CN107746621A - A kind of preparation method of nanometer of Ti-Si composite oxide - Google Patents
A kind of preparation method of nanometer of Ti-Si composite oxide Download PDFInfo
- Publication number
- CN107746621A CN107746621A CN201711249866.6A CN201711249866A CN107746621A CN 107746621 A CN107746621 A CN 107746621A CN 201711249866 A CN201711249866 A CN 201711249866A CN 107746621 A CN107746621 A CN 107746621A
- Authority
- CN
- China
- Prior art keywords
- composite oxide
- preparation
- nanometer
- aged
- titanium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1687—Use of special additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
- Cosmetics (AREA)
- Catalysts (AREA)
Abstract
The preparation method of nanometer Ti-Si composite oxide of the present invention, belongs to field of material preparation, it is characterised in that：Take tetraethyl orthosilicate to be added under agitation in absolute ethyl alcohol, then add salpeter solution, adjust pH, be aged at room temperature after being sufficiently stirred；Separately take isopropyl titanate to be added under agitation in absolute ethyl alcohol, then add ammoniacal liquor and acetylacetone,2,4-pentanedione, adjust solution pH be sufficiently stirred after be aged at room temperature；Silicon dioxide gel is added dropwise in TiO 2 sol, continues stirring and then is ultrasonically treated ageing, titanium silica aerogel is made；Calcined being placed in after prepared titanium silica aerogel vacuum drying in Muffle furnace, ground after cooling and obtain titanium silicon nano composite oxide.Easily realize large-scale production, build with receive differential Rotating fields external wall decorative material finish paint in terms of with potential application prospect, be remarkably improved heat endurance, weatherability, resistance to soiling and the self-cleaning performance of skin ornament materials.
Description
Technical field
The invention belongs to field of material preparation, more particularly to the preparation method of a kind of nanometer of Ti-Si composite oxide.
Background technology
In recent years, it is in all parts of the country to report that " the ceramic tile rain " of high-altitude building falling pounds the accident that car is hurted sb.'s feelings, serious threat city repeatedly
The personal safety of resident.Since 1997, some provinces and cities launch respectively relevant regulations, disable stone materials external wall face brick, because
This, the multifunctional exterior wall ornament materials that exploitation has strong good decorative property, automatical cleaning ability, good weatherability, cost low is increasingly becoming
The study hotspot in the field.But the exterior coating of domestic production has the defects of ornamental and weatherability difference, do not possess certainly yet
Cleaning function, it is difficult to really substitute stone materials external wall decorative material.And want to prepare with automatical cleaning ability, good weatherability it is outer
Wall decoration material, the preparation of super-hydrophobic surface coating is crucial.At present, the main method for preparing super hydrophobic surface is that first structure has
There is the surface of micro-nano layering coarse structure, modifying super hydrophobicity is then carried out to surface using low-surface energy substance.Build micro-nano point
The conventional inorganic nano material of layer coarse structure includes zinc oxide, titanium dioxide, silica etc..
Nano titanium oxide mainly has two kinds of crystal habits of Detitanium-ore-type and rutile-type, wherein anatase titanium dioxide
Because being widely used in the fields such as photocatalysis and photoelectric sensor with excellent photocatalysis and heat endurance, and rutile-type dioxy
Change titanium because being applied to the fields such as building coating, aeronautical material, desalinization with higher heat endurance and weatherability.But
It is, need to be by adulterating dioxy because titanium dioxide powder has the defects of specific surface area is small, surface duct is few, bad mechanical strength
The preparations such as SiClx have the composite oxide material of low-density, high-specific surface area and high porosity, for heterogeneous catalysis, insulation
In the fields such as material, sensor, drug delivery, heavy metal adsorption.
The content of the invention
The present invention is intended to provide the preparation method of a kind of nanometer of Ti-Si composite oxide.
The preparation method of nanometer Ti-Si composite oxide of the present invention, comprises the following steps：（1）Take the positive silicic acid of 10ml
Ethyl ester is added in 80ml absolute ethyl alcohols under agitation, then adds 20ml salpeter solutions, is adjusted pH=2-3, is sufficiently stirred rear chamber
Temperature is lower to be aged；（2）Separately take 5 ml isopropyl titanates to be added under agitation in 120ml absolute ethyl alcohols, then add 1.2ml ammoniacal liquor
With 2.0ml acetylacetone,2,4-pentanediones, pH=8-9 of solution is adjusted, is aged at room temperature after being sufficiently stirred；（3）Silicon dioxide gel is added dropwise
Enter in TiO 2 sol, continue to stir 30min, be then ultrasonically treated 60min, be aged 24h, titanium silica aerogel is made；（4）Will
After prepared titanium silica aerogel is dried in vacuo 36h at 60 DEG C, it is placed in Muffle furnace and calcines 4h, is ground after cooling and obtain titanium silicon
Nano composite oxide.
