CN101234782B - Method for preparing high pure macroparticle anatase type titanium dioxide - Google Patents
Method for preparing high pure macroparticle anatase type titanium dioxide Download PDFInfo
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- CN101234782B CN101234782B CN2008100706813A CN200810070681A CN101234782B CN 101234782 B CN101234782 B CN 101234782B CN 2008100706813 A CN2008100706813 A CN 2008100706813A CN 200810070681 A CN200810070681 A CN 200810070681A CN 101234782 B CN101234782 B CN 101234782B
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Abstract
The invention provides a method for preparing big-particle anatase-type titanium dioxide of high-purity; titanium dioxide of 0.5-2g and alkaline solution of 10-15mol/L with density of 40-60ml are evenly mixed in a stainless steel autoclave or a tetrafluoroethylene vessel; the mixture reacts for 60-100 hours under 453-493 K; pH value of the generated product is regulated to 9-11; and after the product reacts for 2-3 days under 453-493 K in the stainless steel autoclave or the tetrafluoroethylene vessel; after being fully washed by distilled water, the high-purity big-particle anatase-type titanium dioxide is finally obtained by ambient drying for 1-40 hours under 323-373 K. The method for preparing the high-purity big-particle anatase-type titanium dioxide has the advantages of simple operation, low cost, high purity, stable performance and mass synthesis; furthermore, the biggest particle of the prepared big-particle anatase-type titanium dioxide is up to 3.6 micrometers with high purity.
Description
Technical field
The invention belongs to field of nano material preparation, more specifically relate to a kind of preparation method of high pure macroparticle anatase type titanium dioxide.
Background technology
The refractive index of macroparticle anatase type titanium dioxide is 2.52, and is also higher than adamantine refractive index 2.42, is a kind of good optical material.High pure macroparticle anatase type titanium dioxide is a kind of good optical material, can be widely used in optics such as making laser transmitter.But according to Theoretical Calculation, when the anatase titania particle will take place during greater than tens nanometers by anatase octahedrite mutually to the crystal transition of rutile phase.Therefore, the pure phase anatase type titanium dioxide of macroparticle is difficult to synthetic.Traditional sulfuric acid process or adding nucleus method all can not obtain the pure phase anatase type titanium dioxide of macroparticle.The relevant report that the preparation high pure macroparticle anatase type titanium dioxide is not also arranged at present.
Goal of the invention
The preparation method who the purpose of this invention is to provide a kind of high pure macroparticle anatase type titanium dioxide, this method is not only easy and simple to handle, cost is low, purity is high, stable performance, can synthesize in a large number, and the particle of macroparticle anatase type titanium dioxide maximum of preparation reaches 3.6 microns, and has very high purity.
Preparation method of the present invention is: 0.5～2 gram titanium dioxide and concentration are that alkaline solution thorough mixing in stainless steel autoclave or polytetrafluoroethylcontainer container of 40～60 milliliter of 10～15 mol is even, and mixture reacts 60～100h under 453～493K; The product pH value that generates is adjusted to 9～11, be placed on again under 453～493K, react 2～3 days in stainless steel autoclave or the polytetrafluoroethylcontainer container after, behind the distilled water thorough washing, constant pressure and dry 1～40h obtains final high pure macroparticle anatase type titanium dioxide under 323～373K.
Remarkable advantage of the present invention is: the present invention adds under the condition of any tensio-active agent and template at a lower temperature and not, has prepared high pure macroparticle anatase type titanium dioxide with simple method.Maximum particle reaches 3.6 microns, this is the maximum anatase titanium dioxide of synthetic so far, and this method is not only easy and simple to handle, cost is low, purity is high, stable performance, can synthesize in a large number, and the particle of macroparticle anatase type titanium dioxide maximum of preparation reaches 3.6 microns, and has very high purity.At first, the existence of hydroxide ion can change the surface energy of anatase titanium dioxide and form the high pure macroparticle bipyramid.Secondly, the presoma titanate is a laminate structure, and is octahedra by being total to the mode be combined on limit by TiO6.Under hydrothermal condition, the basic structure of titanate is shunk on the fixed position, reduces its interlamellar spacing, and is converted into the anatase titanium dioxide structure.The forming process of macroparticle anatase bipyramid comprises breaking of presoma and dissolves two steps of nucleation.The anatase titania of nuclear shape similarly is the octahedra bipyramid seed that a quilt cuts tip, by eight equal 101} face and two equal { the 001} face is formed.{ surface free energy of 001} face is that { 1.4 times of 101} face, the face that free energy is high will at first disappear in process of growth.According to Ostwald ripening mechanism, the system that free energy is low more is stable more, and the growth of macroparticle is finished by consuming small-particle.Because { free energy of 001} face is higher, and the speed of growth is very fast, and what also disappear is the fastest, has therefore formed the anatase titanium dioxide macroparticle of bicone.
