure 1 Cross-sectional view along CC direction.

[0011] Figure 3 yes Figure 1 Enlarged view of part A in the figure.

[0012] Figure 4 yes Figure 1 Enlarged view of part B in the middle.

[0013] In the figure, 1, rotating drum; 2, inner drum; 3, rotating shaft; 4, partition plate; 5, sleeve; 6, exhaust pipe; 7, drain pipe; 8, discharge hole; 9, material box; 10, material pipe; 11, temporary storage pipe; 12, feed hole; 13, one-way valve; 14, guide ring; 15, feed port. DETAILED DESCRIPTION

[0014] The following are specific embodiments of the present invention and the accompanying drawings to further describe the technical solution of the present invention, but the present invention is not limited to these embodiments.

[0015] like Figure 1-Figure 4As shown, it includes a hollow drum 1, wherein the drum 1 has an inner drum 2 coaxial with the drum 1, the inner drum 2 and the drum 1 are integrally formed, a rotating shaft 3 is fixedly arranged in the inner drum 2, and a spiral partition plate 4 is arranged outside the inner drum 2 and located inside the drum 1, one end of the drum 1 has an intermittent feeding structure, at least one intermittent discharging structure is arranged alternately outside the drum 1, and a heating unit located outside the drum 1 is arranged between adjacent intermittent discharging structures, and the heating unit can control the temperature of different areas, and a heating element is also arranged in the rotating shaft 3, and the heating element provides basic heating for the material in the drum 1, and the internal and external heating method is The method improves the controllability of temperature. The rotating shaft 3 is connected to the power source, which is a motor. The motor is arranged on the frame and connected to the rotating shaft 3 through a pulley. The rotating drum 1 is horizontally placed. The liquid level in the rotating drum 1 is higher than the difference between the outer diameter of the inner drum 2 and the inner diameter of the outer drum, and the liquid level in the rotating drum 1 is lower than the radius of the rotating drum 1. The intermittent discharge structure includes a sleeve 5 rotatably connected to the outer wall of the rotating drum 1, the sleeve 5 is fixedly connected to the frame, the top of the sleeve 5 is provided with an exhaust pipe 6, the bottom of the sleeve 5 is provided with a drainage pipe 7, and the rotating drum 1 is provided with a discharge hole 8, which can be intermittently connected to the exhaust pipe 6 and the drainage pipe 7.

[0016] Furthermore, the intermittent feeding structure is a feeding pump, and the feeding pump controls the feeding in an intermittent feeding manner.

[0017] like Figure 2 and Figure 3 As shown, the intermittent feeding structure includes a material box 9 fixed on the frame, and the rotating drum 1 is rotatably connected to the material box 9. A material pipe 10 is arranged in the material box 9, and a temporary storage tube 11 is slidably connected in the material tube 10 along the radial direction of the rotating drum 1. The top of the temporary storage tube 11 is sealed, and a feeding hole 12 is provided on the side wall of the temporary storage tube 11. A one-way valve 13 is provided at the lower end of the temporary storage tube 11. The rotating drum 1 is provided with a guide ring 14 eccentric to the rotating drum 1, and the lowest point of the guide ring 14 is provided with a feeding port 15 connected to the inner cavity of the rotating drum 1, and the valve block of the one-way valve 13 is against the outer peripheral surface of the guide ring 14. The principle is as follows: during the rotation of the drum 1, the outer peripheral surface of the guide ring 14 in the eccentric position can change the distance between the one-way valve 13 and the outer peripheral surface during the rotation of the drum 1. A ball is hinged on the valve block of the one-way valve 13, which can reduce the friction between the one-way valve 13 and the guide ring 14. When the one-way valve 13 abuts against the guide ring 14, the one-way valve 13 is closed. As the temporary storage tube 11 rises, the feed hole 12 on the temporary storage tube 11 gradually breaks away from the wrapping of the material pipe 10 until it is connected with the material box 9. The material in the material box 9 can enter the temporary storage tube 11. The drum 1 continues to rotate, and the feed hole 12 is gradually closed. The material in the temporary storage tube 11 is enclosed in the temporary storage tube 11. When the guide ring 14 is at the lowest point, there is a gap between the valve block of the one-way valve 13 and the outer wall of the guide ring 14. The one-way valve 13 is opened, and the material in the temporary storage tube 11 can enter the drum 1 through the feed port 15. This is repeated to achieve intermittent feeding.

