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Stable graphene/titanium oxide composite nanosol and preparation method thereof

A nano-sol, graphene solution technology, applied in chemical instruments and methods, physical/chemical process catalysts, photosensitive equipment, etc., can solve the problem that graphene sol cannot exist stably for a long time, cannot prepare transparent films, and cannot adapt to coating processes. and other problems, to achieve the effect of promoting separation, good transparency, and improved photocurrent intensity

Active Publication Date: 2014-06-18
CHINA NAT OFFSHORE OIL CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the composite material of titanium oxide / graphene is mainly powder, and most of them need to be processed at high temperature or high pressure, which greatly limits the use of this composite material
Through literature search, it is found that in the invention patent with the patent number 201010237588.4, the compound prepared by using a reactor is in the form of slurry or powder, and a transparent film cannot be prepared; in the invention patent with the patent number 200910196534.5, the graphene-based Titanium dioxide composite photocatalyst, the obtained catalyst is also in powder state; the Chinese invention patent application number is 201110228170.1 invention patent, although the composite catalyst exists in the form of sol, but the titanium oxide used is P25 titanium oxide, and its particle size is above 30nm , according to the pH value of its solution, this titanium oxide graphene sol cannot exist stably for a long time, nor can it be adapted to industrial large-scale coating process

Method used

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  • Stable graphene/titanium oxide composite nanosol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) 3.125 mg graphene oxide was dissolved in 150 ml water to obtain a graphene oxide aqueous solution with a concentration of 0.0208 mg / ml; hydrochloric acid was added to adjust the pH value of the graphene aqueous solution to 1;

[0027] 2) Take 1ml of n-tetrabutyl titanate and 1.5ml of isopropanol, shake and mix well;

[0028] 3) Stir the graphene oxide aqueous solution on a magnetic stirrer, slowly drop the mixed solution of tetra-n-butyl titanate and isopropanol along the opposite direction of stirring with a dropper, and the dropping speed is 1ml / min;

[0029] 4) Stir and heat the mixed solution in a water bath and condense and reflux. The temperature of the water bath is kept at 80° C., and the condensing and reflux time is 24 hours;

[0030] 5) Add 9.37 μl of hydrazine to the sol after condensation and reflux, and keep stirring in a water bath at 95°C for 12 hours;

[0031] 6) Sonicate the stirred sol for 1 hour (200W) and then perform dialysis treatment in water...

Embodiment 2

[0035] 1) 6.25 mg graphene oxide was dissolved in 150 ml water to obtain a graphene oxide aqueous solution with a concentration of 0.0416 mg / ml; hydrochloric acid was added to adjust the pH value of the graphene aqueous solution to 1;

[0036] 2) Take 1ml of n-tetrabutyl titanate and 1.5ml of isopropanol, shake and mix well;

[0037] 3) Stir the graphene oxide aqueous solution on a magnetic stirrer, slowly drop the mixed solution of tetra-n-butyl titanate and isopropanol along the opposite direction of stirring with a dropper, and the dropping speed is 1ml / min;

[0038] 4) Stir and heat the mixed solution in a water bath and condense and reflux. The temperature of the water bath is kept at 80 degrees, and the condensing and reflux time is 24 hours;

[0039] 5) Add 18.74 μl of hydrazine to the sol after condensation and reflux, and keep stirring in a 95-degree water bath for 12 hours;

[0040]6) Sonicate the stirred sol for 1 hour (200W) and then perform dialysis treatment in ...

Embodiment 3

[0044] 1) 3.125 mg graphene oxide was dissolved in 150 ml water to obtain a graphene oxide aqueous solution with a concentration of 0.0208 mg / ml; hydrochloric acid was added to adjust the pH value of the graphene aqueous solution to 1;

[0045] 2) Take 1ml of n-tetrabutyl titanate and 1.5ml of isopropanol, shake and mix well;

[0046] 3) Stir the graphene oxide aqueous solution on a magnetic stirrer, slowly drop the mixed solution of tetra-n-butyl titanate and isopropanol along the opposite direction of stirring with a dropper, and the dropping speed is 1ml / min;

[0047] 4) Stir and heat the mixed solution in a water bath and condense and reflux. The temperature of the water bath is kept at 80 degrees, and the condensing and reflux time is 24 hours;

[0048] 5) Add 9.37 μl of hydrazine to the sol after condensation and reflux, and keep stirring in an oil bath at 150 degrees for 5 hours;

[0049] 6) The stirred sol was ultrasonicated for 1 hour (250W) and then dialyzed in wate...

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Abstract

The invention discloses a graphene / titanium oxide composite nanosol and a preparation method thereof. The preparation method comprises the following steps: 1) dissolving graphene oxide in a solvent to obtain a graphene oxide solution, and regulating the pH value with acid; 2) adding a mixed liquid of tetra-n-butyl titanate and isopropanol into the graphene oxide solution obtained in the step 1), and carrying out condensation reflux on the mixture to obtain a sol; 3) adding a reducer into the sol to carry out the reaction; and after the reaction finishes, sequentially carrying out ultrasonic treatment and dialytic purifying treatment to obtain the graphene / titanium oxide composite nanosol. The titanium oxide particles in the composite nano sol are very small; the sol can stably exist for a long time by regulating the pH value; and a transparent titanium oxide / graphene composite functional film can be prepared on various substrates by spin coating, spray coating, roller coating and drip coating.

Description

technical field [0001] The invention relates to a stable graphene / titanium oxide composite nano-sol and a preparation method thereof. Background technique [0002] Solar energy has attracted more and more attention because of its clean, renewable and safe features. Photocatalysis technology is a new technology for energy conversion using solar energy, and improving the conversion efficiency of photocatalysis is the top priority to promote the wide application of this technology. Titanium oxide has always been concerned by the field of photocatalysis due to its non-toxic, stable, high storage capacity and low price. Transparent titanium oxide films coated on glass or plastic substrates have been successfully used as functional films in anti-fog, anti-bacteria, anti-mildew, self-cleaning and other fields. Under light conditions, titanium oxide in the film generates photogenerated electrons and holes, and the state change of Ti atoms makes the film change from hydrophobic to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/18H01G9/04H01G9/20H01M14/00
Inventor 高寒阳苏佳纯上官文峰孙洋洲
Owner CHINA NAT OFFSHORE OIL CORP