CN101623625A - Bulky macro-pore titanium dioxide material and preparation method thereof - Google Patents
Bulky macro-pore titanium dioxide material and preparation method thereof Download PDFInfo
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- CN101623625A CN101623625A CN200810012244A CN200810012244A CN101623625A CN 101623625 A CN101623625 A CN 101623625A CN 200810012244 A CN200810012244 A CN 200810012244A CN 200810012244 A CN200810012244 A CN 200810012244A CN 101623625 A CN101623625 A CN 101623625A
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- titanium dioxide
- organic foam
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 53
- 239000000463 material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims description 24
- 239000011148 porous material Substances 0.000 title abstract description 15
- 239000006260 foam Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000006259 organic additive Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 239000002002 slurry Substances 0.000 claims description 24
- 238000005245 sintering Methods 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- 159000000013 aluminium salts Chemical class 0.000 claims description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 159000000003 magnesium salts Chemical class 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 239000000203 mixture Substances 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000012153 distilled water Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 210000004911 serous fluid Anatomy 0.000 abstract 2
- 230000003100 immobilizing effect Effects 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010815 organic waste Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical class [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of catalytic environmental protection, and in particular relates to a method for preparing a bulky macro-pore titanium dioxide material. The aperture of the bulky macro-pore titanium dioxide material is between 200 and 300 micrometers, and the porosity factor thereof is between 80 and 90 percent. The bulky macro-pore titanium dioxide material is prepared by using organic foam as a template which is impregnated in a serous fluid containing titanium dioxide so that the serous fluid is adhered to the organic foam, and calcining the template to remove the organic foam. In the method, titanium dioxide powder is dispersed into distilled water by stirring, and with the assistance of an organic additive, the mixture is adhered to the organic foam, thus the problems that the prior powdered titanium dioxide material is difficult to reclaim and is easy to agglomerate in use can be solved, and a novel matrix material is provided for easily reclaiming the titanium dioxide material or immobilizing other nanometer photocatalysis materials.
Description
Technical field
The invention belongs to catalytic environment resist technology field, be specially a kind of method for preparing block macroporous titanium dioxide material.
Background technology
Along with the continuous progress of human society and the develop rapidly of industry, the discharge capacity of industrial wastewater increases year by year, and mostly has the organic concentration height, biological degradability difference even characteristics such as bio-toxicity are arranged is all given the comprehensive regulation of this type of high concentration hard-degraded organic waste water both at home and abroad and is paid much attention to.At present, the part composition is simple, and biological degradability omits, and the waste water that concentration is lower can obtain handling by making up traditional technology, and the concentration height is difficult to biodegradable waste water treatment work and has very big difficulty technically and economically.Someone predicts, if water resources problems can not get solving, also might cause the global war of using the water resource right for contention, become great economy, society, morals, fitness-for-all problem so water pollutes, 21st century solves human water resources problems and has just become a great challenge.
Although traditional method for treating water can reach the good treatment effect, cause secondary pollution easily.Adopting the pollutant in the photocatalysis technology degrading waste water is a kind of wastewater purification technology that has prospect, has become a research focus in the environmental improvement work in recent years.In the advanced treating and the reuse of waste water, remove hardly degraded organic substance, drink aspect such as underwater micro-organic matter and demonstrate great potential.Photochemical catalyst is the key factor in the photochemical catalytic oxidation process, commonly used have conductor oxidate, sulfide, iodide etc., wherein titanium dioxide is as a kind of semiconductor oxidation photocatalyst, it is good to have chemical stability, the photocatalytic activity height, advantage such as harmless and low price and being widely used.
Also mainly rest on laboratory stage about titanium dioxide in the application aspect the water purification, titanium dioxide mainly is that form with nano powder is dispersed in the water in lab process, and there are two shortcomings in this type of service, the one: be difficult to reclaim; The 2nd: nano powder is reunited easily, thereby has reduced catalytic activity.In order in industry, to use the purpose that technology in this reaches water purification well, must address the above problem.
