CN113181752B - Germane collecting and purifying equipment and method - Google Patents
Germane collecting and purifying equipment and method Download PDFInfo
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- CN113181752B CN113181752B CN202110323153.XA CN202110323153A CN113181752B CN 113181752 B CN113181752 B CN 113181752B CN 202110323153 A CN202110323153 A CN 202110323153A CN 113181752 B CN113181752 B CN 113181752B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/30—Alkali metal compounds
- B01D2251/304—Alkali metal compounds of sodium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/30—Alkali metal compounds
- B01D2251/306—Alkali metal compounds of potassium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/60—Inorganic bases or salts
- B01D2251/604—Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/204—Inorganic halogen compounds
- B01D2257/2045—Hydrochloric acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
Abstract
The invention provides germane collecting and purifying equipment which comprises a first gas storage tank, a condenser and a purifier, wherein a pretreatment device is arranged on one side of the first gas storage tank, an exhaust port of the first gas storage tank is communicated with the pretreatment device through a pipeline, the condenser is arranged on one side of the pretreatment device, the pretreatment device is communicated with a gas inlet of the condenser through a pipeline, the purifier is arranged on one side of the condenser, the exhaust port of the condenser is communicated with the gas inlet of the purifier through a pipeline, a second gas storage tank is arranged on one side of the purifier, the exhaust port of the purifier is communicated with the gas inlet of the second gas storage tank through a pipeline, a liquid storage tank is arranged on one side of the pretreatment device, and a liquid inlet of the liquid storage tank is communicated with the pretreatment device through a pipeline. According to the invention, the pretreatment device is added before purification to primarily filter and purify the germane gas, so that the removal effect of carbon dioxide and acid gas in the germane gas can be greatly improved, the purification effect of the purifier is improved, and the purification effect of the germane gas is better.
Description
Technical Field
The invention relates to the technical field of germane collection, in particular to germane collection and purification equipment and a method.
Background
Germane, a gaseous compound of germanium, is a colorless toxic gas having unpleasant odor at normal temperature and pressure. Stable at room temperature, starts to decompose at around 280 ℃ and almost completely decomposes to elemental germanium and hydrogen at around 350 ℃. The air can burn, and a bluish-red flame is emitted during combustion, but the combustion degree is not as intense as that of silane. Mixtures with oxygen or air are explosive. Reacting with alkali metal in liquid ammonia at normal temperature. Germane is highly autocatalytic and rapidly decomposes once decomposed to form a metal coating. Therefore, the surface of materials such as piping and the like is required to be smooth, not to be dissolved in water, but to be dissolved in hypochlorous acid, slightly to be dissolved in hot concentrated sulfuric acid, to be decomposed by nitric acid, and high-purity germane is required to be used in the industries of semiconductors, photovoltaic solar energy and integrated circuits. Germane is mainly used for producing high purity germanium and germanium epitaxial wafers for the semiconductor industry, since metallic germanium is a good semiconductor material. The method is mainly used for Metal Organic Chemical Vapor Deposition (MOCVD) process in the electronic industry, various amorphous silicon-germanium alloys are prepared together with silane, and compared with silicon, the amorphous a-SiGe alloy has the advantages of lower process temperature, adjustable forbidden band width, complete compatibility with the existing photovoltaic cell process technology and the like, and is mainly used for manufacturing thin-film solar cells.
In the existing germane purification process, a rectifying tower is partially used, but the investment of the rectifying tower is large, and the safety is difficult to guarantee; the other part of the germane is frozen, but the purity of the product is difficult to reach the quality standard of the semiconductor industry, the germane gas often contains carbon dioxide gas, on the other hand, the preparation process of the germane often contains more chloride ions, inevitably contains a small amount of acid gas containing the chloride ions, is not easy to remove as carbon dioxide gas impurities in the germane gas, but greatly influences the use effect of the high-purity germane in the subsequent production application;
on the other hand, the pretreated gas contains a large amount of moisture and other impurities such as digermane, digermane and chlorogermane gas, most of the moisture can be removed in a condensation mode, the subsequent moisture and other impurities are purified by installing a purifier in the treatment system, and the impurities are removed by adopting a chemical method or a freezing method or a physical adsorption method according to the types of the impurities, so that the purpose of gas purification is achieved;
in the purification of germane gas, if a purifier is used to purify germane gas containing many impurities, the impurities cannot be removed, which affects the final germane purity.
Therefore, it is necessary to provide a germane collecting and purifying apparatus and method to solve the above technical problems.
Disclosure of Invention
In order to solve the technical problems, the invention provides germane collecting and purifying equipment and a method which can pretreat germane gas containing impurities and have good pretreatment effect.
