CN105753046B - A kind of porous TiO2The preparation method of block materials - Google Patents
A kind of porous TiO2The preparation method of block materials Download PDFInfo
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- CN105753046B CN105753046B CN201610292024.8A CN201610292024A CN105753046B CN 105753046 B CN105753046 B CN 105753046B CN 201610292024 A CN201610292024 A CN 201610292024A CN 105753046 B CN105753046 B CN 105753046B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Abstract
The invention discloses a kind of porous TiO2The preparation method of block materials, dispersant is used as using ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol etc., using butyl titanate as raw material, precursor solution is made in certain sequence, through gelation process formation macromolecular network structure, direct pressing is molded after drying, then thermally treated process can obtain porous TiO2Block materials；This method processing step is few, apparatus and process is simple, cost is low.
Description
Technical field
The invention belongs to field of material technology, more particularly to a kind of porous TiO2The preparation method of block materials.
Background technology
Nano titanium oxide has the performance such as photocatalysis, antibacterial, self-cleaning, anti-aging, cannot be only used for cosmetics, painting
The field such as material, paint, fine ceramics, it may also be used for air cleaning, the degraded of organic matter.It is right as a kind of high efficiency photocatalyst
The requirement of nano titanium oxide is that have preferably dispersiveness, and the surface-active of nanometer titanic oxide material is with titanium dioxide
The reduction of grain diameter and increase, therefore generally nanometer titanic oxide material there is agglomeration, have influence on its photocatalytic activity
Reduction.It there is also an issue during the use of graininess nano-scale photocatalyst, the problem of exactly reclaiming.Porous two
The problem of titania meterial can not only solve to reunite, the problem of can also solving to reclaim difficulty, poriferous titanium dioxide material will
Ask it that there is tiny perforate, even pore distribution, this patent is that relate to a kind of preparation method of poriferous titanium dioxide material.
The content of the invention
In order to overcome the shortcoming of above-mentioned prior art, it is an object of the invention to provide a kind of porous TiO2Block materials
Preparation method, with reference to liquid phase method and solid phase method, with equipment requirement is simple, short preparation period the characteristics of.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of porous TiO2The preparation method of block materials, using butyl titanate as raw material, absolute ethyl alcohol and deionized water are
Solvent, makes precursor solution, then obtain porous TiO through gelation, drying, dry-pressing and heat treatment process using dispersant2
Block materials.
The dispersant is by ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol and poly- second
Glycol is constituted.
The volume ratio of the absolute ethyl alcohol and deionized water is (1：1)~(1：3).
The mol ratio of the butyl titanate and citric acid is 1：(1~2).
The butyl titanate add into a part of absolute ethyl alcohol solution one, the dispersant add to deionized water with
Solution two is obtained in the mixed liquor of remainder absolute ethyl alcohol, then solution one and solution two are mixed evenly, regulation pH value to 3
~5 obtain precursor solution, by precursor solution in water-bath at 80~85 DEG C to gelation, then the dry formation at 140~160 DEG C
Xerogel, carries out ground sieve and obtains xerogel powder, then this xerogel powder is directly done after drying naturally at room temperature
It is molded, block blank of material is formed, it is finally thermally treated to produce porous TiO2Block materials.
After solution one and solution two are mixed, the concentration range of dispersant each component is 0~1.0mol/L.
The heat treatment is to carry out burying burning in ZnO powders, and temperature is 600~800 DEG C.
Compared with prior art, the porous TiO that the present invention is provided2In the preparation method of block materials, with ethylenediamine tetrem
Acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol etc. are as dispersant, using specific colloidal sol
Process for preparation, makes ion more uniformly be present in gel, after gelation, is directly over the processes such as drying, briquetting, heat treatment and obtains
Obtain porous TiO2Block materials.By controlling the concentration of each material during this, the species and consumption of particularly each dispersant are matched somebody with somebody
Make in the xerogel powder of suitable straight forming, the method that titanium ion is uniformly and stably present in using gelation process solidifying
In rubber powder body, crystal grain forming process and loose structure forming process is set to unite two into one, this not only shortens manufacturing cycle, Er Qieli
With gelation process, crystal structure process is become more uniform, crystal grain particle diameter and be more evenly distributed, so that porous knot
Structure mesopore size and distribution are more uniform.
Embodiment
Embodiments of the present invention are described in detail with reference to embodiment.
Embodiment 1
A kind of porous TiO2The preparation method of block materials, comprises the following steps：
(1) butyl titanate is dissolved in 15mL absolute ethyl alcohols, then weighs dispersant (by ethylenediamine tetra-acetic acid, citric acid, two
Ethene triamine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol composition, wherein polyethylene glycol include polyethylene glycol 400, poly- second again
Glycol 4000 and Macrogol 6000) 35mL volume ratios are dissolved in for 1：In 1 absolute ethyl alcohol and deionized water mixed solution, stir
Mix uniform, two solution are mixed, the concentration of dispersant each component is controlled in 1mol/L, pH value is adjusted after stirring to 3~5 i.e.
