CN104084096A - Method for preparing TiO2@SiO2 core-shell particles with solar heat reflection function - Google Patents
Method for preparing TiO2@SiO2 core-shell particles with solar heat reflection function Download PDFInfo
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- CN104084096A CN104084096A CN201410313570.6A CN201410313570A CN104084096A CN 104084096 A CN104084096 A CN 104084096A CN 201410313570 A CN201410313570 A CN 201410313570A CN 104084096 A CN104084096 A CN 104084096A
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Abstract
The invention discloses TiO2@SiO2 core-shell particles with a solar heat reflection function and a preparation method of the particles. The preparation method comprises the following steps: with tetra-alkyl titanate as a raw material, preparing titanium dioxide particles in a certain particle size range through a sol-gel method; and further modifying the obtained titanium dioxide particles by using tetra-alkoxysilane, thus obtaining the TiO2@SiO2 core-shell particles with the solar heat reflection function. The preparation process of the core-shell particles is simple, and high industrialization capacity and bright application prospect are achieved.
Description
Technical field
The present invention relates to a kind of solar heat reflection TiO
2siO
2the preparation method of nucleocapsid particles, refers more particularly to the preparation technology of the particle of nucleocapsid structure.
Background technology
Solar energy distributes and comprises 5% ultraviolet light, 46% visible ray and 49% near infrared light, in hot season, due to the effect of solar radiation, causes the Energy Load of most cities excessive, and then causes large-scale energy crisis.Recently, studies have found that, some metal oxide particles, as zinc oxide (ZnO), magnesia (MgO), ceria (CeO
2), titanium dioxide (TiO
2) and alundum (Al2O3) (Al
2o
3) etc. particle near infrared band, show very outstanding solar heat reflection ability, these solar heat reflection particles can be used in the fields such as military affairs, plastics and coating, to prepare the heat-barrier material (P.Jeevanandam of solar heat reflection, R.S.Mulukutla, M.Phillips et.al, J.Phys.Chem.C, 2007,111,1912-1918).
Wherein, titanium dioxide is as one of industrialized powder body material the earliest, and its solar heat reflection ability is particularly outstanding, is one of the most frequently used solar heat reflection pigment.Solar heat reflection ability and the grain diameter of titanium dioxide granule has very large associated, have research to point out, particle diameter is that the titanium dioxide of 1.1～1.4 μ m scopes can make titanium dioxide all have good solar heat reflection performance (half of near-infrared wavelength (2500nm)) at whole infrared band.Yet, photocatalysis characteristic due to titanium dioxide, weather resistance decline, especially the colored materials system that can cause added material of main part, the interpolation of titanium dioxide is on the more obvious (Y.Zhang of the impact of the weather resistance of material of main part, H.Yin, A.Wang et.al, J.PHYS.CHEM.SOLIDS, 2010,71,1458 – 1466).Therefore, conventionally need to be coated processing to titanium dioxide, when retaining its solar heat reflection ability, again itself and material of main part be kept apart, thereby play the object that improves material weather resistance.
Summary of the invention
The present invention has prepared a kind of TiO2SiO2 nucleocapsid particles, and this nucleocapsid particles has fabulous solar heat reflection function, and the additive that can be used as reflective insulation material is used.
Technical scheme of the present invention is: take tetralkyl titanate as raw material, the titanium dioxide granule that synthesizes certain particle diameter by sol-gel process, then with tetraalkoxysilane, titanium dioxide granule is coated to processing, finally obtains possessing the TiO2SiO2 nucleocapsid particles of solar heat reflection function.
The TiO that possesses solar heat reflection function the present invention relates to
2siO
2the preparation method of nucleocapsid particles, its concrete steps are as follows:
(A) TiO
2the preparation of (1.1～1.4 μ m) particle
Tetralkyl titanate is dissolved in to small molecular alcohol (C number: 1～4), be configured to the solution A of 5～8wt.%; Lutensol ON50 (BASF) the aqueous surfactant solution B of configuration 0.1M; Get solution B and be dissolved in small molecular alcohol (C number: 1～4), be configured to the solution C of 0.5～1.0wt.%; Solution A is mixed with certain proportion with solution C, mixing quality is than being 1:2～1:4, sum is heated to this mixed solution to react 2～4h at 50～90 ℃, afterwards by product centrifugation, washing, oven dry, finally obtains particle size range at the titanium dioxide granule of 1.1～1.4 μ m.
