CN105088297A - Preparation method of bionic oil-water separation copper net - Google Patents
Preparation method of bionic oil-water separation copper net Download PDFInfo
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Abstract
The invention relates to a preparation method of a bionic oil-water separation copper net; and the preparation method is enlightened by hydrophobic self-cleanness of natural plant leaf surfaces, and an electrochemical deposition method is adopted to prepare super-hydrophobic surfaces with bionic micro-nanoscale double-layer classification. The method comprises the following steps: firstly, diluted hydrochloric acid, acetone and distilled water are used to clean the copper net for pretreatment; then, the copper net is dipped in electroplating liquid for electrochemical deposition, so that the surface morphology features are changed, and a bionic micro-nanoscale double-layer classification structure is formed on the surface of the copper net; after the electric deposition is finished, the copper net with the bionic micro-nanoscale double-layer classification structure is dipped into modifying solution, so that the surface thereof is formed with a low-surface-energy film; and finally, the surface of the copper net has super-hydrophobic and super-oleophylic characteristics. The preparation method of the bionic oil-water separation copper net is simple in operation, controllable in experimental parameters and low in cost, and can be used for manufacturing oil-water separation materials; and the materials have the super-hydrophobic and super-oleophylic characteristics, excellent mechanical stability and the recycling property.
Description
Technical field
The present invention relates to a kind of preparation method of oily water separation copper mesh of super-hydrophobic super-oleophylic, particularly a kind of method adopting electrochemical deposition method to prepare bionical oily water separation copper mesh.
Background technology
In the past several years, whole world oil spill accident constantly occurred, and a large amount of industrial oily waste water is directly discharged in environment simultaneously, pollutes, also serious harm human health to air and soil.Oily water separation has become a stern challenge, causes extensive concern at home and abroad.At present, oily sewage disposal method is mainly divided into: membrane separation process, oil skimmer vessel method, centrifugal separation, biological oxidation process, gravitational separation process, magnetic method, flotation process, absorption method and chemical method.But there is apparatus expensive, complicated process steps in most for the treatment of process, the treatment time is long and cause the problems such as regeneration of contaminated to environment.Although simple, the efficient and method of membrane separation process process oil water separation process is widely used, the problems such as vulnerable to pollution, non-easy cleaning, working cost be high in actual applications.For this reason, investigators are devoted to development of new mould material, if super hydrophobic film, super oleophobic membrane, super-hydrophobic super-oleophylic film etc. are to overcome the problems referred to above.
In oil water separation process, use the selectivity permeable material with special wettability that oil can be made optionally to be repelled by water through grid, easily solve oily water separation problem.At occurring in nature, many plants and insect show excellent super-hydrophobicity, as lotus leaf, roseleaf, marigold petal, rice leaf, water skipper, butterfly's wing and mosquito eyes etc.Be subject to the inspiration of above-mentioned animals and plants hydrophobic property, at the super-hydrophobic sample of ordinary metallic material surface preparation, and can be applied in Practical Project.
People have attempted using multiple method to prepare the copper mesh of super-hydrophobic and super oil-wet behavior, as chemical etching, and electrochemical deposition method, electrical spinning method, sol-gel method, CVD etc.Wherein, electrochemical deposition method is the process being formed the double-deck hierarchy of micro-nano-scale by electrochemistry approach at material surface, and this method is easy, quick, with low cost and easily realize.And on copper mesh, prepare the super-hydrophobic super-oleophylic surface with micro-nano hierarchy, and realize efficient oily water separation target, this is a kind of trial newly, significant to the development of current oily sewage disposal technology.
Summary of the invention
Object of the present invention is just, provide a kind of method adopting electrochemical deposition method to prepare bionical oily water separation copper mesh, made copper mesh has micro-nano hierarchy, and surface hydrophobicity significantly improves, and can realize efficient oily water separation.
The object of the invention is to be achieved through the following technical solutions:
The present invention copies the feature of super-hydrophobicity microtexture in the animal and plant bodies such as water skipper, lotus leaf, Rose and paddy rice, adopt electro-deposition method, copper mesh is prepared the surface of the double-deck hierarchy of micro-nano-scale of similar natural plant leaves, improve the surface property of copper mesh, make it have super-hydrophobic super-oleophylic characteristic.
