Synthesis and purification device and synthesis and purification method for electronic-grade phosphorane by using synthesis and purification device

Abstract

The invention discloses a synthesis and purification device and a synthesis and purification method for electronic grade phosphorane, and relates to the technical field of phosphorane synthesis, the synthesis and purification device comprises a reaction kettle and a liquid nitrogen tank, the top of the reaction kettle is provided with an input pipeline, and the side face of the reaction kettle is connected with a condenser by arranging a pipeline. The synthesis and purification method of the electronic grade phosphorane comprises the following steps: injecting a raw material into a reaction kettle through an input pipeline, carrying out corresponding synthesis operation, starting a servo motor, driving a power sleeve to rotate clockwise, and matching with a hydraulic bin I, a turntable, a torsion spring, an extrusion block, a stress rod I, a half gear ring, a rotating rod I, a rotating rod II, a gear, a bevel gear I and a bevel gear II to synthesize the electronic grade phosphorane. The stirring plate rotates in the horizontal direction, and the mixing plate rotates in the vertical direction, so that the stirring effect of the device is improved, and the synthesis and purification efficiency of the device is improved.

Description

Technical Field

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

[0002] The synthesis and purification technology of electronic grade phosphine is a very important link in high-tech industries such as electronics, semiconductors, and optoelectronics. As an important gas chemical raw material, phosphine is widely used in the growth of semiconductor materials, thin film deposition, and the manufacture of optoelectronic devices. Especially in the manufacture of high-quality semiconductor materials, such as phosphorus-doped silicon, the purity of phosphine is required to be extremely high.

[0003] The existing electronic grade phosphine synthesis and purification device uses a reactor, a condenser, a constant pressure buffer tank, a distillation tower and an adsorption column to perform corresponding synthesis and purification operations, and passes the phosphine that has completed the purification operation into a storage cylinder. However, when the device stirs the raw materials in the reactor, the stirring effect of the raw materials in the reactor is poor, thereby affecting the synthesis yield of phosphine.

[0004] For example, patent application 202010434780.6 discloses a method and device for synthesizing and refining electronic-grade phosphine, which optimizes the reaction temperature, reaction time, alkali solution concentration and other conditions during the reaction process to make the yield of phosphine in the reaction process 15-35%, and the salt solution produced by the side reaction can be further prepared into a salt product, and then the phosphine obtained by the reaction is refined by a low-temperature double-effect distillation process to obtain electronic-grade phosphine with a purity of ≥99.99999%, and the phosphine yield in the refining process is ≥95%. However, the yield of phosphine in the synthesis and refining method and device of electronic-grade phosphine is low during the reaction process, which is difficult to meet the needs of large-scale industrialization.

[0005] Therefore, it is an urgent problem to be solved in the industry to provide an electronic-grade phosphine synthesis and purification device and a synthesis and purification method that can effectively improve the synthesis yield of phosphine and can also purify the synthesized phosphine to meet the demand for industrial large-scale electronic-grade phosphine. Summary of the invention

[0006] In view of the deficiencies of the prior art, the present invention provides an electronic-grade phosphine synthesis and purification device and a purification method, which solve the problems raised in the above background technology. To achieve the above purpose, the present invention is implemented through the following technical scheme: an electronic-grade phosphine synthesis and purification device, including a reactor and a liquid nitrogen tank, the top of the reactor is equipped with an input pipeline, the side of the reactor is connected to a condenser through a pipeline, the side of the condenser is connected to a constant pressure buffer tank through a pipeline, the side of the constant pressure buffer tank is connected to a distillation tower through a pipeline, the side of the distillation tower is connected to an adsorption column through a pipeline, and the liquid nitrogen tank is equipped with a storage cylinder inside; The reactor is provided with a stirring assembly inside, which includes a power sleeve and a hydraulic chamber 1 driven by a servo motor, the side of the power sleeve is rotatably connected with a stirring plate, the top of the power sleeve is transmission-connected with a turntable, the outer side of the turntable is rotatably connected with an extrusion block by setting a torsion spring, the end of the hydraulic chamber 1 close to the extrusion block is slidably connected with a force rod 1 by setting a spring, the end of the hydraulic chamber 1 away from the force rod 1 is slidably connected with a half gear ring, the inner wall of the stirring plate is rotatably connected with a rotating rod 1 and a rotating rod 2 respectively, the outer side of the rotating rod 1 is fixedly connected with a gear and a bevel gear 1, the side of the rotating rod 2 is fixedly connected with a bevel gear 2, and the outer side of the rotating rod 2 is fixedly connected with a hybrid plate. The setting of the stirring assembly improves the synthesis and purification efficiency of the device.

