A distillation tower and a process for producing ultrapure arsine

Abstract

The present invention discloses a distillation tower and a process for producing ultrapure arsine, and relates to the field of distillation processing technology, including a distillation component and a homogenization component, wherein the distillation component includes a tower body, a packing member is fixed on the tower body, an air inlet valve is fixed on the bottom of the outer ring of the tower body, and a liquid inlet valve is fixed on the top of the outer ring of the tower body; the homogenization component is arranged in the tower body, including a liquid distribution member installed in the tower body, including a fixed frame fixed in the tower body, a drainage shell is embedded on the fixed frame, a vertical rod is slid on the fixed frame, and a collection frame is arranged on the top of the fixed frame. The beneficial effect of the present invention is that through the arrangement of the homogenization component, a diversion operation can be performed when the liquid phase increases according to the amount of liquid phase falling, thereby improving the uniform distribution processing efficiency, and at the same time changing the space of the gas phase distribution point to avoid the occurrence of liquid flooding, so that the liquid phase and the gas phase can have good countercurrent contact between the packing, thereby ensuring the overall distillation processing efficiency.

Description

Technical Field

[0001] The invention relates to the technical field of distillation processing, in particular to a distillation tower and a process for producing ultrapure arsine using the distillation tower. Background Art

[0002] The production process of arsine mainly includes two major links: synthesis and purification. In the purification link, the distillation tower is a key equipment that achieves separation through multiple gas-liquid exchanges. A condenser is provided on the top of the tower (for condensation and reflux of light components) and a reboiler is provided at the bottom of the tower (for evaporation of heavy components). Through low-temperature distillation operation, non-condensable gases (such as hydrogen) with a large difference in boiling point from arsine and some volatile impurities can be effectively separated.

[0003] For packed distillation towers, the distillation towers in the prior art generally adopt a continuous distillation method, continuously introducing the liquid phase and the gas phase, and using a distributor to ensure uniform countercurrent contact between the gas and the liquid. When the amount of liquid phase falling increases, the processing time of the fixed distributor increases, and the distribution point is easily blocked or the liquid flow is incompletely covered, which reduces the mass transfer efficiency and affects the subsequent uniformity of the countercurrent contact between the gas and the liquid. Summary of the invention

[0004] In view of the above problems existing in the existing distillation tower, the present invention is proposed.

[0005] Therefore, the problem to be solved by the present invention is that when the amount of liquid falling in the distillation tower in the prior art increases, the processing time of the fixed distributor increases, and distribution point blockage or incomplete liquid flow coverage is prone to occur, thereby reducing the mass transfer efficiency and affecting the uniformity of subsequent gas-liquid countercurrent contact.

[0006] In order to solve the above technical problems, the first object of the present invention is to provide a distillation tower, which includes a plurality of movably connected distillation components and a homogenization component arranged between two adjacent distillation components, wherein:

[0007] Each distillation assembly comprises a tower body, a packing member is fixed to the tower body, an air inlet valve is fixed to the bottom of the outer ring of the tower body at the lowest end, and a liquid inlet valve is fixed to the top of the outer ring of the tower body at the highest end;

[0008] Each homogenizing component is arranged in the tower body, including a liquid distribution part and a gas distribution part installed in the tower body. The liquid distribution part includes a fixed frame fixed in the tower body, a plurality of drainage shells are embedded in the fixed frame, a plurality of vertical rods are penetrated through the edge of the fixed frame, and the vertical rods are in sliding contact with the fixed frame. An annular collecting frame is arranged on the top of the fixed frame, a plurality of diversion pipes are fixed on the bottom of the collecting frame, a water diversion hole is opened on the tube wall of each of the diversion pipes, and a collecting bucket is arranged on the inner side of the collecting frame. The gas distribution part is arranged below the fixed frame, and the gas distribution part includes an annular auxiliary frame fixed in the tower body, a displacement plate is arranged on the top of the auxiliary frame, a plurality of auxiliary gas holes are opened on the displacement plate, and a plurality of slides are slidably connected to the top of the displacement plate.

[0009] As a preferred embodiment of the distillation tower described in the present invention, a plurality of water holes are provided on the outer edge wall of the drainage shell, the top end of the vertical rod is fixed to the bottom of the collecting bucket, a first spring is sleeved on the vertical rod, one end of the first spring is fixedly connected to the fixing frame, the other end of the first spring is fixed to the vertical rod, a second spring is fixed to the bottom of the vertical rod, and the other end of the second spring is fixed to the displacement disk.

