CN1261359C - Preparation method of nano mesoporous titanium dioxide powder - Google Patents
Preparation method of nano mesoporous titanium dioxide powder Download PDFInfo
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- CN1261359C CN1261359C CN 200410081384 CN200410081384A CN1261359C CN 1261359 C CN1261359 C CN 1261359C CN 200410081384 CN200410081384 CN 200410081384 CN 200410081384 A CN200410081384 A CN 200410081384A CN 1261359 C CN1261359 C CN 1261359C
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000004408 titanium dioxide Substances 0.000 title abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001868 water Inorganic materials 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 32
- 239000000047 product Substances 0.000 claims description 12
- 238000003483 aging Methods 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- 239000013543 active substance Substances 0.000 claims description 7
- -1 make aperture 2~15nm Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 241000282326 Felis catus Species 0.000 claims description 4
- 239000003945 anionic surfactant Substances 0.000 claims description 4
- 239000012716 precipitator Substances 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 229920004890 Triton X-100 Polymers 0.000 claims description 2
- 239000013504 Triton X-100 Substances 0.000 claims description 2
- NEUSVAOJNUQRTM-UHFFFAOYSA-N cetylpyridinium Chemical compound CCCCCCCCCCCCCCCC[N+]1=CC=CC=C1 NEUSVAOJNUQRTM-UHFFFAOYSA-N 0.000 claims description 2
- 229960004830 cetylpyridinium Drugs 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 125000001475 halogen functional group Chemical group 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000011148 porous material Substances 0.000 abstract description 8
- 238000001914 filtration Methods 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 3
- 239000011941 photocatalyst Substances 0.000 abstract description 3
- 150000003608 titanium Chemical class 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract 2
- 238000000227 grinding Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011005 laboratory method Methods 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000002699 waste material Substances 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 mesoporous titanium dioxide powder, which is easy for industrial production. The method adopts inorganic titanium salt of titanyl sulfate and sodium hydroxide and inorganic alkali as main raw materials, water as solvent, and addsA surfactant, preparing titanium dioxide coacervate particles, filtering, drying, heat treating and grinding to obtain the titanium dioxide coacervate particles with the aperture of 2-15 nm, the particle diameter of 8-15 nm and the specific surface area of 80-150 m2The anatase type nanometer mesoporous titanium dioxide powder is/g. As the main raw materials are inorganic titanium salt, inorganic alkali and water, the production cost of the whole process is low. The prepared nano mesoporous titanium dioxide has the wall body of anatase type nanocrystalline, can effectively generate photoelectrons and photo-induced cavities after being excited by ultraviolet rays, and is suitable for being used as a photocatalyst. The pore diameter of the mesopores is distributed between 2 nm and 15nm, the particle diameter is 8 nm to 15nm, and the specific surface area is 80 m to 150m2The product has good stability, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation of nanomaterials, especially a kind of preparation method of nanometer mesoporous TiO 2 powder.
Background technology
At present, the research of nano material has in recent years had swift and violent development, and its related application also begins to take shape.Nanocrystalline surface effects and dimensional effect are the most significant character that is different from conventional powder.Be accompanied by the rise of nano material, the material of multiple structures such as nanoporous, nanocrystalline, nanotube has prepared, and catalytic field becomes one of topmost application of these nano structural materials, and other purposes is also demanded exploitation urgently.
For the research of nano material, nano-functional material is its vegetative point with fastest developing speed, and titanic oxide material is again the focus of present nano-functional material research.It not only has good air-sensitive, wet quick characteristic and higher dielectric properties, and the application aspect catalysis is also very extensive.In existing photocatalyst, titanium dioxide nontoxicity and catalytic activity are the highest, have also in addition that resistance to acids and bases is good, chemical property is stable, advantage such as photochemical corrosion does not take place.
Because the mesoporous nano assembly system has special performance and important potential using value, researcher greatly concern and interest have been caused in recent years.The present prepared in laboratory method of nano meso-porous titanium dioxide is mainly sol-gel method: be raw material by organic alkoxide of titanium such as butyl (tetra) titanate etc., the employing mineral acid is a hydrolyst, and organic solvent such as dehydrated alcohol etc. is a medium, obtains colloidal sol earlier and is converted into gel again, drying, roasting makes.Because this method production cost height, preparation cycle is long, is difficult for realizing suitability for industrialized production, therefore up to the present yet there are no the report of suitability for industrialized production nano meso-porous titanium dioxide.