The invention provides germane collecting and purifying equipment which comprises a first gas storage tank, a condenser and a purifier, wherein a pretreatment device is arranged on one side of the first gas storage tank, an exhaust port of the first gas storage tank is communicated with the pretreatment device through a pipeline, the condenser is arranged on one side of the pretreatment device, the pretreatment device is communicated with a gas inlet of the condenser through a pipeline, the purifier is arranged on one side of the condenser, an exhaust port of the condenser is communicated with a gas inlet of the purifier through a pipeline, a second gas storage tank is arranged on one side of the purifier, an exhaust port of the purifier is communicated with a gas inlet of the second gas storage tank through a pipeline, a liquid storage tank is arranged on one side of the pretreatment device, and a liquid inlet of the liquid storage tank is communicated with the pretreatment device through a pipeline;
the pretreatment device comprises a support, a treatment tank, a cover body, a liquid adding device, a scattering device, an ultrasonic shattering device, an exhaust pipe, an annular flow dividing pipe, an air inlet pipe, an air nozzle and a liquid discharge pipe, wherein the support is arranged on one side of the first air storage tank, the treatment tank is fixed at the top of the support, the cover body is fixed at the top of the treatment tank through bolts, the liquid adding device is fixed in the middle of the cover body, the exhaust pipe is fixed at one end of the cover body and is communicated with an air inlet of a condenser through a pipeline, the annular flow dividing pipe is fixed at the bottom of the inner wall of the treatment tank, the air inlet pipe is fixed at one end of the annular flow dividing pipe, one end of the air inlet pipe penetrates through the treatment tank and is communicated with an air outlet of the first air storage tank through a pipeline, the air nozzle is fixed at the top of the annular flow dividing pipe at equal distance, the scattering device is fixed at the bottom of the treatment tank, the ultrasonic shattering device is fixed in the middle of the inner wall of the treatment tank, a liquid discharge pipe is fixed at the bottom of the treatment tank and is communicated with a liquid inlet of the liquid storage tank;
the scattering device comprises a rotating drum, a first rotating shaft, a first bevel gear, a bevel gear ring, a driving box, a first servo motor, a second bevel gear, a first stirring rod and a second stirring rod, the middle part of the treatment tank is rotationally connected with a rotary drum through a bearing, the inner wall of the rotary drum is rotationally connected with a first rotary shaft through a bearing, a first bevel gear is fixed at the bottom of the first rotating shaft, a bevel gear ring is fixed at the bottom of the rotating shaft, a driving box is fixed at the bottom of the treatment tank, the first bevel gear and the bevel gear ring are positioned on the inner wall of the driving box, a first servo motor is fixed on one side of the driving box, a second bevel gear is fixed on the output end of the first servo motor, and the second bevel gear is meshed with the first bevel gear and the bevel gear ring, first stirring rods are fixed to one end, far away from the bevel gear ring, of the rotary drum at equal intervals, and second stirring rods are fixed to one end, far away from the first bevel gear, of the first rotary shaft at equal intervals.
Preferably, the scattering device further comprises an inner gear ring, a second rotating shaft, a first flat gear and a third stirring rod, four the first stirring rod is fixed at one end of the inner gear ring, one end of the second stirring rod is connected with the second rotating shaft through a bearing in a rotating mode, the first flat gear is fixed at the bottom of the second rotating shaft and meshed with the inner gear ring, and the third stirring rod is fixed at one end, away from the first flat gear, of the second rotating shaft.
Preferably, the garrulous device is shaken to ultrasonic wave includes mount, vibrations post, filter screen, ultrasonic transducer and spliced pole, it is fixed with the mount to handle jar inner wall middle part equidistance, and is three the mount middle part is fixed with vibrations post, and is three the mount upper surface is fixed with the filter screen respectively, and is three the aperture of filter screen is and reduces the setting gradually from bottom to top, vibrations bottom of the column portion is fixed with ultrasonic transducer, adjacent two the equidistance is fixed with the spliced pole between the mount.
Preferably, the liquid feeding device includes fixed pipe, runner pipe, hydrojet pipe, atomising head, external gear ring, second servo motor and second spur gear, the lid middle part is rotated through the bearing and is connected with fixed pipe, fixed socle portion is passed the lid and is rotated through mechanical seal and be connected with the runner pipe, runner pipe both ends symmetry is fixed with the hydrojet pipe, hydrojet pipe bottom equidistance is fixed with the atomising head, the runner pipe outside is fixed with the external gear ring, the lid top is fixed with second servo motor, the output of second servo motor passes the lid and is fixed with the second spur gear, and the second spur gear is connected with the meshing of external gear ring.
Preferably, the fixing frame consists of three concentric rings, the concentric rings are connected through fixing rods distributed at equal intervals, and the connecting column and the connecting points of the concentric rings and the fixing rods are fixedly connected.
Preferably, the bottom of the vibration column is fixed with a protective shell, and the ultrasonic transducer is located on the inner wall of the protective shell.
Preferably, a liquid level sensor and a concentration sensor are fixed on the inner wall of the treatment tank.
