A sampling detection device based on trimethylaluminum and its use method

Abstract

The present invention discloses a sampling detection device based on the preparation of trimethylaluminum and a method for using the same, comprising a distillation kettle, a front fraction receiving tank and a plurality of main fraction receiving tanks, wherein the distillation kettle is connected to the front fraction receiving tank through a discharge pipe, the discharge pipe is connected to the plurality of main fraction receiving tanks through a first connecting mechanism, a detection tank is fixedly connected between the plurality of main fraction receiving tanks, and a sampling assembly is arranged on the detection tank. The first connecting mechanism is driven to rotate by a driving mechanism to realize the connection between the discharge pipe and different main fraction receiving tanks, and the second connecting mechanism is driven to rotate synchronously with a connecting piece at the same time of the connection, so that the main fraction receiving tank that has just completed liquid storage is connected to the sampling assembly, and then the sampling assembly is driven to work and extract part of the liquid from the main fraction receiving tank into the detection tank for timely detection through the reverse rotation of the driving mechanism, thereby improving the detection efficiency and safety during the preparation of trimethylaluminum.

Description

Technical Field

[0001] The invention relates to the technical field of trimethylaluminum preparation, and in particular to a sampling detection device based on trimethylaluminum preparation and a use method thereof. Background Art

[0002] Trimethylaluminum is an organic compound, a colorless transparent liquid. It is mainly used as an olefin polymerization catalyst and ignition fuel. It is also used to prepare straight-chain primary alcohols and olefins. It can also be used for the vapor deposition of metal organic compounds. After the production of trimethylaluminum, it needs to be further purified in a distillation kettle. After the distillation, the product needs to be sampled and tested.

[0003] For example, the Chinese invention patent with application number: 202211054302.8, entitled "Method for detecting the content of triethylmethylsilane in trimethylaluminum", discloses a method for detecting the content of triethylmethylsilane in trimethylaluminum, comprising the following steps: S1, mixing a trimethylaluminum sample with an organic solvent to obtain a sample solution; S2, subjecting the sample solution to a hydrolysis reaction to remove the trimethylaluminum in the sample solution, and using an organic solvent to recover the tail gas generated by the hydrolysis reaction to obtain a tail gas absorption liquid; S3, separating the hydrolyzate after the hydrolysis reaction to obtain an organic phase solution; S4, mixing the organic phase solution with the tail gas absorption liquid, and removing the organic solvent to obtain a concentrated solution; and S5, using GC-MS to detect the content of triethylmethylsilane in the concentrated solution, that is, obtaining the content of triethylmethylsilane in the trimethylaluminum sample. The method for detecting the content of triethylmethylsilane in trimethylaluminum according to the embodiment of the present invention has the advantages of a safe and stable detection process and accurate detection results.

[0004] The shortcomings of the prior art are that the existing equipment for preparing trimethylaluminum does not have a sampling and detection device, and the injected trimethylaluminum needs to be manually extracted and transferred to the detection device for detection. Since trimethylaluminum has certain dangers, extreme caution is required during the sampling process to avoid the possibility of trimethylaluminum leakage, and manual sampling is inefficient and has certain shortcomings. Summary of the invention

[0005] The purpose of the present invention is to provide a sampling detection device prepared based on trimethylaluminum and a method of using the same to solve the above-mentioned deficiencies in the prior art.

[0006] In order to achieve the above-mentioned purpose, the present invention provides the following technical solutions: a sampling and detection device based on trimethylaluminum preparation, comprising a distillation kettle, a front fraction receiving tank and a plurality of main fraction receiving tanks, the distillation kettle is connected with the front fraction receiving tank through a discharge pipe, the discharge pipe is connected with the plurality of main fraction receiving tanks through a first connecting mechanism, a detection tank is fixedly connected between the plurality of main fraction receiving tanks, a sampling assembly is arranged on the detection tank, and the plurality of main fraction receiving tanks are connected with the sampling assembly through a second connecting mechanism; further comprising a driving mechanism, which is arranged on the discharge pipe; when the driving mechanism is working, it has the following two stations: in the first station, when the driving mechanism rotates, the discharge pipe is driven to connect with one of the main fraction receiving tanks through the first connecting mechanism for filling and storage, and when the first connecting mechanism is working, the second connecting mechanism is driven to rotate through the connecting piece so that the sampling assembly is connected with another one of the main fraction receiving tanks; in the second station, when the driving mechanism rotates in the opposite direction, the sampling assembly is driven to work through the trigger mechanism, and the trimethylaluminum filled into the main fraction receiving tank is transported to the detection tank for detection.

