CN101746818B - Preparation method of hydrophobic nano-titanium dioxide - Google Patents
Preparation method of hydrophobic nano-titanium dioxide Download PDFInfo
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- CN101746818B CN101746818B CN2008102299968A CN200810229996A CN101746818B CN 101746818 B CN101746818 B CN 101746818B CN 2008102299968 A CN2008102299968 A CN 2008102299968A CN 200810229996 A CN200810229996 A CN 200810229996A CN 101746818 B CN101746818 B CN 101746818B
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Abstract
The invention relates to a hydrophobic nano-titanium dioxide preparation method, in particular to a method for preparing hydrophobic nano-titanium dioxide through a wet process. The invention aims to provide a hydrophobic nano-titanium dioxide preparation method with weak hydrophilicity and strong dispersivity and hydrophobic capability. The preparation method comprises the following steps: nano-titanium dioxide is mixed into emulsion with 20 to 40 percent mass concentration by water; the emulsion is put into a reactor, stirred and heated to 60 to 95 DEG C; after the temperature is kept constant for 5 to 15min, first the pH value of the emulsion is regulated to 4.0 to 5.5 by hydrochloric acid solution with 10 percent concentration, hexamethyl disilazane with 5 to 25 percent content of nano-titanium dioxide is started to be slowly added in, the reflux reaction under 60 to 95 DEG C is kept for 60 to 180min; and after reaction, the emulsion is centrifuged and dewatered, is centrifuged and washed for 3 to 4 times by ethyl alcohol, and the product is obtained after drying.
Description
Technical field:
The present invention relates to a kind of preparation method of hydrophobic nano-titanium dioxide, particularly adopt wet method to prepare the method for hydrophobic nano-titanium dioxide.
Background technology:
Nano titanium oxide is a kind of important multi-usage inorganic functional material; Performance with many excellences; Be widely used in industries such as automotive industry, makeup, wastewater treatment, coating, can adopt chemical precipitation method, sol-gel method, hydrolysis method, microemulsion method, gas gel method, pure titanium salt pyrogenic silica, chemical Vapor deposition process preparation; But,, in organic medium, be difficult to homodisperse, thereby limited the application of nano titanium oxide no matter it all is hydrophilic making the nano titanium oxide how to prepare.
Titanium dioxide nanoparticle is through after the modification, and its surperficial wetting ability can change hydrophobicity into, and remarkable improvement all can take place a series of character such as its photoabsorption, current potential, wetting, dispersion, and its Application Areas will further be widened, and brings into play its excellent performance.
Summary of the invention:
The object of the present invention is to provide the preparation method of weak, the dispersed and hydrophobic nano-titanium dioxide that hydrophobic ability is strong of a kind of wetting ability.
To achieve these goals, the present invention adopts following technical scheme, and preparing method's concrete steps of the present invention are following:
It is 20～40% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle, stirs; The heating emulsion; Be warming up to 60～95 ℃, constant temperature is after 5～15 minutes, and using concentration earlier is that 10% hydrochloric acid soln transfers to 4.0～5.5 with ph value of emulsion; The hexamethyldisilazane of the slow adding of beginning nano titanium oxide consumption 5～25% or SWS-F 221, Union carbide A-162, trimethylethoxysilane, Trimethoxy silane, a chloromethyl triethoxyl silane, γ-r-chloropropyl trimethoxyl silane; Keep 60-95 ℃ of situation refluxed reaction 60～180 minutes, after reaction finishes, centrifugal the removing of emulsion anhydrated; With ethanol centrifuge washing 3～4 times, through being drying to obtain product.
Preparation of nano titanium oxide emulsion both can make water, also can use ethanol or aqueous ethanolic solution.
Beneficial effect of the present invention:
1, nano titanium oxide of the present invention is after hexamethyldisilazane or SWS-F 221, Union carbide A-162, trimethylethoxysilane, Trimethoxy silane, a chloromethyl triethoxyl silane, γ-r-chloropropyl trimethoxyl silane modification; Its wetting ability weakens, and dispersed and hydrophobic ability strengthens;
2, of the present invention nano-titanium dioxide modified even, stable, reaction efficiency is high;
3, the preparing method's of nano titanium oxide of the present invention technology is simple, is easy to realize large-scale industrial production.