[0010] As a preferred solution of the distillation tower described in the present invention, a plurality of first main air holes are opened on the top of the displacement plate, a plurality of second main air holes are opened on the slide plate, and the second main air holes cooperate with the first main air holes.

[0011] As a preferred solution of the distillation tower described in the present invention, a second positioning seat is fixed to one side of the slide, a first positioning seat is fixed to the outer ring of the vertical rod, and a connecting rod is rotatably connected between the second positioning seat and the first positioning seat.

[0012] As a preferred solution of the distillation tower described in the present invention, the collecting hopper is provided with a through hole and cooperates with the drainage shell, an annular drainage hopper is arranged on the top of the collecting hopper, and the outer edge of the drainage hopper is fixed in the tower body.

[0013] As a preferred solution of the distillation tower described in the present invention, an elastic pad is fixed to the inner wall of the collecting frame, and the elastic pad is arranged obliquely.

[0014] As a preferred solution of the distillation tower described in the present invention, a T-block is fixed at the bottom of the slide, a T-slot is opened at the top of the displacement plate and cooperates with the T-block, a plurality of guide rods are fixed at the top of the auxiliary frame, the top of the guide rod passes through the displacement plate, and the guide rod is slidably connected to the displacement plate.

[0015] As a preferred solution of the distillation tower described in the present invention, a reflux nozzle is embedded in the top of the inner cavity of the tower body at the uppermost end, and a grid-type gas distributor is fixed at the bottom of the inner cavity of the tower body at the lowermost end.

[0016] As a preferred embodiment of the distillation tower described in the present invention, an exhaust valve is fixed at the top center of the tower body located at the uppermost end, and a drain valve is fixed at the bottom center of the tower body located at the lowermost end.

[0017] The second object of the present invention is to provide a process for producing ultrapure arsine using the above-mentioned distillation tower, which comprises the following steps:

[0018] (1) When the reactor is in a stirring state, a set amount of concentrated sulfuric acid is slowly added, and a screw feeder is used to control the addition of a set amount of zinc arsenide. The temperature of the reactor is controlled to be 40 to 70 degrees Celsius, the reaction pressure is 0 to 0.25 MPa, and the reaction time is 1 to 6 hours to generate crude arsine;

[0019] (2) The crude arsine is extracted and passed through a primary condenser, a secondary condenser and a constant pressure buffer tank in sequence, the temperature of the primary condenser is controlled to be between -22°C and -18°C, the temperature of the secondary condenser is controlled to be between -42°C and -38°C, and the pressure of the constant pressure buffer tank is controlled to be 0.2 MPa;

[0020] (3) extracting arsine from the constant pressure buffer tank and sequentially entering the first distillation tower, the second distillation tower and the adsorption column to obtain ultrapure arsine, controlling the temperature of the first distillation tower to be between -48 degrees Celsius and -46 degrees Celsius and the pressure to be 0.2 MPa, and controlling the temperature of the second distillation tower to be between -44 degrees Celsius and -42 degrees Celsius and the pressure to be 0.2 MPa; and

[0021] (4) Filling the ultra-pure arsine obtained after adsorption.

[0022] The beneficial effects of the present invention are as follows: by setting up the homogenizing component, a diversion operation can be performed when the liquid phase increases according to the amount of liquid phase falling, thereby improving the uniform distribution processing efficiency, and at the same time changing the space of the gas phase distribution point to avoid liquid flooding, so that the liquid phase and the gas phase can have good countercurrent contact between the fillers, thereby ensuring the overall distillation processing efficiency, and can be well applied in a multi-stage high distillation tower. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without paying creative labor.

[0024] Figure 1 The structural diagram of the distillation tower provided by the present invention.

[0025] Figure 2 A cross-sectional view of a distillation tower provided by the present invention.

[0026] Figure 3 This is a structural diagram of the distillation components of the distillation tower provided by the present invention.

[0027] Figure 4 A separation diagram of the packing elements of the distillation tower provided by the present invention.

[0028] Figure 5 A cross-sectional view of a homogenizing component of a distillation tower provided by the present invention.

[0029] Figure 6 A separation diagram of the liquid distribution components of the distillation tower provided by the present invention.

[0030] Figure 7 The distillation tower provided by the present invention Figure 6 Enlarged view of point A in the middle.

