CN1057982C - Large mass TiO2 mesohole solid and preparing method - Google Patents
Large mass TiO2 mesohole solid and preparing method Download PDFInfo
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- CN1057982C CN1057982C CN98111118A CN98111118A CN1057982C CN 1057982 C CN1057982 C CN 1057982C CN 98111118 A CN98111118 A CN 98111118A CN 98111118 A CN98111118 A CN 98111118A CN 1057982 C CN1057982 C CN 1057982C
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Abstract
The present invention discloses a preparation method of a large mass TiO2 mesohole solid, which comprises the following steps: preparing titanium dioxide sol by using butyl titanate and distilled water as raw materials and alcohol as a solvent by a sol-gel method, and then gelling, drying and heat treating the titanium dioxide sol. The large mass TiO2 mesohole solid prepared by the method of the present invention has the characteristics that the porosity is more than 40%, the specific surface area is more than 70m<2>g<-1>, the pore size distribution is more than 8 to 10 nm, and the mass body volume is more than 150mm<3>. The material prepared by the method is not only used as the carriers of various kinds of catalysts, but also used as a supporter for assembling conductors or nanometer metal particles so as to prepare various kinds of novel mesohole complexes with special functions.
Description
The present invention relates to mesoporous TiO 2 block and preparation.
Titanium dioxide is important inorganic functional material, and it not only has good air-sensitive, wet quick characteristic and higher dielectric properties, also be widely used aspect catalysis, and the range of application of the titanium dioxide powder of nano-scale is wider.In recent years, medium porosity assembling system is owing to have particular performances and important potential using value, and causes people's extensive attention and interest.Present research concentrates on porous silicon, porous silica and porous alumina system mostly, yet to the rare report of the research of mesoporous titanium dioxide assembly system, tracing it to its cause mainly is that the titanium dioxide solid is difficult for obtaining.
Purpose of the present invention just provides a kind of preparation large mass TiO 2 mesohole solid and preparation method thereof.
The inventive method is: use colloidal sol---gel method is a raw material with butyl (tetra) titanate and distilled water, and alcohol is prepared TiO 2 sol for solvent, and gelling again, drying, last thermal treatment make large mass TiO 2 mesohole solid.
Be described in detail the present invention below:
Step 1. with butyl (tetra) titanate and distilled water is raw material, and alcohol is solvent, and Glacial acetic acid is a catalyzer, prepares TiO 2 sol, is encapsulated in the container;
Step 2. will be encapsulated in TiO 2 sol 40 ~ 60 ℃ of gelations in baking oven in the container, more aging dry 2 ~ 3 weeks under 50 ~ 70 ℃ of temperature; Again respectively through 70 ~ 80 ℃ 1 ~ 2 day; 90 ~ 100 ℃ 2 ~ 4 days; 120 ~ 30 ℃ of 4 ~ 6 days dry xerogel pieces that obtain that slowly heat up make the xerogel piece descend with oven temperature at last and slowly cool to room temperature;
Step 3. in 450 ~ 600 ℃ of annealing 4 ~ 8 hours, temperature rise rate made large mass TiO 2 mesohole solid less than 6 ℃/min to the xerogel piece that step 2 is made in atmosphere furnace.
Used alcohol is propyl carbinol, dehydrated alcohol in the inventive method step 1; The mol ratio of butyl (tetra) titanate and Glacial acetic acid is 1: 1.5～8; The mol ratio of butyl (tetra) titanate and water is 1: 2～8; Butyl (tetra) titanate is 1: 8～14 with the mol ratio of alcohol.
With the porosity of the large mass TiO 2 mesohole solid of the inventive method preparation more than 40%, specific surface＞70m
2g
-1Pore size distribution is narrow, mainly at 8～10nm; Block volume can reach more than 150 cubic millimeters.
Mesoporous titanium dioxide solid with the inventive method preparation not only can be used as various support of the catalyst, also can be used as the nano particle of upholder assembled semiconductor or metal, in order to prepare multiple novel mesic hole compound with property.In a word, the inventive method and the product of preparing are current material preparation FRONTIER IN SCIENCE, also are the bases of preparation nano structure device of future generation.
Embodiment:
In a beaker, add 34 milliliters of analytical pure butyl (tetra) titanates, add 40 milliliters of dehydrated alcohols again, stir, add 9 milliliters of Glacial acetic acid while stirring;
In another beaker, add 6 ml distilled waters, add 35 milliliters of dehydrated alcohols again, make it dilution, stir;
The mixing solutions of dehydrated alcohol in second beaker and distilled water is slowly splashed in first beaker, obtain yellow clear sol, be encapsulated in the container, be placed on 1 week in 60 ℃ of baking ovens, make it that colloidal sol---gel conversion take place, aging; And then respectively through 70 ℃ 1 day; 80 ℃ 2 days; 100 ℃ 2 days; 120 ℃ obtained the xerogel piece after the slow intensification drying in 4 days; Turn-off the baking oven power supply, just xerogel slowly cools to room temperature; The xerogel piece is put into atmosphere furnace heat-treats; 120 ℃ are incubated 1 hour; In 2 hours, be warming up to 450 ℃, be incubated 4.5 hours; Power cutoff is cooled to room temperature.The mesoporous titanium dioxide solid porosity of preparing is 48%, and specific surface is 80m
2g
-1Pore size distribution is at 8～10nm; Block volume is more than 160 cubic millimeters.
Claims (6)
1. mesoporous TiO 2 block, the porosity that it is characterized in that block is that specific surface is greater than 70m more than 40%
2g
-1, pore size distribution is mainly 8～10nm; The volume of block is more than 150 cubic millimeters.
