CN106119927B - The method that electrochemical treatments prepare anisotropy water-oil separating copper mesh - Google Patents
The method that electrochemical treatments prepare anisotropy water-oil separating copper mesh Download PDFInfo
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- CN106119927B CN106119927B CN201610478384.7A CN201610478384A CN106119927B CN 106119927 B CN106119927 B CN 106119927B CN 201610478384 A CN201610478384 A CN 201610478384A CN 106119927 B CN106119927 B CN 106119927B
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- 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
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
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- 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
- C25D11/022—Anodisation on selected surface areas
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
Abstract
The invention discloses the methods that electrochemical treatments prepare anisotropy water-oil separating copper mesh, belong to electrochemical treatments technical field.The method prepares oxide side and reduction face on two surfaces of copper mesh respectively by improved anodizing and cathodic electrodeposition.The technical issues of copper mesh can be good at realizing that water-oil separating material controls the selectivity that oil or water are separated, solving the water in oil and oil that a kind of material is provided simultaneously in separation water outlet.Product prepared by the present invention need not carry out subsequent processing and just can be directly used for water-oil separating, and repeatability is preferably.Also, preparation method of the present invention is simple, and the period is short, and product cost is low, easy to use, can mass produce.
Description
Technical field
The invention belongs to electrochemical treatments technical fields, are related to improved anodizing technology and negative electrode electro-deposition technology,
With reference to the performance difference of the copper oxide and cuprous oxide generated in separate type single side treatment technology and processing procedure inherently,
Realize the preparation of structure and property anisotropy copper mesh.Specifically, refer to that a kind of electrochemical treatments prepare anisotropy oil
The method that water detaches copper mesh.
Background technology
With industrialized development, more and more water resources are polluted by oils, and therefore, water-oil separating problem is more next
More cause the concern of people.Although traditional water-oil separating material can realize simple water-oil separating, be limited to its two
The homogeneity of surface properties, cause its can only selectivity separation water outlet or oil.Anodizing technology is by anode metal
It is upper to form fine and close oxidation film, the defects of so as to fulfill metal skin hardness, wear resistance etc. is overcome, expand it using model
It encloses, prolongs the service life.Negative electrode electro-deposition technology refers to simple metal ion or complex ion by electrochemical method in solid
Metallic atom is reduced on (conductor or semiconductor) surface and is attached to electrode surface, so as to obtain the process of a metal layer.Tradition
The problem of separation that water-oil separating material single can only realize oil or water.
Invention content
The problem of for current water-oil separating field, the present invention devise one kind by improved anodizing
And cathodic electrodeposition, with reference to the copper oxide and cuprous oxide generated in separate type single side treatment technology and processing procedure in itself
Intrinsic performance difference is prepared the technology of wellability anisotropy water-oil separating copper mesh, is included the following steps：
The first step, the preparation of electrolyte；
Second step, copper mesh surface preparation；
Third walks, and copper mesh B faces prepare ultra-hydrophilic surface using anodizing；
4th step, copper mesh A faces prepare super hydrophobic surface using cathodic electrodeposition.
The copper mesh can be good at realizing that water-oil separating material controls the selectivity that oil or water are separated, and solve
A kind of material is provided simultaneously with the technical issues of water in the oil and oil in separation water outlet.After product prepared by the present invention is without carrying out
Continuous processing just can be directly used for water-oil separating, and repeatability is preferably.Also, preparation method of the present invention is simple, and the period is short, product cost
It is low, it is easy to use, it can mass produce.
The method that electrochemical treatments provided by the invention prepare anisotropy water-oil separating copper mesh, advantage are：
1st, water-oil separating copper mesh prepared by the present invention effectively realizes water-oil separating material and oil or water is separated
Come selectivity control, solve traditional water-oil separating material can not realize a kind of material be provided simultaneously with separation water outlet in oil and
The technical issues of water in oil.
2nd, water-oil separating copper mesh prepared by the present invention is avoided further only by simple electrochemical treatments to grease point
The step of further physical chemistry modifying being done from material.
3rd, short preparation period of the present invention, method is simple, and product cost is low, easy to use, can mass produce.
Description of the drawings
Fig. 1 is improved anodizing technology provided by the invention and negative electrode electro-deposition technology, at separate type single side
Manage technique device schematic diagram.(a) anodizing (b) cathodic electrodeposition.
Fig. 2 is the SEM pictures of the copper mesh of anodic oxidation and the negative electrode electro-deposition processing of different multiples：In figure a) and A) for not
Handle the SEM pictures on copper mesh surface；B) and B) be anodized copper mesh SEM pictures；C) and C) be negative electrode electro-deposition skill
Art handles the SEM pictures of copper mesh.Wherein a), b), c) scale be 100 μm；A), B), C) scale be 10 μm.
