CN104478043A - Method for preparing super-hydrophilic super-oleophobic electrode material - Google Patents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
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- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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Abstract
The invention provides a method for preparing a super-hydrophilic super-oleophobic electrode material, and relates to a method of constructing a special invasive electrode with super-hydrophilic super-oleophobic performances on the surface of the conventional electrode, belonging to the technical field of functional materials. The method comprises the following steps: by adopting a method of performing micro-nano laser ablation on a columnar array on the surface of the conventional electrode material, performing chemical etching on the etched columnar array by piranha washing liquor, further performing chemical corrosion and treatment on the etched columnar array by aqua regia, thereby forming a composite surface with a micro-nano multistage structure; lowering a contact angle of the electrode surface and the water from 70 degrees to 10 degrees and increasing the contact angle of water and oil drops to 160 degrees from 60 degrees, thereby obtaining the special invasive electrode with super-hydrophilic super-oleophobic performances. The method disclosed by the invention is simple in preparation method and operation process; and the electrode surface with special invasive performance is prepared, so that an electrolyte solution is continuously and effectively electrolyzed by the electrode surface.
Description
Technical field
The invention belongs to technical field of function materials, be specifically related to construct a kind of electrode materials with super hydrophilic super oleophobic performance electrode surface is bionical, solve existing electrode at the medium oil product of organic electrolysis to the attachment of electrode, thus make the technical problem that electric current declines, electrolytic efficiency reduces.
Background technology
In recent years, along with industry and daily necessities improving constantly classes of compounds demand, industrial and life contaminated water also strengthens day by day on the impact that water body environment, basin and residents ' health cause, and is tending towards serious along with going deep into further of process of industrialization.Water pollutions not only can cause large amounts of financial loss, more directly endangers the drinking water safety of resident.In industry and Sewage Pollution thing are discharged, tensio-active agent occupies larger proportion, and the effect of amphiphilic (hydrophilic and oleophylic) group based on its uniqueness, be difficult to remove in water body.The excessive use of tensio-active agent and any discharge cause serious pollution and destruction to natural water body and basin.Traditional method is difficult to realize effective removal and be separated to the tensio-active agent in water body, causes tensio-active agent to become extremely urgent to the pollution of water body, is badly in need of the key issue of the water pollution solved.
Electrochemical electrolysis reaction is that the pollution problem effectively solving tensio-active agent in water body provides effective solution and method.But, traditional electrode material surface is due to the high-adhesiveness to electrochemical electrolysis reaction product, reaction product is adhered at electrode surface, be difficult to be separated removing, electrode surface conductivity and electrolytic efficiency is caused to produce significant decline, and finally make electrolytic reaction stop, be difficult to continual and steady carrying out.By the inspiration on the special wetting property surface of occurring in nature animals and plants, its special wetting property principle is introduced electrode material surface, bionically construct the special wetting property electrode with micro-nano combined multi-stage structure, thus the efficiency of three-phase reaction interface and stability in raising electrochemical reaction, reactant and electrode surface is made to form good contact further, and reaction product and electrode surface realize effectively being separated, thus improve working efficiency, the prolongation electrode working life of working electrode, realize the effective separation to tensio-active agent in water body and removal.
Summary of the invention
The object of the present invention is to provide a kind of electrode materials preparing super hydrophilic super oleophobic, thus the method that efficient electrolysis removes tensio-active agent in water can be continued.The method preparation flow is simple, utilizes the method that high precision mum laser etches and chemical solution corrodes, carries out processing construct at traditional electrode surface, thus obtains of the present inventionly having special infiltrating electrode materials.The electrode materials that can continue efficient electrolysis tensio-active agent of the present invention has super hydrophilic and super thin oil properties under water in atmosphere, under water at its surface contact angle, 150 ° are all greater than to oily organism gasoline, lubricating oil, crude oil etc., and have the low characteristic of sticking of oil droplet.Super hydrophilic super oleophobic electrode materials of the present invention can be applicable to containing tensio-active agent sanitary sewage disposal, be separated and remove and the aspect such as environment protection.Apply this super hydrophilic super oleophobic electrode materials to carry out process to the waste water containing tensio-active agent and there is lasting, efficient, low cost, environmental protection, without the need to other chemical additives, can be used for the advantages such as extensive use.
