CN109316976A - A kind of electrochemical process preparation bionical graphene composite film of super-hydrophobic super-oleophylic - Google Patents
A kind of electrochemical process preparation bionical graphene composite film of super-hydrophobic super-oleophylic Download PDFInfo
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- CN109316976A CN109316976A CN201811250750.9A CN201811250750A CN109316976A CN 109316976 A CN109316976 A CN 109316976A CN 201811250750 A CN201811250750 A CN 201811250750A CN 109316976 A CN109316976 A CN 109316976A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—Metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/38—Hydrophobic membranes
Abstract
The present invention provides a kind of method of graphene composite film for preparing super-hydrophobic super-oleophylic, preparation method includes the following steps, graphite foil and stainless steel cloth are cut into the identical sheet of size by (1), spare；(2) stainless steel cloth in step (1) is immersed into the hydrochloric acid in step (2), it is taken out after 3min, using distilled water flushing stainless steel cloth, cleaning is repeatedly remained to without hydrochloric acid, the stainless steel cloth of removing oxide layer is obtained, it is spare；(3) use step stainless steel cloth as cathode electrode, use graphite foil as anode electrode, it the use of ammonium sulfate and ammonium hydroxide mixed solution is electrolyte, stainless steel cloth is taken out after electrolysis, it is dried with baking oven is put into after distilled water repeated flushing stainless steel cloth to get super-hydrophobic super-oleophylic graphene composite film, graphene composite film prepared by the present invention, super-hydrophobic super-oleophylic, oil-water separation are good.
Description
Technical field
The present invention relates to graphene composite film preparation technical fields, and in particular to a kind of electrochemical process prepares super-hydrophobic super parent
The bionical graphene composite film of oil.
Background technique
Graphene, as a kind of presently found most thin, most hard, the strongest novel nano carbon materials of electrical and thermal conductivity performance
Material, is described as in the industry " dark fund ", is " king of new material ", it be carbon atom with sp2 key close-packed arrays at bi-dimensional cellular
Shape lattice structure has excellent electricity, the physicochemical properties such as mechanics and calorifics.The primary synthetic methods of graphene are as follows at present:
Physical mechanical stripping method, chemistry redox method, chemical vapour deposition technique and electrochemical stripping method.It is fast with national economy
Speed development, oil-containing industrial water largely discharge, and the accident of crude oil leakage also occurs often, has seriously endangered the health and life of the mankind
State balance.Therefore the current most important thing for solving environmental pollution has been processed into oily waste water.It is well known that using low surface
Wettability of the surface can be improved in energy material, generates super hydrophobic surface, and graphene has low-surface-energy, and it has hydrophobic parent
The property of oil.And the surface roughness for increasing material can also increase its hydrophobicity.
Summary of the invention
In order to solve the above-mentioned technical problem, the present invention adheres to graphite in coarse stainless steel wire using electrochemical process on the net
Alkene has successfully prepared super-hydrophobic super-oleophylic graphene composite film material.
The present invention provides a kind of method of graphene composite film for preparing super-hydrophobic super-oleophylic, the preparation method includes
Following steps,
(1) graphite foil and stainless steel cloth are cut into the identical sheet of size, it is spare；
(2) a certain amount of n-hexane and dehydrated alcohol are taken, taking the hydrochloric acid that mass fraction is 37%, 1:1 is mixed by volume with water
It closes, it is spare；The ammonium sulfate of 0.1M is configured, it is spare；Taking a certain amount of mass fraction is 25% ammonium hydroxide and ammonium sulfate
It is mixed by volume for 1:20, it is spare；
(3) stainless steel cloth in step (1) is first put into the n-hexane of 40mL and is impregnated two days, then taken out with distillation
It is put into the dehydrated alcohol of 40mL and impregnates one day after water washing.It is finally immersed into the hydrochloric acid in step (2), is taken out after 3min,
Using distilled water flushing stainless steel cloth, cleaning is repeatedly remained to without hydrochloric acid, obtains the stainless steel cloth of removing oxide layer, spare；
(4) use in step (3) except the stainless steel cloth of oxide layer is as cathode electrode, use stone in step (1)
Black foil is electrolyte using ammonium sulfate in step (2) and ammonium hydroxide mixed solution as anode electrode, and control decomposition voltage is 4-
8V, electrolysis time 2-5h take out stainless steel cloth, with baking oven drying is put into after distilled water repeated flushing stainless steel cloth, i.e.,
Obtain super-hydrophobic super-oleophylic graphene composite film.
