CN102925915B - A kind of method that electrochemical production is nano alumina powder jointed - Google Patents
A kind of method that electrochemical production is nano alumina powder jointed Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000000843 powder Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 32
- 238000005406 washing Methods 0.000 claims abstract description 23
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 19
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 9
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 claims description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000013078 crystal Substances 0.000 claims description 26
- 239000003792 electrolyte Substances 0.000 claims description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000004381 surface treatment Methods 0.000 claims description 11
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 10
- 239000011975 tartaric acid Substances 0.000 claims description 10
- 235000002906 tartaric acid Nutrition 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- HTZCNXWZYVXIMZ-UHFFFAOYSA-M benzyl(triethyl)azanium;chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC1=CC=CC=C1 HTZCNXWZYVXIMZ-UHFFFAOYSA-M 0.000 claims description 6
- KXHPPCXNWTUNSB-UHFFFAOYSA-M benzyl(trimethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1=CC=CC=C1 KXHPPCXNWTUNSB-UHFFFAOYSA-M 0.000 claims description 6
- 150000002891 organic anions Chemical class 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- AJBWDFPJLDDEPQ-UHFFFAOYSA-N 1-(1-bromoethyl)-3-(trifluoromethyl)benzene Chemical compound CC(Br)C1=CC=CC(C(F)(F)F)=C1 AJBWDFPJLDDEPQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 3
- 235000019743 Choline chloride Nutrition 0.000 claims description 3
- OCBHHZMJRVXXQK-UHFFFAOYSA-M benzyl-dimethyl-tetradecylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 OCBHHZMJRVXXQK-UHFFFAOYSA-M 0.000 claims description 3
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 3
- 229960003178 choline chloride Drugs 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 239000003093 cationic surfactant Substances 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 239000004480 active ingredient Substances 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002848 electrochemical method Methods 0.000 description 3
- 150000007522 mineralic acids Chemical class 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- HSEYYGFJBLWFGD-UHFFFAOYSA-N 4-methylsulfanyl-2-[(2-methylsulfanylpyridine-3-carbonyl)amino]butanoic acid Chemical compound CSCCC(C(O)=O)NC(=O)C1=CC=CN=C1SC HSEYYGFJBLWFGD-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses a kind of method that electrochemical production is nano alumina powder jointed, the method adopts after electrolysis of aluminum, its electrolysate is obtained 10 ~ 90nm through washing, hydrothermal treatment consists, washing, drying and calcining nano alumina powder jointed.The present invention, by the adjustment of electric current, voltage and pH and adopt hydrothermal technology, achieves the effective control to alumina particle.The nano alumina powder jointed preparation technology of the inventive method gained is simple, with short production cycle; Productive rate is high, and product stability is good; Environmentally safe.Prepared by the present invention is nano alumina powder jointedly widely used in multiple fields such as military project, automobile, metallurgy, chemical industry, pottery.
Description
Technical Field
The invention relates to a preparation method of alumina, in particular to a method for preparing nano alumina powder by an electrochemical method.
Background
The nanometer alumina is an ultrafine particle with the particle size of 1-100 nm, has extremely strong volume effect, quantum size effect, surface effect and macroscopic quantum tunneling effect, has excellent characteristics in the aspects of high strength, high hardness, wear resistance, corrosion resistance, high temperature resistance and the like, and is widely applied to a plurality of fields such as military industry, automobiles, metallurgy, chemical industry, ceramics and the like as a novel functional material and a novel structural material at present. In recent years, a great deal of documents report that the application of nano-alumina in composite electroplating, fluorescent materials, infrared absorption materials and the like makes a great breakthrough. However, the preparation technology of nano alumina still appears to be slow compared with the application, and still has a plurality of technical problems, which cause unstable product performance and uneven particle size and shape.
