CN109534393A - A kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture - Google Patents
A kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture Download PDFInfo
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- CN109534393A CN109534393A CN201811461148.XA CN201811461148A CN109534393A CN 109534393 A CN109534393 A CN 109534393A CN 201811461148 A CN201811461148 A CN 201811461148A CN 109534393 A CN109534393 A CN 109534393A
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses a kind of preparation methods of the octahedrite nano titanium dioxide powder of witch culture, comprising the following steps: concentrated sulfuric acid solution is added in distilled water and is diluted, dilution heat of sulfuric acid is obtained；Dilution heat of sulfuric acid and titanium source are sequentially added into reaction vessel, is stirred, and oxygen metatitanic acid is synthesized；Tungsten source is added into reaction vessel, stirs later, is uniformly mixed reactant；It is designated value that ammonium hydroxide is added into reaction vessel and adjusts reactant pH value；Distilled water is added in the product, is centrifuged, gives up supernatant, precipitated；Sediment is put into Muffle furnace to calcine, the octahedrite nano titanium dioxide powder of the witch culture of smaller nanoscale can be obtained.The used raw material of the present invention is general chemical, and for preparation process without adding surfactant, the solution of generation is easy to handle and pollution-free, operating procedure is simple, preparation cost is low, the time is short, and repeatability is high, can be quickly obtained the octahedrite nano titanium dioxide powder of witch culture.
Description
Technical field
The present invention relates to nano material technology more particularly to a kind of octahedrite nano titanium dioxide powders of witch culture
Preparation method.
Background technique
Nano-titanium dioxide is because of its Strong oxdiative ability under ultraviolet light, high chemical stability, low cost and environmental-friendly
Etc. characteristics and be widely studied, it is considered to be most promising environment-friendly type catalyst.Since titanium dioxide is through ultraviolet lighting
The carrier generated after penetrating is easy compound, reduces the efficiency of its photocatalytic degradation of organic matter, the biggish taboo domain of titanium dioxide
Broadband seriously restricts its application, and the quick of the electron-hole of titanium dioxide compound also results in its low quantum yield
Weaker photocatalysis efficiency.To improve its photocatalytic activity, in recent years, researcher uses semiconductors coupling, metal or non-gold
Belong to ion doping, the methods of noble metal loading, by changing crystal form, grain size, the crystallinity etc. of titanium dioxide, so that photoproduction
Electronics and the compound of hole are extended.But using tungsten to carry out as Doped ions at present, compound report is less, and prepare
Titanium dioxide powder nanoscale is larger, and production method has production technology complexity, high production cost, pollution in various degree
The problems such as environment and not high repeatability.
Summary of the invention
(1) technical problems to be solved
The purpose of the present invention is to provide a kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture, with
The titanium dioxide powder nanoscale for solving existing preparation method preparation is larger, and production technology is complicated, high production cost, pollutes ring
The problems such as border and not high repeatability.
(2) technical solution
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture, using high-temperature calcination, including with
Lower step:
Step 1: concentrated sulfuric acid solution being added in distilled water and is diluted, and obtains dilution heat of sulfuric acid；
Step 2: sequentially adding dilution heat of sulfuric acid and titanium source into reaction vessel, is stirred, and synthesizes oxygen metatitanic acid；
Step 3: tungsten source being added into reaction vessel, stirs later, is uniformly mixed reactant；
Step 4: ammonium hydroxide being added into reaction vessel, stirring, adjusts reactant pH value to designated value；
Step 5: being added distilled water in the product, and centrifugation is given up supernatant, precipitated；
Step 6: sediment is put into Muffle furnace calcining, obtains the anatase-type nanometer titanium dioxide of witch culture of the present invention
Powder.
Feature of the present invention also resides in:
In step 1, when diluting concentrated sulfuric acid solution, under stirring, concentrated sulfuric acid solution is slowly added into steaming along wall
In distilled water, the dilution heat of sulfuric acid concentration configured is 5mol/L.
In step 2, the titanium source is TiCl4, the TiCl that is added4It is 1 with the dilution heat of sulfuric acid mass ratio being added:
2, and the TiCl4It is to be added under magnetic stirrer state.
