Adsorption column device and process for continuously producing ultrapure phosphorane by using adsorption column device

Abstract

The invention discloses an adsorption column device and a process for continuously producing ultra-pure phosphorane through the adsorption column device, and relates to the technical field of phosphorane adsorption purification, the adsorption column device comprises an adsorption mechanism, the adsorption mechanism comprises a shell, an adsorption column assembly, an annular plate, a lantern ring, a wedge block, a limiting assembly and a transmission assembly, the adsorption column assembly is installed in the shell, and the annular plate is installed in the shell; the transmission assembly is installed on the surface of the shell, the annular plate is installed on the surfaces of the transmission assembly and the shell, and the lantern ring is arranged on the surface of the adsorption column assembly in a sleeving mode. According to the invention, phosphine can be subjected to multi-stage adsorption purification through the adsorption mechanism, and meanwhile, the adsorption column which is used for a long time can be quickly disassembled, assembled and replaced, so that high-pressure gas is not easily blocked in transmission when entering the adsorption column, and the operation efficiency of the whole production line is further improved; the filtering mechanism can be used for preliminarily filtering the phosphorane before entering the adsorption device, so that large impurities and particulate matters possibly entering the adsorption column are intercepted, the service life of the adsorption column is prolonged, and the purity of the prepared phosphorane is improved.

Description

Technical Field

[0001] The invention relates to the technical field of phosphine adsorption purification, in particular to an adsorption column device and a process for continuously producing ultrapure phosphine using the device. Background Art

[0002] Phosphine is an indispensable raw material for crystalline silicon (microcrystalline silicon and amorphous silicon) solar photovoltaic cells, ultra-large-scale integrated circuits, liquid crystal displays, semiconductor light-emitting devices and semiconductor material manufacturing industries. With the improvement of global energy conservation and environmental protection requirements and the advancement of science and technology, the industry has higher and higher requirements for the purity of phosphine. However, in the production process of phosphine, various impurities will inevitably be produced. These impurities have a significant impact on the purity of phosphine. It is necessary to use the adsorption column in the adsorption tower for treatment, and the impurities in the gas are adsorbed by the medium to achieve the purpose of purifying the gas.

[0003] However, in practical applications, there are still some unresolved problems. The following are some common problems of adsorption column devices for continuous production of ultra-pure phosphine: it is not convenient to quickly disassemble and replace adsorption columns that have been used for a long time. When the adsorption column that has been used for a long time is blocked, it will affect the normal transmission of the gas. When the high-pressure gas encounters transmission obstruction when entering the adsorption column, it will cause poor gas flow, thereby affecting the operating efficiency of the entire production line. In addition, the phosphine that has not entered the adsorption device cannot be initially filtered, and large impurities and particulate matter that may enter the adsorption column cannot be intercepted, resulting in the service life of the adsorption column being affected.

[0004] Therefore, providing an adsorption column device suitable for the continuous production of super phosphine and a process for the continuous production of ultrapure phosphine has become an urgent problem to be solved in the industry. Summary of the invention

[0005] In view of the above problems existing in the existing adsorption column device for continuously producing ultrapure phosphine, the present invention is proposed.

[0006] Therefore, the problem to be solved by the present invention is how to solve the problem that it is inconvenient to quickly disassemble and replace the adsorption column that has been used for a long time, the adsorption column that has been used for a long time is blocked, which affects the normal transmission of gas, and the phosphine cannot be preliminarily filtered before entering the adsorption device, resulting in the service life of the adsorption column being affected.

[0007] In order to solve the above technical problems, the present invention provides the following technical solutions: an adsorption column device for continuously producing ultrapure phosphine, comprising: an adsorption mechanism and a filtering mechanism, wherein: The adsorption mechanism comprises a shell, an adsorption column assembly, a ring plate, a sleeve ring, a wedge block, a limit assembly and a transmission assembly. The adsorption column assembly is installed in the shell, and the transmission assembly is installed on the inner wall of the shell. The number of the ring plates is two, which are installed on the outer surface of the transmission assembly and are symmetrically located in the inner cavity of the shell. The number of the sleeve rings is two, which are installed on the outer surface of the transmission assembly and are symmetrically sleeved on the outer surface of the adsorption column assembly. The wedge block is fixedly connected to the outer surface of the sleeve ring. The limit assembly is installed on the inner wall of the shell and is located above the inner cavity. The limit assembly comprises a floating body, a limit rod, a rubber ring and associated components, the float and the limit rod are arranged on the outer surface of the associated components, the float is located above the limit rod, the associated components are located between the float and the limit rod, the associated components are arranged on the inner surface of the shell, and the rubber ring is sleeved on the surface of the lower end of the limit rod; and a filtering mechanism, which is arranged at the air inlet end of the adsorption mechanism, including a box part, a filter mesh cylinder, a cleaning brush and a monitoring power-on component, the filter mesh cylinder is arranged in the inner cavity of the box part, the surface of the cleaning brush is in contact with the surface of the filter mesh cylinder, and the monitoring power-on component is arranged on the upper surface of the box part.

[0008] As a preferred solution of the adsorption column device described in the present invention, the shell member includes a shell, a box door, an upper cover, a lower cover, a first sealing gasket, a second sealing gasket, an upper cover, a lower cover, a ball and an annular groove, the box door is pivotally connected to the outer surface of the shell, the upper cover and the lower cover are respectively fixedly connected to the upper end and the lower end of the inner wall of the shell, the first sealing gasket is fixedly connected to the top of the lower cover, the second sealing gasket is fixedly connected to the bottom of the upper cover, the upper cover is fixedly connected to the top of the shell, the lower cover is fixedly connected to the bottom of the shell, a ring plate is rotatably connected to the outer surface of the lower end of the upper cover, and the other ring plate is rotatably connected to the outer surface of the upper end of the lower cover, the number of the balls is several, and they are respectively arranged between the inner surface of the upper ring plate and the outer surface of the upper cover, and between the inner surface of the lower ring plate and the outer surface of the lower cover, the annular groove is opened at the bottom of the upper cover, the lower end of the limit rod passes through the bottom of the upper cover and is slidably connected to it, the rubber ring is slidably connected in the annular groove, and the surface of the second sealing gasket contacts the surface of the rubber ring.

[0009] As a preferred solution of the adsorption column device described in the present invention, wherein: the adsorption column assembly includes a cylinder, a grid plate, an adsorption material and a limit groove, the bottom of the cylinder is in contact with the top of the first sealing gasket, the top of the cylinder is in contact with the bottom of the second sealing gasket, the grid plate is fixedly connected to the inner wall of the cylinder, the adsorption material is filled in the inner cavity of the cylinder, the limit groove is opened at the top of the cylinder, the limit rod is inserted into the limit groove, and the rubber ring is slidably connected to the limit groove.

[0010] As a preferred solution of the adsorption column device described in the present invention, the associated components include a support block, a slide rod, a fixed plate, an inclined plate, a movable plate, a connecting ring, a short rod, a slot, a first spring and a sealing ring, wherein the support block is fixedly connected to the inner wall of the upper cover, the slide rod is fixedly connected to the top of the support block, the float is sleeved on the surface of the slide rod, the fixed plate is fixedly connected to the bottom of the float, the inclined plates are two in number and are fixedly connected to the middle and lower part of the slide rod symmetrically, the movable plate is rotatably connected to the end of the inclined plate, and the connecting ring is fixedly connected to the limit The upper end of the limiting rod, the slot hole is opened on the surface of the movable plate, and one movable plate surface has two slot holes symmetrically, the number of the short rods is four, one end of two of the short rods is fixedly connected to the bottom of the fixed plate, and the other end is slidably connected to the slot hole on the upper end of the movable plate, one end of the other two short rods is fixedly connected to the top of the connecting ring, and the other end is slidably connected to the slot hole at the lower end of the movable plate, the first spring and the sealing ring are both sleeved on the limiting rod, the two ends of the first spring are respectively fixedly connected to the upper cover and the surface of the connecting ring, and the sealing ring is fixedly connected to the surface of the upper cover.

[0011] As a preferred solution of the adsorption column device described in the present invention, wherein: the transmission assembly includes a rotating member, a force-applying member and a limiting arc plate, the force-applying member is installed between the inner surface of the box door and the outer surface of the rotating member, the rotating member is installed on the outer surfaces of the upper cover, the lower cover and the force-applying member, the number of the limiting arc plates is two, and they are symmetrically fixedly connected to the middle part of the inner wall of the shell, the inner surface of the limiting arc plate is in contact with the outer surface of the cylinder, the force-applying member includes a connecting plate, a connecting block and a short column, the connecting block is fixedly connected to the inner surface of the box door, the short column is fixedly connected to the outer surface of the connecting block, the connecting plate is arranged on the outer surface of the rotating member, and the short column is slidably connected to the inner wall of the connecting plate.

