CN106362717A - Preparation method for supported titanium dioxide photocatalyst - Google Patents
Preparation method for supported titanium dioxide photocatalyst Download PDFInfo
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- CN106362717A CN106362717A CN201610655256.5A CN201610655256A CN106362717A CN 106362717 A CN106362717 A CN 106362717A CN 201610655256 A CN201610655256 A CN 201610655256A CN 106362717 A CN106362717 A CN 106362717A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000004408 titanium dioxide Substances 0.000 title abstract description 3
- 239000000843 powder Substances 0.000 claims abstract description 56
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000002893 slag Substances 0.000 claims abstract description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 150000000703 Cerium Chemical class 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 3
- JSYPRLVDJYQMAI-ODZAUARKSA-N (z)-but-2-enedioic acid;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)\C=C/C(O)=O JSYPRLVDJYQMAI-ODZAUARKSA-N 0.000 claims description 15
- 241000195474 Sargassum Species 0.000 claims description 15
- 241000292525 Titanio Species 0.000 claims description 14
- 229960004756 ethanol Drugs 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 3
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 3
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 230000037396 body weight Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 241001474374 Blennius Species 0.000 abstract 2
- 229920001577 copolymer Polymers 0.000 abstract 2
- 235000012054 meals Nutrition 0.000 abstract 2
- 229910052719 titanium Inorganic materials 0.000 abstract 2
- 239000010936 titanium Substances 0.000 abstract 2
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 239000004254 Ammonium phosphate Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- -1 DSSC Substances 0.000 description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 2
- 235000019289 ammonium phosphates Nutrition 0.000 description 2
- FZIZEIAMIREUTN-UHFFFAOYSA-N azane;cerium(3+) Chemical compound N.[Ce+3] FZIZEIAMIREUTN-UHFFFAOYSA-N 0.000 description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 238000004500 asepsis Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method for a supported titanium dioxide photocatalyst. The preparation method comprises the following steps: weighing raw materials consisting of, by weight, 100 parts of TiO2 powder, 5 to 10 parts of acrylic acid-maleic acid copolymer, 10 to 15 parts of carbide slag, 1 to 2 parts of cerium salt and 8 to 12 parts of seaweed meal; adding the TiO2 powder and the acrylic acid-maleic acid copolymer into an ultrasonic generator and then adding ethanol for an ultrasonic reaction so as to obtain a titanium-based suspension; adding the titanium-based suspension, carbide slag, cerium salt and seaweed meal into a ball mill, adding a proper amount of water and carrying out stirring so as to obtain paste; subjecting the paste to microwave drying at 60 to 80 DEG C for 1 to 2 h, grinding the dried paste into powder and then roasting the powder in a muffle furnace at a temperature of 500 to 700 DEG C for 3 to 5 h so as to obtain the photocatalyst. The preparation method has the advantages of wide sources of the raw materials, low cost, easiness in preparation, high production efficiency, low energy consumption, mild reaction conditions and environment friendliness; and the prepared photocatalyst has good adsorption performance, high catalytic activity and high catalytic efficiency and can efficiently catalyze degradation of organic pollutants in waste water under irradiation of visible light.
Description
Technical field
The present invention relates to catalysis material technical field, specifically a kind of preparation side of load type titania photocatalyst
Method.
Background technology
Since 21 century, the lifting with industrialization paces and the excessive use of natural resourcess, dirty along with various environment
Dye, energy scarcity problem constantly aggravate.Therefore, various pollutions are administered, the pressure finding new forms of energy to alleviate the earth is extremely urgent.
Photocatalysis technology is in wastewater treatment, gas purification, sterilization, antifouling, self-cleaning material, DSSC, cosmetic
The many such as product, gas sensor fields have a wide range of applications.Photocatalysis are can be produced under light excites based on semi-conducting material
Life has the light induced electron of strong reducing property and the fundamental characteristics in the hole with strong oxidizing property, and solid photocatalysts can absorb the sun
Water is become hydrogen by light with biomass decomposition, also the organic pollution in air and water body environment and inorganic pollution can be aoxidized or
Deoxidization, degradation is innocuous substance.Therefore, there is low energy consumption, environmental protection.