[0007] As a further description of the above technical solution:

[0008] The first connecting mechanism includes a liquid outlet pipe connected to each main fraction receiving tank; each of the liquid outlet pipes is fixedly connected to the same first partial arcuate ring, the first partial arcuate ring is provided with a plurality of first through grooves, each of the first through grooves is connected to the corresponding liquid outlet pipe, the first partial arcuate ring is rotatably connected to the second partial arcuate ring, the second partial arcuate ring is provided with a second through groove, the second partial arcuate ring is provided with a connecting pipe, the second through groove is connected to the connecting pipe, one end of the discharge pipe is connected to a hollow cylinder, and the connecting pipe is rotatably connected to the hollow cylinder through a connecting head.

[0009] As a further description of the above technical solution:

[0010] The second connecting mechanism includes an infusion tube connected to each main fraction receiving tank; each of the infusion tubes is fixedly connected to the same third partial arcuate ring, the third partial arcuate ring is provided with a plurality of third through grooves, each of the third through grooves is connected to the corresponding infusion tube, the third partial arcuate ring is rotatably connected to a fourth partial arcuate ring, the fourth partial arcuate ring is provided with a fourth through groove, a sampling tube is provided on the fourth partial arcuate ring, and the fourth through groove is connected to the sampling tube.

[0011] As a further description of the above technical solution:

[0012] The connecting member is an L-shaped plate fixedly connected between the second arc-shaped circular ring and the fourth arc-shaped circular ring.

[0013] As a further description of the above technical solution:

[0014] The sampling assembly includes a piston cylinder fixedly connected to the fourth arc-shaped ring, the piston cylinder is connected to the sampling tube; the bottom of the piston cylinder is connected to a supply pipe, the supply pipe is connected to the detection tank, and a piston unit is arranged on the piston cylinder.

[0015] As a further description of the above technical solution:

[0016] The piston unit includes a piston plate slidably connected in the piston cylinder, a piston rod fixedly connected to the piston plate, and a baffle fixedly connected to the piston rod; a rotating rod is rotatably connected to the L-shaped plate, a gear plate and a cam are fixedly connected to the rotating rod, a track groove is opened on the cam, a limiting rod is fixedly connected to the baffle, and the limiting rod is slidably connected in the track groove.

[0017] As a further description of the above technical solution:

[0018] The driving mechanism includes a reversible motor fixedly connected to the hollow cylinder, a main rotating rod fixedly connected to the output end of the reversible motor, a helical gear ring and a first bevel gear fixedly connected to the main rotating rod; a fixed ring is fixedly connected to the second partial arc-shaped circular ring, a plurality of first single-sided inclined blocks are slidably connected in the fixed ring, an abutment spring is arranged between each of the first single-sided inclined blocks and the fixed ring, the elastic force of the abutment spring drives the first single-sided inclined block to contact the helical gear ring, and the main rotating rod drives the gear plate to engage through a passive component.

[0019] As a further description of the above technical solution:

[0020] The passive component includes an auxiliary rod rotatably connected to the L-shaped plate, the auxiliary rod is fixedly connected to a second bevel gear, the second bevel gear is meshed with the first bevel gear; the auxiliary rod is provided with a gear ring, a plurality of second single-sided bevel blocks are slidably connected in the gear ring, a support spring is provided between each of the second single-sided bevel blocks and the gear ring, a plurality of bevel grooves are opened on the surface of the auxiliary rod, and the elastic force of the support spring drives the second single-sided bevel blocks to engage with the bevel grooves.

[0021] As a further description of the above technical solution:

[0022] The bottom end of the detection tank is also connected to a steam-water separator, and the detection tank is also connected to a gas pipe; the steam-water separator is connected to the front fraction receiving tank through a collecting pipe, and a reflux pipe is provided at the discharge port at the bottom of each main fraction receiving tank, and each reflux pipe is connected to the collecting pipe, and the front fraction receiving tank is connected to the feed port of the distillation kettle through a return pipe.

[0023] A method for using a sampling detection device prepared based on trimethylaluminum, the method for using the sampling detection device prepared based on trimethylaluminum comprising the following steps:

[0024] S1: The crude trimethylaluminum is transferred from the crude product transfer tank to the distillation kettle by nitrogen, and heated and distilled under normal pressure. The trimethylaluminum before the tower top temperature reaches the standard value enters the front fraction receiving tank through the discharge pipe. When the tower top temperature reaches the standard value, the trimethylaluminum enters the main fraction receiving tank through the discharge pipe and the first connecting mechanism;

[0025] S2: When the main fraction receiving tank is filled with an appropriate amount, the driving mechanism is started to rotate, driving the first connecting mechanism to rotate to guide the trimethylaluminum in the discharge pipe to another one for continued collection, and the second connecting mechanism is driven to rotate synchronously through the connecting piece to connect the sampling assembly with the main fraction receiving tank just filled with trimethylaluminum;

[0026] S3: After the adjustment is completed, the driving mechanism is driven to rotate in the opposite direction, the sampling assembly is driven to work through the trigger mechanism, and a certain amount of trimethylaluminum is collected and put into the detection tank for detection.

