A distillation and purification device and method for electronic-grade isopropanolamine

Abstract

The present invention discloses a rectification and purification device and method for electronic-grade isopropylamine, and relates to the technical field of rectification devices. The rectification and purification device and method for electronic-grade isopropylamine include a tower body, a feed pipe, a gas phase collecting pipe, a liquid phase collecting pipe, a reflux pipe and a tray, wherein the tray is fixed in the tower body, and further includes: an inner plate, wherein the inner plate is fixed in the tray, and the inner plate divides the space in the tray into an outer ring portion and an inner peripheral portion; a partition, wherein the partition is provided with a plurality of partitions, wherein the plurality of partitions are fixed in the inner peripheral portion at equal intervals, and the space of the inner peripheral portion is divided into a plurality of liquid inlet channels and a plurality of liquid outlet channels, wherein the liquid inlet channels and the liquid outlet channels are staggered. By arranging a floating plate, the liquid in the liquid inlet channel can be kept horizontal to a certain extent when flowing, thereby avoiding the fluctuation of the liquid level causing uneven distribution of the gas phase, so as to improve the efficiency of two-phase mass transfer.

Description

Technical Field

[0001] The present invention relates to the technical field of distillation devices, in particular to a distillation and purification device and method for electronic-grade isopropanolamine. Background Art

[0002] Electronic-grade isopropanolamine usually refers to monoisopropanolamine, which is a cleaning material used on a large scale in the semiconductor industry. Its purity and impurity control need to meet strict standards. Due to the influence of the production process, monoisopropanolamine products are usually mixed with diisopropanolamine and triisopropanolamine. The boiling points of the three are different. Among them, the boiling point of monoisopropanolamine is 170℃, the boiling point of diisopropanolamine is 249℃, and the boiling point of triisopropanolamine is 305℃. Therefore, distillation is usually used for separation, and the monoisopropanolamine with the lowest boiling point is collected at the top of the distillation tower.

[0003] The processing process of the distillation tower can be summarized as follows: the liquid enters the tower plate from the downcomer, and the gas phase enters the liquid on the tower plate from the bottom of the tower plate, and continues to rise after completing the gas-liquid exchange. During the distillation process, when the liquid flow in the downcomer is large, the liquid level on the tower plate becomes higher on the side close to the liquid inlet and lower on the side close to the liquid discharge. The height of the liquid level has a direct impact on the distribution of the gas. The lower the liquid level, the smaller the resistance to the gas, and the higher the liquid level, the greater the resistance to the gas. As a result, the gas is concentrated in the liquid on the tower plate from the lower liquid level, resulting in the gas not being evenly distributed in the liquid on the tower plate, thereby affecting the efficiency of the gas-liquid exchange. Summary of the Invention

[0004] In view of the deficiencies in the prior art, the present invention provides a device and method for distilling and purifying electronic-grade isopropylamine, which solves the problems raised in the background art.

[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions: a distillation and purification device for electronic grade isopropylamine, comprising a tower body, a feed pipe, a gas phase collecting pipe, a liquid phase collecting pipe, a reflux pipe and a tray, wherein the tray is fixed in the tower body, and further comprising: an inner plate, wherein the inner plate is fixed in the tray, and the inner plate divides the space in the tray into an outer ring portion and an inner ring portion; a partition, wherein a plurality of partitions are provided, and the plurality of partitions are fixed in the inner ring portion at equal intervals, and the space in the inner ring portion is divided into a plurality of liquid inlet channels and a plurality of liquid outlet channels. Liquid outlet channel, the liquid inlet channel and the liquid outlet channel are arranged alternately; an air inlet part, the air inlet part is fixedly arranged in the liquid inlet channel, the bottom end of the air inlet part is connected with an air inlet pipe, the top end of the air inlet part is connected with an air inlet head, and an air inlet hole is provided on the side of the air inlet head close to the liquid inlet channel in the vertical direction; a floating plate, the floating plate is arranged in the liquid inlet channel, and the four sides are in sliding contact with the inner wall of the liquid inlet channel, a floating plug is slidingly provided in the air inlet head, and one end of the floating plug passes through the air inlet hole and is fixedly connected to the floating plate, so that the floating plug moves synchronously with the floating plate in the vertical direction.

[0006] Furthermore, a connecting piece is provided above the floating plate, and each of the floating plates is fixedly connected to the connecting piece.

[0007] Furthermore, the height of the liquid inlet channel is set to be higher than the liquid outlet channel; a liquid outlet is opened on the partition, and the liquid outlet is used to connect the adjacent liquid inlet channel and liquid outlet channel, and a mesh plate is provided in the liquid outlet; a guide flow channel is provided on the side of the partition close to the liquid outlet channel, and the guide flow channel is connected with the liquid outlet, and the guide flow channel is inclined in the opposite direction of the liquid flow direction in the liquid outlet channel.

