CN207153489U - A kind of super hydrophilic and underwater superoleophobic ceramic membrane - Google Patents
A kind of super hydrophilic and underwater superoleophobic ceramic membrane Download PDFInfo
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- CN207153489U CN207153489U CN201720857242.1U CN201720857242U CN207153489U CN 207153489 U CN207153489 U CN 207153489U CN 201720857242 U CN201720857242 U CN 201720857242U CN 207153489 U CN207153489 U CN 207153489U
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Abstract
The utility model provides a kind of super hydrophilic and underwater superoleophobic ceramic membrane, and using porous ceramic film as substrate, substrate surface arranges nano level column titanium dioxide, forms nano titania array.The ceramic membrane structure is less than 10 ° to the static contact angle of water, is more than 150 ° to the contact angle of oil under water, can be used as water-oil separationg film, have excellent oil-water separation and fouling resistance effect.
Description
Technical field
The utility model belongs to functional material technical field, and in particular to a kind of super hydrophilic and underwater superoleophobic pottery
Porcelain film.
Background technology
UF membrane is to efficiently separate new technology in the present age, is widely used in environmental protection and sewage disposal, biomedicine etc.
Field, new approach is provided for recycling economy production.Ceramic membrane is separated made of by the ceramic material of high temperature sintering
Film, due to uniqueness intensity and corrosion resistance, one into market become for film field it is with the fastest developing speed, also most have hair
One of kind of exhibition prospect.
With further investigation of the people to special wellability surface in nature, the preparation side about special wellability surface
Method continues to bring out.The method reported mostly at present all concentrates on to be separated from the water out by oil.In the prior art, ceramic membrane master
To be applied in aqueous phase system, when separating oil phase, due to existing water-oil separating ceramic membrane materials, greasy dirt often adheres to material
Expect in surface and hole, it is difficult to remove so that the filtration flux of film is low, and the efficiency of separation declines, cause equipment investment cost and
Use cost is higher, it is difficult to realizes the marketization.
Patent CN1336352A discloses a kind of Photocatalystic self-cleaning TiO 2 ceramic and preparation method thereof, and it is in ceramic sheet
Photocatalysis film and low temperature for main component by nano titanium oxide are closely compounded with body or in the glaze paint of ceramic manufactured articles
Glaze, TiO 2 sol is loaded into Ceramic glaze, be fired into required Photocatalystic self-cleaning TiO 2 ceramic.But party's legal system
The durability of titanium dioxide in standby Photocatalystic self-cleaning TiO 2 ceramic is relatively low, and easy poisoning and deactivation, influences its use
Life-span.2015, Li etc. was prepared for TiO using anodic oxidation on titanium foam surface2Nanotube carries out water-oil separating, but the party
The Superhydrophilic stability that method refers to is bad；Nano tube structure is unfavorable for constructing for super hydrophilic interface simultaneously
(J.Mater.Chem.A,2015,3,1279)。
Utility model content
The utility model provides a kind of super hydrophilic and underwater superoleophobic ceramic membrane structure, using porous ceramic film as base
Bottom, substrate surface arrange nano level column titanium dioxide, i.e. titanium dioxide is in the form of a column structure, and its diameter is with height in nanometer
Yardstick, nano titania array is formed in substrate surface.
That is, the utility model in porous ceramics substrate surface combination titanium dioxide, titanic oxide material have Superhydrophilic,
The features such as chemical stability is good, corrosion resistance is strong, and in the utility model, titanium dioxide is formed in porous ceramics substrate surface
Nano titania array, the special pattern of one side nano-array make specific surface area very big, further enhance hydrophilicity, separately
One side nano array structure can significantly improve substrate surface roughness, hydrophilic strengthening in oil water separation process
Effectively stop oil molecule simultaneously, realize underwater superoleophobic performance.It is experimentally confirmed that ceramic membrane structure of the present utility model is to water
Static contact angle is less than 10 °, is more than 150 ° to the contact angle of oil under water, can be used as water-oil separationg film, have excellent oil
Water separating effect and fouling resistance effect.
Described porous ceramic film is unlimited, including porous alumina ceramic film etc..
Described oily species is unlimited, including vegetable oil, mineral oil or organic solvent, such as the emulsification of toluene oil emulsion, chloroform
Oil, emulsification edible peanut oil etc..
