CN100430127C - Process for preparing photo-catalytic materials by using strong magnetic field modified titanium-rich slag - Google Patents
Process for preparing photo-catalytic materials by using strong magnetic field modified titanium-rich slag Download PDFInfo
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- CN100430127C CN100430127C CNB2006100471715A CN200610047171A CN100430127C CN 100430127 C CN100430127 C CN 100430127C CN B2006100471715 A CNB2006100471715 A CN B2006100471715A CN 200610047171 A CN200610047171 A CN 200610047171A CN 100430127 C CN100430127 C CN 100430127C
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Abstract
The present invention relates to a method for preparing photo-catalytic materials by using modified titanium-rich slag with strong magnetic fields. The high titanium slag with TiO2 greater than or equal to 87.67% is manually crushed down, is further pulverized, and is carried with ball milling to achieve the average particle size below 5 micrometers. The high titanium slag with ball milling is calcined and activated for one to three hours in constant temperature under the temperature of 400 DEG C to 1200 DEG C, and is milled into fine powder after the temperature is naturally cooled to indoor temperature, and the average particle size achieves below 5 micrometers. The high titanium slag powder is pressed and shaped in one direction, and is arranged in a crucible. The crucible is arranged in a superconductive strong magnetic field system to carry out magnetism increase, the magnetic field strength is 1 T to 12 T, the temperature is raised to 750 DEG C to 900 DEG C, the high titanium slag powder is activated and modified for 0.5 hour to 1.5 hour, the magnetism is reduced to 0 T, the high titanium slag powder is ground into the powder after the temperature is naturally cooled to the room temperature, the average particle size achieves below 5 micrometers, and materials with photo-catalytic activity are prepared. The present invention has simple manufacturing technology, and can effectively develop and utilize the limited titan resource of China. The product cost is low, and the present invention can be widely used for fields of building materials, environment protection, chemical industry, etc.
Description
Technical field
The invention belongs to new material technology field, relate to the preparation of catalysis material, be specifically related to a kind of method of utilizing strong magnetic field modified titanium-rich slag to prepare catalysis material.
Background technology
The Fujishima of Japan in 1972 and Honda find to be subjected to the TiO of light radiation
2The lasting redox reaction that water can take place on the surface (please refer to Fujishima A, Honda K.Photocatalysis of water at a semiconductorelectrode[J], Nature, 1972,238 (5358): 37-38), S.N.Frank in 1976 etc. are used for the photocatalytic degradation pollutant with semi-conducting material and (please refer to Frank S.N, Bard A.J.Heterogeneous photcatalytic oxidation of cyanideion in aqueous solutions at TiO
2Powder[J], J.Am.Chem.Soc., 1977,99 (1): 303-304), the heterogeneous light-catalyzed reaction of semiconductor has obtained going deep into extensive studies since then.Studies show that semi-conductive photocatalysis is that semiconductor produces electron-hole pair under visible light or action of ultraviolet light, and be adsorbed on the O of semiconductor surface
2, H
2O and contaminant molecule are accepted light induced electron or hole, and a series of redox reactions take place, and make toxic pollutant be degraded into material nontoxic or that toxicity is less, thereby form the photocatalytic degradation process.The semiconductor light-catalyst of broad research has TiO at present
2, ZnO, CdS, WO
3, Fe
2O
3, PBs, SnO
2, In
2O
3, ZnS, SrTiO
3, SiO
2Deng tens kinds.These conductor oxidates all have certain photocatalytic activity, but wherein most of chemistry or photochemical corrosion of easily taking place.TiO
2Have good chemical stability and nontoxic, can not cause secondary pollution, it also has characteristics such as oxidability is strong, catalytic activity height in addition, is good anti-biotic material, but pure TiO
2The cost height.
If can replace pure titinium dioxide as catalysis material with high titanium slag, can make full use of the mineral resources of China, not only reduce the cost of catalysis material, and rationally be used for environmental improvement and utilize approach for a large amount of high titanium slag of China provides.
Summary of the invention
At present TiO
2Catalysis material preparation method and high titanium slag utilize the weak point of method, the invention provides a kind of method of utilizing strong magnetic field modified titanium-rich slag to prepare catalysis material.
Catalysis material provided by the present invention adopts high titanium slag to form through pulverizing, roasting, high high-intensity magnetic field activation modification.
Described high titanium slag, the titaniferous amount is with TiO
2Meter, TiO by weight percentage
2〉=87.67%.