A preparation method for bionical oily water separation copper mesh, comprises the following steps:
A, pre-treatment is carried out to copper mesh: copper mesh is positioned over ultrasonic cleaning in dilute hydrochloric acid, acetone and distilled water successively, the oxide film on removing surface and dirt;
B, electrochemical deposition: carry out electrolysis by the copper mesh immersion plating liquid after cleaning, described electroplate liquid is made up of 0.12-0.18mol/L copper sulfate and 0.1-0.3mol/L sulfuric acid, electroplate liquid volume is 150-250ml, under room temperature, using copper coin as anode, copper mesh carries out copper mesh plating as negative electrode, voltage is 3.5-4.5V, electroplating time is 100-400s, after replacement(metathesis)reaction completes, forming microtexture on copper mesh surface is bionical mastoid process body, in copper mesh substrate, namely form the double-deck hierarchy surface of biomimetic micro-nano yardstick;
C, finishing: after having electroplated, the copper mesh with micro-nano double-deck hierarchy is dipped into containing 1.5 × 10
-3in the lauric ethanolic soln of mol/L, take out after 10h, dry under protective atmosphere, just obtain the copper mesh with super-hydrophobic super-oleophylic characteristic.
Beneficial effect of the present invention is: it is simple to operate for bionical oily water separation copper mesh preparation method, experiment parameter is controlled and with low cost, this method can be used for manufacturing oily water separation material, this material has super-hydrophobic super-oleophylic, good mechanical stability and recycling character.
Accompanying drawing explanation
Fig. 1 is the process schematic that employing electrochemical deposition method of the present invention prepares bionical oily water separation copper mesh method.
Fig. 2 be the present invention at voltage 4.0V, the SEM on the bionical oily water separation copper mesh galvanic deposit surface of inventing under different electroplating time figure.
Fig. 2 a is the SEM figure on bionical oily water separation copper mesh galvanic deposit surface of the present invention, and wherein, electroplating time is 0s.
Fig. 2 b is the SEM figure on bionical oily water separation copper mesh galvanic deposit surface of the present invention, and wherein, electroplating time is 100s.
Fig. 2 c is the SEM figure on bionical oily water separation copper mesh galvanic deposit surface of the present invention, and wherein, electroplating time is 150s.
Fig. 2 d is the SEM figure on bionical oily water separation copper mesh galvanic deposit surface of the present invention, and wherein, electroplating time is 250s.
Fig. 2 e is the SEM figure on bionical oily water separation copper mesh galvanic deposit surface of the present invention, and wherein, electroplating time is 300s.
Fig. 2 f is the SEM figure on bionical oily water separation copper mesh galvanic deposit surface of the present invention, and wherein, electroplating time is 400s.
Fig. 3 is the contact angle that the present invention obtains surface the different electrochemical deposition time, and wherein, galvanic deposit voltage is 4V, and electroplating time is respectively 100s, 150s, 200s, 250s, 300s, 350s and 400s.
In figure, 1. direct supply 2. copper coin (anode) 3. beaker 4. electroplate liquid 5. agitator 6. copper mesh (negative electrode).
Embodiment
The inspiration that the present invention is subject to natural plant leaves surface hydrophobicity self-cleaning, adopts electrochemical deposition method on copper mesh matrix, prepare the double-deck hierarchy surface of the micro-nano-scale with natural plant leaves, utilizes its super-hydrophobic super-oleophylic characteristic, realize efficient oily water separation.
The method is first with dilute hydrochloric acid, acetone and distilled water cleaning copper mesh pre-treating technology; Carry out electrochemical deposition by copper mesh immersion plating liquid again, the shape characteristic on copper mesh surface is changed, form the double-deck hierarchy of biomimetic micro-nano yardstick; After galvanic deposit completes, the copper mesh with the double-deck hierarchy of biomimetic micro-nano yardstick is immersed modification solution and makes its surface form low surface energy film, and have super-hydrophobic and super oil-wet behavior, concrete steps are as follows:
A, pre-treatment is carried out to copper mesh: copper mesh is positioned over ultrasonic cleaning in dilute hydrochloric acid, acetone and distilled water successively, the oxide film on removing surface and dirt;
B, electrochemical deposition: carry out electrolysis by the copper mesh immersion plating liquid after cleaning, described electroplate liquid is made up of 0.12-0.18mol/L copper sulfate and 0.1-0.3mol/L sulfuric acid, electroplate liquid volume is 150-250ml, under room temperature, using copper coin as anode, copper mesh carries out copper mesh plating as negative electrode, voltage is 3.5-4.5V, electroplating time is 100-400s, after replacement(metathesis)reaction completes, forming microtexture on copper mesh surface is bionical mastoid process body, in copper mesh substrate, namely form the double-deck hierarchy surface of biomimetic micro-nano yardstick;
C, finishing: after having electroplated, the copper mesh with the double-deck hierarchy of biomimetic micro-nano is dipped into containing 1.5 × 10
-3in the lauric ethanolic soln of mol/L, take out after 10h, dry under protective atmosphere, just obtain the copper mesh with super-hydrophobic super-oleophylic characteristic.