(B) TiO
2siO
2the preparation of nucleocapsid particles
By titanium dioxide by ultrasonic small molecular alcohol (the C number: 1～4) in the middle of solvent that is scattered in, being prepared into concentration is the dispersion liquid that 0.1～1wt.% contains admittedly, add afterwards ammoniacal liquor as catalyst, the ratio that catalyst accounts for gross mass is 1～3wt.%, finally add tetraalkoxysilane to be coated titanium dioxide, the ratio that tetraalkoxysilane accounts for gross mass is 1～5wt.%, reaction temperature is 30～60 ℃, reaction time 2～4h, by product centrifugation, washing, oven dry, finally at 200-600 ℃, calcine 2h, obtain the titanium dioxide granule of coated with silica.
The tetralkyl titanate the best of using is tetraethyl titanate, tetraisopropyl titanate and butyl titanate any time effect better.
The one or any combination aging fruit that the small molecular alcohol that the C number using is 1～4 is methyl alcohol, ethanol, isopropyl alcohol and n-butanol is better.
Tetraalkoxysilane the best of using is tetramethoxy-silicane, tetraethoxysilane and tetraisopropoxysilan any time effect better.
Preferred alcohol is prepared titanium dioxide granule as solvent, and preferably tetraethyl titanate is as titanium dioxide granule precursor.
Preferred alcohol is prepared TiO as solvent
2siO
2nucleocapsid particles, preferably tetraethoxysilane is prepared nucleocapsid particles as silica precursor.
The TiO that the present invention makes
2siO
2xRD spectra and the size distribution curve of nucleocapsid particles are measured according to a conventional method.
The present invention be take tetralkyl titanate as raw material, by sol-gel process, having prepared particle diameter is the titanium dioxide granule of 1.1～1.4 μ m, within the scope of certain PH, it being coated to processing by tetraalkoxysilane, prepare the TiO that possesses solar heat reflection function afterwards
2siO
2nucleocapsid particles, this composite particles surpasses 80% at the reflectivity of infrared band.In addition, due to shell SiO
2coating function, the photocatalysis performance of this composite particles is effectively suppressed, and can not impact the weather resistance of added material, so this composite particles has great application prospect as the additive of material.Meanwhile, this TiO
2siO
2nucleocapsid particles preparation method raw material is easy to get, and preparation process is easy, therefore has stronger application and industrial prospect.
Accompanying drawing explanation
Fig. 1 is TiO
2siO
2the size distribution curve of nucleocapsid particles.
Fig. 2 is TiO
2siO
2the XRD spectra of nucleocapsid particles.
Fig. 3 is TiO
2siO
2nucleocapsid particles is at the reflectivity curve of ultraviolet-visible-near infrared band.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described further.
Embodiment 1:
Tetraethyl titanate is dissolved in the middle of methyl alcohol, is configured to the solution A of 5wt.%; Lutensol ON50 (BASF) the aqueous surfactant solution B of configuration 0.1M; Get solution B and be dissolved in the middle of methyl alcohol, be configured to the solution C of 0.5wt.%; Solution A is evenly mixed with solution C, and mixing quality is than being 1:2, and sum is heated to this mixed solution at 50 ℃ to react 2h, afterwards by product centrifugation, washing, oven dry, finally obtains titanium dioxide granule.
Titanium dioxide is scattered in the middle of methyl alcohol by ultrasonic, being prepared into concentration is the dispersion liquid that 0.1wt.% contains admittedly, add afterwards ammoniacal liquor as catalyst, the ratio that catalyst accounts for gross mass is 1wt.%, finally adds tetraethoxysilane to be coated titanium dioxide, and reaction temperature is 30 ℃, reaction time 2h, by product centrifugation, washing, oven dry, finally at 200 ℃, calcine 2h, obtain the titanium dioxide granule of coated with silica.The TiO making
2siO
2the meta particle diameter of nucleocapsid particles is 1.1 μ m, and the reflectivity at 800nm wavelength place is 82%.
