CN105295457A - Preparation method of carbon nano-tube loaded titanium dioxide top facing coating material - Google Patents
Preparation method of carbon nano-tube loaded titanium dioxide top facing coating material Download PDFInfo
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Abstract
The invention relates to a preparation method of a carbon nano-tube loaded titanium dioxide top facing coating material. The preparation method comprises the following steps: (1) dispersing a titanium source and ethanol in a dispersion container, adding ammonia water to be dispersed, after the ammonia gas is completely volatilized, centrifuging, collecting precipitates, and drying the precipitates for standby application; (2) sequentially adding water and hydrogen peroxide into the dispersion container, increasing the temperature, separately adding the precipitates prepared in the step (1) in two steps, dispersing, adding ammonia water and carbon nano-tubes, facilitating the reaction, ultrasonically dispersing, standing, and after the ammonia gas is completely volatilized, obtaining the carbon nano-tube loaded titanium dioxide top facing coating material. By adopting the preparation method, the weaknesses that the carbon nano-tube loaded titanium dioxide catalyst prepared in the prior art cannot be directly applied to the outer wall top facing can be overcome. The preparation method has advantage that the prepared carbon nano-tube loaded titanium dioxide top facing coating material can be applied to and can be directly used for the outer wall top facing.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide loaded on carbon nano tube overlay coating, be applied in paint field.
Background technology
Within the scope of uv-absorbing, titanium dioxide has photocatalytic activity, its principle is that titanium dioxide will be had an electronics from valence to conduction band during optical radiation, in valence band, produce a hole simultaneously, the hole of such generation is good oxygenant, most photocatalyst is all the oxidation capacity that make use of hole, and the electronics moving to photocatalyst surface is good reductive agent.Photocatalyst is used in coating, utilizes its redox ability, the pollution organic gas in degradable air.
Although photocatalysis titanium dioxide TiO2 have reaction conditions gentleness, degraded completely, the advantage such as non-secondary pollution, in Application Areas, still have larger space to be improved.As, ordinary light photocatalytic titanium dioxide will produce being separated of electronics and hole after ultraviolet excitation, but wherein the overwhelming majority light induced electron before migrating to catalyst surface all with hole again compound, the UV energy absorbed then loses in the mode of heat or fluorescence, therefore causes the photocatalysis efficiency of titanium dioxide low.
Carbon nanotube (CNT) is monodimension nanometer material, because of the mechanics of its excellence, electricity and chemical property, adds its special chemical structure, more and more extensive in the application of every field these years.Carbon nanotube has that unique hollow structure, specific surface area are large, high adsorption capacity, and be desirable support of the catalyst, the compound of carbon nanotube and titanium dioxide can make the absorption region of titanium dioxide produce blue shift, improves its photo-catalysis capability.
Although also there is the preparation method of catalyst for titanium dioxide loaded on carbon nano tube in prior art, as 200910184188.9 and 201310584415.3, what it adopted the dissolution mechanism of carbon nanotube is nitric acid dissolve method, the product catalyst for titanium dioxide loaded on carbon nano tube produced by the method is in acid, when it is as the cover of lacquer painting, its acidity can destroy original lacquer painting, is therefore not suitable as cover and uses.In addition, end product prepared in existing preparation technology is solid state powder, and it directly can not spread upon lacquer painting surface and use as coating, is mainly used in the process of sewage aspect, and is not suitable for the process of organic pollutant.
Therefore provide a kind of preparation method that can directly apply to the titanium dioxide loaded on carbon nano tube overlay coating of exterior wall cover oneself become when business urgently.
Summary of the invention
The invention provides a kind of preparation method of titanium dioxide loaded on carbon nano tube overlay coating, which overcome the shortcoming that catalyst for titanium dioxide loaded on carbon nano tube prepared by existing technique cannot directly apply to exterior wall cover, have and can be applicable to and the advantage that exterior wall cover carries out constructing can be directly used in.
