Rectification device suitable for separation and purification of high-melting-point material

Abstract

The utility model relates to a rectification device suitable for separating and purifying a high-melting-point material, which comprises a condenser, a rectification tower and a rectification kettle which are connected in sequence, and further comprises a gas rising pipe, the riser is sequentially provided with a first port, a second port and a third port from bottom to top, the first port is connected with a steam outlet of the rectifying still, the second port is connected with a feed port in the middle of the rectifying tower, and the third port is connected with the top of the rectifying tower. The device is novel and reasonable in structure, the steam outlet of the rectifying still is connected with the tower top of the rectifying tower by adding the riser, and steam of the rectifying still can be directly sent to the tower top by avoiding a blocked position in the rectifying tower and flows back at a bubble point after passing through the condenser; and the temperature of the reflux liquid returned into the tower is high, so that solidified materials in the tower can be directly heated and are promoted to be melted, the melting time of the high-melting-point materials in the tower is shortened, and the operation efficiency is improved.

Description

Technical field:

[0002] The utility model relates to a distillation device suitable for separating and purifying high melting point materials. Background technology:

[0004] In the production process of fine chemical fields such as medicine, flavors and fragrances, coatings, dyes and functional materials, mixed solutions containing high melting point substances often appear. The main methods for purifying high melting point materials are crystallization and distillation. The distillation of high melting point materials has the following characteristics: First, the boiling points of the components in the material are relatively high, which belongs to the distillation of high boiling point materials; second, the freezing points of the components of the material are high, which is easy to cause blockage of the condenser and pipelines, and even blockage of the filler in the tower. When the distillation device is blocked by materials, the outer wall of the tower section can be heated, and the internal parts of the tower can be heated by heat conduction to slowly melt the solidified material, but this operation takes a long time. Another way is to directly feed the tower kettle, and then heat up the rising steam in the tower to heat the solidified material and melt it, but this operation not only requires a long replacement time, but also may cause the tower kettle pressure to be too high and damage the equipment. Another way is to add solvent to the top of the tower through the top reflux pipeline to dissolve the solidified material, but this method also requires subsequent solvent separation and recovery operations, which has a long process and high energy consumption.

[0005] As market competition becomes increasingly fierce, the requirements for product purity are becoming higher and higher, and distillation will be the main technical means for product separation and purification. To this end, in view of the above problems, it is necessary to design a distillation device suitable for high melting point materials to solve the problem that the internals of the distillation tower are blocked by materials and affect normal operation. Utility model content:

[0007] The utility model makes improvements on the problems existing in the above-mentioned prior art, that is, the technical problem to be solved by the utility model is to provide a distillation device suitable for separating and purifying high melting point materials.

[0008] In order to achieve the above-mentioned purpose, the technical solution adopted by the utility model is: a distillation device suitable for separating and purifying high-melting-point materials, comprising a condenser, a distillation tower and a distillation kettle connected in sequence from top to bottom, the condenser is used to condense the top steam of the distillation tower and reflux the bubble point of the condensate into the distillation tower, and also includes a riser, the riser is provided with a first port, a second port and a third port in sequence from bottom to top, the first port is connected to the steam outlet of the distillation kettle, the second port is connected to the middle feed port of the distillation tower, and the third port is connected to the top of the distillation tower.

[0009] Furthermore, the steam outlet of the distillation kettle is located at the top of the distillation kettle and opens upward.

[0010] Furthermore, the first port, the second port and the third port of the riser are respectively provided with a first valve, a second valve and a third valve for controlling on and off.

[0011] Furthermore, a heat-insulating sleeve is provided on the outer side of the riser.

[0012] Furthermore, the distillation tower is a continuous distillation tower or a batch distillation tower.

[0013] Compared with the prior art, the utility model has the following effects: the utility model has a novel and reasonable structure, and connects the steam outlet of the distillation kettle with the top of the distillation tower by adding a riser pipe. The steam of the distillation kettle can avoid the blockage position in the distillation tower and be directly sent to the top of the tower, and then reflux at the bubble point after passing through the condenser. The reflux liquid returned to the tower has a high temperature and can directly heat the solidified material in the tower to promote its melting, thereby reducing the melting time of the high-melting-point material in the tower and improving the operating efficiency. Description of the drawings:

[0015] Figure 1 It is a schematic diagram of the structure of an embodiment of the utility model.

[0016] In the figure:

[0017] 1-distillation tower; 2-distillation kettle; 3-rising gas pipe; 4-condenser; 5-first port; 6-second port; 7-third port; 8-first valve; 9-second valve; 10-third valve. Specific implementation method:

[0019] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0020] In the description of the present invention, it should be understood that the terms "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside" and "outside" etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0021] like Figure 1As shown, the utility model is a distillation device suitable for separating and purifying high melting point materials, wherein the high melting point compound refers to a compound with a melting point of 40°C to 120°C, and the distillation device comprises a condenser 4, a distillation tower 1 and a distillation kettle 2 which are sequentially connected from top to bottom, the condenser 4 is used to condense the top steam of the distillation tower 1 and make the condensate reflux into the distillation tower in the form of bubble point reflux, which is the prior art; the specific improvement of the distillation device is that it also includes a riser 3 arranged on the side of the distillation tower, and the riser 3 is sequentially provided with a first port 5, a second port 6 and a third port 7 from bottom to top, the first port 5 is connected to the steam outlet of the distillation kettle 2, the second port 6 is connected to the middle feed port of the distillation tower 1, and the third port 7 is connected to the top of the distillation tower 1. The steam outlet of the distillation kettle is connected to the top of the distillation tower through a riser. The steam from the distillation kettle can avoid the blockage position in the distillation tower and be directly sent to the top of the tower. After passing through the condenser, it refluxes at the bubble point. The reflux liquid returned to the tower has a high temperature and can directly heat the solidified materials in the tower to promote their melting, thereby reducing the melting time of high-melting-point materials in the tower and improving operating efficiency.

[0022] In this embodiment, the riser connects the steam outlet of the distillation kettle with the top and middle feed inlet of the distillation tower. When in use, the steam is output by switching different ports (the second port or the third port) of the riser, so that the theoretical plate number of the distillation tower can be flexibly adjusted.

[0023] It should be noted that the structure consisting of the condenser, distillation tower and distillation kettle is the existing technology. During normal operation, the steam in the distillation kettle enters from the bottom of the distillation tower, passes through the internals of the distillation tower and enters the condenser connected to the top of the tower. No further repetition will be made here.

[0024] In this embodiment, the steam outlet of the distillation kettle 2 is located at the top of the distillation kettle 2 and opens upward.

[0025] In this embodiment, the first port 5, the second port 6 and the third port 7 of the riser 3 are respectively provided with a first valve 8, a second valve 9 and a third valve 10 for controlling the opening and closing of the ports. When in use, the riser can be flexibly switched to communicate with the middle part or the top of the distillation tower as needed.

[0026] In this embodiment, the outer side of the riser 3 is provided with an insulation sleeve (not shown in the figure), which plays a role of insulation to prevent the high melting point material vapor from solidifying and blocking the pipeline when it contacts the outer wall of the riser.

[0027] In this embodiment, the distillation tower may be a continuous distillation tower or a batch distillation tower.

[0028] Example 1

[0029] The reaction liquid of isopulegol hydrogenation to produce menthol contains the following components and their mass percentages: 93.95% menthol, 3.85% isopulegol and 2.20% unknown impurities. The purpose of distillation separation is to separate the menthol reaction liquid to obtain menthol with a purity of more than 99%. Since the melting point of menthol is 44°C and the melting point of isopulegol is 90°C, both of them are easy to solidify and block the pipeline and the filler in the tower at room temperature, so the filler of the distillation tower needs to be dredged before separation and purification. 296.3g of menthol reaction liquid was added to the distillation kettle, and the vacuum was turned on. The experimental vacuum degree was set to 30mbar; the distillation kettle was turned on for heating, the heating temperature was 165°C, the valves of the first and third ports of the riser were opened, and the insulation temperature of the riser was 110°C. The steam output from the distillation kettle was directly sent to the top of the distillation tower. The steam at the top of the distillation tower changes phase after passing through the condenser, and the condensate returns to the distillation tower in the form of bubble point reflux. When it flows through the blocked position in the tower, it directly heats the solidified material. After running for 10 minutes, the steam in the riser decreases, and most of the rising steam in the distillation kettle enters the top condenser through the internals of the distillation tower, which indicates that the blocked materials in the tower have all melted. Close the valves of the first and third ports of the riser, and continue to reflux for 15 minutes to ensure that all the high-boiling-point substances remaining in the tower are replaced. The extraction is carried out at a reflux ratio of 15. At this time, the top temperature of the distillation tower is 97.7℃, the bottom temperature of the distillation tower is 126.1℃, and the composition of the produced liquid is 35.219% menthol and 46.246% isopulegol. After 69.43g of transition components were extracted from the top of the tower, the reflux ratio was 5. At this time, the top temperature of the distillation tower was 111.8℃, the bottom temperature was 127.2℃, and the composition of the extracted liquid was 99.461% menthol and 0.463% isopulegol. After the experiment, a total of 179.51g of qualified menthol was obtained.

