CN104874295A - Preparation method of super-hydrophilic self-cleaning multifunctional graded oil-water separation material - Google Patents
Preparation method of super-hydrophilic self-cleaning multifunctional graded oil-water separation material Download PDFInfo
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Abstract
The invention discloses a preparation method of a super-hydrophilic self-cleaning multifunctional graded oil-water separation material. The method comprises the following steps: preparing a porous net-shaped Cu thin film by adopting a hydrogen foam template method; and preparing a chitosan (CS) coating and a CS/PVA coating on the surface of the porous Cu thin film by adopting an impregnation method. The area of a prepared multifunctional oil-water separation thin film is 3*3cm<2>; and the hole diameter of the porous net-shaped thin film is 100-500 microns, and the secondary pore diameter (namely the diameter of a porous structure electroplated on a net-shaped substrate) is 10-120 microns. The contact angle of water in air of a chitosan coating net film is 0-5 degrees, the contact angle of oil under the water is 160+/-5 degrees and the rolling angle of the oil under the water is less than 5 degrees. The prepared self-cleaning multifunctional oil-water separation thin film can be used for preparing oil-water separation and heavy metal adsorption multifunctional materials; and the material has an underwater super-oleophobic property and the good mechanical stability.
Description
Technical field
The present invention relates to a kind of preparation method of water-oil separating material, be specifically related to the multi-functional graduation of a kind of super hydrophilic automatically cleaning.
Background technology
Oil spills and oil-containing industrial water discharge have been worldwide problems, this brings many noxious materials to ocean, be delivered to by marine food chain and comprise in each species body of the mankind from rudimentary plant algae to higher mammal, organism species and human health are on the hazard.And except containing insoluble oil in industrial wastewater, contain a large amount of dispersion emulsion and heavy metal ion toward contact, due to its toxicity and carcinogenesis, heavy metal is considered to " killer " that pose a health risk.Along with the increase of population and the scarcity of freshwater resources, preparation stable circulation can use, become a urgent demand for the multi-functional diffusion barrier removing the oil of different conditions in water and heavy metal ion.
Traditional weight-driven water-oil separating film can only separating emulsions or immiscible oil water mixture, can not separate dissolved metal ion in the solution.With regard to existing oil-water separation mesh film and sorbing material, separation process and adsorption process are carried out all respectively, and the rear water of separation needs to carry out after-treatment and just can re-use.Therefore needing to prepare can function match, carry out the diffusion barrier of water-oil separating and heavy metal adsorption, and diffusion barrier can realize " regeneration " afterwards in use " poisoning ", continues to recycle simultaneously.
The present invention proposes multi-functional nethike embrane combination preparation graduation water-oil separating film, water-oil separating and heavy metal adsorption can be carried out to containing the multi-component mixture such as emulsion, metal ion simultaneously, and separation caudacoria can realize automatically cleaning, can use under the complex environments such as acid-alkali salt.This one body swimming purification renewable membrane, to protection of the environment, maintains ecosystem balance and has very important significance.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of super hydrophilic automatically cleaning multi-functional graduation water-oil separating material, adopt bubble hydrogen template to prepare multi-functional graduation porous compound nethike embrane in conjunction with infusion process.Multi-functional graduation porous compound nethike embrane prepared by the method can carry out water-oil separating and heavy metal adsorption to containing the multi-component mixture such as emulsion, metal ion simultaneously, and separation caudacoria can realize automatically cleaning, can use under the complex environments such as acid-alkali salt.This one body swimming purification renewable membrane, to protection of the environment, maintains ecosystem balance and has very important significance.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for super hydrophilic automatically cleaning multi-functional graduation water-oil separating material, adopts bubble hydrogen template synthesis holey Cu film; Shitosan (CS) coating and CS/ PVA coating is prepared at above-mentioned porous C u film surface by infusion process.Concrete steps are as follows:
One, the preparation of mesh structural porous Cu film:
Adopt the mesh structural porous Cu film of bubble hydrogen template synthesis, its concrete steps are as follows: after carrying out pickling alkali cleaning oil removing and oxide to copper mesh substrate (20-400 order), make anode (2 × 2cm with platinized platinum
2), copper mesh do to electrode cathode (3 × 3cm
2) carrying out electro-deposition, plating solution composition comprises 0.02-4molL
-1cuSO
4and 0.1-5molL
-1h
2sO
4, pH=4.0 ± 0.5, current density is 0.1-8.0 Acm
-2, sedimentation time is 5-40s.