Preferably, resulting aqueous solution is cleaned every time using pH test paper detection in above-mentioned steps (3), until pH test paper is aobvious
Show until being in neutrality.
Preferably, in above-mentioned steps (4), drying temperature is 60 DEG C, drying time 12h.
Preferably, the time of above-mentioned steps (4) electrolysis is 3-4 hours, and voltage control, in 5-7V, drying temperature is in perseverance
60 DEG C of temperature.
Preferably, stainless steel cloth mesh diameter is 40-100 μm in above-mentioned steps (1).
Preferably, ultrasonic vibration tools are cooperated using diamond fretsaw Wire cutting machine tool in above-mentioned steps (1), to stone
Black foil material is cut out.
Preferably, above-mentioned ultrasonic vibration tools power is 350W, ultrasonic frequency 20kHz.
The invention has the benefit that
(1) by using electrolysis method, graphene is directly become attached to the graphite of stainless steel wire net surface from graphene
Alkene, rather than graphene oxide is first generated, then graphene is being generated by restoring.Graphene is generated using one step of electrolysis method,
Graphene raw material does not waste, and technical process is also simpler, time saving.
(2) one step of electrolysis method provided by the invention generates graphene, without the use of necessary oxidant in Hummers method use
And reducing agent, entire technical process need to only use ammonium hydroxide and ammonium sulfate, three industrial wastes discharge amount is few, compared to traditional preparation work
Skill, harmful substance is few in the three wastes, and three-protection design is more single.So production technology provided by the invention, not only high income, and technique
Simply, three-protection design is at low cost, compared to existing production technology, has biggish improvement at yield, environmentally protective aspect.
(3) present invention adheres to graphene in stainless steel wire on the net and obtains graphene composite film, resulting stone by one-step method
Black alkene composite membrane had not only had the low surface property that graphene itself has, but also had both the roughness of silk screen, and composite membrane has super thin
Water super-oleophilic matter quickly can carry out water-oil separating and separation process is simply not necessarily to subsidiary conditions.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph that the graphene composite film that embodiment 1 is prepared amplifies 200 times.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with implementation of the invention
Example, technical scheme in the embodiment of the invention is clearly and completely described.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained without creative efforts, belongs to protection of the present invention
Range.
Embodiment 1
The present invention provides a kind of method of graphene composite film for preparing super-hydrophobic super-oleophylic, the preparation method include with
Lower step,
It is 4*3.5cm that 48 μm of stainless steel cloths, which are cut into size,2, it is also 4*3.5cm that graphite foil, which is cut into onesize,2, will
Stainless steel cloth, which is put into the n-hexane of 40mL, to be impregnated two days, and the dehydrated alcohol that 40mL is put into after being washed with distilled water is then taken out
It is middle to impregnate one day.10mL distilled water and 10mL hydrochloric acid are taken, the hydrochloric acid solution of configuration 1.4M is mixed, after immersion
Stainless steel cloth is put into hydrochloric acid solution, is taken out after 3min, is cleaned with a large amount of distilled water.Ammonium sulfate 2.6428g is taken, is poured into
In the beaker of 250mL, it is charged with 200mL water, is stirred evenly with glass bar.10mL ammonium hydroxide is taken with graduated cylinder, it is slowly fallen
Enter in ammonium sulfate, is stirred evenly with glass bar.With constant pressure bipolar electrode electro-chemical systems, the stainless steel crossed with salt acid soak
Silk screen is as cathode, and graphite foil is as anode, and as electrolyte, voltage control exists the ammonium hydroxide and ammonium sulfate mixed solution of configuration
4-8V ionizes 3 hours, stops experiment.Stainless steel cloth is taken out, 3 times wash with distilled water, is put into thermostatic drying chamber.Temperature
Degree is regulated to 60 DEG C, takes out after 12 hours.
The picture that shooting composite membrane amplifies 200 times under surface sweeping Electronic Speculum surveys the graphene of generation as shown in Fig. 1 in attached drawing
The water oil contact angle of composite membrane, the results showed that 150 ° of the water contact angle of the composite membrane, its oily contact angle are almost 0 °, are demonstrated by
Superpower hydrophobic oleophilic oil.Graphene composite film of the invention is used for kerosene and aqueous mixtures separation, it may be seen that by
In gravity, kerosene penetrates silk screen quickly, and water is because the superpower hydrophobicity of composite membrane has been left to above silk screen.Experiment knot
Fruit shows that the composite membrane can be used in water-oil separating.
