CN105295559B - Method for preparing cyclodextrin loaded titanium dioxide top coating - Google Patents
Method for preparing cyclodextrin loaded titanium dioxide top coating Download PDFInfo
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- CN105295559B CN105295559B CN201510728759.6A CN201510728759A CN105295559B CN 105295559 B CN105295559 B CN 105295559B CN 201510728759 A CN201510728759 A CN 201510728759A CN 105295559 B CN105295559 B CN 105295559B
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Abstract
The invention relates to a method for preparing a cyclodextrin loaded titanium dioxide top coating. The method comprises the following steps: (1) adding a titanium source and ethanol into a dispersion container for dispersing, sequentially adding a cosolvent and ammonia water, adding cyclodextrin, dispersing, centrifuging after ammonia gas is completely volatilized, taking the precipitate, and drying for later use; and (2) sequentially adding water and hydrogen peroxide into the dispersion container, equally adding the precipitate obtained in the step (1) twice, dispersing, sequentially adding the ammonia water and cosolvent, reacting, thereby obtaining the cyclodextrin loaded titanium dioxide top coating after the ammonia gas is completely volatilized. According to the method disclosed by the invention, the defects in the conventional preparation method that the cyclodextrin needs to be subjected to hydrophilic modification, time consumption is high and the prepared product is powder and cannot be directly used for finish coat of exterior wall are overcome, and the method has the advantages that the preparation is time-saving and simple and the finished product can be directly applied to finish coat of the exterior wall for degrading polluted organic gases.
Description
Technical field
The present invention relates to a kind of preparation method of cyclodextrin carried titanium dioxide overlay coating, apply in paint field.
Background technology
In the range of UV absorption, titanium dioxide has photocatalytic activity, its principle be titanium dioxide by light radiation when will
There is an electronics from valence to conduction band, while producing a hole in valence band, the hole for so producing is good oxygen
Agent, most photochemical catalysts are all the oxidabilities that make use of hole, and the electronics for moving to photocatalyst surface is good
Reducing agent.Photochemical catalyst is used in coating, using its redox ability, the pollution organic gas in degradable air.
Although photocatalysis titanium dioxide TiO2 has the advantages that reaction condition is gentle, degraded is complete, non-secondary pollution,
Still there is larger space to be improved in application field.Such as, common photocatalysis titanium dioxide will be produced after ultraviolet excitation
Electronics and the separation in hole, but wherein most light induced electron is migrating to catalyst surface again multiple all with hole
Close, the UV energy of absorption is then lost in the way of heat or fluorescence, therefore causes the photocatalysis efficiency of titanium dioxide low
Under.
Beta-schardinger dextrin is a kind of cyclic oligosaccharides for being capable of the various organic and inorganic and biomolecule objects of selective binding,
There is the cavity structure that specific surface area is larger, it has hydrophobic inner chamber and hydrophilic outside.Cyclodextrin is loaded into photocatalysis two
Cyclodextrin load photocatalysis titanium dioxide resulting on titanium oxide, both the big cavity adsorbance with cyclodextrin and envelope were recognized
(wherein envelope refers to the encapsulation of big cavity to performance, and recognizes to refer to the organic group that has of its inner chamber to organic pollution
Sucking action), and the double grading of the photocatalytic degradation dusty gas with photocatalysis titanium dioxide, so as to ensure that cyclodextrin
Load photocatalysis titanium dioxide has the advantages that quick absorption, either high redox.
Although also have being bonded with the titanium deoxide catalyst of methylol-beta-schardinger dextrin such as in the prior art
200510041898.8, but its there are the following problems：1. need to carry out hydrophilic modifying to cyclodextrin, its course of reaction is quite overflow
It is long, it is not particularly suited for industrialized production；2. what it was prepared is modified titanium dioxide powder, it is impossible to directly apply to exterior wall cover.
Therefore a kind of preparation process is provided time saving, simple and the cyclodextrin of exterior wall cover load dioxy can be directly applied to
Change titanium overlay coating preparation method oneself turn into when business urgently.