Embodiment:
Embodiment 1:
It is 20% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle, stirs the heating emulsion; Be warming up to 95 ℃, constant temperature is after 5 minutes, and using concentration earlier is that 10% hydrochloric acid soln transfers to 5 with ph value of emulsion, slowly adds the hexamethyldisilazane of nano titanium oxide consumption 5%; Keep 95 ℃, back flow reaction 60 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
Embodiment 2:
It is 30% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle, stirs the heating emulsion; Be warming up to 90 ℃, constant temperature is after 10 minutes, and using concentration earlier is that 10% hydrochloric acid soln transfers to 5 with ph value of emulsion, slowly adds the SWS-F 221 of nano titanium oxide consumption 10%; Keep 90 ℃, back flow reaction 100 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
Embodiment 3:
It is 40% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle, stirs the heating emulsion; Be warming up to 85 ℃, constant temperature is after 15 minutes, and using concentration earlier is that 10% hydrochloric acid soln transfers to 4.5 with ph value of emulsion, slowly adds the Union carbide A-162 of nano titanium oxide consumption 15%; Keep 85 ℃, back flow reaction 140 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
Embodiment 4:
It is 30% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle, stirs the heating emulsion; Be warming up to 85 ℃, constant temperature is after 10 minutes, and using concentration earlier is that 10% hydrochloric acid soln transfers to 4.5 with ph value of emulsion, slowly adds the hexamethyldisilazane of nano titanium oxide consumption 15%; Keep 85 ℃, back flow reaction 100 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
Embodiment 5:
It is 40% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle, stirs the heating emulsion; Be warming up to 80 ℃, constant temperature is after 5 minutes, and using concentration earlier is that 10% hydrochloric acid soln transfers to 5.5 with ph value of emulsion, slowly adds the SWS-F 221 of nano titanium oxide consumption 20%; Keep 80 ℃, back flow reaction 140 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
Embodiment 6:
It is 25% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle, stirs the heating emulsion; Be warming up to 95 ℃, constant temperature is after 10 minutes, and using concentration earlier is that 10% hydrochloric acid soln transfers to 5.5 with ph value of emulsion, slowly adds the Union carbide A-162 of nano titanium oxide consumption 5%; Keep 95 ℃, back flow reaction 80 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
Claims (7)
1. the preparation method of a hydrophobic nano-titanium dioxide is characterized in that concrete steps are following: it is 20～40% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle; Stir, the heating emulsion is warming up to 60～95 ℃; Behind the constant temperature 5～15 minutes; Using earlier concentration is that 10% hydrochloric acid soln transfers to 4.0～5.5 with ph value of emulsion, and beginning slowly adds hexamethyldisilazane, SWS-F 221, Union carbide A-162, trimethylethoxysilane, Trimethoxy silane, a chloromethyl triethoxyl silane or a γ-r-chloropropyl trimethoxyl silane of nano titanium oxide consumption 5～25%, keeps 60-95 ℃ of situation refluxed to react 60～180 minutes; After reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
2. according to the preparation method of the said a kind of hydrophobic nano-titanium dioxide of claim 1, it is characterized in that concrete steps are following: it is 20% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle; Stir, the heating emulsion is warming up to 95 ℃; Behind the constant temperature 5 minutes, using earlier concentration is that 10% hydrochloric acid soln transfers to 5 with ph value of emulsion, slowly adds the hexamethyldisilazane of nano titanium oxide consumption 5%; Keep 95 ℃, back flow reaction 60 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
3. according to the preparation method of the said a kind of hydrophobic nano-titanium dioxide of claim 1, it is characterized in that concrete steps are following: it is 30% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle; Stir, the heating emulsion is warming up to 90 ℃; Behind the constant temperature 10 minutes, using earlier concentration is that 10% hydrochloric acid soln transfers to 5 with ph value of emulsion, slowly adds the SWS-F 221 of nano titanium oxide consumption 10%; Keep 90 ℃, back flow reaction 100 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