[0012] As a preferred solution of the adsorption column device described in the present invention, wherein: the rotating part includes a rotating rod, a vertical rod, two top plates, a first gear, teeth, a round block and a second spring, the rotating rod passes through and is rotatably connected between the upper cover and the lower cover, the vertical rod is fixedly connected between the upper cover and the lower cover, the rotating rod and the vertical rod are symmetrically located on both sides of the adsorption column assembly, the connecting plate and the first gear are sleeved on the rotating rod, the two top plates are respectively fixedly connected to the two ends of the rotating rod, the teeth are fixedly connected to the outer edge wall of the ring plate, the teeth are meshed with the first gear, the round block and the second spring are both sleeved on the rotating rod and the vertical rod, the two ends of the second spring are respectively in contact with the surface of the round block and the ring plate, and the sleeve ring is sleeved on the rotating rod and the vertical rod.

[0013] As a preferred embodiment of the adsorption column device described in the present invention, the filtering mechanism also includes a driving member, a linkage assembly and an exhaust pipe, the box member includes a box body, a cover plate and an air inlet pipe, the filter screen cylinder and the cleaning brush are both located in the inner cavity of the box body, the cover plate is fixedly connected to the top of the box body, the driving member is arranged on the outer surfaces of the cover plate and the filter screen cylinder, the linkage assembly is installed on the outer surface of the driving member and the inner wall of the box body, the cleaning brush is installed on the outer surface of the linkage assembly, the monitoring power-on assembly is installed on the top of the cover plate, the air inlet pipe is connected to the outer surface of the box body, the filter screen cylinder is rotatably connected to the bottom of the cover plate, the bottom of the filter screen cylinder is in contact with the inner wall of the box body, and one end of the exhaust pipe is fixedly connected to the bottom of the box body and inserted into the filter screen cylinder.

[0014] As a preferred solution of the adsorption column device described in the present invention, wherein: the monitoring power-on component includes a connecting pipe, a fixed block, a square rod, a piston, a first conductive sheet, a second conductive sheet and a fifth spring, the connecting pipe is fixedly connected to the surface of the cover plate and extends to the inner cavity of the box body, the fixed block is fixedly connected to the inner wall of the connecting pipe, the square rod is slidably connected to the surface of the fixed block, the piston is fixedly connected to one end of the square rod and slidably connected to the inner wall of the connecting pipe, the first conductive sheet is fixedly connected to the other end of the square rod, the second conductive sheet is fixedly connected to the inner wall of the connecting pipe, the fifth spring is sleeved on the square rod, and its two ends are respectively fixedly connected to the fixed block and the piston surface.

[0015] As a preferred solution of the adsorption column device described in the present invention, the driving member includes a second gear, a motor and a third gear, the second gear is sleeved on the upper end surface of the filter mesh cylinder, the motor is fixedly connected to the top of the cover plate, the motor output shaft is fixedly connected to the top of the third gear, and the second gear is meshed with the third gear.

[0016] As a preferred solution of the adsorption column device described in the present invention, the linkage assembly includes a support plate, a rotating column, a convex ring, a vertical plate, a sixth spring, a steel ball, a cross bar and a seventh spring, the support plate is fixedly connected to the inner wall of the box body, the rotating column is fixedly connected to the bottom of the third gear and is rotatably connected to the surface of the support plate, the convex ring is fixedly connected to the lower end of the rotating column, the vertical plate is slidably connected to the surface of the support plate, the sixth spring is sleeved on the surface of the vertical plate, and its two ends are respectively fixedly connected to the vertical plate and the surface of the support plate, the steel ball is rotatably connected to the lower end of the vertical plate and contacts with the surface of the convex ring, the cross bar is fixedly connected to the surface of the cleaning brush and is slidably connected to the surface of the vertical plate, the seventh spring is sleeved on the surface of the cross bar, and its two ends are respectively fixedly connected to the surface of the cleaning brush and the surface of the vertical plate.

[0017] A process for continuously producing ultrapure phosphine, using the above-mentioned adsorption column device, comprises the following steps: S1, add yellow phosphorus and calcium hydroxide to a reactor, and under stirring, add sodium hydroxide solution through a flow meter to control the flow to react, to obtain crude phosphine; S2, condensing the crude phosphine to preliminarily remove high-boiling-point impurities in the crude phosphine, then reheating the crude phosphine, and the vaporized crude phosphine is distilled and then sequentially enters a filtering mechanism (200) and a plurality of adsorption mechanisms (100) connected in series to obtain a gas to be purified; S3, passing the gas to be purified into a light removal tower and a heavy removal tower in sequence to obtain ultrapure phosphine; and S4. Collect the ultrapure phosphine into a steel bottle.

[0018] The beneficial effects of the present invention are as follows: the present invention can perform multi-stage adsorption purification on phosphine through the adsorption mechanism, and is convenient for quickly disassembling and replacing the adsorption column used for a long time, so that the high-pressure gas is not prone to encounter transmission obstruction when entering the adsorption column, so that the gas flows smoothly, thereby improving the operation efficiency of the entire production line; the phosphine before entering the adsorption device can be preliminarily filtered through the filtering mechanism to intercept large impurities and particulate matter that may enter the adsorption column, thereby extending the service life of the adsorption column, and at the same time, the prepared phosphine has the advantages of low production cost, high preparation efficiency and high purity of finished products. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] 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.

[0020] Figure 1 This is the overall three-dimensional structural diagram of the adsorption column device for the continuous production of ultra-pure phosphine.

[0021] Figure 2 A partial three-dimensional structural diagram of an adsorption column device for continuously producing ultra-pure phosphine.

[0022] Figure 3 A partially cutaway perspective structural diagram of the shell of an adsorption column device for the continuous production of ultrapure phosphine.

[0023] Figure 4 Adsorption column device for continuous production of ultrapure phosphine Figure 3 A is an enlarged structural diagram.

[0024] Figure 5 This is a three-dimensional structural diagram of the cylinder of an adsorption column device for continuously producing ultra-pure phosphine.

[0025] Figure 6Adsorption column device for continuous production of ultrapure phosphine Figure 5 A magnified structural diagram of B.

[0026] Figure 7 Adsorption column device for continuous production of ultrapure phosphine Figure 5 Enlarged structure diagram of C in the middle.

[0027] Figure 8 Partial cross-sectional view of an adsorption column device for continuous production of ultrapure phosphine Figure 1 .

[0028] Fig. 9 Adsorption column device for continuous production of ultrapure phosphine Figure 8 The enlarged structure of D in the middle.

[0029] Fig.10 Adsorption column device for continuous production of ultrapure phosphine Figure 8 Enlarged structure diagram of E in the middle.

[0030] Fig.11 Adsorption column device for continuous production of ultrapure phosphine Figure 8 Enlarged structure diagram of F in the middle.

[0031] Fig.12 Adsorption column device for continuous production of ultrapure phosphine Figure 8 Enlarged structural diagram of G in the middle.

[0032] Fig.13 Partial cross-sectional view of an adsorption column device for continuous production of ultrapure phosphine Figure 2 .

[0033] Fig.14 A three-dimensional structural diagram of the associated components of an adsorption column device for continuously producing ultra-pure phosphine.

[0034] Fig.15 A partially cutaway stereoscopic structural diagram of the box of an adsorption column device for continuously producing ultrapure phosphine.

[0035] Fig.16 Adsorption column device for continuous production of ultrapure phosphine Fig.15 Enlarged structure diagram of H in the middle.

[0036] Fig.17 Adsorption column device for continuous production of ultrapure phosphine Fig.15 Enlarged structure diagram of J in the middle.

[0037] Fig.18 Adsorption column device for continuous production of ultrapure phosphine Fig.15 Enlarged structure diagram of K in the middle.

[0038] Fig.19A cutaway perspective structural diagram of the monitoring energized components of an adsorption column device for the continuous production of ultrapure phosphine.

[0039] Fig. 20 A partially cutaway perspective structural diagram of the fixed components of an adsorption column device for the continuous production of ultrapure phosphine.