Two, the preparation of hydrophilic coating on mesh structural porous Cu film:
1, the preparation of CS/Cu nethike embrane:
(1) be slowly immersed in by mesh structural porous Cu film in the acetic acid mixed solution (0.1-10wt.%) of shitosan (CS)/glutaraldehyde (GA), dipping 1-30min, then slowly extract mesh structural porous Cu film, copper mesh surface adhesion has mixing material; The compound method of CS/GA is as follows: the GA solution adding 3-10mL in 100mL CS solution.
(2) by dry in atmosphere for the mesh structural porous Cu film after dipping, then 0.5-5min in NaOH (4wt.%) solution is immersed in, use deionized water rinsing 1-2min, the CS/Cu nethike embrane obtained is kept in deionized water or sodium chloride solution (2mol/L).
2, the preparation of CS/PVA/Cu compound nethike embrane:
(1) compound concentration is 0.1-100wt% polyvinyl acetate (PVA) solution at 60-100 DEG C;
(2) by PVA(0.1-20wt.%) solution and CS(1-20 wt.%) solution mixes with volume ratio 1:1-10, and stirring 0.5-2h together becomes uniform mixed solution;
(3) mesh structural porous Cu film is immersed in 2-20min in mixed solution, air drying, with NaOH (4 wt.%) and the dried copper mesh of deionized water rinsing, obtains CS/PVA coating grid;
(4) CS/PVA coating grid is immersed in glutaraldehyde (GA) solution (0.5-2wt.%), full cross-linked 10-60min at 20-80 DEG C;
(5) be immersed at 20-80 DEG C containing 0.1-10 wt.% NaBH
4with 10-60min in the mixed solution of 0.1-10wt.% NaOH, with deionized water rinsing and air drying, obtain CS/PVA/Cu compound nethike embrane.
Tool of the present invention has the following advantages:
1, shitosan is a kind of natural biomaterial, has good heavy metal ion adsorbed performance and good hydrophily.The present invention utilizes graduation porous copper mesh as substrate, and hydrophily shitosan prepares super hydrophilic water-oil separating and heavy metal adsorption multifunctional mesh as coating.
2, the present invention utilizes the Superhydrophilic matter of chitosan coat can realize anti-oil pollution in use procedure, and CS/PVA can realize water-oil separating under the complex environments such as soda acid and heavy metal adsorption through further crosslinked.
3, traditional water-oil separating material and the application of heavy metal ion adsorbing material are all single processes, can not be separated with the heavy metal ion in water the oil in sewage, heavy metal ion adsorbed coating prepared by the present invention can realize water-oil separating and heavy metal adsorption double process simultaneously.
4, the present invention adopts bubble hydrogen template and infusion process to prepare chitosan coat is a kind of simple, the method that convenient, cost is low, parameter is controlled.
5, relative to other water-oil separating films, multifunctional membrane of the present invention can be applied simultaneously in rapid heavy metal ion adsorption and water-oil separating, and separation process can anti-oil pollution and acid and alkali-resistance, automatically cleaning can be realized after separation, solve the problems such as the after-treatment in the process of disposing of sewage, have a good application prospect.
6, the area of Multifunctional oil moisture scrapping off film that prepared by the present invention is 3*3cm
2, holey film substrate aperture is 100-500 μm, and secondary aperture (that is: the aperture of the loose structure electroplated in mesh substrate) is 10-120 μm.Chitosan coat nethike embrane water in air contact angle is 0-5 °, and oily contact angle is 160 ± 5 ° under water, and oily roll angle is less than 5 ° under water.
7, the Multi-function self-cleaning water-oil separating film that prepared by the present invention can be used for manufacturing water-oil separating and heavy metal adsorption multifunctional material, and this material has super oleophobic properties under water, good mechanical stability.
