CN106348341A - Preparation method of titanium dioxide hollow nanospheres - Google Patents
Preparation method of titanium dioxide hollow nanospheres Download PDFInfo
- Publication number
- CN106348341A CN106348341A CN201610828435.4A CN201610828435A CN106348341A CN 106348341 A CN106348341 A CN 106348341A CN 201610828435 A CN201610828435 A CN 201610828435A CN 106348341 A CN106348341 A CN 106348341A
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- titanium dioxide
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- water
- hollow ball
- dioxide nano
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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
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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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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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of titanium dioxide hollow nanospheres, comprising: dropping titanium tetrachloride into water at a speed of </=0.5 mL/s to obtain emulsion, subjecting the emulsion to solid-liquid separation, washing and drying to obtain dispersed titanium dioxide hollow nanospheres 30-200 nm in sphere diameter and 6-30 nm in sphere shell thickness; preferably, the water has pH of 3-12 and is at 20-100 DEG C, the water is being stirred when the titanium tetrachloride is added, the solid-liquid separation is centrifugal separation at a speed of >/=1000 r/min for a period of >/=5 min, washing refers to the use of deionized water or ethanol to wash separated solids, the separated solids are under centrifugal separation during washing, and drying refers to air-drying the washed solids at normal temperature. The preparation method has the advantages of good simplicity and convenience, low cost and environmental friendliness, and large-scale industrial production and target product commercial application are highly facilitated.
Description
Technical field
The present invention relates to a kind of preparation method of hollow ball, especially a kind of preparation side of titanium dioxide nano hollow ball
Method.
Background technology
Nano titanium oxide because of good stability and band structure, in photocatalysis, opto-electronic conversion, antifog, automatically cleaning, painting
The fields such as material, cosmetics have a wide range of applications.Nano titanium oxide hollow ball compared with medicine ball, have density little,
The optical characteristics that specific surface area is big, thermal stability is good and special.For this reason, people are to obtain nano titanium oxide hollow ball
It is made that unremitting effort, a kind of titanium dioxide that such as Chinese invention patent cn 103803646b announces on November 18th, 2015
The preparation method of titanium hollow ball.First with potassium chloride as surface modifier, tetraethyl orthosilicate prepares silicon dioxide for raw material to the method
Spheroidal particle, recycles the surface charge of silica colloidal spheres and the speed of lifting to prepare silica colloidal crystal mould
Plate, afterwards, first will silica colloidal crystal template immerse in titania gel after slow pull-out film layer, then by the film drying
After layer calcining, erosion removal silica template, obtain product.Though this preparation method can obtain titanium dioxide hollow ball,
There is also weak point, first, method is excessively complicated, need to after the preparation of template, the cladding of titania gel, calcining and
The processes such as the removal of template；Secondly, repeatedly it is related to bronsted lowry acids and bases bronsted lowry solution in preparation process, easily causes environmental pollution；Again, it is obtained
Product in hollow bulb diameter bigger than normal, mostly submicron order, and hollow ball is connected with each other film-like so as to specific surface area has
Limit.
Content of the invention
The technical problem to be solved in the present invention is to overcome weak point of the prior art, provides a kind of hollow ball to be in dispersion
Shape and the preparation method of simple and convenient titanium dioxide nano hollow ball.
For solving the technical problem of the present invention, the technical scheme being adopted is: the preparation side of titanium dioxide nano hollow ball
Method adopts drop-method, particularly completes step as follows:
First titanium tetrachloride is instilled in water with the speed of≤0.5ml/s, obtain emulsion, then carry out solid-liquid successively to emulsion dividing
From, washing and the process being dried, prepared bulb diameter is 30～200nm, the thick nano titania for 6～30nm of spherical shell is hollow
Ball.
Improvement further as the preparation method of titanium dioxide nano hollow ball:
Preferably, the ph value of water is 3～12, and temperature is 20～100 DEG C.
Preferably, when titanium tetrachloride instills, water is stirring；Beneficial to acceleration reaction.
Preferably, solid-liquid separation is processed as centrifugation, its rotating speed >=1000r/min, time >=5min.
Preferably, carrying out washing treatment is to be carried out to separating the solids obtaining using deionized water or ethanol, during cleaning
Separating solids is centrifugation.
Preferably, dried is the solids after cleaning to be placed under room temperature dry.
With respect to the beneficial effect of prior art it is:
First, being characterized using scanning electron microscope and transmission electron microscope respectively to prepared purpose product, from its result,
Purpose product is dispergated titanium dioxide hollow ball；Wherein, the bulb diameter of titanium dioxide hollow ball is 30～200nm, spherical shell
Thick is 6～30nm.This purpose product being made up of dispergated nano titanium oxide hollow ball, both due to nano titanium oxide
Good stability and band structure, but the density having because of nano titanium oxide hollow ball is little, specific surface area is big, heat stability
The good and special optical characteristics of energy, due also to dispergated nano titanium oxide hollow ball has higher specific surface area, thus
Purpose product is made to be extremely easy to be widely used in photocatalysis, opto-electronic conversion, the antifog, field such as automatically cleaning, coating, cosmetics.