Through the literature search of the prior art, various methods for preparing the nano-alumina are found, such as a mechanochemical method, a plasma method, a sol-gel method, a precipitation method, an aluminum ammonium sulfate pyrolysis method, an alkoxide hydrolysis method and the like are disclosed in the prior patent. These methods have various characteristics, but also have some disadvantages, such as high raw material preparation cost, complex process operation, environmental pollution, etc. In addition, the prior art also discloses a technical scheme for preparing nano-alumina by adopting electrochemistry, such as: "electrochemical preparation of ultrafine nanopowder of nano alumina" published in science and technology and engineering 2003,5(3),438-440, which uses aluminum trichloride as an aluminum source, adds ammonia water after electrolysis to gelatinize the solution sol, and then washes, dries and calcines to obtain the nano alumina powder. 2006,13(6), 1798-. Although the methods are all nano-alumina prepared by adopting an electrochemical method, the methods have the defects of high raw material cost and low product efficiency. In view of the above, the present invention is particularly proposed.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the preparation method of the nano-alumina, which has the advantages of low cost, simple experimental conditions, no environmental pollution and easy industrial production.
The technical scheme adopted by the invention for solving the technical problem is as follows: the preparation method comprises the steps of simultaneously taking the aluminum plate after surface treatment as a cathode and an anode to carry out electrolytic reaction; and washing, hydro-thermal treatment, washing, drying and calcining the obtained electrolysis product to obtain the nano aluminum oxide powder.
In the technical scheme of the preparation method: the surface treatment comprises the following steps: firstly, cleaning the surface of the raw material aluminum by using alkali liquor, and then cleaning the surface of the raw material aluminum by using low-concentration inorganic acid. Wherein the inorganic acid is selected from one of hydrochloric acid, nitric acid and sulfuric acid, and the concentration range of the inorganic acid is 0.05-0.5 mol/L; the alkali liquor is selected from one of sodium hydroxide and potassium hydroxide, and the concentration range of the alkali liquor is 0.5-2.5 g/L.
In the preparation method, the effective component in the electrolyte adopted by the electrolysis reaction is 50-500 g/L of cationic surfactant with 5-25 carbon atoms, and the surfactant is any one of choline chloride, benzyltrimethylammonium chloride, beta-methylcholine chloride, benzyltriethylammonium chloride and benzyldimethyltetradecylammonium chloride.
In the preparation method, the electrolysis reaction adopts a direct current power supply.
In the preparation method, the electrolysis is carried out at the pH of 6-10 and the current density of 1-5A/dm2The temperature is 30-90 ℃, and the air supply amount of mechanical stirring or air stirring is 100-3000L/min.
In the electrolytic reaction, when the content of an electrolytic product, namely white aluminum hydroxide powder, in the electrolyte is 3-30%, the electrolyte is filtered and separated, for example, the aluminum hydroxide powder is dynamically separated, and the filtrate is recycled. In this step, the separation of the electrolysis product may be carried out by a separation method known to those skilled in the art.
In the preparation method of the invention, the hydrothermal treatment comprises the following steps: putting the electrolysis product aluminum hydroxide powder into a high-pressure container, adding pure water, seed crystals and organic anions, and carrying out hydrothermal treatment at a constant temperature of 100-300 ℃ and a pressure of 1-87 kg for 1-48 h; wherein the amount of the pure water is 1-8 times of the weight of the aluminum hydroxide powder; the dosage of the organic anion is 0.5 per mill to 10 percent of the weight of the aluminum hydroxide powder.
In the hydrothermal treatment, the seed crystal is nano alumina powder with the particle size of 5-100 nm, and the adding amount of the seed crystal is 1 per thousand-10% of the weight of the aluminum hydroxide powder.
In the preparation method of the invention, the organic anion is one of tartaric acid or citric acid. The washing in the present invention means washing the hydrothermally treated aluminum hydroxide powder with pure water, and the washing water can be recycled after treatment.
In the preparation method of the invention, the calcination conditions are as follows: calcining for 3-15 h at 600-1400 ℃ to obtain the nano alumina.
