CN214734580U - System for preparing high-purity nano aluminum oxide - Google Patents
System for preparing high-purity nano aluminum oxide Download PDFInfo
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- CN214734580U CN214734580U CN202120873226.8U CN202120873226U CN214734580U CN 214734580 U CN214734580 U CN 214734580U CN 202120873226 U CN202120873226 U CN 202120873226U CN 214734580 U CN214734580 U CN 214734580U
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Abstract
The utility model discloses a system for preparing high-purity nanometer alumina relates to alumina preparation technical field, and wherein, the system for preparing high-purity nanometer alumina includes: electrolyte circulation system, aluminium air battery group and aluminium oxide recovery system, electrolyte circulation system with aluminium air battery group intercommunication, electrolyte circulation system with aluminium oxide recovery system intercommunication. The utility model has the advantages that the high-purity nanometer alumina is obtained, and the stable output power is obtained, and 4-4.5 kWh power can be discharged per kilogram of aluminum; the preparation process is short, and the process is environment-friendly and clean; 2 kg of high-purity alumina can be produced per kg of high-purity aluminum.
Description
Technical Field
The utility model relates to an aluminium oxide prepares technical field, and more specifically the system that relates to a preparation high-purity nanometer aluminium oxide that says so.
Background
High purity alumina refers to alumina with a minimum purity of 99.99%, formula Al2O3It is a white solid insoluble in water, odorless, tasteless, extremely hard, and easily hygroscopic without deliquescing (burned without hygroscopic), and is an amphoteric oxide, soluble in inorganic acid and alkaline solutions, and practically insoluble in water and nonpolar organic solvents.
In the prior art, high-purity nano alumina is prepared by discharging through an aluminum-air battery, but the existing device and method have the problems of low efficiency of preparing high-purity alumina and electrochemical pollution.
Therefore, how to provide a system for preparing high-purity nano alumina, which can improve the preparation efficiency of high-purity alumina and reduce electrochemical pollution, is a problem to be solved by those skilled in the art.
SUMMERY OF THE UTILITY MODEL
The purpose of the present invention is to solve at least one of the above mentioned technical drawbacks.
In order to achieve the above objects, a first object of the present invention is to provide a system for preparing high purity nano alumina, comprising: electrolyte circulation system, aluminium air battery group and aluminium oxide recovery system, electrolyte circulation system with aluminium air battery group intercommunication, electrolyte circulation system with aluminium oxide recovery system intercommunication.
Further, the aluminum-air battery pack comprises a plurality of aluminum-air single batteries which are connected in series or in parallel.
Further, every aluminium air cell includes casing, electrolyte, positive pole electrode, negative pole electrode, positive pole utmost point ear, negative pole utmost point ear, inlet, liquid outlet, air inlet and gas vent, the casing includes casing and lower casing, go up the casing with the connection can be dismantled to the casing down, positive pole utmost point ear, air inlet and gas vent are located go up the top of casing, inlet, negative pole utmost point ear are located respectively the both sides of casing down, the liquid outlet is located the bottom of casing down.
Furthermore, the electrolyte circulating system comprises a liquid storage tank, a liquid pump, a storage battery, a liquid distributor and an electrolyte waste liquid tank, wherein the liquid distributor is communicated with the liquid inlet of the aluminum air single battery at the head end of the aluminum air battery pack through a liquid inlet pipeline, the liquid inlet pipeline is provided with the liquid pump, the aluminum air battery pack is communicated with the electrolyte waste liquid tank through a liquid outlet pipeline at the tail end of the aluminum air battery pack, a filter screen is arranged between the liquid outlet pipeline and the electrolyte waste liquid tank, the electrolyte waste liquid tank is communicated with the liquid pump, and the storage battery is respectively electrically connected with the liquid pump and the aluminum air battery pack.
Further, the system for preparing high-purity nano aluminum oxide also comprises a gas purification device, wherein the gas purification device is communicated with the gas inlet of the aluminum air single battery at the head end in the aluminum air battery pack.
Further, the system for preparing the high-purity nano aluminum oxide further comprises an electric control system, wherein the liquid outlet is provided with an electromagnetic valve, and the electric control system is respectively and electrically connected with the electromagnetic valve and the liquid pump.
Further, the system for preparing the high-purity nano aluminum oxide also comprises a heat exchange device, wherein the heat exchange device is arranged at the bottom of the aluminum air battery pack and is used for assisting the aluminum air battery pack in heat dissipation.