The preparation of catalysis material provided by the present invention and method of modifying, processing step is as follows:
1, ball milling: high titanium slag is manually smashed earlier, and with its further pulverizing, this moment, granularity can reach the hundreds of micron on sampling machine.And then reach below 5 microns through smooth roll ball mill ball milling to its particle mean size.
2, roasting: the high titanium slag that ball milling is good is put into Muffle furnace, and under 400～1200 ℃ of temperature, constant temperature calcining activation 1～3 hour is worn into fine powder after high titanium slag naturally cooled to room temperature, and particle mean size reaches below 5 microns.
3, high high-intensity magnetic field activation modification: with above-mentioned high titanium slag powder with press model machine in the mould unidirectional molded after, be placed in the crucible.Then crucible is placed in the superconducting intense magnetic field system and rises magnetic, magnetic field intensity is 1～12T, and temperature is risen to 750～900 ℃, and activation modification is 0.5～1.5 hour under this magnetic field condition and temperature conditions, falls magnetic to 0T.After naturally cooling to room temperature the high titanium slag behind the activation modification is pulverized, its particle mean size reaches below 5 microns.
Through above-mentioned PROCESS FOR TREATMENT, the titanium in the titanium-contained slag changes the material with photocatalytic activity into.
Catalysis material provided by the invention is raw material with the high titanium slag, be prepared from through simple ball mill grinding and activating process such as roasting, high high-intensity magnetic field, cost is low, can be widely used in building materials, environmental protection, fields such as chemical industry, and developing and using limited titanium resource more effectively have very great economic implications.
Description of drawings
Accompanying drawing is the X ray diffracting spectrum of high titanium slag.
The specific embodiment
The high titanium slag of implementing to adopt comes from jinzhou Ferroalloy Plant.Table 1 is the chemical composition of high titanium slag.
The chemical composition of table 1 high titanium slag (weight %)
Embodiment 1
1, ball milling: high titanium slag is manually smashed earlier, and with its further pulverizing, this moment, granularity can reach the hundreds of micron on sampling machine.And then, reach below 5 microns to its particle mean size through smooth roll ball mill mill about 200 hours.
2, roasting: the high titanium slag that ball milling is good is put into Muffle furnace, and under 800 ℃ of temperature, constant temperature calcining activation 2 hours naturally cools to high titanium slag and puts into that agate mortar is manual wears into fine powder after the room temperature, and particle mean size reaches below 5 microns.
3, high high-intensity magnetic field activation modification: with above-mentioned high titanium slag powder with press model machine in the mould of φ 8 unidirectional molded after, be placed in the crucible of φ 10.Then crucible is placed on that (JMTD-12T φ 100mm) rises magnetic in the superconducting intense magnetic field system, magnetic field intensity is 6T, and temperature is risen to 800 ℃, and activation modification is 1 hour under this magnetic field condition and temperature conditions, falls magnetic to 0T.After naturally cooling to room temperature the high titanium slag behind the activation modification is pulverized, its particle mean size reaches below 5 microns.
The methylene blue solution that the high titanium slag powder 0.5g and the 100ml initial concentration of preparation is 5mg/l adds in the reactor, at 300 μ W/cm respectively
2Wavelength is respectively under the UV-irradiation of 254nm and 365nm, behind the degraded 60min, leaves standstill 30min, gets supernatant liquor, and centrifugal again 30min measures solution absorbency three times, calculates its degradation rate and the average degradation rate of final calculating respectively.Result of implementation shows: average degradation rate reaches 43.20% and 20.16% respectively, has improved 13.50% and 7.20% than the original slag of crossing without calcination process respectively for the degradation rate (29.70% and 12.96%) of methyl blue solution.
Embodiment 2
1, ball milling: high titanium slag is manually smashed earlier, and with its further pulverizing, this moment, granularity can reach the hundreds of micron on sampling machine.And then, reach below 5 microns to its particle mean size through smooth roll ball mill mill about 200 hours.
2, roasting: the high titanium slag that ball milling is good is put into Muffle furnace, and under 1200 ℃ of temperature, constant temperature calcining activation 1 hour naturally cools to high titanium slag and puts into that agate mortar is manual wears into fine powder after the room temperature, and particle mean size reaches below 5 microns.
