CN107935039A - A kind of preparation method of titanium oxide water sol - Google Patents
A kind of preparation method of titanium oxide water sol Download PDFInfo
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- CN107935039A CN107935039A CN201711430340.8A CN201711430340A CN107935039A CN 107935039 A CN107935039 A CN 107935039A CN 201711430340 A CN201711430340 A CN 201711430340A CN 107935039 A CN107935039 A CN 107935039A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 66
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 59
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 54
- 239000002253 acid Substances 0.000 claims abstract description 53
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000010936 titanium Substances 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 17
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 11
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims description 21
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 16
- 238000001556 precipitation Methods 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 8
- 238000003916 acid precipitation Methods 0.000 claims description 8
- 229910001882 dioxygen Inorganic materials 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 239000000908 ammonium hydroxide Substances 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- DQTJHJVUOOYAMD-UHFFFAOYSA-N oxotitanium(2+) dinitrate Chemical compound [O-][N+](=O)O[Ti](=O)O[N+]([O-])=O DQTJHJVUOOYAMD-UHFFFAOYSA-N 0.000 claims description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- 239000012467 final product Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 238000002425 crystallisation Methods 0.000 abstract description 7
- 230000008025 crystallization Effects 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 239000002105 nanoparticle Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000001476 alcoholic effect Effects 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 description 15
- 238000002156 mixing Methods 0.000 description 8
- 239000004408 titanium dioxide Substances 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000001376 precipitating effect Effects 0.000 description 6
- 238000009826 distribution Methods 0.000 description 4
- 238000001935 peptisation Methods 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 150000001875 compounds Chemical group 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- -1 weaving Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002115 bismuth titanate Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005314 correlation function Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation method of titanium oxide water sol, aqueous slkali is added slowly in the inorganic salt solution of titanium, the metatitanic acid obtained using the inorganic salt hydrolysis of titanium is primary raw material, after hydrogen peroxide dissolves, obtain water miscible pertitanic acid, deionized water adjustment solid content is added into pertitanic acid solution again and after adding alcoholic solution, then irradiated and stirred the regular hour through ultraviolet light, make TiO using ultraviolet radiation2Sol particles is evenly distributed and average grain diameter reduces, and improves TiO2The crystallization degree of nano-particle at room temperature, traditional mode of heating is replaced with pure ultraviolet light, realizes TiO2Crystallization, obtained transparent water-based TiO 2 sol.Present invention process is simple, easily-controllable, environmental-friendly, and without complex device, manufacturing cost is cheap, obtained TiO2Colloidal particle better crystallinity degree, uniform particle sizes, prepare suitable for a large amount of, possess the possibility of industrialized production, be with a wide range of applications.
Description
Technical field
The present invention relates to inorganic nano colloidal sol technical field, and in particular to it is molten to prepare titanium dioxide water at normal temperatures and pressures
The method of glue.
Background technology
Nano-TiO2With excellent optical property, high chemical stability, heat endurance, nontoxicity, Superhydrophilic, non-
Migration, and being contacted completely with food, thus be widely used in anti-ultraviolet material, weaving, photocatalyst, glass with clean,
In suncream, coating, ink, packaging material for food, paper industry, aerospace industry, in solar cell, it is synthesized and application is ground
Study carefully the research emphasis of always correlation function Material Field.In recent years, as the improvement of people's living standards, to good life
Pursuit also increasingly increase.The application in terms of air purification indoors of optically catalytic TiO 2 product, has also obtained faster hair
Exhibition.
Traditional TiO 2 sol prepares and generally uses hydrolysis method.According to the difference of used raw material, main point
For two major class of organic titanium source and inorganic ti sources.Common organic titanium source is mainly the alkoxide of titanium, generally first dissolves the alkoxide of titanium
In nonaqueous solvents, by stirring and adding inhibitor, control Titanium alkoxides hydrolyze to obtain TiO 2 sol, the method obtain one
As be non-aqueous sol.Since the price of organic titanium source and solvent is somewhat expensive, researchers start with inorganic ti sources system
Standby aqueous sol.Generally include precipitation and two steps of peptization.Allow titaniferous inorganic compound raw under the action of aqueous slkali first
Into titanium dioxide precipitation, by washing, titanium dioxide precipitation is then subjected to peptization under the action of an acid, is dispersed in water again
In, TiO 2 sol is made.During peptization, it will usually introduce microwave heating or traditional heating control reaction speed
Degree.In addition, also have using ultrasonic method to prepare TiO 2 sol, using the mechanism of ultrasonic wave, cavitation and
Fuel factor.
