CN105148562A - Candle-ash-assisted super-hydrophobic and super-oleophilic oil-water separation mesh film as well as preparation method and application of mesh film - Google Patents
Candle-ash-assisted super-hydrophobic and super-oleophilic oil-water separation mesh film as well as preparation method and application of mesh film Download PDFInfo
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Abstract
The invention discloses a candle-ash-assisted super-hydrophobic and super-oleophilic oil-water separation mesh film as well as a preparation method and an application of the mesh film. According to the method, firstly, a copper wire mesh is pretreated for cleaning and oil removal and blown by compressed nitrogen to be dried; an anhydrous sodium sulfate and copper chloride mixed electrolyte solution is prepared; the pretreated copper wire mesh is placed in the electrolyte solution for constant-voltage cathodic electrodeposition of nano-copper under the voltage of 0.3-1.0 V; the copper wire mesh after electrodeposition is placed in a position 1-4 cm higher than the flame of a burning candle for candle ash deposition, and the oil-water separation mesh film having the super-hydrophobic property is obtained through cooling. The contact angle of the mesh film prepared with the method with water is larger than 153 degrees, the contact angle of the mesh film with oil is smaller than 5 degrees, and the mesh film has the higher high-temperature resistance, the good contact angle stability with acid and alkaline solutions and can be used repeatedly. Compared with traditional oil-water separation films, the oil-water separation mesh film better conforms to the environmental protection concept, can be applied to blockage of offshore oil pollution, chemical sewage treatment and the like, and has the broad application prospect.
Description
Technical field
The invention belongs to inorganic-organic hybridization nano technical field of function materials, relate to a kind of water-oil separating film, particularly relate to a kind of super-hydrophobic super-oleophylic oil-water separation mesh film auxiliary by candle ash and its preparation method and application.
Background technology
It is reported, the oil probably having 3,200,000,000 cubic tons every year enters into water body, forms oil-polluted water, the oil film of about 38400000 sq-kms is caused to cover, marine ecosystems suffer sustaining breakdown, waste valuable petroleum resources simultaneously, also directly affect human health and ecological environment.The processing method commonly used for oily waste water at present comprises fence and intercepts and remedy with natural materials such as common cotton wools, and this all can cause secondary pollution and the more multiple resource waste of oil.Even if chemical breakdown agent and biodegradation class process means also exist technology consume the problems such as high, efficiency is low, thus Novel sewage treatment technology is the problem needing research badly.Water-oil separating is the process be separated by water-oil phase by the parting material such as nethike embrane or oil absorption material, if by water-oil separating materials application in sea pollution by oil process, is fully separated with seawater by petroleum-based liquid and reclaims, certainly will play a multiplier effect; In industrial production, the space that water-oil separating material can play a role can not look down upon too, comprises it and is expected to be applied to the insoluble production problem of a series of current social such as oil depot oil-water separation wells, high polymer polymeric emulsification liquid waste processing.
Traditional oily water separation technique also also exists many problems, comprises that the rate of departure is slow, efficiency is low, cyclic utilization rate is low, cost is high, makes it apply and is restricted.And have that special infiltrating oil-water separation mesh film has high separating efficiency, the rate of departure is high, secondary pollution is little, cyclic utilization rate is high, operability is good and consume the advantages such as low, become the focus of present oily water separation technique research field gradually.Have in special infiltrating water-oil separating material, the close and distant property of material plays key effect in oil water separation process.By changing surface of solids degree of roughness and changing its surface energy by modifying specific chemical group, it is the general thinking preparing super thin nethike embrane.
Summary of the invention
The invention provides a kind of super-hydrophobic super-oleophylic oil-water separation mesh film auxiliary by candle ash and its preparation method and application, candle ash being deposited directly to the surface of the copper mesh after electro-deposition roughening, obtaining super-hydrophobic super-oleophylic oil-water separation mesh film by regulating sedimentation time.The air that this nethike embrane retains due to coarse structure in atmosphere and deposit the hydrophobicity of the carbon nano-particles obtained, shows super-hydrophobicity and super-oleophilic, can oil-water separation mixture effectively.When oil water mixture is by this nethike embrane, oil can be then trapped within nethike embrane by nethike embrane water rapidly under gravity, thus reaches the effect of water-oil separating.