Description of drawings
Fig. 1 is the electromicroscopic photograph of product of the present invention, and wherein (a) part is a stereoscan photograph, and (b) part is a transmission electron microscope photo.
Fig. 2 is the X-ray powder diffraction figure of product of the present invention.
Embodiment
The alkaline solution thorough mixing in stainless steel autoclave or polytetrafluoroethylcontainer container that at first with 0.5～2 gram titanium dioxide and concentration is 40～60 milliliter of 10～15 mol is even, and mixture reacts 60～100h under 453～493K; The product pH value that generates is adjusted to 9～11, be placed on again under 453～493K, react 2～3 days in stainless steel autoclave or the polytetrafluoroethylcontainer container after, behind the distilled water thorough washing, constant pressure and dry 1～40h obtains final high pure macroparticle anatase type titanium dioxide under 323～373K.
Described alkaline solution is a caustic soda soln.
The product pH value of described generation is regulated hydrochloric acid or the nitric acid that adopts 0.1～0.5 mol.
The described dry constant pressure and dry that adopts.
The particle of the macroparticle anatase type titanium dioxide maximum that the present invention prepares reaches 3.6 microns, and purity is more than 99%.
Following examples specify the present invention, but are not limited only to this.
Embodiment 1
The caustic soda thorough mixing in stainless steel autoclave or polytetrafluoroethylcontainer container that at first with 1 gram titanium dioxide and 50 ml concns is 10 mol is even, and mixture reacts 72h under 473K; The product pH value that generates is adjusted to 10.5, is placed in stainless steel autoclave or the polytetrafluoroethylcontainer container to react under 473K after 2 days again, and behind the distilled water thorough washing, dry 6h obtains final high pure macroparticle anatase type titanium dioxide under 373K.Described alkaline solution is a caustic soda soln.
The product pH value of described generation is regulated the hydrochloric acid that adopts 0.1 mol.The described dry constant pressure and dry that adopts.Preparation
The particle of the macroparticle anatase type titanium dioxide maximum that goes out reaches 3.6 microns, and purity is more than 99%.
Embodiment 2
The caustic soda thorough mixing in stainless steel autoclave or polytetrafluoroethylcontainer container that at first with 0.5 gram titanium dioxide and 40 ml concns is 10 mol is even, and mixture reacts 60h under 453K; The product pH value that generates is adjusted to 9, is placed in stainless steel autoclave or the polytetrafluoroethylcontainer container to react under 453K after 2 days again, and behind the distilled water thorough washing, dry 1h obtains final high pure macroparticle anatase type titanium dioxide under 323K.Described alkaline solution is a caustic soda soln.
The product pH value of described generation is regulated the nitric acid that adopts 0.1 mol.The described dry constant pressure and dry that adopts.The particle of the macroparticle anatase type titanium dioxide maximum of preparing reaches 3.6 microns, and purity is more than 99%.
Embodiment 3
The caustic soda thorough mixing in stainless steel autoclave or polytetrafluoroethylcontainer container that at first with 2 gram titanium dioxide and 60 ml concns is 15 mol is even, and mixture reacts 100h under 493K; The product pH value that generates is adjusted to 11, is placed in stainless steel autoclave or the polytetrafluoroethylcontainer container to react under 493K after 3 days again, and behind the distilled water thorough washing, dry 40h obtains final high pure macroparticle anatase type titanium dioxide under 373K.Described alkaline solution is a caustic soda soln.