Accompanying drawing explanation
Fig. 1 is bubble hydrogen template synthesis mesh structural porous Cu film apparatus schematic diagram;
Fig. 2 is the preparation process schematic diagram of preparation graduation Cu film and coating;
Fig. 3 is the porous C u microscopic appearance Electronic Speculum figure of preparation;
Fig. 4 is the application process schematic diagram of netted multifunctional oil-water separating net.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Detailed description of the invention one: present embodiment prepares Multi-function self-cleaning water-oil separating material in accordance with the following steps:
One, the preparation (Fig. 1) of mesh structural porous Cu film:
Adopt the mesh structural porous Cu film of bubble hydrogen template synthesis (substrate 20-400 order), its microscopic appearance Electronic Speculum figure as shown in Figure 3.Concrete steps are as follows: after carrying out pickling alkali cleaning oil removing and oxide to copper mesh substrate (20-400 order), make anode (2 × 2cm with platinized platinum
2), copper mesh do to electrode cathode (3 × 3cm
2) carrying out electro-deposition, plating solution composition comprises 0.02-4molL
-1cuSO
4and 0.1-5molL
-1h
2sO
4, pH=4.0 ± 0.5, current density is 0.1-8.0 Acm
-2, sedimentation time is 5-40s.
Two, the preparation (Fig. 2) of hydrophilic coating on mesh structural porous Cu film:
1, the preparation of CS/Cu nethike embrane:
(1) be slowly immersed in by mesh structural porous Cu film in the acetic acid mixed solution of shitosan (CS)/glutaraldehyde (GA), dipping 1-30min, then slowly extract mesh structural porous Cu film, copper mesh surface adhesion has mixing material; The compound method of CS/GA is as follows: the GA(0.1-10wt % adding 3.70mL in 100mL CS solution) solution.
(2) by dry in atmosphere for the mesh structural porous Cu film after dipping, be then immersed in 1min in NaOH (4wt%) solution, use deionized water rinsing 1-2min, the CS/Cu nethike embrane obtained is kept in deionized water or sodium chloride solution (2mol/L).
2, the preparation of CS/PVA/Cu compound nethike embrane:
At (1) 90 DEG C, compound concentration is 0.1-100wt% polyvinyl acetate (PVA) solution;
(2) by PVA(0.1-20wt%) solution and CS(1-20 wt %) solution mixes with volume ratio 1:4, and stirring 1 h together becomes uniform mixed solution;
(3) mesh structural porous Cu film is immersed in 5min in mixed solution, air drying, with NaOH (4 wt %) and the dried copper mesh of deionized water rinsing, obtains CS/PVA coating grid;
(4) CS/PVA coating grid is immersed in glutaraldehyde (GA) solution (1 wt %), full cross-linked 30min at 40 DEG C;
(5) at 40 DEG C, be immersed in 0.1-10 wt % NaBH
4with 30min in 0.1-10wt% NaOH mixed solution, with deionized water rinsing and air drying, obtain CS/PVA/Cu compound nethike embrane.
Three, CS/Cu nethike embrane and the nethike embrane water-oil separating of CS/PVA/Cu compound and heavy metal adsorption process (Fig. 4):
Preparation heavy metal ion solution, as model pollutant, mixes with certain gauging.CS/Cu nethike embrane and CS/PVA/Cu compound nethike embrane are placed on oily-water seperating equipment, carry out water-oil separating and heavy metal adsorption experiment simultaneously, and after separation and absorption terminate, transfer nethike embrane, in the aqueous solution, cleans oil stain residual on compound nethike embrane.CS/PVA/Cu compound nethike embrane is carried out acid and alkali-resistance test, and it is 1h in the solution of 2 and 12 that CS/PVA/Cu compound nethike embrane is immersed in pH respectively, and tests water-oil separating and the heavy metal adsorption performance of the nethike embrane after dipping.Utilize oily-water seperating equipment to test for water-oil separating separative efficiency nethike embrane respectively, after being separated, liquid is measured its oil content by Infrared Oil Determination Instrument and Atomic Absorption Spectrometer (AAS) and is recorded disengaging time.
