CN105926020B - A kind of preparation method of super hydrophilic titanium foam for water-oil separating - Google Patents
A kind of preparation method of super hydrophilic titanium foam for water-oil separating Download PDFInfo
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- CN105926020B CN105926020B CN201610421063.3A CN201610421063A CN105926020B CN 105926020 B CN105926020 B CN 105926020B CN 201610421063 A CN201610421063 A CN 201610421063A CN 105926020 B CN105926020 B CN 105926020B
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- titanium foam
- titanium
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- oil
- foam
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000010936 titanium Substances 0.000 title claims abstract description 48
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 48
- 239000006260 foam Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000012545 processing Methods 0.000 claims abstract description 7
- 238000002203 pretreatment Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003792 electrolyte Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000008151 electrolyte solution Substances 0.000 claims description 4
- 231100001240 inorganic pollutant Toxicity 0.000 claims description 4
- 238000002386 leaching Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 2
- 239000003344 environmental pollutant Substances 0.000 claims 1
- 231100000719 pollutant Toxicity 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 10
- 239000006210 lotion Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 3
- CCYWDIWYFIDBTE-UHFFFAOYSA-N [O-2].[O-2].[F].[Ti+4] Chemical compound [O-2].[O-2].[F].[Ti+4] CCYWDIWYFIDBTE-UHFFFAOYSA-N 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical class [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003653 coastal water Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Water Treatments (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses a kind of preparation method of the super hydrophilic titanium foam for water-oil separating.Preparation method is divided into three material pre-treatment, anodized, ultraviolet lighting steps.Obtained titanium foam surface is made of intrinsic hydrophilic fluorine titanium oxide, while surface is covered with countless nano-cavities, and roughness value Rq reaches 35.6 nm, can further enhance the hydrophilicity on titanium foam surface.The titanium foam has the superoleophobic characteristic of good super-hydrophilic and underwater, and water droplet contact angle is 0 ° in atmosphere, and underwater oil contact angle is 160 °, has good oil-water separation.When filtering accuracy reaches less than 20 μm, which can be also used for lotion separation, and separative efficiency can reach more than 99%.This method is easy to operate, and resulting materials have good stability and Superhydrophilic, and oil-water separation is notable；Simultaneously because titanium material have the characteristics that it is nontoxic, environmental-friendly, oily wastewater processing and oil recycling etc. field tool be of great significance.
Description
Technical field
The present invention relates to titanium foam technical field, specifically, is related to a kind of super hydrophilic titanium foam for water-oil separating
Preparation method.
Background technology
Titanium foam be it is a kind of there is nontoxic, environmental-friendly, good biocompatibility porous metal material, in recent years
Favored be subject to more and more researchers.
The development and application of material, the usually technology of preparing ripe with its are inseparable.The preparation method of titanium foam is near
Year is also interesting.Its preparation principle is by titanium particle and pore creating material（Such as urea）Mixed, then under a certain pressure
Formed by high-temperature calcination（CN103131883A；CN103447533A）.By the parameters during adjusting, can obtain
The titanium foam that porosity differs, so as to provide the space of more more options for its later use.2014, Wang Yao was very waited and is utilized hydrogen
Gas auxiliary law, has prepared cheap, the high titanium foam of porosity（CN104451233A）, further widened titanium foam
Application prospect.
With the progress that coastal waters is exploited, ocean oil accident happens occasionally；Industrial oily wastewater is also being on the increase at the same time.
This brings huge challenge to water-oil separating.Water-oil separating under weight-driven relative to traditional UF membrane, have it is efficient,
The advantage such as energy saving and receive much concern.Porous foam titanium is a kind of good water-oil separating material, but the research of association area is very
It is few.2015, Li et al. was prepared for TiO using anodic oxidation on titanium foam surface2Nanotube carries out water-oil separating, but this method
The Superhydrophilic stability referred to is bad；Nano tube structure is unfavorable for constructing for super hydrophilic interface at the same time（J. Mater. Chem.