Summary of the invention
The object of the present invention is to provide a kind of block macroporous titanium dioxide material and preparation method thereof, can well immobilized titanium dioxide, be difficult to from water, reclaim and easy problem of reuniting to solve present nano-powder, and can be used as the carrier of other catalysis material, be used for fields such as environmental protection, chemical industry.
Technical scheme of the present invention is:
A kind of block macroporous titanium dioxide material, the aperture of block macroporous titanium dioxide material is between 200～300 μ m, and porosity is between 80%～90%.
Described block macroporous titanium dioxide preparation methods is a template with the organic foam, and dipping contains the slurries of titanium dioxide, and slurries stick on the organic foam, removes organic foam by calcining, obtains block macroporous titanium dioxide material.
Described block macroporous titanium dioxide preparation methods, concrete preparation process is as follows:
At first, titania powder and the distilled water part by weight with 1: 20～1: 11 is mixed, add the organic additive of 0.5wt%～3wt% and the inorganic additive of 0.001wt%～0.01wt% simultaneously, be dispersed into uniform thick liquid slurry; Then, organic foam is immersed the liquid slurry, ultrasonic dispersion 10～20min, with the mode of extruding unnecessary slurry is extruded then, the organic foam that is stained with slurry that makes in 70 ℃～110 ℃ electrically heated drying cabinets after dry 24 hours, is removed the porous material that organic foam can obtain different apertures and porosity with the dried foam that is stained with titania slurry sintering under different temperatures such as 1000 ℃～1400 ℃.
Described block macroporous titanium dioxide preparation methods, titanium dioxide are commercial or homemade titania powder, and granularity is 10nm～100nm.First-selected titanic oxide material is commercial P25 type titanium dioxide.Wherein, P25 is a kind of rutile phase and anatase mixture mutually, and wherein anatase accounts for 80wt%, rutile phase 20wt%, specific area 55m
2/ g.
Described block macroporous titanium dioxide preparation methods, organic additive can be one or more of polyethylene glycol, methylcellulose, hydroxyethylcellulose or ethyl orthosilicate; Inorganic additive can form the salt of low-melting compound for magnesium metal salt, metallic aluminium salt or other.
Described block macroporous titanium dioxide preparation methods, organic foam is a polyurethane foam, and its aperture is at 500～900 μ m, and thickness is 0.5 inch, can be cut into arbitrary shape.
Described block macroporous titanium dioxide preparation methods, as required, block macroporous titanium dioxide material is made different shape, as ring-type or square column etc.
Described block macroporous titanium dioxide preparation methods, block macroporous titanium dioxide material is directly as catalyst, or the carrier of catalyst.
Design principle of the present invention is as follows:
The organic foam template is a kind of method for preparing high porosity percent opening material of simple, easy operating, and the porous material of perforate since the superiority of its mass transfer, heat transfer having broad application prospects aspect catalysis and the catalyst carrier.Therefore, the present invention reaches the immobilization of titanium dioxide optical catalyst by a kind of simple porous material preparation method.
The invention has the advantages that:
1. the present invention's organic foam is a template, and the shape of template can arbitrarily be cut out by organic foam, and is simple to operate, is easy to control, and cost is lower.Porosity can reach more than 80% than higher, and is the porous material of perforate.
2. the porous material among the present invention is to be template by organic foam, the slurries of dipping titanium dioxide, and slurries stick on the organic foam under the modification of organic additive, obtain at different temperature lower calcinations.The present invention improves the viscosity of slurries by being added with organic additive, still can obtain good slurries adhesiving effect under the very big situation of the ratio of titania powder and distilled water.
3. the present invention reduces the sintering temperature of titanium dioxide by adding the metallic salt can form low-melting compound, is issued to the purpose of sintering in the temperature that is lower than the titanium dioxide fusing point.