The utility model additionally provides a kind of method for preparing the super hydrophilic and underwater superoleophobic ceramic membrane, including with
Lower step：
(1) using porous ceramic film as substrate, substrate surface after cleaning prepares layer of metal plating titanium layer, obtains titanizing pottery
Porcelain film；
The cleaning treatment method of described substrate is unlimited, as a kind of implementation, successively by substrate be put into deionized water,
Ultrasonic wave cleaning is carried out in absolute ethyl alcohol；
The method that metal-plated titanium layer is prepared in substrate surface is unlimited, using chemical deposition or physical deposition, such as
Magnetron sputtering technique etc..
(2) titanizing ceramic membrane is put into oxidation solution and aoxidized, then cleaned with deionized water, done afterwards
It is dry；
It is hydrogen peroxide, nitric acid and melamine that described oxidation solution, which includes mass percent concentration, concentrated nitric acid with it is double
The volume ratio of oxygen water is (1-5)：The mass volume ratio of (50-100), melamine and hydrogen peroxide is (50-100)：(1-5)mg/
ml.Wherein, hydrogen peroxide is used to titanyl turning to titanium dioxide；Concentrated nitric acid on the one hand can titanium oxide, on the other hand can reduce it is molten
Liquid pH value and stabilized chlorine titanium colloidal sol, reduce colloidal sol in solution and be nucleated, so as to promote the life of nano level column titanium dioxide
It is long；Melamine hydrolyzes caused ammonium ion in acid condition, and the selection of nano-array can be promoted to absorb titanium dioxide.
Preferably, the mass percent concentration of described hydrogen peroxide is 30%.
Preferably, the mass percent concentration of described concentrated nitric acid is 60%-98%.
Preferably, described oxidization time is 2-4 hours.
The collocation method of described oxidation solution is unlimited, including hydrogen peroxide, concentrated nitric acid and melamine are stirred, directly
It is completely dissolved to melamine.Described mixing temperature is preferably 80 DEG C.
In summary, the utility model grows nano titania array on porous ceramic matrices suitable, due to titanium dioxide
Superhydrophilic, improve the oleophobic property under water of matrix.Wherein, metal is plated on porous ceramic film using magnetron sputtering technique
Titanium layer,
Compared with prior art, the utility model has the following advantages that：
(1) ceramic membrane of the present utility model is pollution-free using material non-toxic, has super hydrophilic, underwater superoleophobic property,
It can prevent from blocking ceramic capillary during water-oil separating, it is easy to use；Material safety, economic, environmental protection during as separation oil emulsion,
Oil emulsion efficiency high is separated, has the characteristics that mechanical strength is big, repeat usage is high, stable performance, water surface resistance are small；
(2) preparation method provided by the utility model can large area prepare surface there is nano level column titanium dioxide
Ceramic membrane, technique is simple, abundant raw material, is easy to mass production.
Brief description of the drawings
Fig. 1 is the SEM figures of ceramic membrane prepared by embodiment 1；
Fig. 2 is Fig. 1 enlarged drawing；
Fig. 3 is the underwater chloroform contact angle of ceramic membrane prepared by embodiment 1；
Fig. 4 is the SEM figures of ceramic membrane prepared by embodiment 3；
Fig. 5 is the underwater chloroform contact angle of ceramic membrane prepared by embodiment 3；
Fig. 6 is the SEM figures of ceramic membrane prepared by embodiment 5；
Fig. 7 is the underwater chloroform contact angle of ceramic membrane prepared by embodiment 5；
Fig. 8 is the underwater edible peanut oil contact angle of ceramic membrane prepared by embodiment 11；
Fig. 9 is the SEM figures of ceramic membrane prepared by comparative example 1.
Embodiment
The technical solution of the utility model is further described below in conjunction with some embodiments and accompanying drawing.Need to illustrate
, embodiment described below and term are intended to be easy to understanding of the present utility model, and do not play any restriction effect to it.
Embodiment 1：
In the present embodiment, for ceramic membrane using porous alumina ceramic piece as substrate, substrate surface arranges nano level column
Titanium dioxide, nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane is as follows：
(1) step 1：The immersion of porous alumina ceramic piece is cleaned by ultrasonic in a solvent, to slough potsherd surface
Spot and grease, then dry；
(2) step 2：Potsherd after cleaning is fixed on magnetron sputtering apparatus, using Titanium as target, control sputtering
Time 2h, obtain the potsherd of ti coat on diamond；
(3) step 3：Configuration oxidation solution, it is specifically：By 63% concentrated nitric acid 3ml, 30% hydrogen peroxide 70ml, melamine
Amine 80mg stirring to melamines at 80 DEG C of temperature are completely dissolved；
(4) step 4：The titanizing potsherd that step 2 obtains is put into the oxidation solution that step 3 configures, 80 DEG C of insulations 2 are small
When, the Ti metals that potsherd surface is plated is fully oxidized as TiO2Nano-array.