For achieving the above object, the present invention is achieved by the following technical solutions:
The invention provides a kind of preparation method of the super-hydrophobic super-oleophylic oil-water separation mesh film auxiliary by candle ash, it comprises the following steps:
(1) carry out pretreatment to copper mesh: copper mesh is carried out ultrasonic cleaning by acetone, absolute ethyl alcohol and deionized water successively, take out, compressed nitrogen dries up;
(2) electrolyte solution is prepared: prepare the electrolyte solution be made up of the anhydrous sodium sulfate of 0.01-0.5mol/L and the Copper dichloride dihydrate of 0.01-0.5mol/L;
(3) utilize two electrode systems to carry out electro-deposition: make negative electrode with pretreated copper mesh, platinum plate electrode makes anode, pretreated copper mesh be placed in described electrolyte solution, carry out electro-deposition and obtain Nanometer Copper on copper mesh,
(4) taken out by the copper mesh after electro-deposition, a large amount of deionized water rinsing, compressed nitrogen dries up;
(5) candle ash deposition: is carried out candle ash deposition above the candle flame that the copper mesh after rinsing is placed in burning, cooling, obtains the super-hydrophobic super-oleophylic oil-water separation mesh film that surface has carbon nano-particles naturally.
Further improvement to technique scheme: described copper mesh is 100-400 object brass copper mesh or red copper copper mesh.
Further improvement to technique scheme: distinguish ultrasonic cleaning 3-15 minute successively by acetone, absolute ethyl alcohol and deionized water in described step (1) preprocessing process.
Further improvement to technique scheme: in described step (1) pretreatment, the frequency of ultrasonic cleaning is at 20-60KHz, power bracket is 20-120W.
Further improvement to technique scheme: in described step (3), electro-deposition deposits 5-10 minute under 0.1-1.0V constant voltage condition, at 20-50 DEG C temperature, and the Nanometer Copper particle diameter obtained is at 20-200nm.
Further improvement to technique scheme: above the candle flame in described step (5), the copper mesh after electro-deposition being placed in burning, 1-4 centimeters carries out candle ash deposition 1-10 minute.
Present invention also offers the super-hydrophobic super-oleophylic oil-water separation mesh film that described preparation method obtains.
Further improvement to technique scheme: described oil-water separation mesh film surface forms particle diameter at the carbon nano-particles of 20-50nm, is greater than 150 ° in atmosphere, is less than 5 ° to the contact angle of oil to the contact angle of water.
Present invention also offers the described application of super-hydrophobic super-oleophylic oil-water separation mesh film in oil-water separation mixture.
Further improvement to technique scheme: described oil-water separation mesh film is separated with chemical engineering sewage for separating of sea pollution by oil.
Compared with prior art, the present invention has the following advantages and technique effect:
1, preparation process is simple, and easy to operate, cost is low, and component used easily obtains, and equipment requirement is extremely low.Easily realize suitability for industrialized production.
2, final products stable in properties, can preserve for a long time in indoor environment.
3, prepare the component that relates to of overall process and method all nontoxic, very environmental protection.
4, the super thin performance of oil-water separation mesh film of the present invention is good, and stability is high, can Reusability, and can adapt to different acid or alkali environment and condition of different temperatures, has higher temperature resistance, and goes out excellent contact angle stability to strong acid-base solutions display.
5, oil-water separation mesh film of the present invention rate of departure in oil water separation process is fast, and oil phase substance is easily recycled, and can be applicable to be separated multiple oil water mixture.
The present invention, compared with traditional water-oil separating film, more meets environmental protection concept, has more outstanding using value.Material of the present invention can be applied to obstruct offshore oil pollution, and chemical engineering sewage process etc., have broad application prospects.