Technical scheme of the present invention is as follows:
A preparation method for titanium dioxide loaded on carbon nano tube overlay coating, it comprises the following steps: be weight part below,
(1) 15-18 part titanium source and 63-66 part ethanol are joined in dispersion cup, 8-12min is disperseed under the rotating speed of 350-550rpm, then under the rotating speed of 350-550rpm, add 17-21 part ammoniacal liquor, adjustment rotating speed is to 800-1200rpm, and dispersion 25-35min, after ammonia volatilizees completely, centrifuging and taking throw out, is dried stand-by;
(2) rotating speed is adjusted to 350-550rpm, 44-52 part water and 25-32 part hydrogen peroxide is added successively in dispersion cup, improve temperature to 50-65 DEG C, the throw out that the step (1) adding 7-10 part obtains adds for more than 2 times by dividing, disperse 0.5-2h afterwards, add 7-10 part ammoniacal liquor and 3-8 part carbon nanotube, 0.5-1.5h is reacted under the rotating speed of 350-550rpm, ultrasonic disperse 25-35min, leave standstill afterwards, after ammonia volatilizees completely, obtain titanium dioxide loaded on carbon nano tube overlay coating;
Wherein, described titanium source is titanium tetrachloride or tetrabutyl titanate.
In general, carbon nanotube is substantially water-fast.What the application adopted is excessive ammonia and ultrasonic mode dissolved carbon nanotube.There is a large amount of carboxyls and hydroxyl in the surface of carbon nanotube, the hydroxyl produced in the process of titanium dioxide is being formed with titanium source, should make carbon nanotube loaded on titanium dioxide by the hydrogen bond action continuation physical adsorption between amino-hydroxy, hydroxyl-hydroxyl between the two, and its chemical structure did not change.Therefore, the mode to the acid dissolve that the dissolving of carbon nanotube adopts in existing preparation technology is instead of in the technique of the application, make the titanium dioxide loaded on carbon nano tube overlay coating prepared by the application to be directly used in lacquer painting, and meeting can not be caused brokenly to lacquer painting.Simultaneously because prepared titanium dioxide loaded on carbon nano tube overlay coating is liquid, therefore lacquer painting can be directly applied in as overlay coating, it uses the solid-state photocatalysis titanium dioxide prepared by more existing technique to use convenient, quick, is more applicable for the degraded of organic contamination air.
The preparation method of described titanium dioxide loaded on carbon nano tube overlay coating, it comprises the following steps: be weight part below,
(1) 16 parts of titanium sources and 65 parts of ethanol are joined in dispersion cup, under the rotating speed of 450rpm, disperse 10min, then under the rotating speed of 450rpm, add 19 parts of ammoniacal liquor, adjustment rotating speed, to 1200rpm, disperses 35min, after ammonia volatilizees completely, centrifuging and taking throw out, is dried stand-by;
(2) rotating speed is adjusted to 550rpm, 48 parts of water and 32 parts of hydrogen peroxide are added successively in dispersion cup, improve temperature to 65 DEG C, the throw out that the step (1) adding 10 parts obtains adds for more than 2 times by dividing, and disperses 1h afterwards, add 7 parts of ammoniacal liquor and 3 parts of carbon nanotubes, under the rotating speed of 550rpm, react 1h, ultrasonic disperse 30min, leaves standstill afterwards, after ammonia volatilizees completely, obtain titanium dioxide loaded on carbon nano tube overlay coating.
In the preparation method of this preferred titanium dioxide loaded on carbon nano tube overlay coating, preferred parameter in the optimum ratio of titanium source, carbon nanotube, all kinds of SOLVENTS and preparation technology, the titanium dioxide loaded on carbon nano tube overlay coating that it is prepared not only has the adsorptive power to organic pollutant being better than other titanium dioxide loaded on carbon nano tube overlay coatings, also make it have better catalytic capability simultaneously, higher to the efficiency of the degraded of organic pollutant.
