CN101062781A - Preparation method of rutile type titanium dioxide nano powder - Google Patents
Preparation method of rutile type titanium dioxide nano powder Download PDFInfo
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- CN101062781A CN101062781A CN 200610040215 CN200610040215A CN101062781A CN 101062781 A CN101062781 A CN 101062781A CN 200610040215 CN200610040215 CN 200610040215 CN 200610040215 A CN200610040215 A CN 200610040215A CN 101062781 A CN101062781 A CN 101062781A
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- 238000002360 preparation method Methods 0.000 title claims description 26
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract description 31
- 239000011858 nanopowder Substances 0.000 title abstract description 13
- 239000004408 titanium dioxide Substances 0.000 title abstract description 12
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 124
- 239000007864 aqueous solution Substances 0.000 claims abstract description 51
- 239000003292 glue Substances 0.000 claims abstract description 46
- 239000000243 solution Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 8
- 238000007865 diluting Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 32
- IDIJOAIHTRIPRC-UHFFFAOYSA-J hexaaluminum;sodium;2,2,4,4,6,6,8,8,10,10,12,12-dodecaoxido-1,3,5,7,9,11-hexaoxa-2,4,6,8,10,12-hexasilacyclododecane;iron(2+);triborate;tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Fe+2].[Fe+2].[Fe+2].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-][Si]1([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O1 IDIJOAIHTRIPRC-UHFFFAOYSA-J 0.000 claims description 22
- 229910000246 schorl Inorganic materials 0.000 claims description 22
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000004202 carbamide Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000010790 dilution Methods 0.000 claims description 14
- 239000012895 dilution Substances 0.000 claims description 14
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 14
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 7
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 7
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 7
- 239000001099 ammonium carbonate Substances 0.000 claims description 7
- 229920002401 polyacrylamide Polymers 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 4
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical compound CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 abstract 3
- 238000003756 stirring Methods 0.000 abstract 3
- 238000001914 filtration Methods 0.000 abstract 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000003381 stabilizer Substances 0.000 abstract 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
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- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
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Abstract
The invention discloses a method for preparing rutile type titanium dioxide nano powder. Firstly, adding titanium tetrachloride into water under stirring at 0-10 ℃ to obtain a titanium tetrachloride solution with the molar concentration of 0.1-0.5M, then stirring the titanium tetrachloride solution at 40-100 ℃ for 1.5-2.5 hours to obtain a titanium tetrachloride glue solution, then aging the glue solution for at least 1 day, filtering to obtain a titanium tetrachloride glue solution with the pH value of 1-3, then ultrasonically dispersing the titanium tetrachloride glue solution, and adding a stabilizer to obtain a titanium dioxide sol; firstly, respectively diluting titanium dioxide sol and water according to the volume ratio of 1: 1-5, preparing a titanium tetrachloride aqueous solution according to the mass ratio of titanium tetrachloride to water of 1: 3-15, and mixing the titanium dioxide sol and the water according to the volume ratio of 1: 4-10 to obtain a mixed solution; (c) firstly, stirring the mixed solution at 60-100 ℃ for 2-3 hours, and then filtering, precipitating and drying the mixed solution to obtain rutile type titanium dioxide nano powder. It has high yield and is suitable for industrial production.
Description
Technical field the present invention relates to a kind of method for making of titanium dioxide powder, especially the preparation method of red schorl type titanium oxide nano powder.
Background technology titanium dioxide is one of important metal oxide, can be widely used in industry such as plastics, papermaking, printing-ink, chemical fibre, rubber and makeup.Rise and Development of Preparation Technology along with nano material, the anomalous performance that nano titanium oxide is different from conventional powder body material makes the Application Areas of titanium dioxide that bigger expansion arranged, as can be used as support of the catalyst degradable organic pollutant under ultraviolet irradiation, conversion solar can be electric energy, gas sensor, pressure-active element, the enhancement additive of polymkeric substance, complex function ceramic material structure, nonlinear optical material or the like.At present, people have done some trials and effort in order to obtain it, as " a kind of preparation method of rutile phase titanium dioxide nano-powder " who discloses among the disclosed Chinese invention patent ublic specification of application CN 1631759A on June 29th, 2005.This preparation method becomes the water-sol with the titanium tetrachloride preparation of raw material, and the water-sol is thin up after overaging, heats to make sol-hydrolysis and produce precipitation again, the gained throw out is filtered, and water flushing after drying, and make rutile phase titanium dioxide nano-powder.But this preparation method has unsatisfactory part, and at first, the particle shape of the nano TiO 2 powder that makes is irregular; Secondly, operation is more, causes production process numerous and diverse, and the cost of preparation is increased; Once more, Ti in the entire reaction course
4+Concentration very low, make the productive rate of powder also very low, and only in the laboratory, realize certain distance still being arranged apart from suitability for industrialized production.