Fig. 3 is the contact angle that metal mesh for oil-water separation different surfaces oil with water：Reduction face prepared by negative electrode electro-deposition, sun
Oxide side and untreated copper net surface prepared by pole oxidation is to the contact angle of water and underwater oil.
Fig. 4 is the selective water-oil separating behavior schematic diagram on anisotropy water-oil separating copper mesh surface.
Specific embodiment
Below in conjunction with drawings and examples, the present invention is described in further detail.
The method that the present invention provides anisotropy water-oil separating copper mesh prepared by a kind of electrochemical treatments, the method pass through
Improved anodizing technology and negative electrode electro-deposition technology, with reference to what is generated in separate type single side treatment technology and processing procedure
The performance difference of copper oxide and cuprous oxide inherently realizes the preparation of structure and property anisotropy copper mesh.It is prepared
The copper mesh anodic oxidation face show as super hydrophilic, underwater superoleophobic in air, and negative electrode electro-deposition face shows as surpassing in air
Hydrophobic, super oleophylic under water can be good at realizing the Selective Separation to oil or water in oil water mixture, solve traditional oils
The selectivity control that the problem of separation that water separation material single can only realize oil or water is separated.
The method that electrochemical treatments provided by the invention prepare anisotropy water-oil separating copper mesh, the specific steps are：
The first step, the preparation of electrolyte：
Concentration is prepared in the sodium hydroxide solution of 0.02mol/L to 1mol/L as anode oxidation process electrolyte, is prepared
Concentration is in electrolyte of the copper nitrate solution as cathodic electrodeposition process of 0.02mol/L to 1mol/L.
Second step, copper mesh surface preparation：
The brass wire diameter of copper mesh is chosen between 20~50 μm, mesh diameter first cuts copper mesh between 30~70 μm
For long 2cm, then the rectangle of wide 1cm is cleaned by ultrasonic it 20 minutes respectively with second alcohol and water, is finally dried in drying box
It is dry, it takes out for use.The drying preferred time is 15 minutes.
Third walks, and anodizing prepares ultra-hydrophilic surface：
Water proof processing is carried out to second step pretreatment copper mesh wherein one side (A faces) first, i.e., the A of copper mesh is sealed with marine glue
Face forms water barrier in A faces, prevents it from being handled, and then carries out anode to copper mesh another side (B faces) using D.C. regulated power supply
Oxidation processes, as shown in Figure 1a.Electrolyte is sodium hydroxide solution prepared by the first step, and anode is water proof treated copper mesh,
Cathode is that the distance between platinum electrode, electrode is 0.5~1.5cm, and the electric current for controlling anode oxidation process is 0.2~0.7A, positive
Pole oxidization time is 1~3min.After the completion of processing, take out copper mesh, remove water barrier, then with deionized water clean 15 minutes it
Room temperature naturally dry is for use afterwards, obtains A faces at this time as untreated face, and the copper mesh that B faces are anodic oxidation face.
4th step, cathodic electrodeposition prepare super hydrophobic surface：
The oxide side (B faces) of copper mesh after above-mentioned third step is dried carries out water proof processing, prepares water barrier, prevents its quilt
It handles again, negative electrode electro-deposition processing then is carried out to the A faces of copper mesh, as shown in Figure 1 b.Electrolyte is nitre prepared by the first step
Sour copper solution, anode are platinum electrode, and cathode is the A faces of copper mesh, A facing towards the distance between platinum electrode, two electrodes for 0.5~
1.5cm, it is 1~5V to control the voltage in cathodic electrodeposition process, and the negative electrode electro-deposition time is 0.5~1.5min.Processing is completed
Afterwards, copper mesh is taken out, removes water barrier, room temperature naturally dry after then clean A, B two sides 15 minutes with deionized water at this time must
To A faces are reduction face and anisotropy water-oil separating copper mesh that B faces are oxide side.
The one side prepared by negative electrode electro-deposition after above first anodic oxidation is super hydrophilic, on one side super-hydrophobic wellability respectively to
Different in nature water-oil separating copper mesh, two sides show the selective penetrated property for oil or for water respectively, effectively realize grease point
The selectivity that oil or water are separated is controlled from material.