(5) step 5：The potsherd that step 4 is obtained cleans, and is dried in drying box, that is, obtaining to surface has titanium dioxide battle array
The ceramic membrane of row.
The SEM figures of ceramic membrane obtained above show that nano level titanium dioxide arranges as shown in figure 1, enlarged drawing be Fig. 2
In substrate surface, nano titania array is formed.
Ceramic membrane obtained above is carried out into water contact angle in air to test, underwater chloroform contact angle test, and profit
Separative efficiency is tested.
Water-oil separating Efficiency test method is：The water armored benzene oil emulsion of certain volume is fitted into oily-water seperating equipment,
Add 0.02Mpa external pressures to carry out separation oil emulsion, take former oil emulsion and filtrate sample, survey the front and rear ultraviolet absorptivity of emulsion separation,
Water-oil separating efficiency (%)=(1- filter liquor concentrations/former emulsion concentration) * 100.
Oleophobic property method of testing is under water：Ceramic membrane obtained above is immersed in the container for filling water, instills chloroform,
The size of the underwater oily contact angle of measurement.
The result tested by above method of testing is：Underwater chloroform contact angle is 153.7 ° as described in Figure 3, air
Middle water contact angle is 2 °, and water-oil separating efficiency is 99.2%.
Embodiment 2：
In the present embodiment, ceramic membrane structure is similar to Example 1, is the substrate table using porous alumina ceramic piece as substrate
Face arranges nano level column titanium dioxide, and nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane and the preparation method in embodiment 1 are essentially identical, except that being configured in step 3
During aoxidizing solution, the addition of 63% concentrated nitric acid is 1ml.
The SEM figures of ceramic membrane obtained above are similar to Figure 1, show that nano level titanium dioxide is arranged in substrate table
Face, form nano titania array.
Ceramic membrane obtained above is carried out into water contact angle in air to test, underwater chloroform contact angle test, and profit
Separative efficiency is tested.Method of testing is identical with the method in embodiment 1.
The result tested by above method of testing is：Underwater chloroform contact angle is 151 ° ± 3 °, the contact of air reclaimed water
Angle is 3 °, and water-oil separating efficiency is 97.6%.
Embodiment 3:
In the present embodiment, ceramic membrane structure is similar to Example 1, is the substrate table using porous alumina ceramic piece as substrate
Face arranges nano level column titanium dioxide, and nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane and the preparation method in embodiment 1 are essentially identical, except that being configured in step 3
During aoxidizing solution, the addition of 63% concentrated nitric acid is 5ml.
The SEM figures of ceramic membrane obtained above as shown in figure 4, show that nano level titanium dioxide is arranged in substrate surface,
Form nano titania array.
Ceramic membrane obtained above is carried out into water contact angle in air to test, underwater chloroform contact angle test, and profit
Separative efficiency is tested.Method of testing is identical with the method in embodiment 1.
The result tested by above method of testing is：Underwater chloroform contact angle is 155 ° ± 2 ° as described in Figure 5, empty
Water contact angle is 2 ° in gas, and water-oil separating efficiency is 96.6%.
Embodiment 4：
In the present embodiment, ceramic membrane structure is similar to Example 1, is the substrate table using porous alumina ceramic piece as substrate
Face arranges nano level column titanium dioxide, and nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane and the preparation method in embodiment 1 are essentially identical, except that being configured in step 3
During aoxidizing solution, the addition of 30% hydrogen peroxide is 50ml.
The SEM figures of ceramic membrane obtained above are similar to Figure 1, show that nano level titanium dioxide is arranged in substrate table
Face, form nano titania array.
Ceramic membrane obtained above is carried out into water contact angle in air to test, underwater chloroform contact angle test, and profit
Separative efficiency is tested.Method of testing is identical with the method in embodiment 1.
The result tested by above method of testing is：Underwater chloroform contact angle is 152 ° ± 1 °, the contact of air reclaimed water
Angle is 3 °, and water-oil separating efficiency is 98.6%.
Embodiment 5：
In the present embodiment, ceramic membrane structure is similar to Example 1, is the substrate table using porous alumina ceramic piece as substrate
Face arranges nano level column titanium dioxide, and nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane and the preparation method in embodiment 1 are essentially identical, except that being configured in step 3
During aoxidizing solution, the addition of 30% hydrogen peroxide is 100ml.
The SEM figures of ceramic membrane obtained above as shown in fig. 6, show that nano level titanium dioxide is arranged in substrate surface,
Form nano titania array.