[0031] Figure 8 The distillation tower provided by the present invention Figure 6 Enlarged view of point B in the middle.

[0032] Fig. 9 A separation diagram of the gas distribution components of the distillation tower provided by the present invention.

[0033] Fig.10 The distillation tower provided by the present invention Fig. 9 Enlarged view of center C.

[0034] Fig.11 A top view of the local structure of the distillation tower provided by the present invention.

[0035] Fig.12 The present invention is a schematic diagram of a process for producing ultrapure arsine using the distillation tower provided by the present invention.

[0036] In the figure: 100, distillation assembly; 101, tower body; 102, packing member; 103, air inlet valve; 104, liquid inlet valve; 105, reflux nozzle; 106, grid-type gas distributor; 107, exhaust valve; 108, drain valve; 200, homogenization assembly; 201, liquid distribution member; 201a, fixing frame; 201a-1, drainage shell; 201a-2, water hole; 201a-3, vertical rod; 201a-4, first spring; 201a-5, first positioning seat; 201a-6, second spring; 201b, collection frame; 201a-7, second spring; 201c, collection frame; 201d, first spring; 201d, second ... 1b-1, diversion pipe; 201b-2, water diversion hole; 201b-3, elastic pad; 201c, collecting bucket; 201c-1, through hole; 201d, drainage bucket; 202, gas distribution part; 202a, auxiliary frame; 202a-1, guide rod; 202b, displacement plate; 202b-1, auxiliary gas hole; 202b-2, first main gas hole; 202b-3, T-slot; 202c, slide plate; 202c-1, second main gas hole; 202c-2, second positioning seat; 202c-3, connecting rod; 202c-4, T-block. DETAILED DESCRIPTION

[0037] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific implementation methods of the present invention are described in detail below in conjunction with the accompanying drawings.

[0038] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein, and those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0039] Secondly, the term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The term "in one embodiment" that appears in different places in this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive with other embodiments.

[0040] Example 1

[0041] Reference Figure 1 and Figure 2 , which is the first embodiment of the present invention, and this embodiment provides a distillation tower. The distillation tower for producing ultra-pure arsine includes a distillation component 100 and a homogenization component 200. Through the arrangement of the homogenization component 200, when facing the liquid phase that changes and falls dynamically during the distillation process, when the amount of liquid phase falling increases, a diversion operation is performed to improve the uniform distribution processing efficiency, and at the same time, the space of the gas phase distribution point is changed, so that the liquid phase and the gas phase can have good countercurrent contact between the fillers, thereby ensuring the overall distillation processing efficiency.

[0042] Specifically, the distillation assembly 100 is of a multi-stage design, which includes a plurality of tower bodies 101, and each individual tower body 101 is connected by a sealing flange. This design can flexibly increase or decrease the number of tower bodies 101 and assemble them according to the actual purification and processing requirements of arsine, adjust the overall height of the distillation assembly 100, and also facilitate the inspection or cleaning of the internal components of the tower body 101 in a disassembled state.

[0043] like Figure 3 As shown, a packing member 102 is fixed in each tower body 101, wherein a reflux nozzle 105 is embedded in the top of the inner cavity of the tower body 101 at the uppermost end, and a grid-type gas distributor 106 is fixed at the bottom of the inner cavity of the tower body 101 at the lowermost end. Through the setting of the reflux nozzle 105, the condensed liquid can be re-injected with the assistance of an external pump, and the reflux nozzle 105 is homogenized and sprayed into the tower body 101. Through the setting of the grid-type gas distributor 106, the preliminary uniform treatment of the gas can be achieved, and at the same time, the structure is relatively simple and the pressure drop is low, which significantly improves the gas-liquid mass transfer efficiency.

[0044] An exhaust valve 107 is fixed at the top center of the uppermost tower body 101, and a drain valve 108 is fixed at the bottom center of the lowermost tower body 101. An air intake valve 103 is fixed at the bottom of the outer ring of the tower body 101 at the second lower end, and a liquid intake valve 104 is fixed at the top of the outer ring of the tower body 101 at the second upper end.

[0045] The packing member 102 includes a packing material and two support plates. The support plates are fixed in the tower body 101 , and the packing material is placed between the two support plates.