A, 2015, 3, 1279）.We form intrinsic hydrophilic fluorine oxidation on titanium foam surface by suitable anodized
Nitride layer, stability are good；And nano surface chamber can significantly improve surface roughness, strengthen super hydrophilicity.The titanium foam has
Good oil-water separation.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of super hydrophilic titanium foam for water-oil separating
Preparation method.The present invention is by anodized, the technological means of ultraviolet lighting, come good, the excellent performance for preparing stability
Super hydrophilic water-oil separating titanium foam.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of preparation method of super hydrophilic titanium foam for water-oil separating, includes the following steps：
（1）The pre-treatment of material：By titanium foam, it is cleaned by ultrasonic successively with acetone, ethanol, deionized water, removing surface has
Machine and inorganic pollutant, then leaching is placed in acetone, stand-by；
（2）Anodized：Electrolyte is weighed, adds water and ethylene glycol configuration electrolyte solution stand-by；Then with foam
Titanium is anode, and titanium foil is cathode, under applied voltage effect, carries out anodized, water bath with thermostatic control temperature is 20-50 DEG C；
（3）Ultraviolet lighting processing：Titanium foam is dried, is then irradiated with ultraviolet light, to remove the carbon containing dirt on surface
Dye thing obtains super hydrophilic titanium foam.
As preference, in above-mentioned preparation method, step（1）The titanium foam filtering accuracy of middle use below 200 μm,
Thickness is 0.1-10mm.
As preference, in above-mentioned preparation method, step（2）In used electrolyte be villiaumite.
As preference, in above-mentioned preparation method, step（2）Employed in electrolyte weight percentage be 0.1%-
10%。
As preference, in above-mentioned preparation method, step（2）In two interelectrode distances be 0.1-5cm.
As preference, in above-mentioned preparation method, step（2）Middle to use constant voltage dc source, current density control exists
1-100m A/cm2。
As preference, in above-mentioned preparation method, step（2）Anodic Oxidation processing time is 1-12h.
As preference, in above-mentioned preparation method, step（3）Described in ultraviolet light intensity be 1-100 mW/cm2。
As preference, in above-mentioned preparation method, step（3）Described in the distance of ultraviolet light and titanium foam be 1-
20cm。
As preference, in above-mentioned preparation method, step（3）Described in the ultraviolet light time be 1-60min.
Compared with prior art, the present invention has the advantages that：
The present invention is by anodic oxidation, the method for ultraviolet lighting, to prepare super hydrophilic titanium foam.The foam that the invention obtains
Titanium, surface are made of hydrophilic fluorine titanium oxide, while surface is covered with countless nano-cavities, and roughness value R, reaches
35.6nm, can further enhance the hydrophilicity on titanium foam surface.The titanium foam is super thin with good super-hydrophilic and underwater
Oily characteristic, water droplet contact angle is 0 ° in atmosphere, and underwater oil contact angle is 160 °, has good oil-water separation.When point
Reach less than 20 μm from precision, which can be also used for lotion separation, and separative efficiency can reach more than 99%.The present invention
Preparation method, reagent and material are cheap and simple and easy to get, and operating method is also very simple, and material water-oil separating performance is excellent,
Stability is preferable.
Brief description of the drawings
Fig. 1 is that the low power of the titanium foam before reaction and high power SEM scheme, and surface is more smooth；
Fig. 2 is the low power and high power SEM figures of the titanium foam after reaction, and surface is uniform-distribution with nanoscale cavity；
Fig. 3 is water contact angle in the air of the super hydrophilic titanium foam prepared and underwater oily contact angle figure, and water droplet and oil droplet are equal
For 5 μ l；
Fig. 4 is the lotion separating effect figure of sample, oil content figure and separative efficiency in water after lotion separation.
Embodiment
Embodiment 1
（1）The pre-treatment of material：By 20 μm of separation accuracy, the titanium foam of thickness 1mm（Purity>99.7%）, successively with third
Ketone, ethanol, deionized water are cleaned by ultrasonic 10min in 80KHZ, remove that surface is organic and inorganic pollutant, then leaching are placed in
It is stand-by in acetone.
（2）Anodized：Weighing 0.3g ammonium fluorides adds 15g water and 84.7g ethylene glycol to be configured to percetage by weight
0.3% ammonium fluoride electrolyte solution 100g is stand-by.Then using titanium foam as anode, titanium foil is cathode, and the two poles of the earth distance is 1.5cm,
Under the effect of 80V impressed DC voltages, anodized is carried out, water bath with thermostatic control temperature is 25 DEG C, reacts 8h, takes out, spend
Air-dried after ion water washing.
（3）Ultraviolet lighting processing：By dried titanium foam sample, 90mW/cm is used2Ultraviolet lamp, apart from sample
20cm positions irradiating sample 10 minutes.