[0007] Preferably, a total of six extrusion blocks are provided, and the six extrusion blocks are distributed in a circular array on the turntable.

[0008] Preferably, the stress-bearing rod 1 is located at a side position of the extrusion block and is in contact with the extrusion block.

[0009] Preferably, the bevel gear 2 is located on the side of the bevel gear 1 and is in meshing state with the bevel gear 1.

[0010] Preferably, a scraping assembly is provided inside the reactor, and the scraping assembly includes an electric telescopic rod driven by a linear motor and a fixed seat fixed on the inner wall of the power sleeve, the fixed seat is equipped with a hydraulic device inside, the top of the electric telescopic rod is equipped with a brush plate, the outer side of the second rotating rod is fixedly connected with a cam, the end of the hydraulic device close to the cam is slidably connected to the second force-bearing rod by setting a spring, the end of the hydraulic device away from the second force-bearing rod is slidably connected to the pressure plate, and the side of the brush plate is connected to the first force-bearing plate by setting an elastic telescopic rod. By setting the scraping assembly, the scraping effect of the brush plate on the material attached to the bottom side of the reactor is improved, thereby reducing the waste of raw materials.

[0011] Preferably, the second force-bearing rod is located at the top of the cam and is in contact with the cam.

[0012] Preferably, the force-bearing plate 1 is located on the side of the pressure plate and is in contact with the pressure plate.

[0013] Preferably, a partition assembly is provided between the reactor and the input pipeline, the partition assembly includes a second hydraulic chamber, one end of the second hydraulic chamber close to the first force rod is slidably connected to a connecting rod, and one end of the second hydraulic chamber away from the connecting rod is slidably connected to an arc rod, the interior of the input pipeline is rotatably connected to a through-shaft, the outer side of the shaft is fixedly connected to a second force plate, and the side of the shaft is fixedly connected to a blocking block. By setting the partition assembly, excessive supply of raw materials at one time is prevented, thereby improving the synthesis and purification efficiency of the device.

[0014] Preferably, the second force-bearing plate is located on the side of the arc-shaped rod and is fixed to the arc-shaped rod.

[0015] A method for synthesizing and purifying electronic-grade phosphine using the above-mentioned synthesis and purification device comprises the following steps: Step 1, adding raw materials containing yellow phosphorus and lime into a reactor through an input pipe under a water environment, and controlling the temperature to be 75 to 90° C., and then adding sodium hydroxide solution through an input pipe, the reaction pressure is 0 to 0.3 MPa, and the reaction time is 2 to 5 hours to obtain crude phosphine; Step 2, the crude phosphine is passed into a condenser, the temperature in the condenser is controlled to be -85 to -35°C, and the crude phosphine after freezing and impurity removal is sent to a constant pressure buffer tank to supply gas to the distillation tower and the adsorption column; Step 3: Pass the electronic grade phosphine after the adsorption operation into a storage cylinder placed in a liquid nitrogen tank.

