CN102380363A - Opal-carried nanometer titanium dioxide composite material - Google Patents
Opal-carried nanometer titanium dioxide composite material Download PDFInfo
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- CN102380363A CN102380363A CN2011102537775A CN201110253777A CN102380363A CN 102380363 A CN102380363 A CN 102380363A CN 2011102537775 A CN2011102537775 A CN 2011102537775A CN 201110253777 A CN201110253777 A CN 201110253777A CN 102380363 A CN102380363 A CN 102380363A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention discloses an opal-carried nanometer titanium dioxide composite material. The opal-carried nanometer titanium dioxide composite material is a photocatalyst, and comprises opal as a carrier and nanometer titanium dioxide coated on opal through gel. A preparation method of the opal-carried nanometer titanium dioxide composite material comprises the following steps of 1, uniformly mixing butyl titanate and absolute ethanol, adding an acetic acid solution into the mixture, and stirring for 1 to 3 hours, 2, adding opal into the mixed solution obtained by the step 1, and stirring for 1 to 3 hours, 3, slowly and dropwisely adding an alcohol-acid solution into the mixed solution with the opal by a separating funnel in a time period of 20 to 40 minutes, sharply stirring for 1 to 3 hours, and standing for aging for 8 to 16 hours, 4, washing the products obtained by the step 3 multiple times by absolute ethanol, and then washing the products by deionized water until a pH value of the products is 7, 5, putting the washed products into an oven, carrying out drying at a temperature of 80 to 120 DEG C for 1 to 3 hours, and 6, putting the dried products into a muffle furnace, and carrying out calcination at a temperature of 300 to 800 DEG C for 1 to 3 hours, and cooling to room temperature to obtain the opal-carried nanometer titanium dioxide composite material. The opal-carried nanometer titanium dioxide composite material has high quantum efficiency and a narrow spectrum response scope, is not easy to lose activity, is easy to be recovered, and has obvious effects of high-concentration waste water treatment.
Description
Technical field
The present invention relates to a kind of photoelectric semiconductor material.
Background technology
Since the eighties in 20th century, economy develops rapidly, and living standard improves day by day, and global environmental pollution and energy crisis are also serious day by day, and how effectively control is face of mankind and the key subjects that need to be resolved hurrily with curbing environmental pollution and solving energy problem.Water is the material base that the mankind depend on for existence; But in recent years along with industrial development, water pollutant increases gradually, and human body is caused very big harm; Especially micropollutants of difficult degradation in the water; Can cause anaemia like some metal ion, nervous function imbalance and visceral injury, disordered breathing etc. have a strong impact on people's health.Organic micro-pollutants in the water mainly contains chloride, phenols, hydro carbons, phenol etc., and is very big to the health influence equally.Method for treating water not only can produce secondary pollution at present, and the accessory substance THMs that is produced (Trihalomethanes, haloform) has " three cause " effect.The means that therefore various improvement are polluted have all received people and have paid close attention to greatly.
In numerous environmental pollution treatment technologies, conductor photocatalysis to be directly utilizing solar energy toxic pollutant mineralising the most at last, and is considered to the new technology revolution of the present depollution of environment.Fujishima in 1972 and Honda find that water is at TiO
2Photic decomposition reaction takes place on the monocrystalline electrode, and multiphase photocatalysis reaction having caused people's close attention has since then been carried out a large amount of research from the scholar in fields such as chemistry, physics and material to this.In numerous semiconductor light-catalysts, because nano-TiO
2Have characteristics such as high-specific surface area, high density, lattice defect and high-ratio surface ability; And chemical property is stable, nontoxic, catalytic activity is high, reaction speed is fast, organic degraded is not had selectivity and can make it remarkable advantages such as thorough mineralising, non-secondary pollution, work simplification, thereby becomes the most valued a kind of effective catalyst.
But simultaneously nano titanium oxide also exists quantum efficiency on the low side and spectral response range is narrow; Photochemical catalyst is prone to inactivation, the difficult recovery; To defectives such as the high-concentration waste water treatment effect are undesirable, how to improve its defective, make it apply to the focus that aspect such as environmental pollution improvement becomes people's research better.
Summary of the invention
The object of the present invention is to provide a kind of quantum efficiency high, be difficult for inactivation, be easy to reclaim, to the opal load nano-titanium dioxide composite of good waste water treatment effect.
The present invention mainly be a kind of be carrier with the opal, adhere to the composite of nano titanium oxide on it through gel.
The preparation method of above-mentioned composite is following:
One, the preparation of pure acid solution
1, raw material: mainly comprise absolute ethyl alcohol (chemical pure), red fuming nitric acid (RFNA) (65%-68%, chemical pure) and deionized water, their consumption is just like the lower volume proportionate relationship: absolute ethyl alcohol: deionized water: red fuming nitric acid (RFNA)=1-2: 0.3-0.7: 0.03-0.06.
2, preparation method: above-mentioned three kinds of raw materials are mixed and stir.
Two, the preparation of composite
1, raw material: mainly include butyl titanate (preferably chemical pure), absolute ethyl alcohol (preferably chemical pure), glacial acetic acid (preferably chemical pure), opal and above-mentioned pure acid solution.