[0040] In the figure: 100, adsorption mechanism; 101, shell; 102, adsorption column assembly; 103, ring plate; 104, collar; 105, wedge; 106, limit assembly; 107, transmission assembly; 108, feed pipe; 109, discharge pipe; 110, opening and closing assembly; 111, backwash inlet valve; 112, backwash outlet valve; 113, guide cover; 114, sealing sleeve; 115, fixing assembly; 200, filtering mechanism; 201, box; 202, filter net cylinder; 203, cleaning brush; 204, monitoring power supply assembly; 205, driving member; 206, linkage assembly; 207, exhaust pipe; 208, plugging assembly; 101a, shell; 101b, box door; 101c, upper cover; 101d, lower cover; 101e, first sealing gasket; 101f, second sealing gasket; 101g, upper cover; 101h, lower cover; 101i, ball bearing; 101j, annular groove; 102a, cylinder; 102b, grid plate; 102c, adsorption material; 102d, limit groove; 106a, float; 106b, limit rod; 106c, rubber ring; 106d, associated components; 106d-1, support block; 106d-2, slide rod; 106d-3, fixed plate; 106d-4, inclined plate; 106d-5, movable plate; 106d-6, connecting ring; 106d-7, short rod; 106d-8, slot; 106d-9, first spring; 106d-10, sealing ring; 107a, rotating member; 107b , force-applying member; 107c, limit arc plate; 107a-1, rotating rod; 107a-2, vertical rod; 107a-3, top plate; 107a-4, first gear; 107a-5, teeth; 107a-6, round block; 107a-7, second spring; 107b-1, connecting plate; 107b-2, connecting block; 107b-3, short column; 110a, short block; 110b, valve stem; 110c, valve block; 110d, third spring; 115a, handle; 115b, limit column; 115c, clamping plate; 115d, trough; 115e, square column; 115f, handle block; 115g, clamping column; 115h, fourth spring; 201a, box body; 201b, cover plate; 201c, air intake pipe; 2 04a, connecting pipe; 204b, fixing block; 204c, square rod; 204d, piston; 204e, first conductive sheet; 204f, second conductive sheet; 204g, fifth spring; 205a, second gear; 205b, motor; 205c, third gear; 206a, support plate; 206b, rotating column; 206c, convex ring; 206d, vertical plate; 206e, sixth spring; 206f, steel ball; 206g, cross bar; 206h, seventh spring; 208a, mounting block; 208b, sliding column; 208c, stopper; 208d, tapered column; 208e, eighth spring; 208f, groove; 208g, extrusion plate; 208h, inclined block; 208i, lower pressure plate; 208j, ninth spring. DETAILED DESCRIPTION

[0041] 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.

[0042] 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.

[0043] 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.

[0044] Example 1 Reference Figure 1 to Figure 15 As a first non-limiting embodiment of the present invention, this embodiment provides an adsorption column device for continuously producing ultra-pure phosphine. The adsorption column device for continuously producing ultra-pure phosphine includes an adsorption mechanism 100 and a filtering mechanism 200. The phosphine can be subjected to multi-stage adsorption purification through a plurality of adsorption mechanisms 100 connected in series, and the adsorption columns used for a long time can be quickly disassembled and replaced. The phosphine before entering the adsorption device can be preliminarily filtered through the filtering mechanism 200 to intercept large impurities and particulate matter that may enter the adsorption column.

[0045] Specifically, the adsorption mechanism 100 includes a shell 101, an adsorption column assembly 102, a ring plate 103, a collar 104, a wedge 105, a limit assembly 106 and a transmission assembly 107. The adsorption column assembly 102 is installed in the shell 101, and the transmission assembly 107 is installed on the inner wall of the shell 101. The number of the ring plates 103 is two, which are installed on the outer surface of the transmission assembly 107 and are symmetrically located in the inner cavity of the shell 101. The number of the collar 104 is two, which are installed on the outer surface of the transmission assembly 107 and are symmetrically sleeved on the outer surface of the adsorption column assembly 102. The wedge 105 is fixed. Connected to the outer surface of the ring 104, the limit component 106 is installed on the inner wall of the shell 101 and is located above the inner cavity. The limit component 106 includes a float 106a, a limit rod 106b, a rubber ring 106c and an associated component 106d. The float 106a and the limit rod 106b are arranged on the outer surface of the associated component 106d, the float 106a is located above the limit rod 106, the associated component 106d is located between the float 106a and the limit rod 106b, the associated component 106d is arranged on the inner surface of the shell 101, and the rubber ring 106c is sleeved on the surface of the lower end of the limit rod 106b.

[0046] The adsorption column assembly 102 removes impurity gases and moisture in the passing phosphine, which is a prior art and will not be elaborated here. A hole groove matched with the wedge block 105 is opened on the surface of the ring plate 103. The hole groove and the wedge block 105 are gradually matched by rotating the ring plate 103, and the sleeve ring 104 and the wedge block 105 are moved under the action of the corresponding structure to disengage from the limit of the adsorption column assembly 102 to complete the initial unlocking.

[0047] The float 106a is filled with an inert gas with a low density. The float 106a rises under the action of the gas buoyancy, and then the limit rod 106b and the rubber ring 106c are inserted into the limit groove 102d on the adsorption column assembly 102 under the transmission of the associated assembly 106d. The adsorption column assembly 102 is fixed by the gas in the device. The greater the gas pressure, the better the fixing effect.

[0048] At the same time, when the adsorption column assembly 102 needs to be replaced, only when the gas in the device is basically emptied can the limit rod 106b be separated from the adsorption column assembly 102 to complete the unlocking, so as to avoid disassembly when there is still a large amount of gas in the device, which may cause gas leakage and improve the safety during use. The ring plate 103 is driven by the transmission assembly 107 to complete the fixing or unlocking of the adsorption column assembly 102 by the ring 104.

[0049] Specifically, the filtering mechanism 200 is arranged at the air inlet end of the adsorption mechanism 100, and includes a box 201, a filter mesh cylinder 202, a cleaning brush 203 and a monitoring power-on component 204. The filter mesh cylinder 202 is arranged in the inner cavity of the box 201, the surface of the cleaning brush 203 is in contact with the surface of the filter mesh cylinder 202, and the monitoring power-on component 204 is arranged on the upper surface of the box 201.

[0050] The phosphine entering the adsorption mechanism 100 can be initially filtered through the filter cylinder 202 to intercept large impurities and particulate matter that may enter the adsorption column assembly 102, thereby extending the service life of the adsorption column assembly 102. By monitoring the power-on assembly 204, it can be determined whether the filter cylinder 202 is rotated and cleaned.

[0051] When the pressure in the box 201 is too high, it means that the impurities attached to the surface of the filter cylinder 202 have affected the filtering effect and cannot meet the filtering needs. At this time, the monitoring power-on component 204 is energized to enable the driving component 205 to operate and rotate the filter cylinder 202. At the same time, the cleaning brush 203 is moved up and down under the transmission of the linkage component 206, so as to remove the impurities and particles on the surface of the filter cylinder 202 and improve the filtering efficiency. When the pressure in the box 201 gradually decreases and cannot meet the monitoring power-on component 204, the driving component 205 stops running, the filter cylinder 202 no longer rotates, and the cleaning brush 203 no longer moves.

[0052] Example 2 Reference Figure 2 to Figure 14 , which is the second embodiment of the present invention, and this embodiment is based on the previous embodiment.

[0053] Specifically, the shell 101 includes a shell 101a, a box door 101b, an upper cover 101c, a lower cover 101d, a first sealing gasket 101e, a second sealing gasket 101f, an upper cover 101g, a lower cover 101h, a ball 101i and an annular groove 101j, the box door 101b is pivotally connected to the outer surface of the shell 101a, the upper cover 101c and the lower cover 101d are respectively fixedly connected to the upper end and the lower end of the inner wall of the shell 101a, the first sealing gasket 101e is fixedly connected to the top of the lower cover 101d, the second sealing gasket 101f is fixedly connected to the bottom of the upper cover 101c, the upper cover 101g is fixedly connected to the top of the shell 101a, and the lower cover 101h is fixedly connected to the shell 1 01a bottom, one ring plate 103 is rotatably connected to the outer surface of the lower end of the upper cover 101c, and the other ring plate 103 is rotatably connected to the outer surface of the upper end of the lower cover 101d. There are several balls 101i, which are respectively arranged between the inner surface of the upper ring plate 103 and the outer surface of the upper cover 101c, and between the inner surface of the lower ring plate 103 and the outer surface of the lower cover 101d. The annular groove 101j is opened at the bottom of the upper cover 101c, and the lower end of the limiting rod 106b passes through the bottom of the upper cover 101c and is slidably connected thereto. The rubber ring 106c is slidably connected in the annular groove 101j, and the surface of the second sealing gasket 101f contacts the surface of the rubber ring 106c.

