CN1827529A - Preparation method of nano titanium dioxide precursor - Google Patents
Preparation method of nano titanium dioxide precursor Download PDFInfo
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- CN1827529A CN1827529A CN 200510051445 CN200510051445A CN1827529A CN 1827529 A CN1827529 A CN 1827529A CN 200510051445 CN200510051445 CN 200510051445 CN 200510051445 A CN200510051445 A CN 200510051445A CN 1827529 A CN1827529 A CN 1827529A
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- 239000002243 precursor Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title abstract 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 20
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 18
- 238000007605 air drying Methods 0.000 claims abstract description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 32
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical compound CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 2
- 239000012047 saturated solution Substances 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 26
- 239000011159 matrix material Substances 0.000 abstract description 7
- 239000004408 titanium dioxide Substances 0.000 abstract description 7
- 230000007062 hydrolysis Effects 0.000 abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 239000003960 organic solvent Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 abstract 4
- 239000002131 composite material Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000010936 titanium Substances 0.000 description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- -1 distilled water Chemical compound 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- HFDCVHDLKUZMDI-UHFFFAOYSA-N sulfuric acid titanium Chemical compound [Ti].OS(O)(=O)=O HFDCVHDLKUZMDI-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Abstract
The invention relates to the field of preparation of nano materials, in particular to a preparation method of a nano titanium dioxide precursor. The method comprises the following steps: adding titanium sulfate into water, and stirring until the titanium sulfate is completely dissolved to form a solution A with the concentration of the titanium sulfate being more than 1 mol/L; then adding acetylacetone, and stirring for 0.5-24 h at 15-75 ℃ to form a tan solution B; the molar ratio of the addition amount of the acetylacetone to the titanium sulfate in the solution A is 2-5; and finally, adding the solution B into an acetone solution while stirring, wherein the volume ratio of the solution B to acetone is less than 0.5, continuously stirring, and naturally air-drying or drying the obtained pale yellow particles to obtain the nano titanium dioxide precursor. The method has the advantages of easily available raw materials, low cost, and easy storage and transportation; the prepared nano titanium dioxide precursor has moderate hydrolysis speed, and the reaction condition is easy to control when preparing titanium dioxide; and can be dissolved in organic solvents such as ethanol and the like, and is suitable for preparing the titanium dioxide/organic matrix composite material.
Description
Technical field
The present invention relates to belong to the preparation field of nano material, specifically relate to a kind of preparation method of nano-TiO 2 precursor.
Background technology
Nano titanium oxide is as a kind of important inorganic functional material, because of it has high photocatalytic activity, good weathering resistance, erosion resistance, intensive ultraviolet screening ability and can produce many particular performances such as peculiar colour effect, and enjoy people's attention at numerous areas such as wastewater treatment, sun-proof skin care, coating and automotive industry, transmitter, function ceramics, photocatalysts.In addition, titanium dioxide/organic matrix nano composite material can with many feature set of inorganic, organic, nanoparticle have many specific performances, is just becoming one of research focus of people.
Nano titanium oxide still is that the preparation of titanium dioxide/organic matrix nano composite material all will be selected suitable TiO 2 precursor earlier.Nano-TiO 2 precursor commonly used mainly includes organic titanate, titanium tetrachloride and titanium sulfate.But organic titanate and titanium tetrachloride are liquid phase, and and easy deliquescence, make that the storage of raw material and transportation are very inconvenient; Organic titanate is on the high side simultaneously, causes the cost of product higher, is unfavorable for the popularization of suitability for industrialized production; In addition, the hydrolysis rate of organic titanate and titanium tetrachloride is too fast, is unfavorable for the control of experiment condition.Advantages such as and though titanium sulfate has unsuitable deliquescence, and are cheap, it can only be dissolved in the water, and can not directly be dissolved in the organic solvent, and this has just limited its application aspect preparation titanium dioxide/organic matrix matrix material.
Summary of the invention
The objective of the invention is to overcome in the existing nano-TiO 2 precursor the easy deliquescence of organic titanate and titanium tetrachloride and be unfavorable for that accumulating, price height cause the cost height, hydrolysis rate is too fast and be unfavorable for the control of experiment condition; Titanium sulfate can not directly be dissolved in the organic solvent and limit the defective of its application, thus provide a kind of raw material should get, with low cost, be easy to accumulating, and the preparation method of the moderate nano-TiO 2 precursor of hydrolysis rate.