The method that the preparation that the present invention proposes can continue the super hydrophilic super oleophobic electrode materials of tensio-active agent in high-efficient electrolytic water specifically comprises the following steps:
(1) the constructing of electrode surface micrometre array structure: make laser beam spot diameter reach requirement size by regulating micro-nano laser generator, by micro-nano laser beam focus in electrode material surface, utilize micro-nano laser beam to carry out on a large scale electrode surface, high-precision array etching, obtain the electrode surface structures with micrometer structure array;
(2) chemically modified of micrometre array electrode surface structures: micrometer structure array electrode good for pre-treatment in step (1) is immersed in the Piranha washing lotion configured and soaks, and be placed on electromagnetic heater, control temperature is at 100 DEG C, and thermostatically heating is no longer emerged bubble to Piranha washing lotion;
(3) the constructing of micrometre array electrode surface nanostructure: micrometre array electrode good for pre-treatment in step (2) is immersed in the chloroazotic acid configured, at room temperature soak for a long time, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
The invention has the advantages that:
(1) preparation that the present invention proposes can continue the super hydrophilic super oleophobic electrode materials of tensio-active agent in high-efficient electrolytic water, and its preparation method is simple, and principle obtains convenient, easy handling;
(2) the super hydrophilic super oleophobic electrode materials of the preparation of the present invention's proposition, can be applicable to sanitary sewage disposal, oil-containing water body purification, all has a wide range of applications in fields such as environmental protection;
(3) the super hydrophilic super oleophobic electrode materials of the preparation of the present invention's proposition, is greater than 150 ° to the contact angle of oil under water, and has low characteristic of sticking;
(4) the super hydrophilic super oleophobic electrode materials of preparation that proposes of the present invention, environmentally safe, capable of circulationly repeatedly uses.
Accompanying drawing explanation
Fig. 1 is that the present invention prepares the method flow schematic diagram with special wetting property electrode materials;
Fig. 2 is the method flow diagram that the present invention prepares the super hydrophilic super oleophobic electrode materials that can continue tensio-active agent in high-efficient electrolytic water;
Fig. 3 does not adopt the electrode pair of prior art of the present invention to carry out the digital photograph of electrode surface before and after the reaction of electrolysis treatment containing the waste water of tensio-active agent;
Fig. 4 adopts super hydrophilic super oleophobic electrode materials of the present invention to carry out the digital photograph of electrode surface before and after the reaction of electrolysis treatment to the waste water containing tensio-active agent.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
The preparation that the present invention proposes can continue the super hydrophilic super oleophobic electrode materials of tensio-active agent in high-efficient electrolytic water, and as shown in Figure 1, the method comprises following step:
The first step, constructing of electrode surface micrometre array structure: regulate micro-nano laser generator to make laser beam spot diameter reach 25-250 μm, by micro-nano laser beam focus in electrode material surface, (this electrode materials without during any process without micro-nano multi-level structure, be only conventional flat electrodes, size elects 20mm × 15mm × 0.5mm as), the stepped intervals of setting laser bundle spot is of a size of 25-250 μm and utilizes micro-nano laser beam to carry out on a large scale electrode surface, the high-precision etching of orthogonal array line by line, thus obtain the electrode surface structures (as shown in Figure 2) with micrometer structure array,
Described electrode base materials can adopt noble electrode, is made up of one or more in the inert material such as platinum, gold, is preferably platinum electrode material.
The chemically modified of second step, micrometre array electrode surface structures: micrometer structure array electrode good for pre-treatment in the first step is immersed in the Piranha washing lotion configured and soaks, and be placed on electromagnetic heater, control temperature is at 100 DEG C, thermostatically heating to Piranha washing lotion no longer emerges (about 2-6 hour) bubble, take out the electrode materials etched, repeatedly rinse with deionized water, then utilize nitrogen to dry up stand-by;
Constructing of 3rd step, micrometre array electrode surface nanostructure: micrometre array electrode good for pre-treatment in second step is immersed in the chloroazotic acid configured, at room temperature soak 4-10 hour, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
, there is obvious micro-nano multi-level structure after treatment in the super hydrophilic super oleophobic electrode materials that can continue tensio-active agent in high-efficient electrolytic water adopting the present invention to prepare.As shown in Figure 3, after not adopting the traditional electrode electrolysis of the inventive method process, electrode surface sticks more organic product, thus reduces current efficiency, and reaction is finally interrupted; As shown in Figure 4, after adopting the super hydrophilic super oleophobic electrolysis of the inventive method process, electrode surface does not have organism stick and remain, and achieves lasting efficient electrolytic reaction.