[0054] The upper cover 101c and the lower cover 101d are both trumpet-shaped. The distance between the upper cover 101c and the lower cover 101d can meet the space for placing and installing the adsorption column assembly 102. Under the action of the first sealing gasket 101e, the adsorption column assembly 102 and the lower cover 101d are sealed. Under the action of the second sealing gasket 101f, the adsorption column assembly 102 and the upper cover 101c are initially sealed to prevent leakage of phosphine during the adsorption and purification process.

[0055] The upper cover 101g and the lower cover 101h are fixedly connected to the shell 101a by bolts and nuts, and the ring plate 103 is connected to the upper cover 101c and the lower cover 101d by the ball 101i without affecting the rotation of the ring plate 103. The adsorption column assembly 102 is limited by inserting the limiting rod 106b into the limiting groove 102d, and when the rubber ring 106c is placed in the second sealing gasket 101f and the limiting groove 102d, a secondary seal is performed between the upper end of the adsorption column assembly 102 and the lower end of the upper cover 101c, so that the sealing operation is achieved while fixing, thereby improving safety. When releasing the fixation, there is enough space for the rubber ring 106c to move up through the ring groove 101j, and the adsorption column assembly 102 can be removed without hindering it.

[0056] The adsorption column assembly 102 includes a cylinder 102a, a grid plate 102b, an adsorption material 102c and a limiting groove 102d. The bottom of the cylinder 102a contacts the top of the first sealing gasket 101e, the top of the cylinder 102a contacts the bottom of the second sealing gasket 101f, the grid plate 102b is fixedly connected to the inner wall of the cylinder 102a, the adsorption material 102c is filled in the inner cavity of the cylinder 102a, the limiting groove 102d is opened at the top of the cylinder 102a, the limiting rod 106b is inserted into the limiting groove 102d, and the rubber ring 106c is slidably connected to the limiting groove 102d.

[0057] The cylinder 102a is cylindrical and fits with the lower end of the upper cover 101c and the upper end of the lower cover 101d. The adsorption material 102c is supported by the grid plate 102b to prevent it from falling, and at the same time does not affect the passage of gas. There are three adsorption mechanisms 100, which are of different levels. The difference is that the adsorption materials 102c filled in the adsorption column assembly 102 are different. The adsorption material 102c can be one or more combinations of soda lime, activated carbon, and molecular sieve.

[0058] The associated assembly 106d includes a support block 106d-1, a slide bar 106d-2, a fixed plate 106d-3, an inclined plate 106d-4, a movable plate 106d-5, a connecting ring 106d-6, a short rod 106d-7, a slot 106d-8, a first spring 106d-9 and a sealing ring 106d-10, wherein the support block 106d-1 is fixedly connected to the inner wall of the upper cover 101c, and the slide bar 106d-2 is fixedly connected to the inner wall of the upper cover 101c. The floating body 106a is connected to the top of the support block 106d-1, the floating body 106a is sleeved on the surface of the sliding rod 106d-2, the fixed plate 106d-3 is fixedly connected to the bottom of the floating body 106a, the number of inclined plates 106d-4 is two, and they are fixedly connected to the middle and lower part of the sliding rod 106d-2 symmetrically, the movable plate 106d-5 is rotatably connected to the end of the inclined plate 106d-4, and the connecting ring 106d-6 is fixedly connected to the upper end of the limit rod 106b , a slot 106d-8 is opened on the surface of the movable plate 106d-5, and there are two slots 106d-8 symmetrically on the surface of one movable plate 106d-5, and the number of short rods 106d-7 is four, one end of two short rods 106d-7 is fixedly connected to the bottom of the fixed plate 106d-3, and the other end is slidably connected to the slot 106d-8 at the upper end of the movable plate 106d-5, one end of the other two short rods 106d-7 is fixedly connected to the top of the connecting ring 106d-6, and the other end is slidably connected to the slot 106d-8 at the lower end of the movable plate 106d-5, the first spring 106d-9 and the sealing ring 106d-10 are both sleeved on the limiting rod 106b, and the two ends of the first spring 106d-9 are respectively fixedly connected to the upper cover 101c and the surface of the connecting ring 106d-6, and the sealing ring 106d-10 is fixedly connected to the surface of the upper cover 101c.

[0059] The support block 106d-1 is fixedly connected to the inner wall of the upper cover 101c through a support rod, and the float 106a is slidably connected to the slide rod 106d-2. The slide rod 106d-2 guides and limits the float 106a so that it can only move vertically and will not deviate. There are two fixed plates 106d-3 and two inclined plates 106d-4. The movable plate 106d-5 is rotatably connected to the surface of the inclined plate 106d-4 through a rotating shaft. There are four limit rods 106b, which are arranged in a circular array at the bottom of the connecting ring 106d-6. The first spring 106d-9 can provide power for resetting the connecting ring 106d-6 and the limit rod 106b under the action of its elastic force.

[0060] The sealing ring 106d-10 is used to seal the limit rod 106b and the upper cover 101c, so that when the limit rod 106b moves, the gas will not leak from the gap between it and the upper cover 101c. Two slots 106d-8 are provided on the surface of a movable plate 106d-5. The float 106a drives the fixed plate 106d-3 and the short rod 106d-7 thereon to move up and down, so that the movable plate 106d-5 rotates. Under the action of the slot 106d-8, the connecting ring 106d-6 and the short rod 106d-7 thereon move up and down, thereby realizing the driving of the limit rod 106b, and completing the limitation and unlocking of the adsorption column assembly 102.

[0061] The transmission assembly 107 includes a rotating member 107a, a force member 107b and a limit arc plate 107c. The force member 107b is installed between the inner surface of the box door 101b and the outer surface of the rotating member 107a. The rotating member 107a is installed on the upper cover 101c, the lower cover 101d and the outer surface of the force member 107b. The limit arc plate 107c is two in number and is symmetrically fixedly connected to the middle part of the inner wall of the housing 101a. The inner surface of the limit arc plate 107c In contact with the outer surface of the cylinder 102a, the force-applying member 107b includes a connecting plate 107b-1, a connecting block 107b-2 and a short column 107b-3. The connecting block 107b-2 is fixedly connected to the inner surface of the box door 101b, and the short column 107b-3 is fixedly connected to the outer surface of the connecting block 107b-2. The connecting plate 107b-1 is arranged on the outer surface of the rotating member 107a, and the short column 107b-3 is slidably connected to the inner wall of the connecting plate 107b-1.

[0062] The force-applying member 107b is driven by the opening and closing rotation of the box door 101b, thereby causing the rotating member 107a to operate. Then, under the action of the ring plate 103, the wedge block 105 and the ring 104, the adsorption column assembly 102 is unlocked and fixed. This facilitates the unlocking and fixing operations during maintenance and replacement by opening and closing the box door 101b, thereby improving efficiency. There is no need to use tools to disassemble and assemble the adsorption column assembly 102, and the steps are simple and convenient.

[0063] The adsorption column assembly 102 is initially positioned when placed between the upper cover 101c and the lower cover 101d through the limiting arc plate 107c, so that the adsorption column assembly 102 is aligned with the upper cover 101c and the lower cover 101d, which facilitates the subsequent sleeve of the ring 104 on the surface of the adsorption column assembly 102 and the subsequent insertion of the limiting rod 106b into the limiting groove 102d.

[0064] The connection block 107b-2 is driven to rotate by the rotation of the box door 101b, and then the short column 107b-3 on the connection block 107b-2 slides in the connecting plate 107b-1 and drives the connecting plate 107b-1 to rotate, thereby driving the rotating member 107a. When the box door 101b is closed, the connecting plate 107b-1 contacts the surface of the adsorption column assembly 102, thereby fixing the adsorption column assembly 102 again.