The summary of the invention the technical problem to be solved in the present invention provides a kind of powder regular shape of preparing, the preparation method of the red schorl type titanium oxide nano powder that technology is easy for overcoming weak point of the prior art.
The preparation method of red schorl type titanium oxide nano powder comprises liquid phase method, particularly it is finished according to the following steps: (a) earlier with in the water of titanium tetrachloride in 0～10 ℃ adding is stirred down, obtain the titanium tetrachloride solution that volumetric molar concentration is 0.1～0.5M, again it is stirred down in 40～100 ℃ and obtained the titanium tetrachloride glue in 1.5～2.5 hours, afterwards, earlier the ageing of titanium tetrachloride glue being filtered after 1 day at least and obtaining pH value is 1～3 titanium tetrachloride glue, this titanium tetrachloride glue of ultra-sonic dispersion again, and the adding stablizer gets TiO 2 sol, wherein, the add-on of stablizer is 1～10% (weight) of titanium tetrachloride glue; (b) be 1: 1～5 dilutions by volume with TiO 2 sol and water respectively earlier, and by titanium tetrachloride: the mass ratio of water is 1: 3～15 configuration titanium tetrachloride aqueous solutions, TiO 2 sol after will diluting again mixes mutually with the titanium tetrachloride aqueous solution of configuration and obtains mixing solutions, wherein, the volume ratio between the titanium tetrachloride aqueous solution of TiO 2 sol after the dilution and configuration is 1: 4～10; (c) earlier mixing solutions was stirred 2～3 hours down in 60～100 ℃, again it is filtered, precipitates and drying, make red schorl type titanium oxide nano powder.
As the preparation method's of red schorl type titanium oxide nano powder further improvement, described water is deionized water or distilled water; The frequency of ultrasonic of described ultra-sonic dispersion titanium tetrachloride glue is 10～60KHz; Described stablizer is ethanol or propyl alcohol or methyl ethyl diketone; Described PVP or HPC or PEG or the polyacrylamide of in the titanium tetrachloride aqueous solution of step (b) configuration, adding, and add urea or ammonium bicarbonate solution simultaneously, wherein, the add-on of PVP or HPC or PEG or polyacrylamide is 0.1～2% (weight) of the titanium tetrachloride aqueous solution of configuration, and the add-on of urea or ammonium bicarbonate solution is 0.5～10% (weight) of the titanium tetrachloride aqueous solution of configuration; Described exsiccant temperature is that 80～120 ℃, time are 5～8 hours.
Beneficial effect with respect to prior art is, one, repeatedly use transmission electron microscope, laser particle analyzer and x-ray diffractometer to carry out the sign of form, size-grade distribution, composition and structure respectively to the nano-powder that makes, from the transmission electron microscope photo, particle size distribution figure and the X-ray diffraction spectrogram that obtain as can be known, the class sphere that is shaped as rule of powder, and it is dispersed fine, its particle size distribution is very narrow, only between 20～50nm, crystalline structure is entirely the titanium dioxide of rutile-type; They are two years old, mix with titanium tetrachloride aqueous solution as inductor and prepare red schorl type titanium oxide nano powder by adding TiO 2 sol, both overcome the defective that TiO 2 sol is difficult to disposable a large amount of preparations, simplify technology again, also promoted the quality of finished product red schorl type titanium oxide nano powders; They are three years old, in the titanium tetrachloride aqueous solution of step (b) configuration, add PVP or HPC or PEG or polyacrylamide, and add urea or ammonium bicarbonate solution simultaneously,, also alleviated the reunion of titanium tetrachloride in hydrolytic process in the titanium tetrachloride aqueous solution of configuration except that making hydrolysis carries out rapidly; Its four, the method for preparation is easy, production efficiency height, cost are low, not only are suitable for industrialized scale operation, also are easy to business-like application.
