CN111151233B - Oxygen-deficient TiO2Normal temperature and pressure water phase preparation method - Google Patents
Oxygen-deficient TiO2Normal temperature and pressure water phase preparation method Download PDFInfo
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- CN111151233B CN111151233B CN201911404204.0A CN201911404204A CN111151233B CN 111151233 B CN111151233 B CN 111151233B CN 201911404204 A CN201911404204 A CN 201911404204A CN 111151233 B CN111151233 B CN 111151233B
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000001301 oxygen Substances 0.000 title claims abstract description 29
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 230000002950 deficient Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 71
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims abstract description 33
- 239000002244 precipitate Substances 0.000 claims abstract description 26
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000010936 titanium Substances 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000012071 phase Substances 0.000 claims description 10
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 2
- -1 titanium ions Chemical class 0.000 claims description 2
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- 239000008346 aqueous phase Substances 0.000 claims 2
- 229910010413 TiO 2 Inorganic materials 0.000 abstract description 7
- 238000009776 industrial production Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 238000003916 acid precipitation Methods 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 238000010907 mechanical stirring Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000004098 selected area electron diffraction Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910002661 O–Ti–O Inorganic materials 0.000 description 1
- 229910002655 O−Ti−O Inorganic materials 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000000985 reflectance spectrum Methods 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
- 150000003839 salts Chemical class 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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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
- 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
-
- B01J35/39—
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
Oxygen-deficient TiO2At normal temperature and normal temperatureA pressurized water phase preparation method, comprising the following steps; (1) dissolving an inorganic titanium source in deionized water to obtain a transparent inorganic titanium compound aqueous solution; (2) adding an inorganic alkali solution into the aqueous solution of the inorganic titanium compound in the step (1) until the pH value is 7-10 to obtain a white titanic acid suspension; (3) washing the white titanic acid suspension liquid in the step (2) by using deionized water to obtain a white titanic acid precipitate; (4) dissolving the white titanic acid precipitate in the step (3) by using hydrogen peroxide to obtain a yellow transparent titanium peroxide precursor; (5) and (3) adding hydroxylamine solution into the yellow transparent titanium peroxide precursor obtained in the step (4) at room temperature, mechanically stirring for 60min to obtain yellow precipitate, and filtering and washing to obtain the oxygen-deficient nano TiO 2. The invention has the characteristics of low cost and convenience for large-scale industrial production.
Description
Technical Field
The invention relates to the preparation of oxygen deficient TiO2The technical field, in particular to oxygen-deficient TiO2A normal temperature and pressure water phase preparation method.
Background
TiO2 is a typical photocatalytic material capable of realizing conversion of light energy to electric energy and light energy to chemical energy, and is an energy-saving and environment-friendly coating material capable of realizing comprehensive functions of organic matter degradation, air purification, self-cleaning, antibiosis and the like by utilizing solar energy. However, some inherent disadvantages remain in titanium dioxide and limit its further development. On one hand, the synthesis of the crystalline TiO2 generally requires harsh physical conditions, and the solid phase synthesis temperature is generally higher than 400 ℃; the hydrothermal and solvothermal synthesis temperatures are generally around 200 ℃, but high pressure reaction systems are required. Under the extreme conditions of strong acid and strong alkali, the reaction temperature can be reduced, but the method is not beneficial to environmental protection and large-scale production. By means of titanium metal salts (TiCl)4) Hydrolysis reaction to produce TiO2 due to Ti4+The hydrolysis reaction is very vigorous and can be carried out at room temperature, but the obtained TiO2 has an amorphous structure and needs a high-temperature recrystallization process. On the other hand, TiO2 has a wide forbidden band and can absorb only the sunThe ultraviolet light part of 4 percent of light severely limits the effective application of the TiO2 photocatalytic material to sunlight. The latest research result shows that the existence of a proper amount of defects can expand the response of TiO2 to visible light, so that the photocatalytic activity of TiO2 is effectively improved by improving the utilization efficiency of the TiO to sunlight. At present, the preparation of the oxygen-deficient TiO2 mainly adopts high-temperature hydrogenation treatment or hydrothermal solvothermal high-temperature high-pressure process, and the preparation method is difficult to realize industrial production due to harsh conditions.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the invention aims to provide an oxygen deficient TiO2The normal temperature and pressure water phase preparation method has the characteristics of low cost and convenience for large-scale industrial production.
