CN216062084U

CN216062084U - Trimethyl aluminum purification and distillation equipment

Info

Publication number: CN216062084U
Application number: CN202122690541.XU
Authority: CN
Inventors: 刘任飞; 陆平
Original assignee: Nanda Optoelectronic Semiconductor Materials Co ltd
Current assignee: Nanda Optoelectronic Semiconductor Materials Co ltd
Priority date: 2021-11-04
Filing date: 2021-11-04
Publication date: 2022-03-18
Anticipated expiration: 2031-11-04

Abstract

The utility model relates to the technical field of trimethylaluminum, in particular to trimethylaluminum purification distillation equipment which comprises a distillation mechanism, wherein the distillation mechanism comprises a distillation flask, the bottom of the distillation flask is provided with a heater, the top end of the distillation flask is provided with a bottleneck connecting end, the outer side of the bottleneck connecting end is connected with a pressure relief pipe and a connecting pipe, one end of the connecting pipe, which is far away from the bottleneck connecting end, is connected with a condensation pipe, the outer side of the condensation pipe is connected with a steam outlet, a snake-shaped water cooling pipe is arranged inside the condensation pipe, one end of the condensation pipe, which is far away from the connecting pipe, is connected with a discharging pipe, and the outer side of the discharging pipe is connected with a purification mechanism. When trimethylaluminum steam got into the condenser pipe, can condense steam through the flow of the inside frozen water of snakelike water-cooling tube, avoid steam temperature too high, follow-up unable heat dissipation influences chemical structure, and gas and impurity that produce after the distillation pass the unloading pipe immediately and enter into the purification flask to the realization is to the distillation of material.

Description

Trimethyl aluminum purification and distillation equipment

Technical Field

The utility model relates to the technical field of trimethylaluminum, in particular to trimethylaluminum purification and distillation equipment.

Background

Trimethylaluminum is an organic compound of formula C3H9 Al. Dissolving in organic solvent such as diethyl ether and saturated hydrocarbon. Impurities in organometallic compounds, especially trimethylaluminum, include hydrocarbon components, organosilicon components, alkylaluminum oxides, metal compounds, and the like. Among these impurities, the organosilicon component and the alkylaluminum oxide generally have a higher or similar vapor pressure than trimethylaluminum, and therefore, in the compound semiconductor produced from trimethylaluminum, it may form silicon inclusions and oxygen inclusions, so these impurities are considered to be very harmful.

The prior patent (publication No. CN1749260A) proposes a method for purifying high-purity trimethylaluminum and crude trimethylaluminum, in which high-purity trimethylaluminum can be efficiently removed by an industrially economical and easy method by distilling with high-purity metallic sodium dissolved in trimethylaluminum when impurities are removed from trimethylaluminum by distillation and evaporation. In one aspect of the present invention, there is provided a high purity trimethylaluminum comprising the following impurity components: an organosilicon component of 0.5ppm or less, a chlorine component of 20ppm or less, a hydrocarbon component of 1,000 ppm or less, Ca of 0.05ppm or less, Fe of 0.05ppm or less, Mg of 0.05ppm or less, Na of 0.05ppm or less, Si (silicon component other than the organosilicon component) of 0.07ppm or less, Zn of 0.05ppm or less, and S of 0.05ppm or less. Preferably, the content of the alkylaluminum oxide cannot be higher than 20 ppm. In another aspect of the present invention, there is also provided a refining method of crude trimethylaluminum, comprising removing impurities from crude trimethylaluminum by distillation and evaporation to obtain the above-mentioned high-purity trimethylaluminum.

According to the process of the present invention, high purity trimethylaluminum can be economically produced by an industrially easy and practical method. Epitaxial growth of high purity trimethylaluminum enables the production of materials useful as high performance compound semiconductors. Furthermore, the distillation residue can be used as a catalyst for producing a polyolefin having a higher purity, and the process of the present invention can be compensated in terms of cost due to the industrial applicability.

The preparation and purification of trimethylaluminum are mainly aimed at the distillation of trimethylaluminum, and high-purity trimethylaluminum is obtained through continuous high-temperature evaporation, but the preparation method has the defects of large amount of impurities, impurity purity of the prepared trimethylaluminum, large amount of distillation residues and incapability of combining the distillation and the purification.

Therefore, a trimethylaluminum purification distillation device is provided.