In the preparation method, the pure water is water with the resistivity range of 2-10M omega cm.
As a best mode for carrying out the invention, the following preparation method is preferably adopted in the invention: the aluminum plate after surface treatment is simultaneously used as a cathode and an anode and is placed in electrolyte containing 400g/L of benzyltrimethylammonium chloride at the pH of 8-10; current density 1A/dm2The temperature is 30 ℃, and the air feeding amount is 100L/min. When the powder content in the electrolyte reaches 25%, filtering the bath solution to obtain aluminum hydroxide powder; washing the aluminum hydroxide powder, putting the washed aluminum hydroxide powder into a high-pressure container, adding pure water, seed crystals and tartaric acid accounting for 5 percent of the weight of the aluminum hydroxide powder, and keeping the temperature for 1 hour under the conditions that the temperature is 100 ℃ and the pressure is 30 kg. Taking out, washing with water, drying, and calcining at 1000 ℃ for 6h to obtain the nano-alumina powder.
By adopting the technical scheme, the nano-alumina prepared by the invention has the particle size distribution of 10-90 nm and the specific surface area of 20-120 cm3/g。
Compared with the prior art, the invention has the following beneficial effects:
1. the effective control of the alumina grain diameter is realized by adjusting current, voltage and pH and adopting a hydrothermal treatment technology.
2. The average grain diameter of the prepared nano alumina powder is 10-90 nm.
3. The reagent used in the preparation process of the nano-alumina powder is an organic component with small volatility, does not contain inorganic additives, is more environment-friendly, and simultaneously does not introduce impurity elements.
4. The pure water used in the preparation process of the nano-alumina powder can be recycled, no large amount of waste residues, waste gases and waste water are discharged, and the method is extremely favorable for environmental protection and belongs to an environment-friendly process.
5. The invention has the advantages of simple preparation process, short production period, lower production cost, strong scale benefit and convenient production expansion.
Detailed Description
Example 1
The preparation method of the nano alumina of the embodiment is carried out according to the following steps:
the aluminum plate after surface treatment is simultaneously used as a cathode and an anode and is placed in benzyltrimethylammonium chloride electrolyte with the content of 200g/L, the pH value is 7-8, and the current density is 3A/dm2The electrolytic aluminum plate is carried out under the conditions that the temperature is 60 ℃ and the air feeding amount is 800L/min through air stirring. When the precipitation content in the electrolyte reaches 28%, filtering the bath solution to obtain aluminum hydroxide powder; washing the aluminum hydroxide powder, putting the washed aluminum hydroxide powder into a high-pressure container, and adding pure water, seed crystals and citric acid accounting for 5% of the weight of the filter cake; carrying out hydrothermal treatment for 6h at the constant temperature of 200 ℃ and the pressure of 12 kg; wherein the amount of the pure water is 4 times of the weight of the aluminum hydroxide powder; the seed crystal is nano alumina powder with the grain diameter of 50nm, and the adding amount of the seed crystal is 50 percent of the weight of the aluminum hydroxide powder. The amount of tartaric acid is 6% of the weight of the aluminum hydroxide powder. After hydrothermal treatment, the mixture is taken out, washed by water, dried and calcined for 6 hours at 1250 ℃ to obtain the nano alumina powder.
The nanometer alumina obtained by the preparation process has a particle size of 40nm and a specific surface area of 45m2/g。
Example 2
The preparation method of the nano alumina of the embodiment is carried out according to the following steps:
the aluminum plate after surface treatment is simultaneously used as a cathode and an anode and is placed in an electrolyte containing 400g/L of choline chloride, and the pH value is 8-10, and the current density is 1A/dm2The temperature is 30 ℃, and the air feeding amount is 100L/min. When the precipitation content in the electrolyte reaches 25%, filtering the bath solution to obtain aluminum hydroxide powder; washing aluminum hydroxide powder, putting the washed aluminum hydroxide powder into a high-pressure container, adding pure water, seed crystals and citric acid accounting for 5 percent of the weight of the aluminum hydroxide powder, and carrying out hydrothermal treatment at the constant temperature of 100 ℃ and the constant pressure of 10kg for 1 hour; wherein the amount of the pure water is 3 times of the weight of the aluminum hydroxide powder; the seed crystal is nano alumina powder with the grain diameter of 5nm, and the adding amount of the seed crystal is 1 per mill of the weight of the aluminum hydroxide powder. The amount of citric acid is 6% of the weight of the aluminum hydroxide powder. Taking out after hydrothermal treatment, washing with water, drying, and calcining at 1000 ℃ for 10h to obtain the nano Al2O3And (3) powder.