Preferably, the first servo motor and the second servo motor are both speed reduction motors.
The invention also provides a germane collecting and purifying method, which depends on the germane collecting and purifying equipment provided by the invention, and the purifying method comprises the following steps:
1) germane containing impurities is collected in the first gas storage tank (1), pumped into the pretreatment device (2) through a gas pump and uniformly sprayed out through a gas inlet pipe (29) and an annular shunt pipe (28) in the pretreatment device (2);
2) adding a reaction solution into the treatment tank (22), and reacting the reaction solution with impurities in germane gas, wherein the reaction solution is one of 3-10mol/L sodium hydroxide solution or potassium hydroxide solution;
3) after the acidic impurities in the germane are preliminarily treated by the reaction solution, the germane gas is discharged into a condenser (3) for condensation, then the gas formed after condensation is dehydrated, adsorbed and cleaned by a purifier (4), the purified germane gas is obtained, and the purified germane gas is introduced into a second gas storage tank (5) for collection.
Preferably, the temperature of the reaction solution is between 45 and 80 °.
Compared with the related technology, the germane collecting and purifying equipment and the method provided by the invention have the following beneficial effects:
the invention provides a germane collecting and purifying device and a method, wherein the device comprises the following steps:
1. the pretreatment device is added before purification to primarily filter and purify the germane gas, so that the working efficiency can be greatly improved, the purification effect of the purifier is improved, and the purity of the germane is higher;
2. the first bevel gear and the bevel gear ring are driven to rotate reversely by the first servo motor, so that the first stirring rod and the second stirring rod can be driven to rotate reversely to stir the reaction solution, and the third stirring rod can rotate in a self-rotating manner in the rotating process of the first stirring rod and the second stirring rod, so that the stirring efficiency and the uniformity are greatly improved, the contact area of impurities and the reaction solution is improved, high-frequency vibration is emitted by the ultrasonic transducer, the smashed bubbles are further smashed, the contact area of the impurities and the reaction solution can be further improved, and the impurity removal effect is improved;
3. through setting up the liquid feeding device for second servo motor rotates, and then rotates through external gear ring and second gear drive rotating pipe, and then can drive the spray tube rotatory, makes the atomising head on the spray tube rotate round the rotating pipe in the spraying, makes and continuously spouts even diffusion of water smoke, can also play the effect with germane gas contact in the liquid feeding, further improves reaction effect.
Drawings
FIG. 1 is a schematic view of the overall structure provided by the present invention;
FIG. 2 is a schematic structural diagram of a pretreatment apparatus according to the present invention;
FIG. 3 is a second schematic structural diagram of a pretreatment apparatus according to the present invention;
FIG. 4 is a schematic view of a liquid level sensor according to the present invention;
FIG. 5 is a schematic view of the internal structure of the pretreatment apparatus according to the present invention;
FIG. 6 is a schematic structural diagram of a scattering device according to the present invention;
FIG. 7 is a second schematic view of the scattering device according to the present invention;
FIG. 8 is a schematic structural view of a liquid adding device provided by the present invention;
FIG. 9 is a schematic structural view of an ultrasonic shattering apparatus according to the present invention;
fig. 10 is a schematic view of a fixing frame according to the present invention.
Reference numbers in the figures: 1. a first gas storage tank; 2. a pretreatment device; 21. a support; 22. a treatment tank; 23. a cover body; 24. a liquid adding device; 241. a fixed tube; 242. pipe rotation; 243. a liquid spraying pipe; 244. a spray head; 245. an outer gear ring; 246. a second servo motor; 247. a second spur gear; 25. a breaking device; 251. a rotating drum; 252. a first rotating shaft; 253. a first bevel gear; 254. a bevel gear ring; 255. a drive box; 256. a first servo motor; 257. a second bevel gear; 258. a first stirring rod; 259. a second stirring rod; 2510. an inner gear ring; 2511. a second rotating shaft; 2512. a first spur gear; 2513. a third stirring rod; 26. an ultrasonic vibration crushing device; 261. a fixed mount; 2611. concentric rings; 2612. fixing the rod; 262. vibrating the column; 263. a filter screen; 264. an ultrasonic transducer; 265. connecting columns; 266. a protective shell; 27. an exhaust pipe; 28. an annular shunt tube; 29. an air inlet pipe; 210. a gas showerhead; 211. a liquid discharge pipe; 212. a liquid level sensor; 213. a concentration sensor; 3. a condenser; 4. a purifier; 5. a second gas tank; 6. a liquid storage tank.
Detailed Description
The invention is further described with reference to the following figures and embodiments.