SUMMERY OF THE UTILITY MODEL

The utility model aims to provide trimethylaluminum purification distillation equipment, which can condense steam through the flowing energy of ice water in a serpentine water-cooling pipe, so that the problems that the steam temperature is too high, heat cannot be dissipated subsequently and the chemical structure is influenced are solved, and gas and impurities generated after distillation immediately pass through a feeding pipe and enter a purification flask, so that the distillation of substances is realized; through stirring the steam and the impurity of the inside to purifying the chamber, steam and impurity are gradually by purification mouth suction, pass the purification passageway and get into the purification room, through the work of clarifier to purify the indoor material of purification, realize the purpose of purification then. The problems set forth in the background above are solved by combining distillation and purification equipment.

In order to achieve the purpose, the utility model provides the following technical scheme:

the utility model provides a trimethylaluminum purification distillation plant, including distillation mechanism, distillation mechanism includes the distillation flask, the bottom of distillation flask is provided with the heater, the top of distillation flask is provided with the bottleneck link, the outside of bottleneck link is connected with pressure release pipe and connecting pipe, the left side at the bottleneck link is connected to the pressure release pipe, the right side at the bottleneck link is connected to the connecting pipe, the pressure release pipe highly is less than the height of connecting pipe in bottleneck link junction, distillation flask's inside is pegged graft and is had the thermometer, the one end that the bottleneck link was kept away from to the connecting pipe is connected with the condenser pipe, the outside of condenser pipe is connected with steam outlet, the inside of condenser pipe is provided with snakelike water-cooling tube, the one end that the connecting pipe was kept away from to the condenser pipe is connected with the unloading pipe, the outside of unloading pipe is connected with purification mechanism.

Will treat the trimethylaluminum of distillation purification and place into the distillation flask, heat the distillation flask through the heater, the pressure that the distillation produced is discharged from the pressure release pipe, the steam impurity that the distillation produced etc. is discharged from the connecting pipe, reach the condenser pipe, the inside of condenser pipe sets up snakelike water-cooling tube, the inside of snakelike water-cooling tube can hold the frozen water, when trimethylaluminum steam gets into the condenser pipe, can condense steam through the inside frozen water's of snakelike water-cooling tube flowing, avoid steam temperature too high, follow-up unable heat dissipation, influence chemical structure, gas and impurity that produce after the distillation pass the unloading pipe immediately and enter into the purification flask, thereby realize the distillation to the material.

Preferably, the purification mechanism is internally provided with a purification flask, a driving motor is arranged in the purification flask, a driving screw is connected to the outer side of the driving motor, a movable block is movably connected to the outer side of the driving screw, a shaft lever is connected to the outer side of the movable block, and a bearing plate is connected to one end, far away from the movable block, of the shaft lever.

By starting the driving motor, the driving motor immediately starts working, then drives the driving screw to synchronously rotate, and immediately and synchronously drives the movable block to move on the driving screw along with the rotation of the driving screw, and then the movable block drives the shaft lever to deflect and simultaneously drives the bearing plate to move, thereby realizing the operation of the whole structure.

Preferably, the outer sides of the shaft lever and the bearing plate are both connected with mounting springs, the outer sides of the mounting springs are connected with mounting brackets, one ends, far away from the mounting springs, of the mounting brackets are connected with mounting plates, and the outer sides of the mounting plates are connected with transverse plates.

Through the synchronous motion of the mounting springs which are lapped on the shaft rod and the outer side of the bearing plate, the mounting springs are stretched under the action of centrifugal force, the mounting bracket, the mounting plate and the transverse plate are driven to be stretched synchronously, and the circumferential motion is carried out along with the rotation of the driving screw rod, so that the steam and the impurities in the purification cavity are stirred.

Preferably, the inside of purification mechanism still includes the purification chamber, and the inside in purification chamber still is provided with the purification mouth, and the inboard of purification mouth is connected with the purification passageway, and the one end that the purification mouth was kept away from to the purification passageway is provided with the purification room, and the outside of purification room is provided with the clarifier.

Through stirring the steam and the impurity of the inside to purifying the chamber, steam and impurity are gradually by purification mouth suction, pass the purification passageway and get into the purification room, through the work of clarifier to purify the indoor material of purification, realize the purpose of purification then.

Preferably, the thermometer is a digital thermometer, and the temperature measuring end thereof is inserted into the interior of the distillation flask.

The distillation flask is heated by the heater, the temperature in the distillation flask is accurately measured by the thermometer, and the accurate temperature control during distillation is ensured, so that the distillation quality is ensured.

