A multi-stage adsorption impurity removal device and a production process for ultra-pure arsine

Abstract

The present invention relates to the field of ultrapure arsine processing, and specifically to a multi-stage adsorption and impurity removal device and a production process for ultrapure arsine, wherein the impurity removal device comprises an adsorption device; the adsorption device comprises a primary adsorption tower and a secondary adsorption tower, the primary adsorption tower and the secondary adsorption tower are connected in series through a pipeline, and a propulsion device is provided in the primary adsorption tower and the secondary adsorption tower; the propulsion device comprises a propulsion box, a piston plate and a linear drive assembly; the propulsion box is arranged at a propulsion section, and a top plate and a bottom plate are respectively provided at both ends of the propulsion box, and the top plate and the bottom plate are connected to a packing section; the piston plate is slidably arranged in the propulsion box, and the internal cavity of the propulsion box is divided into a first cavity and a second cavity by the piston plate; the linear drive assembly is arranged on the propulsion box. The present invention realizes the function of stably conveying gas during large-scale production through the adsorption device and the propulsion device, and solves the problem that the high-pressure transmitted gas will be blocked or refluxed when entering multiple adsorption towers connected in series.

Description

Technical Field

[0001] The invention relates to the field of ultrapure arsine processing, and in particular to a multi-stage adsorption and impurity removal device and a production process thereof for ultrapure arsine. Background Art

[0002] In the production process of ultra-pure arsine, adsorption towers are usually used for adsorption and impurity removal. Adsorption towers are often used for gas separation. They adsorb impurities (such as harmful gases, odors, etc.) in the gas through the medium to achieve the purpose of purifying air, purifying waste gas, purifying air conditioning systems, purifying industrial gases, etc. However, existing adsorption equipment usually uses one adsorbent for adsorption, which can only effectively treat a single harmful substance and cannot obtain products with higher purity.

[0003] To this end, Chinese patent CN213790796U discloses a multi-stage adsorption device for purifying trifluoromethane, which is provided with a first adsorption box, a second adsorption box and a third adsorption box and three mesh frames, and the three mesh frames are filled with different adsorption media. Multi-stage adsorption treatment improves the purity of trifluoromethane. When the medium needs to be replaced, it is only necessary to open the respective box covers, take out the internal mesh frames, and replace the adsorbed substances, which facilitates the work of relevant personnel. At the same time, a first fixed block and a second fixed block are provided, so that the first adsorption box, the second adsorption box and the third adsorption box are arranged in a stepped shape, and the gas directly rises for adsorption treatment and discharges in the box, thereby improving the efficiency of adsorption.

[0004] However, when using a multi-stage impurity removal device for adsorption and impurity removal, since multiple adsorption components are connected in series, after the gas enters the adsorption component, the transmission path length and transmission resistance increase accordingly. Although the gas transmission efficiency can be improved to a certain extent by improving the device structure, the improvement effect is limited. In addition, as the number of adsorption components in series increases, the transmission resistance will also increase accordingly. When performing high-pressure gas transmission, it may even cause gas reflux, affecting the gas purification effect. Summary of the invention

[0005] In view of the above problems, a multi-stage adsorption and impurity removal device and a production process for ultra-pure arsine are provided. The adsorption device and the propulsion device solve the problem of transmission obstruction or reflux of high-pressure gas when entering multiple adsorption towers connected in series.

[0006] In order to solve the problems of the prior art, the present invention provides a multi-stage adsorption and impurity removal device, including an adsorption device; the adsorption device includes a first-level adsorption tower and a second-level adsorption tower, the first-level adsorption tower and the second-level adsorption tower are connected in series through a pipeline, and a propulsion device is provided in the first-level adsorption tower and the second-level adsorption tower; a magnetic ball section for dispersing gas, a filling section for adsorbing impurities and a propulsion section are provided in the first-level adsorption tower and the second-level adsorption tower; the propulsion device includes a propulsion box, a piston plate and a linear drive assembly; the propulsion box is arranged in the propulsion section, and a top plate and a bottom plate are respectively provided at both ends of the propulsion box, and the top plate and the bottom plate are connected with the filling section; the piston plate is slidably arranged in the internal cavity of the propulsion box, and the piston plate is tightly matched with the inner wall of the propulsion box, and the internal cavity of the propulsion box is divided into a first cavity and a second cavity by the piston plate; the linear drive assembly is arranged on the propulsion box, and the linear drive assembly is used to drive the piston plate to move back and forth in the propulsion box; the propulsion box is also provided with a connection control mechanism for controlling the connection between the first cavity and the second cavity and the filling section.