[0065] The rotating member 107a includes a rotating rod 107a-1, a vertical rod 107a-2, two top plates 107a-3, a first gear 107a-4, teeth 107a-5, a round block 107a-6 and a second spring 107a-7. The rotating rod 107a-1 is rotatably connected between the upper cover 101c and the lower cover 101d. The vertical rod 107a-2 is fixedly connected between the upper cover 101c and the lower cover 101d. The rotating rod 107a-1 and the vertical rod 107a-2 are symmetrically located on both sides of the adsorption column assembly 102. The connecting plate 107b-1 and the first gear 107a-4 are connected to the upper cover 101c and the lower cover 101d. It is sleeved on the rotating rod 107a-1, and the two top plates 107a-3 are respectively fixedly connected to the two ends of the rotating rod 107a-1, the teeth 107a-5 are fixedly connected to the outer edge wall of the ring plate 103, the teeth 107a-5 are meshed with the first gear 107a-4, the round block 107a-6 and the second spring 107a-7 are both sleeved on the rotating rod 107a-1 and the vertical rod 107a-2, the two ends of the second spring 107a-7 are respectively in contact with the surface of the round block 107a-6 and the ring plate 103, and the ring 104 is sleeved on the rotating rod 107a-1 and the vertical rod 107a-2.

[0066] The rotating rod 107a-1 is rotatably connected to the surface of the upper cover 101c and the lower cover 101d through a sealed bearing. The sealed bearing fixes the rotating rod 107a-1 and seals it at the same time, so there will be no leakage even when it rotates. The opening and closing of the opening and closing assembly 110 can be controlled by whether the top plate 107a-3 rotates and contacts it. The length of the top plate 107a-3 can be designed and adjusted according to the positions of the feed pipe 108 and the discharge pipe 109, as long as it is not affected within the normal rotation range.

[0067] The first gear 107a-4, the connecting plate 107b-1 and the round block 107a-6 are fixedly connected to the surface of the rotating rod 107a-1, and the ring 104 is slidably connected to the surface of the rotating rod 107a-1 and the vertical rod 107a-2. The rotation of the rotating rod 107a-1 can drive the first gear 107a-4 to rotate, and then under the action of the engagement of the teeth 107a-5, the ring plate 103 is rotated to achieve the extrusion movement of the wedge block 105 or the gradual release of the extrusion and return movement. The second spring 107a-7 provides power for the reset of the ring 104 under the action of its rebound after compression.

[0068] Example 3 Reference Figure 15 to Figure 19 , which is the third embodiment of the present invention, and is based on the first two embodiments.

[0069] Specifically, the filter mechanism 200 further includes a driving member 205, a linkage assembly 206 and an exhaust pipe 207. The box 201 includes a box body 201a, a cover plate 201b and an air inlet pipe 201c. The filter screen cylinder 202 and the cleaning brush 203 are both located in the inner cavity of the box body 201a. The cover plate 201b is fixedly connected to the top of the box body 201a. The driving member 205 is arranged on the outer surface of the cover plate 201b and the filter screen cylinder 202. The linkage assembly 206 is installed on the driving member 205. The cleaning brush 203 is installed on the outer surface of the linkage assembly 206, the monitoring power-on assembly 204 is installed on the top of the cover 201b, the air inlet pipe 201c is connected to the outer surface of the box 201a, the filter screen cylinder 202 is rotatably connected to the bottom of the cover 201b, the bottom of the filter screen cylinder 202 is in contact with the inner wall of the box 201a, and one end of the exhaust pipe 207 is fixedly connected to the bottom of the box 201a and inserted into the filter screen cylinder 202.

[0070] The linkage assembly 206 is driven by the operation of the driving member 205, so that the filter screen cylinder 202 rotates while the cleaning brush 203 moves up and down, changing the position of the filter screen cylinder 202 facing the air intake pipe 201c, and cleaning the surface of the filter screen cylinder 202 to achieve better filtering of impurities and particles.

[0071] The cover plate 201b is connected to the top of the box body 201a by bolts, the air inlet pipe 201c is fixedly connected to the surface of the box body 201a, the filter screen cylinder 202 is rotatably connected to the bottom of the cover plate 201b through a bearing, and a sealing ring is arranged between the exhaust pipe 207 and the filter screen cylinder 202 for sealing, while not affecting the normal insertion and removal of the filter screen cylinder 202.

[0072] The monitoring power-on component 204 includes a connecting pipe 204a, a fixed block 204b, a square rod 204c, a piston 204d, a first conductive sheet 204e, a second conductive sheet 204f and a fifth spring 204g. The connecting pipe 204a is fixedly connected to the surface of the cover plate 201b and extends to the inner cavity of the box body 201a. The fixed block 204b is fixedly connected to the inner wall of the connecting pipe 204a. The square rod 204c is slidably connected to the surface of the fixed block 204b. The piston 204d is fixedly connected to one end of the square rod 204c and is slidably connected to the inner wall of the connecting pipe 204a. The first conductive sheet 204e is fixedly connected to the other end of the square rod 204c. The second conductive sheet 204f is fixedly connected to the inner wall of the connecting pipe 204a. The fifth spring 204g is sleeved on the square rod 204c, and its two ends are respectively fixedly connected to the surfaces of the fixed block 204b and the piston 204d.

[0073] The square rod 204c passes through the fixed block 204b and is slidably connected thereto. The piston 204d and the first conductive sheet 204e are guided and limited by the square rod 204c. The first conductive sheet 204e, the second conductive sheet 204f and the motor 205b are connected in a circuit through wires. When the blockage caused by impurities and particles attached to the surface of the filter cylinder 202 cannot meet the filtering requirements, the pressure in the box body 201a gradually increases, thereby overcoming the elastic force of the fifth spring 204g to push the piston 204d to move, so that the square rod 204c and the first conductive sheet 204e move, contact the second conductive sheet 204f to energize and operate the motor 205b, and the rotation and cleaning operation of the filter cylinder 202 are realized under the drive of the corresponding structure, thereby improving the filtering effect.

[0074] When the pressure in the box 201a gradually decreases and cannot overcome the elastic force generated by the compression of the fifth spring 204g, the first conductive sheet 204e and the second conductive sheet 204f are separated and no longer energized, thereby preventing the cleaning brush 203 from being constantly moved and worn out. Cleaning operations can only be performed when necessary, thereby increasing the service life of the cleaning brush 203.

[0075] The driving member 205 includes a second gear 205a, a motor 205b and a third gear 205c. The second gear 205a is sleeved on the upper end surface of the filter screen cylinder 202, the motor 205b is fixedly connected to the top of the cover plate 201b, the output shaft of the motor 205b is fixedly connected to the top of the third gear 205c, and the second gear 205a is meshed with the third gear 205c.

[0076] The second gear 205a is fixedly connected to the surface of the filter screen cylinder 202 by screws, and the third gear 205c is an incomplete gear. The second gear 205a can only rotate one circle when the third gear 205c rotates multiple circles, so that the cleaning brush 203 moving up and down can fully clean the surface of the slowly rotating filter screen cylinder 202. At the same time, the filter screen cylinder 202 can change the position facing the air intake pipe 201c after the rotation stops, so as to avoid always facing the air intake position unchanged, resulting in reduced filtration efficiency, thereby improving the utilization rate of the filter screen cylinder 202.

[0077] The linkage assembly 206 includes a support plate 206a, a rotating column 206b, a convex ring 206c, a vertical plate 206d, a sixth spring 206e, a steel ball 206f, a cross bar 206g and a seventh spring 206h. The support plate 206a is fixedly connected to the inner wall of the box body 201a, the rotating column 206b is fixedly connected to the bottom of the third gear 205c and is rotatably connected to the surface of the support plate 206a, the convex ring 206c is fixedly connected to the lower end of the rotating column 206b, and the vertical plate 206d is slidably connected to the support plate 206a. The sixth spring 206e is sleeved on the surface of the vertical plate 206d, and its two ends are fixedly connected to the surfaces of the vertical plate 206d and the support plate 206a respectively. The steel ball 206f is rotatably connected to the lower end of the vertical plate 206d and contacts the surface of the convex ring 206c. The cross bar 206g is fixedly connected to the surface of the cleaning brush 203 and is slidably connected to the surface of the vertical plate 206d. The seventh spring 206h is sleeved on the surface of the cross bar 206g, and its two ends are fixedly connected to the surfaces of the cleaning brush 203 and the vertical plate 206d respectively.

[0078] The rotating column 206b is rotatably connected to the surface of the support plate 206a through a bearing. The upper end of the rotating column 206b is square and is inserted into the bottom of the third gear 205c. The vertical plate 206d penetrates the support plate 206a and is slidably connected thereto. The cross bar 206g penetrates the vertical plate 206d and is slidably connected thereto. The sixth spring 206e provides power for resetting the moved vertical plate 206d under the action of its elastic force, and at the same time makes the vertical plate 206d more stable when moving.

