CN1261359C - Prepn process of nanometer mesoporous TiO2 powder - Google Patents
Prepn process of nanometer mesoporous TiO2 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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Abstract
The present invention discloses a preparation method of nanometer mesoporous titanium dioxide powder, which is easy for industrialization. The method comprises the following steps: inorganic titanium salt and inorganic hydroxide, including mesoporous sulfate and sodium hydroxide, are adopted as main raw materials, water is adopted as a solvent, and then a surfactant is added to prepare titanium dioxide coagulation particles; the titanium dioxide coagulation particles are filtrated, dried, heated and ground to prepare sharpening titanium type nanometer mesoporous titanium dioxide powder, wherein the hole diameter of the prepared sharpening titanium type nanometer mesoporous titanium dioxide powder is from 2 to 15nm, the particle diameter is from 8 to 15nm, and the specific surface area is from 80 to 150m<2>/g. The inorganic titanium salt, the inorganic hydroxide and the water are adopted as main raw materials, so that the whole technology production cost is low; the wall body of the prepared nanometer mesoporous titanium dioxide powder is sharpening titanium typenanometer quartz, so that the prepared nanometer mesoporous titanium dioxide powder can produce photoelectron and photoproduction positive hole by the excitation of ultraviolet ray, and is suitable for being used as a photocatalyst; the pore size distribution of the mesoporous is from 2 to 15nm, the particle diameter is from 8 to 15nm, and the specific surface area is from 80 to 150m<2>/g, so that the prepared nanometer mesoporous titanium dioxide powder is suitable for industrialization.
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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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 lithium titanate material with high specific energy from mesoporous titanium dioxide |
| SG11201600493WA (en) * | 2013-07-29 | 2016-02-26 | Univ 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 |
| CN113088192B (en) * | 2019-10-13 | 2022-03-25 | 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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