[0016] The electronic-grade phosphine synthesis and purification device and synthesis and purification method provided by the present invention have the following beneficial effects: (1) Inject the raw materials into the reactor through the input pipeline, perform the corresponding synthesis operation, start the servo motor, drive the power sleeve to rotate clockwise, cooperate with the hydraulic chamber 1, the turntable, the torsion spring, the extrusion block, the force rod 1, the half gear ring, the rotating rod 1, the rotating rod 2, the gear, the bevel gear 1 and the bevel gear 2, so that the stirring plate rotates in the horizontal direction and the mixing plate rotates in the vertical direction, thereby improving the stirring effect of the device, thereby improving the synthesis efficiency of phosphine, and the yield of phosphine can reach 25-50%, which greatly improves the industrial synthesis efficiency.

[0017] (2) When the synthesis and purification device is performing the corresponding synthesis operation, the linear motor is activated, and in conjunction with the electric telescopic rod, the hydraulic device, the cam, the second force-bearing rod, the elastic telescopic rod, the first force-bearing plate and the fixed seat, an additional force can be applied to the brush plate in sequence through the pressure plate, thereby improving the scraping effect of the brush plate on the material attached to the bottom side of the reactor, thereby reducing the waste of raw materials, reducing production costs, and providing a guarantee for industrial large-scale production.

[0018] (3) When the force-bearing rod 1 moves, i.e., the material in the reactor is stirred at multiple angles, the input pipeline that was originally in an open state can be closed by cooperating with the hydraulic chamber 2, the rotating shaft, the connecting rod, the arc rod, the force-bearing plate 2 and the blocking block, thereby preventing too much raw material from being fed in at one time, thereby improving the synthesis efficiency of the device. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the technical solutions in the present invention or the prior art, a brief introduction is given below to the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0020] Figure 1 It is a schematic diagram of the overall appearance of the three-dimensional structure of the present invention; Figure 2 It is a schematic diagram of the overall cross-sectional three-dimensional structure of the present invention; Figure 3 It is a schematic diagram of the three-dimensional structure of the stirring assembly of the present invention; Figure 4 For the present invention Figure 3 The enlarged structural diagram at A in the middle; Figure 5 For the present invention Figure 3 The enlarged structural diagram at B in the middle; Figure 6 It is a schematic diagram of the three-dimensional structure of the scraping component of the present invention; Figure 7 For the present invention Figure 6 The enlarged structural diagram at C in the middle; Figure 8 It is a schematic diagram of the three-dimensional structure of the partition assembly of the present invention; Fig. 9 For the present invention Figure 8 Enlarged structural diagram at D in the middle.

[0021] In the figure: 100, reactor; 200, condenser; 300, constant pressure buffer tank; 400, distillation tower; 500, adsorption column; 600, liquid nitrogen tank; 700, storage cylinder; 1100, input pipeline; 800, stirring assembly; 801, power sleeve; 802, hydraulic chamber 1; 803, stirring plate; 804, turntable; 805, torsion spring; 806, extrusion block; 807, force rod 1; 808, half gear ring; 809, rotating rod 1; 810, rotating rod 2; 811, gear; 812, bevel gear 1; 813, bevel gear 2; 814, hybrid plate; 900, scraping assembly; 901, electric telescopic rod; 902, hydraulic device; 903, brush plate; 904, cam; 905, force-bearing rod 2; 906, pressure plate; 907, elastic telescopic rod; 908, force-bearing plate 1; 1000. Partition assembly; 1001. Hydraulic chamber 2; 1002. Rotating shaft; 1003. Connecting rod; 1004. Arc rod; 1005. Force plate 2; 1006. Block. DETAILED DESCRIPTION

[0023] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be clearly and completely described below in conjunction with the drawings of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] Embodiment 1 See also Figure 1-Figure 5 The electronic-grade phosphine synthesis and purification device provided by the present invention is as follows: Figure 1 As shown, it includes a reactor 100 and a liquid nitrogen tank 600, the top of the reactor 100 is equipped with an input pipeline 1100, the side of the reactor 100 is connected to the condenser 200 through a pipeline, the side of the condenser 200 is connected to the constant pressure buffer tank 300 through a pipeline, the side of the constant pressure buffer tank 300 is connected to the distillation tower 400 through a pipeline, the side of the distillation tower 400 is connected to the adsorption column 500 through a pipeline, the side of the adsorption column 500 is connected to the storage cylinder 700 through a pipeline, and the storage cylinder 700 is installed inside the liquid nitrogen tank 600.