[0046] The homogenizing assembly 200 is arranged in the tower body 101, and includes a liquid distribution component 201 and a gas distribution component 202 installed in the tower body 101. The liquid distribution component 201 includes a fixed frame 201a fixed in the tower body 101, and a plurality of drainage shells 201a-1 are embedded in the fixed frame 201a. A plurality of vertical rods 201a-3 are penetrated through the edge of the fixed frame 201a, and the vertical rods 201a-3 are in sliding contact with the fixed frame 201a. An annular collecting frame 201b is arranged on the top of the fixed frame 201a, and a plurality of diversion pipes 201b-1 are fixed at the bottom of the collecting frame 201b. A plurality of water diversion holes 201b-2 are opened on the pipe wall of the diversion pipe 201b-1, and a collecting bucket 201c is arranged on the inner side of the collecting frame 201b. The gas distribution member 202 is arranged below the fixed frame 201a, and includes an annular auxiliary frame 202a fixed in the tower body 101. A displacement plate 202b is arranged on the top of the auxiliary frame 202a. A plurality of auxiliary gas holes 202b-1 are evenly distributed on the displacement plate 202b. A plurality of slide plates 202c are slidably connected to the top of the displacement plate 202b.

[0047] The number of vertical rods 201a-3 and shunt tubes 201b-1 can be flexibly increased or decreased according to actual needs. In the present application, the number of vertical rods 201a-3 is four, and the number of shunt tubes 201b-1 is also four.

[0048] The fixed frame 201a and the auxiliary frame 202a are both fixed in the tower body 101 by bolts and are designed to be detachable, which is convenient for subsequent maintenance or cleaning.

[0049] The arrangement of the diverter pipe 201b-1 and the water diverter hole 201b-2 can drain and transfer the liquid in the collection frame 201b, and evenly diffuse it into the tower body 101 through multiple water diverter holes 201b-2, thereby helping to improve the uniformity of liquid phase distribution and facilitating subsequent uniform gas-liquid contact.

[0050] The provision of the auxiliary gas holes 202 b - 1 can satisfy the requirement of uniform distribution of the rising gas and ensure uniform distribution of the gas in the tower body 101 .

[0051] Example 2

[0052] Reference Figure 2 to Figure 11 , which is the second embodiment of the present invention, and this embodiment is based on the previous embodiment.

[0053] Specifically, Figure 7 As shown, the outer edge wall of each drainage shell 201a-1 is provided with a plurality of water holes 201a-2, the top end of the vertical rod 201a-3 is fixed to the bottom of the collecting bucket 201c, a first spring 201a-4 is sleeved on the vertical rod 201a-3, one end of the first spring 201a-4 is fixedly connected to the fixing frame 201a, the other end of the first spring 201a-4 is fixed to the vertical rod 201a-3, a second spring 201a-6 is fixedly connected to the bottom of the vertical rod 201a-3, and the other end of the second spring 201a-6 is fixedly connected to the displacement plate 202b.

[0054] A through hole 201c-1 is provided on the collecting bucket 201c, and cooperates with the drainage shell 201a-1. Through the setting of the drainage shell 201a-1, the water hole 201a-2 and the through hole 201c-1, the space requirement of the drainage shell 201a-1 can be met. Then, according to the position of the collecting bucket 201c on the drainage shell 201a-1, the liquid temporarily stored in the collecting bucket 201c can be discharged through different numbers of water holes 201a-2, and according to the protruding height of the drainage shell 201a-1 on the collecting bucket 201c, the liquid can be guided to fall by multiple water holes 201a-2.

[0055] By disposing the first spring 201a - 4 , an elastic supporting force can be provided for the vertical rod 201a - 3 , thereby preventing the vertical rod 201a - 3 and the collecting bucket 201c from being randomly displaced without the action of external force.

[0056] By setting the second spring 201a-6, a certain distance can be maintained between the collecting bucket 201c and the displacement plate 202b without external force, and when the collecting bucket 201c moves down a certain distance, the displacement plate 202b will move down accordingly.

[0057] like Fig.10 As shown, the displacement plate 202b is provided with a first main air hole 202b-2, and the slide plate 202c is provided with a plurality of second main air holes 202c-1, which cooperate with the first main air holes 202b-2. In this non-limiting embodiment, the first main air holes 202b-2 are distributed in the center of the displacement plate 202b, and the auxiliary air holes 202b-1 are distributed in the outer side of the displacement plate 202b.

