CN110294493A - A kind of preparation method of nano flower-like structure monocline phase titanic oxide - Google Patents
A kind of preparation method of nano flower-like structure monocline phase titanic oxide Download PDFInfo
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- CN110294493A CN110294493A CN201910658903.1A CN201910658903A CN110294493A CN 110294493 A CN110294493 A CN 110294493A CN 201910658903 A CN201910658903 A CN 201910658903A CN 110294493 A CN110294493 A CN 110294493A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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Abstract
The invention discloses a kind of preparation methods of nano flower-like structure monocline phase titanic oxide, and titanium trichloride dilute hydrochloric acid solution is dissolved in ethylene glycol, and uniformly mixes；Mixture solution is poured into the autoclave with polytetrafluoroethyllining lining；Reaction kettle is put into batch-type furnace, heats and keeps the temperature a period of time, be then cooled to room temperature taking-up；By the solution after reaction, successively with deionized water and dehydrated alcohol wash respectively three times, centrifuge separation, remove impurity；It by gains drying after above-mentioned washing and grinds, obtains nano flower-like structure monoclinic phase titania powder.The beneficial effects of the invention are as follows monoclinic phase dispersability of titanium dioxide obtained by the present invention is good, morphological rules is technical process safety, simple.
Description
Technical field
The invention belongs to solvent-thermally synthesizing nano material technology technical fields, are related to solvent-thermally synthesizing nano flower-like structure list
The preparation method of monoclinic phase titanium dioxide.
Background technique
Titanium dioxide is a kind of nontoxic, harmless and from a wealth of sources catalysis material[2], with other semiconductor catalysis materials
(cadmium sulfide, tin oxide, zinc oxide, zinc sulphide etc.) is compared, and photochemical properties are more stable, have higher catalytic efficiency and
Strong oxdiative ability.
1980, the monocline phase titanic oxide of block particle shape was prepared by high-temperature sintering process by Marchand et al.,
1998, Kasuga et al. synthesized the monocline phase titanic oxide of nanostructure by hydro-thermal method for the first time.Currently, researcher is
The structures such as monoclinic phase titanium dioxide nano thread, nanoparticle, nanometer sheet and nanobelt are prepared, it is different by analysis and summary
The monocline phase titanic oxide of pattern has different performance and application field.So exploring the nanometer shape of monoclinic phase titanium dioxide
Looks are of great significance.
Summary of the invention
It is of the invention the purpose of the present invention is to provide a kind of preparation method of nano flower-like structure monocline phase titanic oxide
Beneficial effect is that monoclinic phase dispersability of titanium dioxide obtained by the present invention is good, morphological rules, and technical process is safe, simple, and process is auxiliary
Hydrotropy liquid and product are easy to handle, therefore this method has boundless application prospect.
The technical scheme adopted by the invention is that following the steps below:
1. titanium trichloride dilute hydrochloric acid solution is dissolved in ethylene glycol, and uniformly mix；
2. pouring into mixture solution in the autoclave with polytetrafluoroethyllining lining；
3. reaction kettle is put into batch-type furnace, a period of time is heated and kept the temperature, taking-up is then cooled to room temperature；
4. by the solution after reaction, successively with deionized water and dehydrated alcohol wash respectively three times, centrifuge separation, go to clean
Matter；
5. by gains drying after above-mentioned washing and grinding, nano flower-like structure monoclinic phase titania powder is obtained.
Further, 1. 3~5ml, 15% titanium trichloride dilute hydrochloric acid solution is dissolved in 30~40ml ethylene glycol by step, and
Even mixing stirs 3~11h using magnetic force thermostatic mixer, is allowed to sufficiently dissolve.
Further, 3. reaction kettle is put into batch-type furnace by step, is heated to 130~160 DEG C, 4~7h of soaking time, then
It is cooled to room temperature taking-up.
Further, step is 4. by the solution after reaction, successively with deionized water and dehydrated alcohol wash respectively three times, centrifugation
Separation removes impurity.