[0007] Preferably, an oblique baffle is slidably mounted on the piston plate, and the oblique baffle is slidably matched with the top plate and the bottom plate; a partition is provided in the thrust box, and the piston plate is slidably matched with the partition; the first cavity and the second cavity are separated into a first sub-cavity and a second sub-cavity by the partition and the oblique baffle, and there is a gap between the partition and the oblique baffle for gas transmission; fillers for adsorbing impurities are provided in the first sub-cavity and the second sub-cavity.

[0008] Preferably, two groups of connection control mechanisms are provided, and the two groups of connection control mechanisms are respectively arranged on the top plate and the bottom plate; two return pipes are respectively arranged on the top plate and the bottom plate, and the two return pipes are respectively connected to the first cavity and the second cavity; at least two direct current pipes are provided, and the two direct current pipes are respectively arranged on the top plate and the bottom plate; the connection component is used to control the connection between the return pipe and the direct current pipe.

[0009] Preferably, each return pipe and direct current pipe is provided with a mounting seat, and a valve plate is slidably provided on the mounting seat; a first elastic member is provided on the mounting seat, and the first elastic member is transmission-connected to the valve plate; an auxiliary control mechanism is provided on the propulsion box, and the auxiliary control mechanism includes a locking assembly and a control assembly; the locking assembly is provided on the mounting seat, and the locking assembly is used to limit the movement of the valve plate under the elastic force of the first elastic member; the control assembly is used to release the movement restriction of the valve plate by the locking assembly.

[0010] Preferably, a support is provided at each return pipe and direct current pipe, and a second elastic member is provided on the support; a clamping block is slidably mounted on the support, and the two ends of the second elastic member are respectively connected to the support and the clamping block; a limit plate is provided on the valve plate, and a clamping groove cooperating with the clamping block is opened on the limit plate, and when the clamping block on the support is plugged into the clamping groove, the movement of the valve plate is limited.

[0011] Preferably, the control assembly includes a push block and a push frame; the push block is slidably arranged on the support; the push frame is connected to the push block, and the push frame and the mounting seat are slidably matched; an oblique guide groove is provided on the card block, and the push block and the oblique guide groove of the card block are slidably matched.

[0012] Preferably, guide rods are provided on the top plate and the bottom plate; a movable frame is slidably provided on the guide rod, a linear guide rail is provided on the movable frame, and the driving end of the linear drive assembly is transmission-connected to the movable frame; fixed shafts are provided at both ends of the oblique baffle, and the fixed shafts are slidably matched with the linear guide rails on the movable frame.

[0013] Preferably, an extension frame is provided on one side of the valve plate away from the mounting seat, and a transverse plate is provided on the end of the extension frame away from the valve plate.

[0014] Preferably, the linear drive assembly includes a rotary driver and a bevel gear; screws are rotatably arranged on the top plate and the bottom plate, and the screws are threadedly connected to the movable frame; the rotary driver is arranged on the propulsion box; two bevel gears are provided, and the two bevel gears are respectively sleeved on the driving end of the rotary driver and the screw, and the two bevel gears are meshed and connected.

[0015] A production process for ultrapure arsine, using the above-mentioned multi-stage adsorption and impurity removal device, comprises the following steps:

[0016] S1. Add zinc arsenide solid particles into dilute sulfuric acid, and then collect the crude arsine obtained after removing water into a low-temperature cold trap;

[0017] S2. After the specified weight of crude arsine is collected in the cold trap, the cold trap is reheated and pressurized, and the vaporized crude arsine enters the primary adsorption tower and the secondary adsorption tower in sequence;

[0018] S3, then passing the gas to be purified into a light removal tower and a heavy removal tower for impurity removal;

[0019] S4. Collect the high-purity arsine after impurities removal into a steel bottle.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] 1. The present invention realizes the function of stable gas delivery during large-scale production through an adsorption device and a propulsion device. A propulsion device is independently arranged in each adsorption tower to avoid affecting the transmission of gas due to the increase in the number of adsorption towers connected in series, and the first-level adsorption tower and the second-level adsorption tower arranged in series are used to remove impurity components one by one, stabilize the quality of the product, obtain ultra-pure arsine, and solve the problem that the high-pressure transmitted gas will be blocked or refluxed when entering multiple adsorption towers connected in series. When the gas enters the propulsion section, the volume of the first cavity and the second cavity is constantly changed through the movement of the piston plate, and then the gas is sucked in when the first cavity is enlarged, and the gas is pushed when the second cavity is reduced, and the connection between the first cavity and the second cavity and the packing section is controlled by the connection control mechanism, so that the gas continuously completes the propulsion action of the gas, so that the gas can be stably transported and the gas reflux is avoided.

[0022] 2. The present invention realizes the function of separating the first cavity and the second cavity by the oblique baffle and the partition. When the volume of the first cavity and the first sub-cavity changes under the push of the piston, the gas between the first cavity and the first sub-cavity flows from the gap between the oblique baffle and the partition under the action of gas pressure to exchange gas, so that the gas is fully in contact with the filler in the first sub-cavity, thereby improving the adsorption effect of impurities.