[0058] Since the slide plate is slidably connected to the top of the displacement plate 202b, when the slide plate 202c is slid, the gas flow space can be adjusted through the overlapping area of ​​the first main air hole 202b-2 and the second main air hole 202c-1. When the slide plate 202c slides and the overlapping area of ​​the first main air hole 202b-2 and the second main air hole 202c-1 increases, the gas transmission space increases, the resistance is small, the pressure drop is reduced, and the risk of liquid flooding is effectively reduced.

[0059] like Fig. 9 As shown, in this embodiment, the number of slide plates 202c is four and they are distributed on the top of the displacement plate 202b. This design can realize the coordination of multiple second main air holes 202c-1 and first main air holes 202b-2 to complete multi-point gas transmission space adjustment and cooperate with the auxiliary air holes 202b-1 to meet the requirements of gas phase homogenization distribution.

[0060] like Fig.10 As shown, one side of the slide plate 202c is fixedly connected to the second positioning seat 202c-2, the outer ring of the vertical rod 201a-3 is fixedly connected to the first positioning seat 201a-5, and a connecting rod 202c-3 is rotatably connected between the second positioning seat 202c-2 and the first positioning seat 201a-5.

[0061] By setting the second positioning seat 202c-2, the first positioning seat 201a-5 and the connecting rod 202c-3, a transmission connection can be achieved. When the displacement disk 202b cannot move further downward, the vertical rod 201a-3 moves further downward, and cooperates with the connecting rod 202c-3 to push the slide plate 202c to move toward the center of the displacement disk 202b.

[0062] An annular drainage hopper 201d is provided on the top of the collecting hopper 201c, and the outer edge of the drainage hopper 201d is fixedly connected to the tower body 101.

[0063] The drainage bucket 201d is installed in the tower body 101 by bolts, and the drainage bucket 201d and the tower body 101 are sealed. The top of the drainage bucket 201d is inclined. This design can facilitate the liquid falling from the upper level to be collected by the drainage bucket 201d and introduced into the collection bucket 201c.

[0064] like Figure 8 As shown, an elastic pad 201b-3 is fixedly connected to the inner wall of the collecting frame 201b, and the elastic pad 201b-3 is inclined.

[0065] A slot is provided on the elastic pad 201b-3, and the vertical rod 201a-3 passes through the elastic pad 201b-3, thereby meeting the movement space requirements of the vertical rod 201a-3 and the first spring 201a-4 to avoid obstruction. The inclined elastic pad 201b-3 can guide the liquid overflowing through the collection bucket 201c and transmit it to the collection frame 201b. When the collection bucket 201c moves downward, the elastic pad 201b-3 produces elastic deformation to avoid obstruction.

[0066] like Fig.10 As shown, a T-block 202c-4 is fixed at the bottom of the slide plate 202c, a T-slot 202b-3 is opened on the top of the displacement plate 202b and cooperates with the T-block 202c-4, and a plurality of guide rods 202a-1 are fixed on the top of the auxiliary frame 202a, the top of the guide rod 202a-1 passes through the displacement plate 202b, and the guide rod 202a-1 is slidably connected to the displacement plate 202b.

[0067] Specifically, the length of the T-block 202c-4 is smaller than the inner diameter of the T-slot 202b-3, and the T-block 202c-4 slides in the T-slot 202b-3, thereby guiding the movement direction of the slide plate 202c through the setting of the T-block 202c-4 and the T-slot 202b-3, preventing the slide plate 202c from moving up, down, forward or backward at will, and can also play a role in positioning and guiding, ensuring the displacement stability of the slide plate 202c, and preventing the slide plate 202c from separating from the displacement plate 202b.

[0068] By providing the guide rod 202a-1, the displacement plate 202b can be guided to move up and down, thereby improving the movement stability of the displacement plate 202b.

[0069] Therefore, when in use, the pretreated liquid arsine is introduced through the liquid inlet valve 104, and in conjunction with the external reboiler, steam is introduced through the air inlet valve 103, the gas phase and the liquid phase are gathered and contacted in the filler 102, the falling liquid phase is countercurrently contacted with the rising steam, and the non-volatile impurities are enriched at the bottom of the tower, so that the purity of the volatile arsine in the gas phase is gradually improved, and in conjunction with the external condenser and reboiler, the liquid formed after the gas is condensed is pumped into the tower body 101 again through the reflux nozzle 105, completing the multi-stage distillation treatment to meet the production and processing needs.

[0070] The upward steam is pre-distributed by the grid-type gas distributor 106 and then enters the multi-stage packing member 102 . The downward liquid is pre-distributed by the reflux nozzle 105 and then also enters the multi-stage packing member 102 . It is further homogenized by the liquid distribution member 201 and the gas distribution member 202 between the multi-stage packing members 102 .