Following examples are only be described in further detail technical scheme of the present invention, instead of limit technical scheme of the present invention.
Embodiment 1
(1) micro-nano laser generator is regulated to make laser beam spot diameter reach 75 μm, by micro-nano laser beam focus in platinum plate electrode material surface, (this electrode materials without during any process without micro-nano multi-level structure, be only conventional flat electrodes, size elects 20mm × 15mm × 0.5mm as), the stepped intervals of setting laser bundle spot be of a size of 75 μm utilize micro-nano laser beam to carry out on a large scale electrode surface, high-precision orthogonal array line by line etching, thus obtain the electrode surface structures with micrometer structure array;
(2) micrometer structure array electrode good for pre-treatment in the first step is immersed in the Piranha washing lotion configured and soak, and be placed on electromagnetic heater, control temperature is at 100 DEG C, thermostatically heating to Piranha washing lotion no longer emerges (about 3 hours) bubble, take out the electrode materials etched, repeatedly rinse with deionized water, then utilize nitrogen to dry up stand-by;
(3) micrometre array electrode good for pre-treatment in second step is immersed in the chloroazotic acid configured, at room temperature soak 4 hours, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
Embodiment 2
(1) micro-nano laser generator is regulated to make laser beam spot diameter reach 75 μm, by micro-nano laser beam focus in golden plate electrode material surface, (this electrode materials without during any process without micro-nano multi-level structure, be only conventional flat electrodes, size elects 20mm × 15mm × 0.5mm as), the stepped intervals of setting laser bundle spot be of a size of 75 μm utilize micro-nano laser beam to carry out on a large scale electrode surface, high-precision orthogonal array line by line etching, thus obtain the electrode surface structures with micrometer structure array;
(2) micrometer structure array electrode good for pre-treatment in the first step is immersed in the Piranha washing lotion configured and soak, and be placed on electromagnetic heater, control temperature is at 100 DEG C, thermostatically heating to Piranha washing lotion no longer emerges (about 3 hours) bubble, take out the electrode materials etched, repeatedly rinse with deionized water, then utilize nitrogen to dry up stand-by;
(3) micrometre array electrode good for pre-treatment in second step is immersed in the chloroazotic acid configured, at room temperature soak 4 hours, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
Embodiment 3
(1) micro-nano laser generator is regulated to make laser beam spot diameter reach 25 μm, by micro-nano laser beam focus in platinum plate electrode material surface, (this electrode materials without during any process without micro-nano multi-level structure, be only conventional flat electrodes, size elects 20mm × 15mm × 0.5mm as), the stepped intervals of setting laser bundle spot be of a size of 25 μm utilize micro-nano laser beam to carry out on a large scale electrode surface, high-precision orthogonal array line by line etching, thus obtain the electrode surface structures with micrometer structure array;
(2) micrometer structure array electrode good for pre-treatment in the first step is immersed in the Piranha washing lotion configured and soak, and be placed on electromagnetic heater, control temperature is at 100 DEG C, thermostatically heating to Piranha washing lotion no longer emerges (about 3 hours) bubble, take out the electrode materials etched, repeatedly rinse with deionized water, then utilize nitrogen to dry up stand-by;
(3) micrometre array electrode good for pre-treatment in second step is immersed in the chloroazotic acid configured, at room temperature soak 4 hours, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
Embodiment 4
(1) micro-nano laser generator is regulated to make laser beam spot diameter reach 50 μm, by micro-nano laser beam focus in platinum plate electrode material surface, (this electrode materials without during any process without micro-nano multi-level structure, be only conventional flat electrodes, size elects 20mm × 15mm × 0.5mm as), the stepped intervals of setting laser bundle spot be of a size of 50 μm utilize micro-nano laser beam to carry out on a large scale electrode surface, high-precision orthogonal array line by line etching, thus obtain the electrode surface structures with micrometer structure array;
(2) micrometer structure array electrode good for pre-treatment in the first step is immersed in the Piranha washing lotion configured and soak, and be placed on electromagnetic heater, control temperature is at 100 DEG C, thermostatically heating to Piranha washing lotion no longer emerges (about 3 hours) bubble, take out the electrode materials etched, repeatedly rinse with deionized water, then utilize nitrogen to dry up stand-by;