The area of Multifunctional oil moisture scrapping off film prepared by present embodiment is 3*3cm
2, holey film substrate aperture is 100-500 μm, and secondary aperture (that is: the aperture of the loose structure electroplated in mesh substrate) is 10-120 μm.Chitosan coat nethike embrane water in air contact angle is 0-5 °, and oily contact angle is 160 ± 5 ° under water, and oily roll angle is less than 5 ° under water.
Control for micro array structure can by regulating current density, electrodeposit reaction time, main salt concentration and electropolymerization pyrrole monomer concentration, pulse voltage, polymerization reaction time.Oil-water separation mixture comprises non-oil water mixture and the emulsion of dissolving each other of dissolving each other.Adsorption of Heavy Metal Ions kind comprises nickel ion, zinc ion, iron ion, cobalt ions, cadmium ion.
Detailed description of the invention two: present embodiment prepares Multi-function self-cleaning water-oil separating material in accordance with the following steps:
One, the preparation of mesh structural porous Cu film:
Adopt the mesh structural porous Cu film of bubble hydrogen template synthesis, its concrete steps are as follows: after carrying out pickling alkali cleaning oil removing and oxide to copper mesh substrate (300 order), make anode (2 × 2cm with platinized platinum
2), copper mesh do to electrode cathode (3 × 3cm
2) carrying out electro-deposition, plating solution composition comprises 0.1molL
-1cuSO
4and 1molL
-1h
2sO
4, pH=4.0 ± 0.5, current density is 7 Acm
-2, sedimentation time is 20s.
Two, the preparation of chitosan coat on mesh structural porous Cu film:
(1) copper mesh of above-mentioned preparation is slowly immersed in the acetic acid mixed solution of shitosan (CS)/glutaraldehyde (GA), and CS/GA preparation is in 100mL CS solution, add GA (1wt %) solution of 3.70 milliliters, dipping 5min.Then slowly extract porous copper mesh, copper mesh surface adhesion has mixing material.
(2) porous web after dipping is dry in atmosphere, and be then immersed in 1min in NaOH (4wt%) solution, use deionized water rinsing 1-2min, the CS/Cu nethike embrane obtained is kept in deionized water or sodium chloride solution (2mol/L).
Three, the water-oil separating of CS/Cu compound nethike embrane and heavy metal adsorption process
Preparation heavy metal ion solution, as model pollutant, mixes with certain gauging.CS/Cu nethike embrane is placed on oily-water seperating equipment, carries out water-oil separating and heavy metal adsorption experiment simultaneously, and after separation and absorption terminate, transfer nethike embrane, in the aqueous solution, cleans oil stain residual on compound nethike embrane.Oily-water seperating equipment is utilized to test for water-oil separating separative efficiency nethike embrane respectively, after being separated, liquid is measured its oil content by Infrared Oil Determination Instrument and Atomic Absorption Spectrometer (AAS) and is recorded disengaging time, separative efficiency 95 ± 4%, Adsorption of Heavy Metal Ions 90 ± 5%.
The area of Multifunctional oil moisture scrapping off film prepared by present embodiment is 3*3cm
2, holey membrane pore size is 40 μm, and secondary aperture (that is: the aperture of the loose structure electroplated in mesh substrate) is 30 μm.Chitosan coat nethike embrane water in air contact angle is 0-2 °, and oily contact angle is 160 ± 2 ° under water, and oily roll angle is less than 3 ° under water.Multi-functional nethike embrane prepared by present embodiment is for using in neutral and alkaline solution (pH=5-13).
Detailed description of the invention three: present embodiment prepares Multi-function self-cleaning water-oil separating material in accordance with the following steps:
One, the preparation of mesh structural porous Cu film:
Adopt the mesh structural porous Cu film of bubble hydrogen template synthesis, its concrete steps are as follows: after carrying out pickling alkali cleaning oil removing and oxide to copper mesh substrate (300 order), make anode (2 × 2cm with platinized platinum
2), copper mesh do to electrode cathode (3 × 3cm
2) carrying out electro-deposition, plating solution composition comprises 0.1molL
-1cuSO
4and 1molL
-1h
2sO
4, pH=4.0 ± 0.5, current density is 7 Acm
-2, sedimentation time is 20s.