[0071] The liquid falls into the collecting bucket 201c under the guidance of the drainage bucket 201d, enters the drainage shell 201a-1 through the water hole 201a-2 for distribution, and then falls again to the next-level filler 102; the gas rises through the auxiliary air hole 202b-1 and the first main air hole 202b-2 for distribution and then enters the filler 102.

[0072] During the multi-stage distillation process, when the amount of liquid falling increases, the collecting bucket 201c will be weighed and move downward. Since the through hole 201c-1 exists to provide movement space for the drainage shell 201a-1, the through hole 201c-1 is located on the collecting bucket 201c and moves downward, and more water holes 201a-2 are gradually exposed, so that the liquid enters the drainage shell 201a-1 through the water holes 201a-2 and then falls, accelerating the uniform fall of the liquid and avoiding liquid retention. The vertical rod 201a-3 moves together with the collecting bucket 201c, and the first spring 201a-4 is compressed. When the liquid temporarily stored in the collecting bucket 201c is discharged, the collecting bucket 201c will automatically reset under the elastic support of the first spring 201a-4.

[0073] When the amount of liquid falling further increases, the multiple water holes 201a-2 are unable to quickly discharge the temporarily stored liquid. In this state, the collecting bucket 201c will move further downward, and the excess liquid will overflow and be placed in the collecting frame 201b with the assistance of the elastic pad 201b-3. After being conducted by the diversion pipe 201b-1, it will be diverted and fall through the diversion hole 201b-2.

[0074] When the collecting bucket 201c moves further downward, under the elastic connection of the second spring 201a-6, the displacement plate 202b will move downward and contact the auxiliary frame 202a. At this time, the displacement plate 202b cannot move again. As the collecting bucket 201c and the vertical rod 201a-3 move downward, the second spring 201a-6 is compressed. Under the connection of the connecting rod 202c-3, the slide plate 202c slides inward, increasing the overlapping area of ​​the second main air hole 202c-1 and the first main air hole 202b-2.

[0075] The overlapping area of ​​the second main air hole 202c-1 and the first main air hole 202b-2 increases to form a large hole for gas to pass through, and the large holes are evenly distributed. The large hole setting reduces the gas velocity, reduces the risk of liquid flooding, and maintains a stable gas distribution, thereby optimizing the contact efficiency. At this time, the auxiliary air hole 202b-1 is located on the outside of the slide plate 202c compared to the small hole design. When the gas passes through, small and uniform bubbles are formed, which enhances the gas-liquid contact area and improves the mass transfer efficiency. The combination of the two is more in line with actual needs.

[0076] In the above process, the distance between the collecting bucket 201c and the displacement disk 202b is reduced. When the liquid flow rate is large, the liquid tends to flow down quickly along the tower wall or local area, which is the channeling phenomenon. Shortening the distance between the two can increase the redistribution frequency, force the liquid to be redispersed, and reduce the problem of uneven liquid distribution. After the liquid falls quickly and evenly, with the cooperation of the second spring 201a-6 and the first spring 201a-4, the collecting bucket 201c can be well reset to meet the dynamic distribution homogenization requirements.

[0077] Example 3

[0078] Reference Figure 3 to Figure 11 , which is the third embodiment of the present invention, and is based on the first two embodiments.

[0079] Specifically, the elastic pad 201b-3 is embedded with a narrow spring steel sheet, which has high elastic limit, high strength, excellent fatigue resistance, good ductility and corrosion resistance, and is used to increase the overall elasticity of the elastic pad 201b-3, maintain the elastic pad 201b-3 in an initial inclined upward state, guide the overflowing liquid well and introduce it into the collection frame 201b, and produce elastic deformation when the collection bucket 201c moves downward, and can quickly return to its original state when the collection bucket 201c is reset. In the actual distillation process, when the collection bucket 201c repeatedly moves, it can still ensure its own good elasticity.

[0080] There are a plurality of water holes 201a-2 distributed in a circular array on the drainage shell 201a-1, and the inner diameter of the vertical water holes 201a-2 gradually increases from top to bottom, that is, the inner diameter of the bottom water hole 201a-2 is larger than the inner diameter of the top water hole 201a-2. With this design, when the temporary storage amount of liquid increases and causes the collecting bucket 201c to gradually move downward, the water holes 201a-2 with larger inner diameters are gradually exposed, which can guide the liquid to fall and discharge more quickly.