According to the technical scheme, compared with the prior art, the utility model discloses a system for preparing high-purity nano alumina, which obtains high-purity nano alumina and stable output power, and can emit 4-4.5 kWh of power per kilogram of aluminum; the preparation process is short, and the process is environment-friendly and clean; 2 kg of high-purity alumina can be produced per kg of high-purity aluminum.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a system for preparing high-purity nano alumina, which is provided by the present invention, for preparing precipitates and reacting residual electrolyte;
fig. 2 is a schematic structural diagram of an electrolyte circulation system provided by the present invention;
fig. 3 is a schematic structural diagram of an aluminum-air cell provided by the present invention;
FIG. 4 is a process flow chart of preparing high purity alumina from the precipitate and the residual electrolyte.
Wherein: 1 is a gas purification device; 2 is an aluminum air battery pack; 21 is an aluminum air single battery; 211 is an anode tab; 212 is an air inlet; 213 is an exhaust hole; 214 is a cathode tab; 215 is a liquid inlet; 216 is a liquid outlet; 3 is a membrane separation device; 4 is an exhaust gas discharge device; 5 is a liquid pump; 6 is a heat exchange device; 7 is a liquid storage tank; 8 is an alumina recovery system; 9 is an electric control system; 10 is a storage battery; 11 is a liquid separator; 12 is a filter screen; 13 is an electrolyte waste liquid box; 14 is a reaction residual electrolyte reaction device; 15 is a precipitate reaction device; 16 is a magnetic stirring reaction kettle; 17 is a vacuum filtration device; 18 is an oven; 19 is an industrial calciner.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Referring to fig. 1-3, the embodiment of the utility model discloses a system for preparing high-purity nanometer alumina, including electrolyte circulation system, aluminium air battery 2, aluminium oxide recovery system 8, gas purification device 1, electrical system 9 and heat exchange device 6.
Wherein, the aluminum-air battery pack 2 comprises a plurality of aluminum-air single batteries 21, the plurality of aluminum-air single batteries 21 are connected in series or in parallel to form the aluminum-air battery pack 2, in this embodiment, the aluminum-air battery pack 2 is formed by connecting a plurality of aluminum-air single batteries 21 in series, each aluminum-air single battery 21 comprises a shell, electrolyte, an anode electrode, a cathode electrode, an anode tab, a cathode tab, a liquid inlet, a liquid outlet, an air inlet and an air outlet, the shell comprises an upper shell and a lower shell, the upper shell and the lower shell are detachably connected, the anode tab, the air inlet and the air outlet are positioned above the upper shell, the liquid inlet and the cathode tab are respectively positioned at two sides of the lower shell, the liquid outlet is positioned at the bottom of the lower shell, the electrolyte is high-purity NaOH or high-purity KOH and high-purity water to prepare high-purity NaOH or alkaline KOH solution, in this embodiment, the electrolyte is preferably a KOH solution.
Electrolyte circulation system includes liquid reserve tank 7, liquid pump 5, battery 10, knockout 11, electrolyte waste liquid case 13, all aluminium air battery cells 21's in knockout 11 and the aluminium air battery group 2 inlet communicates through the feed liquor pipeline one by one, be equipped with liquid pump 5 on the feed liquor pipeline, all aluminium air battery cells 21's in the aluminium air battery group 2 liquid outlet and electrolyte waste liquid case 13 communicate through the liquid outlet pipeline, be equipped with filter screen 12 between liquid outlet pipeline and the electrolyte waste liquid case 13, electrolyte waste liquid case 13 and liquid pump 5 intercommunication, battery 10 respectively with liquid pump 5 and 2 electric connection of aluminium air battery group, wherein, all aluminium air battery cells 21's in the aluminium air battery group 2 gas vent collects and is connected with membrane separator 3, membrane separator 3 is connected with exhaust 4.
The air inlet intercommunication of the aluminium air battery cell 21 of head end in gas purification device 1 and the aluminium air battery group 2, electrical system 9 respectively with solenoid valve and liquid pump 5 electric connection, heat exchange device 6 locates the bottom of aluminium air battery group 2 for give the heat dissipation of aluminium air battery group 2.
In the above embodiment, the storage battery 10 is a lead-acid storage battery, and after the switch of the aluminum-air battery pack 2 is turned on, the lead-acid storage battery 10 supplies power to the liquid pump 5, and the electrolyte in the liquid storage tank 7 is uniformly distributed by the distributor 11 and injected into each aluminum-air single battery 21. The liquid outlet 216 of each aluminum air cell 21 is opened for a period of time, so that a certain amount of liquid is stored in the electrolyte waste liquid tank 13 for the subsequent electrolyte circulation operation.