[0079] The friction between the vertical plate 206d and the convex ring 206c is reduced by the steel ball 206f. When the convex ring 206c rotates and with the cooperation of the sixth spring 206e, the vertical plate 206d can be pushed up and down to move back and forth, thereby making the cross bar 206g and the cleaning brush 203 move back and forth up and down to clean the surface of the filter cylinder 202. The seventh spring 206h makes the cleaning brush 203 better contact with the surface of the filter cylinder 202, thereby improving the cleaning effect.

[0080] Example 4 Reference Figure 3 to Figure 20 , which is the fourth embodiment of the present invention, and this embodiment is based on the first three embodiments.

[0081] Specifically, the feed pipe 108 is fixedly connected to the surface of the upper cover 101g, the discharge pipe 109 is fixedly connected to the surface of the shell 101a, the opening and closing assembly 110 is installed on the inner walls of the feed pipe 108 and the discharge pipe 109, the backwash water inlet valve 111 is connected to the surface of the shell 101a and is located on the lower side thereof, the backwash water outlet valve 112 is connected to the surface of the shell 101a and is located on the upper side thereof, the deflector 113 is fixedly connected to the inner wall of the shell 101a and is located on the upper side thereof, the sealing sleeve 114 is fixedly connected to the inner wall of the ring 104 and is in contact with the surface of the cylinder 102a, and the fixing assembly 115 is installed on the surfaces of the shell 101a and the door 101b.

[0082] The feed pipe 108 is connected to the upper cover 101g, and the discharge pipe 109 is connected to the shell 101a. The feed pipes 108 and discharge pipes 109 on the adjacent adsorption mechanisms 100 are connected to each other through pipes and valves to complete the continuous adsorption and purification treatment of phosphine at different levels. The feed pipe 108 on the front-end adsorption mechanism 100 is connected to the exhaust pipe 207 on the filtering mechanism 200 through pipes and valves, and is externally connected to the water supply pipe and the drainage pipe through the backwashing inlet valve 111 and the backwashing outlet valve 112, so as to facilitate the backwashing of the interior of the adsorption column assembly 102 to remove accumulated impurities. If cleaning is ineffective, it is necessary to consider replacing the adsorption material 102c in the new adsorption column assembly 102 to ensure smooth gas transmission.

[0083] The opening and closing component 110 is used to close and open the feed pipe 108 and the discharge pipe 109 during the opening and closing process of the box door 101b, so as to avoid a large amount of phosphine leakage caused by the corresponding valve not being closed due to negligence when the box door 101b is opened to replace the adsorption column component 102. It can be closed during this process to improve safety, and the phosphine gas entering the shell 101a is guided by the guide cover 113 to avoid direct spraying onto the surface of the float 106a and affecting the position of the float 106a.

[0084] The short block 110a is fixedly connected to the inner walls of the feed pipe 108 and the discharge pipe 109, the valve stem 110b is slidably connected to the surface of the short block 110a and fixedly connected to the surface of the valve block 110c, and the third spring 110d is sleeved on the surface of the valve stem 110b, and its two ends are fixedly connected to the surfaces of the short block 110a and the valve block 110c respectively.

[0085] The valve stem 110b passes through the short block 110a and is slidably connected thereto. When the box door 101b is opened, the rotation of the rotating rod 107a-1 can drive the top plate 107a-3 to rotate, so that the top plate 107a-3 is separated from the squeezing of the valve block 110c. Under the action of the rebound of the third spring 110d, the valve stem 110b and the valve block 110c are reset, and the feed pipe 108 and the discharge pipe 109 are blocked. On the contrary, after the adsorption column assembly 102 is replaced, when the box door 101b is closed, the top plate 107a-3 can squeeze and move the valve block 110c to open it, thereby improving the safety of use.

[0086] The handle 115a is fixedly connected to the surface of the door 101b, the limiting column 115b is fixedly connected to the surface of the shell 101a, the groove 115d is opened in the limiting column 115b, the square column 115e is slidably connected in the groove 115d and fixedly connected to the surface of the handle block 115f, the clamping column 115g is fixedly connected to the surface of the handle block 115f, the surface of the clamping plate 115c is provided with a clamping groove matching with the clamping column 115g, and the clamping column 115g is inserted into the clamping groove, the fourth spring 115h is sleeved on the surface of the square column 115e, and its two ends are respectively fixedly connected to the surface of the handle block 115f and the limiting column 115b, the surface of the clamping plate 115c is provided with a clamping hole matching with the limiting column 115b, and the clamping plate 115c is clamped to the surface of the limiting column 115b.

[0087] The clamping plate 115c is rotatably connected to the surface of the handle 115a through a bearing. The clamping plate 115c is rotated to buckle the clamping hole on the surface of the limiting column 115b, thereby fixing the closed door 101b. The surface of the clamping plate 115c is chamfered. When the clamping plate 115c is rotated and buckled on the surface of the limiting column 115b, the clamping column 115g is squeezed to move it, thereby moving the handle block 115f and the square column 115e, and stretching the fourth spring 115h.

[0088] When the card column 115g is directly opposite to the card slot, the fourth spring 115h rebounds to return the handle block 115f, the card column 115g and the square column 115e to their original positions, so that the card column 115g is inserted into the card slot, and the limiting column 115b and the card plate 115c are fixed for a second time to prevent the card plate 115c from being separated from the limiting column 115b by non-human factors. On the contrary, when releasing the fixation, one only needs to pull the handle block 115f to separate the card column 115g from the card plate 115c, and then rotate the card plate 115c to complete the unlocking of the box door 101b.

[0089] The filter mechanism 200 further includes a plugging assembly 208, which is mounted on the exhaust pipe 207 and the surface of the housing 201a. The plugging assembly 208 includes a mounting block 208a, a sliding column 208b, a stopper 208c, a cone column 208d, an eighth spring 208e, a groove 208f, an extrusion plate 208g, an inclined block 208h, a lower pressure plate 208i and a ninth spring 208j. The mounting block 208a is fixedly connected to the inner wall of the exhaust pipe 207, the sliding column 208b is slidably connected to the surface of the mounting block 208a and is fixedly connected to the bottom of the stopper 208c, and the cone column 208d is fixedly connected to the sliding column 208a. 08b lower end, the eighth spring 208e is sleeved on the surface of the sliding column 208b, and its two ends are respectively fixedly connected to the surface of the stop block 208c and the mounting block 208a, the groove 208f is opened in the box body 201a, the inclined block 208h is slidably connected in the groove 208f, the extrusion plate 208g is fixedly connected to the surface of the inclined block 208h, and passes through the exhaust pipe 207 and contacts with the surface of the cone column 208d, the lower pressure plate 208i is slidably connected to the surface of the box body 201a, and contacts with the surface of the inclined block 208h, and the two ends of the ninth spring 208j are respectively fixedly connected to the inner wall of the groove 208f and the surface of the inclined block 208h.

[0090] When the filter screen cylinder 202 is taken out to flush the box body 201a through the sealing component 208, the exhaust pipe 207 is blocked to prevent liquid from entering the exhaust pipe 207, so that the liquid is discharged from the slag discharge pipe set at the bottom of the box body 201a, and the sliding column 208b penetrates the mounting block 208a and is slidably connected thereto, and the extrusion plate 208g is sealed with the box body 201a and the exhaust pipe 207, and the lower pressure plate 208i is sealed with the box body 201a.

[0091] When the filter screen cartridge 202 is removed, the lower pressure plate 208i is no longer squeezed, and the ninth spring 208j rebounds to cause the inclined block 208h and the extrusion plate 208g to move and reset. The inclined block 208h moves to squeeze and lift the lower pressure plate 208i, and the extrusion plate 208g moves away from the support of the cone column 208d. Under the rebound of the eighth spring 208e, the sliding column 208b, the block 208c and the cone column 208d move down and reset. The block 208c blocks the upper end of the exhaust pipe 207 to prevent liquid from entering during flushing and to prevent blockage and carrying of a large amount of water vapor during subsequent ventilation. On the contrary, after the filter screen cartridge 202 is installed, the block 208c moves upward to open the exhaust pipe 207.

[0092] When in use, the air inlet pipe 201c is connected to the distillation tower through pipelines and valves, and the discharge pipe 109 on the adsorption mechanism 100 at the rear end is connected to the steel cylinder group through pipelines and a pressurizing device. The distilled phosphine is firstly filtered through the filtering mechanism 200 to retain impurities and particles in the box 201a, and then is sequentially adsorbed and purified by the adsorption column assemblies 102 in three different adsorption mechanisms 100 and discharged, so that the ultra-pure phosphine is injected into the steel cylinder.