Description of drawings is described in further detail optimal way of the present invention below in conjunction with accompanying drawing.
Fig. 1 observes the transmission electron microscope photo (TEM image) that the back is taken to the nano-powder that makes with the JEM-200CX type high resolution transmission electron microscope of Japan, can be seen the shape and the granularity of powder by this TEM image;
Fig. 2 is the particle size distribution figure that obtains after the nano-powder that will make is tested it with ZETESIZER 3000HSA type laser particle analyzer, and wherein, ordinate zou is a number percentage ratio, and X-coordinate is a diameter.This particle size distribution figure has demonstrated the distribution range of nano-powder granularity;
Fig. 3 tests the X-ray diffracting spectrum (XRD) that obtain with Philips X ' Pert type x-ray diffractometer to it to the nano-powder that makes, and wherein, ordinate zou is a relative intensity, and X-coordinate is a diffraction angle.Curve among this XRD (a) be original post precipitation again in 400 ℃ of following nano-powders of 2 hours of calcining, curve (b) be original post precipitation without the incinerating nano-powder, curve (c) is R-TiO
2The standard spectral line.By XRD as can be known, there is not essential distinction between curve (a) and the curve (b).
Embodiment is at first buied titanium tetrachloride from market, as deionized water, the distilled water of water, and PVP, HPC, PEG, polyacrylamide, urea and ammonium bicarbonate solution, and as ethanol, propyl alcohol, the methyl ethyl diketone of stablizer.
Embodiment 1: finish preparation according to the following steps: a) earlier with in the deionized water of titanium tetrachloride in 0 ℃ adding is stirred down, obtain the titanium tetrachloride solution that volumetric molar concentration is 0.1M, it is stirred down in 40 ℃ obtained the titanium tetrachloride glue in 2.5 hours again.Afterwards, the ageing of titanium tetrachloride glue being filtered after 1 day obtain pH value earlier is 1 titanium tetrachloride glue, this titanium tetrachloride glue of ultra-sonic dispersion again, and add stablizer and get TiO 2 sol; Wherein, the frequency of ultrasonic of ultra-sonic dispersion titanium tetrachloride glue is 10KHz, and the add-on of stablizer is 10% (weight) of titanium tetrachloride glue, and stablizer is selected ethanol for use.B) be dilution in 1: 1 by volume with TiO 2 sol and deionized water respectively earlier, and by titanium tetrachloride: the mass ratio of deionized water is 1: 15 configuration titanium tetrachloride aqueous solution, and the TiO 2 sol after will diluting again mixes mutually with the titanium tetrachloride aqueous solution of configuration and obtains mixing solutions; In the process of the titanium tetrachloride aqueous solution that allotment is disposed, in the titanium tetrachloride aqueous solution of configuration, add PVP and urea, wherein, the add-on of PVP is 0.1% (weight) of the titanium tetrachloride aqueous solution of configuration, the add-on of urea is 10% (weight) of the titanium tetrachloride aqueous solution of configuration, and the volume ratio between the TiO 2 sol after the dilution and the titanium tetrachloride aqueous solution of configuration is 1: 4; C) earlier mixing solutions was stirred 3 hours down in 60 ℃, again it is filtered, precipitates and dry, the exsiccant temperature is that 80 ℃, time are 8 hours, makes as Fig. 1 and the red schorl type titanium oxide nano powder shown in curve among Fig. 2, Fig. 3.