In described step (2), the throw out equal portions that step (1) obtains are divided 2 times to add.
Described carbon nanotube is adopted as multi-walled carbon nano-tubes.Carbon nanotube can be divided into Single Walled Carbon Nanotube (SWCNT) and multi-walled carbon nano-tubes (MWCNT), comparatively speaking, multi-walled carbon nano-tubes is more active than Single Walled Carbon Nanotube, reason is that multi-wall carbon nano-tube tube-surface exists a large amount of active groups, as carboxyl, hydroxyl etc. and certain chemical imperfection.It is stronger than Single Walled Carbon Nanotube adsorptive power that its chemical structure determines multi-walled carbon nano-tubes.Therefore, the adsorptive power of the catalyst for titanium dioxide loaded on carbon nano tube adopting multi-walled carbon nano-tubes to prepare as raw material is stronger, effectively can improve the degradation capability to organic pollutant.
Compared with prior art, the present patent application has the following advantages:
1) improve the preparation method that tradition uses acid dissolve carbon nanotube, the destruction of lacquer painting can not be caused, make product directly can be used in lacquer painting, and destruction can not be produced to it;
2) end product is solution, can directly be applied in lacquer painting as overlay coating, convenient to use;
3) degraded of organic pollutant is more applicable for compared with the catalyst for titanium dioxide loaded on carbon nano tube of solid state;
4) adsorptive power of the titanium dioxide loaded on carbon nano tube overlay coating prepared by is stronger, effectively can improve the degradation capability to organic pollutant.
Embodiment
Below in conjunction with each embodiment, technical scheme of the present invention is described in detail.
Raw material sources:
Water: ordinary tap water;
Carbon nanotube, multi-walled carbon nano-tubes: Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences produces;
Ethanol: 75% industrial spirit;
Titanium tetrachloride, tetrabutyl titanate: Aladdin is produced, analytical pure;
Chitosan: season aminated chitosan;
Ammoniacal liquor: Xilong Chemical Co., Ltd produces, analytical pure;
Hydrogen peroxide: Xilong Chemical Co., Ltd produces, and analytical pure, content is 30%.
Embodiment 1
The preparation method of a kind of titanium dioxide loaded on carbon nano tube overlay coating of the present invention, it comprises the following steps: be weight part below,
(1) 16 parts of titanium tetrachlorides and 65 parts of ethanol are joined in dispersion cup, 10min is disperseed under the rotating speed of 450rpm, then under the rotating speed of 450rpm, add 19 parts of ammoniacal liquor, adjustment rotating speed is to 1200rpm, and dispersion 35min, after ammonia volatilizees completely, centrifuging and taking throw out, is dried stand-by;
(2) rotating speed is adjusted to 550rpm, 48 parts of water and 32 parts of hydrogen peroxide are added successively in dispersion cup, improve temperature to 65 DEG C, the throw out that the step (1) adding 10 parts obtains divides 2 times by equal portions and adds, disperse 1h afterwards, add 7 parts of ammoniacal liquor and 3 parts of multi-walled carbon nano-tubes, under the rotating speed of 550rpm, react 1h, ultrasonic disperse 30min, leaves standstill afterwards, after ammonia volatilizees completely, obtain titanium dioxide loaded on carbon nano tube overlay coating.
Embodiment 2
The preparation method of a kind of titanium dioxide loaded on carbon nano tube overlay coating of the present invention, it comprises the following steps: be weight part below,
(1) 18 parts of tetrabutyl titanates and 63 parts of ethanol are joined in dispersion cup, 8min is disperseed under the rotating speed of 550rpm, then under the rotating speed of 350rpm, add 21 parts of ammoniacal liquor, adjustment rotating speed is to 800rpm, and dispersion 25min, after ammonia volatilizees completely, centrifuging and taking throw out, is dried stand-by;
(2) rotating speed is adjusted to 350rpm, 52 parts of water and 25 parts of hydrogen peroxide are added successively in dispersion cup, improve temperature to 50 DEG C, the throw out that the step (1) adding 7 parts obtains adds for 3 times by dividing, and disperses 0.5h afterwards, add 10 parts of ammoniacal liquor and 4 parts of carbon nanotubes, under the rotating speed of 350rpm, react 1.5h, ultrasonic disperse 25min, leaves standstill afterwards, after ammonia volatilizees completely, obtain titanium dioxide loaded on carbon nano tube overlay coating.