Embodiment 2
The present invention provides a kind of method of graphene composite film for preparing super-hydrophobic super-oleophylic, the preparation method include with
Lower step, it is 4*3.5cm that 60 μm of stainless steel cloths, which are cut into size,2, it is also 4*3.5cm that graphite foil, which is cut into onesize,2, will
Stainless steel cloth, which is put into the n-hexane of 40mL, to be impregnated two days, and the dehydrated alcohol that 40mL is put into after being washed with distilled water is then taken out
It is middle to impregnate one day.10mL distilled water and 10mL hydrochloric acid are taken, the hydrochloric acid solution of configuration 1.4M is mixed, after immersion
Stainless steel cloth is put into hydrochloric acid solution, is taken out after 3min, is cleaned with a large amount of distilled water.Ammonium sulfate 2.6428g is taken, is poured into
In the beaker of 250mL, it is charged with 200mL water, is stirred evenly with glass bar.10mL ammonium hydroxide is taken with graduated cylinder, it is slowly fallen
Enter in ammonium sulfate, is stirred evenly with glass bar.With constant pressure bipolar electrode electro-chemical systems, the stainless steel crossed with salt acid soak
Silk screen is as cathode, and graphite foil is as anode, and as electrolyte, voltage control exists the ammonium hydroxide and ammonium sulfate mixed solution of configuration
4-8V ionizes 3 hours, stops experiment.Stainless steel cloth is taken out, 3 times wash with distilled water, is put into thermostatic drying chamber.Temperature
Degree is regulated to 60 DEG C, takes out after 12 hours.
Survey the water oil contact angle of the graphene composite film generated, the results showed that the water contact angle of the composite membrane is 145 °, it
Oily contact angle be almost 0 °, be demonstrated by superpower hydrophobic oleophilic oil.Graphene composite film of the invention is used for kerosene and water
Mixture separation, it may be seen that kerosene penetrates silk screen quickly, and water is because of the superpower hydrophobic of composite membrane due to gravity
Property has been left to above silk screen.The experimental results showed that the composite membrane can be used in water-oil separating.
Embodiment 3
The present embodiment prepares a kind of graphene composite film for preparing hydrophobic oleophilic oil, and the preparation method comprises the following steps,
It is 4*3.5cm that 80 μm of stainless steel cloths, which are cut into size,2, it is also 4*3.5cm that graphite foil, which is cut into onesize,2, will
Stainless steel cloth, which is put into the n-hexane of 40mL, to be impregnated two days, and the dehydrated alcohol that 40mL is put into after being washed with distilled water is then taken out
It is middle to impregnate one day.10mL distilled water and 10mL hydrochloric acid are taken, the hydrochloric acid solution of configuration 1.4M is mixed, after immersion
Stainless steel cloth is put into hydrochloric acid solution, is taken out after 3min, is cleaned with a large amount of distilled water.Ammonium sulfate 2.6432g is taken, is poured into
In the beaker of 250mL, it is charged with 200mL water, is stirred evenly with glass bar.10mL ammonium hydroxide is taken with graduated cylinder, it is slowly fallen
Enter in ammonium sulfate, is stirred evenly with glass bar.With constant pressure bipolar electrode electro-chemical systems, the stainless steel crossed with salt acid soak
Silk screen is as cathode, and graphite foil is as anode, and as electrolyte, voltage control exists the ammonium hydroxide and ammonium sulfate mixed solution of configuration
4-8V ionizes 3 hours, stops experiment.Stainless steel cloth is taken out, 3 times wash with distilled water, is put into thermostatic drying chamber.Temperature
Degree is regulated to 60 DEG C, takes out after 12 hours.Survey the water oil contact angle of the graphene composite film generated, the results showed that the composite membrane
136 ° of water contact angle, its oily contact angle is 0 °, is demonstrated by superpower hydrophobic oleophilic oil.Present invention demonstrates that working as stainless steel cloth
Mesh diameter when increasing to 80 μm, still can be used for water-oil separating.
