CN101619177B - Preparation method of nano-titanium dioxide coated nano-aluminium oxide - Google Patents
Preparation method of nano-titanium dioxide coated nano-aluminium oxide Download PDFInfo
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- CN101619177B CN101619177B CN 200910063399 CN200910063399A CN101619177B CN 101619177 B CN101619177 B CN 101619177B CN 200910063399 CN200910063399 CN 200910063399 CN 200910063399 A CN200910063399 A CN 200910063399A CN 101619177 B CN101619177 B CN 101619177B
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- aluminium oxide
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- aluminum hydroxide
- titanium dioxide
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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 177
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000498 ball milling Methods 0.000 claims abstract description 30
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 229960000583 acetic acid Drugs 0.000 claims abstract description 22
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 13
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 239000012670 alkaline solution Substances 0.000 claims abstract description 5
- 159000000013 aluminium salts Chemical class 0.000 claims abstract description 3
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims abstract description 3
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 229940024546 aluminum hydroxide gel Drugs 0.000 claims description 33
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical compound O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 claims description 33
- 230000000694 effects Effects 0.000 claims description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 15
- 238000001149 thermolysis Methods 0.000 claims description 14
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 229940024545 aluminum hydroxide Drugs 0.000 claims description 7
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 230000003292 diminished effect Effects 0.000 claims description 7
- 238000009987 spinning Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 4
- 239000005022 packaging material Substances 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 2
- 238000002525 ultrasonication Methods 0.000 abstract 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 abstract 1
- 230000006837 decompression Effects 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 52
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 34
- 239000011159 matrix material Substances 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 8
- 239000004408 titanium dioxide Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000000654 additive Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000006864 oxidative decomposition reaction Methods 0.000 description 2
- 238000003921 particle size analysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- -1 pottery Substances 0.000 description 2
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002594 sorbent Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000219991 Lythraceae Species 0.000 description 1
- 229910001096 P alloy Inorganic materials 0.000 description 1
- 235000014360 Punica granatum Nutrition 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- RIRXDDRGHVUXNJ-UHFFFAOYSA-N [Cu].[P] Chemical compound [Cu].[P] RIRXDDRGHVUXNJ-UHFFFAOYSA-N 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000012387 aerosolization Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 206010016256 fatigue Diseases 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- DCRSYTGOGMAXIA-UHFFFAOYSA-N zinc;oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4].[Zn+2] DCRSYTGOGMAXIA-UHFFFAOYSA-N 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of nano-titanium dioxide coated nano-aluminium oxide, which comprises the following steps: firstly, dropwise adding an alkaline solution in an aluminium salt solution under the conditions of stirring and ultrasonication, controlling the pH value of a system, and still standing to acquire aluminum hydroxide sol; drying the aluminum hydroxide sol, mixing the aluminum hydroxide sol and water, ball milling, washing the mixture with water until eluate is neutral, filtering by decompression or centrifugalizing, and thermally decomposing to acquire nano-aluminium oxide powder; secondly, adding the nano-aluminium oxide powder into a mixed solution of glacial acetic acid, water and absolute alcohol to acquire the mixture under the conditions of ultrasonication and stirring; adding the mixed solution of butyl titanate and absolute alcohol into the mixture under the conditions of ultrasonication and stirring, still standing, drying and ball milling to acquire the powder; and placing the powder into a furnace at constant temperature, and thermally decomposing to acquire the nano-titanium dioxide coated nano-aluminium oxide powder. The grain diameter of nano-titanium dioxide coated nano-aluminium oxide composite material grains is 1-50 nm, and the purity is higher than 99.8 percent.
Description
Technical field
The present invention relates to fields such as photochemical catalyst, electrochemical catalyst, organic synthesis, meticulous article chemical industry, more specifically relate to a kind of preparation method of nano-titanium dioxide coated nano-aluminium oxide.The prepared nano-titanium dioxide coated nano-aluminium oxide of the present invention can be as photocatalyst, electrochemical catalyst, the catalyzer of organic synthesis and the additive of meticulous article Chemicals etc. of water treatment.