[0093] When the adsorption column assembly 102 is clogged due to long-term use, causing the high-pressure gas to encounter transmission obstruction when entering the adsorption column assembly 102, resulting in poor gas flow, the adsorption column assembly 102 needs to be replaced, and the valve between the distillation tower and the filtering mechanism 200 is closed to discharge the gas in the adsorption mechanism 100 as much as possible, and then the valve is closed. The buoyancy of the float 106a gradually decreases, and under the action of the rebound of the first spring 106d-9 and the downward movement of the float 106a, the connecting ring 106d-6, the limiting rod 106b and the sealing ring 106d-10 move up, and the movable plate 106d-5 rotates, so that the sealing ring 106d-10 disengages from the limiting groove 102d and moves into the ring groove 101j, and the limiting rod 106b moves up and disengages from the limiting groove 102d.

[0094] The box door 101b is rotated to open, thereby driving the connecting block 107b-2 and the short column 107b-3 to rotate. The short column 107b-3 moves in the connecting plate 107b-1 and drives the connecting plate 107b-1 to rotate. The connecting plate 107b-1 rotates to drive the rotating rod 107a-1 and the round block 107a-6, the first gear 107a-4 and the top plate 107a-3 thereon to rotate. The rotation of the top plate 107a-3 disengages it from the closing component 110, closing the feed pipe 108 and the discharge pipe 109.

[0095] The rotation of the first gear 107a-4 causes the teeth 107a-5 and the ring plate 103 to rotate. The ring plate 103 gradually loses its effect on the wedge block 105. Under the action of the rebound of the second spring 107a-7, the ring 104, the sealing sleeve 114 and the wedge block 105 move, and the ring 104 is separated from the limit on the adsorption column assembly 102. The adsorption column assembly 102 can be removed. If it cannot be removed, it means that the gas in the shell 101a has not been exhausted, and the limit rod 106b has not lost the limit on the adsorption column assembly 102. It can be removed only when the gas in the shell 101a is exhausted, thereby improving safety. During installation, the reverse operation is performed in accordance with the disassembly and assembly steps.

[0096] When the blockage caused by impurities and particles attached to the surface of the filter cylinder 202 cannot meet the filtering requirements, the pressure in the box 201a gradually increases, thereby overcoming the elastic force of the fifth spring 204g to push the piston 204d to move, so that the square rod 204c and the first conductive sheet 204e move, contact the second conductive sheet 204f to energize the motor 205b to operate, and the rotation of the output shaft of the motor 205b drives the third gear 205c and the rotating column 206b to rotate. The third gear 205c rotates multiple circles before the second gear 205a and the filter cylinder 202 rotate one circle.

[0097] When the rotation of the rotating column 206b drives the convex ring 206c to rotate and with the cooperation of the sixth spring 206e, it can lift the vertical plate 206d up and down reciprocatingly, and then make the cross bar 206g and the cleaning brush 203 move up and down reciprocatingly, clean the surface of the filter cylinder 202, and improve the filtering effect. The pressure in the box body 201a gradually decreases and cannot overcome the elastic force generated by the compression of the fifth spring 204g, so that the first conductive sheet 204e and the second conductive sheet 204f are separated and no longer energized, thereby stopping the rotation of the filter cylinder 202 and the movement of the cleaning brush 203.

[0098] In summary, the adsorption mechanism 100 can perform multi-stage adsorption purification on phosphine, and at the same time, it is convenient to quickly disassemble and replace the adsorption column that has been used for a long time. Compared with the prior art, the high-pressure gas is not prone to encounter transmission obstruction when entering the adsorption column, so that the gas flows smoothly, thereby improving the operating efficiency of the entire production line. The filtering mechanism 200 can perform preliminary filtration on the phosphine before entering the adsorption device. Compared with the prior art, it can intercept large impurities and particulate matter that may enter the adsorption column, thereby extending the service life of the adsorption column.

[0099] The following is a fifth embodiment of the present invention, which is based on the first four embodiments.

[0100] First, nitrogen or helium is used to purge, replace and evacuate, then yellow phosphorus and calcium hydroxide are added to the reactor, the stirring device of the reactor is started, and the stirring is uniformly stirred at a speed of 90 to 120 r / min; the temperature is controlled to be 80 to 100°C; then the flowmeter is used to control the flow of sodium hydroxide solution, the reaction pressure is 0 to 0.25 MPa, and the reaction time is 1 to 5 hours to obtain crude phosphine. Then, the crude phosphine generated by the reaction is condensed through a primary condenser and a secondary condenser, wherein the temperature of the primary condenser B is controlled to be -50 to -30°C, and the temperature of the secondary condenser C is controlled to be -70 to -50°C, and high-boiling impurities are preliminarily removed by two-stage low-temperature freezing, and then the crude phosphine is reheated, and the vaporized crude phosphine enters the distillation tower for distillation, and then enters the filtering mechanism 200 and multiple adsorption mechanisms 100 connected in series in sequence to obtain the gas to be purified. Then, the gas to be purified is passed through the light removal tower and the heavy removal tower in sequence to obtain ultra-pure phosphine.

[0101] Finally, the ultrapure phosphine is collected in a steel cylinder.

[0102] In this embodiment, the total amount of yellow phosphorus fed is 12000 g, and 2880 g of ultrapure phosphine product with a purity of 99.99995% is finally obtained.

[0103] 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. An adsorption column device, characterized in that: include: The adsorption mechanism (100) and the filtering mechanism (200) are as follows: The adsorption mechanism (100) comprises a shell (101), an adsorption column assembly (102), a ring plate (103), a collar (104), a wedge (105) and a limit assembly (106), wherein the adsorption column assembly (102) is installed in the shell (101), the transmission assembly (107) is installed on the inner wall of the shell (101), the number of the ring plates (103) is two, which are installed on the outer surface of the transmission assembly (107) and are symmetrically located in the inner cavity of the shell (101), the number of the collar (104) is two, which are installed on the outer surface of the transmission assembly (107) and are symmetrically sleeved on the outer surface of the adsorption column assembly (102), and the wedge (105) is fixedly connected to the outer surface of the collar (104). The limiting component (106) is installed on the inner wall of the shell (101) and is located above the inner cavity. The limiting component (106) comprises a float (106a), a limiting rod (106b), a rubber ring (106c) and an associated component (106d). The float (106a) and the limiting rod (106b) are arranged on the outer surface of the associated component (106d). The float (106a) is located above the limiting rod (106b). The associated component (106d) is located between the float (106a) and the limiting rod (106b). The associated component (106d) is arranged on the inner surface of the shell (101). The rubber ring (106c) is sleeved on the surface of the lower end of the limiting rod (106b); and, The filtering mechanism (200) is arranged at the air inlet end of the adsorption mechanism (100), and comprises a box (201), a filter screen cylinder (202), a cleaning brush (203) and a monitoring power-on component (204); the filter screen cylinder (202) is arranged in the inner cavity of the box (201), the surface of the cleaning brush (203) is in contact with the surface of the filter screen cylinder (202), and the monitoring power-on component (204) is arranged on the upper surface of the box (201).

2. The adsorption column device according to claim 1, characterized in that: The shell (101) comprises a shell (101a), a box door (101b), an upper cover (101c), a lower cover (101d), a first sealing gasket (101e), a second sealing gasket (101f), an upper cover (101g), a lower cover (101h), a ball (101i) and an annular groove (101j); the box door (101b) is pivotally connected to the outer surface of the shell (101a); the upper cover (101c) and the lower cover (101d) are respectively fixedly connected to the upper end and the lower end of the inner wall of the shell (101a); the first sealing gasket (101e) is fixedly connected to the top of the lower cover (101d); the second sealing gasket (101f) is fixedly connected to the bottom of the upper cover (101c); the upper cover (101g) is fixedly connected to the top of the shell (101a); the lower cover (101h) is fixedly connected to the Connected to the bottom of the shell (101a), one ring plate (103) is rotatably connected to the outer surface of the lower end of the upper cover (101c), and the other ring plate (103) is rotatably connected to the outer surface of the upper end of the lower cover (101d). The number of the balls (101i) is plural and they are respectively arranged between the inner surface of the upper ring plate (103) and the outer surface of the upper cover (101c), and between the inner surface of the lower ring plate (103) and the outer surface of the lower cover (101d). The annular groove (101j) is opened at the bottom of the upper cover (101c). The lower end of the limit rod (106b) passes through the bottom of the upper cover (101c) and is slidably connected thereto. The rubber ring (106c) is slidably connected in the annular groove (101j), and the surface of the second sealing gasket (101f) contacts the surface of the rubber ring (106c).