Please refer to fig. 1 and fig. 2 in combination, wherein fig. 1 is a schematic diagram of an overall structure provided by the present invention; FIG. 2 is a schematic structural diagram of a pretreatment apparatus according to the present invention; FIG. 3 is a second schematic structural diagram of a pretreatment apparatus according to the present invention; FIG. 4 is a schematic view of a liquid level sensor according to the present invention; FIG. 5 is a schematic view of the internal structure of the pretreatment apparatus according to the present invention; FIG. 6 is a schematic structural diagram of a scattering device according to the present invention; FIG. 7 is a second schematic view of the scattering device according to the present invention; FIG. 8 is a schematic structural view of a liquid adding device provided by the present invention; FIG. 9 is a schematic structural view of an ultrasonic shattering apparatus according to the present invention; fig. 10 is a schematic view of a fixing frame according to the present invention.
In the specific implementation process, as shown in fig. 1, a germane collecting and purifying device comprises a first gas storage tank 1, a condenser 3 and a purifier 4, wherein a pretreatment device 2 is arranged on one side of the first gas storage tank 1, an exhaust port of the first gas storage tank 1 is communicated with the pretreatment device 2 through a pipeline, the condenser 3 is arranged on one side of the pretreatment device 2, the pretreatment device 2 is communicated with an air inlet of the condenser 3 through a pipeline, the purifier 4 is arranged on one side of the condenser 3, an exhaust port of the condenser 3 is communicated with an air inlet of the purifier 4 through a pipeline, a second gas storage tank 5 is arranged on one side of the purifier 4, an exhaust port of the purifier 4 is communicated with an air inlet of the second gas storage tank 5 through a pipeline, a liquid storage tank 6 is arranged on one side of the pretreatment device 2, a liquid inlet of the liquid storage tank 6 is communicated with the pretreatment device 2 through a pipeline, when in use, gas is collected in the first gas storage tank 1, the impurities in the germane gas are subjected to reaction treatment by being placed in a pretreatment device 2, wherein the purity of germane is improved as much as possible by strongly and effectively removing carbon dioxide and acid gas containing chloride ions in the germane gas by using 3-10mol/L strong base solution, such as sodium hydroxide solution or potassium hydroxide solution, the step is a key step of the whole technical scheme of the invention, and the carbon dioxide and the acid gas containing chloride ions in the germane gas can be effectively removed by the design of the technical structure of the invention; enabling the germane gas to enter the condenser 3 for condensation in a relatively pure way, then entering the purifier 4 for thorough purification to obtain purified germane gas, and then entering the second gas storage tank 5 for storage;
referring to fig. 2, 3, 4 and 5, the pretreatment device 2 includes a support 21, a treatment tank 22, a cover 23, a liquid adding device 24, a scattering device 25, an ultrasonic shattering device 26, an exhaust pipe 27, an annular shunt pipe 28, an air inlet pipe 29, an air nozzle 210 and a liquid discharge pipe 211, the support 21 is disposed on one side of a first air storage tank 1, the treatment tank 22 is fixed on the top of the support 21, the cover 23 is fixed on the top of the treatment tank 22 through bolts, the liquid adding device 24 is fixed on the middle portion of the cover 23, the exhaust pipe 27 is fixed on one end of the cover 23, the exhaust pipe 27 is communicated with an air inlet of a condenser 3 through a pipeline, the annular shunt pipe 28 is fixed on the bottom of the inner wall of the treatment tank 22, the air inlet pipe 29 is fixed on one end of the annular shunt pipe 28, one end of the air inlet pipe 29 passes through the treatment tank 22 and is communicated with an air outlet of the first air storage tank 1 through a pipeline, the air nozzle 210 is fixed on the top of the annular shunt pipe 28 at equal distance, the bottom of the treatment tank 22 is fixed with a breaking device 25, the middle part of the inner wall of the treatment tank 22 is fixed with an ultrasonic vibration breaking device 26, the bottom of the treatment tank 22 is fixed with a liquid discharge pipe 211, the liquid discharge pipe 211 is communicated with a liquid inlet of the liquid storage tank 6, a reaction solution is added into the treatment tank 22, germane gas in the first gas storage tank 1 is introduced into the annular shunt pipe 28 through the gas inlet pipe 29 and is sprayed out through the gas spraying head 210, so that the germane gas is contacted with the reaction solution, and impurities in the germane gas, such as carbon dioxide and acid gas containing chlorine ions, are neutralized and reacted through the reaction solution by adopting 3-10mol/L strong base solution, so that the impurities are effectively removed.