Second, preparation method is simple, science, efficiently.It is in dispergated purpose product two that hollow ball has not only been obtained
TiOx nano hollow ball, also has the characteristics that simple and convenient, low cost, environmental protection so as to be easy to industrialization on a large scale
Produce the commercial applications with purpose product.
Brief description
Fig. 1 is that the purpose product that preparation method is obtained is characterized using scanning electron microscope (sem) and transmission electron microscope (tem)
One of result.Wherein, Fig. 1 a is the sem image of purpose product；Fig. 1 b is the tem image of purpose product.
Specific embodiment
Below in conjunction with the accompanying drawings the optimal way of the present invention is described in further detail.
Buy from market first or be voluntarily obtained:
Titanium tetrachloride；
Water；
Deionized water；
Ethanol.
Then,
Embodiment 1
That prepares concretely comprises the following steps:
First titanium tetrachloride is instilled in water with the speed of 0.1ml/s；Wherein, the ph value of water is 3, and temperature is 20 DEG C, and water is
Stirring (or static) state, obtains emulsion.Emulsion is carried out successively with solid-liquid separation, washing and the process being dried again；Wherein, solid-liquid
Separating treatment is centrifugation, and its rotating speed is 1000r/min, the time is 10min, and carrying out washing treatment is using deionized water (or second
Alcohol) it is carried out to separating the solids that obtain, separating solids during cleaning is centrifugation, and dried is will be after cleaning
Solids are placed in dries under room temperature, is obtained and is similar to the titanium dioxide nano hollow ball shown in Fig. 1.
Embodiment 2
That prepares concretely comprises the following steps:
First titanium tetrachloride is instilled in water with the speed of 0.2ml/s；Wherein, the ph value of water is 5, and temperature is 40 DEG C, and water is
Stirring (or static) state, obtains emulsion.Emulsion is carried out successively with solid-liquid separation, washing and the process being dried again；Wherein, solid-liquid
Separating treatment is centrifugation, and its rotating speed is 2000r/min, the time is 8min, and carrying out washing treatment is using deionized water (or second
Alcohol) it is carried out to separating the solids that obtain, separating solids during cleaning is centrifugation, and dried is will be after cleaning
Solids are placed in dries under room temperature, is obtained and is similar to the titanium dioxide nano hollow ball shown in Fig. 1.
Embodiment 3
That prepares concretely comprises the following steps:
First titanium tetrachloride is instilled in water with the speed of 0.3ml/s；Wherein, the ph value of water is 7, and temperature is 60 DEG C, and water is
Stirring (or static) state, obtains emulsion.Emulsion is carried out successively with solid-liquid separation, washing and the process being dried again；Wherein, solid-liquid
Separating treatment is centrifugation, and its rotating speed is 3000r/min, the time is 7min, and carrying out washing treatment is using deionized water (or second
Alcohol) it is carried out to separating the solids that obtain, separating solids during cleaning is centrifugation, and dried is will be after cleaning
Solids are placed in dries under room temperature, and as shown in Figure 1 titanium dioxide nano hollow ball is obtained.
Embodiment 4
That prepares concretely comprises the following steps:
First titanium tetrachloride is instilled in water with the speed of 0.4ml/s；Wherein, the ph value of water is 9, and temperature is 80 DEG C, and water is
Stirring (or static) state, obtains emulsion.Emulsion is carried out successively with solid-liquid separation, washing and the process being dried again；Wherein, solid-liquid
Separating treatment is centrifugation, and its rotating speed is 4000r/min, the time is 6min, and carrying out washing treatment is using deionized water (or second
Alcohol) it is carried out to separating the solids that obtain, separating solids during cleaning is centrifugation, and dried is will be after cleaning
Solids are placed in dries under room temperature, is obtained and is similar to the titanium dioxide nano hollow ball shown in Fig. 1.
Embodiment 5
That prepares concretely comprises the following steps:
First titanium tetrachloride is instilled in water with the speed of 0.5ml/s；Wherein, the ph value of water is 12, and temperature is 100 DEG C, water
For stirring (or static) state, obtain emulsion.Emulsion is carried out successively with solid-liquid separation, washing and the process being dried again；Wherein, Gu
Liquid separating treatment is centrifugation, and its rotating speed is 5000r/min, the time is 5min, and carrying out washing treatment is using deionized water (or second
Alcohol) it is carried out to separating the solids that obtain, separating solids during cleaning is centrifugation, and dried is will be after cleaning
Solids are placed in dries under room temperature, is obtained and is similar to the titanium dioxide nano hollow ball shown in Fig. 1.