In step 3, the tungsten source is ammonium tungstate ((NH4)6H2W12O40), tungsten source and titanium source mass ratio are 1:3~9.
The mass ratio of the tungsten source and titanium source is 1:9.
In step 4, ammonium hydroxide is added by reactant pH value adjustment to 7, mixing time 1h.
In step 5, distilled water centrifugation is added, centrifugal rotational speed 10000r/min, centrifugation time 3min are centrifuged number
It is 3 times.
In step 6, the calcination process is: Muffle furnace being warming up to 750 DEG C, keeps the temperature calcination 4 hours.
(3) beneficial effect
The present invention is with the nonmetallic compound TiCl of Ti4For presoma, ammonium tungstate ((NH4)6H2W12O40) be W donor, ammonia
Water is precipitating reagent and acid-base modifier, TiCl4Synthesis oxygen metatitanic acid is reacted with dilution heat of sulfuric acid, ammonium tungstate is reacted with oxygen metatitanic acid, is led to
Overregulate then octahedrite nano titanium dioxide powder that pH value generates witch culture at high temperature, the titanium dioxide powder of preparation
Nanoscale is smaller, is 220 rans.The raw materials used present invention is general chemical, preparation process is without adding surface
The solution of activating agent, generation is easy to handle and pollution-free, and operating procedure is simple, and preparation cost is low, the time is short, and repeatability is high, can be fast
Speed obtains the octahedrite nano titanium dioxide powder of witch culture.
Detailed description of the invention
Fig. 1 is the XRD diagram of product prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM figure of product prepared by the embodiment of the present invention 1.
Fig. 3 is the EDS figure of product prepared by the embodiment of the present invention 1.
Fig. 4 is the TEM figure of product prepared by the embodiment of the present invention 1.
Fig. 5 is the XRD diagram of product prepared by the embodiment of the present invention 2.
Fig. 6 is the XRD diagram of product prepared by the embodiment of the present invention 3.
Specific embodiment
Embodiment 1
The preparation method of the octahedrite nano titanium dioxide powder of witch culture of the present invention, using high-temperature calcination, specifically
Preparation step is as follows:
Under stirring, concentrated sulfuric acid solution is slowly added into distilled water along wall and is diluted, obtaining concentration is
The dilution heat of sulfuric acid of 5mol/L；
108 ㎏ of dilution heat of sulfuric acid for taking above-mentioned concentration, according to TiCl4TiCl is taken with dilution heat of sulfuric acid quality proportioning 1:2454
㎏, according to ammonium tungstate ((NH4)6H2W12O40) and TiCl46 ㎏ of ammonium tungstate is taken with quality proportioning 1:9, it is spare；
The dilution heat of sulfuric acid and TiCl of above-mentioned quality are sequentially added into reaction vessel4, it is stirred, obtains oxygen metatitanic acid,
TiCl4It is to be slowly added under magnetic stirrer state；
The ammonium tungstate of above-mentioned quality is added into reaction vessel, stir, make reactant be uniformly mixed, backward reaction vessel
Middle addition ammonium hydroxide stirs 1h, is 7 by the pH value adjustment of reaction system, distilled water is added in adjusting the reaction product after pH value
It is centrifuged, centrifugal rotational speed 10000r/min, centrifugation time 3min, centrifugation number is 3 times, gives up supernatant, is sunk
It forms sediment；
Sediment after centrifugation is put into Muffle furnace, muffle furnace is promoted to 750 DEG C, keeps the temperature calcination 4 hours,
Then cooled to room temperature obtains the octahedrite nano titanium dioxide powder of the witch culture of white.
Fig. 1 is the XRD spectrum of this example product, and free from admixture peak occurs, and illustrates that product is pure phase.
Fig. 2 is the SEM pattern photo of this example product, it can be seen that product is in granular form reunion.
Fig. 3 is the EDS map of this example product, illustrates there is element W, Ti, O, C, Pt in product.
Fig. 4 is the TEM map of this example product, it can be seen that product is nanoscale.