The content of the invention
The present invention provides a kind of preparation method of cyclodextrin carried titanium dioxide overlay coating, which overcomes existing preparation side
Need to carry out hydrophilic modifying to cyclodextrin in method, time-consuming and the product prepared is powder, it is impossible to is directly used in exterior wall cover
Shortcoming, can be directly applied to exterior wall cover for the organic gas of pollution degradation with time saving, simple and finished product is prepared
Advantage.
Technical scheme is as follows：
A kind of preparation method of cyclodextrin carried titanium dioxide overlay coating, it is comprised the following steps：Below it is weight
Part,
(1) 10-13 parts of titanium source and 60-63 parts of ethanol are added in dispersion cup, are divided under the rotating speed of 350-550rpm
Dissipate 8-12min；Then under the rotating speed of 350-550rpm, 0.5-2 parts of cosolvent and 12-18 parts of ammoniacal liquor are sequentially added, is added
11-13 parts of cyclodextrin, adjusts rotating speed to 800-1200rpm afterwards, disperses 25-35min, after ammonia volatilizees completely, carry out from
The heart, taking precipitate is dried stand-by；
(2) adjustment rotating speed adds 42-55 parts of water, 33-36 parts of hydrogen peroxide successively to 350-550rpm in dispersion cup,
And more than 2 times additions of the sediment for obtaining 7-15 parts of step (1) point, 0.5-1.5h is disperseed afterwards, then add 4-7 parts of ammonia successively
Water and 0.5-2 parts of cosolvent, afterwards at 30-50 DEG C, 0.5-1.5h are reacted under the rotating speed of 350-550rpm, treat that ammonia is waved completely
Hair, obtains final product cyclodextrin carried titanium dioxide overlay coating；
Wherein, the titanium source is titanium tetrachloride or butyl titanate.
Cyclodextrin in the basic conditions with cosolvent with the help of, can be dissolved in the aqueous solution, and surface exist it is certain
The hydroxyl of content, titanium source can produce substantial amounts of hydroxyl during titanium dioxide is formed；The two is made by the hydrogen bond between hydroxyl
With physical absorption so that cyclodextrin is loaded on titanium dioxide, and do not changed in chemical constitution.Ordinary titanium dioxide
The maximum shortcoming of coating is to cause light induced electron and hole-recombination after certain hour, and the organic big cavity energy that cyclodextrin is present
Substantial amounts of organic pollutant is enough adsorbed, and during this period of time supply light induced electron and hole are entered to organic pollutant in time
Row photocatalytic degradation, so as to improve degradation efficiency.And in the preparation technology hydrophilic modifying need not be carried out to cyclodextrin, carry significantly
Reaction process high, it is adaptable to industrialized production.Meanwhile, the end-product prepared is solution, rather than prepared by existing process
The titania powder for going out, the cyclodextrin carried titanium dioxide overlay coating that the application technique is prepared is modifying titanium dioxide water
Solution, can be directly used for common exterior wall cover.The cyclodextrin carried titanium dioxide overlay coating is used on common exterior wall cover,
Can not only under certain light conditions catalytic degradation organic pollutant, and it has the function of very strong adsorbed gas, tool
There is the dual-use function for first adsorbing and being catalyzed afterwards, catalytic degradation efficiency can be effectively increased.
Preferably, a kind of preparation method of cyclodextrin carried titanium dioxide overlay coating, it is comprised the following steps：It is equal below
It is weight portion,
(1) 13 parts of titanium sources and 60 parts of ethanol are added in dispersion cup, 10min is disperseed under the rotating speed of 400rpm；Connect
Under the rotating speed of 400rpm, sequentially add 1 part of cosolvent and 15 parts of ammoniacal liquor, add 11 parts of cyclodextrin, rotating speed is adjusted afterwards
To 850rpm, disperse 30min, after ammonia volatilizees completely, be centrifuged, taking precipitate, be dried stand-by；
(2) adjustment rotating speed adds 50 parts of water, 33 parts of hydrogen peroxide, and 10 parts are walked successively to 350rpm in dispersion cup
Suddenly more than 2 times additions of the sediment that (1) obtains point, disperse 1h afterwards, then add 6 parts of ammoniacal liquor and 1 part of cosolvent, Zhi Hou successively
45 DEG C, 1h is reacted under the rotating speed of 450rpm, treat that ammonia volatilizees completely, obtain final product cyclodextrin carried titanium dioxide overlay coating.