The difference of copper mesh electroplating time in described step B, can affect the shape characteristic on its surface.
Copper mesh area of the present invention is 4*4cm
2, the aperture of copper mesh substrate is 100 μm, and electrochemical deposition back aperture slightly reduces.
Embodiment 1
A preparation method for bionical oily water separation copper mesh, concrete steps are as follows:
A, pre-treatment is carried out to copper mesh: copper mesh is positioned over ultrasonic cleaning 10min in dilute hydrochloric acid, acetone and distilled water successively, the oxide film on removing surface and dirt;
B, electrochemical deposition: carry out electrolysis by the copper mesh immersion plating liquid after cleaning, described electroplate liquid is made up of 0.12mol/L copper sulfate and 0.1mol/L sulfuric acid, electroplate liquid volume is 150ml, under room temperature, using copper coin as anode, copper mesh carries out copper mesh plating as negative electrode, voltage is 3.5V, and electroplating time is 100s, after having reacted, forming microtexture on copper mesh surface is bionical mastoid process body, in copper mesh substrate, namely form the double-deck hierarchy surface of biomimetic micro-nano yardstick;
C, finishing: after having electroplated, the copper mesh with the double-deck hierarchy of biomimetic micro-nano is dipped into containing 1.5 × 10
-3in the lauric ethanolic soln of mol/L, take out after 10h, dry under nitrogen flowing, drying temperature is 20 DEG C, and time of drying is 5min, just obtains the copper mesh with super-hydrophobic super-oleophylic characteristic.
Embodiment 2
A preparation method for bionical oily water separation copper mesh, concrete steps are as follows:
A, pre-treatment is carried out to copper mesh: copper mesh is positioned over ultrasonic cleaning 10min in dilute hydrochloric acid, acetone and distilled water successively, the oxide film on removing surface and dirt;
B, electrochemical deposition: carry out electrolysis by the copper mesh immersion plating liquid after cleaning, described electroplate liquid is made up of 0.12mol/L copper sulfate and 0.2mol/L sulfuric acid, electroplate liquid volume is 180ml, under room temperature, using copper coin as anode, copper mesh carries out copper mesh plating as negative electrode, voltage is 3.5V, and electroplating time is 150s, after having reacted, forming microtexture on copper mesh surface is bionical mastoid process body, in copper substrate, namely form the double-deck hierarchy surface of biomimetic micro-nano yardstick;
C, finishing: after having electroplated, the copper mesh with the double-deck hierarchy of biomimetic micro-nano is dipped into containing 1.5 × 10
-3in the lauric ethanolic soln of mol/L, take out after 10h, dry under nitrogen flowing, drying temperature is 20 DEG C, and time of drying is 5min, just obtains the copper mesh with super-hydrophobic super-oleophylic characteristic.
Embodiment 3
A preparation method for bionical oily water separation copper mesh, concrete steps are as follows:
A, pre-treatment is carried out to copper mesh: copper mesh is positioned over ultrasonic cleaning 10min in dilute hydrochloric acid, acetone and distilled water successively, the oxide film on removing surface and dirt;
B, electrochemical deposition: carry out electrolysis by the copper mesh immersion plating liquid after cleaning, described electroplate liquid is made up of 0.15mol/L copper sulfate and 0.2mol/L sulfuric acid, and electroplate liquid volume is 200ml; Under room temperature, using copper coin as anode, copper mesh carries out copper mesh plating as negative electrode, voltage is 4.0V, and electroplating time is 250s, after having reacted, forming microtexture on copper mesh surface is bionical mastoid process body, in copper substrate, namely form the double-deck hierarchy surface of biomimetic micro-nano yardstick;
C, finishing: after having electroplated, the copper mesh with the double-deck hierarchy of biomimetic micro-nano is dipped into containing 1.5 × 10
-3in the lauric ethanolic soln of mol/L, take out after 10h, dry under nitrogen flowing, drying temperature is 20 DEG C, and time of drying is 5min, just obtains the copper mesh with super-hydrophobic super-oleophylic characteristic.
