CN101497459A - Method for preparing nano-scale anatase titanium dioxide powder - Google Patents
Method for preparing nano-scale anatase titanium dioxide powder Download PDFInfo
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- CN101497459A CN101497459A CNA200810045342XA CN200810045342A CN101497459A CN 101497459 A CN101497459 A CN 101497459A CN A200810045342X A CNA200810045342X A CN A200810045342XA CN 200810045342 A CN200810045342 A CN 200810045342A CN 101497459 A CN101497459 A CN 101497459A
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Abstract
The invention discloses a method for preparing nanometer anatase titanium dioxide powder, which is characterized in that 100 weight portions of metatitanic acid is washed by 100 to 150 weight portions of deionized water or distilled water for multiple times first to remove SO4<2->; then 1 to 15 weight portions of alkaline foaming agent is added into a water solution, and the pH value is adjusted to be between 8.0 and 11.0; then 1 to 15 weight portions of surfactant is added into the water solution, the mixture is mixed evenly to obtain a precursor; and finally the precursor is placed in a reaction furnace and reacts at a temperature of between 500 and 750 DEG C for 2 to 3h to obtain the anatase titanium dioxide powder with an average grain diameter of between 20 and 80nm and evenly particle size distribution.
Description
Technical field
The present invention relates to a kind of preparation method of Nano titanium dioxide powder, specifically a kind of preparation method who is used as the dichloride in anatase type grade titanium dioxide powder of makeup, photocatalyst, photochromics etc.The preparation field that belongs to nanometer materials.
Background technology
Nano-TiO
2It is a kind of nano material that is most widely used at present, wherein, the dichloride in anatase type grade titanium dioxide has at aspects such as makeup, photocatalyst, photochromics, chemical catalysis agent carrier and chemical fibre delustrings widely and uses owing to have good ultraviolet radiation absorption characteristic and excellent photocatalysis activity.
The preparation method of dichloride in anatase type grade titanium dioxide mainly contains titanium tetrachloride vapour phase oxidation process, titanyl sulfate or titanium sulfate solution liquid phase water solution, sol-gel processing etc.The titanium tetrachloride vapour phase oxidation process prepares nanometer anatase titania need be finished in hot conditions following moment, and this method requires the control condition strictness, the technical difficulty height, and equipment corrosion is serious, the production cost height, general manufacturer is difficult to accept; The particle diameter of the nanometer anatase titania that titanyl sulfate or titanium sulfate solution liquid-phase hydrolysis method make is bigger than normal, and the photocatalytic activity of this kind product is reduced greatly; In adopting the sol-gel method preparation process, titanium colloidal sol is difficult to thoroughly separate with water, makes the powder bonded that makes serious, and the calcining back is difficult to depolymerization, causes the nano titanium dioxide powder bad dispersibility, and particle diameter is bigger.
The Nano titanium dioxide powder is easy to form coacervate owing to have bigger specific surface area and surface energy.Reunion between the Nano titanium dioxide powder generally is divided into two kinds: the soft-agglomerated and hard aggregation between TiO 2 particles.Soft-agglomerated between TiO 2 particles mainly is because due to intergranular Van der Waals force and the Coulomb's force, and this reunion can be eliminated by some chemical actions or the mode that applies mechanical energy; The existence of hard aggregation makes the dispersed variation of product, influences the result of use and the range of application of product.Therefore, how to alleviate the agglomeration between nano-titania particle, be the nano titanium oxide suitability for industrialized production the problem that must solve.
In recent years, Chinese patent CN1363521A makes raw material with metatitanic acid, adopt the positive metatitanic acid of the molten acquisition of alkali, the colloidal sol of the molten acquisition titanium dioxide of acid, with flocculation agent TiO 2 sol is condensed with water squeezing and to handle, separate TiO 2 sol with organic substance extraction, calcining and decomposing is removed organism under the decomposition temperature of flocculation agent again, obtains the nanometer titanium dioxide titanium valve of anatase crystal type.This method complex process, production cost height, be difficult for industrialization.
Chinese patent CN1636880A is added to the metatitanic acid wet stock of certain mass in the distilled water, is mixed with metatitanic acid suspension, dropwise adds Na then
2CO
3The aqueous solution equals 9～11 up to pH; Add after the above-mentioned alkali lye, stir on one side, add carboxylic organism or glycerine on one side as modifier, aging 50～80 ℃ of temperature; Be precipitated to the specific conductivity of filtrate less than 20mS/m with distilled water wash, metatitanic acid after handling as stated above, adding nitric acid and distilled water is 0.1 up to metatitanic acid mixing solutions pH value, at room temperature aging then 1h, suspension after aging is put into the stainless steel hydrolysis still of teflon lined, behind 130～160 ℃ of reactions of temperature 10h, obtain anatase-type nanometer titanium dioxide.This preparation method exists severe reaction conditions, complex process, long reaction time, is unfavorable for the industrialization of nano titanium oxide.