[0027] In the above technical scheme, the present invention provides a sampling detection device based on trimethylaluminum and a method for using the same, which has the following beneficial effects:

[0028] The present invention sets a distillation kettle, a front fraction receiving tank, a main fraction receiving tank, a discharge pipe, a first connecting mechanism, a detection tank, a sampling component, a second connecting mechanism, a driving mechanism, a connecting piece and a trigger mechanism to cooperate with each other. The driving mechanism rotates to drive the first connecting mechanism to rotate, so that the discharge pipe is connected with different main fraction receiving tanks. At the same time, the connecting piece drives the second connecting mechanism to rotate synchronously, so that the main fraction receiving tank that has just completed liquid storage is connected with the sampling component. Then, through the reverse rotation of the driving mechanism, the sampling component is driven to work and extract part of the liquid in the main fraction receiving tank into the detection tank for timely detection. The various structures in the device cooperate with each other, and when different main fraction receiving tanks are replaced, the extracted part of the liquid in the main fraction receiving tank that has just been filled can be automatically transported to the detection tank for detection. All operations are performed in a sealed manner, thereby improving the detection efficiency and safety during the preparation of trimethylaluminum.

[0029] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.

[0030] This application document provides an overview of various implementations or examples of the technology described in the present disclosure, and is not a comprehensive disclosure of the entire scope or all features of the disclosed technology. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can also be obtained based on these drawings.

[0032] Figure 1 A schematic diagram of the overall structure provided by an embodiment of the present invention;

[0033] Figure 2 A schematic diagram of a partial structure of a first connecting mechanism provided in an embodiment of the present invention;

[0034] Figure 3 A schematic diagram of the connection between the sampling component and the local drive mechanism structure provided by an embodiment of the present invention;

[0035] Figure 4 A schematic diagram of another part of the structure of the first connecting mechanism provided in an embodiment of the present invention;

[0036] Figure 5 A longitudinal sectional schematic diagram of the connection between the sample component and the local drive mechanism structure provided by an embodiment of the present invention;

[0037] Figure 6 A cross-sectional view of a gear ring structure provided by an embodiment of the present invention;

[0038] Figure 7 A longitudinal sectional schematic diagram of the connection between the discharge pipe and the connecting pipe structure provided in an embodiment of the present invention;

[0039] Figure 8 A cross-sectional bottom view of a helical gear ring structure provided by an embodiment of the present invention;

[0040] Fig. 9 for Figure 3 The enlarged view of point A in the middle;

[0041] Fig.10 for Figure 4 The enlarged view of point B in the middle;

[0042] Fig.11 for Figure 5 Enlarged view of point C in the middle.

[0043] Description of reference numerals:

[0044] 1. Rectification kettle; 11. Fore fraction receiving tank; 12. Main fraction receiving tank; 13. Discharge pipe; 14. Detection tank; 21. Liquid discharge pipe; 22. First part arc-shaped ring; 23. First through groove; 24. Second part arc-shaped ring; 25. Second through groove; 26. Connecting pipe; 27. Hollow cylinder; 28. Connector; 31. Liquid infusion tube; 32. Third part arc-shaped ring; 33. Third through groove; 34. Fourth part arc-shaped ring; 35. Fourth through groove; 36. Sampling tube; 4. L-shaped plate; 51. Piston cylinder; 52. Supply pipe; 61. Piston plate ; 62. piston rod; 63. baffle; 64. rotating rod; 65. gear plate; 66. cam; 67. track groove; 68. limit rod; 71. reversible motor; 72. main rotating rod; 73. helical gear ring; 74. first bevel gear; 75. fixing ring; 76. first single-sided bevel block; 77. abutment spring; 81. auxiliary rod; 82. second bevel gear; 83. gear ring; 84. second single-sided bevel block; 85. support spring; 86. bevel groove; 91. steam-water separator; 92. gas pipe; 93. collecting pipe; 94. reflux pipe; 95. return pipe. DETAILED DESCRIPTION

[0045] In order to make the purpose, technical solution and advantages of the embodiments of the present disclosure clearer, the technical solution of the embodiments of the present disclosure will be clearly and completely described below in conjunction with the drawings of the embodiments of the present disclosure. Obviously, the described embodiments are part of the embodiments of the present disclosure, not all of the embodiments. Based on the described embodiments of the present disclosure, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present disclosure.