Embodiment 2: finish preparation according to the following steps: a) earlier with in the deionized waters of titanium tetrachloride in 2 ℃ adding is stirred down, obtain the titanium tetrachloride solution that volumetric molar concentration is 0.2M, it is stirred down in 55 ℃ obtained the titanium tetrachloride glue in 2.3 hours again.Afterwards, the ageing of titanium tetrachloride glue being filtered after 2 days obtain pH value earlier is 1.5 titanium tetrachloride glue, this titanium tetrachloride glue of ultra-sonic dispersion again, and add stablizer and get TiO 2 sol; Wherein, the frequency of ultrasonic of ultra-sonic dispersion titanium tetrachloride glue is 25KHz, and the add-on of stablizer is 8% (weight) of titanium tetrachloride glue, and stablizer is selected ethanol for use.B) be dilution in 1: 2 by volume with TiO 2 sol and deionized water respectively earlier, and by titanium tetrachloride: the mass ratio of deionized water is 1: 12 configuration titanium tetrachloride aqueous solution, and the TiO 2 sol after will diluting again mixes mutually with the titanium tetrachloride aqueous solution of configuration and obtains mixing solutions; In the process of the titanium tetrachloride aqueous solution that allotment is disposed, in the titanium tetrachloride aqueous solution of configuration, add PVP and urea, wherein, the add-on of PVP is 0.6% (weight) of the titanium tetrachloride aqueous solution of configuration, the add-on of urea is 8% (weight) of the titanium tetrachloride aqueous solution of configuration, and the volume ratio between the TiO 2 sol after the dilution and the titanium tetrachloride aqueous solution of configuration is 1: 5.5; C) earlier mixing solutions was stirred 2.8 hours down in 70 ℃, again it is filtered, precipitates and dry, the exsiccant temperature is that 90 ℃, time are 7 hours, makes as Fig. 1 and the red schorl type titanium oxide nano powder shown in curve among Fig. 2, Fig. 3.
Embodiment 3: finish preparation according to the following steps: a) earlier with in the deionized waters of titanium tetrachloride in 5 ℃ adding is stirred down, obtain the titanium tetrachloride solution that volumetric molar concentration is 0.3M, it is stirred down in 70 ℃ obtained the titanium tetrachloride glue in 2 hours again.Afterwards, the ageing of titanium tetrachloride glue being filtered after 3 days obtain pH value earlier is 2 titanium tetrachloride glue, this titanium tetrachloride glue of ultra-sonic dispersion again, and add stablizer and get TiO 2 sol; Wherein, the frequency of ultrasonic of ultra-sonic dispersion titanium tetrachloride glue is 35KHz, and the add-on of stablizer is 6% (weight) of titanium tetrachloride glue, and stablizer is selected ethanol for use.B) be dilution in 1: 3 by volume with TiO 2 sol and deionized water respectively earlier, and by titanium tetrachloride: the mass ratio of deionized water is 1: 9 configuration titanium tetrachloride aqueous solution, and the TiO 2 sol after will diluting again mixes mutually with the titanium tetrachloride aqueous solution of configuration and obtains mixing solutions; In the process of the titanium tetrachloride aqueous solution that allotment is disposed, in the titanium tetrachloride aqueous solution of configuration, add PVP and urea, wherein, the add-on of PVP is 1% (weight) of the titanium tetrachloride aqueous solution of configuration, the add-on of urea is 6% (weight) of the titanium tetrachloride aqueous solution of configuration, and the volume ratio between the TiO 2 sol after the dilution and the titanium tetrachloride aqueous solution of configuration is 1: 7; C) earlier mixing solutions was stirred 2.5 hours down in 80 ℃, again it is filtered, precipitates and dry, the exsiccant temperature is that 100 ℃, time are 6.5 hours, makes as Fig. 1 and the red schorl type titanium oxide nano powder shown in curve among Fig. 2, Fig. 3.