In document《Alternative modification methods for sol–gel coatings of
silica,titania and silica–titania using ultraviolet irradiation and water
vapor》In, author investigation densification and crystal effect of the ultraviolet light irradiation to TiO 2 sol coating.《Ultraviolet light spoke
Penetrate the influence research to TiO 2 sol》In, pipe is spontaneous et al. to make TiO 2 sol particle distribution using ultraviolet radiation
Uniformly and average grain diameter reduces, and improves TiO2The crystallization degree of nano-particle at room temperature, text in the result shows that, in " non-light
The TEM patterns of TiO 2 particles are radiated, shows that titanium dioxide nano-particle distribution is relatively scattered, is differed from 3~45nm series, and
It is in irregular shape ", " light radiation processing gained TiO2Nano-particle narrow distribution and regular shape, size concentrate on 5~20nm ".
In document《UV irradiation effects on TiO2thin films》In, author investigation ultraviolet light is to TiO2Film
The influence of performance, simulates the use condition in aerospace applications.Documents disclose alkaline earth metal doping nanometer bismuth titanate and
Its preparation method, Application No. CN 05753048A, which disclose and " utilize ultraviolet radioactive colloidal sol so that complex compound function
Group is in excitation state, that is, has given the certain energy of complex compound, so that in follow-up sintering process, be without too high temperature
Nano-powder can be obtained." etc..Above-mentioned report is the influence for studying ultraviolet light irradiation to the TiO 2 sol prepared,
Rather than how using ultraviolet light the solution of titaniferous to be prepared into TiO 2 sol.
The content of the invention
To overcome above deficiency of the prior art or defect, the present invention to provide a kind of simple titanium oxide water sol
Preparation process, traditional mode of heating is replaced with pure ultraviolet light, and the solution of titaniferous is prepared into titanium dioxide using ultraviolet light
Titanium colloidal sol, realizes the crystallization of titanium dioxide, is produced on a large scale, better crystallinity degree, has wide applicability.
The technical solution used in the present invention is：A kind of preparation method of titanium oxide water sol, including and according to such as
The order of lower processing step carries out：
1) aqueous slkali is added slowly in the inorganic salt solution of titanium, obtains metatitanic acid precipitation, treat that precipitation is backward inclined completely
Deionized water is added in metatitanic acid precipitation, after standing and clarifying, removes supernatant, is in neutrality metatitanic acid precipitation through repeatedly washing；
2) hydrogen peroxide is added into the metatitanic acid being in neutrality after the repeatedly washing precipitation obtained by step 1), it is agitated uniform
Mixing, makes metatitanic acid precipitate peptization, obtains the opaque pertitanic acid solution of yellow；
3) add deionized water into pertitanic acid solution obtained by step 2), adjust the solid content of solution for 0.5~
2wt%, adds alcoholic solution；
4) it will be placed under ultraviolet light and irradiated through the solution obtained by step 3), while mechanical agitation is carried out to the solution,
Transparent water-based TiO 2 sol is can obtain after a period of time.
Further as above-mentioned technical proposal is improved, and the aqueous slkali described in step 1) is sodium hydroxide solution, hydroxide
One or more in potassium solution or ammonium hydroxide.
Further as above-mentioned technical proposal is improved, and the inorganic salt solution of the step 1) titanium is titanyl sulfate, nitric acid
It is one or two kinds of in oxygen titanium, and Ti4+Concentration is 0.05~1mol/l.
Further as above-mentioned technical proposal is improved, the pH value when metatitanic acid described in step 1) precipitates completely for 7~
12。
Further as above-mentioned technical proposal is improved, step 1) the metatitanic acid precipitation being in neutrality after repeatedly washing
PH value be 6.5~7.5.
Further as above-mentioned technical proposal is improved, and the concentration of the step 2) hydrogen peroxide be 20-30%, hydrogen peroxide and
Ti4+Molar ratio be 1~1.5:1.
Further as above-mentioned technical proposal is improved, and the alcohol described in step 3) is one kind in isopropanol or n-butanol
Or two kinds, the additive amount of alcohol is the 0-5wt% of solution quality after adjustment.
Further as above-mentioned technical proposal is improved, and the wavelength of the step 4) ultraviolet light is 100nm-400nm.
Further as above-mentioned technical proposal is improved, and step 4) the ultraviolet light irradiation time is 1-20h.
Further as above-mentioned technical proposal is improved, and the reaction condition of the preparation method is normal temperature and pressure.