[0046] See also Figure 1-11The present embodiment provides a sampling detection device based on trimethylaluminum preparation, comprising a distillation kettle 1, a front fraction receiving tank 11 and a plurality of main fraction receiving tanks 12, the distillation kettle 1 is connected to the front fraction receiving tank 11 through a discharge pipe 13, the discharge pipe 13 is connected to the plurality of main fraction receiving tanks 12 through a first connecting mechanism, the distillation kettle 1, the front fraction receiving tank 11, the main fraction receiving tank 12 and the discharge pipe 13 are all existing equipment, and the connection between the structures is also an existing conventional means, which will not be described in detail here, and the plurality of main fraction receiving tanks 12 are fixedly connected There is a detection tank 14, in which an ICP-MS and a solid particle detector are arranged. The ICP-MS can detect metal impurities in purified trimethylaluminum, and the solid particle detector is used to detect the content of solid particles in purified trimethylaluminum. Both instruments are existing equipment and can be connected by a pipeline. A sampling component is arranged on the detection tank 14, and a plurality of main fraction receiving tanks 12 are connected to the sampling component through a second connecting mechanism; a driving mechanism is also included, which is arranged on the discharge pipe 13; when the driving mechanism is working, it has the following two stations: a first station, When the driving mechanism rotates, the first connecting mechanism drives the discharge pipe 13 to connect with one of the main fraction receiving tanks 12 for filling and storage. When the first connecting mechanism works, the second connecting mechanism is driven to rotate through the connecting piece, so that the sampling assembly is connected with another main fraction receiving tank 12. The first connecting mechanism is driven to rotate by the rotation of the driving mechanism to realize the connection between the discharge pipe 13 and different main fraction receiving tanks 12. At the same time, the second connecting mechanism is driven to rotate synchronously with the connecting piece to connect the main fraction receiving tank 12 that has just completed liquid storage with the sampling assembly. At the second station, when the driving mechanism rotates in the reverse direction, the sampling component is driven to work through the trigger mechanism, and the trimethylaluminum poured into the main fraction receiving tank 12 is transported to the detection tank 14 for detection. Through the reverse rotation of the driving mechanism, the sampling component is driven to work to extract part of the liquid in the main fraction receiving tank 12 into the detection tank 14 for timely detection. The various structures in the device cooperate with each other, and when different main fraction receiving tanks 12 are replaced, the extracted part of the liquid in the main fraction receiving tank 12 that has just been filled can be automatically transported to the detection tank 14 for detection, and the operation efficiency is high.

[0047] Further, the first connecting mechanism includes a liquid outlet pipe 21 connected to each main fraction receiving tank 12; each liquid outlet pipe 21 is fixedly connected to the same first arcuate circular ring 22, and a plurality of first through grooves 23 are provided on the first arcuate circular ring 22, and each first through groove 23 is connected to the corresponding liquid outlet pipe 21; the first arcuate circular ring 22 is rotatably connected to the second arcuate circular ring 24, and a second through groove 25 is provided on the second arcuate circular ring 24; a connecting pipe 26 is provided on the second arcuate circular ring 24, and the second through groove 25 is connected to the connecting pipe 26; one end of the discharge pipe 13 is connected to a hollow cylinder 27, and the connecting pipe 26 is rotatably connected to the hollow cylinder 27 through a connector 28; the first arcuate circular ring 22 and the second arcuate circular ring 24 are of the same size, shape, material, etc., and the first arcuate circular ring 22 and the second arcuate circular ring 24 can be assembled into a complete circular ring, and the specific connection shape can be referred to in the appendix of the specification. Figure 1 , wherein it is necessary to ensure the sealing performance when the first part arc-shaped circular ring 22 and the second first part arc-shaped circular ring 22 are spliced ​​and rotated.

[0048] Furthermore, the second connecting mechanism includes a liquid infusion tube 31 connected to each main fraction receiving tank 12; each liquid infusion tube 31 is fixedly connected to the same third arcuate ring 32, and the third arcuate ring 32 is provided with a plurality of third through grooves 33, and each third through groove 33 is connected to the corresponding liquid infusion tube 31; the third arcuate ring 32 is rotatably connected to a fourth arcuate ring 34, and the fourth arcuate ring 34 is provided with a fourth through groove 35, and the fourth arcuate ring 34 is provided with a There is a sampling tube 36, and the fourth through groove 35 is connected to the sampling tube 36. The third arcuate ring 32 and the fourth arcuate ring 34 are of the same size, shape, material, etc. The third arcuate ring 32 and the fourth arcuate ring 34 can be assembled into a complete circular ring, and the specific connection shape is the same as the shape of the first arcuate ring 22 and the second arcuate ring 24. It is necessary to ensure the sealing of the third arcuate ring 32 and the fourth arcuate ring 34 when they are spliced ​​and rotated.

[0049] In an embodiment further provided by the present invention, the connecting member is an L-shaped plate 4 fixedly connected between the second arc ring 24 and the fourth arc ring 34. The L-shaped plate 4 is configured to drive the fourth arc ring 34 to move synchronously while the second arc ring 24 rotates.

[0050] In an embodiment further provided by the present invention, the sampling assembly includes a piston cylinder 51 fixedly connected to the fourth part arc-shaped ring 34, and the piston cylinder 51 is connected to the sampling tube 36; the bottom of the piston cylinder 51 is connected to a supply pipe 52, and the supply pipe 52 is connected to the detection tank 14. A piston unit is arranged on the piston cylinder 51, and the piston cylinder 51 is arranged to facilitate the sampling of the liquid in the main fraction receiving tank 12 into the detection tank 14 for detection.