Two, the preparation of CS/PVA coating on mesh structural porous Cu nethike embrane:
At (1) 90 DEG C, compound concentration is 10wt% polyvinyl acetate (PVA) solution;
(2) by PVA (2wt.%) solution and CS(10wt.%) solution mixes with volume ratio 1:4, and stirring 1 h together becomes uniform mixed solution.
(3) porous copper mesh is immersed in 5min in mixed solution, air drying, with NaOH (4 wt %) and the dried copper mesh of deionized water rinsing.
(4) CS/PVA coating grid is immersed in glutaraldehyde (GA) solution (1wt.%), full cross-linked 30min at 40 DEG C.
(5) at 40 DEG C, 1.5wt.% NaBH is immersed in
4with 30min in 1wt.%NaOH mixed solution, with deionized water rinsing and air drying, obtain CS/PVA/Cu compound nethike embrane.
Three, the water-oil separating of CS/PVA/Cu compound nethike embrane and heavy metal adsorption process:
Preparation heavy metal ion solution, as model pollutant, mixes with certain gauging.CS/Cu nethike embrane and CS/PVA/Cu compound nethike embrane are placed on oily-water seperating equipment, carry out water-oil separating and heavy metal adsorption experiment simultaneously, and after separation and absorption terminate, transfer nethike embrane, in the aqueous solution, cleans oil stain residual on compound nethike embrane.CS/PVA/Cu compound nethike embrane is carried out acid and alkali-resistance test, and it is 1h in the solution of 2 and 12 that CS/PVA/Cu compound nethike embrane is immersed in pH respectively, and tests water-oil separating and the heavy metal adsorption performance of the nethike embrane after dipping.Utilize oily-water seperating equipment to test for water-oil separating separative efficiency nethike embrane respectively, after being separated, liquid is measured its oil content by Infrared Oil Determination Instrument and Atomic Absorption Spectrometer (AAS) and is recorded disengaging time.
The area of Multifunctional oil moisture scrapping off film prepared by present embodiment is 3*3cm
2, holey film substrate aperture is 40 μm, and secondary aperture (that is: the aperture of the loose structure electroplated in mesh substrate) is 30 μm (inside also has more aperture).CS/PVA coating nethike embrane water in air contact angle is 0-2 °, and oily contact angle is 159 ± 2 ° under water, and oily roll angle is less than 3 ° under water.Multi-functional nethike embrane prepared by present embodiment is for using under pH=2-12 environment.
Claims (10)
1. a preparation method for super hydrophilic automatically cleaning multi-functional graduation water-oil separating material, is characterized in that described method step is as follows:
One, the preparation of mesh structural porous Cu film:
Adopt the mesh structural porous Cu film of bubble hydrogen template synthesis;
Two, the preparation of hydrophilic coating on mesh structural porous Cu film:
(1) be slowly immersed in the acetic acid mixed solution of CS/GA by mesh structural porous Cu film, dipping 1-30min, then slowly extract mesh structural porous Cu film, copper mesh surface adhesion has mixing material;
(2) by dry in atmosphere for the mesh structural porous Cu film after dipping, be then immersed in 0.5-5min in sodium hydroxide solution, use deionized water rinsing 1-2min, obtain CS/Cu nethike embrane.
2. the preparation method of super hydrophilic automatically cleaning according to claim 1 multi-functional graduation water-oil separating material, it is characterized in that the concrete steps of described employing bubble hydrogen template synthesis mesh structural porous Cu film are as follows: after pickling alkali cleaning oil removing and oxide are carried out to copper mesh substrate, make anode with platinized platinum, copper mesh work carries out electro-deposition to electrode cathode, plating solution is by 0.02-4molL
-1cuSO
4and 0.1-5molL
-1h
2sO
4composition, pH=4.0 ± 0.5, current density is 0.1-8.0 Acm
-2, sedimentation time is 5-40s.
3. the preparation method of super hydrophilic automatically cleaning according to claim 2 multi-functional graduation water-oil separating material, it is characterized in that described copper mesh substrate 20-400 order, anode dimension is 2 × 2cm
2, 3 × 3cm is of a size of to electrode cathode
2.