After a few minutes, the reaction rate reaches a maximum, after which the reaction rate is maintained at a steady higher level. At this time, the electromagnetic valve at the liquid outlet 216 below each aluminum air cell 21 is controlled to be opened to a small extent by the electronic control system 9, and the liquid pump 5 works at the same time, so that the electrolyte in the waste liquid tank is input into each aluminum air cell 21 through the liquid separator 11, and at this time, the liquid inlet rate is the same as the liquid discharge rate. The liquid pump 5 can be operated at a lower power in this process. During operation, the lead-acid battery 10 can be charged when the aluminum-air battery pack 2 is under a light load and there is power redundancy. Because the electrolyte is filtered by the filter screen 12, impurities generated by reaction can be effectively removed in the circulation process of the electrolyte, and the inner space of the battery monomer is also flushed. In addition, a hydroxyl ion concentration sensor is arranged at the liquid outlet 216 of the aluminum air single battery 21, and when the concentration of the electrolyte does not support the rapid progress of the battery reaction, new electrolyte is pumped from the liquid storage tank 7 for replacement.
In a low-temperature environment, in consideration of the problem of quick start of the aluminum air single cell 21, a heating device, such as a heating wire or a heating sheet, may be added to the liquid separation device. After the start switch is turned on, if the ambient temperature is low, the heating device is started to heat the electrolyte, and the heated electrolyte is injected into each aluminum air single cell 21. After a certain period of reaction time, the heating device stops working after the proper reaction temperature is reached due to the exothermic heat of reaction. The heat generated by the reaction then maintains the nominal power operation of the aluminum air battery 2.
In order to maintain the rated output power, the initial concentration of KOH electrolyte is higher than 4 mol/L. Although the reaction rate does not drop significantly when the hydroxide concentration is low, the change in output power can be used as a prompt for changing the plate. During the reaction process, the amount of the electrolyte should be proper, and if the amount of the electrolyte is too high, the redundant weight is too high, and the overall power density of the aluminum-air battery pack 2 is reduced.
In the above embodiment, the alumina recovery system 8 collects the precipitate and the reaction residual electrolyte generated during the discharge of the aluminum-air battery 2, wherein the main component of the precipitate is aluminum hydroxide, and the main component of the reaction residual electrolyte is potassium aluminate.
Referring to fig. 4, the present example illustrates the system for preparing high purity nano alumina disclosed above by a method for preparing high purity nano alumina, which includes the treatment of the precipitate and the treatment of the reaction residual electrolyte.
Wherein the content of the first and second substances,
the treatment of the precipitate recovered by the alumina recovery system 8 comprises the following steps:
firstly, dissolving the precipitate in the precipitate reaction device 15 by concentrated sulfuric acid, crystallizing to obtain aluminum sulfate, and preparing the prepared aluminum sulfate into 0.2mol/L solution;
preparing 2.0mol/L ammonium carbonate solution, adding a certain amount of dispersant into the 2.0mol/L ammonium carbonate solution, slowly adding the prepared 0.2mol/L aluminum sulfate solution into the ammonium carbonate solution, stirring the mixture for 1 hour by using a magnetic stirring reaction kettle 16 after the addition is finished, then aging the mixture, and performing suction filtration by using a vacuum suction filtration device 17; in the suction filtration process, washing the precipitate for several times by using distilled water, then washing the precipitate for several times by using absolute ethyl alcohol, and putting the filter cake obtained by suction filtration into an oven 18 for drying to obtain an ammonium aluminum carbonate precursor;
finally, calcining the mixture by an industrial calcining furnace 19 to obtain monodisperse alpha-Al2O3Wherein, the calcination comprises distributed calcination, low-temperature calcination is carried out for 60-90 minutes at about 300 ℃, and then high-temperature calcination is carried out for 90-120 minutes at the temperature rising rate of 20 ℃ per minute and the temperature rising rate of 1200 ℃, thus obtaining the monodisperse alpha-Al2O3。
The treatment of the residual reaction electrolyte recovered by the alumina recovery system 8 comprises the following steps:
the treatment is carried out in a reaction residual electrolyte reaction device 14, first of all in the presence of a main component ofAdding excessive calcium oxide into the residual electrolyte solution of potassium aluminate reaction, reacting calcium oxide with potassium aluminate solution to generate calcium hydroxide, and reacting calcium hydroxide with potassium aluminate to generate hydrated calcium aluminate (3 CaO. Al)2O3·6H2O), SiO in solution2(OH)2 2-The ions react on the surface layer of the hydrated calcium aluminate to generate hydrated garnet sediment, and the silicon impurities in the solution are removed; after removing silicon impurities, adding a proper amount of sodium sulfide into the solution, and reacting sulfur ions with zinc ions in the solution to generate zinc sulfide precipitate so as to remove zinc ions; adding sodium oxalate into the solution, stirring, and filtering to remove magnesium oxalate and calcium salt precipitates; finally obtaining the potassium aluminate solution after impurity removal.