Embodiment 4: finish preparation according to the following steps: a) earlier with in the deionized waters of titanium tetrachloride in 8 ℃ adding is stirred down, obtain the titanium tetrachloride solution that volumetric molar concentration is 0.4M, it is stirred down in 85 ℃ obtained the titanium tetrachloride glue in 1.8 hours again.Afterwards, the ageing of titanium tetrachloride glue being filtered after 4 days obtain pH value earlier is 2.5 titanium tetrachloride glue, this titanium tetrachloride glue of ultra-sonic dispersion again, and add stablizer and get TiO 2 sol; Wherein, the frequency of ultrasonic of ultra-sonic dispersion titanium tetrachloride glue is 50KHz, and the add-on of stablizer is 3% (weight) of titanium tetrachloride glue, and stablizer is selected ethanol for use.B) be dilution in 1: 4 by volume with TiO 2 sol and deionized water respectively earlier, and by titanium tetrachloride: the mass ratio of deionized water is 1: 6 configuration titanium tetrachloride aqueous solution, and the TiO 2 sol after will diluting again mixes mutually with the titanium tetrachloride aqueous solution of configuration and obtains mixing solutions; In the process of the titanium tetrachloride aqueous solution that allotment is disposed, in the titanium tetrachloride aqueous solution of configuration, add PVP and urea, wherein, the add-on of PVP is 1.5% (weight) of the titanium tetrachloride aqueous solution of configuration, the add-on of urea is 3% (weight) of the titanium tetrachloride aqueous solution of configuration, and the volume ratio between the TiO 2 sol after the dilution and the titanium tetrachloride aqueous solution of configuration is 1: 8.5; C) earlier mixing solutions was stirred 2.3 hours down in 90 ℃, again it is filtered, precipitates and dry, the exsiccant temperature is that 110 ℃, time are 5.5 hours, makes as Fig. 1 and the red schorl type titanium oxide nano powder shown in curve among Fig. 2, Fig. 3.
Embodiment 5: finish preparation according to the following steps: a) earlier with in the deionized waters of titanium tetrachloride in 10 ℃ adding is stirred down, obtain the titanium tetrachloride solution that volumetric molar concentration is 0.5M, it is stirred down in 100 ℃ obtained the titanium tetrachloride glue in 1.5 hours again.Afterwards, the ageing of titanium tetrachloride glue being filtered after 5 days obtain pH value earlier is 3 titanium tetrachloride glue, this titanium tetrachloride glue of ultra-sonic dispersion again, and add stablizer and get TiO 2 sol; Wherein, the frequency of ultrasonic of ultra-sonic dispersion titanium tetrachloride glue is 60KHz, and the add-on of stablizer is 1% (weight) of titanium tetrachloride glue, and stablizer is selected ethanol for use.B) be dilution in 1: 5 by volume with TiO 2 sol and deionized water respectively earlier, and by titanium tetrachloride: the mass ratio of deionized water is 1: 3 configuration titanium tetrachloride aqueous solution, and the TiO 2 sol after will diluting again mixes mutually with the titanium tetrachloride aqueous solution of configuration and obtains mixing solutions; In the process of the titanium tetrachloride aqueous solution that allotment is disposed, in the titanium tetrachloride aqueous solution of configuration, add PVP and urea, wherein, the add-on of PVP is 2% (weight) of the titanium tetrachloride aqueous solution of configuration, the add-on of urea is 0.5% (weight) of the titanium tetrachloride aqueous solution of configuration, and the volume ratio between the TiO 2 sol after the dilution and the titanium tetrachloride aqueous solution of configuration is 1: 10; C) earlier mixing solutions was stirred 2 hours down in 100 ℃, again it is filtered, precipitates and dry, the exsiccant temperature is that 120 ℃, time are 5 hours, makes as Fig. 1 and the red schorl type titanium oxide nano powder shown in curve among Fig. 2, Fig. 3.
Select distilled water more respectively for use as water, HPC or PEG or polyacrylamide or ammonium bicarbonate solution, and, repeat the foregoing description 1～5 as the propyl alcohol or the methyl ethyl diketone of stablizer, make equally as Fig. 1 and the red schorl type titanium oxide nano powder shown in curve among Fig. 2, Fig. 3.