[0023] 3. The present invention realizes the function of continuous suction and exhaust through the alternating connection of the reflux pipe and the direct current pipe. When the linear drive assembly controls the piston plate to move upward, the volume of the first cavity and the first sub-cavity is reduced, and the gas in the first cavity and the first sub-cavity is discharged to the bottom of the bottom plate through the reflux pipe on the top plate, and enters the secondary adsorption tower from the bottom pipe through the packing section and the magnetic ball section. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a three-dimensional schematic diagram of a multi-stage adsorption and impurity removal device.

[0025] Figure 2 The invention is a three-dimensional schematic diagram of a propulsion device, a connection control mechanism and an auxiliary control mechanism in a multi-stage adsorption impurity removal device.

[0026] Figure 3 It is a three-dimensional schematic diagram of the internal structure of a propulsion box in a multi-stage adsorption impurity removal device.

[0027] Figure 4 The invention is a cross-sectional schematic diagram of a propulsion box in a multi-stage adsorption impurity removal device.

[0028] Figure 5 The utility model is a three-dimensional schematic diagram of a top plate, a bottom plate and a connecting control mechanism in a multi-stage adsorption impurity removal device.

[0029] Figure 6The invention is a three-dimensional schematic diagram of a connecting control mechanism and an auxiliary control mechanism in a multi-stage adsorption impurity removal device.

[0030] Figure 7 It is a three-dimensional exploded schematic diagram of a locking component in a multi-stage adsorption and impurity removal device.

[0031] Figure 8 The invention is a three-dimensional exploded schematic diagram of a locking component and a control component in a multi-stage adsorption impurity removal device.

[0032] Fig. 9 The invention is a three-dimensional schematic diagram showing a linear drive component and a control component in a multi-stage adsorption impurity removal device in an upwardly moving state on a movable frame.

[0033] Fig.10 The invention is a three-dimensional schematic diagram showing a linear drive component and a control component in a multi-stage adsorption impurity removal device in a downward moving state of a movable frame.

[0034] The numbers in the figure are: 1-adsorption device; 11-first-stage adsorption tower; 12-second-stage adsorption tower; 13-third-stage adsorption tower; 2-propulsion device; 21-propulsion box; 211-top plate; 212-bottom plate; 213-first cavity; 2131-first sub-cavity; 214-second cavity; 2141-second sub-cavity; 215-partition plate; 22-piston plate; 221-oblique baffle; 2211-fixed shaft; 23-linear drive assembly; 231-screw; 232-rotation drive; 233-bevel gear; 3-connection control Mechanism; 31-return pipe; 32-direct current pipe; 33-connecting assembly; 331-mounting seat; 332-valve plate; 333-first elastic member; 334-extension frame; 3341-cross plate; 4-auxiliary control mechanism; 41-locking assembly; 411-support; 4111-second elastic member; 412-block; 4121-oblique guide groove; 413-limiting plate; 4131-slot; 42-control assembly; 421-push block; 422-push frame; 423-guide rod; 424-movable frame; 4241-linear guide rail. DETAILED DESCRIPTION

[0035] In order to further understand the features, technical means, specific objectives and functions of the present invention, the present invention is further described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0036] Reference Figure 1-Figure 4A multi-stage adsorption impurity removal device, comprising an adsorption device 1; the adsorption device 1 comprises a primary adsorption tower 11 and a secondary adsorption tower 12, the primary adsorption tower 11 and the secondary adsorption tower 12 are connected in series through a pipeline, and a propulsion device 2 is provided in each of the primary adsorption tower 11 and the secondary adsorption tower 12; a magnetic ball section for dispersing gas, a filler section for adsorbing impurities and a propulsion section are provided in each of the primary adsorption tower 11 and the secondary adsorption tower 12; the propulsion device 2 comprises a propulsion box 21, a piston plate 22 and a linear drive assembly 23; the propulsion box 21 is arranged in the propulsion section, and top plates 2 are provided at both ends of the propulsion box 21 11 and the bottom plate 212, and the top plate 211 and the bottom plate 212 are connected to the filling section; the piston plate 22 is slidably arranged in the propulsion box 21, and the piston plate 22 is tightly matched with the inner wall of the propulsion box 21, and the internal cavity of the propulsion box 21 is divided into a first cavity 213 and a second cavity 214 by the piston plate 22; the linear drive component 23 is arranged on the propulsion box 21, and the linear drive component 23 is used to drive the piston plate 22 to reciprocate in the propulsion box 21; the propulsion box 21 is also provided with a connection control mechanism 3 for controlling the connection between the first cavity 213 and the second cavity 214 and the filling section.