Embodiment 2:
Tetraethyl titanate is dissolved in the middle of methyl alcohol, is configured to the solution A of 8wt.%; Lutensol ON50 (BASF) the aqueous surfactant solution B of configuration 0.1M; Get solution B and be dissolved in the middle of methyl alcohol, be configured to the solution C of 1wt.%; Solution A is evenly mixed with solution C, and mixing quality is than being 1:4, and sum is heated to this mixed solution at 90 ℃ to react 4h, afterwards by product centrifugation, washing, oven dry, finally obtains titanium dioxide granule.
Titanium dioxide is scattered in the middle of methyl alcohol by ultrasonic, being prepared into concentration is the dispersion liquid that 1wt.% contains admittedly, add afterwards ammoniacal liquor as catalyst, the ratio that catalyst accounts for gross mass is 3wt.%, finally adds tetraethoxysilane to be coated titanium dioxide, and reaction temperature is 60 ℃, reaction time 4h, by product centrifugation, washing, oven dry, finally at 600 ℃, calcine 2h, obtain the titanium dioxide granule of coated with silica.The TiO making
2siO
2the meta particle diameter of nucleocapsid particles is 1.35 μ m, and the reflectivity at 800nm wavelength place is 84.5%.
Embodiment 3:
Tetraethyl titanate is dissolved in the middle of ethanol, is configured to the solution A of 6wt.%; Lutensol ON50 (BASF) the aqueous surfactant solution B of configuration 0.1M; Get solution B and be dissolved in the middle of ethanol, be configured to the solution C of 0.7wt.%; Solution A is evenly mixed with solution C, and mixing quality is than being 1:3, and sum is heated to this mixed solution at 60 ℃ to react 3h, afterwards by product centrifugation, washing, oven dry, finally obtains titanium dioxide granule.
Titanium dioxide is scattered in the middle of ethanol by ultrasonic, being prepared into concentration is the dispersion liquid that 1wt.% contains admittedly, add afterwards ammoniacal liquor as catalyst, the ratio that catalyst accounts for gross mass is 1.5wt.%, finally adds tetraethoxysilane to be coated titanium dioxide, and reaction temperature is 50 ℃, reaction time 3h, by product centrifugation, washing, oven dry, finally at 450 ℃, calcine 2h, obtain the titanium dioxide granule of coated with silica.The TiO making
2siO
2the meta particle diameter of nucleocapsid particles is 1.2 μ m, and the reflectivity at 800nm wavelength place is 86.5%.
Under above-described embodiment, the particle diameter distribution of prepared nucleocapsid sample, XRD and solar heat reflection spectrogram are the 1-3 of Figure of description.
Claims (4)
1. a solar heat reflection TiO
2siO
2the preparation method of nucleocapsid particles, is characterized in that: its concrete steps are as follows:
(A) particle size range is at the TiO of 1.1～1.4 μ m
2the preparation of particle:
It is in the middle of 1～4 small molecular alcohol that tetralkyl titanate is dissolved in to C number, is configured to the solution A of 5～8wt.%; The Lutensol ON50 aqueous surfactant solution B of configuration 0.1M; Getting solution B, to be dissolved in C number be in the middle of 1～4 small molecular alcohol, is configured to the solution C of 0.5～1.0wt.%; Solution A is mixed with solution C, and its mixing quality is than being 1:2～1:4; Afterwards this mixed solution is heated to react 2～4h at 50～90 ℃, afterwards by product centrifugation, washing, oven dry, finally obtains particle size range at the titanium dioxide granule of 1.1～1.4 μ m;
(B) TiO
2siO
2the preparation of nucleocapsid particles:
In the middle of the small molecular alcohol solvent that is 1～4 by the ultrasonic C of being scattered in number by titanium dioxide, being prepared into concentration is the dispersion liquid that 0.1～1wt.% contains admittedly, add afterwards ammoniacal liquor as catalyst, the ratio that catalyst accounts for gross mass is 1～3wt.%, finally add tetraalkoxysilane to be coated titanium dioxide, the ratio that tetraalkoxysilane accounts for gross mass is 1～5wt.%, reaction temperature is 30～60 ℃, reaction time 2～4h, by product centrifugation, washing, oven dry, finally at 200-600 ℃, calcine 2h, obtain the titanium dioxide granule of coated with silica.
2. solar heat reflection TiO according to claim 1
2siO
2the preparation method of nucleocapsid particles, is characterized in that: any that the tetralkyl titanate the best of using is tetraethyl titanate, tetraisopropyl titanate and butyl titanate.