Accompanying drawing explanation
In Fig. 1, (a)-(c) is SEM image under not modified copper mesh different multiples; D ()-(f) to be through after electro-deposition Nanometer Copper roughening SEM image under different amplification; (g)-be (i) through candle ash modify after SEM image under different amplification;
Fig. 2 is copper mesh contact angle result, and wherein (a) is the contact angle of water on not modified copper mesh; B () is the contact angle of water on copper mesh after electro-deposition roughening; C () is the contact angle that candle ash modifies water on copper mesh; D () is the optical photograph of the copper mesh of water droplet after candle ash is modified; E () is the contact angle that candle ash modifies n-hexane on copper mesh; F () is the contact angle that candle ash modifies silicone oil on copper mesh;
Fig. 3 is the stability of super-hydrophobic super-oleophylic retinal surface contact angle under different pH and temperature after candle ash is modified;
Fig. 4 is that after candle ash is modified, oil (chloroform) water of super-hydrophobic super-oleophylic nethike embrane is separated experimentation, and water methyl orange dyes;
Fig. 5 is that after candle ash is modified, oil (silicone oil) water of super-hydrophobic super-oleophylic nethike embrane is separated experimentation, and water methyl orange dyes;
Fig. 6 is water and the silicone oil contact angle result on super-hydrophobic super-oleophylic nethike embrane in embodiment 2;
Fig. 7 is the water-oil separating result of water in embodiment 2 and silicone oil;
Fig. 8 is water and the atoleine contact angle result on super-hydrophobic super-oleophylic nethike embrane in embodiment 3;
Fig. 9 is the water-oil separating result of water and atoleine in embodiment 3;
Figure 10 be in embodiment 4 water and benzinum in online contact angle result;
Figure 11 is the water-oil separating result of water and benzinum in embodiment 4.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is further described in detail.
Embodiment 1
The preparation method of the super-hydrophobic super-oleophylic oil-water separation mesh film of being assisted by candle ash described in the present embodiment comprises the following steps:
1, by copper mesh respectively through acetone, absolute ethyl alcohol and water successively ultrasonic cleaning 5 minutes, compressed nitrogen dries up;
2,1.4204g anhydrous sodium sulfate and 1.7048g Copper dichloride dihydrate is taken, the 0.05mol/L electrolyte solution (molar concentration of anhydrous sodium sulfate is 0.05mol/L, and the molar concentration of Copper dichloride dihydrate is 0.05mol/L) of preparation 200ml;
3, being placed in the electrolyte solution of above-mentioned preparation through pretreated copper mesh, take platinized platinum as anode, pretreated copper mesh as negative electrode, constant voltage electro-deposition 6 minutes under 0.5V voltage, temperature is 25 DEG C;
4, by a large amount of deionized water rinsing of the copper mesh after electro-deposition, compressed nitrogen dries up;
5, the post-depositional copper mesh of upper step is placed in and carries out candle ash deposition 4 minutes apart from candle flame 2 centimetres of eminences of burning, naturally cools; Naturally cool after candle ash deposition, surface forms carbon nano-particles, and carbon nano-particles is interconnected to form super hydrophobic surface, after copper mesh surface deposition in the roughened, combine stronger between carbon nano-particles, super-hydrophobicity has more high stability, and preparation process is simple.
In Fig. 1, (a)-(c) naked copper net specimen surface is smooth; D the copper mesh surface of ()-(f) after electro-deposition roughening has coarse micrometer structure.(g)-(i) after candle ash is modified, deposit carbon nano particle is online in coarse leading to, form micro-nano coarse structure, carbon nano-particles particle diameter is at 20-50nm, connecting between particle reunites forms chain structure, due to the hydrophobicity of this coarse micro-nano compound structure and carbon nano-particles itself, superhydrophobic property is made to be formed into possibility.
Fig. 2 copper mesh contact angle result, wherein (a) is the contact angle of water on not modified copper mesh, 94 °; B () is the contact angle of water on copper mesh after electro-deposition Nanometer Copper roughening, be 55 °; C () is the contact angle of water on sample after candle ash is modified, reach 153 °, water droplet is globulate in its surface, shows super-hydrophobicity; D () is the optical photograph on the sample of water droplet after candle ash is modified; E () is the contact angle that candle ash modifies n-hexane on copper mesh, 0 °, show super-oleophilic; F () is the contact angle that candle ash modifies silicone oil on copper mesh, 3 °, show super-oleophilic.Contact angle test shows that this copper mesh after candle ash is modified shows super-hydrophobic super-oleophylic, for water-oil separating provides condition.