The preparation method of nanometer Ti-Si composite oxide of the present invention, step（1）The mixing time is 30min.
The preparation method of nanometer Ti-Si composite oxide of the present invention, step（1）The digestion time is 36-48h.
The preparation method of nanometer Ti-Si composite oxide of the present invention, step（2）The mixing time is 35min.
The preparation method of nanometer Ti-Si composite oxide of the present invention, step（2）The digestion time is 24h.
The preparation method of nanometer Ti-Si composite oxide of the present invention, step（4）The Muffle furnace calcining heat is
1000-1200℃。
The preparation method of nanometer Ti-Si composite oxide of the present invention, by improved sol-gel process because having
The advantages that technique is simple, reaction condition is gentle, controllability is strong, easily realizes large-scale production, has in structure and receives differential Rotating fields
External wall decorative material finish paint in terms of there is potential application prospect, be remarkably improved skin ornament materials heat surely
Qualitative, weatherability, resistance to soiling and self-cleaning performance.
Embodiment
The preparation method of nanometer Ti-Si composite oxide of the present invention, comprises the following steps：（1）Take the positive silicic acid of 10ml
Ethyl ester is added in 80ml absolute ethyl alcohols under agitation, then adds 20ml salpeter solutions, is adjusted pH=2-3, is sufficiently stirred rear chamber
Temperature is lower to be aged；（2）Separately take 5 ml isopropyl titanates to be added under agitation in 120ml absolute ethyl alcohols, then add 1.2ml ammoniacal liquor
With 2.0ml acetylacetone,2,4-pentanediones, pH=8-9 of solution is adjusted, is aged at room temperature after being sufficiently stirred；（3）Silicon dioxide gel is added dropwise
Enter in TiO 2 sol, continue to stir 30min, be then ultrasonically treated 60min, be aged 24h, titanium silica aerogel is made；（4）Will
After prepared titanium silica aerogel is dried in vacuo 36h at 60 DEG C, it is placed in Muffle furnace and calcines 4h, is ground after cooling and obtain titanium silicon
Nano composite oxide.
The preparation method of nanometer Ti-Si composite oxide of the present invention, step（1）The mixing time is 30min.
Step（1）The digestion time is 36-48h.
The preparation method of nanometer Ti-Si composite oxide of the present invention, step（2）The mixing time is 35min.
Step（2）The digestion time is 24h.
The preparation method of nanometer Ti-Si composite oxide of the present invention, step（4）The Muffle furnace calcining heat is
1000-1200℃.Obtained rutile type titanium nano silicon particles are scattered in the mixing of n-hexane and TMCS mass fractions 8.0%
In liquid, after reacting at room temperature 6h, nano particle is rinsed 2-3 times with appropriate n-hexane, 12 h of last 60 DEG C of vacuum drying, is changed
Property rutile type titanium silicon nanometer complex oxide material, by water contact angle measurement its hydrophobic performance is tested.Work as titanium
Silicon ratio is 3:When 1, the crystal formation of titanium dioxide is based on anatase in 1000 DEG C of calcined products.When temperature is increased to 1100 DEG C,
Belonging to the diffraction maximum of the crystal face of anatase titanium dioxide significantly reduces, and belongs to the crystalline substance of rutile titanium dioxide at 27.4 °
Face diffraction maximum drastically strengthens, and illustrates that raising temperature reduces Detitanium-ore-type, rutile-type increase；It is continuously heating to 1200 DEG C, it is sharp
The characteristic diffraction peak of titanium ore type is very weak, and the characteristic diffraction peak of rutile-type is very strong, illustrates that now calcined product is with golden red
Based on stone-type, but still with the presence of a small amount of Detitanium-ore-type.After 1000 DEG C of calcinings, although the rutile-type in product slightly increases
Add, but still based on anatase；At 1100 DEG C, the diffraction maximum of rutile-type drastically strengthens, only a small amount of Detitanium-ore-type
In the presence of；At 1200 DEG C, Detitanium-ore-type almost disappears.With the increase of titanium silicon mol ratio, the reduction of dioxide-containing silica, anatase
The high-temperature stability of type titanium dioxide is deteriorated, and is partly gradually converted into rutile titanium dioxide, this is due to silica
The influence that steric hindrance acts on to the size of titania weakens, according to critical dimension effect, the grain of titanium dioxide granule
Footpath is bigger, and this crystal transfer temperature is lower, that is, overcomes anatase titanium dioxide-rutile titanium dioxide crystal transfer
Energy barrier reduces.In addition, with the increase of calcining heat, the bad stability of anatase titanium dioxide, progressively it is changed into
Rutile titanium dioxide.When calcining heat reaches 1100 DEG C, the Detitanium-ore-type titanium dioxide in Ti-Si composite oxide powder
Titanium is completely reformed into rutile titanium dioxide, and now, the stability of Ti-Si composite oxide is best.Therefore, titanium silicon is selected to rub
You are than being 5:1 composite aerogel is in 1100 DEG C of calcination processings as the optimal preparation for preparing rutile-type Ti-Si composite oxide
Condition.