Embodiment 2
This embodiment differs from embodiment 1 in that ammonium tungstate and TiCl4It is matched according to the quality of 1:3, to anti-
Answer the dilution heat of sulfuric acid being added in container, TiCl4With ammonium tungstate ((NH4)6H2W12O40) be respectively 36 ㎏, 18 ㎏, 6 ㎏, remaining with
Embodiment 1 is identical.
Fig. 5 is the XRD spectrum that this example prepares product, and display product is pure phase.
Embodiment 3
The difference of the present embodiment and Examples 1 and 2 is the ammonium tungstate and TiCl being added in reaction vessel4Quality proportioning is 1:
6, dilution heat of sulfuric acid, TiCl4With ammonium tungstate ((NH4)6H2W12O40) additional amount is respectively 72 ㎏, 36 ㎏, 6 ㎏
Fig. 6 is the XRD spectrum of this example product, and free from admixture peak occurs, and is pure phase product.
The above described is only a preferred embodiment of the present invention, being not the limitation for doing other forms to the present invention, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But without departing from the technical solutions of the present invention, according to the technical essence of the invention to above embodiments institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection scope of technical solution of the present invention.
Claims (8)
1. a kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture, which comprises the following steps:
Step 1: concentrated sulfuric acid solution being added in distilled water and is diluted, and obtains dilution heat of sulfuric acid；
Step 2: sequentially adding dilution heat of sulfuric acid and titanium source into reaction vessel, is stirred, and synthesizes oxygen metatitanic acid；
Step 3: tungsten source being added into reaction vessel, stirs later, is uniformly mixed reactant；
Step 4: ammonium hydroxide being added into reaction vessel, stirring, adjusts reactant pH value to designated value；
Step 5: being added distilled water in the product, and centrifugation is given up supernatant, precipitated；
Step 6: sediment is put into Muffle furnace calcining, obtains the octahedrite nano titanium dioxide powder of witch culture of the present invention.
2. a kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture according to claim 1, special
Sign is, in step 1, when diluting concentrated sulfuric acid solution, under stirring, concentrated sulfuric acid solution is slowly added into steaming along wall
In distilled water, the dilution heat of sulfuric acid concentration configured is 5mol/L.
3. a kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture according to claim 1, special
Sign is, in step 2, the titanium source is TiCl4, the TiCl that is added4It is 1 with the dilution heat of sulfuric acid mass ratio being added:
2, and the TiCl4It is to be added under magnetic stirrer state.
4. a kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture according to claim 1, special
Sign is, in step 3, the tungsten source is ammonium tungstate ((NH4)6H2W12O40), tungsten source and titanium source mass ratio are 1:3~9.
5. a kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture according to claim 4, special
Sign is that tungsten source and titanium source mass ratio are 1:9.
6. a kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture according to claim 1, special
Sign is, in step 4, ammonium hydroxide is added by reactant pH value adjustment to 7, mixing time 1h.
7. a kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture according to claim 1, special
Sign is, in step 5, distilled water centrifugation, centrifugal rotational speed 10000r/min, centrifugation time 3min is added, centrifugation number is
3 times.
8. a kind of preparation method of the octahedrite nano titanium dioxide powder of witch culture according to claim 1, special
Sign is, in step 6, the calcination process is: Muffle furnace being warming up to 750 DEG C, keeps the temperature calcination 4 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437469A (en) * | 2014-11-18 | 2015-03-25 | 郭燏 | Nanometer titanium dioxide powder for flue gas deodorization/denitration catalyst and preparation method and application thereof |
| WO2017190277A1 (en) * | 2016-05-03 | 2017-11-09 | 广东风华高新科技股份有限公司 | Doped anatase titanium dioxide material, preparation method therefor and use thereof |
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- 2018-12-01 CN CN201811461148.XA patent/CN109534393A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437469A (en) * | 2014-11-18 | 2015-03-25 | 郭燏 | Nanometer titanium dioxide powder for flue gas deodorization/denitration catalyst and preparation method and application thereof |
| WO2017190277A1 (en) * | 2016-05-03 | 2017-11-09 | 广东风华高新科技股份有限公司 | Doped anatase titanium dioxide material, preparation method therefor and use thereof |
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Application publication date: 20190329 |