In the preparation method of the preferred cyclodextrin carried titanium dioxide overlay coating, titanium source, cyclodextrin and cosolvent
With the preferred parameter in the optimum ratio and preparation technology of reactant so that the cyclodextrin carried titanium dioxide cover that it is prepared
Coating materials not only have the absorption affinity to organic pollutant better than other cyclodextrin carried titanium dioxide overlay coatings, while
Also so that it has more preferably catalytic capability, to the in hgher efficiency of the degraded of organic pollutant.
2 additions of the sediment equal portions for obtaining step (1) in the step (2) point, easily facilitate dispersion.
The cosolvent is ethylene glycol, overcomes the general problem for being difficult to be dissolved in water of cyclodextrin, and it is molten with others
Agent is used cooperatively together so that cyclodextrin can preferably be dissolved in water, to prepare cyclodextrin carried titanium dioxide overlay coating
Create condition.
Compared with prior art, the present patent application has advantages below：
1) this technique need not carry out hydrophilic modifying to cyclodextrin, substantially increase reaction process, it is adaptable to industrial metaplasia
Produce；
2) end-product that the application technique is prepared is cyclodextrin carried titanium dioxide washcoating solution, different from existing
Titania powder prepared by technique, can be directly used for common exterior wall cover, substantially increases its range of application and uses
Degree of convenience.
Specific embodiment
Technical scheme is described in detail with reference to each embodiment.
Raw material sources：
Water：Ordinary tap water；
Ethylene glycol：Aladdin is produced, and is analyzed pure；
Ethanol：75% industrial alcohol；
Titanium tetrachloride, butyl titanate：Aladdin is produced, and is analyzed pure；
Cyclodextrin：Aladdin is produced, and analyzes pure, beta-schardinger dextrin；
Ammoniacal liquor：Xilong Chemical Co., Ltd produces, and analyzes pure；
Hydrogen peroxide：Xilong Chemical Co., Ltd produces, and analyzes pure, and content is 30%.
Embodiment 1
A kind of preparation method of cyclodextrin carried titanium dioxide overlay coating of the present invention, it is comprised the following steps：
Weight portion is below,
(1) 13 parts of titanium tetrachlorides and 60 parts of ethanol are added in dispersion cup, are disperseed under the rotating speed of 400rpm
10min；Then under the rotating speed of 400rpm, 1 part of ethylene glycol and 15 parts of ammoniacal liquor are sequentially added, adds 11 parts of beta-schardinger dextrins, it
Adjustment rotating speed disperses 30min to 850rpm afterwards, after ammonia volatilizees completely, is centrifuged, taking precipitate, is dried stand-by；
(2) adjustment rotating speed adds 50 parts of water, 33 parts of hydrogen peroxide, and 10 parts are walked successively to 350rpm in dispersion cup
Suddenly 2 additions of the sediment equal portions that (1) obtains point, disperse 1h afterwards, then add 6 parts of ammoniacal liquor and 1 part of ethylene glycol, Zhi Hou successively
45 DEG C, 1h is reacted under the rotating speed of 450rpm, treat that ammonia volatilizees completely, obtain final product cyclodextrin carried titanium dioxide overlay coating.
Embodiment 2
A kind of preparation method of cyclodextrin carried titanium dioxide overlay coating of the present invention, it is comprised the following steps：
Weight portion is below,
(1) 10 parts of butyl titanates and 63 parts of ethanol are added in dispersion cup, are disperseed under the rotating speed of 350rpm
8min；Then under the rotating speed of 350rpm, 1 part of cosolvent and 15 parts of ammoniacal liquor are sequentially added, adds 11 parts of cyclodextrin, adjusted afterwards
Turn over speed disperses 25min to 800rpm, after ammonia volatilizees completely, is centrifuged, taking precipitate, is dried stand-by；
(2) adjustment rotating speed adds 50 parts of water, 33 parts of hydrogen peroxide, and 10 parts are walked successively to 350rpm in dispersion cup
Suddenly 3 additions of the sediment that (1) obtains point, disperse 1h afterwards, then add 6 parts of ammoniacal liquor and 1 part of cosolvent successively, afterwards 50
DEG C, 1h is reacted under the rotating speed of 350rpm, treat that ammonia volatilizees completely, obtain final product cyclodextrin carried titanium dioxide overlay coating.