[0008] Furthermore, a downcomer is provided in the tower body; a liquid inlet and a liquid discharge part are provided in the outer ring part, the liquid inlet is connected to the downcomer, and the liquid discharge part is connected to another downcomer; a liquid inlet is provided on one side of the inner enclosure plate, and the liquid inlet is used to connect the liquid inlet part and the liquid inlet channel, and a liquid discharge port is provided on the other side of the inner enclosure plate, and the liquid discharge port is used to connect the liquid discharge part and the liquid outlet channel; the upper end of the liquid inlet is lower than the upper end of the partition, and the bottom end of the liquid inlet is flush with the bottom end of the liquid inlet channel; the bottom end of the liquid inlet is flush with the bottom end of the liquid inlet channel.

[0009] Furthermore, a cofferdam is provided in the liquid inlet portion, which serves as a barrier to the liquid inlet, and the cofferdam corresponds to the liquid inlet one by one; the upper end of the cofferdam is higher than the upper end of the liquid inlet; a baffle is fixed in the downcomer, and the baffle is located directly above the cofferdam.

[0010] Furthermore, a gate plate is provided on one side of the outer ring portion close to the liquid inlet portion, and a weir plate is provided on one side of the outer ring portion close to the liquid discharge portion, and the area of ​​the outer ring portion between the gate plate and the weir plate is the overflow portion; when the liquid in the liquid inlet portion is higher than the upper end of the partition plate, the gate plate is lifted to connect the liquid inlet portion with the overflow portion, and when the liquid in the liquid inlet portion is lower than the upper end of the partition plate, the gate plate falls to disconnect the liquid inlet portion from the overflow portion.

[0011] Furthermore, a float chamber is provided in the liquid inlet, and the bottom end of the float chamber is connected to the liquid inlet; a float is provided in the float chamber, and the bottom end of the gate is fixedly connected to the float. When the float rises or falls under the action of buoyancy, it drives the gate to move in the vertical direction.

[0012] Furthermore, the upper end of the inner enclosure plate is higher than the upper end of the partition plate; the inner enclosure plate is provided with an overflow port at the overflow portion, and the upper end of the overflow port is flush with the upper end of the partition plate.

[0013] Furthermore, one side of the overflow part is connected to an overflow pipe, a first connecting pipe is provided on the outside of the tower body, and the overflow pipe is connected to the first connecting pipe; a temporary storage tank is provided on the outside of the tower body, the first connecting pipe is connected to the temporary storage tank, and the feed pipe is connected to a downcomer; a second connecting pipe is connected between the temporary storage tank and the feed pipe, and a reflux pump is installed on the second connecting pipe.

[0014] The present invention also provides a distillation and purification method for electronic-grade isopropanolamine, which is applicable to the distillation and purification device of the electronic-grade isopropanolamine, comprising the following steps:

[0015] Step 1: The isopropanolamine mixed solution is heated and then passed into the feed pipe;

[0016] Step 2: Evenly deliver the isopropylamine mixed liquid into each liquid inlet channel at the liquid inlet portion of the tray;

[0017] Step 3: Steam is introduced into the bottom of the tower body and allowed to enter the liquid inlet channel, where gas-liquid exchange is performed. During the gas-liquid exchange, the lower surface of the floating plate is always in contact with the isopropylamine mixed liquid, and the liquid after the exchange is completed is introduced into the liquid outlet channel;

[0018] Step 4: Collect the gas phase product through the gas phase collecting pipe at the top of the tower body, and collect the liquid phase through the liquid phase collecting pipe at the bottom of the tower body;

[0019] Step 5: When the liquid flow in the tray is too large, lift the gate to allow the excess liquid to flow into the overflow part;

[0020] Step 6: The liquid at the overflow part is passed into the temporary storage tank. When the liquid flow in the tray is low, the liquid in the temporary storage tank is sent into the feed pipe.

[0021] The present invention has the following beneficial effects:

[0022] (1) The distillation and purification device and method of electronic grade isopropylamine are provided with a liquid inlet channel, and an air inlet member and a floating plate are provided in the liquid inlet channel. Liquid and gas phases are exchanged in the liquid inlet channel. The floating plate can keep the liquid level in the liquid inlet channel level to a certain extent when the liquid flows, thereby avoiding uneven distribution of the gas phase caused by fluctuations in the liquid level, so as to improve the efficiency of two-phase mass transfer. At the same time, a floating plug is provided in the air inlet head and moves synchronously with the floating plate, so that the lower surfaces of the floating plate and the floating plug form a sealing surface, which plays an isolating role for the gas phase and the liquid, and prevents the gas phase from escaping from the upper part of the liquid inlet channel.

[0023] (2) The distillation and purification device and method for electronic grade isopropylamine are provided with an overflow portion and a gate plate. When there is too much liquid in the tray, the gate plate can be lifted by a float, so that the excess liquid can flow into the overflow portion and be discharged from the overflow pipe, thereby avoiding excessive liquid accumulation in the tray, which would cause excessive gas phase flow resistance.