The objective of the invention is to realize by the following technical solutions:
The invention provides a kind of preparation method of nano-TiO 2 precursor, comprise the steps:
1) titanium sulfate is added to the water, is stirred to dissolving fully, form the solution A of titanium sulfate concentration greater than 1mol/L;
Described water can be more purified water such as distilled water, redistilled water and deionized water;
The saturated solution of described solution A preferably sulfuric acid titanium;
2) in solution A, add methyl ethyl diketone, stir 0.5～24h down, form brown solution B at 15～75 ℃; The add-on of methyl ethyl diketone and the mol ratio of the titanium sulfate in the solution A are 2～5;
3) under condition of stirring solution B is joined acetone soln, the volume ratio of solution B and acetone then has yellow particle to generate less than 0.5 at once, continues to stir 1～12h, with above-mentioned solution filtration or centrifugal, obtains light yellow particle;
The weight content of water is 0.1～1% in the described acetone soln;
4) the light yellow particle that step 3) is obtained, natural air drying, or under 40～80 ℃, dry 1～10h, obtain nano-TiO 2 precursor of the present invention.
Compared with prior art, the nano-TiO 2 precursor of method preparation provided by the invention has following advantage:
1. this nano-TiO 2 precursor is from titanium sulfate, and raw material should get, and is with low cost.
2. this nano-TiO 2 precursor preparation technology flow process is simple, is suitable for suitability for industrialized production.
3. this nano-TiO 2 precursor is solid, is unsuitable for deliquescence, is easy to store and transportation.
4. this nano-TiO 2 precursor hydrolysis rate is moderate, and reaction conditions is easy to control when preparation titanium dioxide.
5. this nano-TiO 2 precursor directly can obtain the titania nanoparticles of particle diameter at 100～500nm through high-temperature calcination.
6. this nano-TiO 2 precursor directly is dissolved in the water, and need not any processing can obtain particle diameter is about 10nm, the Ti of no agglomeration (OH)
4Particle.
7. this nano-TiO 2 precursor can be dissolved among the organic solvents such as ethanol, is suitable for the preparation of titanium dioxide/organic matrix matrix material.
Description of drawings
Fig. 1 is the TEM photo of the nano-TiO 2 precursor of the embodiment of the invention 1 preparation;
Fig. 2 is the thermal analysis curve of the nano-TiO 2 precursor of the embodiment of the invention 1 preparation;
Fig. 3 is the XRD curve of nano-TiO 2 precursor after 600 ℃ of calcinings of the embodiment of the invention 1 preparation;
Fig. 4 is the direct Ti that obtains soluble in water (OH) of nano-TiO 2 precursor of the embodiment of the invention 1 preparation for using
4Nano particle.
Embodiment
Embodiment 1.
The titanium sulfate (0.078mol) of 10g is joined in the 15ml distilled water, be stirred to dissolving fully, form solution A.The methyl ethyl diketone that adds 20ml (0.2mol) in solution A stirs 24h at 15 ℃, forms brown solution B.Under condition of stirring, solution B 5ml slowly joined the 1L water content and be 1% acetone soln, then have yellow particle to generate at once, continue to stir 12h.Above-mentioned solution is filtered, and the light yellow particle natural air drying with obtaining obtains nano-TiO 2 precursor of the present invention.
With transmission electron microscope (TEM) test, as shown in Figure 1, this nano-TiO 2 precursor is a spheroidal particle, and its powder granularity is in 100～500nm scope.
This nano-TiO 2 precursor is carried out heat analyzes, its TG-DTA curve as shown in Figure 2, when temperature reached 500 ℃, this nano-TiO 2 precursor decomposed fully.
With this nano-TiO 2 precursor 600 ℃ of calcining 2h in retort furnace, can obtain spherical dispersive titania nanoparticles, the particle diameter of this titania nanoparticles is in the scope of 100～500nm, its XRD curve as shown in Figure 3, as seen this titania nanoparticles is a Detitanium-ore-type.