[0081] According to the actual specifications of the tower body 101 and the requirements for gas-liquid homogenization during distillation, the number of the first main air holes 202b-2 and the auxiliary air holes 202b-1 can be flexibly increased or decreased to ensure that the number of the second main air holes 202c-1 is consistent with the number of the first main air holes 202b-2, and the slide plate 202c can cover several first main air holes 202b-2.

[0082] In summary, compared with the prior art, the present device can dynamically adjust the liquid phase distribution and the gas phase distribution according to the amount of liquid phase falling during the distillation process through the setting of the homogenization component 200, thereby ensuring the uniformity of transmission of the two and ensuring the overall distillation processing efficiency.

[0083] Example 4

[0084] like Fig.12 As shown, it is a schematic diagram of the process flow of producing ultrapure arsine using the above-mentioned distillation tower. In this embodiment, first, 5400g of deionized water is added to the reactor A, stirring is turned on, the reactor A is heated to 30°C, 2000g of 98% concentrated sulfuric acid is slowly added, the temperature of the reactor A is controlled not to exceed 40°C, and then 1800g of zinc arsenide is gradually added, sulfuric acid and zinc arsenide react to release heat, the zinc arsenide addition rate is controlled, the reaction liquid temperature is maintained at 40°C, the rotation speed is 120r / min, the system pressure is maintained at 0.2MPa, and the generated arsine crude gas is extracted, and no gas is generated after 5h of reaction, and the reaction is terminated.

[0085] The crude arsine generated by the reaction is extracted into the primary condenser B, and the temperature of the primary condenser B is controlled at -20±2°C; the crude arsine after impurities are removed by the primary condenser B enters the secondary condenser C for deep impurities removal, and the temperature of the secondary condenser C is controlled at -40±2°C; the crude arsine after impurities are removed by the secondary condenser C enters the constant pressure buffer tank D, and the pressure of the constant pressure buffer tank D is controlled at 0.2MPa.

[0086] The arsine produced through the constant pressure buffer tank D is sequentially fed into distillation tower E and distillation tower F, the temperature of distillation tower E is controlled at -47±1°C and the pressure is 0.2MPa, and low-boiling-point impurities are produced from the top of distillation tower E; the arsine produced through distillation tower E enters distillation tower F, the temperature of distillation tower F is controlled at -43±1°C and the pressure is 0.2MPa, and high-boiling-point impurities are produced from the bottom of the tower; the arsine produced through distillation tower F sequentially enters three adsorption columns, namely, adsorption column G, adsorption column H, and adsorption column I, which are respectively filled with activated carbon and molecular sieve combination adsorbents, and ultra-pure arsine is obtained after adsorption.

[0087] The ultrapure arsine obtained is cryogenically filled, the cryogenic filling inlet pressure is 0.16 MPa, and the liquid level height of the liquid nitrogen tank N is 1 / 3 of the height of the cylinder M.

[0088] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, which should all be included in the scope of the claims of the present invention.

Claims

1. A distillation tower, characterized in that: It comprises a plurality of movably connected distillation assemblies (100) and a homogenization assembly (200) arranged between two adjacent distillation assemblies (100), wherein: Each distillation assembly (100) comprises a tower body (101), a packing member (102) being fixed inside the tower body (101), an air inlet valve (103) being fixedly arranged at the bottom of the tower body (101) at the lowest end, and a liquid inlet valve (104) being fixedly arranged at the top of the tower body (101) at the highest end; Each homogenizing assembly (200) is arranged in a tower body (101), and comprises a liquid distribution component (201) and a gas distribution component (202) installed in the tower body (101); the liquid distribution component (201) comprises a fixing frame (201a) fixed in the tower body (101); a plurality of drainage shells (201a-1) are embedded in the fixing frame (201a); a plurality of vertical rods (201a-3) are arranged through the edge of the fixing frame (201a); the vertical rods (201a-3) are in sliding contact with the fixing frame (201a); an annular collection frame (201b) is arranged on the top of the fixing frame (201a); a plurality of gas collecting frames (201b) are fixed on the bottom of the collecting frame (201b); A plurality of flow distribution pipes (201b-1), each of the flow distribution pipes (201b-1) having a plurality of water distribution holes (201b-2) formed on the pipe wall, a collection bucket (201c) being provided inside the collection frame (201b), the gas distribution component (202) being provided below the fixed frame (201a), the gas distribution component (202) comprising an annular auxiliary frame (202a) fixed inside the tower body (101), a displacement plate (202b) being provided on the top of the auxiliary frame (202a), a plurality of auxiliary gas holes (202b-1) being formed on the displacement plate (202b), and a plurality of slide plates (202c) being slidably connected to the top of the displacement plate (202b); The outer edge wall of the drainage shell (201a-1) is provided with a plurality of water holes (201a-2); the top end of the vertical rod (201a-3) is fixed to the bottom of the collecting bucket (201c); a first spring (201a-4) is sleeved on the vertical rod (201a-3); one end of the first spring (201a-4) is fixedly connected to the fixing frame (201a); the other end of the first spring (201a-4) is fixed to the vertical rod (201a-3); a second spring (201a-6) is fixed to the bottom of the vertical rod (201a-3); the other end of the second spring (201a-6) is fixed to the displacement plate (202b); The collecting hopper (201c) is provided with a through hole (201c-1) and cooperates with the drainage shell (201a-1); an annular drainage hopper (201d) is provided on the top of the collecting hopper (201c); and the outer edge of the drainage hopper (201d) is fixed in the tower body (101).