Preferably, steam outlet is the flexible glue pipe material, installs in the top of condenser pipe, and when trimethylaluminium steam got into the condenser pipe, can condense steam through the inside icy water of snakelike water-cooling tube flows, avoids the steam temperature too high, and follow-up unable heat dissipation influences the chemical structure, and in condensation process, cold and hot reaction in turn produces a large amount of steam, and steam passes through steam outlet and discharges, avoids atomizing steam to pile up, influences the equipment and uses.

Compared with the prior art, the utility model has the beneficial effects that:

1. according to the trimethylaluminum purification distillation equipment, the distillation flask is heated by the heater, the temperature in the distillation flask is accurately measured by the thermometer, and the accurate temperature control during distillation is ensured.

2. This trimethylaluminium purification distillation plant, when trimethylaluminium steam got into the condenser pipe, can condense steam through the inside icy water of snakelike water-cooling tube flows, avoids steam temperature too high, follow-up unable heat dissipation, influences chemical structure, and gas and impurity that produce after the distillation pass the unloading pipe immediately and enter into the purification flask to the realization is to the distillation of material.

3. This trimethylaluminum purification distillation plant is stretched through installing support, mounting panel and diaphragm synchronization to be circular motion along with drive screw's rotation, stir the steam and the impurity of the inside in purification chamber, and gradually by purification mouth suction, pass the purification passageway and get into the purification room, through the work of clarifier, thereby purify the indoor material of purification, realize the purpose of purification then.

Drawings

FIG. 1 is a schematic view of the overall structure of the present invention;

FIG. 2 is a schematic view of the internal structure of the condenser tube according to the present invention;

FIG. 3 is a schematic view of the connection structure of the purification flask according to the present invention;

FIG. 4 is a schematic view of a driving motor connection structure according to the present invention;

FIG. 5 is a schematic view of a portion of the structure of FIG. 4 in accordance with the present invention;

FIG. 6 is a schematic view showing a connection structure of a purification chamber according to the present invention;

FIG. 7 is an enlarged view of the structure of area A in FIG. 6 according to the present invention.

In the figure: 1. distilling the flask; 2. a heater; 3. a bottle mouth connecting end; 4. a pressure relief pipe; 5. a thermometer; 6. a connecting pipe; 7. a condenser tube; 8. a steam outlet; 9. a serpentine water-cooled tube; 10. a discharging pipe; 11. a purification flask; 12. a drive motor; 13. a drive screw; 14. a movable block; 15. a shaft lever; 16. a bearing plate; 17. installing a spring; 18. mounting a bracket; 19. mounting a plate; 20. a transverse plate; 21. a purification chamber; 22. purifying; 23. a purification channel; 24. a purification chamber; 25. a purifier.

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.

In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "first", "second", may explicitly or implicitly include one or more of the described features. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise. Furthermore, the terms "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

Referring to fig. 1 to 7, the present invention provides a trimethylaluminum purification and distillation apparatus, which has the following technical scheme:

the utility model provides a trimethylaluminum purification distillation plant, including distillation mechanism, distillation mechanism includes distillation flask 1, distillation flask 1's bottom is provided with heater 2, distillation flask 1's top is provided with bottleneck link 3, the outside of bottleneck link 3 is connected with pressure release pipe 4 and connecting pipe 6, pressure release pipe 4 is connected in the left side of bottleneck link 3, the right side at bottleneck link 3 is connected to connecting pipe 6, pressure release pipe 4 highly is less than the height of connecting pipe 6 in bottleneck link 3 junction, distillation flask 1's inside is pegged graft and is had thermometer 5, the one end that bottleneck link 3 was kept away from to connecting pipe 6 is connected with condenser pipe 7, the outside of condenser pipe 7 is connected with steam outlet 8, the inside of condenser pipe 7 is provided with snakelike water-cooling tube 9, the one end that connecting pipe 6 was kept away from to condenser pipe 7 is connected with unloading pipe 10, the outside of unloading pipe 10 is connected with the purification mechanism.

Will wait to distill the trimethylaluminum of purification and place into distillation flask 1, the pressure that the distillation produced is discharged from pressure release pipe 4, steam impurity that the distillation produced etc. are discharged from connecting pipe 6, reach condenser pipe 7, the inside of condenser pipe 7 sets up snakelike water-cooling tube 9, snakelike water-cooling tube 9's inside can hold the frozen water, when trimethylaluminum steam gets into condenser pipe 7, can condense steam through the inside frozen water's of snakelike water-cooling tube 9 flow, avoid steam temperature too high, follow-up unable heat dissipation, influence chemical structure, gas and impurity that produce after the distillation pass down pipe 10 immediately and enter into purification flask 11, thereby realize the distillation to the material.