Embodiment 3
The preparation method of a kind of titanium dioxide loaded on carbon nano tube overlay coating of the present invention, it comprises the following steps: be weight part below,
(1) 15 parts of titanium tetrachlorides and 66 parts of ethanol are joined in dispersion cup, 12min is disperseed under the rotating speed of 350rpm, then under the rotating speed of 550rpm, add 17 parts of ammoniacal liquor, adjustment rotating speed is to 1000rpm, and dispersion 30min, after ammonia volatilizees completely, centrifuging and taking throw out, is dried stand-by;
(2) rotating speed is adjusted to 450rpm, 44 parts of water and 31 parts of hydrogen peroxide are added successively in dispersion cup, improve temperature to 60 DEG C, the throw out that the step (1) adding 8 parts obtains adds for 4 times by dividing, and disperses 2h afterwards, add 9 parts of ammoniacal liquor and 8 parts of carbon nanotubes, under the rotating speed of 450rpm, react 0.5h, ultrasonic disperse 35min, leaves standstill afterwards, after ammonia volatilizees completely, obtain titanium dioxide loaded on carbon nano tube overlay coating.
Using method according to the titanium dioxide loaded on carbon nano tube overlay coating prepared by preparation method of the application is as follows:
At 2500cm
2common exterior wall paint on spray about 50g titanium dioxide loaded on carbon nano tube overlay coating, maintenance 7d, obtains photocatalysis titanium dioxide overlay coating.This exterior wall paint can adopt white, elastic emulsion paint.
Experimental data
1. the degradation rate data for nitrogen protoxide, nitrogen peroxide and sulfurous gas measured by the titanium dioxide loaded on carbon nano tube overlay coating prepared by the application are as follows:
The testing method of gas degraded: carry out in the confined reaction case of customization, reaction box volume is 500L, built-in ultraviolet lamp source is 254nm × 15w × 2 (wavelength × Power x quantity), and fan (model LS-F95, output rating 4w) is housed to promote the circulation of reactant gases.
Concrete test procedure is as follows:
(1) by the blank cement plate of identical for area (0.25 ㎡) with scribble photocatalzed film cement plate and be placed in two identical reaction boxs respectively;
(2) circulation fan is opened, sealed reaction equipment;
(3) cover gobo, inject quantitative experimental gas, treat stable system 5min;
(4) open ultraviolet lamp, record experimental gas registration every 1min, treat that experimental gas concentration decline is to constant, stops record;
(5) repeated test five times, averaged.
(6) photocatalzed film catalytic efficiency calculates.Specific formula for calculation is as follows:
Rate of photocatalytic oxidation (μ g/ (㎡ .d)):
In formula:
The numerical value (namely initial system gas values deducts gas consumption value in blank experiment, ppb) of Δ gu---photocatalzed film catalyzed degradation dusty gas;
S---coating area, ㎡;
T---the time, sky (d);
M---NO or NO2 or SO2 molecular weight;
V---reaction box volume, m
3;
T---experimental temperature, DEG C;
P---barometric point, pa.
Qi Zhong ㎡ of note: is cm
2equivalent conversion, d is min equivalent conversion.
