CN114307199B - Multistage purification method for purifying organic phosphine - Google Patents
Multistage purification method for purifying organic phosphine Download PDFInfo
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- CN114307199B CN114307199B CN202111656015.XA CN202111656015A CN114307199B CN 114307199 B CN114307199 B CN 114307199B CN 202111656015 A CN202111656015 A CN 202111656015A CN 114307199 B CN114307199 B CN 114307199B
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Abstract
The invention discloses an organic phosphine purification device with multi-stage purification, belonging to the technical field of organic phosphine purification, comprising: purification case, driving motor is installed to purification bottom of the case portion wall, the detection case passes through the inner chamber intercommunication of installing port and purification case, there is the movable plate detection incasement chamber bottom through supporting spring slidable mounting, second touch switch is installed at detection incasement chamber top, the warning light is installed to detection incasement top wall, and second touch switch and warning light electric connection, when purification incasement pressure increases in the device, can push away the movable plate and shift up, makes the space increase of detection case and purification incasement internal connection for reduce the inside atmospheric pressure of purification incasement, and when the atmospheric pressure of purification incasement portion was too big, the movable plate can press second touch switch, makes the warning light luminous, and also makes the air-blower stop work, avoids atmospheric pressure to continue to increase and cause the influence to purification equipment, also avoids influencing the leakproofness of purification equipment, avoids volatile organic phosphine to leak.
Description
Technical Field
The invention relates to the technical field of organic phosphine purification, in particular to a multistage purification method of organic phosphine.
Background
The organic phosphine is an organic compound with a carbon-phosphorus bond, a purifier is used when the organic phosphine is purified by using an organic phosphine solution at present, and a purifier is disclosed in a publication of a multistage purification organic phosphine purifier with the application number of CN201820561486. X;
in the purification process, air can be blown into the purification tank, in order to ensure that the volatile organic phosphine is only discharged from the discharge pipe, other areas of the purification tank are closed, however, the air pressure in the purification tank is easily overlarge, the tightness of a feeding area is easily affected, and the condition that the volatile organic phosphine is leaked exists.
Disclosure of Invention
The invention aims to provide a multistage purification method for purifying organic phosphine, which solves the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a multistage purification's organic phosphine purification device includes: a purification box;
the wall of the bottom of the purification box is provided with a driving motor, an output shaft at the top of the driving motor extends into the inner cavity of the purification box and is connected with a stirring rod, the outer wall of the stirring rod is uniformly provided with a turning plate, the wall of the bottom of the left side of the purification box is provided with a discharge pipe, a valve is arranged on the discharge pipe, the left side wall of the top of the purification box is provided with a feed inlet, and a top cover is inserted in the inner cavity of the feed inlet;
the left side wall of the purification box is provided with an air blower, an air outlet of the air blower is communicated with an inner cavity of the purification box through a guide pipe, the right side wall of the purification box is sequentially provided with a first purification box, a condenser and a second purification box from top to bottom, and the top of the inner cavity of the purification box is sequentially communicated with the inner cavity of the first purification box, the condenser and the second purification box through connecting pipes;
the detection case is installed to purification roof portion wall, the installing port has been seted up to detection case inner chamber bottom, the detection case passes through the inner chamber intercommunication of installing port and purification case, there is the movable plate detection case inner chamber bottom through supporting spring slidable mounting, second touch switch is installed at detection case inner chamber top, the warning light is installed to detection case roof portion wall, and second touch switch and warning light electric connection.
Preferably, the second touch switch is electrically connected to the blower.
Preferably, a first touch switch is installed on the wall of the top of the movable plate, a pressing plate is installed on the top of the inner cavity of the detection box, the pressing plate is located right above the first touch switch, and the first touch switch is electrically connected with the air blower.
Preferably, the top of the inner cavity of the detection box is provided with a mounting hole, a moving rod is inserted into the inner cavity of the mounting hole in a sliding mode through an elastic piece, and the bottom end of the moving rod is connected with the top wall of the pressing plate.
