CN102688753B - Preparation method of monodisperse granular amorphous nanometer TiO2 - Google Patents
Preparation method of monodisperse granular amorphous nanometer TiO2 Download PDFInfo
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- CN102688753B CN102688753B CN201110357325.1A CN201110357325A CN102688753B CN 102688753 B CN102688753 B CN 102688753B CN 201110357325 A CN201110357325 A CN 201110357325A CN 102688753 B CN102688753 B CN 102688753B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000013049 sediment Substances 0.000 claims description 10
- 241000209094 Oryza Species 0.000 claims description 8
- 235000007164 Oryza sativa Nutrition 0.000 claims description 8
- 235000013339 cereals Nutrition 0.000 claims description 8
- 235000009566 rice Nutrition 0.000 claims description 8
- 239000002105 nanoparticle Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 2
- 229910011006 Ti(SO4)2 Inorganic materials 0.000 abstract 3
- 229910017053 inorganic salt Inorganic materials 0.000 abstract 3
- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical compound [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 abstract 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 abstract 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 abstract 1
- 239000012429 reaction media Substances 0.000 abstract 1
- 230000000630 rising effect Effects 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000005300 metallic glass Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- -1 salts titanium sulfate Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 229960002415 trichloroethylene Drugs 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of monodisperse granular amorphous nanometer TiO2 by using inorganic salt Ti(SO4)2. The preparation method comprises the following steps: dissolving the inorganic salt Ti(SO4)2 and polyvinylpyrrolidone in the water as the reaction medium, adding a complexant H2O2, carrying out a hydrothermal reaction in the temperature-change heating manner, namely, heating for 1-2 hours at the constant temperature of 100 DEG C, rising the temperature to 200-240 DEG C and heating for 0.5-1 hours, then heating at 60-80 DEG C for 20-24 hours, after reacting, centrifugally washing and drying the output TiO2 to obtain the monodisperse granular amorphous nanometer TiO2. The preparation method of the monodisperse granular amorphous nanometer TiO2 is simple. The size, structure and shape of the TiO2 nanometer particles can be controlled easily. The reaction is carried out by using the inorganic salt Ti(SO4)2 in the water solution, thereby solving the problem that the cost of the materials is high in the prior art.
Description
Technical field
The invention belongs to catalyst material field, relate to a kind of nano-TiO
2preparation method, specifically, relate to a kind of amorphous nano-TiO
2preparation method, more particularly, relate to a kind of single amorphous nano-TiO of grain of rice shape that disperses
2preparation method.
Background technology
From first observed in 1972 to illumination TiO
2since there is the phenomenon of Optical Electro-Chemistry decomposition water in anode, TiO
2become gradually the focus of Heterogeneous photocatalysis research.Because its cheapness, nontoxic, high catalytic activity and stability etc. become the semi-conductive first-selection of photocatalysis especially, it is the semiconductor light-catalyst of studying at present at most.TiO
2have broad application prospects in field of environment protection as a kind of photochemical catalyst, thereby its research is also quite goed deep into extensive.The organic dyestuff that contains phenyl ring, amido, azo group and the agricultural chemicals that can light aspect sewage disposal decompose in sewage generate harmless inorganic constituents; In air purification field, can remove most organic pollutions such as formaldehyde in indoor environment, trichloro-ethylene, methyl alcohol, toluene by photocatalytic degradation; At antibiosis, nano-TiO
2under the condition of room temperature and illumination, each bacterioid, toxin etc. be can decompose, antibiotic paint, anti-bacteria ceramic, antibacterial furniture and drink water purifying are applied to; Nano-TiO
2strong absorbent and nonpoisonous and tasteless physical property in ultra-violet (UV) band have determined that it also has huge applications potentiality at cosmetic field.