2. The distillation tower according to claim 1, characterized in that: The top of the displacement plate (202b) is provided with a plurality of first main air holes (202b-2), the slide plate (202c) is provided with a plurality of second main air holes (202c-1), and the second main air holes (202c-1) cooperate with the first main air holes (202b-2).

3. The distillation tower according to claim 2, characterized in that: A second positioning seat (202c-2) is fixed on one side of the slide plate (202c), a first positioning seat (201a-5) is fixed on the outer ring of the vertical rod (201a-3), and a connecting rod (202c-3) is rotatably connected between the second positioning seat (202c-2) and the first positioning seat (201a-5).

4. The distillation tower according to claim 1, characterized in that: An elastic pad (201b-3) is fixed to the inner wall of the collection frame (201b), and the elastic pad (201b-3) is arranged in an inclined manner.

5. The distillation tower according to claim 1, characterized in that: A T-shaped block (202c-4) is fixed at the bottom of the slide plate (202c), a T-shaped slot (202b-3) is provided at the top of the displacement plate (202b) and cooperates with the T-shaped block (202c-4), a plurality of guide rods (202a-1) are fixed at the top of the auxiliary frame (202a), the top ends of the guide rods (202a-1) penetrate the displacement plate (202b), and the guide rods (202a-1) are slidably connected to the displacement plate (202b).

6. The distillation tower according to claim 1, characterized in that: A reflux nozzle (105) is embedded in the top of the inner cavity of the tower body (101) at the uppermost end, and a grid-type gas distributor (106) is fixed to the bottom of the inner cavity of the tower body (101) at the lowermost end.

7. The distillation tower according to claim 1, characterized in that: An exhaust valve (107) is fixed at the center of the top of the tower body (101) at the uppermost end, and a drain valve (108) is fixed at the center of the bottom of the tower body (101) at the lowermost end.

8. A process for producing ultrapure arsine, using a distillation tower as claimed in any one of claims 1 to 7, characterized in that: The following steps are involved: (1) When the reactor is in a stirring state, a set amount of concentrated sulfuric acid is slowly added, and a screw feeder is used to control the addition of a set amount of zinc arsenide. The temperature of the reactor is controlled to be 40 to 70 degrees Celsius, the reaction pressure is 0 to 0.25 MPa, and the reaction time is 1 to 6 hours to generate crude arsine; (2) The crude arsine is extracted and passed through a primary condenser, a secondary condenser and a constant pressure buffer tank in sequence, the temperature of the primary condenser is controlled to be between -22°C and -18°C, the temperature of the secondary condenser is controlled to be between -42°C and -38°C, and the pressure of the constant pressure buffer tank is controlled to be 0.2 MPa; (3) extracting arsine from the constant pressure buffer tank and sequentially entering the first distillation tower, the second distillation tower and the adsorption column to obtain ultrapure arsine, controlling the temperature of the first distillation tower to be between -48 degrees Celsius and -46 degrees Celsius and the pressure to be 0.2 MPa, and controlling the temperature of the second distillation tower to be between -44 degrees Celsius and -42 degrees Celsius and the pressure to be 0.2 MPa; and (4) Filling the ultra-pure arsine obtained after adsorption.

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