Preferably, the top wall of the moving rod is provided with a screw hole, an inner cavity of the screw hole is in threaded connection with an adjusting screw rod, and the bottom end of the adjusting screw rod is connected with the top wall of the pressing plate.
Preferably, the installation sleeve is installed on the wall of the top of the purification box, the movable plate is installed on the top of an inner cavity of the installation sleeve in a sliding mode through the reset spring, the connecting rod is installed on the wall of the top of the movable plate, the top end of the connecting rod extends to the outer side of the top of the installation sleeve and is connected with the support plate, the wall of the bottom of the support plate is connected with the pressure rod, the pressing block is installed at the bottom end of the pressure rod, and the top of the inner cavity of the installation sleeve is communicated with the top of the inner cavity of the detection box through the connecting pipe.
Preferably, the top wall of the pressing block is provided with a movable sleeve, and the movable sleeve is sleeved on the outer wall of the pressing rod through an elastic piece in a sliding mode.
Preferably, the threaded sleeve is installed at installation cover inner chamber top, fly leaf top wall rotates installs the threaded rod, the threaded rod top runs through the threaded sleeve and is connected with the connecting rod bottom.
Preferably, the purification method of the organic phosphine with multi-stage purification comprises the following steps:
the first step is as follows: opening the top cover, then pouring the organic phosphine solution into the purification box through the feeding hole, covering the top cover, switching on a power supply of a driving motor and an air blower, working the air blower at the moment, introducing air into the purification box, so as to accelerate volatilization of the organic phosphine in the organic phosphine solution, meanwhile, driving the driving motor to drive a stirring rod to drive a stirring plate to stir the organic phosphine solution, increasing the contact area of the organic phosphine solution and the air, further accelerating volatilization of the organic phosphine, and discharging the volatilized organic phosphine which sequentially enters the first purification box, the condenser and the second purification box through connecting pipes, so as to finish purification of the organic phosphine;
the second step is that: leading-in air to purification incasement portion at the air-blower, and when making the inside atmospheric pressure of purification incasement great, air pressure can push the movable plate and move upward, can press the second touch switch, makes the warning light luminous suggestion staff to make the air-blower stop work, protect purification equipment.
Compared with the prior art, the invention has the beneficial effects that: when purification incasement portion pressure increases in the device, can push away the movable plate and shift up, make detection case and purification incasement portion internal connection's space increase for reduce the atmospheric pressure of purification incasement portion, and when purification incasement portion atmospheric pressure was too big, the movable plate can press the second touch switch, make the warning light luminous, and also make the air-blower stop work, avoid atmospheric pressure to continue to increase and cause the influence to purification equipment, also avoid influencing the leakproofness of purification equipment, avoid volatile organic phosphine to leak.
Drawings
FIG. 1 is a schematic view of the structure of the present invention;
FIG. 2 is a schematic view of the connection structure of the detection box and the movable plate according to the present invention;
FIG. 3 is a schematic view of the connection structure of the pressing rod and the pressing block according to the present invention;
FIG. 4 is an enlarged view of the structure at A of the present invention.
