CN118750893A - Ultra-gravity separation device for solvent purification and control method thereof - Google Patents

Abstract

The present invention provides an ultra-gravity separation device for solvent purification and a control method thereof, the ultra-gravity separation device comprising a shell, a static baffle, and a dynamic baffle, etc. The static baffle comprises: a static baffle connected to the shell, a plurality of first partitions connected to the static baffle and arranged at intervals; the dynamic baffle comprises: a dynamic baffle rotating with a rotating shaft, a plurality of second partitions connected to the dynamic baffle and arranged at intervals; and each first partition and second partition are alternately and annularly arranged at intervals, and form a channel for gas-liquid interaction, i.e., a baffle channel; the gas enters the channel from bottom to top and flows radially in a zigzag manner to interact and condense with the liquid entering the channel from top to bottom; and a drainage channel is provided on the second partition, and the directions of the drainage channels opened on two adjacent second partitions are opposite and staggered. Compared with the prior art, the present application can improve the mass transfer coefficient and the purity of the purified product formed after gas phase condensation.

Description

Ultra-gravity separation device for solvent purification and control method thereof

Technical Field

The invention relates to the field of semiconductors, and in particular to an ultra-gravity separation device for solvent purification and a control method thereof.

Background Art

As one of the important raw materials required by the semiconductor industry, the purity of chemicals such as high-purity wet solvents is crucial to the production of semiconductors or integrated circuits. This is not only related to the material of the equipment, but also to the purification method of the production process.

Traditional chemical production methods mainly use plate towers or packed towers to purify by distillation. However, due to the material and surface treatment of this type of equipment, the purity of the products produced is not high, and it is difficult to meet the semiconductor industry's requirements for ultra-high purity solvents. For example, the distillation tower disclosed in the cyclone shearing ultra-gravity distillation tower disclosed in patent application document CN 202478632U utilizes the principle of ultra-gravity separation. Although it effectively reduces the height of the equipment and solves the problem of short circuit or channeling between the vapor and liquid in the existing ultra-gravity rotary distillation tower, which makes the contact time between the gas and liquid phases too short, thereby reducing the mass transfer efficiency, and greatly improves the purification concentration of the solvent, it still cannot reach PPB level or above.

In addition, the purity of products produced by traditional chemical industry is basically at PPM level or below, mainly because plate towers or packed towers are used for purification, the liquid phase uses a weak gravity field, the liquid film flows slowly, and the mass transfer coefficient is low. In addition, the materials of the production equipment are mainly carbon steel or stainless steel. In this way, ions are easily precipitated during the purification process, resulting in product contamination and difficulty in improving purity.

Therefore, how to provide an ultra-gravity separation device and a control method for solvent purification to improve the mass transfer coefficient and the purity of the purified product formed after gas phase condensation is a technical problem that the present invention urgently needs to solve.

Summary of the invention

The purpose of the present invention is to provide an ultra-gravity separation device for solvent purification treatment, which can improve the mass transfer coefficient and the purity of the purified product formed after gas phase condensation.

In order to achieve the above object, the present invention provides an ultra-gravity separation device for solvent purification, comprising: a shell,

The static baffle ring comprises: a static baffle plate connected to the shell, and a plurality of first partition plates connected to the static baffle plate and arranged at intervals;

The dynamic baffle ring includes: a dynamic baffle plate rotating with the rotating shaft, and a plurality of second partition plates connected to the dynamic baffle plate and arranged at intervals;

Wherein, each first partition plate and the second partition plate are alternately and annularly arranged at intervals to form a channel for gas-liquid interaction;

The gas enters the channel from bottom to top and flows in a zigzag manner to interact and condense with the liquid entering the channel from top to bottom;

Furthermore, drainage channels are provided on the second partition plates, and the drainage channels provided on two adjacent second partition plates are arranged in opposite directions and staggered.