Embodiment 1
The present embodiment provides anodic oxidations and cathodic electrodeposition to prepare super hydrophilic, the super-hydrophobic water-oil separating on one side of one side
The method of copper mesh, the specific steps are：
The first step, the preparation of electrolyte：
0.2g sodium hydrate particles are weighed, is dissolved in 250g deionized waters, is stirred to and is completely dissolved.Weigh 1.16g nitre
Sour copper is dissolved in 200g deionized waters, is stirred to and is completely dissolved.
Second step, copper mesh surface preparation：
Copper mesh is cut to long 2cm, then the rectangle of wide 1cm respectively carries out it with second alcohol and water being cleaned by ultrasonic each
It 20 minutes, is finally dried in drying box for use.The copper mesh wire side brass wire diameter is 20 μm, and mesh diameter is 30 μm.
Third walks, and anodizing prepares ultra-hydrophilic surface：
Water barrier is prepared to the copper mesh A faces taken out in drying box first, water proof processing is carried out, i.e., seals copper mesh with marine glue
A faces, then using D.C. regulated power supply, to copper mesh, non-water proof face B faces carry out anodized.Electrolyte is first step system
Standby sodium hydroxide solution, anode are the B faces of copper mesh, and cathode is that the distance between platinum electrode, electrode is 0.5cm, controls anode
The electric current of oxidation process is 0.2A, anodizing time 1min.After the completion of processing, copper mesh is taken out, removes water barrier, Ran Houyong
Room temperature naturally dry after deionized water is cleaned 15 minutes, obtains the copper mesh that A faces are untreated face and B faces are oxide side at this time.
4th step, cathodic electrodeposition prepare super hydrophobic surface：
The oxide side B faces of copper mesh after third step is dried prepare water barrier, carry out water proof processing, prevent it from being located again
Then reason carries out the A faces of copper mesh negative electrode electro-deposition processing, electrolyte is copper nitrate solution prepared by the first step, and anode is platinum
Electrode, cathode are the A faces of copper mesh, and the A of copper mesh is 0.5cm facing towards the distance between platinum electrode, two electrodes, and control cathode electricity sinks
Voltage during product is 1V, and the negative electrode electro-deposition time is 0.5min.After the completion of processing, copper mesh is taken out, removes water barrier, then
Naturally dry after cleaning A, B two sides 15 minutes with deionized water, it is reduction face and copper that B faces are oxide side to obtain A faces at this time
Net.
Embodiment 2
The present embodiment provides anodic oxidations and cathodic electrodeposition to prepare super hydrophilic, the super-hydrophobic water-oil separating on one side of one side
The method of copper mesh, the specific steps are：
The first step, the preparation of electrolyte：
1g sodium hydrate particles are weighed, is dissolved in 250g deionized waters, is stirred to and is completely dissolved.Weigh 5.8g nitric acid
Copper is dissolved in 200g deionized waters, is stirred to and is completely dissolved.
Second step, copper mesh surface preparation：
Copper mesh is cut to long 2cm, then the rectangle of wide 1cm respectively carries out it with second alcohol and water being cleaned by ultrasonic each
It 20 minutes, is finally dried in drying box for use.The copper mesh wire side brass wire diameter is 50 μm, and mesh diameter is 70 μm.
Third walks, and anodizing prepares ultra-hydrophilic surface：
First to preparing water barrier on the copper mesh A faces taken out in drying box, water proof processing is carried out, i.e., seals copper with marine glue
Then the A faces of net carry out anodized using D.C. regulated power supply to copper mesh B faces.Electrolyte is hydrogen prepared by the first step
Sodium hydroxide solution, anode are copper mesh B faces, and cathode is that the distance between platinum electrode, electrode is 1.5cm, controls anode oxidation process
Electric current be 0.7A, anodizing time 3min.After the completion of processing, copper mesh is taken out, water barrier is removed, then uses deionized water
Room temperature naturally dry after cleaning 15 minutes, obtains the copper mesh that A faces are untreated face and B faces are oxide side at this time.
4th step, cathodic electrodeposition prepare super hydrophobic surface：
The oxide side B faces of copper mesh after third step is dried prepare water barrier, carry out water proof processing, prevent it from being located again
Then reason carries out the A faces of copper mesh negative electrode electro-deposition processing, electrolyte is copper nitrate solution prepared by the first step, and anode is platinum
Electrode, cathode are the A faces of copper mesh, and A is 1.5cm facing towards the distance between platinum electrode, two electrodes, controls cathodic electrodeposition process
In voltage for 5V, the negative electrode electro-deposition time is 1.5min.After the completion of processing, take out copper mesh, remove water barrier, then spend from
Sub- water cleaning A, B two sides naturally dry after 15 minutes, it is reduction face and copper mesh that B faces are oxide side to obtain A faces at this time.