In the figure: 1. a purification box; 2. a drive motor; 3. turning over the board; 4. a blower; 5. a first purge bin; 6. a condenser; 7. a second purge bin; 8. a detection box; 9. moving the plate; 10. a support spring; 11. a first touch switch; 12. pressing a plate; 13. a warning light; 14. a top cover; 15. installing a sleeve; 16. a second touch switch; 17. connecting pipes; 18. a travel bar; 19. adjusting the screw rod; 20. a movable plate; 21. a return spring; 22. a connecting rod; 23. a support plate; 24. a pressure lever; 25. a movable sleeve; 26. pressing into blocks; 27. a threaded rod; 28. and (4) a threaded sleeve.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a technical scheme that: an apparatus for purifying organophosphine with multi-stage purification, please refer to fig. 1, comprising: a purification box 1;
in order to stir the organic phosphine solution in the purification box 1, a driving motor 2 for driving a stirring rod to rotate is arranged on the bottom wall of the purification box 1, an output shaft at the top of the driving motor 2 is connected with the stirring rod in the purification box 1, a turning plate 3 for turning the organic phosphine solution is arranged on the outer wall of the stirring rod, a discharge pipe is arranged on the bottom wall of the left side of the purification box 1, a valve is arranged on the discharge pipe, a feed inlet is formed in the left side wall of the top of the purification box 1, a top cover 14 is inserted into an inner cavity of the feed inlet, and electric equipment related to the device is electrically connected with an external power switch through a wire;
referring to fig. 1, in order to blow air into a purification box 1 and increase a contact area between an organophosphine solution and air, a blower 4 is installed on a left side wall of the purification box 1, an air outlet of the blower 4 is communicated with an inner cavity of the purification box 1 by using a conduit, air is blown into the purification box 1, a first purification box 5, a condenser 6 and a second purification box 7 are sequentially installed on a right side wall of the purification box 1 from top to bottom, the top of the inner cavity of the purification box 1 is sequentially communicated with the inner cavities of the first purification box 5, the condenser 6 and the second purification box 7 by connecting pipes, and the first purification box 5, the condenser 6 and the second purification box 7 are the same as structural devices disclosed in a publication of a multistage purification organophosphine purifier with application number of cn201820561486 ×;
referring to fig. 1 and 2, in order to reduce the air pressure inside the purification box 1, a detection box 8 is installed on the top wall of the purification box 1, a mounting hole is formed in the bottom of an inner cavity of the detection box 8 to communicate the detection box 8 with the inner cavity of the purification box 1, a movable plate 9 is slidably installed at the bottom of the inner cavity of the detection box 8 through a support spring 10, when the pressure inside the purification box 1 increases, the movable plate 9 is pushed to move upwards, so that the space where the detection box 8 is connected with the purification box 1 is increased, the air pressure inside the purification box 1 is reduced, in order to improve the safety, a second touch switch 16 is installed at the top of the inner cavity of the detection box 8, a warning lamp 13 connected with the second touch switch 16 is installed on the top wall of the detection box 8, when the air pressure inside the purification box 1 is too high, the movable plate 9 presses the second touch switch 16 to make the warning lamp 13 emit light, and also stop the operation of the air blower 4, so that the influence on the sealing performance of the purification equipment is avoided, and the influence on the sealing performance of the purification equipment is also avoided, and the second touch switch 16 is electrically connected with the air blower 4;
referring to fig. 2, in order to add a protection measure, a first touch switch 11 for controlling the blower 4 is installed on the top wall of the movable plate 9, a pressing plate 12 located above the first touch switch 11 is installed on the top of the inner cavity of the detection box 8, the pressing plate 12 is firstly contacted with the first touch switch 11 in the process of moving the movable plate 9 upwards, so that the blower 4 stops working, and when the air pressure in the purification box 1 is reduced and the movable plate 9 moves downwards, the blower 4 works again, so that the purification equipment has self-regulation capability;
referring to fig. 2, in order to avoid the pressing plate 12 from preventing the moving plate 9 from contacting the second touch switch 16, the top of the inner cavity of the detection box 8 is provided with a mounting hole, and the inner cavity of the mounting hole is slidably inserted with a moving rod 18 connected with the pressing plate 12 through an elastic member, so that the moving rod 18 can move up the pressing plate 12, in order to change the distance between the pressing plate 12 and the first touch switch 11, the time for controlling the blower 4 is adjusted, the top wall of the moving rod 18 is provided with a screw hole, an adjusting screw 19 passes through the screw hole to be connected with the pressing plate 12, and the position of the adjusting screw 19 is changed by matching with the screw hole, so that the height of the pressing plate 12 is changed.