Background technology
Nano titanium oxide is tiny because of its particle, specific surface area has the not available special effects of conventional material greatly; Colour effect like quantum effect, tunnel effect, uniqueness; And photocatalysis and function such as ultraviolet shielded; Demonstrate wide application prospect at aspects such as functional coating, automobile, makeup, health care, wastewater treatment, environmental protection, correlative study is very active.In recent years, nano titanium oxide is owing to its light stability, the nontoxic solar energy converting that becomes are that electric energy is one of material of the most generally using of solar cell.Nano titanium oxide is behind the ultraviolet irradiation that receives sunshine or luminescent lamp, and inner electronics will excite.The result has just produced the hole of electronegative electronics and positively charged.Electronics makes the hydrogen reduction in air or the water, generates ydrogen peroxide 50, then works to the direction of oxidized surface water molecules in the hole, produces hydroxyl atomic group.These all are active oxygens, and powerful oxidative decomposition capacity is arranged, thereby can decompose, remove the various organism attached to titania surface.Titanium oxide not only has powerful oxidative decomposition capacity, and the advantages such as light of self not decomposing, almost can permanently work and can utilize sunlight and luminescent lamp in addition.In exhaust gas purification, deodorization, water treatment, field such as antifouling, titanium dioxide optical catalyst has wide application potential too.
In addition, the good ultraviolet screener effect that nano titanium oxide has, the transparency and characteristics such as nontoxic make its ideal that becomes sunscreen class skin-protection product add material; Because of it has good dispersiveness, thereby use nano titanium oxide to have the fabulous transparency as the prepared Plastic Packaging Materials of additive; Also, can be used as natural and good ultraviolet line screener regenerated fiber because of its ultraviolet resistance that has and nontoxicity.Simultaneously, nano titanium oxide also can be used as the additive of resin ink colorant, Zylox strengthening agent, solid lubricant, efficient light-sensitive catalyst, sorbent material etc.Abroad, nano titanium oxide is widely used at aspects such as sun care preparations, sedan limousine metal finish paint, electronic industry, duplicating machine industry, high voltage insulating materials, ic substrate, fluorescent tubes.
Nano-aluminium oxide can be used as sorbent material and catalyzer for having that particle size is little, specific surface area is big, porosity is high, adsorptive power is strong and characteristics such as catalytic activity is strong.Perfect along with the product surface treatment process particularly, the soft-agglomerated degree of nano particle obviously reduces, and is good with the consistency of organic polymer material, greatly widened the Application Areas of aluminium sesquioxide.In addition; Because the nano-aluminium oxide crystalline structure is stable, hardness is high, dimensional stability good; The strengthening and toughening that can be widely used in products such as various plastics, rubber, pottery, refractory materials particularly improves ceramic compactness, smooth finish, cold and hot fatigability, fracture toughness property, creep-resistant property and particularly remarkable as the wear resisting property of macromolecular material product.Because nano-aluminium oxide also is the far-infrared emission material of excellent performance, be applied in fiber product and the high-pressure mercury lamp as far infrared emission and lagging material.In addition, α phase aluminium sesquioxide resistivity is high, has the good insulation performance performance, can be applicable in the main accessory and ic substrate of YGA laser brilliant (doped yttrium aluminium pomegranate laser crystals).
Nano titanium oxide and nano-aluminium oxide have many good characteristics and application prospects; But simple nano titanium oxide is during as the additive of photocatalyst, electrochemical catalyst, organic catalyst compound or fine chemical product; The starting material of titanium oxide etc. have higher cost, and the practical efficiency of titanium oxide is lower; And simple nano-aluminium oxide does not possess many good characteristics of nano titanium oxide, like photocatalysis characteristic, ultraviolet shielded effect etc.Therefore; Nano-titanium dioxide coated nano-aluminium oxide NEW TYPE OF COMPOSITE nano material; Can nano titanium oxide and nano-aluminium oxide many advantages separately be got up, prepare the additive that fields such as photochemical catalyst, electrochemical catalyst, organic synthesis, meticulous article chemical industry, plastics, pottery, semi-conductor and optics are with a wide range of applications.