Embodiment 4
A preparation method for bionical oily water separation copper mesh, concrete steps are as follows:
A, pre-treatment is carried out to copper mesh: copper mesh is positioned over ultrasonic cleaning 10min in dilute hydrochloric acid, acetone and distilled water successively, the oxide film on removing surface and dirt;
B, electrochemical deposition: carry out electrolysis by the copper mesh immersion plating liquid after cleaning, described electroplate liquid is made up of 0.15mol/L copper sulfate and 0.3mol/L sulfuric acid, electroplate liquid volume is 220ml, under room temperature, using copper coin as anode, copper mesh carries out copper mesh plating as negative electrode, voltage is 4.0V, and electroplating time is 300s, after having reacted, forming microtexture on copper mesh surface is bionical mastoid process body, in copper mesh substrate, namely form the double-deck hierarchy surface of biomimetic micro-nano yardstick;
C, finishing: after having electroplated, the copper mesh with the double-deck hierarchy of biomimetic micro-nano is dipped into containing 1.5 × 10
-3in the lauric ethanolic soln of mol/L, take out after 10h, dry under nitrogen flowing, drying temperature is 20 DEG C, and time of drying is 5min, just obtains the copper mesh with super-hydrophobic super-oleophylic characteristic.
Embodiment 5
A preparation method for bionical oily water separation copper mesh, concrete steps are as follows:
A, pre-treatment is carried out to copper mesh: copper mesh is positioned over ultrasonic cleaning 10min in dilute hydrochloric acid, acetone and distilled water successively, the oxide film on removing surface and dirt;
B, electrochemical deposition: carry out electrolysis by the copper mesh immersion plating liquid after cleaning, described electroplate liquid is made up of 0.18mol/L copper sulfate and 0.3mol/L sulfuric acid, electroplate liquid volume is 250ml, under room temperature, using copper coin as anode, copper mesh carries out copper mesh plating as negative electrode, voltage is 4.5V, and electroplating time is 400s, after having reacted, forming microtexture on copper mesh surface is bionical mastoid process body, in copper mesh substrate, namely form the double-deck hierarchy surface of biomimetic micro-nano yardstick;
C, finishing: after having electroplated, the copper mesh with the double-deck hierarchy of biomimetic micro-nano is dipped into containing 1.5 × 10
-3in the lauric ethanolic soln of mol/L, take out after 10h, dry under nitrogen flowing, drying temperature is 20 DEG C, and time of drying is 5min, just obtains the copper mesh with super-hydrophobic super-oleophylic characteristic.
Claims (6)
1. a preparation method for bionical oily water separation copper mesh, is characterized in that, comprise the following steps:
A, pre-treatment is carried out to copper mesh: copper mesh is positioned over ultrasonic cleaning in dilute hydrochloric acid, acetone and distilled water successively, the oxide film on removing surface and dirt;
B, electrochemical deposition: carry out electrolysis by the copper mesh immersion plating liquid after cleaning, described electroplate liquid is made up of 0.12-0.18mol/L copper sulfate and 0.1-0.3mol/L sulfuric acid, electroplate liquid volume is under 150-250ml room temperature, using copper coin as anode, copper mesh carries out copper mesh plating as negative electrode, voltage is 3.5-4.5V, electroplating time is 100-400s, after replacement(metathesis)reaction completes, forming microtexture on copper mesh surface is bionical mastoid process body, in copper mesh substrate, namely form the double-deck hierarchy surface of biomimetic micro-nano yardstick;
C, finishing: after having electroplated, the copper mesh with the double-deck hierarchy of biomimetic micro-nano is dipped into containing 1.5 × 10
-3in the lauric ethanolic soln of mol/L, soak after 10h and take out, dry under protective atmosphere, just obtain having the copper mesh that bionic super-hydrophobic surpasses oil-wet behavior.
2. the preparation method of a kind of bionical oily water separation copper mesh according to claim 1, it is characterized in that: electroplate liquid described in step B consists of 0.12mol/L copper sulfate and 0.1mol/L sulfuric acid, volume is 150ml, and voltage is 3.5V, and electroplating time is 100s.
3. the preparation method of a kind of bionical oily water separation copper mesh according to claim 1, it is characterized in that: electroplate liquid described in step B consists of 0.12mol/L copper sulfate and 0.2mol/L sulfuric acid, volume is 180ml, and voltage is 3.5V, and electroplating time is 150s.
4. the preparation method of a kind of bionical oily water separation copper mesh according to claim 1, it is characterized in that: electroplate liquid described in step B consists of 0.15mol/L copper sulfate and 0.2mol/L sulfuric acid, volume is 200ml, and voltage is 4.0V, and electroplating time is 250s.