In order to achieve the purpose, the invention adopts the technical scheme that:
oxygen-deficient TiO2The normal temperature and pressure water phase preparation process includes the following steps;
(1) dissolving an inorganic titanium source in deionized water, wherein the concentration of titanium ions is 0.5-2 mol/L, and obtaining a transparent inorganic titanium compound aqueous solution;
(2) adding inorganic alkali liquor into the aqueous solution of the inorganic titanium compound in the step (1) until the pH value is 7-10 to obtain white titanic acid suspension;
(3) washing the white titanic acid suspension liquid in the step (2) by using deionized water, wherein the conductivity of the washed waste liquid is less than 1000us/cm, and obtaining a white titanic acid precipitate;
(4) dissolving the white titanic acid precipitate in the step (3) by using hydrogen peroxide to obtain a yellow transparent titanium peroxide precursor;
(5) and (3) adding hydroxylamine solution into the yellow transparent titanium peroxide precursor obtained in the step (4) at room temperature, mechanically stirring for 60min to obtain yellow precipitate, and filtering and washing to obtain the oxygen-deficient nano TiO 2.
The inorganic titanium source in the step (1) comprises: titanyl sulfate, titanium sulfate or titanium tetrachloride.
The inorganic alkali liquor in the step (2) comprises: sodium hydroxide, potassium hydroxide or ammonia.
The mass ratio of the hydrogen peroxide to the titanic acid precipitate in the step (4) is as follows: 2-4:1.
The room temperature in the step (5) is 15-25 ℃.
In the step (5), the mol ratio of hydroxylamine to TiO2 is as follows: 1: 20.
the invention has the beneficial effects that:
(1) the method for preparing the oxygen-deficient TiO2 by using the hydroxylamine to reduce the titanium peroxide can obviously improve the catalytic performance of TiO2 and increase the practical application value of TiO 2.
(2) The water phase preparation of the oxygen-deficient TiO2 at normal temperature and normal pressure is suitable for large-scale industrial production.
Drawings
FIG. 1 is an XRD pattern of the product of the present invention at various temperatures (a-25 ℃ C.; b-100 ℃ C.).
FIG. 2 is a Raman plot of the product of the invention at different temperatures (a-25 ℃ C.; b-100 ℃ C.).
FIG. 3 is a TEM image of the product at 25 ℃ (a); HRTEM (b), inset is selected electron diffraction pattern SAED.
FIG. 4 is a graph of UV-Vis for the product at different temperatures (a-25 ℃ C.; b-100 ℃ C.).
FIG. 5 is a graph showing the RhB degradation profile (a-25 ℃ C.; b-100 ℃ C.) under visible light conditions for the product at different temperatures.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1
Adding 8g of titanyl sulfate into 100ml of deionized water (0.5mol/L), and stirring for 60min to obtain a transparent titanyl sulfate solution; under the condition of mechanical stirring, adding ammonia water into the solution until the pH value of the system is 9 to obtain titanic acid precipitation suspension; washing the titanic acid precipitate suspension with deionized water for 3 times to obtain titanic acid precipitate (5.8 g); adding 11.6g of hydrogen peroxide solution (30 wt%) into titanic acid precipitate (the mass ratio of hydrogen peroxide to titanic acid precipitate is 2:1), and stirring to obtain a yellow and transparent titanium peroxide precursor; and adding 0.165g of 50% hydroxylamine solution into the titanium peroxide precursor, and stirring for 60min at the temperature of 25 ℃ to obtain the oxygen-deficient nano TiO 2.