Obviously, those skilled in the art can be carried out respectively to the preparation method of the titanium dioxide nano hollow ball of the present invention
Plant and change with modification without departing from the spirit and scope of the present invention.So, if these modifications and modification to the present invention belong to
Within the scope of the claims in the present invention and its equivalent technologies, then the present invention is also intended to comprise these changes and modification.
Claims (6)
1. a kind of preparation method of titanium dioxide nano hollow ball, using drop-method it is characterised in that to complete step as follows:
First titanium tetrachloride is instilled in water with the speed of≤0.5ml/s, obtains emulsion, then emulsion is carried out successively solid-liquid separation,
Washing and the process being dried, prepared bulb diameter is 30～200nm, the thick titanium dioxide nano hollow ball for 6～30nm of spherical shell.
2. the preparation method of titanium dioxide nano hollow ball according to claim 1, it is characterized in that the ph value of water for 3～
12, temperature is 20～100 DEG C.
3. the preparation method of titanium dioxide nano hollow ball according to claim 1, when it is characterized in that titanium tetrachloride instills,
Water is stirring.
4. the preparation method of titanium dioxide nano hollow ball according to claim 1, is characterized in that solid-liquid separation is processed as
Centrifugation, its rotating speed >=1000r/min, time >=5min.
5. the preparation method of titanium dioxide nano hollow ball according to claim 1, is characterized in that carrying out washing treatment is use
Deionized water or ethanol are carried out to separating the solids obtaining, and separating solids during cleaning is centrifugation.
6. the preparation method of titanium dioxide nano hollow ball according to claim 1, is characterized in that dried is will be clear
Solids after washing are placed in dries under room temperature.
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| CN201610828435.4A CN106348341B (en) | 2016-09-18 | 2016-09-18 | The preparation method of titanium dioxide nano hollow ball |
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| CN106348341B CN106348341B (en) | 2017-10-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107867717A (en) * | 2017-09-30 | 2018-04-03 | 常熟理工学院 | Based on hollow-core construction purple TiO2Michaelis resonance anti-fake product and its method for anti-counterfeit |
| CN107879374A (en) * | 2017-09-30 | 2018-04-06 | 常熟理工学院 | Monodisperse hollow structure green TiO2Material and preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834021A (en) * | 2006-04-07 | 2006-09-20 | 浙江工业大学 | Prepn. process of mesic hole hollow ball-shape titania powder |
| CN102583523A (en) * | 2012-01-12 | 2012-07-18 | 石家庄铁道大学 | Non-template method for preparation of titanium-oxide hollow microsphere with nanometer structure |
| CN102765754A (en) * | 2012-07-20 | 2012-11-07 | 中国科学院金属研究所 | Method for preparing porous TiO2 quasi-monodispersed micron hollow spheres |
| JP2015164881A (en) * | 2014-02-04 | 2015-09-17 | 高知県公立大学法人 | Method for synthesizing doped, core-shell, or dispersion type spherical porous anatase titanium oxide nanoparticle |
-
2016
- 2016-09-18 CN CN201610828435.4A patent/CN106348341B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834021A (en) * | 2006-04-07 | 2006-09-20 | 浙江工业大学 | Prepn. process of mesic hole hollow ball-shape titania powder |
| CN102583523A (en) * | 2012-01-12 | 2012-07-18 | 石家庄铁道大学 | Non-template method for preparation of titanium-oxide hollow microsphere with nanometer structure |
| CN102765754A (en) * | 2012-07-20 | 2012-11-07 | 中国科学院金属研究所 | Method for preparing porous TiO2 quasi-monodispersed micron hollow spheres |
| JP2015164881A (en) * | 2014-02-04 | 2015-09-17 | 高知県公立大学法人 | Method for synthesizing doped, core-shell, or dispersion type spherical porous anatase titanium oxide nanoparticle |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107867717A (en) * | 2017-09-30 | 2018-04-03 | 常熟理工学院 | Based on hollow-core construction purple TiO2Michaelis resonance anti-fake product and its method for anti-counterfeit |
| CN107879374A (en) * | 2017-09-30 | 2018-04-06 | 常熟理工学院 | Monodisperse hollow structure green TiO2Material and preparation method |
| CN107867717B (en) * | 2017-09-30 | 2019-10-18 | 常熟理工学院 | Based on hollow structure purple TiO2Michaelis resonance anti-fake product and its method for anti-counterfeit |
| CN107879374B (en) * | 2017-09-30 | 2019-12-27 | 常熟理工学院 | Monodisperse hollow structure green TiO2Material and preparation method |
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| CN106348341B (en) | 2017-10-10 |
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