The aeroge being dried to obtain at a temperature of 60 DEG C is the loose spherical nanoparticle of internal structure, has and preferably divides
Property is dissipated, because constant pressure and dry process can reduce the pore blockage effect of sample, forms orderly porous network structure；1100
DEG C calcining after, form rutile type nano Ti-Si composite oxide, with the increase of calcining heat, the agglomeration of sample is tight
Weight, sample particle are changed into dense packing, and the specific surface area and pore volume of sample reduce；TMCS is modified, is grown because surface introduces
Hydrophobic grouping-CH3 of chain, not only reduces surface hydrophilic group-OH number, while makes a nanometer Ti-Si composite oxide table
Face forms a kind of smooth, orderly micro-nano network structure, and this is the master that titanium silicon nano composite oxide surface possesses super-hydrophobicity
Want reason.Water contact angle is the important parameter for characterizing material hydrophobic performance, and so-called super hydrophobic surface refers to the contact with water
Angle is more than 150 ° of surface.Aeroge has certain hydrophily, but its hydrophily is not strong after 60 DEG C are dried.From FTIR light
Spectrum sees that, although there is a large amount of-OH on 60 DEG C of dried aeroge surfaces, the product specific surface area of generation is big, has mesoporous nano
Structure, cause water to its surface wet relative difficulty；The micro-nano structure of the nano composite oxide generated after 1100 DEG C of calcinings is more
It is regular, drastically reduced plus surface-OH, its hydrophily is further reduced；TMCS is modified, due to surface residual-OH
Almost substituted completely by-CH3, contact angle is significantly increased as 154.7 °, presents excellent ultra-hydrophobicity.
Claims (6)
1. the preparation method of a kind of nanometer of Ti-Si composite oxide, it is characterised in that comprise the following steps：（1）Take the positive silicic acid of 10ml
Ethyl ester is added in 80ml absolute ethyl alcohols under agitation, then adds 20ml salpeter solutions, is adjusted pH=2-3, is sufficiently stirred rear chamber
Temperature is lower to be aged；（2）Separately take 5 ml isopropyl titanates to be added under agitation in 120ml absolute ethyl alcohols, then add 1.2ml ammoniacal liquor
With 2.0ml acetylacetone,2,4-pentanediones, pH=8-9 of solution is adjusted, is aged at room temperature after being sufficiently stirred；（3）Silicon dioxide gel is added dropwise
Enter in TiO 2 sol, continue to stir 30min, be then ultrasonically treated 60min, be aged 24h, titanium silica aerogel is made；（4）Will
After prepared titanium silica aerogel is dried in vacuo 36h at 60 DEG C, it is placed in Muffle furnace and calcines 4h, is ground after cooling and obtain titanium silicon
Nano composite oxide.
2. the preparation method of according to claim 1 nanometer of Ti-Si composite oxide, it is characterised in that：Step（1）It is described
Mixing time is 30min.
3. the preparation method of according to claim 2 nanometer of Ti-Si composite oxide, it is characterised in that：Step（1）It is described
Digestion time is 36-48h.