[0037] The present invention realizes the function of stable gas delivery during large-scale production through the adsorption device 1 and the propulsion device 2. The propulsion device 2 is independently arranged in each adsorption tower to avoid affecting the transmission of gas due to the increase in the number of adsorption towers connected in series, and the impurity components are removed one by one through the first-level adsorption tower 11 and the second-level adsorption tower 12 arranged in series, so as to stabilize the quality of the product and obtain ultra-pure arsine, thereby solving the problem that the gas transmitted under high pressure will be blocked or refluxed when entering multiple adsorption towers connected in series. The adsorption device 1 also includes a three-level adsorption tower 13, and the first-level adsorption tower 11, the second-level adsorption tower 12 and the third-level adsorption tower 13 are connected in series, wherein the packing section of the first-level adsorption tower 11 is filled with soda lime, the packing section of the second-level adsorption tower 12 is filled with molecular sieve, and the packing section of the third-level adsorption tower 13 is filled with soda lime and activated carbon, and the packing section is purged and activated at high temperature after filling. During purging or activation, nitrogen is carried out from top to bottom, the outlet is fully open, and a flow controller is arranged at the inlet to control the flow, and the propulsion device 2 is also arranged in the third-level adsorption tower 13. And the first-level adsorption tower 11, the second-level adsorption tower 12 and the third-level adsorption tower 13 are all provided with a controller for human-computer interaction. Two magnetic ball sections and two packing sections are all provided in the first-level adsorption tower 11, the second-level adsorption tower 12 and the third-level adsorption tower 13. After the gas enters the adsorption tower from the air inlet pipe, it passes through the magnetic ball section, the packing section, the propulsion section, the packing section and the magnetic ball section in sequence. When producing ultra-pure arsine, the operator first adds zinc arsenide solid particles to the dilute sulfuric acid, and then collects the crude arsine obtained after dehydration into a low-temperature cold trap. After the crude arsine of a specified weight is collected in the cold trap, the cold trap is reheated and pressurized, and then the gasified crude arsine is transmitted to the first-level adsorption tower 11. The gas is dispersed when passing through the magnetic ball section, and can then contact with the packing more evenly to ensure the purification effect. When the gas is passed into the first-stage adsorption tower 11, the controller sends a signal to the linear drive component 23, and the linear drive component 23 controls the piston plate 22 to move back and forth in the propulsion box 21. When the gas enters the propulsion section, the volume of the first cavity 213 and the second cavity 214 is continuously changed through the movement of the piston plate 22, so that the gas is sucked in when the first cavity 213 is enlarged, and the gas is pushed when the second cavity 214 is reduced, and the connection between the first cavity 213 and the second cavity 214 and the filling section is controlled by the connection control mechanism 3, so that the gas continuously completes the propulsion action of the gas, so that the gas can be stably transported and the gas backflow is avoided.

[0038] Reference Figure 3 and Figure 4: An oblique baffle 221 is slidably mounted on the piston plate 22, and the oblique baffle 221 is slidably matched with the top plate 211 and the bottom plate 212; a partition 215 is provided in the propulsion box 21, and the piston plate 22 is slidably matched with the partition 215; the first cavity 213 and the second cavity 214 are separated into a first sub-cavity 2131 and a second sub-cavity 2141 by the partition 215 and the oblique baffle 221, and there is a gap between the partition 215 and the oblique baffle 221 for gas transmission; fillers for adsorbing impurities are provided in the first sub-cavity 2131 and the second sub-cavity 2141.

[0039] The present invention realizes the function of separating the first cavity 213 and the second cavity 214 through the oblique baffle 221 and the partition 215, and the first sub-cavity 2131 and the second sub-cavity 2141 are provided with fillers for absorbing impurities. In order to prevent the piston plate 22 from contacting with the fillers, the fillers are arranged in contact with the bottom plate 212 and the top plate 211, and the piston plate 22 is restricted. However, due to the oblique setting of the oblique baffle 221, when the linear drive assembly 23 drives the piston plate 22 to move, the volume change speeds of the first cavity 213 and the first sub-cavity 2131 are not synchronized. An extension plate is provided in the middle of the oblique baffle 221. The extension plate is slidably matched with the piston plate 22, and the extension plate and the piston plate 22 are tightly matched to ensure the sealing of the piston plate 22. Since the piston plate 22 and the top plate 211 and the bottom plate 212 are slidably matched, the moving path of the piston plate 22 is fixed, and the piston plate 22 is tilted. Therefore, an extension plate is provided on the oblique baffle 221 to ensure the stable movement of the oblique baffle 221. When the first cavity 213 and the first sub-cavity 2131 change in volume under the push of the piston plate 22, the first cavity 213 and the first sub-cavity 2131 flow from the gap between the oblique baffle 221 and the partition 215 under the action of air pressure to exchange gas, so that the gas is fully in contact with the filler in the first sub-cavity 2131, thereby improving the adsorption effect on impurities. When the piston plate 22 moves upward, the gas in the first cavity 213 and the first sub-cavity 2131 is as follows: Figure 4 Indicated by the arrow.