Open or the report of related patent U.S. Patent No. technology that many titanium oxide, aluminium sesquioxide nano material are arranged.Chinese patent (application number 200910116178.9) discloses " adopting the method for chemical nickel plating copper-phosphorus alloy solid support of modified nano titanium dioxide "; Chinese patent (application number 200910002490.8) discloses " a kind of preparation method of iron-doped nitrogen-doped nano titanium dioxide powder "; Chinese patent (application number 200810243732.8) discloses " a kind of preparation method of nano titanium oxide-zinc oxide composite powder "; Chinese patent (application number 200810123979.2) discloses " a kind of preparation method of doped nanometer titanium oxide photocatalyst "; Chinese patent (application number 200810031600.9) discloses " preparation method of Ag-carried nanometer titanium dioxide "; Chinese patent (ZL 200610085237.X) discloses " nanometer titanium dioxide/selenium dioxide composition and preparation method thereof "; Chinese patent (ZL 02147872.4) discloses " a kind of nano titanium oxide ", and Chinese patent (ZL 99116814.3) discloses " a kind of preparation method of nano titanium oxide ".USP (application number 20090110929) discloses " a kind of rare earth doped titanium oxide and preparation method thereof "; USP (application number 20090098042) discloses " a kind of preparation method of titanium oxide "; USP (application number 20090175757) discloses " preparation method of a kind of titanium oxide/SWCN matrix material "; USP (application number 20080064592 and 20080279760) discloses " a kind of synthetic, preparation method of titanium dioxide nanoparticle " respectively; USP (application number 20080044345) discloses " a kind of production technique of titanium oxide "; USP (application number 20080260626) discloses " a kind of titanium dioxide optical catalyst "; USP (application number 20080141905) discloses " a kind of surface modifying treatment of titanium dioxide pigment particles ", and USP (application number 20080108740) discloses " a kind of TiO 2 pigment of surface-treated ".Chinese patent (ZL 01124048.2) discloses a kind of " preparation method of nano-aluminium oxide "; Chinese patent (ZL 03110932.2) discloses a kind of " combustion synthesis method prepares the method for α type nano-aluminium oxide powder "; Chinese patent (ZL200610045653.7) discloses a kind of " nanometer alumina composite phosphatized film and preparation method thereof ", and Chinese patent (ZL 200610011919.6) discloses a kind of " aerosolization method nano-aluminium oxide ultrafine powder method of manufacture " etc.In the existing technology, do not see that also the technology of nano-titanium dioxide coated nano-aluminium oxide composite material and preparation method thereof discloses or is used.
Summary of the invention
The objective of the invention is to be to provide a kind of preparation method of nano-titanium dioxide coated nano-aluminium oxide; Easy to implement the method; Simple to operate, the nano-titanium dioxide coated nano-aluminium oxide matrix material of preparation has little, the good characteristics such as dispersiveness of particle size distribution range.
The present invention realizes through following technical scheme: the preparation method of said a kind of nano-titanium dioxide coated nano-aluminium oxide matrix material comprises the steps:
A kind of preparation method of nano-titanium dioxide coated nano-aluminium oxide the steps include:
A, stir and the condition of UW effect under, be in the aluminum salt solution of 0.1～12mol/L to concentration, dripping concentration is the alkaline solution of 0.1～12mol/L; The pH value of control reaction system is 8.5～12.5; Reacted 10～60 minutes, left standstill 0.5～24 hour, obtain aluminum hydroxide sol; Drying is 0.5～24 hour under 60～100 ℃ of conditions, obtains aluminum hydroxide gel; With aluminum hydroxide gel and volume be that the water of 1～3 times of aluminum hydroxide gel volume mixes, aluminum hydroxide gel to elutant behind the ball milling 5～60 minutes, water washing ball milling for neutral or do not have that acid ion detects, filtration under diminished pressure (less than 100Kpa) or spinning; Aluminum hydroxide gel thermolysis under 150～550 ℃ of conditions with cleaning obtains the nano-aluminium oxide powder;
B, under UW effect and stirring, 25～55 ℃ temperature condition; The above-mentioned nano-aluminium oxide powder of 5～80g is joined in the mixing solutions of 1～30ml Glacial acetic acid min. 99.5 and 1～40ml water and 5～100ml absolute ethyl alcohol; Thorough mixing obtains the mixture of nano-aluminium oxide and Glacial acetic acid min. 99.5, water and absolute ethyl alcohol; Under UW effect and stirring, 25～55 ℃ temperature condition, in 10～60 minutes, 1.0～20ml butyl(tetra)titanate and 2～50ml absolute ethyl alcohol mixed solution are added drop-wise in the mixture of above-mentioned nano-aluminium oxide and Glacial acetic acid min. 99.5, water and absolute ethyl alcohol; Left standstill 0.5～24 hour, drying is 0.5～24 hour under 80～120 ℃ of conditions, ball milling; Obtain the metatitanic acid gel and coat the aluminium oxide powder end; Metatitanic acid gel that ball milling is good coats the aluminium oxide powder end and places the temperature programmed control stove, is warming up to 350～650 ℃, constant temperature 0.5～24 hour with the temperature rise rate of 1～10 ℃ of PM; Thermolysis obtains the nano-titanium dioxide coated nano-aluminium oxide powder.