The beneficial effects of the invention are as follows：Aqueous slkali is added slowly in the inorganic salt solution of titanium by the present invention, with the nothing of titanium
The metatitanic acid that machine salt hydrolysis obtain is primary raw material, after hydrogen peroxide dissolves, obtains water miscible pertitanic acid, then to peroxide titanium
After the solid content of deionized water adjustment system is added in acid solution and adds alcoholic solution, then one is irradiated and stirred through ultraviolet light
The fixed time, makes TiO 2 sol particle distribution uniformly and average grain diameter reduces, improve TiO using ultraviolet radiation2Receive
The crystallization degree of rice corpuscles at room temperature, traditional mode of heating is replaced with pure ultraviolet light, realizes the crystalline substance of titanium dioxide
Change, obtained transparent titanium oxide water sol.Present invention process is simple, easily-controllable, environmental-friendly, without complex device, system
Standby titania colloid particles better crystallinity degree of low cost, obtained, uniform particle sizes, prepare suitable for a large amount of, possess industry
Change manufacturing feasibility, be with a wide range of applications.
Embodiment
The present invention is specifically described with reference to embodiment, in order to technical field personnel to the present invention
Understand.It is necessary that herein the present invention will be further described it is emphasized that embodiment is only intended to, it is impossible to be interpreted as to this
The limitation of invention protection domain, fields person skilled in the art, according to foregoing invention content to non-made by the present invention
The modifications and adaptations of matter, should still fall within protection scope of the present invention.Mentioned raw materials following at the same time are unspecified,
For commercial product；It is processing step known to a person skilled in the art that the processing step or preparation method not referred in detail, which are,
Or preparation method.
Embodiment 1
A kind of preparation method of titanium oxide water sol, including and carried out according to the order of following processing step：
1) after the aqueous solution of titanyle sulfate for configuring 0.1mol/l at normal temperatures and pressures first, while slowly adding while stirring
Enter ammonium hydroxide, metatitanic acid is precipitated completely, at this time, the pH of metatitanic acid precipitation is 10, then adds deionized water in being precipitated to metatitanic acid,
Stir, stand and outwell supernatant after clarifying, after repeatedly washing, it is 7.5 to make the pH that metatitanic acid precipitates；
2) dioxygen that concentration is 20% is added into the metatitanic acid being in neutrality after the repeatedly washing precipitation obtained by step 1)
Water, hydrogen peroxide and Ti4+Molar ratio be 1：1, agitated uniformly mixing, obtains the opaque pertitanic acid solution of yellow；
3) deionized water is added into pertitanic acid solution obtained by step 2) again, its solid content is adjusted to 1wt%, and add
Enter the n-butanol of 1wt%；
4) it will be placed under the ultraviolet lamp of centre wavelength 254nm and irradiated through the solution obtained by step 3), while to solution
Be stirred, 5 it is small when after, obtain transparent titanium oxide water sol, make TiO 2 sol particle using ultraviolet radiation
It is evenly distributed and average grain diameter reduces, improves TiO2The crystallization degree of nano-particle at room temperature, so as to fulfill titanium dioxide
Crystallization.
Embodiment 2
A kind of preparation method of titanium oxide water sol, including and carried out according to the order of following processing step：
1) after the aqueous solution of titanyle sulfate for configuring 0.1mol/l at normal temperatures and pressures first, while slowly adding while stirring
Enter ammonium hydroxide, metatitanic acid is added deionized water after precipitating completely, stir, stand and outwell supernatant after clarifying, through repeatedly washing
The pH that metatitanic acid precipitates is set to be adjusted to 7.2；
2) dioxygen that concentration is 20% is added into the metatitanic acid being in neutrality after the repeatedly washing precipitation obtained by step 1)
Water, hydrogen peroxide and Ti4+Molar ratio be 1：1, agitated uniformly mixing, obtains the opaque pertitanic acid solution of yellow；
3) deionized water is added into pertitanic acid solution obtained by step 2) again, its solid content is adjusted to 1wt%, and add
Enter the isopropanol of 1wt%；
4) it will be placed under the ultraviolet lamp of centre wavelength 254nm and irradiated through the solution obtained by step 3), while to solution
Be stirred, 5 it is small when after, obtain transparent titanium oxide water sol.