Fig. 3 is that the chemical stability of surface wettability of copper mesh after candle ash is modified and heat endurance characterize.The water droplet of different pH value all at about 150 °, shows stronger acid and alkali-resistance chemical stability at its surface contact angle, due to super hydrophobic surface " mattress " effect, makes acid and alkali corrosion ion be difficult to destroy this super hydrophobic surface; By this separation nethike embrane through high-temperature process, test its heat endurance, at 375 DEG C, still remain good hydrophobicity, until 400 DEG C, structural collapse, carbon film destroys, nethike embrane changes hydrophily into, shows that the super-hydrophobic super-oleophylic nethike embrane that this candle ash is modified has higher heat endurance.
Super-hydrophobic super-oleophylic nethike embrane after described candle ash is modified is cut into sizeable circle and inserts in the middle of connector as filter core, screwing hermetic.Termination injector syringe on connector, lower end be collection container be used for access be separated after liquid.Device is vertically placed; The mixed liquor of chloroform and water is imported syringe, and chloroform can be collected by lower end vessel by filter core, and water can be blocked in the syringe of upper end.See Fig. 4.
Fig. 4 is that after candle ash is modified, super-hydrophobic super-oleophylic nethike embrane is for the separation process of chloroform and profit, and water methyl orange dyes.As can be seen from the figure, due to the super-hydrophobic super-oleophylic character of nethike embrane, chloroform can pass through nethike embrane by rapid permeability, and the water after methyl orange dyeing is trapped on nethike embrane.Illustrate that this nethike embrane has good oil-water separation, it reaches 96% to the water-oil separating efficiency of chloroform.
Fig. 5 is super-hydrophobic super-oleophylic copper mesh water-oil separating experimentation after candle ash is modified, and in Fig. 5, water methyl orange dyes, and oil is undyed silicone oil.As seen from the figure, silicone oil can rapidly by this super-hydrophobic super-oleophylic net, and the water of dyeing is due to the super-hydrophobicity of nethike embrane, is directly trapped in online, also cannot penetrate through nethike embrane under gravity, illustrate that nethike embrane has good oil-water separation.
Embodiment 2
The preparation method of the super-hydrophobic super-oleophylic oil-water separation mesh film of being assisted by candle ash described in the present embodiment comprises the following steps:
1, by copper mesh respectively through acetone, absolute ethyl alcohol and water successively ultrasonic cleaning 5 minutes, compressed nitrogen dries up;
2,1.4204g anhydrous sodium sulfate and 1.7048g Copper dichloride dihydrate is taken, the 0.05mol/L electrolyte solution (molar concentration of anhydrous sodium sulfate is 0.05mol/L, and the molar concentration of Copper dichloride dihydrate is 0.05mol/L) of preparation 200ml;
3, being placed in the electrolyte solution of above-mentioned preparation through pretreated copper mesh, take platinized platinum as anode, pretreated copper mesh as negative electrode, constant voltage electro-deposition 5 minutes under 0.7V voltage, temperature is 30 DEG C;
4, by a large amount of deionized water rinsing of the copper mesh after electro-deposition, compressed nitrogen dries up;
5, the post-depositional copper mesh of upper step is placed in and carries out candle ash deposition 6 minutes apart from candle flame 2 centimetres of eminences of burning, naturally cools; Obtain the super-hydrophobic super-oleophylic oil-water separation mesh film that surface has carbon nano-particles.
Super-hydrophobic super-oleophylic nethike embrane after candle ash is modified is cut into sizeable circle inserts in the middle of homemade connector as filter core, screwing hermetic.Termination injector syringe on connector, device is vertically placed; Pour the mixed liquor of silicone oil and water into, silicone oil can be collected by lower end vessel by filter core, and water can be blocked in the barrel of upper end.
