CN1332908C - Process for preparing porous titanium dioxide ceramic - Google Patents
Process for preparing porous titanium dioxide ceramic Download PDFInfo
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- CN1332908C CN1332908C CNB2005101198379A CN200510119837A CN1332908C CN 1332908 C CN1332908 C CN 1332908C CN B2005101198379 A CNB2005101198379 A CN B2005101198379A CN 200510119837 A CN200510119837 A CN 200510119837A CN 1332908 C CN1332908 C CN 1332908C
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- suspension
- tio
- tio2
- polymethylmethacrylate
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Abstract
The present invention discloses a preparation method for porous titanium dioxide ceramic. The present invention is characterized in that spherical polymethylmethacrylate and TiO2 are used as main raw materials, and polyethylenimine and glycol are used as auxiliary raw materials. Distilled water is respectively added in the polymethylmethacrylate and the TiO2 so as to manufacture suspensions, and the pH values of the two suspensions can be strictly controlled. The polyethylenimine is added in the TiO2 suspension and is used as dispersing agent for ultrasound. The TiO2 suspension after ultrasound can be slowly added in the polymethylmethacrylate suspension which is slowly mixed and is added with the glycol. After the processes of vacuum pumping filter, drying and calcining, the mixed suspension can fabricate TiO2 nano stage porous ceramic with controllable hole diameter dimension and uniform hole diameter distribution. The present invention has the characteristics of simple production device, convenient operation and easy control, and the fabricated TiO2 porous ceramic has the characteristics of controllable hole diameter dimension and uniform hole diameter distribution.
Description
Technical field
The present invention relates to a kind of preparation method of micrometer level porous titanium dioxide ceramic, the preparation method of the micrometer level porous titanium dioxide ceramic that particularly a kind of even aperture distribution and aperture size are controlled.
Background technology
Because TiO
2Porous ceramics is in catalysis, separates, and more and more attracting people's interest in the widespread use aspect lightweight structural material and the biomaterial, particularly at water treatment research field, TiO
2That porous ceramics has is efficient, energy-conservation, cleaning, nontoxic, advantage such as the catalysis scope is wide, has broad application prospects aspect environment.At present, preparation TiO
2The porous ceramics method is a lot, and what wherein people were with the most use is to add pore-forming material, foam impregnation method, sol-gel method.Wherein people are with the most use is to add pore-forming material, and by the dry pressing preparation, but the prepared porous ceramics size distribution of this technology is inhomogeneous, and pore size presents randomness, and the employed organic pore-forming agents of this kind method can produce a large amount of tiny cracks.
Summary of the invention
The object of the present invention is to provide the preparation method of the controlled micrometer level porous titanium dioxide ceramic of a kind of even aperture distribution and aperture size.
The present invention utilizes the polymer suspension polymerization technique, with TiO
2Ceramic particle and spherical polymethylmethacrylate are made suspension respectively, as template, have successfully prepared even aperture distribution, the TiO of controllable aperture with single dispersive pore-forming material polymethylmethacrylate
2Porous ceramics.
Concrete preparation process may further comprise the steps:
(1) selects satisfactory spherical polymethyl methacrylate, TiO for use
2Be main raw material, polymine and ethylene glycol are auxiliary material;
(2) with above-mentioned main raw material polymethyl methacrylate and TiO
2Adding distil water is made suspension respectively, and the pH that adjusts separately is 7-9; At TiO
2Adding polymine in the suspension makes its dispersion agent and carries out ultrasonic; With ultrasonic good TiO
2Suspension adds in the suspension of polymethylmethacrylate at leisure, slowly stirs and adds ethylene glycol;
(3) above-mentioned mixed suspension is passed through vacuum filtration, in air, dry in the shade, thereby obtain polymethylmethacrylate and TiO
2Complex body; When treating that complex body moisture is fewer, it is dry that it is put into loft drier, and heating is then put into electric furnace in 200 ℃ of calcining 1.5-3h down with complex body, and 500 ℃ are continued behind the calcining 3-4h naturally cooling in electric furnace down, thus the TiO that obtains having even aperture distribution
2Micrometer level porous pottery.