(3) micrometre array electrode good for pre-treatment in second step is immersed in the chloroazotic acid configured, at room temperature soak 4 hours, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
Embodiment 5
(1) micro-nano laser generator is regulated to make laser beam spot diameter reach 100 μm, by micro-nano laser beam focus in platinum plate electrode material surface, (this electrode materials without during any process without micro-nano multi-level structure, be only conventional flat electrodes, size elects 20mm × 15mm × 0.5mm as), the stepped intervals of setting laser bundle spot be of a size of 100 μm utilize micro-nano laser beam to carry out on a large scale electrode surface, high-precision orthogonal array line by line etching, thus obtain the electrode surface structures with micrometer structure array;
(2) micrometer structure array electrode good for pre-treatment in the first step is immersed in the Piranha washing lotion configured and soak, and be placed on electromagnetic heater, control temperature is at 100 DEG C, thermostatically heating to Piranha washing lotion no longer emerges (about 3 hours) bubble, take out the electrode materials etched, repeatedly rinse with deionized water, then utilize nitrogen to dry up stand-by;
(3) micrometre array electrode good for pre-treatment in second step is immersed in the chloroazotic acid configured, at room temperature soak 4 hours, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
Embodiment 6
(1) micro-nano laser generator is regulated to make laser beam spot diameter reach 150 μm, by micro-nano laser beam focus in platinum plate electrode material surface, (this electrode materials without during any process without micro-nano multi-level structure, be only conventional flat electrodes, size elects 20mm × 15mm × 0.5mm as), the stepped intervals of setting laser bundle spot be of a size of 150 μm utilize micro-nano laser beam to carry out on a large scale electrode surface, high-precision orthogonal array line by line etching, thus obtain the electrode surface structures with micrometer structure array;
(2) micrometer structure array electrode good for pre-treatment in the first step is immersed in the Piranha washing lotion configured and soak, and be placed on electromagnetic heater, control temperature is at 100 DEG C, thermostatically heating to Piranha washing lotion no longer emerges (about 3 hours) bubble, take out the electrode materials etched, repeatedly rinse with deionized water, then utilize nitrogen to dry up stand-by;
(3) micrometre array electrode good for pre-treatment in second step is immersed in the chloroazotic acid configured, at room temperature soak 4 hours, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
Embodiment 7
(1) micro-nano laser generator is regulated to make laser beam spot diameter reach 75 μm, by micro-nano laser beam focus in platinum plate electrode material surface, (this electrode materials without during any process without micro-nano multi-level structure, be only conventional flat electrodes, size elects 20mm × 15mm × 0.5mm as), the stepped intervals of setting laser bundle spot be of a size of 75 μm utilize micro-nano laser beam to carry out on a large scale electrode surface, high-precision orthogonal array line by line etching, thus obtain the electrode surface structures with micrometer structure array;
(2) chemically modified of micrometre array electrode surface structures: micrometer structure array electrode good for pre-treatment in the first step is immersed in the Piranha washing lotion configured and soaks, and be placed on electromagnetic heater, control temperature is at 100 DEG C, thermostatically heating to Piranha washing lotion no longer emerges (about 3 hours) bubble, take out the electrode materials etched, repeatedly rinse with deionized water, then utilize nitrogen to dry up stand-by;
(3) the constructing of micrometre array electrode surface nanostructure: micrometre array electrode good for pre-treatment in second step is immersed in the chloroazotic acid configured, at room temperature soak 6 hours, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
Embodiment 8
(1) micro-nano laser generator is regulated to make laser beam spot diameter reach 75 μm, by micro-nano laser beam focus in electrode material surface, (this electrode materials without during any process without micro-nano multi-level structure, be only conventional flat electrodes, size elects 20mm × 15mm × 0.5mm as), the stepped intervals of setting laser bundle spot be of a size of 75 μm utilize micro-nano laser beam to carry out on a large scale electrode surface, high-precision orthogonal array line by line etching, thus obtain the electrode surface structures with micrometer structure array;
(2) micrometer structure array electrode good for pre-treatment in the first step is immersed in the Piranha washing lotion configured and soak, and be placed on electromagnetic heater, control temperature is at 100 DEG C, thermostatically heating to Piranha washing lotion no longer emerges (about 3 hours) bubble, take out the electrode materials etched, repeatedly rinse with deionized water, then utilize nitrogen to dry up stand-by;