Further preferably, the second partition plate is provided with a plurality of drainage holes from top to bottom, and a drainage plate connected to the second partition plate and protruding outward; and one end of the drainage plate is connected to the drainage hole to form the drainage channel.

Further preferably, the arrangement directions of the guide plates on two adjacent second partition plates are opposite to each other.

Further preferably, each of the first partition plates and the second partition plates is parallel to the axial direction of the rotating shaft; and the static baffle plates and the dynamic baffle plates are perpendicular to the axial direction of the rotating shaft.

Further preferably, the guide plate is a flexible body and/or an elastic member.

Further preferably, the drainage channel is a tapered channel.

Further preferably, the diameter of the drainage hole is 0.5-1 mm.

Further preferably, the intervals between two adjacent drainage holes in the circumferential direction and the longitudinal direction are both 15 to 30 mm.

Further preferably, the thickness of the first partition plate and the second partition plate is 1 mm to 5 mm.

The guide plate comprises a first guide plate and a second guide plate which are arranged alternately;

The first inclination angle between the first guide plate and the second partition plate (22) is 30° to 75°;

The second inclination angle between the second guide plate and the second partition plate (22) is 30° to 75°;

And/or, the guide plate is provided with a plurality of slits along its circumference.

Further preferably, the gap between the top of the guide plate of the second partition plate located on the gas inlet side of the channel and the static baffle forms a gas inlet; the gap between the top of the guide plate of the second partition plate located on the gas outlet side of the channel and the static baffle forms a gas outlet; wherein the liquid flows in from the gas outlet and flows out from the gas inlet.

Further preferably, the guide plate of the second partition plate located at the gas outlet side of the channel is arranged adjacent to the rotation axis.

Further preferably, there are at least multiple groups of static baffles and dynamic baffles, and they are equidistantly arranged in sequence from bottom to top along the axial direction of the rotating shaft; a liquid inlet is provided on one side of the top of the shell, and a distillation gas outlet is provided on the other side; a liquid inlet is provided on one side of the lower part of the shell, and a drain port is provided at the bottom of the other side; a reflux liquid inlet is provided on the side wall of the middle part of the shell, and the reflux liquid inlet is located between two adjacent groups of static baffles and the dynamic baffles.

Further preferably, the shell, the static baffle ring and the dynamic baffle ring are all made of pure titanium, and the surface roughness is less than or equal to 0.25 μm.

The present application also provides a control method for an ultra-gravity separation device for solvent purification treatment, which is used to control the ultra-gravity separation device for solvent purification treatment, comprising:

causing the rotating shaft to rotate to rotate the moving baffle;

After the liquid enters the channel from bottom to top and flows in a zigzag manner, the gas enters the channel from top to bottom and flows in a zigzag manner to perform mutual condensation.

Compared with the prior art, the ultra-gravity separation device for purifying solvents provided in the present application can improve the mass transfer coefficient and the purity of the purified product formed after gas phase condensation.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG1 is a schematic diagram of the internal structure of an ultra-gravity separation device for solvent purification in a first embodiment of the present invention;

FIG2 is a schematic diagram of the partial structure of the static baffle ring and the dynamic baffle ring in the first embodiment of the present invention;

FIG3 is a partial top view of a preferred guide plate in the first embodiment of the present invention;

FIG4 is a partial side view of a preferred guide plate in the first embodiment of the present invention;

FIG. 5 is a schematic diagram of the porous structure of the drainage holes in the first embodiment of the present invention.

Figure markings: shell 1, intermediate feed port 5, reflux liquid inlet 6, static baffle 7, liquid inlet 8, distillation gas outlet 9, static baffle plate 71, first partition plate 72, dynamic baffle 2, second partition plate 22, guide plate 221, gap 2211, guide plate 222, guide hole 220, hole 2201, hole 2202, guide channel 223, gap 2211, rotating shaft 16.

DETAILED DESCRIPTION

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 described embodiments 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 creative work are within the scope of protection of the present invention.