Resulting materials, by initial flat surface（Fig. 1）It is changed into the surface being made of countless nano-cavities（Such as Fig. 2）.From
Macroscopically see, material is in black gray expandable, and water contact angle is 0 ° in air, and underwater oil contact angle is 160 °（Such as Fig. 3）.Separated by lotion
Experiment is understood：The material has good oil-water separation, and lotion separative efficiency can reach more than 99%, and for two
Toluene, separative efficiency is close to 100%.The material has very strong prospects for commercial application（Such as Fig. 4）.
Embodiment 2：
（1）The pre-treatment of material：By 20 μm of separation accuracy, the titanium foam of thickness 1mm（Purity>99.7%）, successively with third
Ketone, ethanol, deionized water are cleaned by ultrasonic 10min in 80KHZ, remove that surface is organic and inorganic pollutant, then leaching are placed in
It is stand-by in acetone.
（2）Anodized：Weighing 0.4g ammonium fluorides adds 18g water and 81.6g ethylene glycol to be configured to percetage by weight
0.4% ammonium fluoride electrolyte solution 100g is stand-by.Then using titanium foam as anode, titanium foil is cathode, and the two poles of the earth distance is 1.5cm,
Under the effect of 80V impressed DC voltages, anodized is carried out, water bath with thermostatic control temperature is 25 DEG C, reacts 6h, takes out, spend
Air-dried after ion water washing.
（3）Ultraviolet lighting processing：By dried titanium foam sample, 90mW/cm is used2Ultraviolet lamp, apart from sample
20cm positions irradiating sample 10 minutes.
Resulting materials, pattern and water-oil separating performance are basically identical with embodiment 1.
Claims (1)
1. a kind of preparation method of super hydrophilic titanium foam, it is characterised in that include the following steps：
（1）The pre-treatment of material：By titanium foam, be cleaned by ultrasonic successively with acetone, ethanol, deionized water, remove surface it is organic with
And inorganic pollutant, then leaching is placed in acetone, stand-by；
（2）Anodized：Electrolyte is weighed, adds water and ethylene glycol configuration electrolyte solution stand-by；Then using titanium foam as
Anode, titanium foil are cathode, under applied voltage effect, carry out anodized, water bath with thermostatic control temperature is 20-50 DEG C；
（3）Ultraviolet lighting processing：Titanium foam is dried, is then irradiated with ultraviolet light, to remove the carbon based pollutants on surface
Obtain super hydrophilic titanium foam；
Step（1）The titanium foam filtering accuracy of middle use is below 200 μm, thickness 0.1-10mm；
Step（2）In used electrolyte be villiaumite；
Step（2）Employed in electrolyte weight percentage be 0.1%-10%；
Step（2）In two interelectrode distances be 0.1-5cm；
Step（2）Middle to use constant voltage dc source, current density is controlled in 1-100m A/cm2；
Step（2）Anodic Oxidation processing time is 1-12h；
Step（3）Described in ultraviolet light intensity be 1-100 mW/cm2；
Step（3）Described in the distance of ultraviolet light and titanium foam be 1-20cm；
Step（3）Described in the ultraviolet light time be 1-60min.
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| CN108179454A (en) * | 2017-12-29 | 2018-06-19 | 重庆大学 | A kind of preparation method of the super infiltration titanium foam of water-oil separating |
| CN108516605A (en) * | 2018-05-11 | 2018-09-11 | 湖南国昶能源科技有限公司 | A kind of Self-priming oil-water separator |
| CN110038569B (en) * | 2019-05-22 | 2021-11-19 | 安徽理工大学 | Janus Cu (OH)2@Cu2O/Cu net and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302630A (en) * | 2008-01-17 | 2008-11-12 | 上海交通大学 | Method for preparing metal by means of solid oxide electrolytic cell |
| CN103173835A (en) * | 2011-12-22 | 2013-06-26 | 中国科学院大连化学物理研究所 | Treating method of metallic titanium material |
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| CN103949167B (en) * | 2014-04-21 | 2016-06-08 | 北京航空航天大学 | A kind of preparation method with automatically cleaning and the micro-nano oil-water separation film of superoleophobic character under water |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302630A (en) * | 2008-01-17 | 2008-11-12 | 上海交通大学 | Method for preparing metal by means of solid oxide electrolytic cell |
| CN103173835A (en) * | 2011-12-22 | 2013-06-26 | 中国科学院大连化学物理研究所 | Treating method of metallic titanium material |
Non-Patent Citations (1)
| Title |
|---|
| A New Route for Surface Modification: Fluorine-Induced Superhydrophilicity;Zhi-Yong Luo;《The Journal of Physical Chemistry C》;20160513;第120卷;第11183页实验部分 * |
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