3. The adsorption column device according to claim 2, characterized in that: The adsorption column assembly (102) comprises a cylinder (102a), a grid plate (102b), an adsorption material (102c) and a limiting groove (102d); the bottom of the cylinder (102a) contacts the top of a first sealing gasket (101e); the top of the cylinder (102a) contacts the bottom of a second sealing gasket (101f); the grid plate (102b) is fixedly connected to the inner wall of the cylinder (102a); the adsorption material (102c) is filled in the inner cavity of the cylinder (102a); the limiting groove (102d) is opened at the top of the cylinder (102a); the limiting rod (106b) is inserted into the limiting groove (102d); and the rubber ring (106c) is slidably connected to the limiting groove (102d).

4. The adsorption column device according to claim 2, characterized in that: The associated component (106d) comprises a support block (106d-1), a slide rod (106d-2), a fixed plate (106d-3), an inclined plate (106d-4), a movable plate (106d-5), a connecting ring (106d-6), a short rod (106d-7), a slot (106d-8), a first spring (106d-9) and a sealing ring (106d-10), wherein the support block (106d-1) is fixedly connected to the inner wall of the upper cover (101c), and the slide rod (106d-2 ) is fixedly connected to the top of the support block (106d-1), the floating body (106a) is sleeved on the surface of the sliding rod (106d-2), the fixed plate (106d-3) is fixedly connected to the bottom of the floating body (106a), the inclined plates (106d-4) are two in number and are fixedly connected to the middle and lower part of the sliding rod (106d-2) in a left-right symmetrical manner, the movable plate (106d-5) is rotatably connected to the end of the inclined plate (106d-4), and the connecting ring (106d-6) is fixedly connected to the limiting rod (1 06d-3), the slot (106d-8) is opened on the surface of the movable plate (106d-5), and one movable plate (106d-5) has two symmetrical slots (106d-8) on its surface, the number of the short rods (106d-7) is four, one end of two short rods (106d-7) is fixedly connected to the bottom of the fixed plate (106d-3), and the other end is slidably connected to the slot (106d-8) at the upper end of the movable plate (106d-5), and the other two short rods (106d- 7), one end of which is fixedly connected to the top of the connecting ring (106d-6), and the other end of which is slidably connected to the slot (106d-8) at the lower end of the movable plate (106d-5); the first spring (106d-9) and the sealing ring (106d-10) are both sleeved on the limiting rod (106b); the two ends of the first spring (106d-9) are respectively fixedly connected to the surface of the upper cover (101c) and the connecting ring (106d-6); and the sealing ring (106d-10) is fixedly connected to the surface of the upper cover (101c).

5. The adsorption column device according to claim 4, characterized in that: The adsorption mechanism (100) further comprises a transmission assembly (107), wherein the transmission assembly (107) comprises a rotating member (107a), a force-applying member (107b) and a position-limiting arc plate (107c), wherein the force-applying member (107b) is installed between the inner surface of the box door (101b) and the outer surface of the rotating member (107a), and the rotating member (107a) is installed on the outer surfaces of the upper cover (101c), the lower cover (101d) and the force-applying member (107b). There are two position-limiting arc plates (107c) and they are symmetrically fixedly connected to the middle part of the inner wall of the housing (101a). The inner surface of the arc plate (107c) contacts the outer surface of the cylinder (102a); the force-applying member (107b) comprises a connecting plate (107b-1), a connecting block (107b-2) and a short column (107b-3); the connecting block (107b-2) is fixedly connected to the inner surface of the box door (101b); the short column (107b-3) is fixedly connected to the outer surface of the connecting block (107b-2); the connecting plate (107b-1) is arranged on the outer surface of the rotating member (107a); and the short column (107b-3) is slidably connected to the inner wall of the connecting plate (107b-1).

6. The adsorption column device according to claim 1, characterized in that: The filtering mechanism (200) further comprises a driving member (205), a linkage assembly (206) and an exhaust pipe (207); the box member (201) comprises a box body (201a), a cover plate (201b) and an air intake pipe (201c); the filter screen cylinder (202) and the cleaning brush (203) are both located in the inner cavity of the box body (201a); the cover plate (201b) is fixedly connected to the top of the box body (201a); the driving member (205) is arranged on the outer surfaces of the cover plate (201b) and the filter screen cylinder (202); the linkage assembly (206) is installed on the driving member (201c); 5) and the inner wall of the box body (201a), the cleaning brush (203) is installed on the outer surface of the linkage component (206), the monitoring power supply component (204) is installed on the top of the cover plate (201b), the air inlet pipe (201c) is connected to the outer surface of the box body (201a), the filter screen cylinder (202) is rotatably connected to the bottom of the cover plate (201b), the bottom of the filter screen cylinder (202) is in contact with the inner wall of the box body (201a), and one end of the exhaust pipe (207) is fixedly connected to the bottom of the box body (201a) and inserted into the filter screen cylinder (202).

7. The adsorption column device according to claim 6, characterized in that: The monitoring power-on component (204) comprises a connecting pipe (204a), a fixing block (204b), a square rod (204c), a piston (204d), a first conductive sheet (204e), a second conductive sheet (204f) and a fifth spring (204g); the connecting pipe (204a) is fixedly connected to the surface of the cover plate (201b) and extends to the inner cavity of the box body (201a); the fixing block (204b) is fixedly connected to the inner wall of the connecting pipe (204a); and the square rod (204c) is slidably connected to the connecting pipe (204a). The surface of the fixed block (204b), the piston (204d) is fixedly connected to one end of the square rod (204c) and slidably connected to the inner wall of the connecting tube (204a), the first conductive sheet (204e) is fixedly connected to the other end of the square rod (204c), the second conductive sheet (204f) is fixedly connected to the inner wall of the connecting tube (204a), and the fifth spring (204g) is sleeved on the square rod (204c), and its two ends are respectively fixedly connected to the fixed block (204b) and the surface of the piston (204d).

8. The adsorption column device according to claim 6, characterized in that: The driving member (205) comprises a second gear (205a), a motor (205b) and a third gear (205c); the second gear (205a) is sleeved on the upper end surface of the filter screen cylinder (202); the motor (205b) is fixedly connected to the top of the cover plate (201b); the output shaft of the motor (205b) is fixedly connected to the top of the third gear (205c); and the second gear (205a) is meshed with the third gear (205c).

9. The adsorption column device according to claim 8, characterized in that: The linkage assembly (206) comprises a support plate (206a), a rotating column (206b), a convex ring (206c), a vertical plate (206d), a sixth spring (206e), a steel ball (206f), a cross bar (206g) and a seventh spring (206h), wherein the support plate (206a) is fixedly connected to the inner wall of the box body (201a), the rotating column (206b) is fixedly connected to the bottom of the third gear (205c) and is rotatably connected to the surface of the support plate (206a), the convex ring (206c) is fixedly connected to the lower end of the rotating column (206b), and the vertical plate (206d) is slidably connected to the support plate ( The sixth spring (206e) is sleeved on the surface of the vertical plate (206d), and its two ends are respectively fixedly connected to the surface of the vertical plate (206d) and the surface of the support plate (206a); the steel ball (206f) is rotatably connected to the lower end of the vertical plate (206d) and contacts the surface of the convex ring (206c); the cross bar (206g) is fixedly connected to the surface of the cleaning brush (203) and slidably connected to the surface of the vertical plate (206d); the seventh spring (206h) is sleeved on the surface of the cross bar (206g), and its two ends are respectively fixedly connected to the surface of the cleaning brush (203) and the surface of the vertical plate (206d).

10. A process for continuously producing ultrapure phosphine, using an adsorption column device as claimed in any one of claims 1 to 9, characterized in that: The following steps are involved: S1, add yellow phosphorus and calcium hydroxide to a reactor, and under stirring, add sodium hydroxide solution through a flow meter to control the flow to react, to obtain crude phosphine; S2, condensing the crude phosphine to preliminarily remove high-boiling-point impurities in the crude phosphine, then reheating the crude phosphine, and the vaporized crude phosphine is distilled and then sequentially enters a filtering mechanism (200) and a plurality of adsorption mechanisms (100) connected in series to obtain a gas to be purified; S3, passing the gas to be purified into a light removal tower and a heavy removal tower in sequence to obtain ultrapure phosphine; and S4. Collect the ultrapure phosphine into a steel bottle.

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