Embodiment 3
The present embodiment provides anodic oxidations and cathodic electrodeposition to prepare super hydrophilic, the super-hydrophobic water-oil separating on one side of one side
The method of copper mesh, the specific steps are：
The first step, the preparation of electrolyte：
0.5g sodium hydrate particles are weighed, is dissolved in 250g deionized waters, is stirred to and is completely dissolved.Weigh 2.9g nitric acid
Copper is dissolved in 200g deionized waters, is stirred to and is completely dissolved.
Second step, copper mesh surface preparation：
Copper mesh is cut to long 2cm, then the rectangle of wide 1cm respectively carries out it with second alcohol and water being cleaned by ultrasonic each
It 20 minutes, is finally dried in drying box for use.The copper mesh wire side brass wire diameter is 35 μm, and mesh diameter is 50 μm.
Third walks, and anodizing prepares ultra-hydrophilic surface：
Water proof processing is carried out to the copper mesh A faces taken out in drying box first, i.e., the A of copper mesh is sealed with marine glue (water barrier)
Then face carries out anodized using D.C. regulated power supply to copper mesh B faces.Electrolyte is sodium hydroxide prepared by the first step
Solution, anode are copper mesh B faces, and cathode is that the distance between platinum electrode, electrode is 1cm, and the electric current for controlling anode oxidation process is
0.5A, anodizing time 2min.After the completion of processing, copper mesh is taken out, water barrier is removed, then cleans 15 points with deionized water
Room temperature naturally dry after clock obtains the copper mesh that A faces are untreated face and B faces are oxide side at this time.
4th step, cathodic electrodeposition prepare super hydrophobic surface：
The oxide side B faces of copper mesh after third step is dried prepare water barrier, carry out water proof processing, prevent it from being located again
Then reason carries out the A faces of copper mesh negative electrode electro-deposition processing, electrolyte is copper nitrate solution prepared by the first step, and anode is platinum
Electrode, cathode are the A faces of copper mesh, and A is 1cm facing towards the distance between platinum electrode, two electrodes, is controlled in cathodic electrodeposition process
Voltage for 3V, the negative electrode electro-deposition time is 1min.After the completion of processing, copper mesh is taken out, water barrier is removed, then uses deionized water
A, B two sides naturally dry after 15 minutes is cleaned, it is reduction face and copper mesh that B faces are oxide side to obtain A faces at this time.
Microcosmic shape is carried out to the two sides of anisotropy water-oil separating copper mesh prepared in embodiment using environmental scanning electronic microscope
Looks are observed：For anodized surface, as shown in Fig. 2, copper mesh surface exhibits nano-scale splits striated structure, and negative electrode electro-deposition
The copper mesh surface of processing, there are nano level chondritics, they considerably increase the roughness on copper mesh surface, this causes copper mesh
Hydrophilic oxide side it is more hydrophilic, hydrophobic reduction face is more hydrophobic.
The behavior of water droplet and oil droplet (chloroform) on two surfaces of copper mesh is observed using contact angle measurement,
As shown in figure 3, the contact angle of water is 151.3 ° on reduction face prepared by cathodic electrodeposition, in oxygen prepared by anodic oxidation reactions
The contact angle of water is 21.3 ° on change face；Meanwhile reduction is 0 ° in face of the contact angle of underwater oil, contact of the oxide side to underwater oil
Angle is 152.1 °.Therefore it can obtain to draw a conclusion, for copper mesh prepared by embodiment, the oxide side prepared from anodizing
The reduction face prepared to cathodic electrodeposition, oil can be quickly through, and water cannot pass through；Conversely, from reduction face to oxidation
Face, water can be quickly through, and oil cannot pass through.As shown in figure 4, test(ing) liquid a) is oil water mixture, when copper mesh
Oxide side is upper, and reduction face is under, and with the dropwise addition of oil water mixture, oil can be with quick penetration sample, and water can not pass through, 2s
After completing filling, 3s completes separation, and 5min figures are with the comparison of 3s figures without other variations.B) test(ing) liquid is oil water mixture,
When the reduction face of copper mesh is upper, oxide side is under, and with the dropwise addition of oil water mixture, water can be quickly through sample, and oil is then
It can not pass through.