[0025] like Figure 2~Figure 5 As shown, the interior of the reactor 100 is provided with a stirring assembly 800, which includes a power sleeve 801 and a hydraulic chamber 1 802 driven by a servo motor. The side of the power sleeve 801 is rotatably connected to a stirring plate 803, and the top of the power sleeve 801 is connected to a turntable 804. The outer side of the turntable 804 is rotatably connected to an extrusion block 806 by setting a torsion spring 805. There are six extrusion blocks 806 in total, and the six extrusion blocks 806 are distributed in a circular array on the turntable 804. The end of the hydraulic chamber 1 802 close to the extrusion block 806 is slidably connected to a force rod 1 807 by setting a spring. The force rod 1 807 is located at the side of the extrusion block 806 and contacts the extrusion block 806. The end of the hydraulic chamber 1 802 away from the force rod 1 807 is slidably connected to a half gear ring 808. When the raw materials are injected into the reactor 100 through the input pipeline 1100 and the corresponding synthesis operation is performed, the servo motor is started to Figure 3 and Figure 4 As shown in the figure, the power sleeve 801 driven by the servo motor rotates clockwise, and the power sleeve 801 can drive the turntable 804 connected to it to rotate clockwise, so that the power sleeve 801 drives the extrusion block 806 to rotate clockwise through the torsion spring 805, and the extrusion block 806 can squeeze the force-bearing rod 807. At this time, the side of the extrusion block 806 away from the force-bearing rod 807 is restricted by the turntable 804 and cannot rotate, so that the extrusion block 806 squeezes the force-bearing rod 807 and drives the force-bearing rod 807 to move with the compression spring, and the force-bearing rod 807 immediately moves into the hydraulic chamber 802, so that the pressure in the hydraulic chamber 802 increases, driving the half gear ring 808 slidingly connected to the hydraulic chamber 802 to move sideways.

[0026] The inner wall of the stirring plate 803 is rotatably connected to a rotating rod 1 809 and a rotating rod 2 810 respectively, the outer side of the rotating rod 1 809 is fixedly connected to a gear 811 and a bevel gear 1 812, the side of the rotating rod 2 810 is fixedly connected to a bevel gear 2 813, the bevel gear 2 813 is located on the side of the bevel gear 1 812 and is in a meshing state with the bevel gear 1 812, and the outer side of the rotating rod 2 810 is fixedly connected to a hybrid plate 814. The half gear ring 808 moves sideways, so that the half gear ring 808 begins to mesh with the gear 811; at the same time, when the power sleeve 801 rotating clockwise drives the stirring plate 803 connected to it to rotate, the stirring plate 803 drives the gear 811 located thereon to revolve, so that the gear 811 rotates under the restriction of the half gear ring 808, thereby driving the rotating rod 1 809 fixedly connected to the gear 811 to rotate, so that the rotating rod 1 809 drives the bevel gear 1 812 fixedly connected to it to rotate, and the bevel gear 1 812 drives the bevel gear 2 813 meshed with it to rotate, so that the bevel gear 2 813 drives the rotating rod 2 810 fixedly connected to it to rotate, and the rotating rod 2 810 drives the mixing plate 814 fixedly connected to it to rotate; at this time, the stirring plate 803 rotates in the horizontal direction, and the mixing plate 814 on the stirring plate 803 rotates in the vertical direction, which improves the stirring effect of the device, thereby improving the synthesis and purification efficiency of the device.

[0027] When the hybrid board 814 is not needed, the servo motor is started to Figure 3 and Figure 4As shown in , the power sleeve 801 driven by the servo motor rotates counterclockwise, and similarly, the extrusion block 806 rotates counterclockwise. Because the torsion force of the torsion spring 805 is less than the elastic force of the spring, when the extrusion block 806 rotates counterclockwise to the force rod 1 807 and squeezes the force rod 1 807, the extrusion block 806 rotates with the torsion spring 805 as the axis, thereby avoiding the force rod 1 807, so that the force rod 1 807 does not move. Similarly, the half gear ring 808 does not mesh with the gear 811 due to movement, thereby disabling the hybrid plate 814. The device can be used in different situations to reduce power loss.