Embodiment 4
The present embodiment prepares a kind of graphene composite film for preparing hydrophobic oleophilic oil, and the preparation method comprises the following steps,
It is 4*3.5cm that 100 μm of stainless steel cloths, which are cut into size,2, it is also 4*3.5cm that graphite foil, which is cut into onesize,2,
Stainless steel cloth is put into the n-hexane of 40mL and is impregnated two days, then takes out the anhydrous second for being put into 40mL after being washed with distilled water
It is impregnated one day in alcohol.10mL distilled water and 10mL hydrochloric acid are taken, the hydrochloric acid solution of configuration 1.4M is mixed, after immersion
Stainless steel cloth be put into hydrochloric acid solution, take out after 3min, cleaned with a large amount of distilled water.Ammonium sulfate 2.6432g is taken,
Enter in the beaker of 250mL, is charged with 200mL water, is stirred evenly with glass bar.10mL ammonium hydroxide is taken with graduated cylinder, slowly by it
It pours into ammonium sulfate, is stirred evenly with glass bar.With constant pressure bipolar electrode electro-chemical systems, crossed with salt acid soak stainless
Steel wire is as cathode, and graphite foil is as anode, and the ammonium hydroxide and ammonium sulfate mixed solution of configuration are as electrolyte, voltage control
In 4-8V, 3 hours are ionized, stop experiment.Stainless steel cloth is taken out, 3 times wash with distilled water, is put into thermostatic drying chamber.
Temperature is regulated to 60 DEG C, takes out after 12 hours.Survey the water oil contact angle of the graphene composite film generated, the results showed that the composite membrane
120 ° of water contact angle, its oily contact angle is 10 °, is demonstrated by superpower hydrophobic oleophilic oil.Present invention demonstrates that working as stainless steel wire
When the mesh diameter of net increases to 100 μm, it still can be used for water-oil separating.
Embodiment 5
The present embodiment prepares a kind of graphene composite film for preparing hydrophobic oleophilic oil, and the preparation method comprises the following steps,
It is 4*3.5cm that 120 μm of stainless steel cloths, which are cut into size,2, it is also 4*3.5cm that graphite foil, which is cut into onesize,2,
Stainless steel cloth is put into the n-hexane of 40mL and is impregnated two days, then takes out the anhydrous second for being put into 40mL after being washed with distilled water
It is impregnated one day in alcohol, takes 10mL distilled water and 10mL hydrochloric acid, the hydrochloric acid solution of configuration 1.4M is mixed, after immersion
Stainless steel cloth be put into hydrochloric acid solution, take out after 3min, cleaned with a large amount of distilled water.
Ammonium sulfate 2.6478g is taken, is poured into the beaker of 250mL, 200mL water is charged with, is stirred with glass bar
Uniformly.10mL ammonium hydroxide is taken with graduated cylinder, is poured slowly into ammonium sulfate, is stirred evenly with glass bar.With the double electricity of constant pressure
Pole electro-chemical systems, the stainless steel cloth for using salt acid soak to cross is as cathode, and graphite foil is as anode, the ammonium hydroxide and sulphur of configuration
Sour ammonium mixed solution ionizes 3 hours in 4-8V, stops experiment as electrolyte, voltage control.Stainless steel cloth is taken out, is used
Distilled water cleans 3 times, is put into thermostatic drying chamber.Temperature is regulated to 60 DEG C, takes out after 12 hours.
Survey the water oil contact angle of the graphene composite film generated, the results showed that 115 ° of the water contact angle of the composite membrane, it
Oily contact angle is 20 °, is demonstrated by superpower hydrophobic oleophilic oil.Present invention demonstrates that the mesh diameter when stainless steel cloth increases to
At 120 μm, it still can be used for water-oil separating.
Embodiment 6
The present embodiment prepares a kind of graphene composite film for preparing hydrophobic oleophilic oil, and the preparation method comprises the following steps,
It is 4*3.5cm that 150 μm of stainless steel cloths, which are cut into size,2, it is also 4*3.5cm that graphite foil, which is cut into onesize,2,
Stainless steel cloth is put into the n-hexane of 40mL and is impregnated two days, then takes out the anhydrous second for being put into 40mL after being washed with distilled water
It is impregnated one day in alcohol, takes 10mL distilled water and 10mL hydrochloric acid, the hydrochloric acid solution of configuration 1.4M is mixed, after immersion
Stainless steel cloth be put into hydrochloric acid solution, take out after 3min, cleaned with a large amount of distilled water.