Example 2
Adding 8g of titanyl sulfate into 100ml of deionized water, and stirring for 60min to obtain a transparent titanyl sulfate solution; under the condition of mechanical stirring, adding ammonia water into the solution until the pH value of the system is 9 to obtain titanic acid precipitation suspension; washing the titanic acid precipitate suspension liquid for 3 times by using deionized water to obtain titanic acid precipitate; adding 15ml of hydrogen peroxide solution (30 wt%) into titanic acid precipitate, and stirring to obtain a yellow transparent titanium peroxide precursor; and adding 0.165g of 50% hydroxylamine solution into the titanium peroxide precursor, and stirring for 60min at 100 ℃ to obtain the nano TiO 2.
Example 3
Adding 32g of titanyl sulfate into 100ml of deionized water (2mol/L), and stirring for 60min to obtain a transparent titanyl sulfate solution; under the condition of mechanical stirring, adding ammonia water into the solution until the pH value of the system is 9 to obtain titanic acid precipitation suspension; washing the titanic acid precipitate suspension with deionized water for 3 times to obtain titanic acid precipitate (23.2 g); adding 92.5g of hydrogen peroxide solution (30 wt%) into titanic acid precipitate (the mass ratio of hydrogen peroxide to titanic acid precipitate is 4:1), and stirring to obtain a yellow and transparent titanium peroxide precursor; and adding 0.66g of 50% hydroxylamine solution into the titanium peroxide precursor, and stirring for 60min at 25 ℃ to obtain the oxygen-deficient nano TiO 2.
Example 4
Adding 20g of titanyl sulfate into 100ml of deionized water (1mol/L), and stirring for 60min to obtain a transparent titanyl sulfate solution; under the condition of mechanical stirring, adding ammonia water into the solution until the pH value of the system is 9 to obtain titanic acid precipitation suspension; washing the titanic acid precipitate suspension with deionized water for 3 times to obtain titanic acid precipitate (14.5 g); 57.82g of hydrogen peroxide solution (30 wt%) is added into titanic acid precipitate (the mass ratio of hydrogen peroxide to titanic acid precipitate is 4:1), and yellow transparent titanium peroxide precursor is obtained by stirring; and adding 0.42g of 50% hydroxylamine solution into the titanium peroxide precursor, and stirring for 60min at 25 ℃ to obtain the oxygen-deficient nano TiO 2.
As shown in fig. 1, the TiO2 samples obtained at different synthesis temperatures showed typical diffraction peaks at 2 θ of 25.1 °, 37.7 °, 48.4 °, 54.1 °, 63.0 °, corresponding to the crystal planes of anatase TiO2(101), (004), (200), (115) and (204) (JCPDS card number 21-1272), respectively. At the reaction temperature of 25 ℃, the diffraction peak gradually became weaker and broadened, indicating that the crystallinity of the 25 ℃ sample was inferior to that of the higher temperature sample, which may lead to the formation of surface oxygen vacancies. There was little phase change at different reduction temperatures and no other diffraction peaks were observed. We observed a slight shift of the 25 ℃ diffraction peak to higher angles. According to the bragg equation, it is shown that the crystal spacing of TiO2 decreases at 25 ℃, which can be explained by the oxygen vacancies generated by the reduction reaction at low temperature.
As shown in fig. 2, the raman spectrum can observe the change in structure and short-range distortion caused by defects. Anatase TiO2 belongs to D4h (I41/amd) space group, and has five Raman activation modes at 149, 199, 399, 515 and 637cm-1There correspond to Eg, B1g, A1g + B1g and Eg modes. The peak of the 25 ℃ sample was significantly broadened from 149cm compared to the 100 ℃ sample-1Move to 147cm-1. It is further shown that surface oxygen vacancies disrupt the external vibration of the O-Ti-O bond and the symmetry of the anatase TiO2 lattice. Raman spectroscopy clearly supports the presence of surface oxygen vacancies, consistent with XRD results.