[0024] Of course, any product implementing the present invention does not necessarily need to achieve all of the advantages described above at the same time. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0026] Figure 2 This is a schematic diagram of the internal structure of the tower body of the present invention;

[0027] Figure 3 This is a schematic diagram of the internal structure of the tray of the present invention;

[0028] Figure 4 This is a schematic top view of the interior of the tray of the present invention;

[0029] Figure 5 This is a schematic cross-sectional view of the interior of the tray of the present invention;

[0030] Figure 6 This is a schematic diagram of the structure of the inner periphery and outer ring of the tray of the present invention;

[0031] Figure 7 This is a schematic diagram of the internal structure of the liquid inlet portion on the tray of the present invention;

[0032] Figure 8 This is a schematic diagram of the coordination structure of the liquid inlet channel, the liquid outlet channel and the floating plate of the present invention;

[0033] Figure 9 This is a schematic diagram of the coordination structure of the liquid inlet channel and the liquid outlet channel of the present invention;

[0034] Figure 10 It is a schematic planar cross-sectional view of the cooperation structure of the liquid inlet channel, the liquid outlet channel and the floating plate of the present invention;

[0035] Figure 11 This is a schematic diagram of the air intake structure of the present invention;

[0036] Figure 12 This is a schematic top view of the air intake member of the present invention;

[0037] Figure 13 For the present invention Figure 7 Enlarged schematic diagram of area A in the middle;

[0038] Figure 14 It is a schematic diagram of the float and gate plate matching structure from a top view of the present invention.

[0039] In the figure, 1, tower body; 2, feed pipe; 3, gas phase collection pipe; 4, liquid phase collection pipe; 5, reflux pipe; 6, overflow pipe; 7, first connecting pipe; 8, temporary storage tank; 9, second connecting pipe; 10, reflux pump; 11, downcomer; 111, baffle; 12, tray; 13, inner panel; 14, air inlet pipe; 15, partition; 151, liquid outlet; 152, guide channel; 16, mesh plate; 17, flat plate ;19. Channel plate;21. Air inlet;211. Air inlet head;212. Air inlet hole;22. Float plug;23. Float plate;24. Connecting piece;25. Liquid inlet part;26. Cofferdam;27. Liquid inlet port;28. Liquid discharge part;29. Liquid discharge port;30. Overflow part;31. Gate plate;32. Weir plate;33. Float chamber;34. Vertical plate;35. Folding plate;36. Float;37. Overflow port;38. Lifting plate. DETAILED DESCRIPTION

[0040] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. 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 making creative efforts are within the scope of protection of the present invention.

[0041] In the description of the present invention, it should be understood that the terms "opening", "upper", "lower", "thickness", "top", "middle", "length", "inside", "around" and the like indicating orientation or positional relationship are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the components or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0042] The following is based on Figures 1-14 The present invention provides an apparatus and method for distilling and purifying electronic-grade isopropanolamine.

[0043] See also Figures 1-10, an embodiment of the present invention provides a technical solution: a distillation and purification device for electronic-grade isopropanolamine, comprising a tower body 1, a feed pipe 2, a gas phase collecting pipe 3, a liquid phase collecting pipe 4, a reflux pipe 5 and a tray 12, wherein the feed pipe 2 is installed near the middle of the tower body 1 to transport the liquid to be separated into the tower body 1, the gas phase collecting pipe 3 is located at the top of the tower body 1, for collecting the required gas phase, the liquid phase collecting pipe 4 is located at the bottom of the tower body 1, for collecting the separated liquid substance, a plurality of trays 12 are provided, which are distributed at intervals and fixed inside the tower body 1, and the trays 12 and the inner wall of the tower body 1 need to be sealed, the reflux pipe 5 is provided at the upper part of the tower body 1, and is located above all the trays 12, after the collected gas phase is condensed and separated, a part is collected as a product, and the other part is re-sent into the tower body 1 through the reflux pipe 5, and the steam is sent into the tower through the bottom end of the tower body 1 (the steam inlet is not drawn in the figure).

[0044] Combine Figure 3 An inner panel 13 is provided inside the tray 12, and the inner panel 13 divides the space inside the tray 12 into an outer ring portion and an inner ring portion. Specifically, the tray 12 can be considered to be composed of a circular bottom plate and an annular side plate. The part between the inner panel 13 and the annular side plate is the outer ring portion, and the part inside the inner panel 13 is the inner ring portion.

[0045] In addition, a liquid inlet 25 and a liquid discharge 28 are provided in the outer ring portion, and a downcomer 11 is also provided in the tower body 1. The liquid discharge 28 of the upper layer is connected to the liquid inlet 25 of the lower layer through the downcomer 11. It can also be understood that the liquid inlet 25 in one layer of tray 12 is connected to one downcomer 11, and the liquid discharge 28 is connected to another downcomer 11.