Summary of the invention
Long for the preparation method's production cost height, the preparation cycle that overcome existing nano meso-porous titanium dioxide, as to be difficult for realizing suitability for industrialized production deficiency, technical problem to be solved by this invention provides a kind of preparation method who is easy to the nanometer mesoporous TiO 2 powder of suitability for industrialized production.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of nanometer mesoporous TiO 2 powder, adopt the precipitator method, with titanyl sulfate and sodium hydroxide is raw material, water is solvent, add tensio-active agent, make aperture 2～15nm, particle diameter 8～15nm, specific surface area 80～150m through following processing step
2The dichloride in anatase type mesoporous TiO 2 powder of/g:
(1) adding concentration in container is that 20～35% sodium hydroxide solutions and weight percent are 1～5% surfactant soln and stir, the volume ratio of sodium hydroxide solution and surfactant soln is 10: 1～5: 1, dripping concentration is the titanyl sulfate solution of 130～170g/L, stop to pH=6.5～7 dripping, to the TiO 2 precursor white precipitate ageing that produces 1-6 hour;
(2) TiO 2 precursor that above-mentioned ageing is good filters, with temperature greater than 35 ℃ hot water washing sediment till the sulfate radical-free, then product is placed 80～110 ℃ dry 5～8 hours of baking oven;
(3) drying is good TiO 2 precursor places retort furnace, is warming up to 450～650 ℃ with the heat-up rate of 5～10 ℃/min, is incubated 1.0～2.5 hours, pulverizes promptly after being cooled to room temperature.
The invention has the beneficial effects as follows: because employing is that inorganic titanium salt and mineral alkali are main raw material, water is medium, makes that whole explained hereafter cost is low.Body of wall is the dichloride in anatase type crystalline substance in the nano meso-porous titanium dioxide of preparation, can effectively produce photoelectron and photohole after ultraviolet ray excited, is suitable for using photocatalyst.Mesoporous pore size distribution between 2～15nm, particle diameter 8～15nm, specific surface area 80～150m
2/ g has stability preferably, is suitable for suitability for industrialized production.
Through the fine setting preparation condition,, can obtain the mesohole nano-titanium dioxide powder of different apertures, different specific surface areas as: kinds of surfactants, calcining intensity etc.
Embodiment
The present invention is further described below in conjunction with embodiment.
The preparation method of nanometer mesoporous TiO 2 powder adopts the precipitator method, is raw material with titanyl sulfate and sodium hydroxide, and water is solvent, adds tensio-active agent, makes aperture 2～15nm, particle diameter 8～15nm, specific surface area 80～150m through following processing step
2The dichloride in anatase type mesoporous TiO 2 powder of/g:
(1) adding concentration in container is that 20～35% sodium hydroxide solutions and weight percent are 1～5% surfactant soln and stir, the volume ratio of sodium hydroxide solution and surfactant soln is 10: 1～5: 1, at the uniform velocity slowly drip the titanyl sulfate solution that concentration is 130～170g/L, stop to pH=6.5～7 dripping, to the TiO 2 precursor white precipitate ageing that produces 1-6 hour; Preferably at the uniform velocity slowly drip when dripping titanyl sulfate solution, local temperature is too high because of the generation of reaction neutralization heat so that solution is unlikely to.As long as drip titanyl sulfate solution make pH＜7 all can, it stops when preferably being controlled at pH=7, so just can not cause the waste of raw material.
(2) TiO 2 precursor that above-mentioned ageing is good filters, with temperature greater than 35 ℃ hot water washing sediment till the sulfate radical-free, place 80～110 ℃ dry 5～8 hours of baking oven then;
(3) drying is good TiO 2 precursor places retort furnace, is warming up to 450～650 ℃ with the heat-up rate of 5～10 ℃/min, is incubated 1.0～2.5 hours, and power cutoff is cooled to pulverize after the room temperature and promptly gets product.
Above-mentioned tensio-active agent can adopt cats product, anion surfactant or nonionogenic tenside, cats product such as N-halo cetyl pyridinium, anion surfactant such as Sodium dodecylbenzene sulfonate, nonionogenic tenside such as polyoxyethylene glycol, Triton X-100 etc.