[0051] Specifically, the piston unit includes a piston plate 61 slidably connected in the piston cylinder 51, a piston rod 62 is fixedly connected to the piston plate 61, and a baffle 63 is fixedly connected to the piston rod 62; a rotating rod 64 is rotatably connected to the L-shaped plate 4, a gear plate 65 and a cam 66 are fixedly connected to the rotating rod 64, a track groove 67 is provided on the cam 66, a limiting rod 68 is fixedly connected to the baffle 63, and the limiting rod 68 is slidably connected in the track groove 67, and the shape of the track groove 67 is consistent with the shape of the cam 66, so that after the cam 66 rotates, the limiting rod 68 cooperates with the track groove 67 to drive the baffle 63 to move up and down, and drive the piston plate 61 in the piston cylinder 51 to move to realize the liquid pumping operation.

[0052] In the embodiment provided by the present invention, the driving mechanism includes a reversible motor 71 fixedly connected to the hollow cylinder 27, the reversible motor 71 is connected to an external power supply and a control switch, a main rotating rod 72 is fixedly connected to the output end of the reversible motor 71, a helical gear ring 73 and a first bevel gear 74 are fixedly connected to the main rotating rod 72; a fixing ring 75 is fixedly connected to the second part arc-shaped circular ring 24, a plurality of first single-sided inclined blocks 76 are slidably connected in the fixing ring 75, abutment springs 77 are arranged between each first single-sided inclined block 76 and the fixing ring 75, the elastic force of the abutment springs 77 drives the first single-sided inclined block 76 to contact the helical gear ring 73, the main rotating rod 72 drives the gear plate 65 to engage through the passive component, a groove for the first single-sided inclined block 76 to slide is arranged in the fixing ring 75, and the first One side of the single-sided inclined block 76 is set to be inclined, and the other side is set to be flat. One side of the teeth on the helical gear ring 73 is set to be inclined, and the other side is set to be flat. When the rotating rod 64 drives the helical gear ring 73 to rotate, the inclined side of the helical teeth of the helical gear ring 73 contacts the inclined surface of the first single-sided inclined block 76. At this time, the rotation of the helical gear ring 73 cannot drive the second part of the arc ring 24 through the fixed ring 75. On the contrary, when the main rotating rod 72 rotates in another direction, when the flat side of the teeth of the helical gear ring 73 contacts the flat side of the first single-sided inclined block 76, the helical gear ring 73 is abutted by the first single-sided inclined block 76, so that the fixed ring 75 can be driven to rotate synchronously through the first single-sided inclined block 76, and the rotation of the fixed ring 75 drives the second part of the arc ring 24 to rotate synchronously to achieve switching.

[0053] Specifically, the passive component includes an auxiliary rod 81 rotatably connected to the L-shaped plate 4, and a second bevel gear 82 is fixedly connected to the auxiliary rod 81, and the second bevel gear 82 is meshed with the first bevel gear 74; a gear ring 83 is provided on the auxiliary rod 81, and a plurality of second single-sided inclined blocks 84 are slidably connected in the gear ring 83, and a support spring 85 is provided between each second single-sided inclined block 84 and the gear ring 83, and a plurality of inclined grooves 86 are provided on the surface of the auxiliary rod 81, and the elastic force of the support spring 85 drives the second single-sided inclined block 84 to engage with the inclined groove 86, and a groove for the second single-sided inclined block 84 to slide is provided in the gear ring 83, and the first single-sided inclined block 76 One side of the auxiliary rod 81 is arranged in a bevel shape, and the other side thereof is arranged in a plane shape. One side of the bevel groove 86 is arranged in a bevel shape, and the other side thereof is arranged in a plane shape. When the auxiliary rod 81 rotates, the bevel side of the bevel groove 86 arranged inside it contacts the bevel side of the second single-sided bevel block 84. At this time, the rotation of the auxiliary rod 81 cannot drive the gear plate 65 to rotate through the second single-sided bevel block 84. On the contrary, when the auxiliary rod 81 rotates in another direction, when the plane side of the bevel groove 86 contacts the plane side of the second single-sided bevel block 84, the gear ring 83 is abutted by the second single-sided bevel block 84, so that the gear plate 65 can be driven to rotate synchronously through the second single-sided bevel block 84.