[0046] In addition, a plurality of partitions 15 are fixedly arranged at equal intervals in the inner peripheral portion, and the plurality of partitions 15 divide the space of the inner peripheral portion into a plurality of liquid inlet channels and a plurality of liquid outlet channels. The liquid inlet channels and the liquid outlet channels are arranged in a staggered manner. It can be understood that both sides of a single liquid inlet channel are liquid outlet channels, and both sides of a single liquid outlet channel are liquid inlet channels. It should be noted that only one side of a liquid inlet channel or liquid outlet channel located at the boundary of the inner peripheral portion has a liquid outlet channel or liquid inlet channel (combined with Figure 4 , as shown in the figure, the boundary of the inner part is a liquid inlet channel, and one side of it is a liquid outlet channel).

[0047] Specifically, the liquid inlet channel is connected to the liquid inlet portion 25 and is not connected to the liquid outlet channel. The liquid outlet channel is connected to the liquid discharge portion 28 and is not connected to the liquid inlet channel. Moreover, each liquid inlet channel is not connected to each other in the inner peripheral portion, and each liquid outlet channel is also not connected to each other in the inner peripheral portion. Multiple liquid inlet channels are used to separate the liquid entering the inner peripheral portion to improve the uniformity of liquid distribution. A liquid outlet 151 is opened on the partition 15, and the liquid outlet 151 is used to connect adjacent liquid inlet channels and liquid outlet channels.

[0048] In addition, combined Figure 5 An air inlet part 21 is fixedly provided in the liquid inlet channel, and the bottom end of the air inlet part 21 is connected to the air inlet pipe 14. The air inlet pipe 14 can transfer the gas phase of the next layer to the air inlet part 21 of the upper layer under the action of pressure. An air inlet head 211 is connected to the top of the air inlet part 21. An air inlet hole 212 is opened in the vertical direction on the side of the air inlet head 211 close to the liquid inlet channel, so that the gas phase enters the liquid inlet channel through the air inlet hole 212. Preferably, two air inlet heads 211 are provided on one air inlet head 211 to increase the air intake volume.

[0049] In addition, a float plate 23 is provided in the liquid inlet channel. The four sides of the float plate 23 are in sliding contact with the inner wall of the liquid inlet channel. When the liquid flows through the liquid inlet channel, the float plate 23 moves upward under the buoyancy. A tiny gap is allowed to be left between the four sides of the float plate 23 and the inner wall of the liquid inlet channel, which can be controlled within 1 mm. The pressure between the two should not be too large, so as to avoid excessive friction that causes the float plate 23 to be unable to move. In addition, when the liquid inlet channel is full of liquid, the lower surface of the float plate 23 is in contact with the surface of the liquid. The float plate 23 can keep the liquid in the liquid inlet channel level to a certain extent when it flows, thereby avoiding uneven distribution of the gas phase caused by fluctuations in the liquid level. For example, when the liquid level is high at a certain point, the force on the gas phase increases, causing the gas phase to escape from the lower liquid level, resulting in the liquid at the high liquid level failing to contact the gas phase, thereby reducing the mass transfer efficiency.

[0050] And, combined with Figure 10-12 A float plug 22 is provided in the air inlet head 211. One end of the float plug 22 passes through the air inlet hole 212 and is fixed to the float plate 23. The two move synchronously to block the gas phase in the air inlet head 211 and prevent the gas phase from escaping from the air inlet hole 212 above the float plug 22. Preferably, the lower surface of the float plug 22 is flush with the lower surface of the float plate 23. When the float plate 23 moves, the float plug 22 moves together. When the liquid level rises or falls, the float plate 23 floats up or down accordingly. At this time, the air inlet hole 21 2 is located below the liquid level, and the side of the floating plate 23 contacts the side of the air inlet head 211 and the side of the float 22, so that the lower surface of the floating plate 23 and the float 22 forms a sealing surface, which plays a role in isolating the gas phase and the liquid. At this time, the gas phase is blocked by the float 22 and only enters the liquid from the air inlet hole 212 below the liquid level, and then flows through the liquid outlet 151 with the liquid. It will not escape from the top of the liquid inlet channel or will escape in small amounts, thereby separating the gas phase from the liquid outside the liquid inlet channel.

[0051] Specifically, during the distillation process, the liquid enters the liquid inlet part 25 through the downcomer 11, then flows through the liquid inlet channel, and then enters the liquid discharge channel through the liquid outlet 151, and then enters the liquid discharge part 28, and enters the liquid inlet part 25 on the next tray 12 from the downcomer 11 until it reaches the bottom of the tower body 1. The float plate 23 floats up as the liquid level rises under the action of buoyancy. After the steam is introduced into the tower body 1, the gas phase in the tower body 1 enters the gas inlet part 21 through the gas inlet pipe 14 and is squeezed into the liquid from the gas inlet hole 212. Under the isolation effect of the float plate 23 and the float plug 22, the gas phase can also be constrained in the liquid inlet channel when the liquid level changes and be discharged from the liquid outlet 151 along with the liquid.