The product pH value of described generation is regulated the nitric acid that adopts 0.5 mol.The described dry constant pressure and dry that adopts.The particle of the macroparticle anatase type titanium dioxide maximum of preparing reaches 3.6 microns, and purity is more than 99%.
Embodiment 4
The caustic soda thorough mixing in stainless steel autoclave or polytetrafluoroethylcontainer container that at first with 1.5 gram titanium dioxide and 50 ml concns is 12 mol is even, and mixture reacts 70h under 470K; The product pH value that generates is adjusted to 10, is placed in stainless steel autoclave or the polytetrafluoroethylcontainer container to react under 470K after 3 days again, and behind the distilled water thorough washing, dry 20h obtains final high pure macroparticle anatase type titanium dioxide under 353K.Described alkaline solution is a caustic soda soln.
The product pH value of described generation is regulated the hydrochloric acid that adopts 0.5 mol.The described dry constant pressure and dry that adopts.The particle of the macroparticle anatase type titanium dioxide maximum of preparing reaches 3.6 microns, and purity is more than 99%.
Embodiment 5
The caustic soda thorough mixing in stainless steel autoclave or polytetrafluoroethylcontainer container that at first with 1.5 gram titanium dioxide and 45 ml concns is 13 mol is even, and mixture reacts 80h under 483K; The product pH value that generates is adjusted to 10.5, is placed in stainless steel autoclave or the polytetrafluoroethylcontainer container to react under 483K after 2 days again, and behind the distilled water thorough washing, dry 30h obtains final high pure macroparticle anatase type titanium dioxide under 373K.Described alkaline solution is a caustic soda soln.
The product pH value of described generation is regulated the hydrochloric acid that adopts 0.3 mol.The described dry constant pressure and dry that adopts.The particle of the macroparticle anatase type titanium dioxide maximum of preparing reaches 3.6 microns, and purity is more than 99%.
Claims (3)
1. the preparation method of an anatase titanium dioxide, it is characterized in that: described preparation method is: 0.5～2 gram titanium dioxide and 40～60 ml concns are that alkaline solution thorough mixing in stainless steel autoclave or polytetrafluoroethylcontainer container of 10～15 mol is even, and mixture reacts 60～100h under 453～493K; The product pH value that generates is adjusted to 9～11, be placed on again under 453～493K, react 2～3 days in stainless steel autoclave or the polytetrafluoroethylcontainer container after, behind the distilled water thorough washing, constant pressure and dry 1～40h obtains final high pure macroparticle anatase type titanium dioxide under 323～373K; The particle of the above-mentioned high pure macroparticle anatase type titanium dioxide maximum of preparing reaches 3.6 microns.
2. the preparation method of anatase titanium dioxide according to claim 1, it is characterized in that: described alkaline solution is a caustic soda soln.
3. the preparation method of anatase titanium dioxide according to claim 1 is characterized in that: the hydrochloric acid or the nitric acid of product pH value adjusting employing 0.1～0.5 mol of described generation.
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| CN2008100706813A CN101234782B (en) | 2008-02-29 | 2008-02-29 | Method for preparing high pure macroparticle anatase type titanium dioxide |
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| CN103230787A (en) * | 2013-04-18 | 2013-08-07 | 中国科学院长春光学精密机械与物理研究所 | Preparation method of {001} surface-exposed anatase-phase titanium dioxide microsphere photocatalyst |
| CN103754930B (en) * | 2014-01-07 | 2015-07-22 | 福建师范大学 | Octahedron anatase TiO2 orderly superstructure as well as preparation and application thereof |
| JP6943178B2 (en) * | 2017-12-28 | 2021-09-29 | 住友大阪セメント株式会社 | Titanium oxide powder, and dispersions and cosmetics using it |
| JPWO2019131871A1 (en) * | 2017-12-28 | 2020-12-24 | 住友大阪セメント株式会社 | Titanium oxide powder, and dispersions and cosmetics using it |
| JP6988471B2 (en) * | 2017-12-28 | 2022-01-05 | 住友大阪セメント株式会社 | Titanium oxide powder, and dispersions and cosmetics using it |
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