Then, stirring the potassium aluminate solution after impurity removal in a magnetic stirring reaction kettle 16, raising the temperature to a specified temperature, adding seed crystals, mixing and stirring, and introducing CO at a certain flow rate2，N2The mixed gas of (2) to increase the supersaturation degree of the solution and promote the decomposition of the solution into two products of aluminum hydroxide and potassium carbonate; stopping ventilation after the decomposition is finished, and performing vacuum filtration by using a vacuum filtration device 17 to perform solid-liquid separation; washing the aluminum hydroxide filter cake with deionized water and then drying;
dissolving the obtained aluminum hydroxide filter cake by using concentrated hydrochloric acid or concentrated sulfuric acid to obtain aluminum salt; al (B) is3+Salt solution is dropped into NH4HCO3Reacting in the solution to generate aluminum ammonium carbonate; after precipitating the ammonium aluminum carbonate, drying the ammonium aluminum carbonate in the oven 18, calcining and pyrolyzing the dried ammonium aluminum carbonate in the industrial calciner 19 at high temperature to finally generate alumina particles which do not agglomerate, are uniformly distributed, have refined grains and have the grain diameter of about 50 nm.
And sanding the generated alumina, thinning the granularity, and drying the sanded alumina to obtain the nano alumina finished product.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. A system for preparing high-purity nano alumina is characterized by comprising the following components: electrolyte circulation system, aluminium air battery and aluminium oxide recovery system, electrolyte circulation system with aluminium air battery intercommunication, electrolyte circulation system with aluminium oxide recovery system intercommunication, aluminium air battery includes a plurality of aluminium air battery cell, and is a plurality of aluminium air battery cell is established ties or connects in parallel, every aluminium air battery cell includes casing, electrolyte, anode electrode, cathode electrode, anode tab, cathode tab, inlet, liquid outlet, air inlet and gas vent, the casing includes casing and lower casing, go up the casing with the connection can be dismantled to the casing down, anode tab, air inlet and gas vent are located the top of last casing, inlet, cathode tab are located respectively the both sides of casing down, the liquid outlet is located the bottom of casing down, electrolyte circulation system includes liquid reserve tank, aluminium air battery, Liquid pump, battery, knockout and electrolyte waste liquid case, the knockout with head end in the aluminium air battery group the inlet of aluminium air battery cell passes through the feed liquor pipeline intercommunication, is equipped with on the feed liquor pipeline the liquid pump, terminal in the aluminium air battery group the liquid outlet of aluminium air battery cell with the electrolyte waste liquid case passes through the liquid outlet pipeline intercommunication, the liquid outlet pipeline with be equipped with the filter screen between the electrolyte waste liquid case, the electrolyte waste liquid case with the liquid pump intercommunication, the battery respectively with the liquid pump with aluminium air battery group electric connection.
2. The system for preparing high-purity nano aluminum oxide according to claim 1, further comprising a gas purification device, wherein the gas purification device is communicated with the gas inlet of the aluminum air single cell at the head end of the aluminum air battery pack.
3. The system for preparing high-purity nano aluminum oxide according to claim 1, further comprising an electric control system, wherein the liquid outlet is provided with an electromagnetic valve, and the electric control system is electrically connected with the electromagnetic valve and the liquid pump respectively.
4. The system for preparing high-purity nano aluminum oxide according to claim 1, further comprising a heat exchange device, wherein the heat exchange device is arranged at the bottom of the aluminum-air battery pack and is used for assisting the aluminum-air battery pack in dissipating heat.
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| CN113120932A (en) * | 2021-04-26 | 2021-07-16 | 济南易航新材料科技有限公司 | System and method for preparing high-purity nano aluminum oxide |
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