A kind of nano-titanium dioxide coated nano-aluminium oxide matrix material of the present invention forms through method for preparing.
In order to realize the present invention better, described aluminium salt comprises any mixing of one or both or three kinds in aluminum chloride, aluminum nitrate and the Tai-Ace S 150;
Described alkaline solution comprises any mixing of one or both or three kinds in sodium hydroxide, Pottasium Hydroxide, the ammonia soln;
Described water is zero(ppm) water or deionized water.
The present invention compared with prior art has following advantage and beneficial effect:
1, nano-titanium dioxide coated nano-aluminium oxide matrix material size distribution homogeneous, the purity of utilizing the present invention to prepare are high, and the particle size distribution scope of matrix material is that 1～50nm, purity are higher than 99.5% (the mass percentage content sum of titanium oxide and aluminium sesquioxide);
2, utilize the thickness, content etc. of grain diameter, the coated by titanium dioxide layer of the nano-titanium dioxide coated nano-aluminium oxide matrix material that the present invention prepares to be easy to control; Can change production technique according to different purposes in good time, produce content of titanium dioxide difference, different, the performance different composite materials of grain diameter;
3, the nano-titanium dioxide coated nano-aluminium oxide NEW TYPE OF COMPOSITE nano material of utilizing the present invention to prepare; To advancing nano titanium oxide and nano-aluminium oxide matrix material application, raising titanium oxide specific surface area and service efficiency in fields such as photochemical catalyst, electrochemical catalyst, organic synthesis, meticulous article chemical industry; Reduce the production cost of nano titanium oxide associated materials; And can use repeatedly or recycling as catalyzer, have good social benefit and economic benefit;
4, the nano titanium oxide coating Al 2 O 3 composition technology of utilizing the present invention to prepare is flexible, equipment is simple, starting material are cheap, the comprehensive production cost of matrix material is low, is easy to realize large-scale industrial production.
Embodiment
Below in conjunction with embodiment, the present invention is done detailed description further.
Embodiment 1:
A kind of preparation method of nano-titanium dioxide coated nano-aluminium oxide matrix material, its step is following:
The first step is in the liquor alumini chloridi of 0.1mol/L to concentration under the condition of stirring and UW effect, and dripping concentration is the sodium hydroxide solution of 0.1mol/L; The pH value about 8.5 of control reaction system; Reacted 10 minutes, left standstill 0.5 hour, obtain aluminum hydroxide sol; 60 ℃ of dryings 24 hours, obtain aluminum hydroxide gel; With aluminum hydroxide gel and volume be that the zero(ppm) water of 1 times of aluminum hydroxide gel volume mixes, ball milling 5 minutes, use behind the distilled water wash ball milling aluminum hydroxide gel to elutant for neutral or do not have that cl ions detects, filtration under diminished pressure (less than 100Kpa) or spinning; Aluminum hydroxide gel thermolysis under 150 ℃ of conditions with cleaning obtains the nano-aluminium oxide powder;
Second step is under UW effect and stirring, 25 ℃ temperature condition; The above-mentioned nano-aluminium oxide powder of 5g is joined in the mixing solutions of 1ml Glacial acetic acid min. 99.5 and 1ml zero(ppm) water and 5ml absolute ethyl alcohol; Thorough mixing obtains the mixture of nano-aluminium oxide and Glacial acetic acid min. 99.5, zero(ppm) water and absolute ethyl alcohol; Under UW effect and stirring, 25 ℃ temperature condition; In 10 minutes; 1ml butyl(tetra)titanate and 2ml absolute ethyl alcohol mixed solution are added drop-wise in the mixture of above-mentioned nano-aluminium oxide and Glacial acetic acid min. 99.5, water and absolute ethyl alcohol, left standstill 2 hours, drying is 0.5 hour under 120 ℃ of conditions; Ball milling obtains the metatitanic acid gel and coats aluminium sesquioxide; Metatitanic acid gel that ball milling is good coats aluminium sesquioxide and places the temperature programmed control stove, is warming up to 650 ℃ with the temperature rise rate of 10 ℃ of PMs, constant temperature 0.5 hour, and thermolysis obtains the nano-titanium dioxide coated nano-aluminium oxide composite powder.