Embodiment 1

As shown in Figures 1 and 2, this embodiment provides an ultra-gravity separation device for solvent purification, which is mainly composed of a shell 1, a static baffle 7 and a dynamic baffle 2 arranged in the shell 1. The ultra-gravity separation device can be used as a primary distillation tower, or multiple ultra-gravity separation devices can be connected in series to form a multi-stage distillation tower to purify solvents, especially solvents used in the semiconductor industry.

The static deflector ring 7 is mainly composed of a static deflector plate 71 connected to the inner wall of the cavity of the shell 1, a plurality of first partition plates 72 connected to the static deflector plate 71 and arranged at intervals, and the like.

The dynamic baffle ring 2 is mainly composed of a dynamic baffle plate 21 rotating with the rotating shaft 16, a plurality of second partition plates 22 connected to the dynamic baffle plate 21 and arranged at intervals, etc. The dynamic baffle plate 21 is connected to the rotating shaft 16 through a corresponding shaft fixing member.

Furthermore, the first partition plates 72 and the second partition plates 22 are alternately arranged in an annular manner to form a channel for gas-liquid interaction, namely, a baffle channel 12. The first partition plates 72 and the second partition plates 22 are both annular plates.

The gas enters the channel from bottom to top and flows radially in a zigzag manner as shown in the arrow direction of FIG1 to interact with the liquid entering the channel from top to bottom for condensation. The liquid is preferably any one of the solvents such as n-hexane, n-octane or isopropanol. The gas is preferably the vapor corresponding to the liquid.

Furthermore, the second partition plates 22 are provided with drainage channels 223 , and the drainage channels 223 opened on two adjacent second partition plates 22 are in opposite directions and are staggered.

From the above content, it can be seen that: by arranging staggered drainage channels 223 on the moving baffle ring, at least part of the liquid is thrown out from the small hole at high speed under the action of centrifugal force, and hits the non-porous static baffle ring to form fine droplets, which are in countercurrent contact with the gas phase, and the gas and liquid phases are fully mixed, which greatly improves the mass transfer coefficient and the purity of the purified product formed after the gas phase condensation, so that through multi-layer mass transfer treatment, the purity of the final product after the gas phase condensation can reach above PPM level, and the efficiency of heat exchange is improved, and energy consumption is reduced.

Further preferably, in order to meet the design and requirements in practical applications, the second partition plate 22 is provided with a plurality of drainage holes 220 from top to bottom, and a drainage plate connected to the second partition plate 22 and protruding outward. In addition, one end of the drainage plate is connected to the drainage hole to form a drainage channel 223. This structure can not only improve the liquid segmentation effect, but also further improve the mass transfer coefficient and mass transfer efficiency, and prolong the time period of gas-liquid two-phase contact, thereby greatly improving the solvent purification concentration.

Further preferably, the arrangement directions of the guide plates on the two adjacent second partition plates 22 are set in opposite directions, such as the guide plates 221 and the guide plates 222 arranged alternately as shown in FIG2. This structure can play a good drainage role and prolong the interaction time, so that the liquid can be further impacted and broken into fine droplets by the guide plates under the action of centrifugal force, so as to fully achieve the mixing of the gas-liquid two phases, thereby improving the mass transfer coefficient.

Specifically, the first inclination angle between the guide plate 221 and the second partition plate 22 is preferably 30° to 90° downward, and the first inclination angle of 45° is only used as an example for illustration. The second inclination angle between the guide plate 222 and the second partition plate 22 is preferably 30° to 90° upward, and the second inclination angle of 45° is only used as an example for illustration. Through this arrangement, the formed drainage channels 223 can be arranged in an upper and lower staggered manner. The diameter of the drainage hole is 0.5 to 1 mm. The spacing between two adjacent drainage holes 220 in the circumferential and longitudinal directions can preferably be 15 to 30 mm, and this embodiment only takes the spacing of 20 mm as an example for illustration.