[0052] See Figure 3 、 Figure 4 and Figure 10 In order to keep the heights of the multiple floats 23 always the same, thereby keeping the liquid level in all liquid inlet channels consistent, a connector 24 is provided above the float 23, and each float 23 is fixedly connected to the connector 24. It should be noted that when the float 23 is at the lowest point, the connector 24 cannot contact the partition 15, and the specific structure can be set to a rake shape.

[0053] See Figures 8-10 In order to improve the fluidity of the liquid in the inner peripheral part, the height of the liquid inlet channel is set to be higher than the liquid outlet channel, so that there is a height difference between the liquid inlet channel and the liquid outlet channel, so that the liquid flows from the liquid inlet channel into the liquid outlet channel. A mesh plate 16 is provided in the liquid outlet 151. The area of ​​the holes on the mesh plate 16 is smaller than the air inlet hole 212, so that the large bubbles in the liquid inlet channel can be divided into small bubbles when passing through the mesh plate 16, thereby increasing the gas-liquid contact area. At the same time, the presence of the mesh plate 16 can increase the resistance of the liquid in the liquid inlet channel when it flows out, so that a certain height of the liquid level can be maintained even when the liquid flow rate in the liquid inlet channel is small.

[0054] In addition, a guide channel 152 is provided on the side of the partition 15 close to the liquid outlet channel. The guide channel 152 is connected to the liquid outlet port 151, and the guide channel 152 is inclined in the opposite direction of the liquid flow direction in the liquid outlet channel. Since liquid in the two adjacent liquid inlet channels flows into the same liquid outlet channel, the two liquid outlet ports 151 are opposite to each other on both sides of the liquid outlet channel. When the liquid flows into the liquid outlet channel, it first rushes against each other and has a tendency to reflux, and then is brought back to the drain portion 28 to promote the formation of turbulence, thereby enhancing the disturbance and mixing of the remaining gas phase and liquid, and reducing the gas phase in the liquid entering the next layer of tray 12.

[0055] Specifically, a flat plate 17 is provided at the bottom of the liquid inlet channel. The flat plate 17 serves as the bottom surface of the liquid inlet channel. A recessed portion may be provided on the flat plate 17, and the air inlet member 21 may be accommodated in the recessed portion. Preferably, the upper surface of the air inlet member 21 located in the recessed portion is flush with the upper side surface of the flat plate 17, so that the bottom surface of the liquid inlet channel forms a plane, thereby reducing the resistance to liquid flow. A channel plate 19 is provided at the bottom of the liquid outlet channel. Both sides of the channel plate 19 are fixedly connected to the flat plate 17 and the partition plate 15 while maintaining sealing. Preferably, the cross-section of the channel plate 19 is V-shaped. The guide channel 152 may be composed of two parallel plates, and the lower end of the guide channel 152 is fixed to the channel plate 19.

[0056] See Figure 5-Figure 8 A liquid inlet 27 is provided on one side of the inner panel 13, and the liquid inlet 27 is used to connect the liquid inlet part 25 and the liquid inlet channel. A liquid drain port 29 is provided on the other side of the inner panel 13, and the liquid drain port 29 is used to connect the liquid drain part 28 and the liquid outlet channel. The liquid enters the liquid inlet channel from the liquid inlet 27, enters the liquid outlet channel from the liquid outlet 151, and then flows out through the liquid drain port 29.

[0057] In addition, it is preferred that the upper end of the liquid inlet 27 is lower than the upper end of the partition 15, and the bottom end of the liquid inlet 27 is flush with the bottom end of the liquid inlet channel, so as to avoid the liquid flowing directly from the liquid inlet 27 into the liquid outlet channel when the liquid flow rate is too large, and it is preferred that the bottom end of the liquid inlet portion 25 is flush with the bottom end of the liquid inlet channel. A lifting plate 38 can be provided at the liquid inlet portion 25, and the lifting plate 38 serves as the bottom end of the liquid inlet portion 25, so that the liquid inlet portion 25 and the liquid inlet channel are in the same plane, thereby avoiding liquid accumulation in the liquid inlet portion 25.

[0058] See Figure 3 as well as Figure 5-Figure 8 In order to make the liquid flow evenly into different liquid inlets 27, a cofferdam 26 is provided in the liquid inlet portion 25. The cofferdam 26 serves as a barrier for the liquid inlets 27, and the cofferdam 26 corresponds to the liquid inlets 27 one by one. The upper end of the cofferdam 26 is higher than the upper end of the liquid inlet 27. The liquid in the liquid inlet portion 25 will first gather on the outside of the cofferdam 26. When the liquid level is higher than the upper end of the cofferdam 26, it enters the inner side of the cofferdam 26 and enters the liquid inlet channel through the liquid inlet 27, thereby preventing the liquid from concentrating into one or more of the liquid inlet channels. A through hole can be provided at the bottom end of the cofferdam 26 to prevent liquid accumulation.