Obviously, those skilled in the art can carry out various changes and modification to the preparation method of red schorl type titanium oxide nano powder of the present invention and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (6)
1, a kind of preparation method of red schorl type titanium oxide nano powder comprises liquid phase method, it is characterized in that finishing according to the following steps:
(a) earlier with in the water of titanium tetrachloride in 0～10 ℃ adding is stirred down, obtain the titanium tetrachloride solution that volumetric molar concentration is 0.1～0.5M, again it is stirred down in 40～100 ℃ and obtained the titanium tetrachloride glue in 1.5～2.5 hours, afterwards, earlier the ageing of titanium tetrachloride glue being filtered after 1 day at least and obtaining pH value is 1～3 titanium tetrachloride glue, this titanium tetrachloride glue of ultra-sonic dispersion again, and the adding stablizer gets TiO 2 sol, wherein, the add-on of stablizer is 1～10% (weight) of titanium tetrachloride glue;
(b) be 1: 1～5 dilutions by volume with TiO 2 sol and water respectively earlier, and by titanium tetrachloride: the mass ratio of water is 1: 3～15 configuration titanium tetrachloride aqueous solutions, TiO 2 sol after will diluting again mixes mutually with the titanium tetrachloride aqueous solution of configuration and obtains mixing solutions, wherein, the volume ratio between the titanium tetrachloride aqueous solution of TiO 2 sol after the dilution and configuration is 1: 4～10;
(c) earlier mixing solutions was stirred 2～3 hours down in 60～100 ℃, again it is filtered, precipitates and drying, make red schorl type titanium oxide nano powder.
2, the preparation method of red schorl type titanium oxide nano powder according to claim 1 is characterized in that water is deionized water or distilled water.
3, the preparation method of red schorl type titanium oxide nano powder according to claim 1, the frequency of ultrasonic that it is characterized in that ultra-sonic dispersion titanium tetrachloride glue is 10～60KHz.
4, the preparation method of red schorl type titanium oxide nano powder according to claim 1 is characterized in that stablizer is ethanol or propyl alcohol or methyl ethyl diketone.
5, the preparation method of red schorl type titanium oxide nano powder according to claim 1, it is characterized in that in the titanium tetrachloride aqueous solution of step (b) configuration, adding PVP or HPC or PEG or polyacrylamide, and add urea or ammonium bicarbonate solution simultaneously, wherein, the add-on of PVP or HPC or PEG or polyacrylamide is 0.1～2% (weight) of the titanium tetrachloride aqueous solution of configuration, and the add-on of urea or ammonium bicarbonate solution is 0.5～10% (weight) of the titanium tetrachloride aqueous solution of configuration.
6, the preparation method of red schorl type titanium oxide nano powder according to claim 1 is characterized in that the exsiccant temperature is that 80～120 ℃, time are 5～8 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105712398A (en) * | 2016-05-10 | 2016-06-29 | 湖北天瓷电子材料有限公司 | Method for preparing adjustable-particle-size adjustable-specific-area titanium dioxide by direct heating |
| CN105967230A (en) * | 2016-05-10 | 2016-09-28 | 湖北天瓷电子材料有限公司 | Provides method for preparing ultrafine titanium dioxide by using two-component dispersant |
| CN109704399A (en) * | 2019-02-20 | 2019-05-03 | 山东国瓷功能材料股份有限公司 | A kind of high dispersing rutile type titanium dioxide and preparation method thereof |
| CN114853056A (en) * | 2022-04-25 | 2022-08-05 | 武汉工程大学 | Preparation method of nano-scale titanium dioxide with controllable particle size |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1277749C (en) * | 2004-11-16 | 2006-10-04 | 浙江工业大学 | Process for preparing rutile phase titanium dioxide nano-powder |
| CN100335416C (en) * | 2005-04-18 | 2007-09-05 | 江苏大学 | Method for preparing rutile type nanometer Ti02 in low temperature using carboxylic acid as finishing agent |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105712398A (en) * | 2016-05-10 | 2016-06-29 | 湖北天瓷电子材料有限公司 | Method for preparing adjustable-particle-size adjustable-specific-area titanium dioxide by direct heating |
| CN105967230A (en) * | 2016-05-10 | 2016-09-28 | 湖北天瓷电子材料有限公司 | Provides method for preparing ultrafine titanium dioxide by using two-component dispersant |
| CN105967230B (en) * | 2016-05-10 | 2017-05-03 | 湖北天瓷电子材料有限公司 | Provides method for preparing ultrafine titanium dioxide by using two-component dispersant |
| CN109704399A (en) * | 2019-02-20 | 2019-05-03 | 山东国瓷功能材料股份有限公司 | A kind of high dispersing rutile type titanium dioxide and preparation method thereof |
| CN114853056A (en) * | 2022-04-25 | 2022-08-05 | 武汉工程大学 | Preparation method of nano-scale titanium dioxide with controllable particle size |
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