Ceramic membrane obtained above is carried out into water contact angle in air to test, underwater chloroform contact angle test, and profit
Separative efficiency is tested.Method of testing is identical with the method in embodiment 1.
The result tested by above method of testing is：Underwater chloroform contact angle is empty as shown in fig. 7, for 155 ° ± 2 °
Water contact angle is 2 ° in gas, and water-oil separating efficiency is 98.8%.
Embodiment 6：
In the present embodiment, ceramic membrane structure is similar to Example 1, is the substrate table using porous alumina ceramic piece as substrate
Face arranges nano level column titanium dioxide, and nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane and the preparation method in embodiment 1 are essentially identical, except that being configured in step 3
During aoxidizing solution, the addition of melamine is 50mg.
The SEM figures of ceramic membrane obtained above are similar to Figure 1, show that nano level titanium dioxide is arranged in substrate table
Face, form nano titania array.
Ceramic membrane obtained above is carried out into water contact angle in air to test, underwater chloroform contact angle test, and profit
Separative efficiency is tested.Method of testing is identical with the method in embodiment 1.
The result tested by above method of testing is：Underwater chloroform contact angle is 156 ° ± 1 °, the contact of air reclaimed water
Angle is 2 °, and water-oil separating efficiency is 99.1%.
Embodiment 7：
In the present embodiment, ceramic membrane structure is similar to Example 1, is the substrate table using porous alumina ceramic piece as substrate
Face arranges nano level column titanium dioxide, and nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane and the preparation method in embodiment 1 are essentially identical, except that being configured in step 3
During aoxidizing solution, the addition of melamine is 100mg.
The SEM figures of ceramic membrane obtained above are similar to Figure 1, show that nano level titanium dioxide is arranged in substrate table
Face, form nano titania array.
Ceramic membrane obtained above is carried out into water contact angle in air to test, underwater chloroform contact angle test, and profit
Separative efficiency is tested.Method of testing is identical with the method in embodiment 1.
The result tested by above method of testing is：Underwater chloroform contact angle is 154 ° ± 2 °, the contact of air reclaimed water
Angle is 6 °, and water-oil separating efficiency is 97.8%.
Embodiment 8：
In the present embodiment, ceramic membrane structure is similar to Example 1, is the substrate table using porous alumina ceramic piece as substrate
Face arranges nano level column titanium dioxide, and nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane and the preparation method in embodiment 1 are essentially identical, except that the oxygen in step 4
It is 4 hours to change the time.
The SEM figures of ceramic membrane obtained above are similar to Figure 1, show that nano level titanium dioxide is arranged in substrate table
Face, form nano titania array.
Ceramic membrane obtained above is carried out into water contact angle in air to test, underwater chloroform contact angle test, and profit
Separative efficiency is tested.Method of testing is identical with the method in embodiment 1.
The result tested by above method of testing is：Underwater chloroform contact angle is 153 ° ± 2 °, the contact of air reclaimed water
Angle is 6 °, and water-oil separating efficiency is 99.3%.
Embodiment 9：
In the present embodiment, ceramic membrane structure is similar to Example 1, is the substrate table using porous alumina ceramic piece as substrate
Face arranges nano level column titanium dioxide, and nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane and the preparation method in embodiment 1 are essentially identical, except that splashing in step 2
The time is penetrated as 1 hour.
The SEM figures of ceramic membrane obtained above are similar to Figure 1, show that nano level titanium dioxide is arranged in substrate table
Face, form nano titania array.
Ceramic membrane obtained above is carried out into water contact angle in air to test, underwater chloroform contact angle test, and profit
Separative efficiency is tested.Method of testing is identical with the method in embodiment 1.
The result tested by above method of testing is：Underwater chloroform contact angle is 151 ° ± 2 °, the contact of air reclaimed water
Angle is 5 °, and water-oil separating efficiency is 99.1%.
Embodiment 10：
In the present embodiment, ceramic membrane structure is similar to Example 1, is the substrate table using porous alumina ceramic piece as substrate
Face arranges nano level column titanium dioxide, and nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane and the preparation method in embodiment 1 are essentially identical, except that splashing in step 2
The time is penetrated as 3 hours.
The SEM figures of ceramic membrane obtained above are similar to Figure 1, show that nano level titanium dioxide is arranged in substrate table
Face, form nano titania array.
Ceramic membrane obtained above is carried out into water contact angle in air to test, underwater chloroform contact angle test, and profit
Separative efficiency is tested.Method of testing is identical with the method in embodiment 1.