Embodiment 3
A kind of preparation method of cyclodextrin carried titanium dioxide overlay coating of the present invention, it is comprised the following steps：
Weight portion is below,
(1) 11 parts of titanium sources and 61 parts of ethanol are added in dispersion cup, 12min is disperseed under the rotating speed of 550rpm；Connect
Under the rotating speed of 550rpm, sequentially add 0.5 part of cosolvent and 12 parts of ammoniacal liquor, add 13 parts of cyclodextrin, adjustment afterwards turns
Speed disperses 35min to 1200rpm, after ammonia volatilizees completely, is centrifuged, taking precipitate, is dried stand-by；
(2) adjustment rotating speed adds 55 parts of water, 35 parts of hydrogen peroxide successively to 450rpm in dispersion cup, and by 7 parts of steps
(1) 4 additions of the sediment for obtaining point, disperse 0.5h afterwards, then add 7 parts of ammoniacal liquor and 0.5 part of cosolvent successively, afterwards 30
DEG C, 0.5h is reacted under the rotating speed of 550rpm, treat that ammonia volatilizees completely, obtain final product cyclodextrin carried titanium dioxide overlay coating.
Embodiment 4
A kind of preparation method of cyclodextrin carried titanium dioxide overlay coating of the present invention, it is comprised the following steps：
Weight portion is below,
(1) 11 parts of titanium sources and 63 parts of ethanol are added in dispersion cup, 11min is disperseed under the rotating speed of 550rpm；Connect
Under the rotating speed of 450rpm, sequentially add 2 parts of cosolvents and 18 parts of ammoniacal liquor, add 12 parts of cyclodextrin, rotating speed is adjusted afterwards
To 900rpm, disperse 30min, after ammonia volatilizees completely, be centrifuged, taking precipitate, be dried stand-by；
(2) adjustment rotating speed adds 42 parts of water, 36 parts of hydrogen peroxide, and 15 parts are walked successively to 550rpm in dispersion cup
Suddenly 5 additions of the sediment that (1) obtains point, disperse 1.5h afterwards, then add 4 parts of ammoniacal liquor and 2 parts of cosolvents successively, afterwards 30
DEG C, 1.5h is reacted under the rotating speed of 450rpm, treat that ammonia volatilizees completely, obtain final product cyclodextrin carried titanium dioxide overlay coating.
The application method of the cyclodextrin carried titanium dioxide overlay coating prepared by the preparation method of foundation the application is as follows：
In 2500cm2Common exterior wall paint on spray about 50g cyclodextrin carried titanium dioxide overlay coatings, conserve 7d,
Obtain photocatalysis titanium dioxide overlay coating.The exterior wall paint can use white, elastic emulsion paint.
Experimental data
1. nitric oxide, titanium dioxide measured by the cyclodextrin carried titanium dioxide overlay coating prepared by the application are directed to
The degradation rate data of nitrogen and sulfur dioxide are as follows：
The method of testing of gas degraded：Carried out in the confined reaction case of customization, reaction chamber volume is 500L, built-in ultraviolet
Lamp source is 254nm × 15w × 2 (wavelength × Power x quantity), and equipped with fan (model LS-F95, power output 4w) with promotion
The circulation of reacting gas.
Specific testing procedure is as follows：
(1) by the blank cement plate of area identical (0.25 ㎡) and scribble photocatalzed film cement plate and be respectively placed in two phases
In same reaction chamber；
(2) circulation fan is opened, consersion unit is sealed；
(3) gobo is covered, quantitative experimental gas are injected, stable system is treated 5 minutes；
(4) uviol lamp is opened, experimental gas registration is recorded every 1min, treat that experimental gas concentration decline, to constant, stops note
Record；
(5) retest five times, averaged.