[0028] When in use, raw materials containing yellow phosphorus and lime are added into the reactor 100 through the input pipe 1100 in a water environment, and the temperature is controlled to be 75 to 90° C. Then, sodium hydroxide solution is added through the input pipe 1100, and the reaction pressure is 0 to 0.3 MPa. The servo motor is started to Figure 3 and Figure 4 As shown in the figure, the power sleeve 801 driven by the servo motor is driven to rotate clockwise, and the power sleeve 801 can drive the turntable 804 connected thereto to rotate clockwise, so that the power sleeve 801 drives the extrusion block 806 to rotate clockwise through the torsion spring 805, and the extrusion block 806 can squeeze the force-bearing rod 807. At this time, the side of the extrusion block 806 away from the force-bearing rod 807 is restricted by the turntable 804 and cannot rotate, so that the extrusion block 806 squeezes the force-bearing rod 807 and drives the force-bearing rod 807 to move with the compression spring, and the force-bearing rod 807 immediately moves into the hydraulic chamber 802, so that the pressure in the hydraulic chamber 802 increases, driving the half gear ring 808 slidingly connected to the hydraulic chamber 802 to move sideways, so that the half gear ring 808 begins to mesh with the gear 811; at the same time, When the clockwise rotating power sleeve 801 drives the stirring plate 803 connected to it to rotate, the stirring plate 803 drives the gear 811 thereon to revolve, so that the gear 811 rotates on itself under the restriction of the half gear ring 808, thereby driving the rotating rod 1 809 fixedly connected to the gear 811 to rotate, so that the rotating rod 1 809 drives the bevel gear 1 812 fixedly connected to it to rotate, and the bevel gear 1 812 drives the bevel gear 2 813 meshing with it to rotate, so that the bevel gear 2 813 drives the rotating rod 2 810 fixedly connected to it to rotate, and the rotating rod 2 810 drives the mixing plate 814 fixedly connected to it to rotate; at this time, the stirring plate 803 rotates in the horizontal direction, and the mixing plate 814 on the stirring plate 803 rotates in the vertical direction to mix the raw materials, and the reaction time is 2 to 5 hours.

[0029] After the mixing is completed, crude phosphine is obtained, and the crude phosphine is passed into the condenser 200, the temperature in the condenser 200 is controlled to be -85 to -35°C, and the crude phosphine after freezing and impurity removal is sent to the constant pressure buffer tank 300, and gas is supplied to the distillation tower 400 and the adsorption column 500, and the electronic grade phosphine after the adsorption operation is completed is passed into the storage cylinder 700 placed in the liquid nitrogen tank 600.

[0030] When the hybrid board 814 is not needed, the servo motor is started to Figure 3 and Figure 4 As shown in the figure, the power sleeve 801 driven by the servo motor is driven to rotate counterclockwise, and similarly, the extrusion block 806 is rotated counterclockwise. Because the torsion force of the torsion spring 805 is less than the elastic force of the spring, when the extrusion block 806 rotates counterclockwise to the force-bearing rod 1 807 and squeezes the force-bearing rod 1 807, the extrusion block 806 rotates with the torsion spring 805 as the axis, thereby avoiding the force-bearing rod 1 807, so that the force-bearing rod 1 807 does not move. Similarly, the half gear ring 808 does not engage with the gear 811 due to movement, thereby disabling the hybrid plate 814.