[0054] In the solution further provided by the present invention, the bottom end of the detection tank 14 is also connected to a water-gas separator 91, and the water-gas separator 91 is used to separate gas and liquid. The detection tank 14 is also connected to a gas pipe 92; the water-gas separator 91 is connected to the front fraction receiving tank 11 through a collection pipe 93, and the gas pipe 92 is connected to an external inert gas tank for protecting the flowing trimethylaluminum. After the detection is completed, the two enter the water-gas separator 91 of the device for separation, and the separated trimethylaluminum enters the collection pipe 93 through the collection pipe 93. To the front fraction receiving tank 11, a reflux pipe 94 is provided at the discharge port at the bottom of each main fraction receiving tank 12, and each reflux pipe 94 is connected to the collecting pipe 93. The front fraction receiving tank 11 is connected to the feed port of the distillation kettle 1 through the return pipe 95. The purpose of providing the reflux pipe 94 at the discharge port at the bottom of the main fraction receiving tank 12 and connecting the reflux pipe 94 and the front fraction receiving tank 11 is to guide the trimethylaluminum that fails the detection in the main fraction receiving tank 12 back to the distillation kettle 1 for further treatment.

[0055] A method for using a sampling detection device prepared based on trimethylaluminum, the method for using a sampling detection device prepared based on trimethylaluminum comprising the following steps:

[0056] S1: The crude trimethylaluminum is transferred from the crude product transfer tank to the distillation kettle 1 by nitrogen, and is heated and distilled under normal pressure. The trimethylaluminum before the tower top temperature reaches the standard value enters the front fraction receiving tank 11 through the discharge pipe 13. When the tower top temperature reaches the standard value, the trimethylaluminum enters the main fraction receiving tank 12 through the discharge pipe 13 and the first connecting mechanism;

[0057] S2: When the main fraction receiving tank 12 is filled with an appropriate amount, the driving mechanism is started to rotate, driving the first connecting mechanism to rotate to guide the trimethylaluminum in the discharge pipe 13 to another one for continued collection, and the second connecting mechanism is driven to rotate synchronously through the connecting piece to connect the sampling assembly with the main fraction receiving tank 12 that has just been filled with trimethylaluminum;

[0058] S3: After the adjustment is completed, the driving mechanism is driven to rotate in the opposite direction, the sampling assembly is driven to work through the trigger mechanism, and a certain amount of trimethylaluminum is collected and put into the detection tank 14 for detection.

[0059] Working principle: During operation, the trimethylaluminum rectified by the distillation kettle 1 enters the second through groove 25 in the second arc-shaped circular ring 24 through the discharge pipe 13, the hollow cylinder 27 and the connecting pipe 26, and enters the first through groove 23 connected with the second through groove 25 into the liquid discharge pipe 21, and then falls into the main fraction receiving tank 12. When the main fraction receiving tank 12 is completed and needs to be switched, the reversible motor 71 is started, and the main rotating rod 72 is driven to rotate by the rotation of the reversible motor 71. The rotation of the main rotating rod 72 drives the helical gear ring 73 and the first bevel gear 74 connected thereto to rotate synchronously, and the helical gear ring 73 and the first bevel gear 74 are driven to rotate synchronously. The ring 73 rotates so that the plane side of its helical teeth contacts the plane of the first single-sided inclined block 76 in the fixed ring 75. At this time, the helical ring 73 rotates through the influence of the blocked first single-sided inclined block 76, driving the fixed ring 75 to rotate with the rotation of the helical ring 73. The fixed ring 75 is fixedly connected to the second arc-shaped circular ring 24. Through the rotation of the second arc-shaped circular ring 24, the second through groove 25 provided thereon can be driven to rotate to another first through groove 23 on the first arc-shaped circular ring 22. At this time, the liquid passes through the first through groove 23 and the liquid outlet pipe 21 into another main fraction receiving tank 12 for storage;

[0060] The second arcuate ring 24 rotates through the L-shaped plate 4 to drive the fourth arcuate ring 34 to rotate synchronously, so that the fourth through groove 35 on the fourth arcuate ring 34 is connected with another third through groove 33 of the third arcuate ring 32. At the same time, the first bevel gear 74 rotates with the main rotating rod 72 and meshes with the second bevel gear 82 on the auxiliary rod 81, thereby driving the auxiliary rod 81 to rotate synchronously, but the rotation direction of the auxiliary rod 81 is the same as the inclination direction of the bevel side of the internal bevel groove 86 thereof. Since the rotation of the gear ring 83 will be resisted by the gear plate 65, the rotation of the auxiliary rod 81 through the bevel groove 86 cannot drive the gear ring 83 to rotate synchronously.