At present, the conductor photocatalysis material of domestic and international most study is mainly metal-oxide and sulfide, such as ti02,
W03, zno, fe203, cds etc..Ti02 because its active height, good stability, fast light burn into are nontoxic, low cost and other advantages, mesh
Before become a kind of the most valued photocatalyst.But ti02 also has the shortcomings that itself as photocatalyst, such as the band gap of ti02 is relatively
Wide (eg=3.2 ev), can only absorb ultraviolet light, and ultraviolet light only accounts for the 4% about of solar energy, therefore, ti02 is to the sun
The utilization rate of light is very low.Because its granule of ti02 powder body material is excessively trickle, it is easy to inactivate in use environment and condenses, be difficult
Sedimentation, leads to it to be difficult to separate, reclaim and reuse.For solving the above problems, increase its stability in use, ti02 is loaded
On certain carrier, such as glass, silica gel, activated carbon etc., but these carriers exist that mechanical strength is weaker, chemical stability and heat
Stability difference etc. is limited to.Therefore, how to improve the photocatalytic activity of photocatalyst and stability is current study hotspot.
Content of the invention
The present invention is directed to the problem that existing photocatalyst exists, and provides a kind of preparation of load type titania photocatalyst
Method.The photocatalyst of this method preparation has that specific surface area is big, catalysis activity is high, the utilization rate height to light source, good stability,
Environment-protecting asepsis, low cost, the advantages of can repeatedly use.
In order to realize object above, the technical solution used in the present invention is as follows:
A kind of preparation method of load type titania photocatalyst, comprises the following steps:
(1) ratio weighs each raw material: 100 parts of ti02 powder body, acrylic acid maleic acid 5-10 part, carbide in parts by weight
Slag 10-15 part, cerium salt 1-2 part and Sargassum powder 8-12 part；
(2) ti02 powder body and acrylic acid maleic acid are added in ultrasonic generator, add ethanol, be 40- in frequency
Ultrasonic 30-60min under 60khz, obtains titanio suspension；
(3) titanio suspension, carbide slag, cerium salt and Sargassum powder are added ball mill, add suitable quantity of water stirring, obtain pastel；
(4) by above-mentioned pastel at 60-80 DEG C microwave drying 1-2h, be dried after grind into powder, place into muffle furnace in temperature
Spend for roasting 3-5h at 500-700 DEG C, that is, obtain photocatalyst.
Preferably, the above ti02 raw powder's production technology is as follows: 1l ethanol is added the solution of tetrabutyl titanate of 1l
Middle stirring 60min, obtains a solution；Take 0.3kg ammonium phosphate to be dissolved in the distilled water of 2l, add 3l dehydrated alcohol, add
The concentrated nitric acid stirring 30min of 0.2l, obtains b solution；Under agitation b solution is added in a solution, obtain TiO 2 precursor and coagulate
Glue；Gel is dried at 100 DEG C, grinds, obtain presoma powder body；Again by presoma powder body at 600 DEG C roasting 5h, you can
Obtain ti02 powder body.
Preferably, the above cerium salt includes one of cerous sulfate, cerous nitrate or ammonium ceric nitrate.
Preferably, the addition of the above ethanol is 2-3 times of ti02 powder body weight.
Preferably, the described stirring of above step (3) is stirring 30-60min under rotating speed is for 300-500r/min.
Preferably, the heating rate of the above roasting is 5-10 DEG C/min.
Preferably, the described grinding of above step (4) is to grind the material to particle diameter for 0.5-2.0mm.
Compared with prior art, advantages of the present invention and having the beneficial effect that
1st, the photocatalyst that the inventive method is obtained has larger specific surface area, good pore structure and more catalysis and lives
Property center, improve the absorption property of catalyst so that light induced electron and hole can efficiently separate, so improve catalyst
Activity and efficiency, expand the absorption in visible-range for the catalyst, greatly improve the utilization rate to sunlight for the catalyst.
2nd, the present invention, using acrylic acid maleic acid as dispersant, can solve titanium dioxide powder in use environment
In be easy to inactivate and condense, the problem of not free settling.
3rd, the present invention is using carbide slag and Sargassum powder as carrier, catalyst performance can not only be made more stable it is easier to
Separate, reclaim and be used repeatedly moreover it is possible to improve absorption property and the photocatalysis performance of catalyst.
4th, the photocatalyst specific surface area of present invention preparation is 200-300m2/ g, the degradation rate to rhodamine b in 60 minutes
Reach more than 93%.
5th, the present invention has that raw material sources are extensive, with low cost, preparation process is simple, production efficiency high, energy consumption is low, reaction
Mild condition, environmental friendliness, absorption property are good, catalysis activity is high, high catalytic efficiency the advantages of, can efficiently under visible light exposure
Catalytic degradation wastewater organic pollutant, has good economic benefit, social benefit and ecological benefits, is more suitable for industrial life
Produce.
Specific embodiment
Below in conjunction with specific embodiment, this programme is further illustrated, but be not limited to protection scope of the present invention.