The nano alumina powder prepared by the embodiment has the particle diameter of 50nm basically, the particles are dispersed and have uniform size, and the specific surface area is 35m2/g。
Example 3
The preparation method of the nano alumina of the embodiment is carried out according to the following steps:
the aluminum plate after surface treatment is simultaneously used as a cathode and an anode and is placed in electrolyte containing benzyltriethylammonium chloride with the content of 400g/L at the pH value of 8-10 and the current density of 5A/dm2The temperature is 90 ℃, and the air stirring air supply quantity is 1000L/min. When the content of aluminum hydroxide powder in the electrolyte reaches 30%, filtering the bath solution to obtain aluminum hydroxide powder; washing aluminum hydroxide powder, putting into a high-pressure container, and adding pure waterTartaric acid accounting for 10 percent of the weight of the seed crystal and the aluminum hydroxide powder at the temperature of 300 ℃; carrying out hydrothermal treatment for 30 hours at the constant temperature under the pressure of 87 kg; wherein the amount of the pure water is 5 times of the weight of the aluminum hydroxide powder; the seed crystal is nano alumina powder with the grain diameter of 100nm, and the adding amount of the seed crystal is 10 percent of the weight of the aluminum hydroxide powder. The amount of tartaric acid was 2% by weight of the aluminum hydroxide powder. After hydrothermal treatment, the product is taken out, washed by pure water, dried and calcined for 10 hours at 1300 ℃ to obtain the nano Al2O3And (3) powder.
The nano-alumina powder prepared by the embodiment has the particle size of 90nm and the specific surface area of 22m2/g。
Example 4
The preparation method of the nano alumina of the embodiment is carried out according to the following steps:
the raw material aluminum plate after surface treatment is simultaneously used as a cathode and an anode and is placed in beta-methyl choline chloride electrolyte with the content of 50g/L, and the pH value is 7-8, and the current density is 3A/dm2The electrolytic aluminum plate was carried out at a temperature of 60 ℃ under conditions of air stirring and air supply of 3000L/min. When the precipitation content in the electrolyte reaches 3%, filtering the bath solution to obtain aluminum hydroxide powder; washing aluminum hydroxide powder, putting the washed aluminum hydroxide powder into a high-pressure container, adding pure water, seed crystals and tartaric acid, and carrying out hydrothermal treatment at the constant temperature of 100 ℃ and the pressure of 32kg for 24 hours; wherein the amount of the pure water is 8 times of the weight of the aluminum hydroxide powder; the seed crystal is nano alumina powder with the grain diameter of 20nm, and the adding amount of the seed crystal is 3 percent of the weight of the aluminum hydroxide powder. The dosage of the tartaric acid is 0.5 per mill of the weight of the aluminum hydroxide powder. Taking out after hydrothermal treatment, washing with water, drying, and calcining at 1400 ℃ for 3h to obtain the nano alumina powder.