Further, 5. step is dried using vacuum drying oven, is dried at 50~80 DEG C, and grinding vessel grind for agate
Alms bowl.
Detailed description of the invention
11h is stirred in Fig. 1 embodiment 3, heating temperature is gained nano flower-like structure monocline phase titanic oxide at 160 DEG C
X-ray diffractogram；
Fig. 2 is the photo of nano flower-like structure monocline phase titanic oxide prepared by the present invention under scanning electron microscope, is put
Big multiple is 100,000 times；
Fig. 3 is the photo of nano flower-like structure monocline phase titanic oxide prepared by the present invention under scanning electron microscope, is put
Big multiple is 30,000 times；
Fig. 4 is the photo of nano flower-like structure monocline phase titanic oxide prepared by the present invention under transmission electron microscope.
Specific embodiment
The present invention is described in detail With reference to embodiment.
[embodiment 1]
15% titanium trichloride dilute hydrochloric acid solution of 3ml is dissolved in 30ml ethylene glycol, is stirred using magnetic force thermostatic mixer
3h is allowed to uniformly mix.Above-mentioned mixed solution is poured into the autoclave with polytetrafluoroethyllining lining, case is then moved into
Formula furnace is heated to 150 DEG C, soaking time 5h, then naturally cools to room temperature taking-up.Solution after reaction is used into deionization respectively
Water and dehydrated alcohol centrifuge washing are three times.Gains after above-mentioned washing are dried in the vacuum oven at 60 DEG C, are obtained
To the monocline phase titanic oxide of flower-like nanometer spherical structure.Through detecting, gained TiO2The floriform appearance of-B is poor.
[embodiment 2]
15% titanium trichloride dilute hydrochloric acid solution of 3ml is dissolved in 30ml ethylene glycol, is stirred using magnetic force thermostatic mixer
7h is allowed to uniformly mix.Above-mentioned mixed solution is poured into the autoclave with polytetrafluoroethyllining lining, case is then moved into
Formula furnace is heated to 150 DEG C, soaking time 6h, then naturally cools to room temperature taking-up.Solution after reaction is used into deionization respectively
Water and dehydrated alcohol centrifuge washing are three times.Gains after above-mentioned washing are dried in the vacuum oven at 80 DEG C, are obtained
To the monocline phase titanic oxide of flower-like nanometer spherical structure.Through detecting, gained TiO2The floriform appearance of-B is general.
[embodiment 3]
15% titanium trichloride dilute hydrochloric acid solution of 3ml is dissolved in 30ml ethylene glycol, is stirred using magnetic force thermostatic mixer
11h is allowed to uniformly mix.Above-mentioned mixed solution is poured into the autoclave with polytetrafluoroethyllining lining, is then moved into
Batch-type furnace is heated to 160 DEG C, soaking time 5h, then naturally cools to room temperature taking-up.By the solution after reaction spend respectively from
Sub- water and dehydrated alcohol centrifuge washing are three times.Gains after above-mentioned washing are dried in the vacuum oven at 60 DEG C,
Obtain the monocline phase titanic oxide of flower-like nanometer spherical structure.Through detecting, gained TiO2The floriform appearance of-B is preferable.
Using the phase structure of powder obtained by X-ray diffraction analysis, as a result as shown in Figure 1；Utilize Flied emission scanning electron
Microscope observes gained monocline phase titanic oxide (TiO2- B) pattern and size, as a result as shown in Figures 2 and 3；Utilize transmission
Electron microscope observation gained monocline phase titanic oxide, as a result as shown in Figure 4.Acquired results show proposed by the present invention molten
The monoclinic phase titanium dioxide product of agent thermal synthesis method preparation is the nano flower-like structure assembled by nanometer sheet, wherein nanometer
Piece thickness is uniform, and size is in 10nm or less.Its technical process safety, simple, good dispersion, regular shape are uniform.Using receiving
The shape and size of rice flower-like structure monocline phase titanic oxide can prepare semiconductor devices in the related fields of its application,
The fields such as lithium cell cathode material, photochemical catalyst, sode cell electrode material, humidity sensor material and air purifier also have wide
Application prospect.