Claims (5)
1. the method that electrochemical treatments prepare anisotropy water-oil separating copper mesh, it is characterised in that：Include the following steps：
The first step, the preparation of electrolyte；
Second step, copper mesh surface preparation；
Third walks, and copper mesh B faces prepare ultra-hydrophilic surface using anodizing；
4th step, copper mesh A faces prepare super hydrophobic surface using cathodic electrodeposition；
It is molten that the electrolyte includes the copper nitrate that the sodium hydroxide solution that uses of anodizing and cathodic electrodeposition use
Liquid；
Concentration of sodium hydroxide solution is in 0.02mol/L to 1mol/L；Copper nitrate solution concentration is in 0.02mol/L to 1mol/L；
Third step anodizing prepares the detailed process of ultra-hydrophilic surface and is：Water barrier is prepared in the A faces of copper mesh, electrolyte is
Sodium hydroxide solution, anode are the B faces of copper mesh, and cathode is that the distance between platinum electrode, electrode is 0.5~1.5cm, controls anode
The electric current of oxidation process is 0.2~0.7A, and anodizing time is 1~3min；After the completion of processing, copper mesh is taken out, removes water proof
Layer, room temperature naturally dry after then being cleaned 15 minutes with deionized water, super hydrophilic oxidation is prepared in the B faces of copper mesh
Face；
The detailed process that 4th step cathodic electrodeposition prepares super hydrophobic surface is：Water barrier is prepared in oxide side, electrolyte is
Copper nitrate solution, anode are platinum electrode, and cathode is the A faces of copper mesh, A facing towards the distance between platinum electrode, two electrodes for 0.5~
1.5cm, it is 1~5V to control the voltage in cathodic electrodeposition process, and the negative electrode electro-deposition time is 0.5~1.5min；Processing is completed
Afterwards, copper mesh is taken out, removes water barrier, then clean the room temperature naturally dry later of two sides 15 minutes with deionized water, in the A of copper mesh
The reduction face of super oleophylic is prepared in face；
The water barrier is one layer of marine glue.
2. the method that electrochemical treatments according to claim 1 prepare anisotropy water-oil separating copper mesh, it is characterised in that：
In second step, the brass wire diameter of the copper mesh of selection is between 20~50 μm, and mesh diameter is between 30~70 μm.
3. the method that electrochemical treatments according to claim 1 prepare anisotropy water-oil separating copper mesh, it is characterised in that：
Second step copper mesh surface preparation includes, and copper mesh first is cut to long 2cm, then the rectangle of wide 1cm uses second alcohol and water respectively
It is cleaned by ultrasonic 20 minutes, is finally dried 15 minutes in drying box, taken out for use.
4. a kind of anisotropy water-oil separating copper mesh, it is characterised in that：It is prepared using the preparation method in claim 1；
The two sides of the copper mesh is respectively oxide side and reduction face, realizes the separation of oil water mixture.
5. the application of anisotropy water-oil separating copper mesh according to claim 4, it is characterised in that：Oil water mixture is in institute
The oxide side for stating copper mesh instills, then oil cannot be passed through by copper mesh and water；When oil water mixture the reduction face of copper mesh instill, then
Water cannot be passed through by copper mesh and oil.
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| CN107043948A (en) * | 2017-04-27 | 2017-08-15 | 湖北大学 | A kind of preparation method of the super hydrophilic/superoleophobic stainless (steel) wire under water separated for oil hydrosol |
| CN109381893B (en) * | 2017-08-03 | 2020-04-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Super-hydrophilic oleophobic material, preparation method and application thereof |
| CN108468078B (en) * | 2018-03-15 | 2021-02-09 | 北京航空航天大学 | Preparation method and application of gradient wettability surface |
| 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 |
| CN112774256B (en) * | 2020-12-17 | 2022-02-18 | 北京航空航天大学 | Preparation method and application of Janus copper mesh with heterostructure in air |
| CN114250457A (en) * | 2021-12-29 | 2022-03-29 | 北京航空航天大学 | Janus-gradient composite wettability copper wire capable of realizing ultra-fast liquid drop transmission and preparation method thereof |
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| CN103320832B (en) * | 2013-06-25 | 2016-04-06 | 北京航空航天大学 | The method of wetting property gradient surface is constructed in anodic oxidation |
| CN104726926A (en) * | 2013-12-20 | 2015-06-24 | 中国科学院兰州化学物理研究所 | Bionic micro-nano structure aluminium surface preparation method |
| CN103849905A (en) * | 2014-03-26 | 2014-06-11 | 哈尔滨工业大学 | Preparation method of oil/water separation material |
| CN105088297A (en) * | 2015-07-09 | 2015-11-25 | 吉林大学 | Preparation method of bionic oil-water separation copper net |
| CN105641973A (en) * | 2016-01-25 | 2016-06-08 | 四川大学 | Preparation method of nano-structure oil-water separation net membrane with self-cleaning and underwater super-oleophobic characteristics |
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