Embodiment 1: add 25% sodium hydroxide solution 50ml in container, add weight percent again and be 5% surfactant polyethylene 5ml, stir; The titanyl sulfate solution that slowly at the uniform velocity drips concentration and be 130g/L equals 7.0 to the pH value and stops to beaker; 3 hours after-filtration of ageing, be precipitated to the filtrate sulfate radical-free with temperature greater than 50 ℃ hot wash till; Place 85 ℃ of baking ovens after 8 hours product, it is changed in the retort furnace heat-treat, heat-up rate is controlled at about 5 ℃/min, slowly is warming up to 450 ℃, is incubated 1 hour, and power cutoff is cooled to room temperature; Grind, promptly get product.
The nanometer mesoporous TiO 2 powder of preparation is characterized in that: anatase titanium dioxide; The specific surface area 149m of nanometer mesoporous TiO 2 powder
2/ g, pore size distribution: 10～15nm, particle diameter is: 8.0nm, pore volume is: 0.388cm
3/ g.
Embodiment 2: add 25% sodium hydroxide solution 50ml in container, add weight percent again and be 3% surfactant polyethylene 5ml, stir; The titanyl sulfate solution that slowly at the uniform velocity drips concentration and be 150g/L equals 7.0 to the pH value and stops to beaker; 3 hours after-filtration of ageing, be precipitated to the filtrate sulfate radical-free with temperature greater than 50 ℃ hot wash till; Place 85 ℃ of baking ovens after 8 hours product, it is changed in the retort furnace heat-treat, heat-up rate is controlled at about 5 ℃/min, slowly is warming up to 550 ℃, is incubated 1.5 hours, and power cutoff is cooled to room temperature; Grind, promptly get product.
The nanometer mesoporous TiO 2 powder of preparation is characterized in that: anatase titanium dioxide; The specific surface area 103m of nanometer mesoporous TiO 2 powder
2/ g, pore size distribution: 5-10nm, particle diameter is: 10nm, pore volume is: 0.347cm
3/ g.
Embodiment 3: add 25% sodium hydroxide solution 50ml in container, add weight percent again and be 1% surfactant polyethylene 5ml, stir; The titanyl sulfate solution that slowly at the uniform velocity drips concentration and be 170g/L equals 6.5 to the pH value and stops to beaker; 3 hours after-filtration of ageing, be precipitated to the filtrate sulfate radical-free with temperature greater than 50 ℃ hot wash till; Place 85 ℃ of baking ovens after 8 hours product, it is changed in the retort furnace heat-treat, heat-up rate is controlled at about 5 ℃/min, slowly is warming up to 650 ℃, is incubated 1 hour, and power cutoff is cooled to room temperature; Grind, promptly get product.
The nanometer mesoporous TiO 2 powder of preparation is characterized in that: anatase titanium dioxide; The specific surface area 81m of nanometer mesoporous TiO 2 powder
2/ g, pore size distribution: 2-8nm, particle diameter is: 15nm, pore volume is: 0.289cm
3/ g.
Claims (8)
1, a kind of preparation method of nanometer mesoporous TiO 2 powder, adopting the precipitator method, is raw material with titanyl sulfate and sodium hydroxide, and water is solvent, add tensio-active agent, make aperture 2～15nm, particle diameter 8～15nm, specific surface area 80～150m through following processing step
2The dichloride in anatase type mesoporous TiO 2 powder of/g:
(1) adding concentration in container is that 20～35% sodium hydroxide solutions and weight percent are 1～5% surfactant soln and stir, the volume ratio of sodium hydroxide solution and surfactant soln is 10: 1～5: 1, dripping concentration is the titanyl sulfate solution of 130～170g/L, stop to pH=6.5～7 dripping, to the TiO 2 precursor white precipitate ageing that produces 1-6 hour;
(2) TiO 2 precursor that above-mentioned ageing is good filters, with temperature greater than 35 ℃ hot water washing sediment till the sulfate radical-free, place 80～110 ℃ dry 5～8 hours of baking oven then;
(3) drying is good TiO 2 precursor places retort furnace, is warming up to 450～650 ℃ with the heat-up rate of 5～10 ℃/min, is incubated 1.0～2.5 hours, is cooled to pulverize after the room temperature promptly to get the dichloride in anatase type mesoporous TiO 2 powder.
2, the preparation method of nanometer mesoporous TiO 2 powder as claimed in claim 1 is characterized in that: described tensio-active agent is a cats product.
3, the preparation method of nanometer mesoporous TiO 2 powder as claimed in claim 2 is characterized in that: described cats product is a N-halo cetyl pyridinium.