Referring to fig. 6 and 7, the breaking device 25 includes a rotating drum 251, a first rotating shaft 252, a first bevel gear 253, a bevel gear ring 254, a driving box 255, a first servo motor 256, a second bevel gear 257, a first stirring rod 258 and a second stirring rod 259, the rotating drum 251 is rotatably connected to the middle of the processing tank 22 through a bearing, the first rotating shaft 252 is rotatably connected to the inner wall of the rotating drum 251 through a bearing, the first bevel gear 253 is fixed to the bottom of the first rotating shaft 252, the bevel gear ring 254 is fixed to the bottom of the rotating drum 251, the driving box 255 is fixed to the bottom of the processing tank 22, the first bevel gear 253 and the bevel gear ring 254 are located on the inner wall of the driving box 255, the first servo motor 256 is fixed to one side of the driving box 255, the second bevel gear 257 is fixed to the output end of the first servo motor 256, the first stirring rod 258 is engaged with the first bevel gear 253 and the bevel gear ring 254, one end of the rotating drum 251 far from the bevel gear ring 254 is fixed at equal distance, a second stirring rod 259 is fixed on one end of the first rotating shaft 252 far away from the first bevel gear 253 at equal intervals; the scattering device 25 further comprises an internal gear ring 2510, a second rotating shaft 2511, a first flat gear 2512 and a third stirring rod 2513, wherein one end of each of the four first stirring rods 258 is fixed with the internal gear ring 2510, one end of each of the second stirring rods 259 is rotatably connected with the second rotating shaft 2511 through a bearing, the bottom of the second rotating shaft 2511 is fixed with the first flat gear 2512, the first flat gear 2512 is meshed with the internal gear ring 2510, one end of the second rotating shaft 2511 far away from the first flat gear 2512 is fixed with the third stirring rod 2513, the first servo motor 256 rotates to drive the second bevel gear 257 to rotate, the bevel gear ring 254 and the first bevel gear 253 can be driven to rotate simultaneously, the rotating directions are opposite, the rotating drum 251 and the first rotating shaft 252 can be driven to rotate reversely, the first stirring rod 258 and the second stirring rod 259 can be driven to stir the reaction solution, and the second rotating shaft 2511 can be driven while the second stirring rod 259 rotates, because the first pinion 2512 on the second pivot 2511 meshes with the internal gear ring 2510 for the rotation of first pinion 2512, and then drives the rotation of third puddler 2513 through second pivot 2511, can improve the stirring effect to the alkali solution of reaction to can break up the bubble of air jet 210 spun, make the bubble can evenly float upwards.
Referring to fig. 9 and 10, the ultrasonic shattering device 26 includes a fixing frame 261, a vibration column 262, a filter screen 263, ultrasonic transducers 264 and a connecting column 265, the fixing frame 261 is fixed in the middle of the inner wall of the treatment tank 22 at equal intervals, the vibration column 262 is fixed in the middle of the three fixing frames 261, the filter screen 263 is fixed on the upper surface of each of the three fixing frames 261, the apertures of the three filter screens 263 are gradually reduced from bottom to top, the ultrasonic transducers 264 are fixed at the bottom of the vibration column 262, wherein the ultrasonic transducers 264 are the conventional ultrasonic transducers and are matched with the supporting appliances such as the ultrasonic generator, which is the prior art that has been disclosed, and is not described in detail in principle, the bottom of the vibration column 262 is fixed with a protective shell 266, the ultrasonic transducers 264 are located on the inner wall of the protective shell 266 to facilitate the protection of the ultrasonic transducers 264, the connecting column 265 is fixed between two adjacent fixing frames 261 at equal intervals, after the bubble drifts upwards, the bubble contacts with filter screen 263, through the aperture on filter screen 263, come to cut the bubble, and the aperture of three filter screen 263 reduces gradually from bottom to top, the gradable is smashed the bubble, and when the bubble misses filter screen 263, send ultrasonic vibration through ultrasonic transducer 264, through vibrations post 262 and mount 261, with high frequency vibrations dispersion to filter screen 263 on, when the bubble passes filter screen 263, will the bubble shatter through high frequency vibrations, can improve the area of contact of bubble and reaction solution greatly, make the alkali solution of reaction have bigger contact surface with germane gas, thereby make in the reaction of impurity with more high-efficient the matter that closes, especially get rid of carbon dioxide's effect repeatedly.