Embodiment 3
A kind of preparation method of titanium oxide water sol, including and carried out according to the order of following processing step：
1) after the titanyl nitrate solution for configuring 0.05mol/l at normal temperatures and pressures first, while slowly adding while stirring
Enter ammonium hydroxide, metatitanic acid is added deionized water after precipitating completely, stir, stand and outwell supernatant after clarifying, through repeatedly washing
The pH that metatitanic acid precipitates is set to be adjusted to 7.0；
2) dioxygen that concentration is 20% is added into the metatitanic acid being in neutrality after the repeatedly washing precipitation obtained by step 1)
Water, hydrogen peroxide and Ti4+Molar ratio be 1：1, agitated uniformly mixing, obtains the opaque pertitanic acid solution of yellow；
3) deionized water is added into pertitanic acid solution obtained by step 2) again, its solid content is adjusted to 1wt%, and add
Enter the n-butanol of 1wt%；
4) it will be placed under the ultraviolet lamp of centre wavelength 254nm and irradiated through the solution obtained by step 3), while to solution
Be stirred, 5 it is small when after, obtain transparent titanium oxide water sol.
Embodiment 4
A kind of preparation method of titanium oxide water sol, including and carried out according to the order of following processing step：
1) after the aqueous solution of titanyle sulfate for configuring 0.1mol/l at normal temperatures and pressures first, while slowly adding while stirring
Enter ammonium hydroxide, metatitanic acid is added deionized water after precipitating completely, stir, stand and outwell supernatant after clarifying, through repeatedly washing
The pH that metatitanic acid precipitates is set to be adjusted to 6.5；
2) dioxygen that concentration is 20% is added into the metatitanic acid being in neutrality after the repeatedly washing precipitation obtained by step 1)
Water, hydrogen peroxide and Ti4+Molar ratio be 1：1, agitated uniformly mixing, obtains the opaque pertitanic acid solution of yellow；
3) deionized water is added into pertitanic acid solution obtained by step 2) again, its solid content is adjusted to 1wt%, and add
Enter the n-butanol of 1wt%；
4) it will be placed under the ultraviolet lamp of centre wavelength 365nm and irradiated through the solution obtained by step 3), while to solution
Be stirred, 20 it is small when after, obtain transparent titanium oxide water sol.
Embodiment 5
A kind of preparation method of titanium oxide water sol, including and carried out according to the order of following processing step：
1) after the aqueous solution of titanyle sulfate for configuring 0.1mol/l at normal temperatures and pressures first, while slowly adding while stirring
Enter sodium hydroxide solution, metatitanic acid is added deionized water after precipitating completely, stir, stand and supernatant is outwelled after clarifying, pass through
The pH that repeatedly washing precipitates metatitanic acid is adjusted to 7.5；
2) dioxygen that concentration is 20% is added into the metatitanic acid being in neutrality after the repeatedly washing precipitation obtained by step 1)
Water, hydrogen peroxide and Ti4+Molar ratio be 1：1, agitated uniformly mixing, obtains the opaque pertitanic acid solution of yellow；
3) deionized water is added into pertitanic acid solution obtained by step 2) again, its solid content is adjusted to 1wt%, and add
Enter the n-butanol of 1wt%；
4) it will be placed under the ultraviolet lamp of centre wavelength 100nm and irradiated through the solution obtained by step 3), while to solution
Be stirred, 5 it is small when after, obtain transparent titanium oxide water sol.
Embodiment 6
A kind of preparation method of titanium oxide water sol, including and carried out according to the order of following processing step：
1) after the aqueous solution of titanyle sulfate for configuring 0.1mol/l at normal temperatures and pressures first, while slowly adding while stirring
Enter potassium hydroxide solution, metatitanic acid is added deionized water after precipitating completely, stir, stand and supernatant is outwelled after clarifying, pass through
The pH that repeatedly washing precipitates metatitanic acid is adjusted to 7.5；
2) dioxygen that concentration is 20% is added into the metatitanic acid being in neutrality after the repeatedly washing precipitation obtained by step 1)
Water, hydrogen peroxide and Ti4+Molar ratio be 1：1, agitated uniformly mixing, obtains the opaque pertitanic acid solution of yellow；
3) deionized water is added into pertitanic acid solution obtained by step 2) again, its solid content is adjusted to 1wt%, and add
Enter the n-butanol of 1wt%；
4) it will be placed under the ultraviolet lamp of centre wavelength 400nm and irradiated through the solution obtained by step 3), while to solution
Be stirred, 5 it is small when after, obtain transparent titanium oxide water sol.