4. according to the preparation method of the said a kind of hydrophobic nano-titanium dioxide of claim 1, it is characterized in that concrete steps are following: it is 40% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle; Stir, the heating emulsion is warming up to 85 ℃; Behind the constant temperature 15 minutes, using earlier concentration is that 10% hydrochloric acid soln transfers to 4.5 with ph value of emulsion, slowly adds the Union carbide A-162 of nano titanium oxide consumption 15%; Keep 85 ℃, back flow reaction 140 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
5. according to the preparation method of the said a kind of hydrophobic nano-titanium dioxide of claim 1, it is characterized in that concrete steps are following: it is 30% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle; Stir, the heating emulsion is warming up to 85 ℃; Behind the constant temperature 10 minutes, using earlier concentration is that 10% hydrochloric acid soln transfers to 4.5 with ph value of emulsion, slowly adds the hexamethyldisilazane of nano titanium oxide consumption 15%; Keep 85 ℃, back flow reaction 100 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
6. according to the preparation method of the said a kind of hydrophobic nano-titanium dioxide of claim 1, it is characterized in that concrete steps are following: it is 40% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle; Stir, the heating emulsion is warming up to 80 ℃; Behind the constant temperature 5 minutes, using earlier concentration is that 10% hydrochloric acid soln transfers to 5.5 with ph value of emulsion, slowly adds the SWS-F 221 of nano titanium oxide consumption 20%; Keep 80 ℃, back flow reaction 140 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
7. according to the preparation method of the said a kind of hydrophobic nano-titanium dioxide of claim 1, it is characterized in that concrete steps are following: it is 25% emulsion that the nano titanium oxide water is modulated into mass concentration, places reaction kettle; Stir, the heating emulsion is warming up to 95 ℃; Behind the constant temperature 10 minutes, using earlier concentration is that 10% hydrochloric acid soln transfers to 5.5 with ph value of emulsion, slowly adds the Union carbide A-162 of nano titanium oxide consumption 5%; Keep 95 ℃, back flow reaction 80 minutes is after reaction finishes; Centrifugal remove of emulsion anhydrated, with ethanol centrifuge washing 3～4 times, through being drying to obtain product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102010000B (en) * | 2010-10-25 | 2014-07-16 | 江苏考普乐新材料有限公司 | Nano titanium dioxide and preparation method thereof |
| CN102516828A (en) * | 2011-12-19 | 2012-06-27 | 西南科技大学 | Preparation method of hydrophobic aluminum chromium phosphate |
| CN102675927A (en) * | 2012-05-10 | 2012-09-19 | 西南科技大学 | Preparation method of hydrophobic aluminum phosphate |
| CN102732066A (en) * | 2012-06-07 | 2012-10-17 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium dioxide modification method |
| CN107839606A (en) * | 2017-11-08 | 2018-03-27 | 信利光电股份有限公司 | A kind of system and rearview mirror for removing body surface water smoke |
| CN107901832A (en) * | 2017-11-08 | 2018-04-13 | 信利光电股份有限公司 | A kind of system and rearview mirror for removing body surface water mist |
| CN108485329A (en) * | 2018-05-05 | 2018-09-04 | 泉州三欣新材料科技有限公司 | A kind of super-hydrophilic self-cleaning coating sol and its preparation and application |
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| CN101076313A (en) * | 2004-12-13 | 2007-11-21 | 株式会社资生堂 | Modified powder and cosmetic composition using same |
| CN101186764A (en) * | 2006-11-23 | 2008-05-28 | 德古萨股份公司 | Hydrophobic titanium oxide fine powder and its producing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101076313A (en) * | 2004-12-13 | 2007-11-21 | 株式会社资生堂 | Modified powder and cosmetic composition using same |
| CN101186764A (en) * | 2006-11-23 | 2008-05-28 | 德古萨股份公司 | Hydrophobic titanium oxide fine powder and its producing method |
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