Above-mentioned polymine molecular weight is 10000; The void content of porous ceramics can be by changing polymkeric substance and TiO
2The volume ratio of particle suspension liquid is controlled; The pore dimension of porous ceramics can be controlled by the size that changes polymkeric substance, to satisfy the requirement of different aperture size.
Production unit of the present invention is simple, and is easy to operate, easily control; Prepared TiO
2Porous ceramics has the controlled and equally distributed characteristics in aperture of aperture size.
Embodiment
Embodiment one
(1) selects spherical polymethyl methacrylate of 700nm and 500nmTiO for use
2Be main raw material, polymine and ethylene glycol are auxiliary material;
(2) with above-mentioned main raw material polymethyl methacrylate and TiO
2Adding distil water is made suspension respectively, and adjusts pH value separately, by potential measurement, selects for use the pH=7.8 can be so that both can be good at sticking; Wherein at TiO
2Adding the 0.05wt% polymine in the suspension makes its dispersion agent and carried out ultrasonic 10 minutes;
(3) consider controllable aperture, select for use suspension vol to compare TiO
2/ polymethylmethacrylate=0.3
With ultrasonic good TiO
2Suspension adds in the suspension of polymethylmethacrylate at leisure, slowly stirs and adds 0.1wt% ethylene glycol;
(4) above-mentioned mixed suspension is passed through vacuum filtration, in air, dry in the shade, thereby obtain polymethylmethacrylate and TiO
2Complex body;
When (5) treating that above-mentioned complex body moisture is fewer, it is dry that it is put into loft drier, with the rate of heating of 1 ℃/min, complex body put into electric furnace calcine 2h down in 200 ℃ then, 500 ℃ continue down calcining 4h after in electric furnace naturally cooling, thereby the TiO that obtains having even aperture distribution
2Micrometer level porous pottery, the sample gas porosity behind the sintering is measured as 78.2% by Archimedes's method, and scanning electron microscopic observation is to the about 600nm of pore dimension size.
Embodiment two
(1) selects the spherical polymethyl methacrylate of about 600nm and about 400nmTiO for use
2Be main raw material, polymine and ethylene glycol are auxiliary material;
(2) with above-mentioned main raw material polymethyl methacrylate and TiO
2Adding distil water is made suspension respectively, and adjusts pH value separately, by potential measurement, selects for use the pH=7.8 can be so that both can be good at sticking; Wherein at TiO
2Adding the 0.05wt% polymine in the suspension makes its dispersion agent and carried out ultrasonic 10 minutes;
(3) consider controllable aperture, select TiO for use
2/ polymethylmethacrylate (suspension vol ratio)=0.4
With ultrasonic good TiO
2Suspension adds in the suspension of polymethylmethacrylate at leisure, and slowly stir and add 0.1wt% ethylene glycol,
(4) above-mentioned mixed suspension is passed through vacuum filtration, in air, dry in the shade, thereby obtain polymethylmethacrylate and TiO
2Complex body;
When (5) treating that above-mentioned complex body moisture is fewer, it is dry that it is put into loft drier, with the rate of heating of 1 ℃/min, complex body put into electric furnace calcine 2h down in 200 ℃ then, 500 ℃ continue down calcining 4h after in electric furnace naturally cooling, thereby the TiO that obtains having even aperture distribution
2Micrometer level porous pottery, the sample gas porosity behind the sintering is measured as 74.8% by Archimedes's method, and scanning electron microscopic observation is to the about 450nm of pore dimension size.