[0040] Reference Figure 2 , Figure 4 and Figure 5 : There are two groups of connection control mechanisms 3, and the two groups of connection control mechanisms 3 are respectively arranged on the top plate 211 and the bottom plate 212; two return pipes 31 are respectively arranged on the top plate 211 and the bottom plate 212, and the two return pipes 31 are respectively connected to the first cavity 213 and the second cavity 214; there are at least two direct current pipes 32, and the two direct current pipes 32 are respectively arranged on the top plate 211 and the bottom plate 212; the connection component 33 is used to control the connection between the return pipe 31 and the direct current pipe 32.

[0041] The present invention realizes the function of continuous air extraction and exhaust by alternately connecting the reflux pipe 31 and the direct current pipe 32. When the linear drive assembly 23 controls the piston plate 22 to move upward, the volume of the first cavity 213 and the first sub-cavity 2131 is reduced, and the gas in the first cavity 213 and the first sub-cavity 2131 is discharged to the bottom of the bottom plate 212 through the reflux pipe 31 on the top plate 211, and enters the secondary adsorption tower 12 from the pipeline at the bottom of the secondary adsorption tower 12 through the filler section and the magnetic ball section. The volume of the second cavity 214 and the second sub-cavity 2141 increases, and the air pressure decreases. The gas is sucked from the top of the top plate 211 through the reflux pipe 31 on the bottom plate 212. After the gas enters the second sub-cavity 2141, it contacts the filler in the second sub-cavity 2141 to adsorb impurities. When the linear drive assembly 23 controls the piston plate 22 to move downward, the volume of the first cavity 213 and the first sub-cavity 2131 increases, the air pressure decreases, and air is sucked in through the direct current pipe 32 on the top plate 211, and the volume of the second cavity 214 and the second sub-cavity 2141 decreases, the air pressure increases, and exhaust is discharged through the direct current pipe 32 on the bottom plate 212, and then the movement of the piston pushes the gas to move in the primary adsorption tower 11, and stably transmits it to the secondary adsorption tower 12 to remove impurities from the gas.

[0042] Reference Figure 4 and Figure 6 : A mounting seat 331 is provided at each return pipe 31 and direct current pipe 32, and a valve plate 332 is slidably provided on the mounting seat 331; a first elastic member 333 is provided on the mounting seat 331, and the first elastic member 333 is transmission-connected with the valve plate 332; an auxiliary control mechanism 4 is provided on the propulsion box 21, and the auxiliary control mechanism 4 includes a locking assembly 41 and a control assembly 42; the locking assembly 41 is provided on the mounting seat 331, and the locking assembly 41 is used to limit the movement of the valve plate 332 under the elastic force of the first elastic member 333; the control assembly 42 is used to release the movement restriction of the valve plate 332 by the locking assembly 41.

[0043] The present invention realizes the function of controlling the connection between the return pipe 31 and the direct current pipe 32 through the mounting seat 331, the valve plate 332, the first elastic member 333, the locking assembly 41 and the control assembly 42. The mounting seats 331 at the return pipe 31 and the direct current pipe 32 are arranged opposite to each other relative to the top plate 211 or the bottom plate 212, so that the piston plate 22 drives the control assembly 42 on the direct current pipe 32 when pushing the valve plate 332 on the return pipe 31. The valve plate 332 is arranged on one side of the bottom plate 212 and the top plate 211 close to the piston plate 22. When the piston plate 22 moves toward the top plate 211, when the piston plate 22 abuts against the valve plate 332 on the top plate 211, the thrust provided by the piston plate 22 overcomes the elastic force of the first elastic member 333 to push the valve plate 332 to move, and the return pipe 31 or the direct current pipe 32 is blocked by the valve plate 332. When the valve plate 332 is in the blocking state, the valve plate 332 is fixed by the locking assembly 41 to prevent the valve plate 332 from being reset under the elastic force of the first elastic member 333 during the subsequent movement of the piston plate 22. When the piston plate 22 moves to the bottom plate 212, the movement of the valve plate 332 on the bottom plate 212 is controlled by the pushing action of the piston plate 22. At the same time, the piston plate 22 drives the oblique baffle plate 221 to move, and the control component 42 is driven by the movement of the oblique baffle plate 221. The control component 42 releases the restriction of the locking component 41 on the top plate 211, and the locking component 41 releases the restriction on the movement of the valve plate 332. The valve plate 332 is reset under the elastic force of the first elastic member 333, thereby opening the return pipe 31. At the same time, the valve plate 332 on the direct current pipe 32 is pushed by the pushing action of the oblique baffle plate 221 to achieve the effect of blocking the direct current pipe 32, and the opening and closing switching of the return pipe 31 and the direct current pipe 32 is completed.