Chinese patent CN1076319C is with H
2TiO
3And H
2SO
4The TiOSO that reaction generates
4Be raw material, urea is the precipitation from homogeneous solution agent, TiOSO
4Concentration be 1.44 * 10
-3G/L, urea and TiOSO
4Weight ratio be 1:1～5:1, the temperature of reaction of hydrolysis of urea is 95～110 ℃, the reaction times is 2.5～4h, generates TiO (OH)
2, with TiO (OH)
2At 800～1000 ℃ of calcinings of temperature, 2.5～3.5h, obtain nano level TiO
2The technology of this method is simpler, but temperature of reaction is higher, and the nano titanium oxide that makes is reunited easily, influences its application.
Chinese patent CN1156403C selects for use the intermediates of sulfuric acid titanium powder plant production to be main raw material, and is molten through alkali, washing, the hydrochloric acid peptization, organic water squeezing, distillation, thermal treatment, technologies such as pulverizing can be prepared the nano titanium oxide of anatase titanium dioxide, rutile-type and mixed crystal type.This method exists that product single crystal form purity is lower, complex process, be difficult for shortcomings such as industrialization.
Summary of the invention
The objective of the invention is to provide a kind of preparation method of nano-scale anatase titanium dioxide powder, be characterized in that the product that this method makes can satisfy the application of nano-scale anatase titanium dioxide powder in fields such as makeup, photocatalyst, photochromics and chemical catalysis agent carriers at the deficiencies in the prior art.
Purpose of the present invention is realized that by following technical measures wherein raw materials used umber is weight fraction except that specified otherwise.
With 100 parts of metatitanic acids, with deionized water or distilled water 100-150 part flushing several, remove SO earlier
4 2-In the above-mentioned aqueous solution, add alkaline whipping agent 1-15 part then, regulate pH value to 8.0～11.0, add 1～15 part of surface-modifying agent again, make presoma after mixing, at last presoma is placed Reaktionsofen, 2～3h acquires median size 20-80nm, the anatase titanium dioxide powder of even particle size distribution in 500～750 ℃ of reactions of temperature.
The alkalescence whipping agent is at least a in urea, volatile salt, bicarbonate of ammonia, ammonium nitrate, azo dimethyl formamide, sodium bicarbonate and the lime carbonate;
Surface-modifying agent is at least a in stearic acid, water glass, Tai-Ace S 150, polyvinyl alcohol, polyoxyethylene glycol, Lanthanum trichloride and the Cerium II Chloride;
The nano-scale anatase titanium dioxide powder for preparing according to the method described above.
Nano-scale anatase titanium dioxide powder is used for makeup, photocatalyst, photochromics and chemical catalysis agent carrier field.
Performance test
Nano-scale anatase titanium dioxide powder adopts the X-ray diffractometer test as shown in Figure 1.The result shows: the grain-size of the nano-scale anatase titanium dioxide powder that makes is 20-80nm.
Nano-scale anatase titanium dioxide powder adopts transmissioning electric mirror test as shown in Figure 2.The result shows: the median size of the nano-scale anatase titanium dioxide powder that makes is 20-80nm.
The present invention has following advantage:
1 is raw material with the metatitanic acid, and raw material sources are abundant, and are cheap, saves cost.
2 temperature of reaction are low, and the reaction times is short, save energy.
3 preparation technologies are simple, and control helps suitability for industrialized production easily.
4 alkaline whipping agents can be removed H residual in the meta-titanium acid solution
+, also can in calcination process, emit gas, reduce the intergranular reunion of Nano titanium dioxide;
5 surface-modifying agents can further reduce the intergranular reunion of Nano titanium dioxide, make the product granularity uniform distribution, the size that make tiny, thereby enlarge the use range of titanium dioxide.
Description of drawings
Fig. 1 is the X-ray diffractogram of nano-scale anatase titanium dioxide powder;
Fig. 2 is the transmission electron microscope picture of nano-scale anatase titanium dioxide powder.
Embodiment
Below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the content of the invention described above.
Embodiment 1:
With metatitanic acid 100g, with deionized water 100ml flushing for several times, remove SO earlier
4 2-Urea 1g is added in the metatitanic acid aqueous solution, regulate pH value to 8, add stearic acid 15g again, uniform mixing makes presoma, at last presoma is placed Reaktionsofen, in 600 ℃ of reactions of temperature 2.5h, obtain median size 20nm, the anatase titanium dioxide powder of even particle size distribution.
Embodiment 2:
With metatitanic acid 100g, with distilled water 120ml flushing for several times, remove SO earlier
4 2-To mix in the azo dimethyl formamide 1g and the urea 5g adding metatitanic acid aqueous solution, regulate pH value to 9, and then adding water glass 2g, uniform mixing makes presoma, at last presoma is placed Reaktionsofen, in 750 ℃ of reactions of temperature 2h, obtain median size 40nm, the anatase titanium dioxide powder of even particle size distribution.