[0030] Example 2

[0031] The raw material liquid to be separated contains the following components and their mass percentages: 2,4-difluorochlorobenzene 22.51%, 2,6-difluorochlorobenzene 66.04%. The purpose of distillation and purification is to separate the raw material liquid to obtain 2,6-difluorochlorobenzene with a purity of more than 99%. Since the melting point of 2,6-difluorochlorobenzene is 40°C, the material solidifies and blocks the filler in the tower after the previous batch of separation and purification operations. Therefore, the filler of the distillation tower needs to be dredged before starting distillation. Add 513.9g of raw material liquid to the distillation kettle, turn on the vacuum, set the experimental vacuum degree to 50mbar, turn on the distillation kettle heating, the heating temperature is 130°C, open the valves of the first and third ports of the riser, the riser insulation temperature is 100°C, and the steam output from the distillation kettle is directly sent to the top of the distillation tower. The steam at the top of the distillation tower undergoes a phase change after passing through the condenser, and the condensate returns to the tower in the form of bubble point reflux, and directly heats the solidified material when flowing through the blocked position in the tower. After running for 8 minutes, the steam in the riser pipe decreased, and most of the rising steam in the distillation kettle entered the top condenser through the internals of the distillation tower, indicating that the blocked materials in the tower have been completely melted. Close the valves of the first and third ports of the riser pipe and continue full reflux for 15 minutes. Then the reflux ratio is 20 for extraction. At this time, the top temperature of the distillation tower is 75.5 ℃, the bottom temperature of the distillation tower is 92.2 ℃, and the composition of the produced liquid is 85.35% of 2,4-difluorochlorobenzene and 14.62% of 2,6-difluorochlorobenzene. After 212.68g of transition components were extracted from the top of the tower, the reflux ratio was 30 for extraction. At this time, the top temperature of the tower was 83.7 ℃, the bottom temperature of the tower was 106.9 ℃, and the composition of the produced liquid was 99.42% of 2,6-difluorochlorobenzene and 0.45% of 2,4-difluorochlorobenzene. After the distillation, a total of 217.89g of qualified 2,6-difluorochlorobenzene was obtained.

[0032] Example 3

[0033] The raw material liquid to be separated contains the following components: a small amount of light component impurities, 50% naphthalene, and the remaining material is lubricating oil. The purpose of the experiment is to separate the lubricating oil and naphthalene in the raw material and obtain qualified lubricating oil. Since the melting point of naphthalene is 80°C, the residual naphthalene material after the previous batch of separation and purification operations solidifies and blocks the filler in the tower, so the filler of the distillation tower needs to be dredged before the distillation starts. 1083.77g of raw material liquid is added to the distillation kettle, the vacuum is turned on, the experimental vacuum is set to 20mbar, the distillation kettle is turned on for heating, the heating temperature is 300°C, the valves at the first and third ports of the riser are opened, the riser insulation temperature is 200°C, and the steam output from the distillation kettle is directly sent to the top of the distillation tower. The top steam undergoes a phase change after passing through the condenser, and the condensate returns to the distillation tower in the form of bubble point reflux, and directly heats the solidified material when flowing through the blocked position in the tower. After 10 minutes of operation, the steam in the riser pipe decreased, and most of the rising steam in the distillation kettle entered the top condenser through the tower internals, indicating that the blocked materials in the tower have all melted. Close the valves of the first and third ports of the riser pipe, and continue the full reflux operation for 10 minutes. Then, the reflux ratio was 5, the top temperature of the distillation tower was 218.6℃, and 223.5g of naphthalene was produced. After the naphthalene was produced, the top temperature of the tower rose to 283.2℃, and the lubricating oil continued to be produced until there was no material produced at the top of the tower. After the experiment, a total of 223.5g of qualified lubricating oil was obtained.

[0034] If the present invention discloses or involves components or structures that are fixedly connected to each other, then, unless otherwise stated, the fixed connection can be understood as: a detachable fixed connection (for example, connection using bolts or screws), and can also be understood as: a non-detachable fixed connection (for example, riveting, welding). Of course, the mutual fixed connection can also be replaced by an integrated structure (for example, manufactured by one-piece molding using a casting process) (except where it is obviously impossible to use an one-piece molding process).

[0035] In addition, unless otherwise stated, the terms used to indicate positional relationships or shapes in any of the technical solutions disclosed in the above utility model include states or shapes that are approximate, similar or close thereto.

[0036] Any component provided by the utility model can be assembled from multiple separate components, or can be a separate component manufactured by an integrated molding process.

[0037] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the utility model rather than to limit it. Although the utility model has been described in detail with reference to the preferred embodiments, ordinary technicians in the relevant field should understand that the specific implementation methods of the utility model can still be modified or some technical features can be replaced by equivalents without departing from the spirit of the technical solution of the utility model, which should be included in the scope of the technical solution for protection of the utility model.

Claims

1. A distillation device suitable for separation and purification of high melting point materials, comprising a condenser, a distillation tower and a distillation kettle connected in sequence from top to bottom, the condenser is used to condense the top steam of the distillation tower and reflux the condensate bubble point into the distillation tower, characterized in that: It also includes a riser, which is provided with a first port, a second port and a third port in sequence from bottom to top, the first port is connected to the steam outlet of the distillation kettle, the second port is connected to the middle feed port of the distillation tower, and the third port is connected to the top of the distillation tower.

2. A distillation device suitable for separation and purification of high melting point materials according to claim 1, characterized in that: The steam outlet of the rectification kettle is located at the top of the rectification kettle and opens upward.

3. A distillation device suitable for separation and purification of high melting point materials according to claim 1, characterized in that: The first port, the second port and the third port of the riser are respectively provided with a first valve, a second valve and a third valve for controlling on and off.

4. A distillation device suitable for separation and purification of high melting point materials according to claim 1, characterized in that: The outer side of the riser is sleeved with a heat-insulating sleeve.

5. A distillation device suitable for separation and purification of high melting point materials according to claim 1, characterized in that: The distillation tower is a continuous distillation tower or a batch distillation tower.

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