Since the guide plate 221 and the second partition plate 22 are spaced apart in the channel, when the liquid flows through different sections along the direction indicated by the arrow in Figure 2, it can be broken up and impacted by the guide plates from different directions, so that the formed fine droplets are more uniform, further improving the mass transfer coefficient and enabling full mixing of the gas-liquid two phases, further improving the mass transfer coefficient.

Obviously, it should be noted that the first inclination angle and the second inclination angle in this embodiment can also be other degrees, such as 30 degrees, 60 degrees, 75 degrees, or other degrees less than 90 degrees, etc., which will not be specifically described or limited here. The drainage hole can be a single hole or a porous structure to serve as an area for dividing and breaking up the liquid. The porous structure can refer to the hole 2201 and the hole 2202 shown in Figure 5.

Further preferably, the guide plates 221 on each second partition plate 22 are arranged along the direction of gas inflow, toward the corresponding static baffle plate 71, so that a dispersion space and a mixing area are formed between two adjacent static baffle plates 71, so that the liquid interacts with the gas after being dispersed in the dispersion space, and is remixed in the mixing area and then mixed with the gas, which not only avoids obstruction of the flow direction of gas and liquid, but also greatly improves the mass transfer coefficient and heat exchange efficiency in the process of alternating dispersion and mixing of the liquid with the gas.

Further preferably, each of the first partition plates 72 and the second partition plates 22 is parallel to the axial direction of the rotating shaft 16 ; and the static baffle plates 71 and the dynamic baffle plates 21 are perpendicular to the axial direction of the rotating shaft 16 .

Preferably, the drain plate 221 is a flexible body and/or an elastic member. This structure can increase the swing amplitude of the drain plate 221 when it rotates with the partition plate, thereby achieving a good effect of breaking up the liquid, so as to maximize the gas-liquid interaction and achieve full interaction. Among them, as a preferred method, the drain plate 221 is formed by stamping when the drainage hole is opened, or it can be set on the second partition plate 22 by welding, gluing or clamping after the drainage hole is opened. However, this embodiment only takes the drain plate 221 formed by stamping when the drainage hole is opened as an example for illustration.

In addition, as another preferred embodiment, as shown in FIG. 3 and FIG. 4 , the guide plate 221 and/or the guide plate 222 are provided with a plurality of slits 2211 along the circumference thereof, so that a portion of the thinner guide plate 221 can form a flexible body or an elastic body. Among them, the slits 2211 are extended along the length direction of the guide plate. Moreover, the thickness of the first partition plate 72 and the second partition plate 22 are preferably 1 to 5 mm, and the spacing of 3 mm is only used as an example for illustration, which not only facilitates the second partition plate 22 to form the guide plate 221 by stamping, but also makes the guide plate 221 have good elasticity. In addition, it is worth mentioning that the guide plate 222 in this embodiment may also be provided with a plurality of the above-mentioned slits 2211 along the circumference thereof. Among them, the width of the slit 2211 is preferably 1 mm to 3 mm.

Further preferably, in order to facilitate the convergence of the liquid and control its flow path, the gap between the top of the guide plate of the second partition plate 22 located on the gas inlet side of the channel and the static baffle 71 forms a gas inlet. The gap between the top of the guide plate of the second partition plate 22 located on the gas outlet side of the channel and the static baffle 71 forms a gas outlet, and the guide tube 10 is sleeved on the through hole of the static baffle to form an axial channel 13.

Further preferably, the gap between the top of the guide plate of the second partition plate 22 located on the gas inlet side of the channel and the static baffle 71 forms a gas inlet. The gap between the top of the guide plate of the second partition plate 22 located on the gas outlet side of the channel and the static baffle 71 forms a gas outlet. Among them, the liquid flows in from the gas outlet and flows out from the gas inlet. Through this structure, the gas entering from the bottom of the shell can always enter from top to bottom in the gas-liquid interaction channel, and due to the limitation of the channel structure, the liquid flowing in above the shell enters from bottom to top, so that the gas and liquid are bound to interact, and the length of the interaction space of the channel and the interaction time are extended, the liquid phase uses the gravity field to enhance the efficiency of the interaction condensation of gas and liquid.