(6) photocatalzed film catalytic efficiency is calculated.Specific formula for calculation is as follows：
Rate of photocatalytic oxidation (μ g/ (㎡ .d))：
In formula：
(i.e. initial system gas values subtract blank pair to the numerical value of Δ gu --- photocatalzed film catalytic degradation dusty gas
According to the facts test middle gas consumption value, ppb)；
S --- coat side Ji , ㎡；
T --- time, day (d)；
M --- NO or NO2 or SO2 molecular weight；
V --- reaction chamber volume, m3；
T --- experimental temperature, DEG C；
P --- atmospheric pressure, pa.
Note：Qi Zhong ㎡ are cm2Equivalent conversion, d is min equivalent conversions.
Table 1 --- the cyclodextrin with pollution degradation gas loads each implementation of photocatalytic nanometer titanium dioxide overlay coating
The experimental data of the degradation rate of nitric oxide, nitrogen dioxide and sulfur dioxide that example is measured
From table 1, it is apparent that embodiments herein 1-4 is respectively provided with degraded nitric oxide, nitrogen dioxide and dioxy
Change sulphur effect, and degradation efficiency to a certain extent with reaction mixture in Ti content and cyclodextrin load capacity into just
Than.Wherein best results of embodiment 1.
2. contact angle correction data
The model of table 2-- optimal cases embodiment 1 and the contact angle Data Comparison of blank coating model
| Sample name | Former contact angle/° | Ultraviolet lighting contact angle/° |
| The model of embodiment 1 | 10 | 4.5 |
| Blank coating model | 72 | 72 |
Note：Ultraviolet lighting contact angle test mode is constant temperature and humidity room protection 7d, ultraviolet lighting after model construction is finished
After 24h, contact angle is tested.
From table 2 it can be seen that the model contact angle of embodiment 1 of photocatalysis cover is relatively low, contact angle is more original after illumination
5.5 ° are reduced, this is relevant with the hydrophily that catalysis material titanium dioxide is showed, and titanium dioxide can be bright after ultraviolet lighting
Aobvious raising hydrophily, illustrates that optically catalytic TiO 2 performance is enlivened；And 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 correction data
The model of table 3-- optimal cases embodiment 1 is contrasted with blank coating model degradation rate
| Sample name | N0 degradation rates/% | N02Degradation rate/% | S02Degradation rate/% |
| The model of embodiment 1 | 89 | 67 | 93 |
| Blank model | 33 | 30 | 42 |
From table 3 it can be seen that the model of the optimal case embodiment 1 with photocatalysis cover is organic with significantly degrading
The function of dusty gas.
In sum, the present invention prepared by overlay coating can not only under certain light conditions the organic gas of catalytic degradation
Body, and coating has the function of very strong absorption organic pollutant, with the dual-use function that is catalyzed afterwards is first adsorbed, effectively improves
Degradation efficiency.
The preparation method of cyclodextrin carried titanium dioxide overlay coating of the present invention is not only limited only to above-mentioned
Embodiment, every any improvement or replacement according to the principle of the invention all should be within protection scope of the present invention.
Claims (4)
1. a kind of preparation method of cyclodextrin carried titanium dioxide overlay coating, it is characterised in that：It is comprised the following steps, below
It is weight portion,
(1) 10-13 parts of titanium source and 60-63 parts of ethanol are added in dispersion cup, 8- is disperseed under the rotating speed of 350-550rpm
12min；Then under the rotating speed of 350-550rpm, 0.5-2 parts of cosolvent and 12-18 parts of ammoniacal liquor are sequentially added, adds 11-13
Part cyclodextrin, adjusts rotating speed to 800-1200rpm afterwards, disperses 25-35min, after ammonia volatilizees completely, is centrifuged, and takes
Sediment, is dried stand-by；
(2) adjustment rotating speed adds 42-55 parts of water, 33-36 parts of hydrogen peroxide successively to 350-550rpm in dispersion cup, and will
More than 2 times additions of the sediment point that 7-15 parts of step (1) obtains, disperse 0.5-1.5h afterwards, then add successively 4-7 part ammoniacal liquor with
0.5-2 parts of cosolvent, afterwards at 30-50 DEG C, 0.5-1.5h is reacted under the rotating speed of 350-550rpm, treats that ammonia volatilizees completely, i.e.,
Obtain cyclodextrin carried titanium dioxide overlay coating；
Wherein, the titanium source is titanium tetrachloride or butyl titanate.