[0061] When the second through groove 25 is connected with the appropriate first through groove 23, the fourth through groove 35 is also connected with the third through groove 33 on the main fraction receiving tank 12 that has just been filled. At this time, the reversible motor 71 is driven to rotate in the opposite direction. When the reversible motor 71 drives the main rotating rod 72 to rotate in the opposite direction, the inclined surface side of the bevel gear ring 73 arranged thereon contacts the inclined surface side of the first single-sided inclined block 76. At this time, the teeth of the bevel gear ring 73 abut the first single-sided inclined block 76 to push the abutment spring 77 to move toward the inside of the fixed ring 75, and the fixed ring 75 does not rotate. If the fixed ring 75 does not rotate, the positions of the second arc-shaped circular ring 24 and the fourth arc-shaped circular ring 34 will not be adjusted. When the first When the bevel gear 74 rotates in the opposite direction, it will mesh with the second bevel gear 82 and rotate in the opposite direction. The second bevel gear 82 drives the auxiliary rod 81 to rotate in the opposite direction synchronously. At this time, the plane side of the bevel groove 86 in the auxiliary rod 81 contacts the plane end of the second single-sided bevel block 84. At this time, the second single-sided bevel block 84 is driven by the rotational force of the auxiliary rod 81 to drive the gear ring 83 to rotate synchronously. The gear ring 83 meshes with the gear plate 65 and rotates synchronously. The rotation of the gear plate 65 drives the cam 66 to rotate through the rotating rod 64. After the cam 66 rotates, the contact plate with the baffle 63 changes. The baffle 63 will move up and down reciprocatingly under the influence of the limit rod 68 and the track groove 67 on the cam 66. The baffle 63 moves back and forth After the piston plate 61 in the piston cylinder 51 is moved, the piston rod 62 can drive the piston plate 61 in the piston cylinder 51 to move, thereby driving the pressure in the piston cylinder 51 to change, so that the trimethyl aluminum poured into the main fraction receiving tank 12 can be sucked into the third through groove 33 through the infusion tube 31, and then sucked into the piston cylinder 51 through the sampling tube 36 on the fourth through groove 35. When the piston plate 61 is downward, the trimethyl aluminum sucked into the piston cylinder 51 will be pressed into the detection tank 14 through the supply pipe 52 for detection. After a certain amount of liquid is extracted, the reversible motor 71 can be turned off. At this time, the external supply device is started to supply gas to the gas pipe 92, so that the inert gas flows in the detection tank 14. , the attached trimethylaluminum can be taken away to avoid affecting the next test result, and the trimethylaluminum detected by the detection tank 14 and the trimethylaluminum flowing with the inert gas finally enter the steam-water separator 91 for separation, and then the trimethylaluminum enters the front fraction receiving tank 11 through the collecting pipe 93, and enters the distillation kettle 1 through the return pipe 95 on the front fraction receiving tank 11 for reprocessing. When the detection tank 14 detects unqualified trimethylaluminum, the trimethylaluminum stored in the main fraction receiving tank 12 will enter the collecting pipe 93 through the reflux pipe 94, and then enter the distillation kettle 1 through the main fraction receiving tank 12 and the return pipe 95 for re-purification.