Description of drawings:
Fig. 1 is the preparation flow figure that template prepares the block macroporous titanium dioxide material of perforate for organic foam.
Fig. 2 is the organic foam micro-structure diagram.
Fig. 3 is the SEM photo of the porous material that makes.
Fig. 4 is the photo of the porous material that makes.
Fig. 5 is the linear shrinkage ratio of material during sintering under the different temperatures.
Fig. 6 is the porosity of material during sintering under the different temperatures.
The specific embodiment:
As shown in Figure 1, the technological process of the block macroporous titanium dioxide material preparation method of the present invention is as follows:
At first, titanium dioxide, water, additive are mixed, carry out ultrasonic dispersion, form colloidal sol (thick liquid slurry); Then, organic foam is immersed in the colloidal sol, carry out soaking paste and handle; After the low temperature drying, sintering is removed organic foam.
Embodiment
As shown in Figure 2, the polyurethane organic foam is handled 15min for 70 ℃ through the NaOH of 15wt% solution, to remove the barrier film that defoams between the muscle of hole.With titania powder (P25 type, granularity be 10～50nm) and distilled water mix with 1: 20～1: 11 part by weight, add the inorganic additive of the organic additive of 0.5wt%～3wt% and 0.001wt%～G.01wt% simultaneously, ultrasonic dispersion 10 minutes; When waiting to be dispersed into uniform thick liquid slurry, the organic foam of handling is immersed thick liquid starch ultrasonic 20 minutes; With the mode of extruding unnecessary slurry is extruded then, with the organic foam that is stained with slurry that makes behind 110 ℃ of dry 24h, the foamed material that each composition dipping in the above-mentioned example is obtained is (1000 ℃～1400 ℃) sintering under different temperature respectively, removes organic foam.Fig. 3 is the SEM photo of the porous material that makes, and Fig. 4 is the photo of the porous material that makes, and from Fig. 3-Fig. 4 as can be seen, the aperture of porous material is in 200～300 mu m ranges.
Table 1
Same slurry composition (table 1 embodiment 4), during sintering, the linear shrinkage ratio of material is as shown in table 2 under different temperatures:
Table 2
Fig. 5 is the linear shrinkage ratio of material during sintering under the different temperatures, as can be seen from Figure 5 along with the rising of sintering temperature, the linear shrinkage of material also increases in the sintering process, from 1000 ℃ to 1200 ℃ change procedure, shrinking than very fast, the change procedure, shrinkage factor begins slack-off from 1200 ℃ to 1300 ℃.
Same slurry composition (table 1 embodiment 4), during sintering, the porosity of material is as shown in table 3 under different temperatures:
Table 3
Fig. 6 is the porosity of material during sintering under the different temperatures, and the percent opening of the porous material that makes with this kind method still can reach more than 80% behind 1400 ℃ of sintering than higher.
Embodiment result shows, the present invention is for being template with the organic foam, and the block titanic oxide material of preparation macropore provides a kind of new matrix material for the easy recoveryization that reaches titanic oxide material or for the immobilization of other nano-photocatalyst material.
Claims (9)
1. a block macroporous titanium dioxide material is characterized in that, the aperture of block macroporous titanium dioxide material is between 200～300 μ m, and porosity is between 80%～90%.
2. according to the described block macroporous titanium dioxide preparation methods of claim 1, it is characterized in that, is template with the organic foam, dipping contains the slurries of titanium dioxide, slurries stick on the organic foam, remove organic foam by calcining, obtain block macroporous titanium dioxide material.
3. according to the described block macroporous titanium dioxide preparation methods of claim 2, it is characterized in that the preparation process of slurries that contains titanium dioxide is as follows:
Titania powder and the distilled water part by weight with 1: 20～1: 11 is mixed, add the organic additive of 0.5wt%～3wt% and the inorganic additive of 0.001wt%～0.01wt% simultaneously, be dispersed into uniform thick liquid slurry.