The nano-alumina powder prepared by the embodiment has the particle size of 10nm and the specific surface area of 120m2/g。
Example 5
The preparation method of the nano alumina of the embodiment is carried out according to the following steps:
the raw material aluminum plate after surface treatment is simultaneously used as a cathode and an anode and is placed in a benzyltrimethylammonium chloride electrolyte with the content of 500g/L, and the pH value is 6-7, and the current density is 5A/dm2The aluminum plate was electrolyzed at a temperature of 30 ℃ under a condition of a mechanical agitation air supply of 2000L/min. When the precipitation content in the electrolyte reaches 10%, filtering the bath solution to obtain aluminum hydroxide powder; washing aluminum hydroxide powder, putting the washed aluminum hydroxide powder into a high-pressure container, adding pure water, seed crystals and citric acid, and carrying out hydrothermal treatment at the constant temperature of 300 ℃ and the constant pressure of 7kg for 48 hours; wherein the amount of the pure water is 1 time of the weight of the aluminum hydroxide powder; the seed crystal is nano alumina powder with the grain diameter of 30nm, and the adding amount of the seed crystal is 1 percent of the weight of the aluminum hydroxide powder. The amount of citric acid is 5% of the weight of the aluminum hydroxide powder. Taking out after hydrothermal treatment, washing with water, drying, and calcining at 1250 ℃ for 10h to obtain the nano alumina powder.
The nano-alumina powder prepared by the embodiment has the particle size of 30nm and the specific surface area of 55m2/g。
Example 6
The preparation method of the nano alumina of the embodiment is carried out according to the following steps:
the raw material aluminum plate after surface treatment is simultaneously used as a cathode and an anode and is placed in a benzyldimethyl tetradecyl ammonium chloride electrolyte with the content of 300g/L, the pH value is 8-10, and the current density is 5A/dm2The aluminum plate was electrolyzed at 30 ℃ with a mechanical agitation air feed rate of 100L/min. When the precipitation content in the electrolyte reaches 20%, filtering the bath solution to obtain aluminum hydroxide powder; washing aluminum hydroxide powder, putting the washed aluminum hydroxide powder into a high-pressure container, adding pure water, seed crystals and tartaric acid, and carrying out hydrothermal treatment at the constant temperature of 100 ℃ and the pressure of 37kg for 48 hours; wherein,the consumption of the pure water is 2 times of the weight of the aluminum hydroxide powder; the seed crystal is nano alumina powder with the grain diameter of 70nm, and the adding amount of the seed crystal is 8 percent of the weight of the aluminum hydroxide powder; the amount of tartaric acid is 10% of the weight of the aluminum hydroxide powder. Taking out after hydrothermal treatment, washing with water, drying, and calcining at 1200 ℃ for 8h to obtain the nano alumina powder.
The nano alumina powder prepared in this example has a particle size of 70nm and a specific surface area of 27m2/g。
The embodiments in the above embodiments can be further combined or replaced, and the embodiments are only used for describing the preferred embodiments of the present invention, and do not limit the concept and scope of the present invention, and various changes and modifications made to the technical solution of the present invention by those skilled in the art without departing from the design idea of the present invention belong to the protection scope of the present invention.
Claims (8)
1. The preparation method of the nano alumina is characterized in that the preparation method comprises the steps of simultaneously taking a raw material aluminum plate after surface treatment as a cathode and an anode to carry out electrolytic reaction; washing, hydro-thermal treatment, washing, drying and calcining the obtained electrolysis product to obtain nano alumina powder; the electrolytic reaction adopts an electrolyte containing 50-500 g/L of cationic surfactant with 5-25 carbon atoms as an active ingredient, wherein the surfactant is any one of benzyl trimethyl ammonium chloride, choline chloride, beta-methyl choline chloride, benzyl triethyl ammonium chloride and benzyl dimethyl tetradecyl ammonium chloride; the hydrothermal treatment comprises the following steps: filtering an electrolysis product aluminum hydroxide powder, putting the filtered electrolysis product aluminum hydroxide powder into a high-pressure container, adding pure water, seed crystals and organic anions, and carrying out hydrothermal treatment at a constant temperature of 100-300 ℃ and a pressure of 1-87 kg for 1-48 h; wherein the amount of the pure water is 1-8 times of the weight of the aluminum hydroxide powder; the dosage of the organic anion is 0.5 per mill to 10 percent of the weight of the aluminum hydroxide powder.