[0031] Embodiment 2 See also Figure 1-Figure 7 On the basis of the first embodiment, a scraping assembly 900 is provided inside the reactor 100, and the scraping assembly 900 includes an electric telescopic rod 901 driven by a linear motor and a fixing seat fixed on the inner wall of the power sleeve 801, a hydraulic device 902 is installed inside the fixing seat, and a brush plate 903 is installed on the top of the electric telescopic rod 901. When performing the corresponding synthetic operation, the linear motor is enabled to drive the electric telescopic rod 901 driven by the linear motor to reciprocate a certain distance in the vertical direction, so that the electric telescopic rod 901 drives the brush plate 903 installed thereon to reciprocate a certain distance, and the material attached to the bottom side of the reactor 100 is scraped off.

[0032] The outer side of the rotating rod 810 is fixedly connected with a cam 904, and one end of the hydraulic device 902 close to the cam 904 is slidably connected with a force rod 905 through a spring. The force rod 905 is located at the top of the cam 904 and contacts the cam 904. The end of the hydraulic device 902 away from the force rod 905 is slidably connected with a pressure plate 906. When the brush plate 903 scrapes the material and when the rotating rod 810 rotates, the cam 904 fixedly connected to the rotating rod 810 can be driven to rotate. When the protruding part of the cam 904 squeezes the force rod 905, the force rod 905 can be driven to move upward, and the hydraulic device 902 slidably connected to the force rod 905 increases the pressure in the hydraulic device 902, and drives the pressure plate 906 slidably connected to the hydraulic device 902 to move.

[0033] The side of the brush plate 903 is connected to the force plate 1 908 by setting an elastic telescopic rod 907. The force plate 1 908 is located on the side of the pressure plate 906 and is in contact with the pressure plate 906. When the pressure plate 906 moves, the force plate 1 908 can be squeezed, and the force plate 1 908 then applies an additional force to the brush plate 903 through multiple elastic telescopic rods 907; when the protruding part of the cam 904 moves away from the force rod 2 905 as it rotates, the force rod 2 905 can be reset under the action of the spring connected to it, and the pressure plate 906 is reset in the same way. In this way, an additional force can be applied to the brush plate 903 in turn through the pressure plate 906. The scraping effect of the brush plate 903 on the material attached to the bottom side of the reactor 100 is improved, thereby reducing the waste of raw materials.

[0034] When in use, on the basis of the first embodiment, when performing the corresponding synthesis operation, the linear motor is activated to drive the electric telescopic rod 901 driven by the linear motor to reciprocate a certain distance in the vertical direction, so that the electric telescopic rod 901 drives the brush plate 903 mounted thereon to reciprocate a certain distance, and the material attached to the bottom side of the reactor 100 is scraped off, and when the rotating rod 810 rotates, the cam 904 fixedly connected to the rotating rod 810 can be driven to rotate, and when the protruding part of the cam 904 squeezes the force-bearing rod 905, the force-bearing rod 905 can be driven to move upward , cooperates with the hydraulic device 902 that is slidably connected to the force-bearing rod 2 905, so that the pressure in the hydraulic device 902 increases, driving the pressure plate 906 that is slidably connected to the hydraulic device 902 to move, so that the pressure plate 906 squeezes the force-bearing plate 1 908, and the force-bearing plate 1 908 then applies an additional force to the brush plate 903 through a plurality of elastic telescopic rods 907; when the protruding part of the cam 904 moves away from the force-bearing rod 2 905 as it rotates, the force-bearing rod 2 905 can be reset under the action of the spring connected thereto, and similarly, the pressure plate 906 is reset, so that an additional force can be applied to the brush plate 903 in turn through the pressure plate 906.

[0035] Embodiment 3 See also Figure 1-Figure 9On the basis of the first and second embodiments, a partition assembly 1000 is provided between the reactor 100 and the input pipeline 1100, and the partition assembly 1000 includes a hydraulic chamber 2 1001, and the end of the hydraulic chamber 2 1001 close to the stress rod 1 807 is slidably connected to the connecting rod 1003, and the end of the hydraulic chamber 2 1001 away from the connecting rod 1003 is slidably connected to the arc rod 1004. When the stress rod 1 807 moves, that is, when the material in the reactor 100 is stirred at multiple angles, the stress rod 1 807 can drive the connecting rod 1003 fixedly connected thereto to move, and cooperate with the hydraulic chamber 2 1001 slidably connected to the connecting rod 1003, so that the pressure in the hydraulic chamber 2 1001 is reduced, and the arc rod 1004 slidably connected to the hydraulic chamber 2 1001 is driven to move a certain distance, and the arc rod 1004 is then retracted into the hydraulic chamber 2 1001.