Example 2:
referring to fig. 1, 3 and 4, on the basis of embodiment 1, in order to improve the sealing performance of the feeding region, an installation sleeve 15 is installed on the top wall of a purification box 1, a movable plate 20 is installed on the top of an inner cavity of the installation sleeve 15 in a sliding manner through a return spring 21, a connecting rod 22 is installed on the top wall of the movable plate 20, the top end of the connecting rod 22 extends to the outside of the top of the installation sleeve 15 and is connected with a support plate 23, the bottom wall of the support plate 23 is connected with a pressing rod 24, a pressing block 26 is installed at the bottom end of the pressing rod 24, the top of the inner cavity of the installation sleeve 15 is communicated with the top of the inner cavity of a detection box 8 through a connecting pipe 17, when the movable plate 9 moves upwards, air on the top of the inner cavity of the detection box 8 can enter the top of the inner cavity of the installation sleeve 15, the movable plate 20 moves downwards, the threaded rod 27 penetrates through the threaded sleeve 28, the connecting rod 22 rotates, the pressing block 26 moves above the top cover 14, then the movable plate 20 continues to move downwards, the pressing block 26 is pressed above the top cover 14, the top cover 14 is installed at the feed inlet more tightly, the sealing performance of the position is guaranteed, the threaded sleeve 28 is installed at the top of the inner cavity of the installation sleeve 15, the threaded rod 27 is installed on the wall of the top of the movable plate 20 in a rotating mode, the top end of the threaded rod 27 penetrates through the threaded sleeve 28 and is connected with the bottom end of the connecting rod 22, the movable sleeve 25 is installed on the wall of the top of the pressing block 26, and the movable sleeve 25 is sleeved on the outer wall of the pressing rod 24 in a sliding mode through an elastic piece;
compared with the embodiment 1, the components such as the pressing block 26 and the pressing rod 24 are added, the pressing block 26 moves downwards to press the top cover 14 when the moving plate 9 moves upwards, and the sealing performance of the feeding area is improved.
A multistage purification method for organic phosphine comprises the following steps:
the first step is as follows: opening the top cover 14, then pouring the organic phosphine solution into the purification box 1 through the feeding hole, covering the top cover 14, switching on the power supplies of the driving motor 2 and the air blower 4, working the air blower 4 at the moment, introducing air into the purification box 1, so as to accelerate volatilization of the organic phosphine in the organic phosphine solution, meanwhile, driving the driving motor 2 to drive the stirring rod to stir the organic phosphine solution, increasing the contact area of the organic phosphine solution and the air, further accelerating volatilization of the organic phosphine, enabling the volatilized organic phosphine to sequentially enter the first purification box 5, the condenser 6 and the second purification box 7 through the connecting pipes, and then discharging the volatilized organic phosphine, so as to complete purification of the organic phosphine;
the second step is that: when the air blower 4 introduces air into the purification box 1 and the air pressure in the purification box 1 is high, the air pressure pushes the movable plate 9 to move upwards, the second touch switch 16 is pressed, the warning lamp 13 emits light to prompt a worker, the air blower 4 stops working, and purification equipment is protected.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The utility model provides an organic phosphine purification device of multistage purification which characterized in that: the method comprises the following steps: a purification tank (1); the wall of the bottom of the purification box (1) is provided with a driving motor (2), an output shaft at the top of the driving motor (2) extends into the inner cavity of the purification box (1) and is connected with a stirring rod, the outer wall of the stirring rod is uniformly provided with a turning plate (3), the wall of the bottom of the left side of the purification box (1) is provided with a discharge pipe, a valve is arranged on the discharge pipe, the left side wall of the top of the purification box (1) is provided with a feed inlet, and a top cover (14) is inserted into the inner cavity of the feed inlet;
the air blower (4) is installed on the left side wall of the purification box (1), an air outlet of the air blower (4) is communicated with an inner cavity of the purification box (1) through a guide pipe, a first purification box (5), a condenser (6) and a second purification box (7) are sequentially installed on the right side wall of the purification box (1) from top to bottom, and the top of the inner cavity of the purification box (1) is sequentially communicated with the inner cavity of the first purification box (5), the inner cavity of the condenser (6) and the inner cavity of the second purification box (7) through connecting pipes;