As shown in Figure 6, wherein (a) shows that water is being separated the contact angle (contact angle is 153 °) on nethike embrane, and (b) shows that silicone oil is being separated the contact angle (contact angle is 6 °) on nethike embrane.As shown in Figure 7, water methyl orange dyes water-oil separating result, and oil is silicone oil, and water-oil separating efficiency is 92%.
Embodiment 3
The preparation method of the super-hydrophobic super-oleophylic oil-water separation mesh film of being assisted by candle ash described in the present embodiment comprises the following steps:
1, by copper mesh respectively through acetone, absolute ethyl alcohol and water successively ultrasonic cleaning 5 minutes, compressed nitrogen dries up;
2,0.7102g anhydrous sodium sulfate and 0.8524g Copper dichloride dihydrate is taken, the 0.025mol/L electrolyte solution (molar concentration of anhydrous sodium sulfate is 0.025mol/L, and the molar concentration of Copper dichloride dihydrate is 0.025mol/L) of preparation 200ml;
3, being placed in the electrolyte solution of above-mentioned preparation through pretreated copper mesh, take platinized platinum as anode, copper mesh as negative electrode, constant voltage electro-deposition 4 minutes under 0.8V voltage, temperature is 25 DEG C;
4, by a large amount of deionized water rinsing of the copper mesh after electro-deposition, compressed nitrogen dries up;
5, the post-depositional copper mesh of upper step is placed in and carries out candle ash deposition 5 minutes apart from candle flame 1 centimetre of eminence of burning, naturally cools; Obtain the super-hydrophobic super-oleophylic oil-water separation mesh film that surface has carbon nano-particles.
Super-hydrophobic super-oleophylic nethike embrane after candle ash is modified is cut into sizeable circle inserts in the middle of connector as filter core, screwing hermetic.Termination injector syringe on connector, device is vertically placed; Pour the mixed liquor of atoleine and water into, atoleine can be collected by lower end vessel by filter core, and water can be blocked in the syringe of upper end.
As shown in Figure 8, wherein (a) shows that water is being separated the contact angle (contact angle is 152 °) on nethike embrane, and (b) shows that atoleine is being separated the contact angle (contact angle is 8 °) on nethike embrane.As shown in Figure 9, water methyl orange dyes in water-oil separating, and oil is atoleine, and water-oil separating efficiency is 95%.
Embodiment 4
The preparation method of the super-hydrophobic super-oleophylic oil-water separation mesh film of being assisted by candle ash described in the present embodiment comprises the following steps:
1, by copper mesh through acetone, absolute ethyl alcohol and water successively ultrasonic cleaning 5 minutes, compressed nitrogen dries up;
2,2.1306g anhydrous sodium sulfate and 2.5572g Copper dichloride dihydrate is taken, the 0.075mol/L electrolyte solution (molar concentration of anhydrous sodium sulfate is 0.075mol/L, and the molar concentration of Copper dichloride dihydrate is 0.075mol/L) of preparation 200ml;
3, being placed in the electrolyte solution of above-mentioned preparation through pretreated copper mesh, take platinized platinum as anode, copper mesh as negative electrode, constant voltage electro-deposition 4 minutes under 0.6V voltage, temperature is 25 DEG C;
4, by a large amount of deionized water rinsing of the copper mesh after electro-deposition, compressed nitrogen dries up;
5, the post-depositional copper mesh of upper step is placed in and carries out candle ash deposition 4 minutes apart from candle flame 1 centimetre of eminence of burning, naturally cools; Obtain the super-hydrophobic super-oleophylic oil-water separation mesh film that surface has carbon nano-particles.
Super-hydrophobic super-oleophylic nethike embrane after candle ash is modified is cut into sizeable circle inserts in the middle of homemade connector as filter core, screwing hermetic.Termination injector syringe on connector, device is vertically placed; Pour the mixed liquor of benzinum and water into, benzinum can be collected by lower end vessel by filter core, and water can be blocked in the syringe of upper end.