4. the preparation method of according to claim 3 nanometer of Ti-Si composite oxide, it is characterised in that：Step（2）It is described
Mixing time is 35min.
5. the preparation method of according to claim 4 nanometer of Ti-Si composite oxide, it is characterised in that：Step（2）It is described
Digestion time is 24h.
6. the preparation method of according to claim 5 nanometer of Ti-Si composite oxide, it is characterised in that：Step（4）It is described
Muffle furnace calcining heat is 1000-1200 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711249866.6A CN107746621A (en) | 2017-12-01 | 2017-12-01 | A kind of preparation method of nanometer of Ti-Si composite oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711249866.6A CN107746621A (en) | 2017-12-01 | 2017-12-01 | A kind of preparation method of nanometer of Ti-Si composite oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107746621A true CN107746621A (en) | 2018-03-02 |
Family
ID=61250002
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711249866.6A Withdrawn CN107746621A (en) | 2017-12-01 | 2017-12-01 | A kind of preparation method of nanometer of Ti-Si composite oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107746621A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810598A (en) * | 2019-01-11 | 2019-05-28 | 深圳市欧科力科技有限公司 | A kind of preparation method of the antifouling building coating of low-surface-energy |
| CN111875996A (en) * | 2020-07-28 | 2020-11-03 | 几何智慧城市科技(广州)有限公司 | Super-hydrophobic coating capable of self-cleaning and degrading organic pollutants and preparation method thereof |
-
2017
- 2017-12-01 CN CN201711249866.6A patent/CN107746621A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810598A (en) * | 2019-01-11 | 2019-05-28 | 深圳市欧科力科技有限公司 | A kind of preparation method of the antifouling building coating of low-surface-energy |
| CN111875996A (en) * | 2020-07-28 | 2020-11-03 | 几何智慧城市科技(广州)有限公司 | Super-hydrophobic coating capable of self-cleaning and degrading organic pollutants and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101134586B (en) | Method for preparing nano alumina hollow ball | |
| CN104046117B (en) | Titanium dioxide/cenosphere composite particles, sunlight reflective insulation filler, coating and preparation method thereof | |
| CN107163855B (en) | A kind of silica aerogel reflective insulation exterior wall paint and preparation method thereof | |
| CN103861574B (en) | A kind of preparation method of Ti-Si composite oxide | |
| CN107185515B (en) | A kind of photochemical catalyst and preparation method thereof for sewage disposal | |
| CN105129805B (en) | Preparation method of silicon oxide/tin antimony oxide/zinc oxide ternary composite material | |
| CN100510171C (en) | Preparation method of carbon coated TiO* core-shell composite nanometer powder | |
| CN107163294A (en) | A kind of far infrared composite powder | |
| CN102613245B (en) | Preparation method of nano-silica aerogels | |
| CN104785349A (en) | Efficient preparation method for nano-scale solid powder | |
| CN103730259B (en) | A kind of nanocrystalline titanium dioxide film of two-specification pore structure and manufacturing method of nanocrystalline titanium dioxide film and preparation method thereof | |
| CN101786900B (en) | Preparation method of quaternary xerogel | |
| CN105217676B (en) | Titania aerogel with nanometer sheet and nano-porous structure and preparation method thereof | |
| CN105036186B (en) | A kind of nano titanium oxide | |
| CN106732724A (en) | A kind of N doping TiO2The preparation method of hollow nano-material | |
| CN107746621A (en) | A kind of preparation method of nanometer of Ti-Si composite oxide | |
| CN110357117B (en) | Spherical zirconium silicate powder and preparation method and application thereof | |
| CN108658130A (en) | A method of preparing iron oxide and aerosil simultaneously from iron tailings | |
| CN102718256A (en) | Preparation method for titania microspheres with adjustable grain sizes | |
| CN104925816A (en) | Titanium dioxide modified rod-shaped silicon dioxide nuclear shell material and preparation method thereof | |
| CN105668622B (en) | A kind of method of gas phase atomic deposition titanium dioxide coating | |
| CN101565296B (en) | Method for preparing hydrophobic SiO<2>-TiO<2>-ZrO<2> xerogel | |
| CN103408330B (en) | Adopt the method that Alumina gel is modified ceramic surface | |
| JP4631013B2 (en) | Acicular titanium oxide fine particles, production method thereof and use thereof | |
| CN103657586A (en) | Preparation method of novel SiO2-coated TiO2 material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180302 |