Ti02 powder preparation method described in following examples is as follows: 1l ethanol is added the solution of tetrabutyl titanate of 1l
Middle stirring 60min, obtains a solution；Take 0.3kg ammonium phosphate to be dissolved in the distilled water of 2l, add 3l dehydrated alcohol, add
The concentrated nitric acid stirring 30min of 0.2l, obtains b solution；Under agitation b solution is added in a solution, be further continued for stirring 30min, obtain two
Titania precursor body gel；Gel is dried at 100 DEG C, grinds, obtain presoma powder body；Again by presoma powder body 600
Roasting 5h at DEG C, you can obtain ti02 powder body.
Embodiment 1
A kind of preparation method of load type titania photocatalyst, comprises the following steps:
(1) proportionally weigh each raw material: ti02 powder body 10kg, acrylic acid maleic acid 0.6kg, carbide slag 1.0kg, nitre
Sour cerium 0.1kg and Sargassum powder 0.8kg；
(2) ti02 powder body and acrylic acid maleic acid are added in ultrasonic generator, add 20kg ethanol, in frequency be
Ultrasonic 60min under 40khz, obtains titanio suspension；
(3) titanio suspension, carbide slag, cerous nitrate and Sargassum powder are added ball mill, add 35kg water, in rotating speed be
Stir 30min under 500r/min, obtain pastel；
(4) by above-mentioned pastel at 60 DEG C microwave drying 2h, be dried after grind to form particle diameter be 1.0mm powder, place into horse
Boiling stove roasting 4h at temperature is 600 DEG C, that is, obtain photocatalyst.
Embodiment 2
A kind of preparation method of load type titania photocatalyst, comprises the following steps:
(1) proportionally weigh each raw material: ti02 powder body 10kg, acrylic acid maleic acid 0.8kg, carbide slag 1.2kg, nitre
Sour cerium 0.15kg and Sargassum powder 1.0kg；
(2) ti02 powder body and acrylic acid maleic acid are added in ultrasonic generator, add 25kg ethanol, in frequency be
Ultrasonic 45min under 50khz, obtains titanio suspension；
(3) titanio suspension, carbide slag, cerous nitrate and Sargassum powder are added ball mill, add 40kg water, in rotating speed be
Stir 60min under 300r/min, obtain pastel；
(4) by above-mentioned pastel at 80 DEG C microwave drying 1.5h, be dried after grind to form particle diameter be 1.0mm powder, place into
Muffle furnace roasting 5h at temperature is 500 DEG C, that is, obtain photocatalyst.
Embodiment 3
A kind of preparation method of load type titania photocatalyst, comprises the following steps:
(1) proportionally weigh each raw material: ti02 powder body 10kg, acrylic acid maleic acid 0.5kg, carbide slag 1.5kg, sulfur
Sour cerium 0.15kg and Sargassum powder 1.2kg；
(2) ti02 powder body and acrylic acid maleic acid are added in ultrasonic generator, add 20kg ethanol, in frequency be
Ultrasonic 30min under 60khz, obtains titanio suspension；
(3) titanio suspension, carbide slag, cerous sulfate and Sargassum powder are added ball mill, add 40kg water, in rotating speed be
Stir 60min under 500r/min, obtain pastel；
(4) by above-mentioned pastel at 70 DEG C microwave drying 2h, be dried after grind to form particle diameter be 1.0mm powder, place into horse
Boiling stove roasting 3h at temperature is 700 DEG C, that is, obtain photocatalyst.
Embodiment 4
A kind of preparation method of load type titania photocatalyst, comprises the following steps:
(1) proportionally weigh each raw material: ti02 powder body 10kg, acrylic acid maleic acid 1.0kg, carbide slag 1.2kg, nitre
Sour cerium ammonium 0.20kg and Sargassum powder 1.2kg；
(2) ti02 powder body and acrylic acid maleic acid are added in ultrasonic generator, add 30kg ethanol, in frequency be
Ultrasonic 30min under 60khz, obtains titanio suspension；
(3) titanio suspension, carbide slag, ammonium ceric nitrate and Sargassum powder are added ball mill, add 40kg water, in rotating speed be
Stir 45min under 400r/min, obtain pastel；
(4) by above-mentioned pastel at 80 DEG C microwave drying 1h, be dried after grind to form particle diameter be 2.0mm powder, place into horse
Boiling stove roasting 3.5h at temperature is 600 DEG C, that is, obtain photocatalyst.