2. the preparation method of cyclodextrin carried titanium dioxide overlay coating according to claim 1, it is characterised in that：Its bag
Following steps are included, weight portion is below,
(1) 13 parts of titanium sources and 60 parts of ethanol are added in dispersion cup, 10min is disperseed under the rotating speed of 400rpm；Then exist
Under the rotating speed of 400rpm, 1 part of cosolvent and 15 parts of ammoniacal liquor are sequentially added, add 11 parts of cyclodextrin, adjust rotating speed extremely afterwards
850rpm, disperses 30min, after ammonia volatilizees completely, is centrifuged, taking precipitate, is dried stand-by；
(2) adjustment rotating speed adds 50 parts of water, 33 parts of hydrogen peroxide successively to 350rpm in dispersion cup, and by 10 parts of steps (1)
More than 2 times additions of the sediment for obtaining point, disperse 1h afterwards, then add 6 parts of ammoniacal liquor and 1 part of cosolvent successively, afterwards at 45 DEG C,
1h is reacted under the rotating speed of 450rpm, treats that ammonia volatilizees completely, obtain final product cyclodextrin carried titanium dioxide overlay coating.
3. the preparation method of cyclodextrin carried titanium dioxide overlay coating according to claim 1, it is characterised in that：It is described
2 additions of the sediment equal portions for obtaining step (1) in step (2) point.
4., according to the preparation method of any described cyclodextrin carried titanium dioxide overlay coatings of claim 1-3, its feature exists
In：The cosolvent is ethylene glycol.
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| CN107501636A (en) * | 2017-09-08 | 2017-12-22 | 宣城市聚源精细化工有限公司 | A kind of preparation method of Beta-cyclodextrin-based phosphorus flame retardant |
| CN107652822A (en) * | 2017-10-11 | 2018-02-02 | 广东华兹卜新材料科技有限公司 | A kind of aqueous colorful art coatings and preparation method thereof |
| CN114100331B (en) * | 2020-08-31 | 2022-12-13 | 中国石油化工股份有限公司 | Volatile organic matter treatment material and preparation method and application thereof |
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| CN1698961A (en) * | 2005-04-05 | 2005-11-23 | 陕西师范大学 | Photocatalyst for bonding titanium dioxide with carboxymethyl-beta-cyclodextrin |
| CN103752348A (en) * | 2014-02-20 | 2014-04-30 | 华东理工大学 | Magnetic composite photocatalyst |
| CN104645960A (en) * | 2013-11-20 | 2015-05-27 | 李志刚 | Preparation method of composite titanium dioxide/carbon nano-tube |
| CN104893375A (en) * | 2015-06-03 | 2015-09-09 | 福州大学 | Organic-inorganic hybrid photocatalysis top coating as well as preparation method and application thereof |
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| JP5670466B2 (en) * | 2009-11-13 | 2015-02-18 | 中国石油化工股▲ふん▼有限公司 | Supported nonmetallocene catalyst, process for its production and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1698961A (en) * | 2005-04-05 | 2005-11-23 | 陕西师范大学 | Photocatalyst for bonding titanium dioxide with carboxymethyl-beta-cyclodextrin |
| CN104645960A (en) * | 2013-11-20 | 2015-05-27 | 李志刚 | Preparation method of composite titanium dioxide/carbon nano-tube |
| CN103752348A (en) * | 2014-02-20 | 2014-04-30 | 华东理工大学 | Magnetic composite photocatalyst |
| CN104893375A (en) * | 2015-06-03 | 2015-09-09 | 福州大学 | Organic-inorganic hybrid photocatalysis top coating as well as preparation method and application thereof |
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