But TiO
2in photochemical catalyst, there are two Main Bottlenecks that affect its practical application: the one, catalyst quantum productive rate is lower; The 2nd, band gap width is too high, causes its optic response scope narrower.Existing many literature research TiO
2the relation of different crystalline phases, crystallite dimension, defect density, surface species and distortion of lattice stress etc. and catalytic activity, in recent years to nano-TiO
2preparation and Photocatalytic Performance Study also become focus, Chinese patent CN 101597083A discloses a kind of dispersed nano TiO
2preparation method, the method is taking titanate esters as presoma, under surfactant exists, carries out solvent thermal reaction anatase type nano TiO in ethanol
2.Chinese patent CN 101073769A has announced a kind of steam hydrolysis legal system for nano-TiO
2method, the method utilizes the hydrolysis of titanium tetrachloride in ethanolic solution to prepare TiO
2nano particle obtains crystalline state TiO after roasting
2.The organic metal titanium precursor thing that it should be noted that the use that has in these preparation methods, some uses organic solvent, preparation cost is high,
In addition, most is about TiO
2light-catalysed research all concentrates on crystalline state TiO
2, seldom pay close attention to its amorphous state (amorphous TiO
2) character.But nearest achievement in research shows, amorphous metal oxide also has advantages of many potential, amorphous TiO
2research also had certain progress, it is found that amorphous TiO
2more easily be processed into difformity and form, but the more chemical substance of adulterating, although amorphous TiO
2without visible light catalysis activity, but after area load doping, photocatalytic activity improves greatly, also can utilize the amorphous TiO of dye sensitization
2realize the dyestuff contaminant of degrading under visible ray.The use titanate esters Hydrolyze method such as Wang Qi have been prepared amorphous TiO
2, and for visible light photoactivated degradation of dye pollutant, prepared amorphous TiO
2the photocatalytic degradation of rhodamine B is had to good effect (Wang Qi etc., catalysis journal, 2011,32:1076).
Summary of the invention
The present invention is directed to the existing nano-TiO of preparing
2in technology, use metal organic titanate and organic solvent, reaction condition harsher, the unmanageable technical problem of its size, structure and pattern, provides a kind of single amorphous nano-TiO that disperses
2preparation method.The method technique is simple, and reaction condition is gentleer, prepared amorphous TiO
2size, structure and pattern easily control, the present invention is achieved by the following technical solutions:
A kind of single amorphous nano-TiO that disperses
2preparation method.It is characterized in that, described method comprises the steps:
1. by 0.05-1.0 molL
-1ti (SO
4)
2with 10 gL
-1polyvinylpyrrolidone is dissolved in the water, and adds the H of 3.5-7 % (volume ratio)
2o
2;
2. above-mentioned mixed liquor is transferred in the autoclave of liner tetrafluoroethene, at 100 DEG C of heated at constant temperature 1-2 h, be then warmed up to 200-240 DEG C of heating 0.5-1 h, be finally transferred to again 60-80 DEG C of heating 20-24 h, obtain containing TiO
2mixed liquor;
3. by the above-mentioned TiO that contains
2mixed liquor cooling after, centrifugal under certain rotating speed, outwell supernatant liquid, and water and ethanol repeated washing, obtain white nano-TiO
2sediment;
4. the sediment obtaining in step (3) is put into drying box dry, obtain single amorphous nano-TiO that disperses
2.
Wherein, in step (3), described centrifugal rotational speed is 8000-10000 r/min, and centrifugation time is 5-10 min.
Further, in step (4), dry temperature is 60-80 DEG C, and the dry time is 12-24 h.
The invention has the advantages that: predecessor used is cheap inorganic salts titanium sulfate, in the aqueous solution, reacts, and preparation cost is low; The nano-TiO that the method is prepared
2grain shape homogeneous, monodispersity is good.
Brief description of the drawings
Fig. 1 is the prepared TiO of embodiment mono-
2the SEM of sample and TEM photo.
Fig. 2 is the prepared TiO of embodiment bis-
2the SEM of sample and TEM photo.
Detailed description of the invention
Below by embodiment, the present invention is described in further detail:
Embodiment mono-:
(1) by 0.05 molL
-1ti (SO
4)
2with 10 gL
-1polyvinylpyrrolidone is dissolved in the water, and adds the H of 3.5 % (volume ratio)
2o
2for complexant;
(2) above-mentioned mixed liquor is transferred in the autoclave of liner tetrafluoroethene, at 100 DEG C of heated at constant temperature 1 h, be then warmed up to 200 DEG C of heating 1 h, be finally transferred to again 80 DEG C of heating 20 h, obtain containing TiO
2mixed liquor;
(3) by the above-mentioned TiO that contains
2mixed liquor cooling after, under 10000 r/min rotating speeds, centrifugal 10 min, outwell supernatant liquid, and water and ethanol repeated washing three times, obtain white TiO
2sediment;
(4) sediment obtaining in step (3) is put into dry 24 h of 80 DEG C of drying boxes, obtained single amorphous nano-TiO that disperses
2.
Embodiment bis-:
(1) by 1.0 molL
-1ti (SO
4)
2with 10 gL
-1polyvinylpyrrolidone is dissolved in the water, and adds the H of 7 % (volume ratio)
2o
2for complexant;
(2) above-mentioned mixed liquor is transferred in the autoclave of liner tetrafluoroethene, at 100 DEG C of heated at constant temperature 1 h, be then warmed up to 200 DEG C of heating 1 h, be finally transferred to again 80 DEG C of heating 20 h, obtain containing TiO
2mixed liquor;
(3) by the above-mentioned TiO that contains
2mixed liquor cooling after, under 10000 r/min rotating speeds, centrifugal 10 min, outwell supernatant liquid, and water and ethanol repeated washing three times, obtain white TiO
2sediment;
(4) sediment obtaining in step (3) is put into dry 24 h of 80 DEG C of drying boxes, obtained single amorphous nano-TiO that disperses
2.