[0036] The input pipeline 1100 is rotatably connected to a rotating shaft 1002 that penetrates through it. A second force plate 1005 is fixedly connected to the outside of the rotating shaft 1002. The second force plate 1005 is located at the side of the arc rod 1004 and is fixed to the arc rod 1004. A blocking block 1006 is fixedly connected to the side of the rotating shaft 1002. When the arc rod 1004 is retracted into the second hydraulic chamber 1001, the second force plate 1005 fixedly connected to the arc rod 1004 can be driven to rotate at a certain angle, so that the second force plate 1005 drives the rotating shaft 1002 fixedly connected thereto to rotate, and the rotating shaft 1002 drives the blocking block 1006 fixedly connected thereto to rotate at a certain angle, thereby closing the input pipeline 1100 that was originally in an open state. This prevents excessive supply of raw materials at one time, thereby improving the efficiency of synthesis and purification of the device.

[0037] When the force bearing rod 807 is reset, the partition assembly 1000 is reset accordingly, and the input pipe 1100 is restored to the open state, so as to facilitate the next activation of the device.

[0038] During use, on the basis of Embodiment 1 and Embodiment 2, when the force-bearing rod 1 807 moves, that is, when the material in the reactor 100 is stirred at multiple angles, the force-bearing rod 1 807 can drive the connecting rod 1003 fixedly connected thereto to move, and cooperate with the hydraulic bin 2 1001 slidably connected to the connecting rod 1003, so that the pressure in the hydraulic bin 2 1001 is reduced, and the arc rod 1004 slidably connected to the hydraulic bin 2 1001 is driven to move a certain distance, and the arc rod 1004 is then retracted into the hydraulic bin. Inside the second 1001, the force-bearing plate 1005 fixedly connected to the arc rod 1004 is driven to rotate at a certain angle, so that the force-bearing plate 1005 drives the rotating shaft 1002 fixedly connected thereto to rotate, and the rotating shaft 1002 drives the blocking block 1006 fixedly connected thereto to rotate at a certain angle, thereby closing the input pipe 1100 that was originally in an open state; when the force-bearing rod 1 807 is reset, the partition assembly 1000 is reset accordingly, and the input pipe 1100 is restored to an open state.

[0039] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A synthesis and purification device, comprising a reactor (100) and a liquid nitrogen tank (600), wherein the top of the reactor (100) is equipped with an input pipeline (1100), the side of the reactor (100) is connected to a condenser (200) via a pipeline, the side of the condenser (200) is connected to a constant pressure buffer tank (300) via a pipeline, the side of the constant pressure buffer tank (300) is connected to a distillation tower (400) via a pipeline, the side of the distillation tower (400) is connected to an adsorption column (500) via a pipeline, and the liquid nitrogen tank (600) is equipped with a storage cylinder (700) inside; Features: The reactor (100) is provided with a stirring assembly (800) inside. The stirring assembly (800) comprises a power sleeve (801) driven by a servo motor and a hydraulic chamber (802). The side of the power sleeve (801) is rotatably connected to a stirring plate (803). The top of the power sleeve (801) is rotatably connected to a rotating disk (804). The outer side of the rotating disk (804) is rotatably connected to an extrusion block (806) via a torsion spring (805). The end of the hydraulic chamber (802) close to the extrusion block (806) is rotatably connected to the rotating disk (804). The spring is slidably connected to a force-bearing rod 1 (807); an end of the hydraulic chamber 1 (802) away from the force-bearing rod 1 (807) is slidably connected to a half gear ring (808); the inner wall of the stirring plate (803) is rotatably connected to a rotating rod 1 (809) and a rotating rod 2 (810); the outer side of the rotating rod 1 (809) is fixedly connected to a gear (811) and a bevel gear 1 (812); the side of the rotating rod 2 (810) is fixedly connected to a bevel gear 2 (813); and the outer side of the rotating rod 2 (810) is fixedly connected to a hybrid plate (814).

