CN103964497B - A kind of method preparing ultra-fine sub-titanium dioxide powder - Google Patents
A kind of method preparing ultra-fine sub-titanium dioxide powder Download PDFInfo
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- CN103964497B CN103964497B CN201410230218.6A CN201410230218A CN103964497B CN 103964497 B CN103964497 B CN 103964497B CN 201410230218 A CN201410230218 A CN 201410230218A CN 103964497 B CN103964497 B CN 103964497B
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Abstract
The present invention relates to a kind of method preparing ultra-fine sub-titanium dioxide powder, its step is as follows: A, proportionally take titanium dioxide powder and titanium hydride powder; B, drop in oversaturated KCl and the NaCl aqueous solution and carry out dispersed with stirring respectively; C, above-mentioned mixed solution is filtered respectively, dry; D, titanium hydride powders coated for KCl and NaCl is carried out high-temperature dehydrogenation process, then coated with KCl and NaCl titania powder, and the full and uniform mixing of KCl and NaCl powder; E, mixed uniformly powder to be heated under vacuum, then furnace cooling; F, carry out washing obtain ultra-fine sub-titanium dioxide powder; The invention solves the problem that purification ultrafine titanium powder is difficult to prepare, add purity and the dispersiveness of titanium valve simultaneously, improve production efficiency, powder size controllability is good.
Description
Technical field
The present invention relates to a kind of preparation method of ultra-fine sub-titanium dioxide powder.
Background technology
There is TinO
2the sub-titanium oxide of n-1 chemical general formula has unique physics, chemistry and chemical property, and comprise excellent electroconductibility, its electric conductivity 1500S/cm, far above graphite; Extremely strong chemical stability, strong alkali-acid resistance; Wide electrochemical stability potential window, stablize allusion quotation Wei window in the aqueous solution at more than 3.0V, this makes it at various chemical power source, comprises lead storage battery, flow battery, fuel cell field have broad application prospects.Wherein Ti
4o
7, Ti
5o
9conductivity best, be the ideal material of additives for battery.
Sub-titanium oxide is the titanium dioxide having oxygen defect, and existing preparation method is mainly by heating TiO under an inert atmosphere
2obtain with metal titanium, also can at high temperature use reductive agent as the reduction such as hydrogen, carbon TiO
2obtained.In production process, sub-titanium oxide is very easily subject to the impact of reaction conditions, is difficult to accurately control, and the sub-titanium oxide product quality therefore adopting aforesaid method to produce is not high.The application of sub-titanium oxide in battery material mainly adds positive and negative electrode in powder form and promotes positive and negative electrode performance.Prepare in scheme at existing sub-titanium dioxide powder, raw material powder easily occurs to reunite under being in direct contact with high temperature and granularity is not controlled, and reactant composition, reductive agent dispersiveness in the feed had a negative impact to reaction times and reaction homogeneity.
Summary of the invention
In order to avoid the deficiencies in the prior art part, the present invention proposes the titania powder of specific morphology and a certain amount of titanium valve to react in the salt of molten state to generate sub-titanium oxide, through the sub-titanium dioxide powder washed, drying and other steps obtains pattern and particle diameter is controlled.
The present invention is achieved by the following technical programs:
Prepare a method for ultra-fine sub-titanium dioxide powder, its step is as follows:
A, take titania powder and titanium hydride powders respectively, take the quality of titania powder and titanium hydride powders according to TiO
2+ TiH
2→ xTi
4o
7+ yTi
5o
9(x+y=1) reflect that equation calculates;
B, the above-mentioned titania powder that takes and titanium hydride powders to be dropped in oversaturated KCl and the NaCl aqueous solution respectively, stir, titania powder and titanium hydride powders are fully disperseed in the solution;
C, above-mentioned mixed solution to be filtered respectively, dry, obtain the coated titania powder of KCl and NaCl and titanium hydride powders;
D, titanium hydride powders coated for KCl and NaCl is carried out high-temperature dehydrogenation process, then coated with KCl and NaCl titania powder, and the full and uniform mixing of KCl and NaCl powder, wherein: the gross weight of the coated titanium hydride powders of KCl and NaCl and titania powder and the gross weight of KCl and NaCl powder are than being 1:9 ~ 11;
E, mixed uniformly powder to be heated under vacuum, and fully stir, then furnace cooling;
F, cooled mixture carried out washing and obtain ultra-fine sub-titanium dioxide powder.
Further, the mixed solution in described step C adopts the filter paper filtering of 3 ~ 5um, carries out drying after filtration in 90 ~ 110 DEG C of high temperature air atmosphere.
Further, in described step D, high-temperature dehydrogenation process is carried out under 600 ~ 800 DEG C of elevated temperature in vacuo, and the high-temperature dehydrogenation treatment time controlled at 2 ~ 4 hours.
Further, the mixed powder in described step e is placed in vacuum apparatus to be heated to 900 ~ 1100 DEG C, is incubated 4 ~ 10 hours, then furnace cooling.