The result tested by above method of testing is：Underwater chloroform contact angle is 156 ° ± 1 °, the contact of air reclaimed water
Angle is 5 °, and water-oil separating efficiency is 98.8%.
Embodiment 10：
In the present embodiment, ceramic membrane structure is similar to Example 1, is the substrate table using porous alumina ceramic piece as substrate
Face arranges nano level column titanium dioxide, and nano titania array is formed in substrate surface.
The preparation method of the ceramic membrane is identical with the preparation method in embodiment 1.
The SEM figures of ceramic membrane obtained above are identical with Fig. 1, show that nano level titanium dioxide is arranged in substrate surface,
Form nano titania array.
Ceramic membrane obtained above is subjected to underwater edible peanut oil contact angle test, method of testing is：It is made above-mentioned
Ceramic membrane be immersed in the container for filling water, instill edible peanut oil, measure the size of underwater oily contact angle, the result of test
As shown in figure 8, underwater edible peanut oil contact angle is 151.3 ± 3 °.
Water-oil separating Efficiency test method is：The water bag edible peanut oil of certain volume is fitted into oily-water seperating equipment,
Add 0.02Mpa external pressures to carry out separation edible peanut oil, take the crude oil aqueous solution and filtrate sample, survey the front and rear ultraviolet suction of emulsion separation
Luminosity, water-oil separating efficiency is up to 98.6%.
Comparative example 1：
The present embodiment is the comparative example of embodiment 1.
In the present embodiment, the preparation method and the preparation method in embodiment 1 of ceramic membrane are essentially identical, except that
During step 3 configuration oxidation solution, melamine is added without.That is, the concrete configuration method for aoxidizing solution is as follows：
63% concentrated nitric acid 3ml, 30% hydrogen peroxide 70ml are stirred at 80 DEG C of temperature.
The SEM figures of ceramic membrane obtained above are entirely different with Fig. 1, show the pattern of ceramic bases, the institute of below figure 9
Show, nano titania array is not formed in substrate surface.
The technical solution of the utility model is described in detail embodiment described above, it should be understood that above institute
Only specific embodiment of the utility model is stated, is not limited to the utility model, it is all in spirit of the present utility model
Interior done any modification, supplement or similar fashion replacement etc., should be included within the scope of protection of the utility model.
Claims (4)
1. a kind of super hydrophilic and underwater superoleophobic ceramic membrane, using porous ceramic film as substrate, it is characterized in that：Substrate surface is arranged
Nano level column titanium dioxide is arranged, nano titania array is formed in substrate surface.
2. the super hydrophilic and underwater superoleophobic ceramic membrane as shown in claim 1, it is characterized in that：Described porous ceramic film
Including porous alumina ceramic film.
3. the super hydrophilic and underwater superoleophobic ceramic membrane as shown in claim 1, it is characterized in that：Described oily species includes
Vegetable oil, mineral oil or organic solvent.
4. the super hydrophilic and underwater superoleophobic ceramic membrane as shown in claim 1, it is characterized in that：To the static contact angle of water
Less than 10 °, 150 ° are more than to the contact angle of oil under water.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107213801A (en) * | 2017-07-14 | 2017-09-29 | 中国科学院宁波材料技术与工程研究所 | Super hydrophilic and superoleophobic under water a kind of ceramic membrane and preparation method thereof |
| CN109012216A (en) * | 2018-08-23 | 2018-12-18 | 中冶华天工程技术有限公司 | New function ceramic membrane materials and preparation method thereof |
| CN109490352A (en) * | 2018-12-28 | 2019-03-19 | 中山大学 | Multifactor low temperature sleet freezing environment simulated testing system |
-
2017
- 2017-07-14 CN CN201720857242.1U patent/CN207153489U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107213801A (en) * | 2017-07-14 | 2017-09-29 | 中国科学院宁波材料技术与工程研究所 | Super hydrophilic and superoleophobic under water a kind of ceramic membrane and preparation method thereof |
| CN107213801B (en) * | 2017-07-14 | 2023-09-19 | 中国科学院宁波材料技术与工程研究所 | Super-hydrophilic and underwater super-oleophobic ceramic membrane and preparation method thereof |
| CN109012216A (en) * | 2018-08-23 | 2018-12-18 | 中冶华天工程技术有限公司 | New function ceramic membrane materials and preparation method thereof |
| CN109490352A (en) * | 2018-12-28 | 2019-03-19 | 中山大学 | Multifactor low temperature sleet freezing environment simulated testing system |
| CN109490352B (en) * | 2018-12-28 | 2021-07-09 | 中山大学 | Multi-factor low-temperature freezing rain icing environment simulation test system |
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