The experimental data of the degradation rate of table 1---nitrogen protoxide, nitrogen peroxide and sulfurous gas that each embodiment with the carbon nanotube loaded photocatalytic nanometer titanium dioxide overlay coating of pollution degradation gas records
As apparent from table 1 can, the embodiment 1-3 of the application all has the effect of degraded nitrogen protoxide, nitrogen peroxide and sulfurous gas, and wherein the effect of embodiment 1 and 3 is all better.Degradation efficiency not only depends on titanium content in reaction mixture and chitosan content, is also decided by hydrogen peroxide input amount.Titanium content reduction can cause photo-catalysis capability to reduce, and hydrogen peroxide addition reduces, and corresponding OH can be caused to measure and reduce, slowing of degraded gas.Although the addition of the carbon nanotube in embodiment 3 is compared with the increase to some extent in embodiment 1, photocatalysis efficiency is a little more than embodiment 1, and the reaction mixture of example 3 is also unstable, can layering after leaving standstill 24h.Therefore, considering, is optimum formula in embodiment 1.
2. contact angle correlation data
The model of table 2--preferred embodiment embodiment 1 and the contact angle Data Comparison of blank coating model
| Sample name | Former contact angle/° | Ultraviolet lighting contact angle/° |
| Embodiment 1 model | 12 | 6 |
| Blank coating model | 72 | 72 |
Note: ultraviolet lighting contact angle test mode is after model construction, fixed temperature and humidity room protection 7d, after ultraviolet lighting 24h, test contact angle.
As can be seen from Table 2, the embodiment 1 model contact angle of photochemical catalysis cover is lower, what after illumination, contact angle was more original reduces 6 °, this is relevant with the wetting ability that photocatalyst material titanium dioxide shows, and titanium dioxide significantly can improve wetting ability after ultraviolet lighting, illustrate that optically catalytic TiO 2 performance is enlivened; Blank coating model then shows as non-hydrophilic, even if ultraviolet lighting still maintains the original state substantially, without any photocatalytic activity, does not possess the function of degraded organic gas.
3. degradation rate correlation data
Model and the blank coating model degradation rate of table 3--preferred embodiment embodiment 1 contrast
| Sample name | N0 degradation rate/% | N0 2Degradation rate/% | S0 2Degradation rate/% |
| Embodiment 1 model | 88 | 70 | 92 |
| Blank model | 33 | 30 | 42 |
As can be seen from Table 3, the model with the preferred embodiment embodiment 1 of photochemical catalysis cover has the function of significantly degraded organic pollutant.
In sum, the overlay coating prepared by the present invention can not only under certain light conditions catalyzed degradation organic gas, and coating has the function of very strong absorption organic pollutant, has the dual-use function of catalysis after first absorption, effectively improves degradation efficiency.
The preparation method of titanium dioxide loaded on carbon nano tube overlay coating of the present invention has more than and is only confined to above-described embodiment, and every any improvement according to the principle of the invention or replacement, all should within protection scope of the present invention.
Claims (4)
1. a preparation method for titanium dioxide loaded on carbon nano tube overlay coating, is characterized in that: it comprises the following steps, is below weight part,
(1) 15-18 part titanium source and 63-66 part ethanol are joined in dispersion cup, 8-12min is disperseed under the rotating speed of 350-550rpm, then under the rotating speed of 350-550rpm, add 17-21 part ammoniacal liquor, adjustment rotating speed is to 800-1200rpm, and dispersion 25-35min, after ammonia volatilizees completely, centrifuging and taking throw out, is dried stand-by;
(2) rotating speed is adjusted to 350-550rpm, 44-52 part water and 25-32 part hydrogen peroxide is added successively in dispersion cup, improve temperature to 50-65 DEG C, the throw out that the step (1) adding 7-10 part obtains adds for more than 2 times by dividing, disperse 0.5-2h afterwards, add 7-10 part ammoniacal liquor and 3-8 part carbon nanotube, 0.5-1.5h is reacted under the rotating speed of 350-550rpm, ultrasonic disperse 25-35min, leave standstill afterwards, after ammonia volatilizees completely, obtain titanium dioxide loaded on carbon nano tube overlay coating;
Described titanium source is titanium tetrachloride or tetrabutyl titanate.