Referring to fig. 3 and 8, the liquid adding device 24 includes a fixed pipe 241, a rotating pipe 242, a liquid spraying pipe 243, a spraying head 244, an outer gear ring 245, a second servo motor 246 and a second flat gear 247, the middle part of the cover 23 is rotatably connected with the fixed pipe 241 through a bearing, the bottom of the fixed pipe 241 penetrates through the cover 23 and is rotatably connected with the rotating pipe 242 through a mechanical seal, the two ends of the rotating pipe 242 are symmetrically fixed with the liquid spraying pipes 243, the spraying heads 244 are fixed at the bottom of the liquid spraying pipes 243 at equal intervals, the outer gear ring 245 is fixed on the outer side of the rotating pipe 242, the top of the cover 23 is fixed with the second servo motor 246, the output end of the second servo motor 246 penetrates through the cover 23 and is fixed with the second flat gear 247, the second flat gear 247 is engaged with the outer gear ring 245, the inner wall of the processing tank 22 is fixed with the liquid level sensor 212 and the concentration sensor 213, wherein, the liquid level sensor 212 and the concentration sensor 213 adopt the existing disclosed technology, in principle, it is not repeated, the fixed pipe 241 continuously injects the reaction solution into the spray pipe 243 and sprays the reaction solution through the spray head 244, so that a large amount of reaction solution mist is distributed in the processing tank 22, germane gas coming out of the reaction solution contacts with the reaction solution mist before entering the exhaust pipe 27, and further effectively contacts with germane gas to improve the reaction effect, and the second servo motor 246 rotates to drive the second flat gear 247 to rotate, and further drives the outer gear ring 245 to rotate, so that the spray pipe 243 on the rotating pipe 242 rotates, so that the mist is distributed more uniformly, and the reaction solution is sprayed out through the spray head 244 and falls into the liquid reaction solution, so that the reaction solution in the processing tank 22 can be supplemented, the concentration of the reaction solution in the processing tank 22 can be kept in a certain reasonable effective range, and the redundant reacted reaction solution is discharged through the liquid discharge pipe 211, so that the proper level of liquid is maintained in the treatment tank 22.
Referring to fig. 10, the fixing frame 261 is composed of three concentric rings 2611, the concentric rings 2611 are connected by fixing rods 2612 which are equidistantly distributed, and the connecting column 265 and the connecting point of the concentric rings 2611 and the fixing rods 2612 are fixedly connected, and are integrated by the concentric rings 2611 and the fixing rods 2612, so that ultrasonic waves can be conveniently transmitted.
The first servo motor 256 and the second servo motor 246 are both speed reduction motors, and by providing a speed reduction mechanism, the output torque can be increased, and the rotation speed can be reduced.
The inner wall of the treatment tank 22 may be provided with more than one heat exchanger or electric heating wire to heat the reaction solution in the treatment tank 22 and increase the reaction rate.
The electric elements in the preprocessing device 2 are controlled by the controller and the single chip, and the circuits and the control related to the present invention are the prior art, which are not described in detail herein.
The invention also comprises a germane collecting and purifying method, which depends on the germane collecting and purifying equipment provided by the invention, and the purifying method comprises the following steps:
1) germane containing impurities is collected in the first gas storage tank 1, pumped into the pretreatment device 2 through a gas pump and uniformly sprayed out through a gas inlet pipe 29 and an annular shunt pipe 28 in the pretreatment device 2;
2) adding a reaction solution into the treatment tank 22, and reacting the reaction solution with impurities in germane gas, wherein the reaction solution is one of 3-10mol/L sodium hydroxide solution or potassium hydroxide solution;
3) after preliminarily treating acid impurities and carbon dioxide in germane through reaction solution, discharging germane gas into a condenser 3 for condensation, dehydrating and adsorbing and cleaning the gas formed after condensation through a purifier 4 to obtain purified germane gas, and introducing the purified germane gas into a second gas storage tank 5 for collection. Most of moisture in the germane crude product can be removed by condensation in the condenser 3, the germane gas enters the purifier 4 after passing through the condenser 3, further dehydration is carried out in the purifier 4, and other impurities such as digermane, chlorogermane, epoxy germane and a small amount of hydrogen are removed. The specific removal scheme is a purification device in the prior art, such as a purification device formed by combining a common absorber for removing the above related impurities and a cold trap for removing hydrogen, and the specific selection of conditions including the molecular sieve used by the absorber can be selected according to specific process conditions and impurity parameters, which belongs to the prior art and is not a technical problem to be solved by the present invention, and therefore, the details are not repeated herein.
The temperature of the reaction solution is between 45 and 80 ℃, and the reaction rate can be improved by increasing the ambient temperature to ensure that the molecules are more active.