Referring to fig. 3-4, in one embodiment of the present invention, the interior of the purifying mechanism includes a purifying flask 11, a driving motor 12 is disposed in the purifying flask 11, a driving screw 13 is connected to the outside of the driving motor 12, a movable block 14 is movably connected to the outside of the driving screw 13, a shaft rod 15 is connected to the outside of the movable block 14, and a receiving plate 16 is connected to one end of the shaft rod 15 far from the movable block 14.

By starting the driving motor 12, the driving motor 12 immediately starts to work, and then drives the driving screw 13 to synchronously rotate, and with the rotation of the driving screw 13, the movable block 14 is immediately and synchronously driven to move on the driving screw 13, and the movable block 14 then drives the shaft rod 15 to deflect and simultaneously drives the bearing plate 16 to move, so that the operation of the whole structure is realized.

Referring to fig. 5, as an embodiment of the present invention, an installation spring 17 is connected to the outer sides of the shaft lever 15 and the receiving plate 16, an installation bracket 18 is connected to the outer side of the installation spring 17, an installation plate 19 is connected to one end of the installation bracket 18 away from the installation spring 17, and a transverse plate 20 is connected to the outer side of the installation plate 19.

By the synchronous movement of the mounting spring 17 overlapped on the outer sides of the shaft lever 15 and the bearing plate 16, the mounting spring 17 is stretched under the action of centrifugal force, and drives the mounting bracket 18, the mounting plate 19 and the transverse plate 20 to be stretched synchronously, and the circumferential movement is carried out along with the rotation of the driving screw 13, so that the steam and the impurities in the purifying cavity 21 are stirred.

Referring to fig. 6 to 7, as an embodiment of the present invention, a purification chamber 21 is further included inside the purification mechanism, a purification port 22 is further disposed inside the purification chamber 21, a purification passage 23 is connected to an inner side of the purification port 22, a purification chamber 24 is disposed at an end of the purification passage 23 away from the purification port 22, and a purifier 25 is disposed outside the purification chamber 24.

By stirring the steam and impurities inside the purification chamber 21, the steam and impurities are gradually sucked in by the purification port 22, pass through the purification passage 23, enter the purification chamber 24, and are purified by the operation of the purifier 25, thereby purifying the substance inside the purification chamber 24, and further achieving the purpose of purification.

Referring to FIG. 1, in one embodiment of the present invention, a thermometer 5 is a digital thermometer, and its temperature measuring end is inserted into the distillation flask 1.

The distillation flask 1 is heated by the heater 2, the temperature in the distillation flask 1 is accurately measured by the thermometer 5, and the accurate temperature control during distillation is ensured, so that the distillation quality is ensured.

Referring to fig. 2, as an embodiment of the present invention, the steam outlet 8 is made of a flexible rubber hose and is installed above the condensation duct 7.

When trimethylaluminum steam got into the condenser pipe, can condense steam through the flow of the inside frozen water of snakelike water-cooled tube 9, avoid steam temperature too high, follow-up unable heat dissipation influences the chemical structure, and in the condensation process, cold and hot reaction in turn produces a large amount of steam, and steam passes through steam outlet 8 and discharges, avoids atomizing steam to pile up, influences equipment and uses.

The working principle is as follows: when the distillation device is used, trimethylaluminum to be distilled and purified is placed into the distillation flask 1, the distillation flask 1 is heated through the heater 2, the temperature in the distillation flask 1 is accurately measured through the thermometer 5, accurate temperature control during distillation is guaranteed, pressure generated by distillation is discharged from the pressure relief pipe 4, steam impurities generated by distillation and the like are discharged from the connecting pipe 6 and reach the condensation pipe 7, the serpentine water-cooling pipe 9 is arranged inside the condensation pipe 7, ice water can be contained inside the serpentine water-cooling pipe 9, when trimethylaluminum steam enters the condensation pipe 7, the steam can be condensed through flowing of the ice water inside the serpentine water-cooling pipe 9, the phenomenon that the steam temperature is too high, subsequent heat dissipation cannot be achieved, the chemical structure is affected is avoided, and gas and impurities generated after distillation immediately pass through the discharging pipe 10 and enter the purification flask 11, and therefore distillation of substances is achieved.