[0059] In addition, a baffle 111 is fixedly provided in the downcomer 11 and is located directly above the cofferdam 26 . The baffle 111 shields the upper part of the cofferdam 26 to prevent the liquid flowing down from the downcomer 11 from directly entering the inner side of the cofferdam 26 .

[0060] See Figure 7 、 Figure 13 and Figure 14In order to prevent the downcomer 11 from being blocked when the liquid flow rate is too large, a gate plate 31 is provided on the side of the outer ring portion near the liquid inlet portion 25, and a weir plate 32 is provided on the side of the outer ring portion near the liquid discharge portion 28. Preferably, the weir plate 32 is half the height of the partition 15. The area of ​​the outer ring portion between the gate plate 31 and the weir plate 32 is the overflow portion 30. When the liquid in the liquid inlet portion 25 is higher than the upper end of the partition 15, that is, when the liquid level is too high, the gate plate 31 is lifted to connect the liquid inlet portion 25 with the overflow portion 30, so that part of the liquid enters the overflow portion 30. When the liquid in the liquid inlet portion 25 is lower than the upper end of the partition 15, the gate plate 31 falls to disconnect the liquid inlet portion 25 from the overflow portion 30.

[0061] See Figure 13 and Figure 14 The action of the gate 31 can be achieved by the following methods:

[0062] A float chamber 33 is provided in the liquid inlet part 25, and the bottom end of the float chamber 33 is connected to the liquid inlet part 25. The float chamber 33 can be composed of a vertical plate 34 and a folding plate 35. The vertical plate 34 is close to the side of the liquid inlet part 25, and the folding plate 35 is close to the side of the liquid discharge part 28. The bottom ends of the vertical plate 34 and the folding plate 35 are kept at a certain distance from the surface of the lifting plate 38, and both are fixed on the inner panel 13. The gap between the vertical plate 34 and the folding plate 35 near the liquid inlet part 25 is the connection point between the bottom end of the float chamber 33 and the liquid inlet part 25.

[0063] In addition, a float 36 is provided in the float chamber 33, the bottom end of the gate 31 is fixedly connected to the float 36, and the gate 31 is slidably mounted on the folding plate 35. The liquid level in the float chamber 33 is flush with the liquid level of the liquid inlet portion 25. When the float 36 rises or falls under the action of buoyancy, it drives the gate 31 to move in the vertical direction. When the liquid level in the float chamber 33 is low, that is, the buoyancy is insufficient to drive the float 36 to rise, the gate 31 does not move, thereby separating the space below the folding plate 35, even if the liquid inlet portion 25 is not connected to the overflow portion 30, when the liquid level in the float chamber 33 is high, the buoyancy drives the float 36 to move upward, thereby causing the gate 31 to move upward, thereby opening the space below the folding plate 35, that is, the liquid inlet portion 25 is connected to the overflow portion 30, and then allowing the liquid to flow to the overflow portion 30.

[0064] See Figure 3 、 Figure 6 and Figure 7 In order to avoid excessive liquid inventory in the inner panel 13, which would result in excessive gas phase flow resistance, the upper end of the inner panel 13 is made higher than the upper end of the partition 15, and an overflow port 37 is provided at the overflow portion 30 of the inner panel 13. The upper end of the overflow port 37 is flush with the upper end of the partition 15, so that when the liquid level in the inner panel 13 is higher than the partition 15, excess liquid can enter the overflow portion 30 through the overflow port 37.

[0065] See Figure 1-Figure 3An overflow pipe 6 is connected to one side of the overflow part 30, a first connecting pipe 7 is provided on the outside of the tower body 1, the overflow pipe 6 is connected to the first connecting pipe 7, and a temporary storage tank 8 is provided on the outside of the tower body 1, the first connecting pipe 7 is connected to the temporary storage tank 8, and a feed pipe 2 is also provided on the outside of the tower body 1, the feed pipe 2 is connected to a downcomer 11, a second connecting pipe 9 is connected between the temporary storage tank 8 and the feed pipe 2, and a reflux pump 10 is installed on the second connecting pipe 9.

[0066] Specifically, when the overflow portion 30 is filled with liquid, part of the liquid passes over the weir plate 32 and enters the discharge portion 28, and the other part enters the first connecting pipe 7 through the overflow pipe 6 and then flows into the temporary storage tank 8. The reflux pump 10 can re-input the liquid in the temporary storage tank 8 into the feed pipe 2 through the second connecting pipe 9 to re-participate in the two-phase mass transfer. The excess liquid can be retained in the temporary storage tank 8 to play the role of regulating the liquid level in the tray 12.