Claims (4)
1. the preparation method of a porous titanium dioxide ceramic is characterized in that the steps include:
(1) with spherical polymethyl methacrylate and TiO
2Be main raw material, polymine and ethylene glycol are auxiliary material;
(2) with polymethyl methacrylate and TiO
2Adding distil water is made suspension respectively, and the pH value of two kinds of suspension of strict control is 7-9; At TiO
2Adding polymine in the suspension makes its dispersion agent and carries out ultrasonic; With ultrasonic good TiO
2Suspension adds in the suspension of polymethylmethacrylate at leisure, slowly stirs and adds ethylene glycol;
(3) above-mentioned mixed suspension is passed through vacuum filtration, in air, dry in the shade, thereby obtain polymethylmethacrylate and TiO
2Complex body; When treating that complex body moisture is fewer, it is dry that it is put into loft drier, and heating is then put into electric furnace in 200 ℃ of calcining 1.5-3h down with complex body, and 500 ℃ are continued behind the calcining 3-4h naturally cooling in electric furnace down, thus the TiO that obtains having even aperture distribution
2Micrometer level porous pottery.
2. preparation method as claimed in claim 1 is characterized in that the polymine molecular weight is 10000.
3. preparation method as claimed in claim 1, the void content that it is characterized in that porous ceramics is by changing polymethyl methacrylate and TiO
2The volume ratio of particle suspension liquid is controlled.
4. preparation method as claimed in claim 1 is characterized in that the pore dimension of porous ceramics is controlled by the size that changes polymethyl methacrylate, to satisfy the requirement of different aperture size.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101198379A CN1332908C (en) | 2005-11-08 | 2005-11-08 | Process for preparing porous titanium dioxide ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101198379A CN1332908C (en) | 2005-11-08 | 2005-11-08 | Process for preparing porous titanium dioxide ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1793027A CN1793027A (en) | 2006-06-28 |
| CN1332908C true CN1332908C (en) | 2007-08-22 |
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ID=36804691
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005101198379A Expired - Fee Related CN1332908C (en) | 2005-11-08 | 2005-11-08 | Process for preparing porous titanium dioxide ceramic |
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| Country | Link |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101265121B (en) * | 2008-04-02 | 2011-07-06 | 西安理工大学 | Method for preparing porous ceramic by electrostatic field and magnetic field co-inducing crystallization technique |
| CN103360047B (en) * | 2013-07-25 | 2015-04-01 | 中国石油化工股份有限公司 | TiO2 ceramic and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6245849B1 (en) * | 1999-06-02 | 2001-06-12 | Sandia Corporation | Fabrication of ceramic microstructures from polymer compositions containing ceramic nanoparticles |
| CN1554617A (en) * | 2003-12-26 | 2004-12-15 | 四川大学 | Biological active nano titanium oxide ceramic for hard tissue repairing and its preparing method |
| CN1587325A (en) * | 2004-08-05 | 2005-03-02 | 复旦大学 | High stability high transparency rutile type nano titanium dioxide slurry and its dispersively preparing method |
| CN1644631A (en) * | 2004-12-27 | 2005-07-27 | 华南师范大学 | Production of nanometer titanium dioxide particle with organic film coating |
| JP2005255952A (en) * | 2004-03-15 | 2005-09-22 | Mitsubishi Pencil Co Ltd | Water-based ink composition |
-
2005
- 2005-11-08 CN CNB2005101198379A patent/CN1332908C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6245849B1 (en) * | 1999-06-02 | 2001-06-12 | Sandia Corporation | Fabrication of ceramic microstructures from polymer compositions containing ceramic nanoparticles |
| CN1554617A (en) * | 2003-12-26 | 2004-12-15 | 四川大学 | Biological active nano titanium oxide ceramic for hard tissue repairing and its preparing method |
| JP2005255952A (en) * | 2004-03-15 | 2005-09-22 | Mitsubishi Pencil Co Ltd | Water-based ink composition |
| CN1587325A (en) * | 2004-08-05 | 2005-03-02 | 复旦大学 | High stability high transparency rutile type nano titanium dioxide slurry and its dispersively preparing method |
| CN1644631A (en) * | 2004-12-27 | 2005-07-27 | 华南师范大学 | Production of nanometer titanium dioxide particle with organic film coating |
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|---|---|
| CN1793027A (en) | 2006-06-28 |
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