Embodiment tri-:
(1) by 0.05 molL
-1ti (SO
4)
2with 10 gL
-1polyvinylpyrrolidone is dissolved in the water, and adds the H of 3.5 % (volume ratio)
2o
2;
(2) above-mentioned mixed liquor is transferred in the autoclave of liner tetrafluoroethene, at 100 DEG C of heated at constant temperature 1 h, be then warmed up to 240 DEG C of heating 30 min, be finally transferred to again 60 DEG C of heating 24 h, obtain containing TiO
2mixed liquor;
(3) by the above-mentioned TiO that contains
2mixed liquor cooling after, under 10000 r/min rotating speeds, centrifugal 10 min, outwell supernatant liquid, and water and ethanol repeated washing three times, obtain white TiO
2sediment;
(4) sediment obtaining in step (3) is put into dry 24 h of 80 DEG C of drying boxes, obtained single amorphous nano-TiO that disperses
2.
There is not obvious diffraction maximum in the x-ray diffractogram of powder spectrum of sample, shows TiO prepared by the method for the invention
2product is amorphous state.
Fig. 1 utilizes single amorphous TiO of dispersion that prepared by method described in the embodiment of the present invention one
2different amplification SEM (SEM) photo.Photo from figure can be found out, by controlling reaction condition, can obtain grain of rice shape dispersed nano TiO
2, gained TiO
2nanoparticle Size is even, and pattern is regular.Grain of rice shape TiO
2the length of nano particle and wide be respectively 180nm and 100nm.Transmission electron microscope (TEM) photo that Fig. 1 the 2nd width figure is this sample.As can be seen from the figure, rice-granule nano TiO
2evenly, monodispersity is good for size.Electronic diffraction result shows does not have obvious diffraction pattern to occur, shows that gained sample is amorphous state.
Fig. 2 is the prepared TiO of embodiment bis-
2the SEM of sample and TEM photo, SEM photo shows gained TiO
2nanoparticle Size is even, and pattern is regular, is still grain of rice shape.TEM photo shows grain of rice shape TiO
2nanoparticle Size is even, and monodispersity is good.Electronic diffraction result shows does not have obvious diffraction pattern to occur, shows that this sample is also amorphous state.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; do not deviate from other any change of doing under principle of the present invention and technical process, substitute, simplification etc.; be equivalent displacement, within all protection scope of the present invention should being included in.
Claims (1)
1. single amorphous nano-TiO of grain of rice shape that disperses
2preparation method.It is characterized in that, described method comprises the steps:
(1) by 0.05 molL
-1ti (SO
4)
2with 10 gL
-1polyvinylpyrrolidone is dissolved in the water, and adds the H in volume ratio 3.5 %
2o
2for complexant;
(2) above-mentioned mixed liquor is transferred in the autoclave of liner tetrafluoroethene, at 100 DEG C of heated at constant temperature 1 h, be then warmed up to 200 DEG C of heating 1 h, be finally transferred to again 80 DEG C of heating 20 h, obtain containing TiO
2mixed liquor;
(3) by the above-mentioned TiO that contains
2mixed liquor cooling after, under 10000 r/min rotating speeds, centrifugal 10 min, outwell supernatant liquid, and water and ethanol repeated washing three times, obtain white TiO
2sediment;
(4) sediment obtaining in step (3) is put into dry 24 h of 80 DEG C of drying boxes, obtained single amorphous nano-TiO that disperses
2;
Gained TiO
2nanoparticle Size is even, and pattern is regular; Grain of rice shape TiO
2the length of nano particle and wide be respectively 180nm and 100nm.
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| CN105129809A (en) * | 2015-10-12 | 2015-12-09 | 上海第二工业大学 | Sea-urchin-shaped nanometer nickel silicate hollow sphere and preparation method thereof |
| CN107385880B (en) * | 2017-08-22 | 2020-05-19 | 海宁滴滴箱包智能科技有限公司 | Preparation method of high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber |
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Non-Patent Citations (2)
| Title |
|---|
| 杨茂丽.纳米氧化物的制备与性能研究.《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》.2011,(第4期), |
| 纳米氧化物的制备与性能研究;杨茂丽;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20110430(第4期);15-44 * |
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