Ammonium sulfate 2.6478g is taken, is poured into the beaker of 250mL, 200mL water is charged with, is stirred with glass bar
Uniformly.10mL ammonium hydroxide is taken with graduated cylinder, is poured slowly into ammonium sulfate, is stirred evenly with glass bar.With the double electricity of constant pressure
Pole electro-chemical systems, the stainless steel cloth for using salt acid soak to cross is as cathode, and graphite foil is as anode, the ammonium hydroxide and sulphur of configuration
Sour ammonium mixed solution ionizes 3 hours in 4-8V, stops experiment as electrolyte, voltage control.Stainless steel cloth is taken out, is used
Distilled water cleans 3 times, is put into thermostatic drying chamber.Temperature is regulated to 60 DEG C, takes out after 12 hours.
Survey the water oil contact angle of the graphene composite film generated, the results showed that the water contact angle of the composite membrane is 107 DEG C, it
Oily contact angle be 26 °, be demonstrated by superpower hydrophobic oleophilic oil.Present invention demonstrates that the mesh diameter when stainless steel cloth increases
When to 150 μm, it still can be used for water-oil separating.
Table 1 lists stainless steel steel wire mesh diameter in embodiment 1-6 and contacts to graphene composite film oil contact angle and water
The influence at angle, according to table 1, when stainless steel cloth mesh diameter is between 40-100 μm, hydrophobic effect is good, oleophylic effect
Fruit is unrelated with stainless steel cloth mesh diameter.
Influence of the 1 stainless steel cloth mesh diameter of table to graphene composite film oil contact angle and water contact angle
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that:
It is still possible to modify the technical solutions described in the foregoing embodiments, or part of technical characteristic is carried out etc.
With replacement；And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution
Spirit and scope.
Claims (7)
1. a kind of method for the graphene composite film for preparing super-hydrophobic super-oleophylic, feature exist, the described method comprises the following steps,
(1) graphite foil and stainless steel cloth are cut into the identical sheet of size, it is spare；
(2) a certain amount of n-hexane and dehydrated alcohol are taken, taking the hydrochloric acid that mass fraction is 37%, 1:1 is mixed by volume with water,
It is spare；The ammonium sulfate of 0.1M is configured, it is spare；Take the ammonium hydroxide and ammonium sulfate that a certain amount of mass fraction is 25% by body
Product is spare than being that 1:20 is mixed；
(3) stainless steel cloth in step (1) is first put into the n-hexane of 40mL and is impregnated two days, then taken out with distillation washing
It is put into the dehydrated alcohol of 40mL and impregnates one day after washing.It is finally immersed into the hydrochloric acid in step (2), is taken out after 3min, used
Distilled water flushing stainless steel cloth, cleaning are repeatedly remained to without hydrochloric acid, obtain the stainless steel cloth of removing oxide layer, spare；
(4) use in step (3) except the stainless steel cloth of oxide layer is as cathode electrode, use graphite foil in step (1)
It the use of ammonium sulfate in step (2) and ammonium hydroxide mixed solution is electrolyte as anode electrode, control decomposition voltage is 4-8V, electricity
The solution time is 2-5h, takes out stainless steel cloth, is dried with baking oven is put into after distilled water repeated flushing stainless steel cloth to get super thin
The super oleophylic graphite alkene composite membrane of water.
2. the method for the graphene composite film of preparation super-hydrophobic super-oleophylic according to claim 1, which is characterized in that described
Resulting aqueous solution is cleaned every time using pH test paper detection in step (3), until pH test paper shows and is in neutrality.
3. the method for the graphene composite film of preparation super-hydrophobic super-oleophylic according to claim 1, which is characterized in that described
In step (4), drying temperature is 60 DEG C, drying time 12h.
4. the method for the graphene composite film of preparation super-hydrophobic super-oleophylic according to claim 1, which is characterized in that described
The time of step (4) electrolysis is 3-4 hours, and voltage control, in 5-7V, drying temperature is at 60 DEG C of constant temperature.
5. the method for the graphene composite film of preparation super-hydrophobic super-oleophylic according to claim 1, which is characterized in that described
Stainless steel cloth mesh diameter is 40-100 μm in step (1).
6. the method for the graphene composite film of preparation super-hydrophobic super-oleophylic according to claim 1, which is characterized in that described
Ultrasonic vibration tools are cooperated using diamond fretsaw Wire cutting machine tool in step (1), grapheme material is cut out.
7. the method for the graphene composite film of preparation super-hydrophobic super-oleophylic according to claim 1, which is characterized in that described
Ultrasonic vibration tools power is 350W, ultrasonic frequency 20kHz.
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