3. solar heat reflection TiO according to claim 1
2siO
2the preparation method of nucleocapsid particles, is characterized in that: the one or any combination that small molecular alcohol the best that the C number using is 1～4 is methyl alcohol, ethanol, isopropyl alcohol and n-butanol.
4. solar heat reflection TiO according to claim 1
2siO
2the preparation method of nucleocapsid particles, is characterized in that: any that tetraalkoxysilane the best of using is tetramethoxy-silicane, tetraethoxysilane and tetraisopropoxysilan.
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| JP2018094495A (en) * | 2016-12-12 | 2018-06-21 | 富士ゼロックス株式会社 | Titanium oxide particles and method for producing the same, composition for forming photocatalyst, photocatalyst and structure |
| JP2018094494A (en) * | 2016-12-12 | 2018-06-21 | 富士ゼロックス株式会社 | Titanium oxide particles and method for producing the same, composition for forming photocatalyst, photocatalyst and structure |
| JP2019048738A (en) * | 2017-09-08 | 2019-03-28 | 富士ゼロックス株式会社 | Titanium oxide aerogel particle, method for producing titanium oxide aerogel particle, photocatalyst-forming composition, photocatalyst and structure |
| CN110305415A (en) * | 2019-07-24 | 2019-10-08 | 金旸（厦门）新材料科技有限公司 | A kind of heat-insulated PP composite material and its prepare raw material and preparation method and application |
| CN111995895A (en) * | 2020-08-31 | 2020-11-27 | 宁波瑞凌新能源科技有限公司 | Particulate material and use thereof |
| CN112812361A (en) * | 2020-12-31 | 2021-05-18 | 浙江三时纪新材科技有限公司 | Preparation method of silicon dioxide powder filler, powder filler obtained by preparation method and application of powder filler |
| CN112978793A (en) * | 2021-03-23 | 2021-06-18 | 河南大学 | TiO22W nano-particles, preparation method and application thereof |
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| JP2018094495A (en) * | 2016-12-12 | 2018-06-21 | 富士ゼロックス株式会社 | Titanium oxide particles and method for producing the same, composition for forming photocatalyst, photocatalyst and structure |
| JP2018094494A (en) * | 2016-12-12 | 2018-06-21 | 富士ゼロックス株式会社 | Titanium oxide particles and method for producing the same, composition for forming photocatalyst, photocatalyst and structure |
| JP2019048738A (en) * | 2017-09-08 | 2019-03-28 | 富士ゼロックス株式会社 | Titanium oxide aerogel particle, method for producing titanium oxide aerogel particle, photocatalyst-forming composition, photocatalyst and structure |
| JP7077550B2 (en) | 2017-09-08 | 2022-05-31 | 富士フイルムビジネスイノベーション株式会社 | Titanium oxide airgel particles, method for producing titanium oxide airgel particles, composition for forming a photocatalyst, photocatalyst, and structure. |
| CN110305415A (en) * | 2019-07-24 | 2019-10-08 | 金旸（厦门）新材料科技有限公司 | A kind of heat-insulated PP composite material and its prepare raw material and preparation method and application |
| CN110305415B (en) * | 2019-07-24 | 2021-04-20 | 金旸（厦门）新材料科技有限公司 | Heat-insulating polypropylene composite material, and preparation raw materials, preparation method and application thereof |
| CN111995895A (en) * | 2020-08-31 | 2020-11-27 | 宁波瑞凌新能源科技有限公司 | Particulate material and use thereof |
| CN112812361A (en) * | 2020-12-31 | 2021-05-18 | 浙江三时纪新材科技有限公司 | Preparation method of silicon dioxide powder filler, powder filler obtained by preparation method and application of powder filler |
| CN112812361B (en) * | 2020-12-31 | 2024-01-09 | 浙江三时纪新材科技有限公司 | Preparation method of silicon dioxide powder filler, powder filler obtained by preparation method and application of powder filler |
| CN112978793A (en) * | 2021-03-23 | 2021-06-18 | 河南大学 | TiO22W nano-particles, preparation method and application thereof |
| CN112978793B (en) * | 2021-03-23 | 2022-03-08 | 河南大学 | TiO22W nano-particles, preparation method and application thereof |
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Application publication date: 20141008 |