the detection box (8) is installed on the wall of the top of the purification box (1), an installation opening is formed in the bottom of an inner cavity of the detection box (8), the detection box (8) is communicated with the inner cavity of the purification box (1) through the installation opening, a movable plate (9) is installed on the bottom of the inner cavity of the detection box (8) in a sliding mode through a supporting spring (10), a second touch switch (16) is installed on the top of the inner cavity of the detection box (8), a warning lamp (13) is installed on the wall of the top of the detection box (8), and the second touch switch (16) is electrically connected with the warning lamp (13);
the wall of the top of the purification box (1) is provided with an installation sleeve (15), the top of an inner cavity of the installation sleeve (15) is provided with a movable plate (20) in a sliding mode through a return spring (21), the wall of the top of the movable plate (20) is provided with a connecting rod (22), the top end of the connecting rod (22) extends to the outer side of the top of the installation sleeve (15) and is connected with a support plate (23), the wall of the bottom of the support plate (23) is connected with a pressure lever (24), the bottom end of the pressure lever (24) is provided with a pressing block (26), and the top of the inner cavity of the installation sleeve (15) is communicated with the top of the inner cavity of the detection box (8) through a connecting pipe (17);
a movable sleeve (25) is arranged on the top wall of the pressing block (26), and the movable sleeve (25) is sleeved on the outer wall of the pressing rod (24) in a sliding mode through an elastic piece;
threaded sleeve (28) are installed at installation cover (15) inner chamber top, fly leaf (20) top wall rotates installs threaded rod (27), threaded rod (27) top run through threaded sleeve (28) and be connected with connecting rod (22) bottom.
2. The purification apparatus of organic phosphine with multi-stage purification according to claim 1, wherein: the second touch switch (16) is electrically connected with the blower (4).
3. The purification apparatus of organic phosphine with multi-stage purification according to claim 1, wherein: first touch switch (11) are installed to movable plate (9) top wall, clamp plate (12) are installed at detection case (8) inner chamber top, clamp plate (12) are located first touch switch (11) directly over, first touch switch (11) and air-blower (4) electric connection.
4. The purification apparatus of organic phosphine with multi-stage purification according to claim 3, wherein: the top of the inner cavity of the detection box (8) is provided with a mounting hole, a moving rod (18) is slidably inserted into the inner cavity of the mounting hole through an elastic piece, and the bottom end of the moving rod (18) is connected with the top wall of the pressing plate (12).
5. The purification device of organic phosphine with multi-stage purification according to claim 4, wherein: the top wall of the moving rod (18) is provided with a screw hole, an inner cavity of the screw hole is in threaded connection with an adjusting screw rod (19), and the bottom end of the adjusting screw rod (19) is connected with the top wall of the pressing plate (12).
6. The purification device of organic phosphine with multi-stage purification according to claim 1, wherein: the first step is as follows: opening a top cover (14), pouring an organic phosphine solution into a purification box (1) through a feeding hole, covering the top cover (14), switching on a power supply of a driving motor (2) and an air blower (4), working the air blower (4), introducing air into the purification box (1) so as to accelerate volatilization of the organic phosphine in the organic phosphine solution, driving the driving motor (2) to drive a stirring rod to stir the organic phosphine solution by a turning plate (3), increasing the contact area of the organic phosphine solution and the air, further accelerating volatilization of the organic phosphine, and discharging the volatilized organic phosphine which sequentially enters a first purification box (5), a condenser (6) and a second purification box (7) through connecting pipes so as to finish purification of the organic phosphine;
the second step is that: when the air blower (4) introduces air into the purification box (1) and the air pressure in the purification box (1) is large, the air pressure pushes the moving plate (9) to move upwards, the second touch switch (16) is pressed, the warning lamp (13) emits light to prompt a worker, the air blower (4) stops working, and purification equipment is protected.
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