2. The method according to claim 1, wherein the electrolysis reaction is carried out using a direct current as a power source.
3. The method according to claim 1, wherein the electrolysis is carried out at a pH of 6 to 10 and a current density of 1 to 5A/dm2The temperature is 30-90 ℃, and the air supply amount of mechanical stirring or air stirring is 100-3000L/min.
4. The preparation method according to claim 1, wherein the electrolyte is filtered and separated when the content of white aluminum hydroxide powder as an electrolysis product in the electrolyte is 3 to 30 percent.
5. The preparation method according to claim 1, wherein the seed crystal is nano alumina powder with a particle size of 5-100 nm, and the dosage of the seed crystal is 1-10% of the weight of the aluminum hydroxide powder.
6. The method of claim 1, wherein the organic anion is one of tartaric acid or citric acid.
7. The method of claim 1, wherein the calcining conditions are as follows: calcining for 3-15 hours at 600-1400 ℃ to obtain the nano aluminum oxide.
8. The preparation method according to claim 1, wherein the preparation method comprises the following steps: the aluminum plate after surface treatment is simultaneously used as a cathode and an anode, and is placed in electrolyte containing benzyltrimethylammonium chloride with the amount of 400g/L at the pH of 8-10; current density 1A/dm2Electrolyzing the aluminum plate at the temperature of 30 ℃ under the condition that the air stirring air supply amount is 100L/min, and filtering the bath solution to obtain aluminum hydroxide powder when the solid content in the electrolyte reaches 25%; washing aluminum hydroxide powder, putting the washed aluminum hydroxide powder into a high-pressure container, adding pure water, seed crystals and tartaric acid accounting for 5 percent of the weight of the aluminum hydroxide powder, and keeping the temperature for 1h at 100 ℃ and under the pressure of 30 kg; taking out, washing with water, drying, and calcining at 1000 deg.C for 6h to obtain nanometer alumina powder.
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| CN1556250A (en) * | 2003-12-31 | 2004-12-22 | �Ϻ���ͨ��ѧ | Electrolysis preparation method of nano cuprous oxide |
| CN1789496A (en) * | 2004-12-15 | 2006-06-21 | 广东工业大学 | Electrochemical preparation method of nano ceric oxide |
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| US2833707A (en) * | 1951-01-29 | 1958-05-06 | Guareschi Pietro | Electrolytic production of alumina |
| JPS61284590A (en) * | 1985-06-10 | 1986-12-15 | Mitsubishi Heavy Ind Ltd | Production of alumina particle |
| CN1286725C (en) * | 2004-05-14 | 2006-11-29 | 山东铝业股份有限公司 | Method for preparing high-pruity alumina powder |
| CN102320638A (en) * | 2011-08-04 | 2012-01-18 | 中国铝业股份有限公司 | Preparation method of low-sodium fine grain alumina |
| CN102560521A (en) * | 2012-01-14 | 2012-07-11 | 新疆哥兰德新能源有限公司 | Method for electrochemically preparing high-purity aluminum oxide |
| CN102583472A (en) * | 2012-03-30 | 2012-07-18 | 中国铝业股份有限公司 | Method for preparing pseudo-boehmite with different crystallinity degrees |
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| CN1556250A (en) * | 2003-12-31 | 2004-12-22 | �Ϻ���ͨ��ѧ | Electrolysis preparation method of nano cuprous oxide |
| CN1789496A (en) * | 2004-12-15 | 2006-06-21 | 广东工业大学 | Electrochemical preparation method of nano ceric oxide |
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| "电化学合成纳米FeOOH的电解工艺研究";张强等;《绍兴文理学院学报》;20091231;第29卷(第10期);第30-32页 * |
| "电化学合成纳米α-Fe2O3的工艺研究";张强等;《化学工业与工程技术》;20090831;第30卷(第4期);第11-13页 * |
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