(3) micrometre array electrode good for pre-treatment in second step is immersed in the chloroazotic acid configured, at room temperature soak 8 hours, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
Embodiment 9
(1) micro-nano laser generator is regulated to make laser beam spot diameter reach 75 μm, by micro-nano laser beam focus in platinum plate electrode material surface, (this electrode materials without during any process without micro-nano multi-level structure, be only conventional flat electrodes, size elects 20mm × 15mm × 0.5mm as), the stepped intervals of setting laser bundle spot be of a size of 75 μm utilize micro-nano laser beam to carry out on a large scale electrode surface, high-precision orthogonal array line by line etching, thus obtain the electrode surface structures with micrometer structure array;
(2) micrometer structure array electrode good for pre-treatment in the first step is immersed in the Piranha washing lotion configured and soak, and be placed on electromagnetic heater, control temperature is at 100 DEG C, thermostatically heating to Piranha washing lotion no longer emerges (about 3 hours) bubble, take out the electrode materials etched, repeatedly rinse with deionized water, then utilize nitrogen to dry up stand-by;
(3) micrometre array electrode good for pre-treatment in second step is immersed in the chloroazotic acid configured, at room temperature soak 10 hours, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
Claims (10)
1. prepare a method for electrode materials, it is characterized in that, described method comprises the following steps:
(1) the constructing of electrode surface micrometre array structure: make laser beam spot diameter reach requirement size by regulating laser generator, by laser beam focus in electrode material surface, utilize laser beam to carry out array etching to electrode surface, obtain the electrode surface structures with micrometer structure array;
(2) chemically modified of micrometre array electrode surface structures: micrometer structure array electrode good for pre-treatment in step (1) is immersed in the Piranha washing lotion configured and soaks, and be placed on electromagnetic heater, control temperature is at 100 DEG C, and thermostatically heating is no longer emerged bubble to Piranha washing lotion;
(3) the constructing of micrometre array electrode surface nanostructure: micrometre array electrode good for pre-treatment in step (2) is immersed in the chloroazotic acid configured, at room temperature soak for a long time, formed after nanostructure until micrometre array structure through chemical corrosion, take out the electrode soaked, use ethanol and washed with de-ionized water respectively, and dry up with nitrogen, obtain that there is special infiltrating electrode surface.
2. method according to claim 1, is characterized in that, the diameter of the laser beam spot that described laser generator excites is 25-250 μm, and the optical maser wavelength that described laser generator excites is 700-800nm.
3. method according to claim 1 and 2, is characterized in that: described laser etching method utilizes based on Numeric Control Technology, and laser is process medium, makes work material instant melting or gasification under laser radiation.
4. method according to claim 1 and 2, is characterized in that: described electrode is noble electrode, is made up of one or more in inert material.
5. method according to claim 1 and 2, is characterized in that: the micrometer structure array of described laser ablation is micron columnar arrays, and the spacing between two adjacent columnar structures is 25 μm-250 μm.
6. method according to claim 5, is characterized in that: by regulating the spacing between described two adjacent columnar structures, can the wetting property state on control electrode surface.
7. the method according to claim 1,2 or 6, is characterized in that: the diameter of the columnar arrays of described laser ablation is micron order yardstick.
8. method according to claim 1, is characterized in that: the time utilizing Piranha washing lotion to soak reaction in described step (2) is 2-6 hour.
9. the method according to claim 1 or 8, is characterized in that: described Piranha washing lotion 2.3-3: 1 is prepared by volume the vitriol oil and superoxol.
10. method according to claim 1, is characterized in that: the time utilizing chloroazotic acid to soak reaction in described step (3) is 4-8 hour.
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| CN112547462A (en) * | 2020-11-23 | 2021-03-26 | 重庆大学 | Preparation method of wear-resistant super-hydrophobic coating on surface of sampling needle |
| CN112547462B (en) * | 2020-11-23 | 2022-12-09 | 重庆大学 | Preparation method of wear-resistant super-hydrophobic coating on surface of sampling needle |
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