Embodiment 5
A kind of preparation method of load type titania photocatalyst, comprises the following steps:
(1) proportionally weigh each raw material: ti02 powder body 10kg, acrylic acid maleic acid 0.8kg, carbide slag 1.5kg, nitre
Sour cerium ammonium 0.20kg and Sargassum powder 1.2kg；
(2) ti02 powder body and acrylic acid maleic acid are added in ultrasonic generator, add 30kg ethanol, in frequency be
Ultrasonic 60min under 40khz, obtains titanio suspension；
(3) titanio suspension, carbide slag, ammonium ceric nitrate and Sargassum powder are added ball mill, add 35kg water, in rotating speed be
Stir 60min under 300r/min, obtain pastel；
(4) by above-mentioned pastel at 80 DEG C microwave drying 2h, be dried after grind to form particle diameter be 2.0mm powder, place into horse
Boiling stove roasting 3h at temperature is 700 DEG C, that is, obtain photocatalyst.
The photocatalysis test of catalyst: below by the light by commercial p-25 photocatalyst and various embodiments of the present invention preparation
Catalyst contrasts to the degradation rate of rhodamine b, and measurement result is as shown in the table:
The photocatalyst of each embodiment preparation and p-25 photocatalyst are weighed 1g respectively, puts into sieve that 1l concentration is 100mg/l
Red bright b simulated water sample, adds in the reactor of quartzy interlayer, using the mercury lamp of 300w as ultraviolet source, is 300r/ in rotating speed
Under min, stirring radiation 1h, using the concentration of rhodamine b in Water By High Performance Liquid sample, calculates photocatalyst for degrading
Rate.
As seen from table, the photocatalyst prepared by various embodiments of the present invention has higher photocatalytic activity, to rhodamine b's
Degradation rate all reaches more than 93%, significantly larger than presently commercially available product, has good market prospect.
Above content is it cannot be assumed that the present invention is embodied as being confined to these explanations, for the technical field of the invention
Those of ordinary skill for, under the premise of without departing from present inventive concept, some simple deduction or replace can also be made, all answer
When being considered as belonging to the scope of patent protection that the present invention is determined by claims of being submitted to.
Claims (7)
1. a kind of preparation method of load type titania photocatalyst it is characterised in that: comprise the following steps:
(1) ratio weighs each raw material: 100 parts of ti02 powder body, acrylic acid maleic acid 5-10 part, carbide in parts by weight
Slag 10-15 part, cerium salt 1-2 part and Sargassum powder 8-12 part；
(2) ti02 powder body and acrylic acid maleic acid are added in ultrasonic generator, add ethanol, be 40- in frequency
Ultrasonic 30-60min under 60khz, obtains titanio suspension；
(3) titanio suspension, carbide slag, cerium salt and Sargassum powder are added ball mill, add suitable quantity of water stirring, obtain pastel；
(4) by above-mentioned pastel at 60-80 DEG C microwave drying 1-2h, be dried after grind into powder, place into muffle furnace in temperature
Spend for roasting 3-5h at 500-700 DEG C, that is, obtain photocatalyst.
2. according to claim 1 load type titania photocatalyst preparation method it is characterised in that: described ti02 powder
The preparation method of body is as follows: stirs 60min in solution of tetrabutyl titanate 1l ethanol being added 1l, obtains a solution；Take 0.3kg phosphorus
Sour ammonium is dissolved in the distilled water of 2l, adds 3l dehydrated alcohol, adds the concentrated nitric acid stirring 30min of 0.2l, obtains b solution；
Under agitation b solution is added in a solution, obtain TiO 2 precursor gel；Gel is dried at 100 DEG C, grinds, obtain
Presoma powder body；Again by presoma powder body at 600 DEG C roasting 5h, you can ti02 powder body.
3. according to claim 1 load type titania photocatalyst preparation method it is characterised in that: described cerium salt bag
Include one of cerous sulfate, cerous nitrate or ammonium ceric nitrate.
4. according to claim 1 load type titania photocatalyst preparation method it is characterised in that: described ethanol
Addition is 2-3 times of ti02 powder body weight.
5. according to claim 1 load type titania photocatalyst preparation method it is characterised in that: step (3) institute
Stating stirring is stirring 30-60min under rotating speed is for 300-500r/min.
6. according to claim 1 load type titania photocatalyst preparation method it is characterised in that: described roasting
Heating rate is 5-10 DEG C/min.
7. according to claim 1 load type titania photocatalyst preparation method it is characterised in that: step (4) institute
Stating grinding is to grind the material to particle diameter for 0.5-2.0mm.
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| CN103553587A (en) * | 2013-11-11 | 2014-02-05 | 黑龙江大学 | Preparation method and using method of graded hole TiO2 ceramic photocatalyst |
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