Further preferably, the guide plate of the second partition plate 22 located at the gas outlet side of the channel is arranged adjacent to the rotation axis.

Further preferably, in order to realize the recycling of the gas and liquid after distillation and improve the purity of the product, there are at least multiple groups of the above-mentioned static baffles 7 and dynamic baffles 2, and they are equidistantly arranged in sequence from bottom to top along the axial direction of the rotating shaft. A liquid inlet 8 is provided on one side of the top of the shell 1, and a distilled gas outlet 9 is provided on the other side. A gas phase inlet 11 is provided on one side of the lower part of the shell 1, and a liquid discharge port 15 is provided on the bottom of the other side. A reflux liquid inlet 6 and an intermediate feed port 5 are provided on the side wall of the middle part of the shell 1, and the reflux liquid inlet 6 and the intermediate feed port 5 are respectively located between the corresponding and adjacent two groups of static baffles 7 and dynamic baffles 2. Among them, the liquid flows in from the liquid inlet 8 and flows out from the gas phase inlet 11.

Further preferably, the shell, the static baffle 7, the dynamic baffle 2, the first partition plate 72 and the second partition plate 22 are all made of pure titanium, and the surface roughness is less than or equal to 0.25 μm, so that through the internal EP treatment after processing, a dense protective film is formed to effectively prevent ion precipitation, thereby ensuring the purity of the purified product and ensuring that it reaches the PPM level or above. Obviously, if it is necessary to explain, the material of the first partition plate 72 and the second partition plate 22 in this embodiment can also be made of other metal materials, such as stainless steel, copper or silver, etc., to improve the thermal conductivity of the metal material and improve the above-mentioned mass transfer coefficient. Here, no specific limitation or repeated description is made.

This embodiment also provides a control method for controlling the ultra-gravity separation device for purifying a solvent, comprising the following steps:

Step 1: Start the motor to rotate the rotating shaft to rotate the baffle ring 2.

Step 2: Open the corresponding inlet to allow the liquid to flow in a zigzag manner from bottom to top into the channel, and then allow the gas to flow in a zigzag manner from top to bottom into the channel to perform cross-condensation.

Through the above steps, it can be known that: by arranging staggered drainage channels 223 on the moving baffle ring, at least part of the liquid is thrown out from the small hole at high speed under the action of centrifugal force, and hits the non-porous static baffle ring to form fine droplets, which are in countercurrent contact with the gas phase, and the gas and liquid phases are fully mixed, which greatly improves the mass transfer coefficient and the purity of the purified product formed after the gas phase condensation, so that through multi-layer mass transfer treatment, the purity of the final product after the gas phase condensation can reach above PPM level, and the efficiency of heat exchange is improved, and energy consumption is reduced.

The present invention is described in detail above in conjunction with the embodiments of the accompanying drawings. A person skilled in the art can make various variations of the present invention according to the above description. Therefore, certain details in the embodiments should not constitute a limitation of the present invention, and the scope of protection of the present invention shall be defined by the scope of the attached claims.

Claims (10)