5. the preparation method of a kind of bionical oily water separation copper mesh according to claim 1, it is characterized in that: electroplate liquid described in step B consists of 0.15mol/L copper sulfate and 0.3mol/L sulfuric acid, volume is 220ml, and voltage is 4.0V, and electroplating time is 300s.
6. the preparation method of a kind of bionical oily water separation copper mesh according to claim 1, it is characterized in that: electroplate liquid described in step B consists of 0.18mol/L copper sulfate and 0.3mol/L sulfuric acid, volume is 250ml, and voltage is 4.5V, and electroplating time is 400s.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119927A (en) * | 2016-06-27 | 2016-11-16 | 北京航空航天大学 | Electrochemical treatments prepares the method for anisotropy oil-water separation copper mesh |
| CN106319588A (en) * | 2016-10-31 | 2017-01-11 | 常州瑞丰特科技有限公司 | Electrochemical deposition based method for preparing metal material surface super-hydrophobic film |
| CN106823469A (en) * | 2017-01-10 | 2017-06-13 | 华南理工大学 | Super-hydrophobic super-oleophylic copper mesh without low-surface energy substance modification and preparation method thereof |
| CN106943887A (en) * | 2017-03-03 | 2017-07-14 | 四川农业大学 | A kind of method that step electro-deposition prepares super-hydrophobic/oleophylic oil-water separation mesh film |
| CN106987876A (en) * | 2017-03-03 | 2017-07-28 | 四川农业大学 | A kind of preparation method of super-hydrophobic/oleophylic water-oil separating Ni Cu composite deposite nethike embranes |
| CN108579467A (en) * | 2018-03-23 | 2018-09-28 | 吉林大学 | Bionical water-oil separationg film and preparation method based on butterfly's wing oil-stain-preventing characteristic and purposes |
| CN112853420A (en) * | 2021-01-14 | 2021-05-28 | 同曦集团有限公司 | Fluoride-free super-hydrophobic self-cleaning antibacterial mildew-proof antiviral stainless steel and preparation method thereof |
| CN110237568B (en) * | 2019-05-24 | 2022-03-08 | 深圳中拓天达环境工程有限公司 | Preparation method of high-flux switch type oil-water separation net film based on natural bionics |
| CN115364698A (en) * | 2022-05-19 | 2022-11-22 | 同济大学 | Organic metal framework loaded copper mesh surface separation membrane and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119927A (en) * | 2016-06-27 | 2016-11-16 | 北京航空航天大学 | Electrochemical treatments prepares the method for anisotropy oil-water separation copper mesh |
| CN106319588A (en) * | 2016-10-31 | 2017-01-11 | 常州瑞丰特科技有限公司 | Electrochemical deposition based method for preparing metal material surface super-hydrophobic film |
| CN106823469A (en) * | 2017-01-10 | 2017-06-13 | 华南理工大学 | Super-hydrophobic super-oleophylic copper mesh without low-surface energy substance modification and preparation method thereof |
| CN106943887A (en) * | 2017-03-03 | 2017-07-14 | 四川农业大学 | A kind of method that step electro-deposition prepares super-hydrophobic/oleophylic oil-water separation mesh film |
| CN106987876A (en) * | 2017-03-03 | 2017-07-28 | 四川农业大学 | A kind of preparation method of super-hydrophobic/oleophylic water-oil separating Ni Cu composite deposite nethike embranes |
| CN106943887B (en) * | 2017-03-03 | 2019-11-12 | 四川农业大学 | A kind of method that step electro-deposition prepares super-hydrophobic/oleophylic oil-water separation mesh film |
| CN108579467A (en) * | 2018-03-23 | 2018-09-28 | 吉林大学 | Bionical water-oil separationg film and preparation method based on butterfly's wing oil-stain-preventing characteristic and purposes |
| CN110237568B (en) * | 2019-05-24 | 2022-03-08 | 深圳中拓天达环境工程有限公司 | Preparation method of high-flux switch type oil-water separation net film based on natural bionics |
| CN112853420A (en) * | 2021-01-14 | 2021-05-28 | 同曦集团有限公司 | Fluoride-free super-hydrophobic self-cleaning antibacterial mildew-proof antiviral stainless steel and preparation method thereof |
| CN115364698A (en) * | 2022-05-19 | 2022-11-22 | 同济大学 | Organic metal framework loaded copper mesh surface separation membrane and preparation method and application thereof |
| CN115364698B (en) * | 2022-05-19 | 2023-08-04 | 同济大学 | Organic metal frame loaded copper mesh surface separation membrane and preparation method and application thereof |
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Application publication date: 20151125 |