2. the preparation method of titanium dioxide loaded on carbon nano tube overlay coating according to claim 1, is characterized in that: it comprises the following steps, is below weight part,
(1) 16 parts of titanium sources and 65 parts of ethanol are joined in dispersion cup, under the rotating speed of 450rpm, disperse 10min, then under the rotating speed of 450rpm, add 19 parts of ammoniacal liquor, adjustment rotating speed, to 1200rpm, disperses 35min, after ammonia volatilizees completely, centrifuging and taking throw out, is dried stand-by;
(2) rotating speed is adjusted to 550rpm, 48 parts of water and 32 parts of hydrogen peroxide are added successively in dispersion cup, improve temperature to 65 DEG C, the throw out that the step (1) adding 10 parts obtains adds for more than 2 times by dividing, and disperses 1h afterwards, add 7 parts of ammoniacal liquor and 3 parts of carbon nanotubes, under the rotating speed of 550rpm, react 1h, ultrasonic disperse 30min, leaves standstill afterwards, after ammonia volatilizees completely, obtain titanium dioxide loaded on carbon nano tube overlay coating.
3. the preparation method of titanium dioxide loaded on carbon nano tube overlay coating according to claim 1, is characterized in that: divide 2 times by the throw out equal portions that step (1) obtains in described step (2) and add.
4., according to the preparation method of the arbitrary described titanium dioxide loaded on carbon nano tube overlay coating of claim 1-3, it is characterized in that: described carbon nanotube is adopted as multi-walled carbon nano-tubes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106009866A (en) * | 2016-07-27 | 2016-10-12 | 合肥旭阳铝颜料有限公司 | Dual coated aqueous aluminum pigment for antifouling paint |
| CN112048202A (en) * | 2020-09-14 | 2020-12-08 | 陈佳 | Preparation method of steel-based corrosion-resistant super-hydrophobic coating |
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| CN1544552A (en) * | 2003-11-28 | 2004-11-10 | 厦门大学 | Tunnel fireproof paint based on nano-surface-treatment technology and method for making same |
| CN101637720A (en) * | 2009-08-26 | 2010-02-03 | 南京大学 | Method for preparing catalyst for titanium dioxide loaded on carbon nano tube |
| CN102151561A (en) * | 2011-01-22 | 2011-08-17 | 浙江理工大学 | Photocatalyst consisting of carbon nanotubes loaded with titanium dioxide and preparation method thereof |
| CN104645960A (en) * | 2013-11-20 | 2015-05-27 | 李志刚 | Preparation method of composite titanium dioxide/carbon nano-tube |
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- 2015-10-30 CN CN201510729166.1A patent/CN105295457B/en active Active
Patent Citations (4)
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| CN1544552A (en) * | 2003-11-28 | 2004-11-10 | 厦门大学 | Tunnel fireproof paint based on nano-surface-treatment technology and method for making same |
| CN101637720A (en) * | 2009-08-26 | 2010-02-03 | 南京大学 | Method for preparing catalyst for titanium dioxide loaded on carbon nano tube |
| CN102151561A (en) * | 2011-01-22 | 2011-08-17 | 浙江理工大学 | Photocatalyst consisting of carbon nanotubes loaded with titanium dioxide and preparation method thereof |
| CN104645960A (en) * | 2013-11-20 | 2015-05-27 | 李志刚 | Preparation method of composite titanium dioxide/carbon nano-tube |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106009866A (en) * | 2016-07-27 | 2016-10-12 | 合肥旭阳铝颜料有限公司 | Dual coated aqueous aluminum pigment for antifouling paint |
| CN112048202A (en) * | 2020-09-14 | 2020-12-08 | 陈佳 | Preparation method of steel-based corrosion-resistant super-hydrophobic coating |
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