CN109502638A - A kind of preparation method of titanium dioxide microballoon sphere - Google Patents
A kind of preparation method of titanium dioxide microballoon sphere Download PDFInfo
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- CN109502638A CN109502638A CN201811473063.3A CN201811473063A CN109502638A CN 109502638 A CN109502638 A CN 109502638A CN 201811473063 A CN201811473063 A CN 201811473063A CN 109502638 A CN109502638 A CN 109502638A
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- titanium dioxide
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a kind of preparation method of titanium dioxide microballoon sphere, belongs to technical field of inorganic material.The present invention is synthetically prepared titanium dioxide microballoon sphere by room temperature；The present invention, by addition butyl titanate, provides titanium material source in the first step for the synthesis of titanium dioxide microballoon sphere.On the other hand by the way that deionized water is added, it is effectively controlled the pattern variation of titanium dioxide, is finally synthesizing titanium dioxide microballoon sphere.The preparation method is easily controllable, low in cost, and technique is relatively easy, and large-scale production may be implemented.
Description
Technical field
The present invention relates to technical field of inorganic material, more particularly to a kind of preparation method of titanium dioxide microballoon sphere.
Background technique
Titanium dioxide (TiO2) become in conductor photocatalysis material due to its excellent photoelectric conversion and physical and chemical performance
Research hotspot.Titanium dioxide nanocrystalline semiconductor solar cell is using nano-crystal porous film electrode, by increasing its surface
No matter the long-pending photoelectric conversion efficiency to improve battery, this technology have certain development latent in theoretical basis and application technology
Power has a possibility that replacing silicon solar cell and traditional solar cell power generation, to TiO2The nano crystal semiconductor sun
The further investigation of energy battery, greatly promotes the development in nanostructure Photoelectrochemistry of semiconductor new branch of science field.In environmental pollution
Improvement, TiO2In the case where energy is greater than the light irradiation of its forbidden bandwidth, generate electronics and hole pair, then light induced electron migrate to
Catalyst surface realizes efficiently separating for photo-generated carrier, the Strong oxdiative ability of photohole and the reducing power of conduction band electron
Can effectively redox major part organic matter and some metal ions, this point is based on, in control of environmental pollution side
Mask is of great importance.Therefore, titanium dioxide is prepared with important researching value and application value.
Prepare TiO2Method have very much, such as liquid phase preparation process, physical vaporous deposition, chemical vapour deposition technique, electricity
Chemical method etc..Using different processes, ingredient, structure, orientation and the cost of the titanium dioxide of preparation etc. are
Difference.Solid phase method is mainly carried out using thermal decomposition or the variation of solid phase-solid phase, but equipment energy consumption is big, and product purity is low；Chemistry
Vapour deposition process, which is brought reactant in reactor by carrier gas, to react, but equipment operation is complicated, needs strict control substrate temperature
Degree.The present invention uses room temperature synthetic method, amount of reactant etc. is added to control crystal growth by regulation, synthesis of titanium dioxide is micro-
Ball, the complicated technology synthesis for other titanium dioxide that compare, the technique relative ease, relative inexpensiveness.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of titanium dioxide microballoon sphere, above-mentioned of the existing technology to solve
Problem, the preparation method is easily controllable, low in cost, and technique is relatively easy, and large-scale production may be implemented.
To achieve the above object, the present invention provides following schemes:
The present invention provides a kind of preparation method of titanium dioxide microballoon sphere, comprising the following steps:
(1) it weighs butyl titanate to be added in beaker, dehydrated alcohol is then added, magnetic agitation keeps the two sufficiently mixed
It closes；
(2) octadecylamine is weighed, is added in step (1) resulting mixed solution, magnetic agitation；
(3) the mixed solution and dripping deionized water prepared by step (2) is then stood；
(4) the resulting uniform suspension of step (3) is removed into supernatant, resulting precipitated product is repeatedly clear with dehydrated alcohol
It washes, is put into drying box, 60 DEG C of heat preservation drying, obtain titanium dioxide microballoon sphere in baking oven.
Preferably, it is 1~10g that quality, which is added, in the butyl titanate, and 10~40mL is added in the dehydrated alcohol.
Preferably, the magnetic agitation time is 10~60min in the step (1).
Preferably, in step (2), the octadecylamine quality is 0.5~2.5g.
Preferably, the magnetic agitation time is 0.5~2.5h in the step (2).
Preferably, in step (3), the deionized water additional amount is 0~5mL.
Preferably, time of repose is 0.5~2.5h in the step (3).
The invention discloses following technical effects:
The present invention is synthetically prepared titanium dioxide microballoon sphere by room temperature；
The present invention, by addition butyl titanate, provides titanium material source in the first step for the synthesis of titanium dioxide microballoon sphere；
On the other hand by the way that the amount of deionized water is added, it is effectively controlled the pattern variation of titanium dioxide, is finally synthesizing titanium dioxide
Microballoon.The preparation method is easily controllable, low in cost, and technique is relatively easy, and large-scale production may be implemented.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the TiO for being not added with deionized water2Scanning electron microscope (SEM) photograph (SEM)；
Fig. 2 is the TiO for adding 2.5ml deionized water2The scanning electron microscope (SEM) photograph (SEM) of microballoon, resulting TiO2Microsphere surface compared with
To be smooth, diameter is in 800nm or less.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing and specific real
Applying mode, the present invention is described in further detail.