3, high high-intensity magnetic field activation modification: with above-mentioned high titanium slag powder with press model machine in the mould of φ 8 unidirectional molded after, be placed in the crucible of φ 10.Then crucible is placed on that (JMTD-12T φ 100mm) rises magnetic in the superconducting intense magnetic field system, magnetic field intensity is 6T, and temperature is risen to 900 ℃, and activation modification is 0.5 hour under this magnetic field condition and temperature conditions, falls magnetic to 0T.After naturally cooling to room temperature the high titanium slag behind the activation modification is pulverized, its particle mean size reaches below 5 microns.
Embodiment 3
1, ball milling: high titanium slag is manually smashed earlier, and with its further pulverizing, this moment, granularity can reach the hundreds of micron on sampling machine.And then, reach below 5 microns to its particle mean size through smooth roll ball mill mill about 200 hours.
2, roasting: the high titanium slag that ball milling is good is put into Muffle furnace, and under 400 ℃ of temperature, constant temperature calcining activation 3 hours naturally cools to high titanium slag and puts into that agate mortar is manual wears into fine powder after the room temperature, and particle mean size reaches below 5 microns.
3, high high-intensity magnetic field activation modification: with above-mentioned high titanium slag powder with press model machine in the mould of φ 8 unidirectional molded after, be placed in the crucible of φ 10.Then crucible is placed on that (JMTD-12T φ 100mm) rises magnetic in the superconducting intense magnetic field system, magnetic field intensity is 6T, and temperature is risen to 750 ℃, and activation modification is 1.5 hours under this magnetic field condition and temperature conditions, falls magnetic to 0T.After naturally cooling to room temperature the high titanium slag behind the activation modification is pulverized, its particle mean size reaches below 5 microns.
Embodiment 4
1, ball milling: high titanium slag is manually smashed earlier, and with its further pulverizing, this moment, granularity can reach the hundreds of micron on sampling machine.And then, reach below 5 microns to its particle mean size through smooth roll ball mill mill about 200 hours.
2, roasting: the high titanium slag that ball milling is good is put into Muffle furnace, and under 800 ℃ of temperature, constant temperature calcining activation 2 hours naturally cools to high titanium slag and puts into that agate mortar is manual wears into fine powder after the room temperature, and particle mean size reaches below 5 microns.
3, high high-intensity magnetic field activation modification: with above-mentioned high titanium slag powder with press model machine in the mould of φ 8 unidirectional molded after, be placed in the crucible of φ 10.Then crucible is placed on that (JMTD-12T φ 100mm) rises magnetic in the superconducting intense magnetic field system, magnetic field intensity is 4T, and temperature is risen to 800 ℃, and activation modification is 1 hour under this magnetic field condition and temperature conditions, falls magnetic to 0T.After naturally cooling to room temperature the high titanium slag behind the activation modification is pulverized, its particle mean size reaches below 5 microns.
1, ball milling: high titanium slag is manually smashed earlier, and with its further pulverizing, this moment, granularity can reach the hundreds of micron on sampling machine.And then, reach below 5 microns to its particle mean size through smooth roll ball mill mill about 200 hours.
2, roasting: the high titanium slag that ball milling is good is put into Muffle furnace, and under 800 ℃ of temperature, constant temperature calcining activation 2 hours naturally cools to high titanium slag and puts into that agate mortar is manual wears into fine powder after the room temperature, and particle mean size reaches below 5 microns.
3, high high-intensity magnetic field activation modification: with above-mentioned high titanium slag powder with press model machine in the mould of φ 8 unidirectional molded after, be placed in the crucible of φ 10.Then crucible is placed on that (JMTD-12T φ 100mm) rises magnetic in the superconducting intense magnetic field system, magnetic field intensity is 1T, and temperature is risen to 800 ℃, and activation modification is 1 hour under this magnetic field condition and temperature conditions, falls magnetic to 0T.After naturally cooling to room temperature the high titanium slag behind the activation modification is pulverized, its particle mean size reaches below 5 microns.
Embodiment 6
1, ball milling: high titanium slag is manually smashed earlier, and with its further pulverizing, this moment, granularity can reach the hundreds of micron on sampling machine.And then, reach below 5 microns to its particle mean size through smooth roll ball mill mill about 200 hours.
2, roasting: the high titanium slag that ball milling is good is put into Muffle furnace, and under 800 ℃ of temperature, constant temperature calcining activation 2 hours naturally cools to high titanium slag and puts into that agate mortar is manual wears into fine powder after the room temperature, and particle mean size reaches below 5 microns.