Beneficial effect of the present invention is as follows: (1) directly uses after ultra-fine titanium hydride powders coated for KCl and NaCl is carried out dehydrogenation, namely solves the problem that purification ultrafine titanium powder is difficult to prepare, also can increase purity and the dispersiveness of titanium valve simultaneously; (2) promote that titanium and titanium dioxide react by the salt of molten state, improve production efficiency; (3) raw material powder under molten state does not contact each other, and powder size is controlled.
Embodiment
The present invention will be described in detail further below.
Prepare a method for ultra-fine sub-titanium dioxide powder, its step is as follows:
A, according to TiO
2+ TiH
2→ xTi
4o
7+ yTi
5o
9(x+y=1) reflect that equation calculates, electronic balance takes titania powder and titanium hydride powders respectively, makes the mass ratio of taken titanium dioxide powder and titanium hydride powders be 39:5, powder size requires as 1-10 μm;
B, the above-mentioned titania powder that takes and titanium hydride powders to be dropped in oversaturated KCl and the NaCl aqueous solution respectively, stir 10 minutes with stirrer, obtain the suspension of KCl and the NaCl aqueous solution containing titania powder and titanium hydride powders respectively;
C, above-mentioned mixed solution is adopted the filter paper filtering of 3 ~ 5um, in thermostatic drying chamber, carry out drying in 100 DEG C of air atmosphere after filtration, obtain the coated titania powder of KCl and NaCl and titanium hydride powders respectively;
D, by titanium hydride powders coated for KCl and NaCl in 700 DEG C of vacuum high temperature furnaces 1.0 × 10
-3dehydroepiandrosterone derivative 3 hours under Pa vacuum condition, then coated with KCl and NaCl titania powder, and the full and uniform mixing in V-type mixer of KCl and NaCl powder, wherein: the gross weight of the coated titanium hydride powders of KCl and NaCl and titania powder and the gross weight of KCl and NaCl powder are than being 1:10;
E, mixed uniformly powder loaded in heat-resistance stainless steel crucible, in vacuum furnace, be heated to 900 ~ 1100 DEG C of insulations 8 hours, vacuum DEG C controls 1.0 × 10
-2pa, and fully stir, then furnace cooling;
F, cooled mixture carried out washing and obtain ultra-fine sub-titanium dioxide powder, wherein containing 40%Ti
4o
7and 60%Ti
5o
9.
The problem solving purification ultrafine titanium powder and be difficult to prepare of the present invention, adds purity and the dispersiveness of titanium valve, promotes that titanium and titanium dioxide react, improve production efficiency by the salt of molten state; Raw material powder under molten state does not contact each other, and powder size is controlled.
Claims (3)
1. prepare a method for ultra-fine sub-titanium dioxide powder, it is characterized in that: comprise step as follows:
A, take titania powder and titanium hydride powders respectively, take titania powder and titanium hydride powders mass ratio be 39:5;
B, the above-mentioned titania powder that takes and titanium hydride powders to be dropped in oversaturated KCl and the NaCl aqueous solution respectively, stir, titania powder and titanium hydride powders are fully disperseed in the solution;
C, above-mentioned mixed solution to be filtered respectively, dry, obtain the coated titania powder of KCl and NaCl and titanium hydride powders;
D, titanium hydride powders coated for KCl and NaCl is carried out high-temperature dehydrogenation process, then coated with KCl and NaCl titania powder, and the full and uniform mixing of KCl and NaCl powder, wherein: the gross weight of the titania powder that KCl and NaCl is coated and titanium hydride powders and the gross weight of KCl and NaCl powder are than being 1:9 ~ 11;
E, mixed uniformly powder to be heated under vacuum, and fully stir, then furnace cooling;
F, cooled mixture carried out washing and obtain ultra-fine sub-titanium dioxide powder;
Mixed powder in described step e is placed in vacuum apparatus to be heated to 900 ~ 1100 DEG C, is incubated 4 ~ 10 hours, then furnace cooling.
2. a kind of method preparing ultra-fine sub-titanium dioxide powder according to claim 1, is characterized in that: the mixed solution in described step C adopts the filter paper filtering of 3 ~ 5 microns, carries out drying after filtration in 90 ~ 110 DEG C of high temperature air atmosphere.
3. a kind of method preparing ultra-fine sub-titanium dioxide powder according to claim 1, is characterized in that: in described step D, high-temperature dehydrogenation process is carried out under 600 ~ 800 DEG C of elevated temperature in vacuo, and the high-temperature dehydrogenation treatment time controlled at 2 ~ 4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410230218.6A CN103964497B (en) | 2014-05-28 | 2014-05-28 | A kind of method preparing ultra-fine sub-titanium dioxide powder |
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|---|---|---|---|
| CN201410230218.6A CN103964497B (en) | 2014-05-28 | 2014-05-28 | A kind of method preparing ultra-fine sub-titanium dioxide powder |
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| CN103964497B true CN103964497B (en) | 2016-03-23 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912972B (en) * | 2010-08-05 | 2011-12-28 | 成都韵智科技有限公司 | Preparation method of superfine Ti powders |
| CN103274456B (en) * | 2013-06-05 | 2016-01-20 | 四川大学 | Doped Ti 4o 7powder and preparation method thereof |
| CN103787409B (en) * | 2014-01-10 | 2016-03-23 | 四川大学 | Ti 3o 5raw powder's production technology |
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