Through laser particle size analysis and chemical analysis; The grain diameter scope that the gained nano titanium oxide coats Al 2 O 3 composition is 15～50nm; Median size is about 30nm, and purity is 99.51% (the mass percentage content sum of titanium oxide and aluminium sesquioxide).
Embodiment 2:
A kind of preparation method of nano-titanium dioxide coated nano-aluminium oxide matrix material, its step is following:
The first step is in the aluminum nitrate solution of 4mol/L to concentration under the condition of stirring and UW effect, drips the potassium hydroxide solution of 4mol/L concentration; The pH value about 9.5 of control reaction system; Reacted 20 minutes, left standstill 3 hours, obtain aluminum hydroxide sol; Drying is 6 hours under 80 ℃ of conditions, obtains aluminum hydroxide gel; With aluminum hydroxide gel and volume be that the zero(ppm) water of 3 times of aluminum hydroxide gel volumes mixes, ball milling 30 minutes, to use aluminum hydroxide gel to elutant behind the distilled water wash ball milling be neutral, filtration under diminished pressure (less than 100Kpa) or spinning; Aluminum hydroxide gel thermolysis under 450 ℃ of conditions with cleaning obtains the nano-aluminium oxide powder;
Second step is under UW effect and stirring, 45 ℃ temperature condition; The above-mentioned nano-aluminium oxide powder of 30g is joined in the mixing solutions of 15ml Glacial acetic acid min. 99.5 and 30ml zero(ppm) water and 50ml absolute ethyl alcohol; Thorough mixing obtains the mixture of nano-aluminium oxide and Glacial acetic acid min. 99.5, zero(ppm) water and absolute ethyl alcohol; Under UW effect and stirring, 45 ℃ temperature condition, in 30 minutes, 10ml butyl(tetra)titanate and 30ml absolute ethyl alcohol mixed solution are added drop-wise in the mixture of above-mentioned nano-aluminium oxide and Glacial acetic acid min. 99.5, zero(ppm) water and absolute ethyl alcohol; Left standstill 6 hours, drying is 6 hours under 100 ℃ of conditions, ball milling; Obtain the metatitanic acid gel and coat the aluminium oxide powder end; Metatitanic acid gel that ball milling is good coats the aluminium oxide powder end and places the temperature programmed control stove, is warming up to 350 ℃, constant temperature 24 hours with the temperature rise rate of 1 ℃ of PM; Thermolysis obtains the nano-titanium dioxide coated nano-aluminium oxide composite powder.
Through laser particle size test and chemical analysis; The grain diameter scope of gained nano-titanium dioxide coated nano-aluminium oxide matrix material is 10～20nm; Median size is about 15nm, and purity is 99.85% (the mass percentage content sum of titanium oxide and aluminium sesquioxide).
Embodiment 3:
A kind of preparation method of nano-titanium dioxide coated nano-aluminium oxide matrix material, its step is following:
The first step stir and the condition of UW effect under, be that mole blended such as dropping, total concn are the sodium hydroxide of 6mol/L, the mixing solutions of Pottasium Hydroxide in the aluminum chloride, Tai-Ace S 150 mixing solutions of 6mol/L to waiting mole mixing, total concn; The pH value about 10.5 of control reaction system; Reacted 50 minutes, left standstill 12 hours, obtain aluminum hydroxide sol; Drying is 20 hours under 80 ℃ of conditions, obtains aluminum hydroxide gel; Aluminum hydroxide gel and volume are that the zero(ppm) water of 1.5 times of aluminum hydroxide gel volumes mixes, ball milling 45 minutes, use aluminum hydroxide gel to elutant behind the distilled water wash ball milling for neutral or do not have cl ions or sulfate ion, filtration under diminished pressure (less than 100Kpa) or a spinning; Aluminum hydroxide gel thermolysis under 350 ℃ of conditions with cleaning obtains the nano-aluminium oxide powder;
Second step is under UW effect and stirring, 35 ℃ temperature condition; The above-mentioned nano-aluminium oxide powder of 20g is joined in the mixing solutions of 12ml Glacial acetic acid min. 99.5 and 15ml water and 30ml absolute ethyl alcohol; Thorough mixing obtains the mixture of nano-aluminium oxide and Glacial acetic acid min. 99.5, water and absolute ethyl alcohol; Under UW effect and stirring, 35 ℃ temperature condition; In 40 minutes; 8ml butyl(tetra)titanate and 10ml absolute ethyl alcohol mixed solution are added drop-wise in the mixture of above-mentioned nano-aluminium oxide and Glacial acetic acid min. 99.5, water and absolute ethyl alcohol, left standstill 16 hours, drying is 8 hours under 90 ℃ of conditions; Ball milling obtains the metatitanic acid gel and coats aluminium sesquioxide; Metatitanic acid gel that ball milling is good coats aluminium sesquioxide and places the temperature programmed control stove, is warming up to 550 ℃ with the temperature rise rate of 5 ℃ of PMs, constant temperature 12 hours, and thermolysis obtains the nano-titanium dioxide coated nano-aluminium oxide composite powder.