[0067] When in use (working), the liquid to be separated is transported into the tower body 1 through the feed pipe 2 and enters one of the trays 12 through the downcomer 11. The liquid in the tray 12 first enters the liquid inlet part 25, and enters the liquid inlet channel through the cofferdam 26 and the liquid inlet 27. The steam is sent into the tower through the bottom end of the tower body 1, and enters the air inlet part 21 through the air inlet pipe 14, and then enters the liquid inlet channel from the air inlet hole 212 on the air inlet head 211. The float plate 23 rises as the liquid level rises, and drives the float 22 to move synchronously. The gas phase and the liquid mix in the liquid inlet channel and enter the liquid outlet channel through the liquid outlet 151. The gas phase is separated from the liquid outside the liquid inlet channel. After the mass transfer is completed, the liquid enters the discharge part 28 through the discharge port 29 and enters the next tray 12 through another downcomer 11. The above process is repeated until it reaches the bottom of the tower body 1 and is discharged from the liquid phase collecting pipe 4. The gas phase passes through the air inlet pipe 14 at the bottom end of the upper tray 12 under the action of pressure, and the above process is repeated until it reaches the top of the tower body 1 and is discharged from the gas phase collecting pipe 3.

[0068] When the liquid flow in the tray 12 is too large, the liquid level in the liquid inlet 25 rises, causing the float 36 in the float chamber 33 to float up and drive the gate 31 to move upward, thereby connecting the liquid inlet 25 with the overflow part 30. The liquid entering the overflow part 30 enters the first connecting pipe 7 through the overflow pipe 6 and enters the temporary storage tank 8 for temporary storage. The reflux pump 10 can re-input the liquid in the temporary storage tank 8 into the feed pipe 2 through the second connecting pipe 9.

[0069] The present invention also provides a distillation and purification method for electronic-grade isopropanolamine, which is applicable to the distillation and purification device for electronic-grade isopropanolamine, comprising the following steps:

[0070] Step 1: The isopropanolamine mixed solution is heated and then introduced into the feed pipe 2;

[0071] Step 2: Evenly feed the isopropylamine mixed solution into each liquid inlet channel at the liquid inlet portion 25 of the tray 12;

[0072] Step 3: Steam is introduced into the bottom of the tower body 1 and allowed to enter the liquid inlet channel, where gas-liquid exchange is performed. During the gas-liquid exchange, the lower surface of the floating plate 23 is always in contact with the isopropylamine mixed liquid, and the liquid after the exchange is completed is passed into the liquid outlet channel;

[0073] Step 4: Collect the gaseous product through the gaseous phase collecting pipe 3 at the top of the tower body 1, and collect the liquid phase through the liquid phase collecting pipe 4 at the bottom of the tower body 1;

[0074] Step 5: When the liquid flow in the tray 12 is too large, lift the gate 31 to allow the excess liquid to flow into the overflow portion 30;

[0075] Step 6: The liquid at the overflow portion 30 is passed into the temporary storage tank 8 . When the liquid flow rate in the tray 12 is low, the liquid in the temporary storage tank 8 is fed into the feed pipe 2 .

[0076] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that includes a list of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0077] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to the specific embodiments described. Obviously, many modifications and variations are possible based on the content of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A distillation and purification device for electronic grade isopropanolamine, comprising a tower body (1), a feed pipe (2), a gas phase collecting pipe (3), a liquid phase collecting pipe (4), a reflux pipe (5) and a tray (12), wherein the tray (12) is fixedly arranged in the tower body (1), characterized in that , also includes: An inner panel (13), the inner panel (13) being fixedly mounted in the tray (12), and the inner panel (13) dividing the space in the tray (12) into an outer ring portion and an inner peripheral portion; a partition (15), wherein a plurality of the partitions (15) are provided, and the plurality of partitions (15) are fixedly arranged in the inner peripheral portion at equal intervals, and divide the space of the inner peripheral portion into a plurality of liquid inlet channels and a plurality of liquid outlet channels, wherein the liquid inlet channels and the liquid outlet channels are arranged in a staggered manner; An air inlet member (21), the air inlet member (21) being fixedly mounted in the liquid inlet passage, the bottom end of the air inlet member (21) being connected to an air inlet pipe (14), the top end of the air inlet member (21) being connected to an air inlet head (211), and the air inlet head (211) being provided with an air inlet hole (212) in a vertical direction on a side close to the liquid inlet passage; A floating plate (23) is provided in the liquid inlet channel, and its four sides are in sliding contact with the inner wall of the liquid inlet channel. A floating plug (22) is slidably provided in the air inlet head (211), and one end of the floating plug (22) passes through the air inlet hole (212) and is fixedly connected to the floating plate (23), so that the floating plug (22) moves synchronously with the floating plate (23) in the vertical direction; The partition plate (15) is provided with a liquid outlet (151), the liquid outlet (151) is used to connect adjacent liquid inlet channels and liquid outlet channels, and a mesh plate (16) is provided inside the liquid outlet (151); A guide flow channel (152) is provided on one side of the partition (15) close to the liquid outlet channel, the guide flow channel (152) is communicated with the liquid outlet (151), and the guide flow channel (152) is inclined in the opposite direction of the liquid flow direction in the liquid outlet channel; A downcomer (11) is further provided in the tower body (1); A liquid inlet (25) and a liquid discharge (28) are provided in the outer ring portion, wherein the liquid inlet (25) is communicated with the downcomer (11), and the liquid discharge (28) is communicated with another downcomer (11); A gate plate (31) is provided on one side of the outer ring portion close to the liquid inlet portion (25), a weir plate (32) is provided on one side of the outer ring portion close to the liquid discharge portion (28), and the area of ​​the outer ring portion between the gate plate (31) and the weir plate (32) is an overflow portion (30); When the liquid in the liquid inlet (25) is higher than the upper end of the partition (15), the gate (31) is lifted to connect the liquid inlet (25) with the overflow (30); when the liquid in the liquid inlet (25) is lower than the upper end of the partition (15), the gate (31) is lowered to disconnect the liquid inlet (25) from the overflow (30); A float chamber (33) is provided in the liquid inlet portion (25), and the bottom end of the float chamber (33) is in communication with the liquid inlet portion (25); A float (36) is provided in the float chamber (33), and the bottom end of the gate plate (31) is fixedly connected to the float (36). When the float (36) rises or falls under the action of buoyancy, it drives the gate plate (31) to move in the vertical direction.