2. The synthesis and purification device according to claim 1, characterized in that: A total of six extrusion blocks (806) are provided, and the six extrusion blocks (806) are distributed in a circular array on the turntable (804).

3. The synthesis and purification device according to claim 1, characterized in that: The force bearing rod 1 (807) is located on the side of the extrusion block (806) and is in contact with the extrusion block (806).

4. The synthesis and purification device according to claim 1, characterized in that: The bevel gear 2 (813) is located on the side of the bevel gear 1 (812) and is in meshing state with the bevel gear 1 (812).

5. The synthesis and purification device according to claim 1, characterized in that: A scraping assembly (900) is arranged inside the reactor (100), and the scraping assembly (900) comprises an electric telescopic rod (901) driven by a linear motor and a fixing seat fixed on the inner wall of a power sleeve (801), the fixing seat is equipped with a hydraulic device (902) inside, the top of the electric telescopic rod (901) is equipped with a brush plate (903), the outer side of the second rotating rod (810) is fixedly connected to a cam (904), the end of the hydraulic device (902) close to the cam (904) is slidably connected to the second force-bearing rod (905) by means of a spring, the end of the hydraulic device (902) away from the second force-bearing rod (905) is slidably connected to a pressure plate (906), and the side of the brush plate (903) is connected to the first force-bearing plate (908) by means of an elastic telescopic rod (907).

6. The synthesis and purification device according to claim 5, characterized in that: The second force bearing rod (905) is located at the top of the cam (904) and is in contact with the cam (904).

7. The synthesis and purification device according to claim 5, characterized in that: The force-bearing plate 1 (908) is located on the side of the pressure plate (906) and is in contact with the pressure plate (906).

8. The synthesis and purification device according to claim 1, characterized in that: A partition assembly (1000) is provided between the reactor (100) and the input pipeline (1100), and the partition assembly (1000) comprises a second hydraulic chamber (1001), an end of the second hydraulic chamber (1001) close to the first force-bearing rod (807) is slidably connected to a connecting rod (1003), an end of the second hydraulic chamber (1001) away from the connecting rod (1003) is slidably connected to an arc-shaped rod (1004), the interior of the input pipeline (1100) is rotatably connected to a penetrating rotating shaft (1002), the outer side of the rotating shaft (1002) is fixedly connected to a second force-bearing plate (1005), and a side of the rotating shaft (1002) is fixedly connected to a blocking block (1006).

9. The synthesis and purification device according to claim 8, characterized in that: The second force-bearing plate (1005) is located on the side of the arc-shaped rod (1004) and is in a fixed state with the arc-shaped rod (1004).

10. A method for synthesizing and purifying electronic grade phosphine, using the synthesis and purification device as described in any one of claims 1 to 9, characterized in that: The following steps are involved: Step 1: Add raw materials containing yellow phosphorus and lime into a reaction kettle (100) through an input pipe (1100) in a water environment, and control the temperature to be 75 degrees Celsius to 90 degrees Celsius, and then add a sodium hydroxide solution through the input pipe (1100), the reaction pressure is 0 to 0.3 MPa, and the reaction time is 2 to 5 hours to obtain crude phosphine; Step 2: The crude phosphine is introduced into the condenser (200), the temperature in the condenser (200) is controlled to be between -85 degrees Celsius and -35 degrees Celsius, and the crude phosphine after freezing and impurity removal is sent into the constant pressure buffer tank (300) to supply gas to the distillation tower (400) and the adsorption column (500); Step 3: Pass the electronic grade phosphine after the adsorption operation is completed into a storage cylinder (700) placed in a liquid nitrogen tank (600).

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