As shown in Figure 10, wherein (a) shows that water is being separated the contact angle (contact angle is 155 °) on nethike embrane, and (b) shows that benzinum is being separated the contact angle (contact angle is 1 °) on nethike embrane.As shown in figure 11, water methyl orange dyes water-oil separating result, and oil is benzinum, and water-oil separating efficiency is 94%.
Above embodiment only in order to technical scheme of the present invention to be described, but not is limited; Although with reference to previous embodiment to invention has been detailed description, for the person of ordinary skill of the art, still can modify to the technical scheme described in previous embodiment, or equivalent replacement is carried out to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of the present invention's technical scheme required for protection.
Claims (10)
1. a preparation method for the super-hydrophobic super-oleophylic oil-water separation mesh film of being assisted by candle ash, is characterized in that it comprises the following steps:
(1) carry out pretreatment to copper mesh: copper mesh is carried out ultrasonic cleaning by acetone, absolute ethyl alcohol and deionized water successively, take out, compressed nitrogen dries up;
(2) electrolyte solution is prepared: prepare the electrolyte solution be made up of the anhydrous sodium sulfate of 0.01-0.5mol/L and the Copper dichloride dihydrate of 0.01-0.5mol/L;
(3) utilize two electrode systems to carry out electro-deposition: make negative electrode with pretreated copper mesh, platinum plate electrode makes anode, pretreated copper mesh be placed in described electrolyte solution, carry out electro-deposition and obtain Nanometer Copper on copper mesh,
(4) taken out by the copper mesh after electro-deposition, a large amount of deionized water rinsing, compressed nitrogen dries up;
(5) candle ash deposition: is carried out candle ash deposition above the candle flame that the copper mesh after rinsing is placed in burning, cooling, obtains the super-hydrophobic super-oleophylic oil-water separation mesh film that surface has carbon nano-particles naturally.
2. the preparation method of the super-hydrophobic super-oleophylic oil-water separation mesh film auxiliary by candle ash according to claim 1, is characterized in that: described copper mesh is 100-400 object brass copper mesh or red copper copper mesh.
3. the preparation method of the super-hydrophobic super-oleophylic oil-water separation mesh film auxiliary by candle ash according to claim 1, is characterized in that: distinguish ultrasonic cleaning 3-15 minute successively by acetone, absolute ethyl alcohol and deionized water in described step (1) preprocessing process.
4. the preparation method of the super-hydrophobic super-oleophylic oil-water separation mesh film auxiliary by candle ash according to claim 3, it is characterized in that: in described step (1) pretreatment, the frequency of ultrasonic cleaning is at 20-60KHz, power bracket is 20-120W.
5. the preparation method of the super-hydrophobic super-oleophylic oil-water separation mesh film auxiliary by candle ash according to claim 1, it is characterized in that: in described step (3), electro-deposition deposits 5-10 minute under 0.1-1.0V constant voltage condition, at 20-50 DEG C temperature, and the Nanometer Copper particle diameter obtained is at 20-200nm.
6. the preparation method of the super-hydrophobic super-oleophylic oil-water separation mesh film auxiliary by candle ash according to claim 1, is characterized in that: above the candle flame in described step (5), the copper mesh after electro-deposition being placed in burning, 1-4 centimeters carries out candle ash deposition 1-10 minute.
7. the super-hydrophobic super-oleophylic oil-water separation mesh film that obtains of preparation method described in any one of claim 1-6.
8. super-hydrophobic super-oleophylic oil-water separation mesh film according to claim 7, is characterized in that: described oil-water separation mesh film surface forms particle diameter at the carbon nano-particles of 20-50nm, is greater than 150 ° in atmosphere, is less than 5 ° to the contact angle of oil to the contact angle of water.
9. the application of super-hydrophobic super-oleophylic oil-water separation mesh film according to claim 7 in oil-water separation mixture.
10. the application of super-hydrophobic super-oleophylic oil-water separation mesh film according to claim 9 in oil-water separation mixture, is characterized in that: described oil-water separation mesh film is separated with chemical engineering sewage for separating of sea pollution by oil.
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| 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 |
| CN105999769A (en) * | 2016-06-06 | 2016-10-12 | 集美大学 | Preparation method for oil-water separation mesh |
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