2. the preparation method of block according to claim 1 mainly comprises colloidal sol---gel method, it is characterized in that with butyl (tetra) titanate and distilled water be raw material, and alcohol is solvent, and Glacial acetic acid is a catalyzer, makes TiO 2 sol; To be encapsulated in TiO 2 sol in the container in 40～60 ℃ of following gelations, again in 50～70 ℃ of aging down dry 2～3 weeks, descended 1～2 day through 70～80 ℃ respectively again, 90～100 ℃ were descended 2～4 days, 120～130 ℃ slowly heated up dry to obtain the xerogel piece down in 4～6 days, then, make the xerogel piece slowly cool to room temperature; At last with the xerogel piece in atmosphere furnace in 450～600 ℃ of annealing 4～8 hours, temperature rise rate is less than 6 ℃/minute, obtains the mesoporous TiO 2 block.
3. method according to claim 2 is characterized in that it being that the mol ratio of butyl (tetra) titanate and water is 1: 2～8, and titanium ester butyl ester is 1: 8～14 with the mol ratio of alcohol.
4. according to claim 2 or 3 described methods, it is characterized in that alcohol is propyl carbinol or dehydrated alcohol.
5. method according to claim 2, the mol ratio that it is characterized in that butyl (tetra) titanate and Glacial acetic acid is 1: 1.5～8.
6. method according to claim 2 is characterized in that, adds 34 milliliters of analytical pure butyl (tetra) titanates in a beaker, adds 40 milliliters of dehydrated alcohols again, stirs, and adds 9 milliliters of Glacial acetic acid while stirring; In another beaker, add 6 ml distilled waters, add 35 milliliters of dehydrated alcohols again, make it dilution, stir; The mixing solutions of dehydrated alcohol in second beaker and distilled water is slowly splashed in first beaker, obtain yellow clear sol, be encapsulated in the container, be placed on 1 week in 60 ℃ of baking ovens, make it that colloidal sol---gel conversion take place, aging; And then respectively through 70 ℃ 1 day; 80 ℃ 2 days; 100 ℃ 2 days; 120 ℃ obtained the xerogel piece after the slow intensification drying in 4 days; Turn-off the baking oven power supply, make desiccant gel slowly cool to room temperature; The xerogel piece is put into atmosphere furnace heat-treats: 120 ℃ are incubated 1 hour; In 2 hours, be warming up to 450 ℃, be incubated 4.5 hours; Power cutoff is cooled to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98111118A CN1057982C (en) | 1998-01-14 | 1998-01-14 | Large mass TiO2 mesohole solid and preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98111118A CN1057982C (en) | 1998-01-14 | 1998-01-14 | Large mass TiO2 mesohole solid and preparing method |
Publications (2)
| Publication Number | Publication Date |
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| CN1186774A CN1186774A (en) | 1998-07-08 |
| CN1057982C true CN1057982C (en) | 2000-11-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN98111118A Expired - Fee Related CN1057982C (en) | 1998-01-14 | 1998-01-14 | Large mass TiO2 mesohole solid and preparing method |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1110361C (en) * | 1998-12-04 | 2003-06-04 | 中国科学院大连化学物理研究所 | Nanometer-level TiO2 photocatalyst carried by metal net and its preparation |
| CN1100836C (en) * | 1999-06-30 | 2003-02-05 | 中国科学院感光化学研究所 | Process for synthesizing titanium sol-gel paint under light induction |
| DE10232868A1 (en) * | 2002-07-19 | 2004-02-05 | Oxeno Olefinchemie Gmbh | Fine-pore catalyst and process for the hydrogenation of aromatic compounds |
| CN1305997C (en) * | 2004-03-10 | 2007-03-21 | 复旦大学 | Metal oxide pore material with excellent electrochromism performance and its preparation process |
| US7541012B2 (en) * | 2004-07-07 | 2009-06-02 | The Hong Kong University Of Science And Technology | Catalytic material and method of production thereof |
| CN1325381C (en) * | 2005-05-23 | 2007-07-11 | 北京工业大学 | Method for preparing medium pore molecular sieve of titanium dioxide |
| CN100347248C (en) * | 2006-01-06 | 2007-11-07 | 浙江大学 | Method for preparing broad-spectrum excitation responsible coating self-cleaning protector |
| CN100450925C (en) * | 2006-10-27 | 2009-01-14 | 清华大学 | Process for synthesizing mesoporous TiO2 using phosphotungstic acid as template agent |
| CN101671052B (en) * | 2009-09-08 | 2011-06-08 | 西安瑞联近代电子材料有限责任公司 | Method for preparing anatase-shaped nano TiO2 |
| CN101830503B (en) * | 2010-04-13 | 2012-10-17 | 沈阳化工学院 | Method for preparing novel porous honeycomb mesoporous titanium dioxide material |
| CN102738974B (en) * | 2012-07-06 | 2013-11-06 | 浙江凯文磁钢有限公司 | Method for increasing compressive strength of tile-shaped magnet for permanent magnet motor |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5116943A (en) * | 1974-08-01 | 1976-02-10 | Mitsubishi Electric Corp | HOROGURAMUKIROKUHOHO |
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1998
- 1998-01-14 CN CN98111118A patent/CN1057982C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5116943A (en) * | 1974-08-01 | 1976-02-10 | Mitsubishi Electric Corp | HOROGURAMUKIROKUHOHO |
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| CN1186774A (en) | 1998-07-08 |
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