After steam and distillation impurities enter the purification flask 11, the driving motor 12 is started to work immediately by starting the driving motor 12, then the driving screw 13 is driven to rotate synchronously, the movable block 14 is driven to move on the driving screw 13 immediately and synchronously along with the rotation of the driving screw 13, the movable block 14 drives the shaft lever 15 to deflect and drives the bearing plate 16 to move simultaneously, at the moment, the mounting spring 17 lapped on the outer sides of the shaft lever 15 and the bearing plate 16 moves synchronously, the mounting spring 17 is stretched under the action of centrifugal force and drives the mounting bracket 18, the mounting plate 19 and the transverse plate 20 to be stretched synchronously and move circularly along with the rotation of the driving screw 13, the steam and the impurities in the purification cavity 21 are stirred and are gradually sucked by the purification port 22, pass through the purification channel 23 and enter the purification chamber 24, and pass through the work of the purifier 25, thereby purifying the substance inside the purifying chamber 24 and then achieving the purpose of purification.

The electric elements in the document are electrically connected with an external main controller and 220V mains supply through a transformer, the main controller can be a conventional known device controlled by a computer and the like, the product model provided by the utility model is only used according to the structural characteristics of the product, the product can be adjusted and modified after being purchased, so that the product is more matched with and accords with the technical scheme of the utility model, the product model is a technical scheme of the optimal application of the technical scheme, the product model can be replaced and modified according to the required technical parameters, and the product model is familiar to the technical personnel in the field, so that the technical scheme provided by the utility model can clearly obtain the corresponding use effect.

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 utility model, the scope of which is defined in the appended claims and their equivalents.

Claims

1. The utility model provides a trimethylaluminum purification distillation plant, includes distillation mechanism, its characterized in that: the distillation mechanism comprises a distillation flask (1), a heater (2) is arranged at the bottom of the distillation flask (1), a bottleneck connecting end (3) is arranged at the top end of the distillation flask (1), a pressure relief pipe (4) and a connecting pipe (6) are connected to the outer side of the bottleneck connecting end (3), the pressure relief pipe (4) is connected to the left side of the bottleneck connecting end (3), the connecting pipe (6) is connected to the right side of the bottleneck connecting end (3), the height of the pressure relief pipe (4) at the connecting position of the bottleneck connecting end (3) is lower than that of the connecting pipe (6), a thermometer (5) is inserted into the distillation flask (1), a condensing pipe (7) is connected to one end, far away from the bottleneck connecting end (3), of the connecting pipe (6), and a steam outlet (8) is connected to the outer side of the condensing pipe (7), the novel purifying device is characterized in that a snake-shaped water-cooling pipe (9) is arranged inside the condensation pipe (7), one end, far away from the connecting pipe (6), of the condensation pipe (7) is connected with a discharging pipe (10), and the outer side of the discharging pipe (10) is connected with a purifying mechanism.

2. A trimethylaluminum purification distillation apparatus according to claim 1, wherein: purification mechanism's inside is including purification flask (11), the inside of purification flask (11) is provided with driving motor (12), the outside of driving motor (12) is connected with drive screw (13), the outside swing joint of drive screw (13) has movable block (14), the outside of movable block (14) is connected with axostylus axostyle (15), the one end that movable block (14) were kept away from in axostylus axostyle (15) is connected with accepts board (16).

3. A trimethylaluminum purification distillation apparatus according to claim 2, wherein: the outer sides of the shaft lever (15) and the bearing plate (16) are both connected with mounting springs (17), the outer sides of the mounting springs (17) are connected with mounting brackets (18), one ends, far away from the mounting springs (17), of the mounting brackets (18) are connected with mounting plates (19), and the outer sides of the mounting plates (19) are connected with transverse plates (20).

4. A trimethylaluminum purification distillation apparatus according to claim 1, wherein: purification mechanism's inside still including purification chamber (21), the inside of purification chamber (21) still is provided with purification mouth (22), the inboard of purification mouth (22) is connected with purification passageway (23), the one end that purification mouth (22) were kept away from in purification passageway (23) is provided with purification room (24), the outside of purification room (24) is provided with clarifier (25).

5. A trimethylaluminum purification distillation apparatus according to claim 1, wherein: the thermometer (5) is a digital thermometer, and the temperature measuring end of the thermometer is inserted into the distillation flask (1).

6. A trimethylaluminum purification distillation apparatus according to claim 1, wherein: the steam outlet (8) is made of a soft rubber pipe material and is arranged above the condensation pipe (7).