Embodiment 3:
With metatitanic acid 100g, with deionized water 150ml flushing for several times, remove SO earlier
4 2-Volatile salt 10g is dissolved in the metatitanic acid aqueous solution, regulates pH value to 11, and then add Cerium II Chloride 1g, uniform mixing makes presoma, at last presoma is placed Reaktionsofen, in 700 ℃ of reactions of temperature 2h, obtain median size 80nm, the anatase titanium dioxide powder of even particle size distribution.
Embodiment 4:
With metatitanic acid 100g, with deionized water 130ml flushing for several times, remove SO earlier
4 2-Bicarbonate of ammonia 5g and sodium bicarbonate 10g are dissolved in the metatitanic acid aqueous solution, regulate pH value to 10, and then adding polyvinyl alcohol 2g and polyoxyethylene glycol 2 gram and Lanthanum trichloride 1g, uniform mixing makes presoma, at last presoma is placed Reaktionsofen, in 500 ℃ of reactions of temperature 3h, obtain median size 30nm, the anatase titanium dioxide powder of even particle size distribution.
Claims (5)
1, a kind of preparation method of nano-scale anatase titanium dioxide powder is characterized in that this method is with metatitanic acid 100 weight parts, with deionized water or distilled water 100-150 weight part flushing several, removes SO earlier
4 2-In the above-mentioned aqueous solution, add alkaline whipping agent 1-15 weight part then, regulate pH value to 8.0～11.0, add surface-modifying agent 1～15 weight part again, make presoma after mixing, at last presoma is placed Reaktionsofen, in 500～750 ℃ of reactions of temperature, 2～3h, acquire median size 20-80nm, the anatase titanium dioxide powder of even particle size distribution.
2,, it is characterized in that alkaline whipping agent is at least a in urea, volatile salt, bicarbonate of ammonia, ammonium nitrate, azo dimethyl formamide, sodium bicarbonate and the lime carbonate according to the preparation method of the described nano-scale anatase titanium dioxide powder of claim 1.
3,, it is characterized in that surface-modifying agent is at least a in stearic acid, water glass, polyvinyl alcohol, polyoxyethylene glycol, Lanthanum trichloride and the Cerium II Chloride according to the preparation method of the described nano-scale anatase titanium dioxide powder of claim 1.
4, the nano-scale anatase titanium dioxide powder for preparing according to the described method of claim 1.
5, be used for makeup, photocatalyst, photochromics and chemical catalysis agent carrier field according to the described nano-scale anatase titanium dioxide powder of claim 4.
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| CNA200810045342XA CN101497459A (en) | 2008-02-02 | 2008-02-02 | Method for preparing nano-scale anatase titanium dioxide powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103586017A (en) * | 2013-11-22 | 2014-02-19 | 西南化工研究设计院有限公司 | Preparation method of titanium and tungsten powder for flue gas denitration catalyst and product prepared through preparation method |
| CN105949718A (en) * | 2016-05-06 | 2016-09-21 | 安徽和润特种玻璃有限公司 | High-hardness heat-resistant coating for anti-dazzle glass |
| CN106243680A (en) * | 2016-08-01 | 2016-12-21 | 江苏卧尔康家居用品有限公司 | A kind of nano titanium oxide strengthens the preparation method of polyurethane material |
| CN106365200A (en) * | 2016-09-19 | 2017-02-01 | 攀枝花学院 | High-purity ultra-fine titanium dioxide prepared from industrial metatitanic acid and preparation method of titanium dioxide |
-
2008
- 2008-02-02 CN CNA200810045342XA patent/CN101497459A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103586017A (en) * | 2013-11-22 | 2014-02-19 | 西南化工研究设计院有限公司 | Preparation method of titanium and tungsten powder for flue gas denitration catalyst and product prepared through preparation method |
| CN103586017B (en) * | 2013-11-22 | 2015-03-25 | 西南化工研究设计院有限公司 | Preparation method of titanium and tungsten powder for flue gas denitration catalyst and product prepared through preparation method |
| CN105949718A (en) * | 2016-05-06 | 2016-09-21 | 安徽和润特种玻璃有限公司 | High-hardness heat-resistant coating for anti-dazzle glass |
| CN106243680A (en) * | 2016-08-01 | 2016-12-21 | 江苏卧尔康家居用品有限公司 | A kind of nano titanium oxide strengthens the preparation method of polyurethane material |
| CN106243680B (en) * | 2016-08-01 | 2020-11-17 | 江苏卧尔康家居用品有限公司 | Preparation method of nano titanium dioxide reinforced polyurethane material |
| CN106365200A (en) * | 2016-09-19 | 2017-02-01 | 攀枝花学院 | High-purity ultra-fine titanium dioxide prepared from industrial metatitanic acid and preparation method of titanium dioxide |
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Open date: 20090805 |