[0044] Reference Figure 6 and Figure 7 : A support 411 is provided at each return pipe 31 and direct current pipe 32, and a second elastic member 4111 is provided on the support 411; a clamping block 412 is slidably mounted on the support 411, and the two ends of the second elastic member 4111 are respectively connected to the support 411 and the clamping block 412; a limiting plate 413 is provided on the valve plate 332, and a clamping groove 4131 cooperating with the clamping block 412 is opened on the limiting plate 413, and when the clamping block 412 on the support 411 is plugged into the clamping groove 4131, the movement of the valve plate 332 is limited.

[0045] The present invention realizes the function of fixing the valve plate 332 through the support 411, the second elastic member 4111, the block 412 and the limit plate 413. When the valve plate 332 is pushed, it overcomes the elastic force of the first elastic member 333 under the action of the thrust and moves, and the valve plate 332 drives the limit plate 413 to move. When the clamping groove 4131 is aligned with the block 412, the block 412 is plugged and matched with the clamping groove 4131 under the elastic force of the second elastic member 4111, and the movement of the valve plate 332 is limited by the cooperation between the block 412 on the support 411 and the clamping groove 4131, so as to prevent the valve plate 332 from being reset under the elastic force of the first elastic member 333, and keep the valve plate 332 in a closed state.

[0046] Reference Figure 6-Figure 8 : The control component 42 includes a push block 421 and a push frame 422; the push block 421 is slidably set on the support 411; the push frame 422 is connected to the push block 421, and the push frame 422 is slidably matched with the mounting seat 331; an oblique guide groove 4121 is opened on the clamping block 412, and the push block 421 is slidably matched with the oblique guide groove 4121 of the clamping block 412.

[0047] The present invention realizes the function of releasing the movement restriction of the locking assembly 41 on the valve plate 332 through the push block 421, the push frame 422 and the oblique guide groove 4121. When the piston plate 22 moves to the bottom plate 212, the oblique baffle 221 on the piston plate 22 pushes the push frame 422 on the top plate 211, and the push frame 422 drives the push block 421 to move, and the push block 421 squeezes the oblique guide groove 4121 on the block 412, and then overcomes the elastic force of the second elastic member 4111 through the squeezing force, pushing the block 412 to move in the direction away from the slot 4131. After the block 412 is separated from the slot 4131, the block 412 no longer hinders the movement of the limit plate 413, and the valve plate 332 is reset under the elastic force of the first elastic member 333 to enter the open state.

[0048] Reference Figure 8-Figure 10 : The top plate 211 and the bottom plate 212 are both connected to a guide rod 423; a movable frame 424 is slidably arranged on the guide rod 423, a linear guide rail 4241 is arranged on the movable frame 424, and a driving end of the linear drive assembly 23 is transmission-connected to the movable frame 424; both ends of the oblique baffle 221 are provided with a fixed shaft 2211, and the fixed shaft 2211 is slidably matched with the linear guide rail 4241 on the movable frame 424.

[0049] The present invention realizes the function of pushing the push frame 422 to move by moving the oblique baffle 221 through the guide rod 423 , the movable frame 424 , the linear guide rail 4241 and the fixed shaft 2211 . When the piston plate 22 moves toward the bottom plate 212, the oblique baffle 221 on the piston plate 22 pushes the linear guide 4241 on the movable frame 424 through the fixed shaft 2211, and then drives the movable frame 424 to move through the linear guide 4241. After the movable frame 424 contacts the push frame 422 on the top plate 211, it pushes the push frame 422 to move, and the push frame 422 drives the push block 421 to move. The push block 421 squeezes the oblique guide groove 4121 on the block 412, and then overcomes the elastic force of the second elastic member 4111 through the squeezing force, and pushes the block 412 to move in the direction away from the slot 4131. After the block 412 is separated from the slot 4131, the block 412 no longer hinders the movement of the limit plate 413, and the valve plate 332 is reset under the elastic force of the first elastic member 333 to enter the open state.

[0050] Reference Figure 6 An extension frame 334 is provided on one side of the valve plate 332 away from the mounting seat 331 , and a transverse plate 3341 is provided on the end of the extension frame 334 away from the valve plate 332 .