Embodiment 1
1) it weighs 5g butyl titanate to be added in 50ml beaker, then addition 40ml dehydrated alcohol, magnetic agitation 10min,
So that the two is sufficiently mixed；
2) 0.5g octadecylamine is weighed, is added in the resulting mixed solution of step 1), and magnetic agitation 1h；
3) deionized water of 0ml is added dropwise to mixed solution prepared by step 2), then stands 1h；
4) the resulting uniform suspension of step 3) is removed into supernatant, resulting precipitated product is repeatedly clear with dehydrated alcohol
It washes, is put into drying box, 60 DEG C of heat preservation drying, do not obtain titanium dioxide microballoon sphere in baking oven.
Embodiment 2
1) it weighs 5g butyl titanate to be added in 50ml beaker, then addition 40ml dehydrated alcohol, magnetic agitation 10min,
So that the two is sufficiently mixed；
2) 0.5g octadecylamine is weighed, is added in the resulting mixed solution of step 1), and magnetic agitation 1h；
3) deionized water of 0.5ml is added dropwise to mixed solution prepared by step 2), then stands 1h；
4) the resulting uniform suspension of step 3) is removed into supernatant, resulting precipitated product is repeatedly clear with dehydrated alcohol
It washes, is put into drying box, 60 DEG C of heat preservation drying, obtain titanium dioxide microballoon sphere in baking oven.
Embodiment 3
1) it weighs 5g butyl titanate to be added in 50ml beaker, then addition 40ml dehydrated alcohol, magnetic agitation 10min,
So that the two is sufficiently mixed；
2) 0.5g octadecylamine is weighed, is added in the resulting mixed solution of step 1), and magnetic agitation 1h；
3) deionized water of 2.5ml is added dropwise to mixed solution prepared by step 2), then stands 1h；
4) the resulting uniform suspension of step 3) is removed into supernatant, resulting precipitated product is repeatedly clear with dehydrated alcohol
It washes, is put into drying box, 60 DEG C of heat preservation drying, obtain titanium dioxide microballoon sphere in baking oven.
Embodiment described above is only that preferred embodiment of the invention is described, and is not carried out to the scope of the present invention
It limits, without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention
Various changes and improvements, should all fall into claims of the present invention determine protection scope in.
Claims (7)
1. a kind of preparation method of titanium dioxide microballoon sphere, which comprises the following steps:
(1) it weighs butyl titanate to be added in beaker, dehydrated alcohol is then added, magnetic agitation is sufficiently mixed the two；
(2) octadecylamine is weighed, is added in step (1) resulting mixed solution, magnetic agitation；
(3) the mixed solution and dripping deionized water prepared by step (2) is then stood；
(4) the resulting uniform suspension of step (3) being removed into supernatant, resulting precipitated product is cleaned repeatedly with dehydrated alcohol,
It is put into drying box, 60 DEG C of heat preservation drying, obtain titanium dioxide microballoon sphere in baking oven.
2. a kind of preparation method of titanium dioxide microballoon sphere according to claim 1, which is characterized in that in step (1), institute
Stating butyl titanate and quality is added is 1~10g, and 10~40mL is added in the dehydrated alcohol.
3. a kind of preparation method of titanium dioxide microballoon sphere according to claim 1, which is characterized in that in the step (1)
The magnetic agitation time is 10~60min.
4. a kind of preparation method of titanium dioxide microballoon sphere according to claim 1, which is characterized in that in step (2), institute
Stating octadecylamine quality is 0.5~2.5g.
5. a kind of preparation method of titanium dioxide microballoon sphere according to claim 1, which is characterized in that in the step (2)
The magnetic agitation time is 0.5~2.5h.
6. a kind of preparation method of titanium dioxide microballoon sphere according to claim 1, which is characterized in that in step (3), institute
Stating deionized water additional amount is 0~5mL.
7. a kind of preparation method of titanium dioxide microballoon sphere according to claim 1, which is characterized in that in the step (3)
Time of repose is 0.5~2.5h.
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| CN201811473063.3A CN109502638A (en) | 2018-12-04 | 2018-12-04 | A kind of preparation method of titanium dioxide microballoon sphere |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101214999A (en) * | 2007-12-27 | 2008-07-09 | 浙江大学 | Method for preparing doping titanium dioxide nano crystal |
| CN101318694A (en) * | 2008-06-20 | 2008-12-10 | 浙江大学 | Method for preparing titanium dioxide nanocrystalline with highlight catalytic activity in low-temperature |
| CN101890343A (en) * | 2010-06-29 | 2010-11-24 | 浙江大学 | Low temperature surface modification method for titanium dioxide nanocrystal |
| CN103706347A (en) * | 2013-12-09 | 2014-04-09 | 上海应用技术学院 | TiO2 microsphere and preparation method therefor |
-
2018
- 2018-12-04 CN CN201811473063.3A patent/CN109502638A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101214999A (en) * | 2007-12-27 | 2008-07-09 | 浙江大学 | Method for preparing doping titanium dioxide nano crystal |
| CN101318694A (en) * | 2008-06-20 | 2008-12-10 | 浙江大学 | Method for preparing titanium dioxide nanocrystalline with highlight catalytic activity in low-temperature |
| CN101890343A (en) * | 2010-06-29 | 2010-11-24 | 浙江大学 | Low temperature surface modification method for titanium dioxide nanocrystal |
| CN103706347A (en) * | 2013-12-09 | 2014-04-09 | 上海应用技术学院 | TiO2 microsphere and preparation method therefor |
Non-Patent Citations (2)
| Title |
|---|
| 丁莹莹: "纳米晶TiO2材料的制备及其光电子特性的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 向礼琴等: "准单分散球形二氧化钛颗粒的可控制备研究", 《无机材料学报》 * |
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Application publication date: 20190322 |