The working principle is as follows:
when in use, a reaction solution is added into the processing tank 22, germane gas in the first gas storage tank 1 is introduced into the annular shunt tube 28 through the gas inlet pipe 29 and then is sprayed out through the spray head 210, so that the germane gas contacts with the reaction solution, impurities in the germane gas are neutralized and reacted through the reaction solution, in the process, the first servo motor 256 rotates to drive the second bevel gear 257 to rotate, the bevel gear ring 254 and the first bevel gear 253 can be driven to rotate simultaneously, the rotation directions are opposite, the rotary drum 251 and the first rotary shaft 252 can be driven to rotate reversely, the first stirring rod 258 and the second stirring rod 259 rotate reversely, so that the reaction solution is stirred, the second rotary shaft 2511 is driven to revolve while the second stirring rod 259 rotates, and the first flat gear 2512 on the second rotary shaft 2511 is meshed with the inner gear ring 2510, so that the first flat gear 2512 rotates, and then the third stirring rod 2513 is driven to rotate by the second rotating shaft 2511, so that the stirring effect on the reaction solution can be improved, and bubbles sprayed by the air nozzle 210 can be dispersed, so that the bubbles can uniformly float upwards, after the bubbles float upwards, the bubbles are contacted with the filter screen 263 and cut through small holes on the filter screen 263, the aperture of the three filter screens 263 is gradually reduced from bottom to top, the bubbles can be crushed in a grading manner, the bubbles miss the filter screen 263, and simultaneously generate ultrasonic vibration by the ultrasonic transducer 264, the high-frequency vibration is dispersed on the filter screen 263 through the vibration column 262 and the fixing frame 261, the bubbles are shattered through the high-frequency vibration while passing through the filter screen 263, so that the contact area between the bubbles and the reaction solution can be greatly improved, the reaction solution can effectively react and neutralize impurities in germane gas, and the reaction solution is continuously injected into the liquid spraying pipe 243 through the fixing pipe 241, and is sprayed out through the spray head 244, so that a large amount of reaction solution mist is distributed in the treatment tank 22, germane gas coming out from the reaction solution is in contact with the reaction solution mist before entering the exhaust pipe 27, the reaction effect is further improved, the second flat gear 247 is driven to rotate through the rotation of the second servo motor 246, and then the outer gear ring 245 is driven to rotate, so that the spray pipe 243 on the rotating pipe 242 rotates, the mist is distributed more uniformly, and the reaction solution is sprayed out through the spray head 244 and falls into the liquid reaction solution, so that the reaction solution in the treatment tank 22 can be supplemented, the concentration of the reaction solution in the treatment tank 22 is kept within a certain range, and the redundant reacted reaction solution is discharged through the liquid discharge pipe 211, so that the proper liquid level in the treatment tank 22 is kept.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. The utility model provides a germane collecting and purifying equipment, includes first gas holder (1), condenser (3) and clarifier (4), its characterized in that, first gas holder (1) one side is equipped with preprocessing device (2), and the gas vent of first gas holder (1) passes through pipeline and preprocessing device (2) intercommunication, preprocessing device (2) one side is equipped with condenser (3), preprocessing device (2) pass through the air inlet intercommunication of pipeline and condenser (3), condenser (3) one side is equipped with clarifier (4), and the gas vent of condenser (3) passes through the air inlet intercommunication of pipeline and clarifier (4), clarifier (4) one side is equipped with second gas holder (5), and the gas vent of clarifier (4) passes through the air inlet intercommunication of pipeline and second gas holder (5), preprocessing device (2) one side is equipped with liquid reserve tank (6), and the liquid inlet of the liquid storage tank (6) is communicated with the pretreatment device (2) through a pipeline;
the pretreatment device (2) comprises a support (21), a treatment tank (22), a cover body (23), a liquid adding device (24), a scattering device (25), an ultrasonic vibration and fragmentation device (26), an exhaust pipe (27), an annular shunt pipe (28), an air inlet pipe (29), an air nozzle (210) and a liquid discharge pipe (211), wherein the support (21) is arranged on one side of the first air storage tank (1), the treatment tank (22) is fixed on the top of the support (21), the cover body (23) is fixed on the top of the treatment tank (22) through bolts, the liquid adding device (24) is fixed in the middle of the cover body (23), the exhaust pipe (27) is fixed at one end of the cover body (23), the exhaust pipe (27) is communicated with an air inlet of the condenser (3) through a pipeline, the annular shunt pipe (28) is fixed at the bottom of the inner wall of the treatment tank (22), and the air inlet pipe (29) is fixed at one end of the annular shunt pipe (28), one end of the air inlet pipe (29) penetrates through the treatment tank (22) and is communicated with an air outlet of the first air storage tank (1) through a pipeline, air nozzles (210) are fixed on the top of the annular shunt pipe (28) at equal intervals, a scattering device (25) is fixed at the bottom of the treatment tank (22), an ultrasonic vibration crushing device (26) is fixed in the middle of the inner wall of the treatment tank (22), a liquid discharge pipe (211) is fixed at the bottom of the treatment tank (22), and the liquid discharge pipe (211) is communicated with a liquid inlet of the liquid storage tank (6);
the scattering device (25) comprises a rotary drum (251), a first rotating shaft (252), a first bevel gear (253), a bevel gear ring (254), a driving box (255), a first servo motor (256), a second bevel gear (257), a first stirring rod (258) and a second stirring rod (259), the middle part of the treatment tank (22) is rotatably connected with the rotary drum (251) through a bearing, the inner wall of the rotary drum (251) is rotatably connected with the first rotating shaft (252) through a bearing, the bottom of the first rotating shaft (252) is fixedly provided with the first bevel gear (253), the bottom of the rotary drum (251) is fixedly provided with the bevel gear ring (254), the bottom of the treatment tank (22) is fixedly provided with the driving box (255), the first bevel gear (253) and the bevel gear ring (254) are positioned on the inner wall of the driving box (255), one side of the driving box (255) is fixedly provided with the first servo motor (256), and the output end of the first servo motor (256) is fixedly provided with the second bevel gear (257), and the second bevel gear (257) is meshed with the first bevel gear (253) and the bevel gear ring (254), a first stirring rod (258) is fixed at one end of the rotating drum (251) far away from the bevel gear ring (254) at equal intervals, and a second stirring rod (259) is fixed at one end of the first rotating shaft (252) far away from the first bevel gear (253) at equal intervals.