[0051] The present invention realizes the function of facilitating the piston plate 22 to push the valve plate 332 through the extension frame 334 and the cross plate 3341, and at the same time achieves the effect of adjusting the initial contact position between the piston plate 22 and the valve plate 332. In the process of the piston plate 22 moving toward the valve plate 332, when the piston plate 22 contacts the cross plate 3341 on the extension frame 334, the cross plate 3341 is pushed to close the valve plate 332. Through the arrangement of the extension frame 334 and the cross plate 3341, the piston plate 22 can push the valve plate 332 in advance, and then reserve space for filling the adsorbent on the first sub-cavity 2131 and the second sub-cavity 2141, so as to avoid the squeezing effect between the piston plate 22 and the adsorbent.

[0052] Reference Fig. 9 and Fig.10 : The linear drive assembly 23 includes a rotary driver 232 and a bevel gear 233; a screw 231 is rotatably provided on the top plate 211 and the bottom plate 212, and the screw 231 is threadedly connected to the movable frame 424; the rotary driver 232 is provided on the propulsion box 21; there are two bevel gears 233, and the two bevel gears 233 are respectively sleeved on the driving end of the rotary driver 232 and the screw 231, and the two bevel gears 233 are meshed and connected.

[0053] The present invention realizes the function of driving the movable frame 424 to move through the screw rod 231 , the rotary driver 232 and the bevel gear 233 , and further promotes the movement of the oblique baffle plate 221 and the piston plate 22 through the movable frame 424 . The rotary driver 232 is preferably a servo motor, which is electrically connected to the controller. After the operator starts the device, the controller sends a signal to the rotary driver 232. After receiving the signal, the rotary driver 232 drives the screw 231 to rotate through the bevel gear 233. The screw 231 drives the movable frame 424 threadedly connected to it to move, and then the movable frame 424 pushes the oblique baffle 221 and the piston plate 22 to move, and controls the piston plate 22 to move back and forth in the propulsion box 21. When the gas enters the propulsion section, the volume of the first cavity 213 and the second cavity 214 changes continuously through the movement of the piston plate 22, and then the gas is sucked in when the first cavity 213 increases, and the gas is pushed when the second cavity 214 shrinks. The connection between the first cavity 213 and the second cavity 214 and the filling section is controlled through the connection control mechanism 3 to perform the gas propulsion operation.

[0054] Reference Figure 1-Figure 5 A production process for ultrapure arsine, using the above-mentioned multi-stage adsorption and impurity removal device, comprises the following steps:

[0055] S1. Add zinc arsenide solid particles into dilute sulfuric acid, and then collect the crude arsine obtained after removing water into a low-temperature cold trap;

[0056] S2, after the specified weight of crude arsine is collected in the cold trap, the cold trap is reheated and pressurized, and the vaporized crude arsine enters the primary adsorption tower 11 and the secondary adsorption tower 12 in sequence;

[0057] S3, then passing the gas to be purified into a light removal tower and a heavy removal tower for impurity removal;

[0058] S4. Collect the high-purity arsine after impurities removal into a steel bottle.

[0059] The above embodiments only express one or several implementation modes of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the present invention. It should be pointed out that, for those of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the attached claims.

Claims

1. A multi-stage adsorption impurity removal device, characterized in that: It comprises an adsorption device (1); The adsorption device (1) comprises a primary adsorption tower (11) and a secondary adsorption tower (12); the primary adsorption tower (11) and the secondary adsorption tower (12) are connected in series via a pipeline; and a propulsion device (2) is provided in each of the primary adsorption tower (11) and the secondary adsorption tower (12); The first-stage adsorption tower (11) and the second-stage adsorption tower (12) are both provided with a magnetic ball section for dispersing gas, a filler section for adsorbing impurities, and a propulsion section; The propulsion device (2) comprises a propulsion box (21), a piston plate (22) and a linear drive assembly (23); The propulsion box (21) is arranged in the propulsion section, and a top plate (211) and a bottom plate (212) are respectively provided at two ends of the propulsion box (21), and the top plate (211) and the bottom plate (212) are connected to the packing section; The piston plate (22) is arranged in an internal cavity of the propulsion box (21) so as to be liftable, and the piston plate (22) is tightly matched with the inner wall of the propulsion box (21), and the internal cavity of the propulsion box (21) is divided into a first cavity (213) and a second cavity (214) by the piston plate (22); The linear drive assembly (23) is arranged on the propulsion box (21), and the linear drive assembly (23) is used to drive the piston plate (22) to reciprocate in the propulsion box (21); The propulsion box (21) is also provided with a communication control mechanism (3) for controlling the communication between the first cavity (213) and the second cavity (214) and the filling section; An oblique baffle (221) is slidably mounted on the piston plate (22), and the oblique baffle (221) is slidably matched with the top plate (211) and the bottom plate (212); A partition plate (215) is provided in the propulsion box (21), and the piston plate (22) is slidably matched with the partition plate (215); Two groups of connection control mechanisms (3) are provided, and the two groups of connection control mechanisms (3) are respectively arranged on the top plate (211) and the bottom plate (212); The two return pipes (31) are respectively arranged on the top plate (211) and the bottom plate (212), and the two return pipes (31) are respectively connected to the first cavity (213) and the second cavity (214); At least two direct current tubes (32) are provided, and the two direct current tubes (32) are respectively arranged on the top plate (211) and the bottom plate (212); The connecting component (33) is used to control the connection between the return pipe (31) and the direct flow pipe (32); An auxiliary control mechanism (4) is provided on the propulsion box (21), and the auxiliary control mechanism (4) comprises a locking component (41) and a control component (42); The locking assembly (41) is arranged on the mounting seat (331), and the locking assembly (41) is used to limit the movement of the valve plate (332) under the elastic force of the first elastic member (333); The control component (42) is used to release the restriction on the movement of the valve plate (332) imposed by the locking component (41).