2. A rectification and purification device for electronic-grade isopropylamine according to claim 1, characterized in that: A connecting piece (24) is provided above the floating plate (23), and each floating plate (23) is fixedly connected to the connecting piece (24).

3. A rectification and purification device for electronic-grade isopropylamine according to claim 2, characterized in that: The height of the liquid inlet channel is set to be higher than the liquid outlet channel.

4. A rectification and purification device for electronic-grade isopropylamine according to claim 3, characterized in that: A liquid inlet (27) is provided on one side of the inner panel (13), and the liquid inlet (27) is used to connect the liquid inlet portion (25) and the liquid inlet channel. A liquid discharge port (29) is provided on the other side of the inner panel (13), and the liquid discharge port (29) is used to connect the liquid discharge portion (28) and the liquid discharge channel. The upper end of the liquid inlet (27) is lower than the upper end of the partition (15), and the bottom end of the liquid inlet (27) is flush with the bottom end of the liquid inlet channel; The bottom end of the liquid inlet portion (25) is flush with the bottom end of the liquid inlet channel.

5. A rectification and purification device for electronic-grade isopropylamine according to claim 4, characterized in that: A cofferdam (26) is provided in the liquid inlet portion (25), and the cofferdam (26) serves as a barrier for the liquid inlet (27), and the cofferdam (26) corresponds to the liquid inlet (27) in a one-to-one manner; The upper end of the cofferdam (26) is higher than the upper end of the liquid inlet (27); A baffle (111) is fixedly provided in the downcomer (11), and the baffle (111) is located directly above the cofferdam (26).

6. A rectification and purification device for electronic-grade isopropylamine according to claim 5, characterized in that: The upper end of the inner panel (13) is higher than the upper end of the partition (15); The inner enclosure plate (13) is provided with an overflow port (37) at the overflow portion (30), and the upper end of the overflow port (37) is flush with the upper end of the partition plate (15).

7. A rectification and purification device for electronic-grade isopropylamine according to claim 6, characterized in that: One side of the overflow portion (30) is connected to an overflow pipe (6), and a first connecting pipe (7) is provided outside the tower body (1), and the overflow pipe (6) is connected to the first connecting pipe (7); A temporary storage tank (8) is provided outside the tower body (1), the first connecting pipe (7) is in communication with the temporary storage tank (8), and the feed pipe (2) is in communication with a downcomer (11); A second connecting pipe (9) is connected between the temporary storage tank (8) and the feed pipe (2), and a reflux pump (10) is installed on the second connecting pipe (9).

8. A method for rectifying and purifying electronic-grade isopropanolamine, suitable for the rectifying and purifying device for electronic-grade isopropanolamine according to any one of claims 1 to 7, characterized in that: The following steps are involved: Step 1: The isopropanolamine mixed solution is heated and then introduced into the feed pipe (2); Step 2: Evenly feed the isopropylamine mixed solution into each liquid inlet channel at the liquid inlet portion (25) of the tray (12); Step 3: Steam is introduced into the bottom of the tower body (1) and allowed to enter the liquid inlet channel, and gas-liquid exchange is performed in the liquid inlet channel. During the gas-liquid exchange, the lower surface of the floating plate (23) is always in contact with the isopropylamine mixed liquid, and the liquid after the exchange is completed is introduced into the liquid outlet channel; Step 4: collecting gaseous products through the gaseous phase collecting pipe (3) at the top of the tower body (1), and collecting liquid products through the liquid phase collecting pipe (4) at the bottom of the tower body (1); Step 5: When the liquid flow in the tray (12) is too large, the gate (31) is lifted to allow the excess liquid to flow into the overflow portion (30); Step 6: The liquid at the overflow portion (30) is passed into the temporary storage tank (8). When the liquid flow rate in the tray (12) is low, the liquid in the temporary storage tank (8) is sent to the feed pipe (2).

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