[0018] The essence of this scheme is that a liquid storage area is formed between adjacent circles of the partition plates 4 in the rotating drum 1, and adjacent liquid storage areas are separated under the treatment of the liquid level setting. Specifically, the liquid level is higher than the bottom of the inner drum 2 and lower than the top of the inner drum 2, so that the outer peripheral surface of the inner drum 2 and the spiral partition plate 4 complete the isolation of each liquid storage area, and the mixed material to be distilled is spread in small quantities and multiple areas. In addition, this scheme is positive pressure distillation, and the pressure is generated because the volatile substances in each liquid storage area exist above the liquid surface. Therefore, it is not difficult to see that compared with the traditional distillation method, this scheme distributes the material, increases the heating surface and the bubble escape surface, and also realizes continuous feeding and discharging. For positive pressure distillation, no pressure source is required, and the positive pressure distillation is realized by utilizing the principle that the gas storage space between adjacent liquid storage areas is separated and the gas pressure increases after heating.

[0019] The specific embodiments described herein are merely examples of the spirit of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in similar ways, but they will not deviate from the spirit of the present invention or exceed the scope defined by the appended claims.

Claims

1. A multi-stage continuous fractionation device for synthesizing a vitamin B6 intermediate, characterized in that: The invention comprises a hollow drum (1), wherein the drum (1) has an inner drum (2) coaxial with the drum (1), the inner drum (2) and the drum (1) are integrally formed, a rotating shaft (3) is fixedly arranged inside the inner drum (2), the inner drum (2) has a spiral partition plate (4) located inside the drum (1), one end of the drum (1) has an intermittent feeding structure, the drum (1) is provided with at least one intermittent discharging structure at intervals, the rotating shaft (3) is connected to a power source, the drum (1) is rotatably connected to a frame, and the drum (1) is transversely The rotary drum (1) is provided with a liquid level higher than the difference between the outer diameter of the inner drum (2) and the inner diameter of the outer drum, and the liquid level higher than the radius of the rotary drum (1); the intermittent discharge structure comprises a sleeve (5) rotatably connected to the outer wall of the rotary drum (1), the sleeve (5) being fixedly connected to the frame, the top of the sleeve (5) being provided with an exhaust pipe (6), the bottom of the sleeve (5) being provided with a liquid discharge pipe (7), the rotary drum (1) being provided with a discharge hole (8), the discharge hole (8) being capable of intermittently communicating with the exhaust pipe (6) and the liquid discharge pipe (7).

2. A multi-stage continuous fractionation device for synthesizing a vitamin B6 intermediate according to claim 1, characterized in that: The intermittent feeding structure is a feeding pump.

3. A multi-stage continuous fractionation device for synthesizing a vitamin B6 intermediate according to claim 1, characterized in that: The intermittent feeding structure comprises a material box (9) fixed on a frame, the rotating drum (1) is rotatably connected to the material box (9), a material pipe (10) is provided in the material box (9), a temporary storage pipe (11) is slidably connected in the material pipe (10) along the radial direction of the rotating drum (1), the top of the temporary storage pipe (11) is sealed, a feeding hole (12) is provided on the side wall of the temporary storage pipe (11), a one-way valve (13) is provided at the lower end of the temporary storage pipe (11), the rotating drum (1) is provided with a guide ring (14) eccentric to the rotating drum (1), the lowest point of the guide ring (14) is provided with a feeding port (15) connected to the inner cavity of the rotating drum (1), and the valve block of the one-way valve (13) is against the outer peripheral surface of the guide ring (14).

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