2. A multi-stage adsorption impurity removal device according to claim 1, characterized in that: The first cavity (213) and the second cavity (214) are separated into a first sub-cavity (2131) and a second sub-cavity (2141) by a partition (215) and an oblique baffle (221), and a gap for gas transmission is provided between the partition (215) and the oblique baffle (221); Fillers for adsorbing impurities are provided in both the first sub-cavity (2131) and the second sub-cavity (2141).

3. A multi-stage adsorption impurity removal device according to claim 1, characterized in that: Each return pipe (31) and each direct flow pipe (32) is provided with a mounting seat (331), and a valve plate (332) is slidably provided on the mounting seat (331); A first elastic member (333) is provided on the mounting seat (331), and the first elastic member (333) is drivingly connected to the valve plate (332).

4. A multi-stage adsorption impurity removal device according to claim 3, characterized in that: A support (411) is provided at each return pipe (31) and each direct flow pipe (32), and a second elastic member (4111) is provided on the support (411); A clamping block (412) is slidably mounted on the support (411), and two ends of the second elastic member (4111) are respectively connected to the support (411) and the clamping block (412); A limit plate (413) is provided on the valve plate (332), and a clamping groove (4131) that cooperates with the clamping block (412) is provided on the limit plate (413). When the clamping block (412) on the support (411) is plugged into and matched with the clamping groove (4131), the movement of the valve plate (332) is limited.

5. A multi-stage adsorption impurity removal device according to claim 4, characterized in that: The control assembly (42) includes a push block (421) and a push frame (422); The push block (421) is slidably disposed on the support (411); The push frame (422) is connected to the push block (421), and the push frame (422) is slidably matched with the mounting seat (331); An oblique guide groove (4121) is formed on the clamping block (412), and the pushing block (421) is slidably matched with the oblique guide groove (4121) of the clamping block (412).

6. A multi-stage adsorption impurity removal device according to claim 5, characterized in that: The top plate (211) and the bottom plate (212) are both connected with guide rods (423); A movable frame (424) is slidably disposed on the guide rod (423), a linear guide rail (4241) is disposed on the movable frame (424), and a driving end of the linear drive assembly (23) is drivingly connected to the movable frame (424); Both ends of the oblique baffle (221) are provided with fixed shafts (2211), and the fixed shafts (2211) at both ends are respectively slidably matched with the linear guide rails (4241) of the two movable frames (424).

7. The multi-stage adsorption impurity removal device according to claim 3, characterized in that: An extension frame (334) is provided on one side of the valve plate (332) away from the mounting seat (331), and a transverse plate (3341) is provided on one end of the extension frame (334) away from the valve plate (332).

8. The multi-stage adsorption impurity removal device according to claim 6, characterized in that: The linear drive assembly (23) includes a rotary drive (232) and a bevel gear (233); A screw rod (231) is rotatably disposed on the top plate (211) and the bottom plate (212), and the screw rod (231) is threadedly connected to the movable frame (424); The rotary driver (232) is arranged on the propulsion box (21); Two bevel gears (233) are provided, and the two bevel gears (233) are respectively sleeved on the driving end of the rotary driver (232) and the screw rod (231), and the two bevel gears (233) are meshedly connected.

9. A production process for ultrapure arsine, using a multi-stage adsorption and impurity removal device as claimed in any one of claims 1 to 8, characterized in that: The following steps are involved: S1. Add zinc arsenide solid particles into dilute sulfuric acid, and then collect the crude arsine obtained after removing water into a low-temperature cold trap; S2, after a specified weight of crude arsine is collected in the cold trap, the cold trap is reheated and pressurized, and the vaporized crude arsine enters the primary adsorption tower (11) and the secondary adsorption tower (12) in sequence; S3, then passing the gas to be purified into a light removal tower and a heavy removal tower for impurity removal; S4. Collect the high-purity arsine after impurities removal into a steel bottle.

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