Their consumption is just like the lower volume proportionate relationship: butyl titanate: absolute ethyl alcohol: acetum=1-2:3-5: 0.3-0.9, wherein acetum is the 70-90 % acetic acid by the glacial acetic acid preparation.
Opal is particle diameter 100 nanometers-10 micron, and said opal is made a general reference dissimilar opal both domestic and external, and is added with the 0.4-5g opal in every milliliter of butyl titanate.
2, preparation method:
(1) butyl titanate is evenly mixed with absolute ethyl alcohol, add acetum, vigorous stirring 1-3 h;
(2) in above-mentioned solution, slowly add opal, stir 1-3 h;
(3) in above-mentioned product, slowly drip above-mentioned pure acid solution with separatory funnel again, 20-40 min dropwises, again behind the vigorous stirring 1-3 h, and still aging 8-16 h;
(4) earlier with the above-mentioned product of absolute ethanol washing 2-3 time, be washed till neutrality with deionized water again, with the butyl titanate in the removal gel;
(5) above-mentioned product is placed 80-120 ℃ the dry 1-3 h of baking oven;
(6) product that drying is finished places Muffle furnace at 300-800 ℃ of roasting 1-3 h, and the crystal formation of nano titanium oxide is changed, and room temperature to be reduced to obtains product of the present invention.
Because the opal specific area is big; Have loose structure, adsorptivity is strong, advantages such as heat, good light stability; Utilize micro-nano technology to be ground into opal the powder of micro/nano level; Thereby nano titanium oxide is loaded on the opal, not only kept the good absorption property of opal but also given its excellent photocatalytic performance, avoided the industrial shortcoming that goes up nano titanium oxide serious agglomeration, bad recycling simultaneously.Utilize sol-gel process that nano titanium oxide is loaded on the carrier, under the irradiation of sunshine or ultraviolet light, can produce the very strong hydroxyl free radical of oxidation, thereby reach decomposing organic pollutant, the effect with air quality of purifying waste water.
The present invention compared with prior art has following advantage: quantum efficiency is high, and spectral response range is narrow, is difficult for inactivation, easy recovery, and is obvious to the high-concentration waste water treatment effect, is that the methylene blue solution removal efficiency of 20mg/L reaches 92% to initial concentration during 8h.
The specific embodiment
Embodiment 1:
Get 40 ml absolute ethyl alcohols (chemical pure), 10 ml deionized waters, 0.6 ml concentration and be 68% red fuming nitric acid (RFNA), stir, be prepared into alkyd solution with glass bar.10 ml butyl titanates (chemical pure) are evenly mixed with 40 ml absolute ethyl alcohols (chemical pure), and it is the acetum of 90 % that the back adds 3 g concentration, behind vigorous stirring 1 h; Slowly adding 4 g particle diameters is the opal of 100 nanometers, slowly drips above-mentioned alkyd solution with separatory funnel after stirring 3 h, dropwises behind 20 min; Behind vigorous stirring 3 h, still aging 12 h are earlier with absolute ethanol washing 2 times; Be washed till neutrality with deionized water again; After be placed on dry 2 h in 80 ℃ the baking oven, drying high-temperature roasting 3 h in the Muffle furnace that is placed on 300 ℃ that finish, room temperature to be reduced to obtains product of the present invention.
Embodiment 2:
Get 30 ml absolute ethyl alcohols (chemical pure), 6 ml deionized waters, 1.0 ml concentration and be 66% red fuming nitric acid (RFNA), stir, be prepared into alkyd solution with glass bar.15 ml butyl titanates (chemical pure) are evenly mixed with 50 ml absolute ethyl alcohols (chemical pure), and it is the acetum of 70 % that the back adds 9 g concentration, behind vigorous stirring 2 h; Slowly add 22 g particle diameters and be 10 microns opal, slowly drip above-mentioned alkyd solution with separatory funnel after stirring 2 h, dropwise behind 30 min; Behind vigorous stirring 2 h, still aging 8 h are earlier with absolute ethanol washing 2 times; Be washed till neutrality with deionized water again; After be placed on dry 3 h in 100 ℃ the baking oven, drying high-temperature roasting 2 h in the Muffle furnace that is placed on 500 ℃ that finish, room temperature to be reduced to obtains product of the present invention.
Embodiment 3:
Get 20 ml absolute ethyl alcohols (chemical pure), 14 ml deionized waters, 1.2 ml concentration and be 65% red fuming nitric acid (RFNA), stir, be prepared into alkyd solution with glass bar.20 ml butyl titanates (chemical pure) are evenly mixed with 30 ml absolute ethyl alcohols (chemical pure), and it is the acetum of 80 % that the back adds 6 g concentration, behind vigorous stirring 3 h; Slowly add 50 g particle diameters and be 0.5 micron opal, slowly drip above-mentioned alkyd solution with separatory funnel after stirring 1 h, dropwise behind 40 min; Behind vigorous stirring 1 h, still aging 16 h are earlier with absolute ethanol washing 3 times; Be washed till neutrality with deionized water again; After be placed on dry 1 h in 120 ℃ the baking oven, drying high-temperature roasting 1 h in the Muffle furnace that is placed on 800 ℃ that finishes, room temperature to be reduced to obtains product of the present invention.