Through laser particle size test and chemical analysis; The grain diameter scope of gained nano-titanium dioxide coated nano-aluminium oxide matrix material is 5～20nm; Median size is about 12nm, and purity is 99.7% (the mass percentage content sum of titanium oxide and aluminium sesquioxide).
Embodiment 4:
A kind of preparation method of nano-titanium dioxide coated nano-aluminium oxide matrix material, its step is following:
The first step stir and the condition of UW effect under, in the mixing solutions that waits mole mixes, total concn is 6mol/L aluminum chloride, Tai-Ace S 150 and aluminum nitrate, drip the mixing solutions of the sodium hydroxide, Pottasium Hydroxide and the ammoniacal liquor that wait a mole mixing, total concn 6mol/L; The pH value about 9.5 of control reaction system; Reacted 45 minutes, left standstill 3 hours, obtain aluminum hydroxide sol; Drying is 12 hours under 90 ℃ of conditions, obtains aluminum hydroxide gel; Aluminum hydroxide gel and volume are that the deionized water of 2.5 times of aluminum hydroxide gel volumes mixes, ball milling 40 minutes, use aluminum hydroxide gel to elutant behind the deionized water wash ball milling as neutrality or do not have cl ions or sulfate ion, filtration under diminished pressure (less than 100Kpa) or spinning; Thermolysis under 350 ℃ of conditions obtains the nano-aluminium oxide powder;
Second step is under UW effect and stirring, 45 ℃ temperature condition; The above-mentioned nano-aluminium oxide powder of 30g is joined in the mixing solutions of 15ml Glacial acetic acid min. 99.5 and 20ml water and 10ml absolute ethyl alcohol; Thorough mixing obtains the mixture of nano-aluminium oxide and Glacial acetic acid min. 99.5, deionized water and absolute ethyl alcohol; Under UW effect and stirring, 45 ℃ temperature condition; In 45 minutes; 12ml butyl(tetra)titanate and 25ml absolute ethyl alcohol mixed solution are added drop-wise in the mixture of above-mentioned nano-aluminium oxide and Glacial acetic acid min. 99.5, deionized water and absolute ethyl alcohol, left standstill 0.5 hour, drying is 12 hours under 110 ℃ of conditions; Ball milling obtains the metatitanic acid gel and coats aluminium sesquioxide; Metatitanic acid gel that ball milling is good coats aluminium sesquioxide and places the temperature programmed control stove, is warming up to 450 ℃ with the temperature rise rate of 2 ℃ of PMs, constant temperature 3 hours, and thermolysis obtains the nano-titanium dioxide coated nano-aluminium oxide composite powder.
Through laser particle size test and chemical analysis, the grain diameter scope of gained nano titanium oxide coated silica matrix material is 1～15nm, and median size is about 10nm, and purity is 99.65% (the mass percentage content sum of titanium oxide and aluminium sesquioxide).