Precursor solution is obtained, the wherein mol ratio of titanium ion and citric acid is 1：1.
(2) by precursor solution, in water-bath at 80 DEG C, to gelation, then at 140 DEG C, drying forms xerogel, at room temperature
Naturally powder is ground sieving after drying.
(3) by the direct dry pressing of dry powder after sieving, block blank of material is formed, finally block blank of material exists
Carry out burying to burn in ZnO powders obtaining porous TiO2Block materials, heat treatment temperature is 600 DEG C.The porous TiO of gained2Block materials
In be open-celled structure, crystallite dimension is about 150nm~300nm, and gap size is 100nm~150nm.
Embodiment 2
A kind of porous TiO2The preparation method of block materials, comprises the following steps：
(1) butyl titanate is dissolved in 15mL absolute ethyl alcohols, then weighs dispersant (by ethylenediamine tetra-acetic acid, citric acid, two
Ethene triamine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol composition) 35mL volume ratios are dissolved in for 1：3 absolute ethyl alcohol and go from
In sub- water mixed solution, stir, two solution are mixed, the concentration of dispersant each component is controlled in 0.5mol/L.Stirring is equal
After even, regulation pH value to 3~5 obtains precursor solution, and the wherein mol ratio of titanium ion and citric acid is 1：2.
(2) by precursor solution, in water-bath at 85 DEG C, to gelation, then at 160 DEG C, drying forms xerogel, at room temperature
Naturally powder is ground sieving after drying.
(3) by the direct dry pressing of dry powder after sieving, block blank of material is formed, finally block blank of material exists
Carry out burying to burn in ZnO powders obtaining porous TiO2Block materials, heat treatment temperature is 800 DEG C.The porous TiO of gained2Block materials
In be open-celled structure, crystallite dimension is about 150nm~300nm, and gap size is 100nm~150nm.
Embodiment 3
A kind of porous TiO2The preparation method of block materials, comprises the following steps：
(1) butyl titanate is dissolved in 15mL absolute ethyl alcohols, then weighs dispersant (by ethylenediamine tetra-acetic acid, citric acid, two
Ethene triamine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol composition) 35mL volume ratios are dissolved in for 1:2 absolute ethyl alcohol and go
In ion water mixed solution, stir, two solution mixed, the concentration of dispersant each component is controlled 0.01 respectively, 0.03,
0.1、0.2、0.4、1.0mol/L.After stirring, regulation pH value to 3~5 obtains precursor solution, wherein titanium ion and lemon
The mol ratio of lemon acid is 1：1.5.
(2) by precursor solution, in water-bath at 80 DEG C, to gelation, then at 150 DEG C, drying forms xerogel, at room temperature
Naturally powder is ground sieving after drying.
(3) by the direct dry pressing of dry powder after sieving, block blank of material is formed, finally block blank of material exists
Carry out burying to burn in ZnO powders obtaining porous TiO2Block materials, heat treatment temperature is 700 DEG C.The porous TiO of gained2Block materials
In be open-celled structure, crystallite dimension is about 150nm~300nm, and gap size is 100nm~150nm.
Claims (4)
1. a kind of porous TiO2The preparation method of block materials, using butyl titanate as raw material, absolute ethyl alcohol and deionized water are molten
Agent, makes precursor solution, then obtain porous TiO through gelation, drying, dry-pressing and heat treatment process using dispersant2Block
Body material；
The dispersant is by ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol and polyethylene glycol
Composition；
Characterized in that,
The butyl titanate adds into a part of absolute ethyl alcohol to obtain solution one, and the dispersant is added to deionized water and residue
Solution two is obtained in the mixed liquor of part absolute ethyl alcohol, then solution one and solution two are mixed evenly, regulation pH value to 3~5
Precursor solution, by precursor solution in water-bath at 80~85 DEG C to gelation, then dried at 140~160 DEG C and form dry
Gel, carries out ground sieve and obtains xerogel powder, then this xerogel powder is directly carried out into dry-pressing after drying naturally at room temperature
Shaping, forms block blank of material, finally thermally treated to produce porous TiO2Block materials.
2. porous TiO according to claim 12The preparation method of block materials, it is characterised in that the absolute ethyl alcohol and go
The volume ratio of ionized water is (1：1)~(1：3).
3. porous TiO according to claim 12The preparation method of block materials, it is characterised in that the butyl titanate and lemon
The mol ratio of lemon acid is 1：(1~2).
4. porous TiO according to claim 12The preparation method of block materials, it is characterised in that the heat treatment is in ZnO
Carry out burying burning in powder, temperature is 600~800 DEG C.
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| CN100411995C (en) * | 2004-09-15 | 2008-08-20 | 中国科学院合肥物质科学研究院 | Process for preparing titanium dioxide nano mesoporous balls |
| CN101279766A (en) * | 2008-04-25 | 2008-10-08 | 陕西科技大学 | Preparation of spherical nano-titanic oxide |
| CN101318694B (en) * | 2008-06-20 | 2010-06-16 | 浙江大学 | Method for preparing titanium dioxide nanocrystalline with highlight catalytic activity in low-temperature |
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