Claims (2)
1. opal load nano-titanium dioxide photocatalysis agent is characterized in that: it is a carrier with the opal, adheres to the composite of nano titanium oxide on it through gel.
2. the preparation method of the opal load nano-titanium dioxide photocatalysis agent of claim 1 is characterized in that:
(1) preparation of pure acid solution:
(1) raw material: comprise that mainly absolute ethyl alcohol, concentration are red fuming nitric acid (RFNA) and the deionized water of 65%-68%, their consumption is just like the lower volume proportionate relationship: absolute ethyl alcohol: deionized water: red fuming nitric acid (RFNA)=1-2: 0.3-0.7: 0.03-0.06;
(2) preparation method: above-mentioned three kinds of raw materials are mixed and stir;
(2) preparation of composite:
(1) raw material: mainly include butyl titanate, absolute ethyl alcohol, glacial acetic acid, opal and above-mentioned pure acid solution;
Their consumption is just like the lower volume proportionate relationship: butyl titanate: absolute ethyl alcohol: acetum=1-2: 3-5: 0.3-0.9, and wherein acetum is the 70-90 % acetic acid by the glacial acetic acid preparation;
Opal is particle diameter 100 nanometers-10 micron, is added with the 0.4-5g opal in every milliliter of butyl titanate;
(2) preparation method:
1. butyl titanate is evenly mixed with absolute ethyl alcohol, add acetum, vigorous stirring 1-3 h;
2. slowly add opal, stir 1-3 h;
3. slowly drip above-mentioned pure acid solution with separatory funnel, 20-40 min dropwises, again behind the vigorous stirring 1-3 h, and still aging 8-16 h;
4. earlier with absolute ethanol washing 2-3 time, be washed till neutrality with deionized water again;
5. be placed on dry 1-3 h in 80-120 ℃ the baking oven;
6. drying finishes and is placed in the Muffle furnace at 300-800 ℃ of roasting 1-3 h.
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| CN2011102537775A CN102380363A (en) | 2011-08-31 | 2011-08-31 | Opal-carried nanometer titanium dioxide composite material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102806055A (en) * | 2012-07-26 | 2012-12-05 | 华中科技大学 | Method for preparing core-shell type composite with nano material coated with titanium dioxide |
| CN102993785A (en) * | 2012-11-13 | 2013-03-27 | 王丕轩 | Preparation method for TiO2/opal composite powder material |
| CN106693971A (en) * | 2016-12-14 | 2017-05-24 | 河南理工大学 | Preparation method of heterogeneous Fenton catalyst taking opoka as carrier |
| CN106799235A (en) * | 2017-02-28 | 2017-06-06 | 河南理工大学 | A kind of preparation method of the heterogeneous Fenton catalyst with opoka as carrier |
| CN110250083A (en) * | 2019-05-06 | 2019-09-20 | 中国计量大学 | A kind of seawater fish jar with purification of water quality ability makes scape stone and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101033089A (en) * | 2006-05-24 | 2007-09-12 | 吴丽娜 | Photocatalysis anion water purifier |
| CN101322944A (en) * | 2008-07-28 | 2008-12-17 | 吉林大学 | Composite photocatalyst prepared from stephanoporate mineral and method thereof |
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2011
- 2011-08-31 CN CN2011102537775A patent/CN102380363A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033089A (en) * | 2006-05-24 | 2007-09-12 | 吴丽娜 | Photocatalysis anion water purifier |
| CN101322944A (en) * | 2008-07-28 | 2008-12-17 | 吉林大学 | Composite photocatalyst prepared from stephanoporate mineral and method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘莹峰等: "超细蛋白石制备及其性能研究", 《齐齐哈尔大学学报》, vol. 19, no. 3, 30 September 2003 (2003-09-30), pages 79 - 80 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102806055A (en) * | 2012-07-26 | 2012-12-05 | 华中科技大学 | Method for preparing core-shell type composite with nano material coated with titanium dioxide |
| CN102993785A (en) * | 2012-11-13 | 2013-03-27 | 王丕轩 | Preparation method for TiO2/opal composite powder material |
| CN102993785B (en) * | 2012-11-13 | 2015-01-14 | 王丕轩 | Preparation method for TiO2/opal composite powder material |
| CN106693971A (en) * | 2016-12-14 | 2017-05-24 | 河南理工大学 | Preparation method of heterogeneous Fenton catalyst taking opoka as carrier |
| CN106799235A (en) * | 2017-02-28 | 2017-06-06 | 河南理工大学 | A kind of preparation method of the heterogeneous Fenton catalyst with opoka as carrier |
| CN110250083A (en) * | 2019-05-06 | 2019-09-20 | 中国计量大学 | A kind of seawater fish jar with purification of water quality ability makes scape stone and preparation method thereof |
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Application publication date: 20120321 |