This nano-TiO 2 precursor 10g is dissolved in the 1L deionized water, stirs 0.5～2h, need not be any other processing, can obtain the Ti (OH) of white
4Particle.Its SEM photo as shown in Figure 4, the Ti that obtains (OH)
4The particle diameter of nano particle is about 10nm, and no agglomeration has good dispersiveness.This particle is calcined under differing temps, also can be obtained titania nanoparticles.
Embodiment 2.
The titanium sulfate (0.1mol) of 12.8g is joined in the 10ml redistilled water, be stirred to dissolving fully, form solution A.The methyl ethyl diketone that adds 0.2mol in solution A stirs 0.5h at 75 ℃, forms brown solution B.Under condition of stirring, solution B 50ml slowly joined the 1L water content and be 0.1% acetone soln, then have yellow particle to generate at once, continue to stir 1h.With above-mentioned solution centrifugal, the light yellow particle that obtains is dried 10h at 40 ℃, obtain nano-TiO 2 precursor of the present invention.
Embodiment 3.
The titanium sulfate (0.1mol) of 12.8g is joined in the 100ml deionized water, be stirred to dissolving fully, form solution A.The methyl ethyl diketone that adds 0.5mol in solution A stirs 12h at 50 ℃, forms brown solution B.Under condition of stirring, solution B 200ml slowly joined the 1L water content and be 0.5% acetone soln, then have yellow particle to generate at once, continue to stir 5h.With above-mentioned solution centrifugal, the light yellow particle that obtains is dried 1h at 80 ℃, obtain nano-TiO 2 precursor of the present invention.
Claims (5)
1, a kind of preparation method of nano-TiO 2 precursor comprises the steps:
1) titanium sulfate is added to the water, is stirred to dissolving fully, form the solution A of titanium sulfate concentration greater than 1mol/L;
2) in solution A, add methyl ethyl diketone, stir 0.5～24h down, form brown solution B at 15～75 ℃; The add-on of methyl ethyl diketone and the mol ratio of the titanium sulfate in the solution A are 2～5;
3) under condition of stirring solution B is joined acetone soln, the volume ratio of solution B and acetone then has yellow particle to generate less than 0.5 at once, continues to stir 1～12h, with above-mentioned solution filtration or centrifugal, obtains light yellow particle;
4) the light yellow particle that step 3) is obtained, natural air drying or oven dry obtain nano-TiO 2 precursor of the present invention.
2, the preparation method of nano-TiO 2 precursor as claimed in claim 1 is characterized in that: described water is distilled water, redistilled water or deionized water.
3, the preparation method of nano-TiO 2 precursor as claimed in claim 1 is characterized in that: described solution A is the saturated solution of titanium sulfate.
4, the preparation method of nano-TiO 2 precursor as claimed in claim 1 is characterized in that: the weight content of water is 0.1～1% in the described acetone soln.
5, the preparation method of nano-TiO 2 precursor as claimed in claim 1 is characterized in that: the oven dry described in the step 4) is to carry out 1～10h under 40～80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100514453A CN1331760C (en) | 2005-03-04 | 2005-03-04 | Preparation method of nano titanium dioxide precursor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100514453A CN1331760C (en) | 2005-03-04 | 2005-03-04 | Preparation method of nano titanium dioxide precursor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1827529A true CN1827529A (en) | 2006-09-06 |
| CN1331760C CN1331760C (en) | 2007-08-15 |
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|---|---|---|---|
| CNB2005100514453A Expired - Fee Related CN1331760C (en) | 2005-03-04 | 2005-03-04 | Preparation method of nano titanium dioxide precursor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106280251A (en) * | 2016-08-10 | 2017-01-04 | 袁春华 | A kind of preparation method of LED encapsulation nano composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1295977A (en) * | 2000-12-19 | 2001-05-23 | 中国科学院上海硅酸盐研究所 | Simple method for preparing titanium dioxide collosol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106280251A (en) * | 2016-08-10 | 2017-01-04 | 袁春华 | A kind of preparation method of LED encapsulation nano composite material |
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| CN1331760C (en) | 2007-08-15 |
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Granted publication date: 20070815 Termination date: 20170304 |