The above is only not to make limit in any form to the present invention to better embodiment of the invention
System, any simple modification that embodiment of above is made according to the technical essence of the invention, equivalent variations and modification,
Belong in the range of technical solution of the present invention.
Claims (5)
1. a kind of preparation method of nano flower-like structure monocline phase titanic oxide, it is characterised in that follow the steps below:
1. titanium trichloride dilute hydrochloric acid solution is dissolved in ethylene glycol, and uniformly mix；
2. pouring into mixture solution in the autoclave with polytetrafluoroethyllining lining；
3. reaction kettle is put into batch-type furnace, a period of time is heated and kept the temperature, taking-up is then cooled to room temperature；
4. by the solution after reaction, successively with deionized water and dehydrated alcohol wash respectively three times, centrifuge separation, remove impurity；
5. by gains drying after above-mentioned washing and grinding, nano flower-like structure monoclinic phase titania powder is obtained.
2. according to a kind of preparation method of nano flower-like structure monocline phase titanic oxide described in claim 1, it is characterised in that: institute
It states step 1. 3~5ml15% titanium trichloride dilute hydrochloric acid solution is dissolved in 30~40ml ethylene glycol, and uniformly mixes, using magnetic
Power thermostatic mixer stirs 3~11h, is allowed to sufficiently dissolve.
3. according to a kind of preparation method of nano flower-like structure monocline phase titanic oxide described in claim 1, it is characterised in that: institute
It states step 3. reaction kettle is put into batch-type furnace, is heated to 130~160 DEG C, 4~7h of soaking time is then cooled to room temperature and takes
Out.
4. according to a kind of preparation method of nano flower-like structure monocline phase titanic oxide described in claim 1, it is characterised in that: institute
State step 4. for the solution after reaction, successively with deionized water and dehydrated alcohol wash respectively three times, centrifuge separation, go to clean
Matter.
5. according to a kind of preparation method of nano flower-like structure monocline phase titanic oxide described in claim 1, it is characterised in that: institute
It states step to be 5. dried using vacuum drying oven, be dried at 50~80 DEG C, grinding vessel are agate mortar.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111762814A (en) * | 2020-07-02 | 2020-10-13 | 西南大学 | TiO2(B) Preparation and application of @ RGO aerogel negative electrode material |
| CN112194178A (en) * | 2020-10-20 | 2021-01-08 | 福州大学 | Titanium dioxide and Prussian blue ordered assembly state mesomorphic nano material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105129849A (en) * | 2015-09-17 | 2015-12-09 | 上海大学 | Flowerlike nano-sized titanium dioxide material and template-free preparation method thereof |
| CN106732493A (en) * | 2016-12-06 | 2017-05-31 | 吉林大学 | A kind of preparation method of nano-sheet monocline crystal titanium dioxide B photochemical catalysts |
-
2019
- 2019-07-22 CN CN201910658903.1A patent/CN110294493A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105129849A (en) * | 2015-09-17 | 2015-12-09 | 上海大学 | Flowerlike nano-sized titanium dioxide material and template-free preparation method thereof |
| CN106732493A (en) * | 2016-12-06 | 2017-05-31 | 吉林大学 | A kind of preparation method of nano-sheet monocline crystal titanium dioxide B photochemical catalysts |
Non-Patent Citations (1)
| Title |
|---|
| 代国宾: "TiO2 纳米晶制备条件对降解亚甲基蓝的影响研究", 《水处理技术》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111762814A (en) * | 2020-07-02 | 2020-10-13 | 西南大学 | TiO2(B) Preparation and application of @ RGO aerogel negative electrode material |
| CN112194178A (en) * | 2020-10-20 | 2021-01-08 | 福州大学 | Titanium dioxide and Prussian blue ordered assembly state mesomorphic nano material and preparation method thereof |
| CN112194178B (en) * | 2020-10-20 | 2021-06-01 | 福州大学 | Titanium dioxide and Prussian blue ordered assembly state mesomorphic nano material and preparation method thereof |
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