4, the preparation method of nanometer mesoporous TiO 2 powder as claimed in claim 1 is characterized in that: described tensio-active agent is an anion surfactant.
5, the preparation method of nanometer mesoporous TiO 2 powder as claimed in claim 4 is characterized in that: described anion surfactant is a Sodium dodecylbenzene sulfonate.
6, the preparation method of nanometer mesoporous TiO 2 powder as claimed in claim 1 is characterized in that: described tensio-active agent is a nonionogenic tenside.
7, the preparation method of nanometer mesoporous TiO 2 powder as claimed in claim 6 is characterized in that: described nonionogenic tenside is a polyoxyethylene glycol.
8, the preparation method of nanometer mesoporous TiO 2 powder as claimed in claim 6 is characterized in that: described nonionogenic tenside is a Triton X-100.
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| CN 200410081384 CN1261359C (en) | 2004-12-02 | 2004-12-02 | Preparation method of nano mesoporous titanium dioxide powder |
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|---|---|---|---|
| CN 200410081384 CN1261359C (en) | 2004-12-02 | 2004-12-02 | Preparation method of nano mesoporous titanium dioxide powder |
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| CN1636879A CN1636879A (en) | 2005-07-13 |
| CN1261359C true CN1261359C (en) | 2006-06-28 |
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325381C (en) * | 2005-05-23 | 2007-07-11 | 北京工业大学 | Method for preparing medium pore molecular sieve of titanium dioxide |
| CN100368301C (en) * | 2005-09-13 | 2008-02-13 | 山东轻工业学院 | Mesoporous nanopowder titanium dioxide bionic synthesis method |
| CN100450925C (en) * | 2006-10-27 | 2009-01-14 | 清华大学 | Process for synthesizing mesoporous TiO2 using phosphotungstic acid as template agent |
| CN100579911C (en) * | 2007-11-23 | 2010-01-13 | 中国科学院过程工程研究所 | Method for low-temperature synthesis of titanium dioxide nano powder |
| CN101773820B (en) * | 2009-12-30 | 2012-11-21 | 长沙学院 | Method for preparing visible light active photocatalyst through dye sensitization |
| CN102134096B (en) * | 2011-05-03 | 2012-07-04 | 河北工业大学 | Method for preparing porous titanium oxide nano material |
| CN102820459A (en) * | 2012-07-20 | 2012-12-12 | 合肥国轩高科动力能源有限公司 | Preparation method for synthesizing high-specific-energy lithium titanate material from mesoporous titanium dioxide |
| WO2015016779A1 (en) * | 2013-07-29 | 2015-02-05 | National University Of Singapore | Titanium dioxide photocatalysts for reverse osmosis concentrate recovery |
| CN103771507B (en) * | 2013-12-25 | 2015-06-24 | 武汉工程大学 | Humidity sensitivity material as well as preparation method and application thereof |
| FR3016360B1 (en) * | 2014-01-14 | 2018-08-24 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | PROCESS FOR THE PREPARATION OF A METAL OXIDE POWDER, PROCESS FOR PRODUCING A METAL OXIDE PASTILLE, AND USES OF POWDER AND PASTILLE AS EXTENDED THEREFROM |
| CN109850939B (en) * | 2018-12-26 | 2021-03-23 | 龙蟒佰利联集团股份有限公司 | Preparation method of disordered mesoporous nano titanium dioxide |
| CN110054983A (en) * | 2019-05-09 | 2019-07-26 | 山东光韵智能科技有限公司 | One kind hating oily self-cleaning dust-proof coatings and its manufacturing method |
| CN110560025B (en) * | 2019-08-01 | 2023-04-28 | 江门市三尚新材料科技有限公司 | Photocatalyst material and preparation method thereof |
| CN110698982B (en) * | 2019-10-13 | 2021-04-30 | 福建恒安集团有限公司 | Intelligent temperature-adjusting non-woven fabric, intelligent temperature-adjusting coating and intelligent temperature-adjusting disposable hygienic product |
| CN112588283B (en) * | 2020-11-25 | 2023-05-23 | 内江师范学院 | Carbon quantum dot/mesoporous Kong Cengzhuang titanium dioxide and preparation method and application thereof |
| CN114011393A (en) * | 2021-10-27 | 2022-02-08 | 安徽元琛环保科技股份有限公司 | Mesoporous TiO2Preparation method of supported efficient denitration catalyst and prepared denitration catalyst |
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