4. according to the described block macroporous titanium dioxide preparation methods of claim 2, it is characterized in that, after organic foam immersed liquid slurry, ultrasonic dispersion 10～20 minutes, with the mode of extruding unnecessary slurry is extruded then, after the organic foam drying that is stained with slurry that makes, remove organic foam at 1000 ℃～1400 ℃ sintering.
5. according to the described block macroporous titanium dioxide preparation methods of claim 3, it is characterized in that titanium dioxide is commercial or homemade titania powder, its granularity is 10nm～100nm.
6. according to the described block macroporous titanium dioxide preparation methods of claim 3, it is characterized in that organic additive is one or more of polyethylene glycol, methylcellulose, hydroxyethylcellulose or ethyl orthosilicate; Inorganic additive is that metal magnesium salts, metallic aluminium salt or some other can form the metallic salt of low-melting compound.
7. according to the described block macroporous titanium dioxide preparation methods of claim 2, it is characterized in that the concrete material of organic foam is the polyurethane organic foam, its aperture is 500～900 μ m, and thickness is 0.5 inch.
8. according to the described block macroporous titanium dioxide preparation methods of claim 2, it is characterized in that as required, block macroporous titanium dioxide material is made different shape.
9. according to the described block macroporous titanium dioxide preparation methods of claim 2, it is characterized in that block macroporous titanium dioxide material is directly as catalyst, or the carrier of catalyst.
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| CN200810012244A CN101623625A (en) | 2008-07-09 | 2008-07-09 | Bulky macro-pore titanium dioxide material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830504A (en) * | 2010-04-19 | 2010-09-15 | 中国科学院广州能源研究所 | Method for preparing multistage pore titanium oxide foam block material |
| CN101900681A (en) * | 2010-07-23 | 2010-12-01 | 哈尔滨工业大学 | Water body chemical oxygen demand rapid measurement device |
| CN102451671A (en) * | 2010-10-29 | 2012-05-16 | 中国科学院金属研究所 | Complex-phase block-shaped macroporous titanium dioxide material and preparation method thereof |
| CN103447099A (en) * | 2013-09-27 | 2013-12-18 | 上海第二工业大学 | Method for manufacturing block photocatalytic material by using foaming method |
| CN105110787A (en) * | 2015-07-31 | 2015-12-02 | 武汉理工大学 | Method for preparing photocatalytic foamed ceramics |
| CN108511664A (en) * | 2018-03-30 | 2018-09-07 | 吉林师范大学 | A kind of lithium-sulfur cell diaphragm and preparation method thereof |
-
2008
- 2008-07-09 CN CN200810012244A patent/CN101623625A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830504A (en) * | 2010-04-19 | 2010-09-15 | 中国科学院广州能源研究所 | Method for preparing multistage pore titanium oxide foam block material |
| CN101900681A (en) * | 2010-07-23 | 2010-12-01 | 哈尔滨工业大学 | Water body chemical oxygen demand rapid measurement device |
| CN102451671A (en) * | 2010-10-29 | 2012-05-16 | 中国科学院金属研究所 | Complex-phase block-shaped macroporous titanium dioxide material and preparation method thereof |
| CN103447099A (en) * | 2013-09-27 | 2013-12-18 | 上海第二工业大学 | Method for manufacturing block photocatalytic material by using foaming method |
| CN103447099B (en) * | 2013-09-27 | 2016-04-27 | 上海第二工业大学 | A kind of foaming prepares the method for block catalysis material |
| CN105110787A (en) * | 2015-07-31 | 2015-12-02 | 武汉理工大学 | Method for preparing photocatalytic foamed ceramics |
| CN108511664A (en) * | 2018-03-30 | 2018-09-07 | 吉林师范大学 | A kind of lithium-sulfur cell diaphragm and preparation method thereof |
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Application publication date: 20100113 |