2. The germane collecting and purifying device according to claim 1, wherein the scattering device (25) further comprises an inner gear ring (2510), a second rotating shaft (2511), a first flat gear (2512) and a third stirring rod (2513), the inner gear ring (2510) is fixed at one end of each of the four first stirring rods (258), the second rotating shaft (2511) is rotatably connected at one end of each of the second stirring rods (259) through a bearing, the first flat gear (2512) is fixed at the bottom of each of the second rotating shafts (2511), the first flat gear (2512) is meshed with the inner gear ring (2510) and the third stirring rod (2513) is fixed at one end, far away from the first flat gear (2512), of each of the second rotating shafts (2511).
3. Purification equipment is collected to germane of claim 1, characterized in that, ultrasonic wave shakes garrulous device (26) and includes mount (261), vibrations post (262), filter screen (263), ultrasonic transducer (264) and spliced pole (265), it is fixed with mount (261), three to handle jar (22) inner wall middle part equidistance the mount (261) middle part is fixed with vibrations post (262), three mount (261) upper surface is fixed with filter screen (263) respectively, and three the aperture of filter screen (263) is the setting of dwindling gradually from bottom to top, vibrations post (262) bottom is fixed with ultrasonic transducer (264), adjacent two equidistance between mount (261) is fixed with spliced pole (265).
4. The germane collecting and purifying equipment according to claim 1, wherein the liquid adding device (24) comprises a fixed pipe (241), a rotating pipe (242), a liquid spraying pipe (243), a spraying head (244), an outer gear ring (245), a second servo motor (246) and a second flat gear (247), the middle part of the cover body (23) is rotatably connected with the fixed pipe (241) through a bearing, the bottom of the fixed pipe (241) penetrates through the cover body (23) and is rotatably connected with the rotating pipe (242) through mechanical sealing, the two ends of the rotating pipe (242) are symmetrically fixed with the liquid spraying pipes (243), the bottom of the liquid spraying pipe (243) is equidistantly fixed with the spraying head (244), the outer gear ring (245) is fixed on the outer side of the rotating pipe (242), the top of the cover body (23) is fixed with the second servo motor (246), the output end of the second servo motor (246) penetrates through the cover body (23) and is fixed with the second flat gear (247), and the second flat gear (247) is in meshed connection with the outer gear ring (245).
5. The germane collecting and purifying apparatus according to claim 3, wherein the fixing frame (261) is composed of three concentric rings (2611), the concentric rings (2611) are connected by fixing rods (2612) which are distributed at equal intervals, and the connecting column (265) and the connection points of the concentric rings (2611) and the fixing rods (2612) are fixedly connected.
6. The germane collecting and purifying device according to claim 5, wherein a protective shell (266) is fixed at the bottom of the vibration column (262), and the ultrasonic transducer (264) is positioned on the inner wall of the protective shell (266).
7. The germane collecting and purifying apparatus according to claim 1, wherein a liquid level sensor (212) and a concentration sensor (213) are fixed on the inner wall of the processing tank (22).
8. The germane collecting and purifying apparatus according to claim 4, wherein the first servo motor (256) and the second servo motor (246) are each a reduction motor.
9. A germane collection and purification method based on the germane collection and purification apparatus according to any one of claims 1 to 8, wherein the purification method comprises:
1) germane containing impurities is collected in the first gas storage tank (1), pumped into the pretreatment device (2) through a gas pump and uniformly sprayed out through a gas inlet pipe (29) and an annular shunt pipe (28) in the pretreatment device (2);
2) adding a reaction solution into the treatment tank (22), and reacting the reaction solution with impurities in germane gas, wherein the reaction solution is one of 3-10mol/L sodium hydroxide solution or potassium hydroxide solution;
3) after the acidic impurities in the germane are preliminarily treated by the reaction solution, the germane gas is discharged into a condenser (3) for condensation, then the gas formed after condensation is dehydrated, adsorbed and cleaned by a purifier (4), the purified germane gas is obtained, and the purified germane gas is introduced into a second gas storage tank (5) for collection.
10. The germane collection and purification method according to claim 9, wherein the temperature of the reaction solution is between 45 ° and 80 °.
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| CN114832600B (en) * | 2022-04-02 | 2023-07-25 | 山西六建集团有限公司 | Be used for building construction carbon neutralization emission treatment facility |
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