Embodiment 7
A kind of preparation method of titanium oxide water sol, including and carried out according to the order of following processing step：
1) after the aqueous solution of titanyle sulfate for configuring 0.1mol/l at normal temperatures and pressures first, while slowly adding while stirring
Enter ammonium hydroxide, metatitanic acid is added deionized water after precipitating completely, stir, stand and outwell supernatant after clarifying, through repeatedly washing
The pH that metatitanic acid precipitates is set to be adjusted to 7.5；
2) dioxygen that concentration is 20% is added into the metatitanic acid being in neutrality after the repeatedly washing precipitation obtained by step 1)
Water, hydrogen peroxide and Ti4+Molar ratio be 1：1, agitated uniformly mixing, obtains the opaque pertitanic acid solution of yellow；
3) deionized water is added into pertitanic acid solution obtained by step 2) again, its solid content is adjusted to 1wt%, and add
Enter the n-butanol of 1wt%；
4) it will be placed under the ultraviolet lamp of centre wavelength 194nm and irradiated through the solution obtained by step 3), while to solution
Be stirred, 1 it is small when after, obtain transparent titanium oxide water sol.
Above-described embodiment is the preferred embodiment of the present invention, all with similar technique of the invention and the equivalence changes made,
The protection category of the present invention should all be belonged to.
Claims (10)
- A kind of 1. preparation method of titanium oxide water sol, it is characterised in that the order including and according to following processing step Carry out：1) aqueous slkali is added slowly in the inorganic salt solution of titanium, obtains metatitanic acid precipitation, treat to precipitate backward metatitanic acid completely Deionized water is added in precipitation, after standing and clarifying, removes supernatant, is in neutrality metatitanic acid precipitation through repeatedly washing；2) hydrogen peroxide is added into the metatitanic acid being in neutrality after the repeatedly washing precipitation obtained by step 1), it is agitated uniformly mixed Close, obtain the opaque pertitanic acid solution of yellow；3) deionized water being added into pertitanic acid solution obtained by step 2), the solid content for adjusting solution is 0.5~2wt%, then Add alcohol；4) it will be placed under ultraviolet light and irradiated through the solution obtained by step 3), while mechanical agitation is carried out to the solution, to obtain the final product To transparent titanium oxide water sol.
- 2. the preparation method of titanium oxide water sol according to claim 1, it is characterised in that：Alkali described in step 1) Solution is the one or more in sodium hydroxide solution, potassium hydroxide solution or ammonium hydroxide.
- 3. the preparation method of titanium oxide water sol according to claim 1, it is characterised in that：Step 1) the titanium Inorganic salt solution is titanyl sulfate, one or two kinds of in titanyl nitrate, and Ti4+Concentration is 0.05~1mol/l.
- 4. the preparation method of water-based TiO 2 sol according to claim 1, it is characterised in that：It is inclined described in step 1) PH value when metatitanic acid precipitates completely is 7~12.
- 5. the preparation method of water-based TiO 2 sol according to claim 1, it is characterised in that：Step 1) is described through more The pH value for the metatitanic acid precipitation being in neutrality after secondary washing is 6.5~7.5.
- 6. the preparation method of titanium oxide water sol according to claim 1, it is characterised in that：Step 2) the dioxygen The concentration of water is 20-30%, hydrogen peroxide and Ti4+Molar ratio be 1~1.5：1.
- 7. the preparation method of titanium oxide water sol according to claim 1, it is characterised in that：Alcohol described in step 3) To be one or two kinds of in isopropanol or n-butanol, the additive amount of alcohol is the 0-5wt% of solution quality after adjustment.
- 8. the preparation method of titanium oxide water sol according to claim 1, it is characterised in that：Purple described in step 4) The outer a length of 100nm-400nm of light wave.
- 9. the preparation method of titanium oxide water sol according to claim 1, it is characterised in that：Purple described in step 4) Outer smooth exposure time is 1-20h.
- 10. the preparation method of titanium oxide water sol according to claim 1, it is characterised in that the preparation method Reaction condition be normal temperature and pressure.
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| CN108998146A (en) * | 2018-08-21 | 2018-12-14 | 芜湖聚焰生物质能源科技有限公司 | The biomass moulding solid fuel production preparation method and resistive connection slag agent of resistive connection slag agent |
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| CN113003617B (en) * | 2021-02-26 | 2023-11-14 | 南方科技大学 | Multi-element oxide and preparation method and application thereof |
| CN115024315A (en) * | 2022-04-22 | 2022-09-09 | 北京富莱士博科技发展有限公司 | Synthetic method of antibacterial nano hydrosol |
| CN115818705A (en) * | 2022-11-21 | 2023-03-21 | 重庆德强化工有限公司 | Method for preparing superfine barium titanate by using nano titanium dioxide |
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