Fig. 3 shows TEM and HRTEM images of a 25 ℃ sample in the form of nanoparticle aggregates. The lattice spacing of 0.325nm corresponds to the (110) plane of anatase TiO2 in fig. 3 b. The Selected Area Electron Diffraction (SAED) mode (inset in fig. 3 a) exhibits well-resolved diffraction rings, indicating that the TiO2 nanoparticles have good crystallinity even at 25 ℃.
As shown in fig. 4: the uv-vis diffuse reflectance spectra of both samples are shown in fig. 4. The predominant absorption of the sample at 100 ℃ is in the UV wavelength range ((C))<400nm), the main absorption edge of the sample at 25 ℃ extends into the visible range. The band gap energies of the samples at 25 ℃ and 100 ℃ were 2.90eV and 3.10eV, respectively. The reduction of the band gap is advantageous for the photocatalysis of visible light. The improvement in visible light absorption of the sample at 25 ℃ is attributed to the formation of oxygen vacancies due to the formation of surface oxygen vacancies after reduction at low temperatures, resulting in Ti3+Is present.
FIG. 5 shows TiO2 nanoparticlesDecomposition of RhB by the particles under visible light. The photocatalytic degradation process of rhodamine B comprises dark reaction adsorption and photoproduction e-/h+The generation and separation of pairs, redox reactions and desorption of products. For the 100 ℃ sample, the decomposition rate of RhB in visible light was 33.2%, while that of the sample at 25 ℃ was 70.0%. The presence of oxygen vacancies traps electrons to facilitate the separation of photo-generated electrons and holes. The photocatalytic activity of the sample is improved.
Claims (6)
1. Oxygen-deficient TiO2The water phase preparation method under room temperature and normal pressure is characterized by comprising the following steps;
(1) dissolving an inorganic titanium source in deionized water, wherein the concentration of titanium ions is 0.5-2 mol/L, and obtaining a transparent inorganic titanium compound aqueous solution;
(2) adding an inorganic alkali solution into the aqueous solution of the inorganic titanium compound in the step (1) until the pH value is 7-10 to obtain a white titanic acid suspension;
(3) washing the white titanic acid suspension liquid in the step (2) by using deionized water, wherein the conductivity of the washed waste liquid is less than 1000 mu S/cm, and obtaining a white titanic acid precipitate;
(4) dissolving the white titanic acid precipitate in the step (3) by using hydrogen peroxide to obtain a yellow transparent titanium peroxide precursor;
(5) adding hydroxylamine solution into the yellow transparent titanium peroxide precursor obtained in the step (4) at room temperature, mechanically stirring for 60min to obtain yellow precipitate, filtering and washing to obtain the oxygen-deficient nano TiO2。
2. An oxygen deficient TiO according to claim 12The method for preparing the aqueous phase at room temperature and normal pressure is characterized in that the inorganic titanium source in the step (1) comprises the following steps: titanyl sulfate, titanium sulfate or titanium tetrachloride.
3. An oxygen deficient TiO according to claim 12The room-temperature normal-pressure water phase preparation method is characterized in that the inorganic alkali liquor in the step (2) comprises the following steps: sodium hydroxide, hydrogenPotassium oxide or ammonia.
4. An oxygen deficient TiO according to claim 12The preparation method of the water phase at room temperature and normal pressure is characterized in that the mass ratio of the hydrogen peroxide to the titanic acid precipitate in the step (4) is as follows: 2-4:1.
5. An oxygen deficient TiO according to claim 12The method for preparing the water phase at room temperature and normal pressure is characterized in that the room temperature in the step (5) is 15-25 ℃.
6. An oxygen deficient TiO according to claim 12The aqueous phase preparation method under room temperature and normal pressure is characterized in that hydroxylamine and TiO in the step (5)2The molar ratio is as follows: 1: 20.
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