[0062] The above description is only by way of illustration of certain exemplary embodiments of the present invention. It is undoubted that those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A sampling detection device based on trimethylaluminum, comprising a distillation kettle (1), a front fraction receiving tank (11) and a plurality of main fraction receiving tanks (12), characterized in that: The distillation kettle (1) is connected to the front fraction receiving tank (11) through a discharge pipe (13), the discharge pipe (13) is connected to a plurality of main fraction receiving tanks (12) through a first connecting mechanism, a detection tank (14) is fixedly connected between the plurality of main fraction receiving tanks (12), a sampling assembly is arranged on the detection tank (14), and the plurality of main fraction receiving tanks (12) are connected to the sampling assembly through a second connecting mechanism; It also includes a driving mechanism, which is arranged on the discharge pipe (13); When the drive mechanism is working, it has the following two positions: At the first station, when the driving mechanism rotates, the first connecting mechanism drives the discharge pipe (13) to communicate with one of the main fraction receiving tanks (12) for filling and storage, and when the first connecting mechanism is in operation, the second connecting mechanism is driven to rotate through the connecting piece so that the sampling assembly is connected with another of the main fraction receiving tanks (12); At the second station, when the driving mechanism rotates in the reverse direction, the trigger mechanism drives the sampling assembly to work, and the trimethylaluminum poured into the main fraction receiving tank (12) is transported to the detection tank (14) for detection; The first connecting mechanism comprises a liquid outlet pipe (21) connected to each main fraction receiving tank (12); The same first arcuate circular ring (22) is fixedly connected to each of the liquid outlet pipes (21); a plurality of first through grooves (23) are provided on the first arcuate circular ring (22); each of the first through grooves (23) is communicated with the corresponding liquid outlet pipe (21); a second arcuate circular ring (24) is rotatably connected to the first arcuate circular ring (22); a second through groove (25) is provided on the second arcuate circular ring (24); a connecting pipe (26) is provided on the second arcuate circular ring (24); the second through groove (25) is communicated with the connecting pipe (26); one end of the material outlet pipe (13) is communicated with a hollow cylinder (27); the connecting pipe (26) is rotatably connected to the hollow cylinder (27) via a connector (28); The second connecting mechanism comprises a liquid infusion pipe (31) connected to each main fraction receiving tank (12); Each of the infusion tubes (31) is fixedly connected to the same third arc-shaped circular ring (32), and a plurality of third through grooves (33) are provided on the third arc-shaped circular ring (32), and each of the third through grooves (33) is communicated with the corresponding infusion tube (31); a fourth arc-shaped circular ring (34) is rotatably connected to the third arc-shaped circular ring (32), and a fourth through groove (35) is provided on the fourth arc-shaped circular ring (34); a sampling tube (36) is provided on the fourth arc-shaped circular ring (34), and the fourth through groove (35) is communicated with the sampling tube (36); The connecting member is an L-shaped plate (4) fixedly connected between the second arc-shaped circular ring (24) and the fourth arc-shaped circular ring (34); The sampling assembly comprises a piston cylinder (51) fixedly connected to the fourth arc-shaped ring (34), and the piston cylinder (51) is connected to the sampling tube (36); The bottom of the piston cylinder (51) is connected to a supply pipe (52), the supply pipe (52) is connected to a detection tank (14), and a piston unit is provided on the piston cylinder (51); The piston unit comprises a piston plate (61) slidably connected in the piston cylinder (51), a piston rod (62) being fixedly connected to the piston plate (61), and a baffle (63) being fixedly connected to the piston rod (62); The L-shaped plate (4) is rotatably connected to a rotating rod (64), the rotating rod (64) is fixedly connected to a gear plate (65) and a cam (66), the cam (66) is provided with a track groove (67), the baffle plate (63) is fixedly connected to a limiting rod (68), and the limiting rod (68) is slidably connected in the track groove (67); The driving mechanism comprises a reversible motor (71) fixedly connected to the hollow cylinder (27), a main rotating rod (72) fixedly connected to the output end of the reversible motor (71), and a helical gear ring (73) and a first bevel gear (74) fixedly connected to the main rotating rod (72); A fixing ring (75) is fixedly connected to the second arc-shaped circular ring (24), and a plurality of first single-sided inclined blocks (76) are slidably connected in the fixing ring (75). A contact spring (77) is provided between each of the first single-sided inclined blocks (76) and the fixing ring (75), and the elastic force of the contact spring (77) drives the first single-sided inclined block (76) to contact the helical gear ring (73), and the main rotating rod (72) drives the gear plate (65) to mesh through the passive component; The passive component comprises an auxiliary rod (81) rotatably connected to the L-shaped plate (4), a second bevel gear (82) being fixedly connected to the auxiliary rod (81), and the second bevel gear (82) is meshed with the first bevel gear (74); The auxiliary rod (81) is provided with a gear ring (83), and a plurality of second single-sided inclined blocks (84) are slidably connected in the gear ring (83). A support spring (85) is provided between each of the second single-sided inclined blocks (84) and the gear ring (83). A plurality of inclined grooves (86) are provided on the surface of the auxiliary rod (81), and the elastic force of the support spring (85) drives the second single-sided inclined blocks (84) to engage with the inclined grooves (86).

2. A sampling detection device based on trimethylaluminum according to claim 1, characterized in that: The bottom end of the detection tank (14) is also connected to a steam-water separator (91), and the detection tank (14) is also connected to a gas pipe (92); The steam-water separator (91) is connected to the front fraction receiving tank (11) through a collecting pipe (93), and a reflux pipe (94) is provided at the discharge port at the bottom of each main fraction receiving tank (12). Each reflux pipe (94) is connected to the collecting pipe (93), and the front fraction receiving tank (11) is connected to the feed port of the distillation kettle (1) through a return pipe (95).

3. A method for using a sampling detection device based on trimethylaluminum, which is used for the sampling detection device based on trimethylaluminum as claimed in any one of claims 1 to 2, characterized in that: The method for using the sampling detection device prepared based on trimethylaluminum comprises the following steps: S1: The crude trimethylaluminum product is transferred from the crude product transfer tank to the distillation kettle (1) by nitrogen, and heated and distilled under normal pressure. The trimethylaluminum before the tower top temperature reaches the standard value enters the front fraction receiving tank (11) through the discharge pipe (13). After the tower top temperature reaches the standard value, the trimethylaluminum enters the main fraction receiving tank (12) through the discharge pipe (13) and the first connecting mechanism. S2: When the main fraction receiving tank (12) is filled with an appropriate amount of trimethyl aluminum, the driving mechanism is started to rotate, driving the first connecting mechanism to rotate to guide the trimethyl aluminum in the discharge pipe (13) to another one for continued collection, and the second connecting mechanism is driven to rotate synchronously through the connecting piece to connect the sampling assembly with the main fraction receiving tank (12) that has just been filled with trimethyl aluminum; S3: After the adjustment is completed, the driving mechanism is driven to rotate in the opposite direction, and the sampling assembly is driven to work through the trigger mechanism, and a certain amount of trimethylaluminum is collected and put into the detection tank (14) for detection.

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