3, high high-intensity magnetic field activation modification: with above-mentioned high titanium slag powder with press model machine in the mould of φ 8 unidirectional molded after, be placed in the crucible of φ 10.Then crucible is placed on that (JMTD-12T φ 100mm) rises magnetic in the superconducting intense magnetic field system, magnetic field intensity is 12T, and temperature is risen to 800 ℃, and activation modification is 1 hour under this magnetic field condition and temperature conditions, falls magnetic to 0T.After naturally cooling to room temperature the high titanium slag behind the activation modification is pulverized, its particle mean size reaches below 5 microns.
Claims (1)
1, a kind of method of utilizing strong magnetic field modified titanium-rich slag to prepare catalysis material is characterized in that processing step is as follows:
1. ball milling, with the titaniferous amount with TiO
2Meter, TiO by weight percentage
2〉=87.67% high titanium slag manually smashes earlier, with its further pulverizing, and then reaches below 5 microns through smooth roll ball mill ball milling to its particle mean size on sampling machine;
2. roasting, the high titanium slag that ball milling is good is put into Muffle furnace, and under 400～1200 ℃ of temperature, constant temperature calcining activation 1～3 hour is worn into fine powder with high titanium slag after naturally cooling to room temperature, and particle mean size reaches below 5 microns;
3. high high-intensity magnetic field activation modification, with above-mentioned high titanium slag powder with press model machine in the mould unidirectional molded after, be placed in the crucible, then crucible is placed in the superconducting intense magnetic field system and rises magnetic, magnetic field intensity is 1～12T, and temperature is risen to 750～900 ℃, activation modification is 0.5～1.5 hour under this magnetic field condition and temperature conditions, fall magnetic to 0T, the high titanium slag behind the activation modification is pulverized after naturally cooling to room temperature, its particle mean size reaches below 5 microns.
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| CNB2006100471715A CN100430127C (en) | 2006-07-10 | 2006-07-10 | Process for preparing photo-catalytic materials by using strong magnetic field modified titanium-rich slag |
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| CNB2006100471715A CN100430127C (en) | 2006-07-10 | 2006-07-10 | Process for preparing photo-catalytic materials by using strong magnetic field modified titanium-rich slag |
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| CN1883789A CN1883789A (en) | 2006-12-27 |
| CN100430127C true CN100430127C (en) | 2008-11-05 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100537023C (en) * | 2007-11-08 | 2009-09-09 | 武汉科技大学 | Photocatalyst having response to visible light and preparation thereof |
| CN112521142B (en) * | 2020-12-08 | 2022-04-26 | 西南科技大学 | Photocatalytic ceramic, preparation method thereof and method for degrading organic dye RhB |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3961940A (en) * | 1973-11-20 | 1976-06-08 | Mitsubishi Kinzoku Kogyo Kabushiki Kaisha | Post-treatment of ilmenite ore subjected to selective chlorination treatment |
| CN1446624A (en) * | 2002-05-31 | 2003-10-08 | 东北大学 | Method for preparing photocatalysis material by using iron blast-furnace slag containing titanium |
| CN1775957A (en) * | 2005-11-25 | 2006-05-24 | 东北大学 | Ecological treating method for blast furnace slag containing titanium |
-
2006
- 2006-07-10 CN CNB2006100471715A patent/CN100430127C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3961940A (en) * | 1973-11-20 | 1976-06-08 | Mitsubishi Kinzoku Kogyo Kabushiki Kaisha | Post-treatment of ilmenite ore subjected to selective chlorination treatment |
| CN1446624A (en) * | 2002-05-31 | 2003-10-08 | 东北大学 | Method for preparing photocatalysis material by using iron blast-furnace slag containing titanium |
| CN1775957A (en) * | 2005-11-25 | 2006-05-24 | 东北大学 | Ecological treating method for blast furnace slag containing titanium |
Non-Patent Citations (4)
| Title |
|---|
| 含钛高炉渣催化剂光催化降解亚甲基蓝. 杨合，薛向欣，左良，杨中东.过程工程学报，第4卷第3期. 2004 |
| 含钛高炉渣催化剂光催化降解亚甲基蓝. 杨合，薛向欣，左良，杨中东.过程工程学报，第4卷第3期. 2004 * |
| 高钛渣作为光催化材料降解邻硝基酚的实验研究. 赵娜，杨合，薛向欣，刘卯，田海川，董学文.硅酸盐学报，第33卷第2期. 2005 |
| 高钛渣作为光催化材料降解邻硝基酚的实验研究. 赵娜，杨合，薛向欣，刘卯，田海川，董学文.硅酸盐学报，第33卷第2期. 2005 * |
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