1. An ultra-gravity separation device for solvent purification, characterized in that it comprises: a housing (1), A static baffle ring (7) comprising: a static baffle plate (71) connected to the shell (1), and a plurality of first partition plates (72) connected to the static baffle plate (71) and arranged at intervals; The dynamic baffle ring (2) comprises: a dynamic baffle plate (21) rotating with the rotating shaft, and a plurality of second partition plates (22) connected to the dynamic baffle plate (21) and arranged at intervals; Wherein, each first partition plate (72) and second partition plate (22) are alternately arranged in an annular space and form a channel (12) for gas-liquid interaction; The gas enters the channel (12) from bottom to top and flows in a zigzag manner to interact and condense with the liquid entering the channel from top to bottom; Furthermore, the second partition plate (22) is provided with a drainage channel, and the drainage channels opened on two adjacent second partition plates (22) are arranged in opposite directions and staggered. 2. The ultra-gravity separation device for solvent purification according to claim 1 is characterized in that a plurality of drainage holes are provided on the second partition plate (22) from top to bottom, and a drainage plate is connected to the second partition plate (22) and protrudes outward; and one end of the drainage plate is connected to the drainage hole to form the drainage channel. 3. The ultra-gravity separation device for solvent purification according to claim 1 is characterized in that the arrangement directions of the guide plates on two adjacent second partition plates (22) are set in opposite directions. 4. The ultra-gravity separation device for solvent purification according to claim 1 is characterized in that each first partition plate (72) and the second partition plate (22) are parallel to the axial direction of the rotating shaft; the static baffle plate (71) and the dynamic baffle plate (21) are perpendicular to the axial direction of the rotating shaft. 5. The ultra-gravity separation device for solvent purification according to claim 2, characterized in that the guide plate is a flexible body and/or an elastic member; The drainage channel is a tapered channel; The diameter of the drainage hole is 0.5 to 1 mm; The spacing between two adjacent drainage holes (220) in the circumferential direction and the longitudinal direction is 15 to 30 mm; The thickness of the first partition plate (72) and the second partition plate (22) is 1 mm to 5 mm; The guide plate comprises a first guide plate and a second guide plate which are arranged alternately; The first inclination angle between the first guide plate and the second partition plate (22) is 30° to 75°; The second inclination angle between the second guide plate and the second partition plate (22) is 30° to 75°; And/or, the guide plate is provided with a plurality of slits along its circumference. 6. The ultra-gravity separation device for solvent purification according to claim 2 is characterized in that the gap between the top of the guide plate of the second partition plate (22) located on the gas inlet side of the channel and the static baffle (71) forms a gas inlet; the gap between the top of the guide plate of the second partition plate (22) located on the gas outlet side of the channel and the static baffle (71) forms a gas outlet, and a guide tube (10) is sleeved on the through hole of the static baffle and forms an axial channel (13); wherein the liquid flows in from the gas outlet and flows out from the gas inlet. 7. The ultra-gravity separation device for solvent purification according to claim 1, characterized in that the guide plate of the second partition plate (22) located on the gas outlet side of the channel is arranged adjacent to the rotating shaft. 8. An ultra-gravity separation device for solvent purification according to any one of claims 1 to 7, characterized in that there are at least multiple groups of static baffles (7) and dynamic baffles (2), and they are equidistantly arranged in sequence from bottom to top along the axial direction of the rotating shaft; a liquid inlet (8) is provided on one side of the top of the shell (1), and a distillation gas outlet (9) is provided on the other side; a gas phase inlet (11) is provided on one side of the lower part of the shell (1), and a drain port (15) is provided at the bottom of the other side; a reflux liquid inlet (6) and an intermediate feed port (5) are provided on the side wall of the middle part of the shell (1), and the reflux liquid inlet (6) and the intermediate feed port (5) are respectively located between two corresponding and adjacent groups of static baffles (7) and the dynamic baffles (2). 9. The ultra-gravity separation device for solvent purification according to claim 1 is characterized in that the shell, the static baffle (7) and the dynamic baffle (2) are all made of pure titanium, and the surface roughness is less than or equal to 0.25 μm. 10. A method for controlling an ultra-gravity separation device for solvent purification, used for controlling the ultra-gravity separation device for solvent purification according to any one of claims 1 to 9, characterized in that it comprises: The rotating shaft is caused to rotate so as to rotate the moving baffle ring (2); After the liquid enters the channel from bottom to top and flows in a zigzag manner, the gas enters the channel from top to bottom and flows in a zigzag manner to perform mutual condensation.