4. the preparation method of super hydrophilic automatically cleaning according to claim 1 multi-functional graduation water-oil separating material, is characterized in that in described acetic acid mixed solution, and the concentration of CS/GA is 0.1-10wt.%.
5. the preparation method of the super hydrophilic automatically cleaning multi-functional graduation water-oil separating material according to claim 1 or 4, is characterized in that the compound method of described CS/GA is as follows: the GA solution adding 3-10mL in 100mL CS solution.
6. a preparation method for super hydrophilic automatically cleaning multi-functional graduation water-oil separating material, is characterized in that described method step is as follows:
One, the preparation of mesh structural porous Cu film:
Adopt the mesh structural porous Cu film of bubble hydrogen template synthesis;
Two, the preparation of hydrophilic coating on mesh structural porous Cu film:
(1) mixed with volume ratio 1:1-10 with 1-20 wt.%CS solution by 0.1-20wt.%PVA solution, stirring 0.5-2h together becomes uniform mixed solution;
(2) mesh structural porous Cu film is immersed in 2-20min in mixed solution, air drying, with NaOH and the dried copper mesh of deionized water rinsing, obtains CS/PVA coating grid;
(3) CS/PVA coating grid is immersed in glutaraldehyde solution, full cross-linked 10-60min at 20-80 DEG C;
(4) at 20-80 DEG C, NaBH is immersed in
4with 10-60min in NaOH mixed solution, with deionized water rinsing and air drying, obtain CS/PVA/Cu compound nethike embrane.
7. the preparation method of super hydrophilic automatically cleaning according to claim 6 multi-functional graduation water-oil separating material, it is characterized in that the concrete steps of described employing bubble hydrogen template synthesis mesh structural porous Cu film are as follows: after pickling alkali cleaning oil removing and oxide are carried out to copper mesh substrate, make anode with platinized platinum, copper mesh work carries out electro-deposition to electrode cathode, plating solution is by 0.02-4molL
-1cuSO
4and 0.1-5molL
-1h
2sO
4composition, pH=4.0 ± 0.5, current density is 0.1-8.0 Acm
-2, sedimentation time is 5-40s.
8. the preparation method of super hydrophilic automatically cleaning according to claim 7 multi-functional graduation water-oil separating material, it is characterized in that described copper mesh substrate 20-400 order, anode dimension is 2 × 2cm
2, 3 × 3cm is of a size of to electrode cathode
2.
9. the preparation method of super hydrophilic automatically cleaning according to claim 1 multi-functional graduation water-oil separating material, is characterized in that the concentration of described glutaraldehyde solution is 0.5-2wt.%.
10. the preparation method of super hydrophilic automatically cleaning according to claim 1 multi-functional graduation water-oil separating material, is characterized in that NaBH in described mixed solution
4concentration is 0.1-10 wt.%, NaOH concentration is 0.1-10wt.%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028696A (en) * | 2019-04-16 | 2019-07-19 | 广东石油化工学院 | A kind of hydrophilic and oleophobic sponge and its preparation method and application |
| CN111013199A (en) * | 2019-12-31 | 2020-04-17 | 常州大学 | Preparation method of intelligent pH response type melamine foam oil-water separation material |
-
2015
- 2015-05-04 CN CN201510220518.0A patent/CN104874295B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028696A (en) * | 2019-04-16 | 2019-07-19 | 广东石油化工学院 | A kind of hydrophilic and oleophobic sponge and its preparation method and application |
| CN110028696B (en) * | 2019-04-16 | 2021-09-10 | 广东石油化工学院 | Hydrophilic oleophobic sponge and preparation method and application thereof |
| US20210346823A1 (en) * | 2019-04-16 | 2021-11-11 | Guangdong University Of Petrochemical Technology | Hydrophilic/oleophobic sponge, preparation method and use thereof |
| US11964220B2 (en) * | 2019-04-16 | 2024-04-23 | Guangdong University Of Petrochemical Technology | Hydrophilic/oleophobic sponge, preparation method and use thereof |
| CN111013199A (en) * | 2019-12-31 | 2020-04-17 | 常州大学 | Preparation method of intelligent pH response type melamine foam oil-water separation material |
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