Embodiment 5:
A kind of preparation method of nano-titanium dioxide coated nano-aluminium oxide matrix material, its step is following:
The first step is in the liquor alumini chloridi of 12mol/L to concentration under the condition of stirring and UW effect, and dripping concentration is the sodium hydroxide solution of 12mol/L; The pH value of control reaction system is 12.5; Reacted 60 minutes, left standstill 24 hours, obtain aluminum hydroxide sol; Drying is 0.5 hour under 100 ℃ of conditions, obtains aluminum hydroxide gel; Aluminum hydroxide gel and volume are that the zero(ppm) water of 1.5 times of aluminum hydroxide gel volumes mixes, ball milling 60 minutes, use aluminum hydroxide gel to elutant behind the distilled water wash ball milling for neutral or do not have cl ions, filtration under diminished pressure (less than 100Kpa) or a spinning; Thermolysis under 550 ℃ of conditions obtains the nano-aluminium oxide powder;
Second step is under UW effect and stirring, 55 ℃ temperature condition; The above-mentioned nano-aluminium oxide powder of 80g is joined in the mixing solutions of 30ml Glacial acetic acid min. 99.5 and 40ml zero(ppm) water and 100ml absolute ethyl alcohol; Thorough mixing obtains the mixture of nano-aluminium oxide and Glacial acetic acid min. 99.5, zero(ppm) water and absolute ethyl alcohol; Under UW effect and stirring, 55 ℃ temperature condition; In 60 minutes; 20ml butyl(tetra)titanate and 50ml absolute ethyl alcohol mixed solution are added drop-wise in the mixture of above-mentioned nano-aluminium oxide and Glacial acetic acid min. 99.5, zero(ppm) water and absolute ethyl alcohol, left standstill 24 hours, drying is 24 hours under 80 ℃ of conditions; Ball milling obtains the metatitanic acid gel and coats aluminium sesquioxide; Metatitanic acid gel that ball milling is good coats aluminium sesquioxide and places the temperature programmed control stove, is warming up to 450 ℃ with the temperature rise rate of 10 ℃ of PMs, constant temperature 12 hours, and thermolysis obtains the nano-titanium dioxide coated nano-aluminium oxide composite powder.
Through laser particle size analysis and chemical analysis; The grain diameter scope of gained nano-titanium dioxide coated nano-aluminium oxide matrix material is 1～10nm; Median size is about 5nm, and purity is 99.6% (the mass percentage content sum of titanium oxide and silicon-dioxide).
As stated, can realize the present invention preferably.
Claims (1)
1. the preparation method of a nano-titanium dioxide coated nano-aluminium oxide the steps include:
A, stir and the condition of UW effect under; To concentration is in the aluminum salt solution of 0.1～12mol/L, and dripping concentration is the alkaline solution of 0.1～12mol/L, and the pH value of control reaction system is 8.5～12.5; Reacted 10～60 minutes; Left standstill 0.5～24 hour, and obtained aluminum hydroxide sol, drying is 0.5～24 hour under 60～100 ℃ of conditions; Obtain aluminum hydroxide gel; With aluminum hydroxide gel and volume be that the water of 1～3 times of aluminum hydroxide gel volume mixes, aluminum hydroxide gel to elutant behind the ball milling 5～60 minutes, water washing ball milling for neutral or do not have that acid ion detects, filtration under diminished pressure or spinning, the aluminum hydroxide gel thermolysis under 150～550 ℃ of conditions with cleaning obtains the nano-aluminium oxide powder;
B, under UW effect and stirring, 25～55 ℃ temperature condition; The above-mentioned nano-aluminium oxide powder of 5～80g is joined in the mixing solutions of 1～30ml Glacial acetic acid min. 99.5 and 1～40ml water and 5～100ml absolute ethyl alcohol; Mix, obtain the mixture of nano-aluminium oxide and Glacial acetic acid min. 99.5, water and absolute ethyl alcohol; Under UW effect and stirring, 25～55 ℃ temperature condition, in 10～60 minutes, 1.0～20ml butyl(tetra)titanate and 2～50ml absolute ethyl alcohol mixed solution are added drop-wise in the mixture of above-mentioned nano-aluminium oxide and Glacial acetic acid min. 99.5, water and absolute ethyl alcohol; Left standstill 0.5～24 hour, drying is 0.5～24 hour under 80～120 ℃ of conditions, ball milling; Obtain the metatitanic acid gel and coat aluminium sesquioxide; Metatitanic acid gel that ball milling is good coats aluminium sesquioxide and places the temperature programmed control stove, is warming up to 350～650 ℃, constant temperature 0.5～24 hour with the temperature rise rate of 1～10 ℃ of PM; Thermolysis obtains the nano-titanium dioxide coated nano-aluminium oxide composite powder;
Described aluminium salt comprises any mixing of one or both or three kinds in aluminum chloride, aluminum nitrate, the Tai-Ace S 150;
Described alkaline solution comprises any mixing of one or both or three kinds in sodium hydroxide solution, potassium hydroxide solution, the ammoniacal liquor;
Described water is zero(ppm) water or deionized water.
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