CN102698471B - Oil-water separating mesh film and preparation method thereof - Google Patents
Oil-water separating mesh film and preparation method thereof Download PDFInfo
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- CN102698471B CN102698471B CN201210152727.2A CN201210152727A CN102698471B CN 102698471 B CN102698471 B CN 102698471B CN 201210152727 A CN201210152727 A CN 201210152727A CN 102698471 B CN102698471 B CN 102698471B
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Abstract
The invention discloses an oil-water separating mesh film and a preparation method thereof. The preparation method comprises the following steps of: 1) dissolving polylactic acid in an organic solvent to obtain a polylactic acid solution; 2) adding a porogen into the polylactic acid solution and evenly mixing to obtain a mixed solution; and 3) carrying out phase separation on the mixed solution, so as to obtain the oil-water separating mesh film. The experiment of the invention proves that the oil-water separating mesh film disclosed by the invention has the characteristics of stability and high separation efficiency; the oil-water separating mesh film can be prepared in large area, the separated oil can be recycled, the separating mesh film can be repeatedly used, and the separation effect can not be influenced. After being used and abandoned, the oil-water separating mesh film can be degraded in the natural environment, so that the secondary pollution can be avoided. The biodegradable oil-water separating mesh film with super-hydrophobic and super-oleophylic properties can be used for oil-water separation of oily sewage containing edible oil, gasoline and the like.
Description
Technical field
The invention belongs to chemical, technical field of function materials, particularly a kind of water-oil separating nethike embrane and preparation method thereof.
Background technology
Along with a large amount of discharges of oil-polluted water in productive life and the frequent generation of Crude Oil at Sea leakage accident, become for the exploration of water-oil separating and research the important topic that is related to people's lives, economic development and Environmental security, and oily water separation technique there is vital effect for problems such as the purifications of solution water pollution and fuel oil.There are many drawbacks as Gravity separate, centrifugal separation, electric separation, adsorbing separation, dissolved air flotation etc. in the method for traditional processing water-oil separating, some separative efficiencies are not high, some chemical agent interpolations too much cause secondary pollution, and the energy consumption also having is too high, costly.New isolation technics is the current major measure that solves sewage disposal and oil purification both at home and abroad as the use of separating and filtering film becomes gradually, at present, utilize filtering net film material and oil absorption material prepared by hydrophobic/lipophilic material successfully to realize the efficient separation that contains in a large number the oil water mixtures of oil slick, for the application of different wellability materials in water-oil separating stepped a successful step.Particularly utilize the different interfacial properties of oil and water, and the special wellability of material (comprising super-hydrophobic, super hydrophilic, super oleophobic, super-oleophilic) builds water-oil separating material, now become one of the study hotspot in this field, to the design and development of effective film material important step wherein especially.
Three kinds of water-oil separating nethike embrane or oil-water separating nets with super-hydrophobic and super oleophylic function in CN1387932A, CN101518695A and CN1721030A, are introduced respectively.Although these separation nethike embranes have all reached the effect of water-oil separating, all have separately certain shortcoming.Some preparation process complexity, the organic matter that some uses are fluorine-containing, what have need to add number of chemical reagent, the preparation of these water-oil separating nethike embranes simultaneously all needs to add as steel mesh, copper mesh, other fabric web such as nylon wire are as support, increase cost of manufacture, water-oil separating nethike embrane material used itself mostly also is the synthetic macromolecular material of chemical industry simultaneously, be difficult for degraded, the lipophile of material itself, make nethike embrane very easily by oil pollution, separate after use, be difficult for processing, conventionally use and burn, the processing method of burying can cause again the secondary pollution problems of environment.
Summary of the invention
An object of the present invention is to provide a kind of method of preparing water-oil separating nethike embrane.
Method provided by the invention, comprises the steps:
1) PLA is dissolved in the organic solvent of PLA described in solubilized, obtains PLA solution;
2) in described PLA solution, add pore-foaming agent to mix, obtain mixed liquor;
3) described mixed liquor is separated, obtains water-oil separating nethike embrane.
In said method, in step 1), the organic solvent of PLA is at least one in Isosorbide-5-Nitrae-dioxane, carrene, chloroform, carbon tetrachloride and toluene described in described solubilized; The molecular weight of described PLA is 50000-100000; The molecular weight of described PLA is specially 69000;
Step 2) in, described pore-foaming agent is inorganic salts, polyethylene glycol or atoleine; Described inorganic salts are specially sodium chloride;
In step 3), described in be separated as described mixed liquor is mixed with the solvent orange 2 A that does not dissolve described PLA, collect solid phase, described solvent orange 2 A is specially absolute ethyl alcohol.
In said method, in step 1), the final concentration of described PLA in described PLA solution is 0.02-0.2g/mL;
Step 2) in, the PLA in described PLA solution and the mass ratio of described pore-foaming agent are 4: 1-4: 3;
In step 3), the time of described mixing is 10-60min, and the time of described mixing is specially 30min.
In said method, in described step 3), also comprise the steps:, by removing described pore-foaming agent, dry in the solvent B of pore-foaming agent described in described solid phase immersion solubilized, to obtain water-oil separating nethike embrane;
Described in described solubilized, the solvent B of pore-foaming agent is specially water, and described dry temperature is 40 DEG C; The time of described immersion is 4-12 hour.
In said method, described water-oil separating nethike embrane has following 1)-3) middle a kind of, two or three feature:
1) described water-oil separating nethike embrane has micron and nano combined loose structure;
2) at the nethike embrane of water-oil separating described in air, the contact angle of water is greater than to 150 °;
3) be 0 ° at the nethike embrane of water-oil separating described in air to oily contact angle.
In said method, the size in described hole is 50nm-300um;
Be 150 °-160 ° at the nethike embrane of water-oil separating described in air to the contact angle of water.
The water-oil separating nethike embrane being prepared by above-mentioned method is also the scope of protection of the invention.
Above-mentioned water-oil separating nethike embrane has following 1)-3) middle a kind of, two or three feature:
1) described water-oil separating nethike embrane has micron and nano combined loose structure;
2) at the nethike embrane of water-oil separating described in air, the contact angle of water is greater than to 150 °;
3) be 0 ° at the nethike embrane of water-oil separating described in air to oily contact angle.
In above-mentioned water-oil separating nethike embrane, the size in described hole is 50nm-300um;
Be 150 °-160 ° at the nethike embrane of water-oil separating described in air to the contact angle of water.
Above-mentioned water-oil separating nethike embrane or the application of above-mentioned PLA in separating oil aqueous mixtures are also the scope of protection of the invention; Described oil is specially n-hexane, benzinum, animal oil, vegetable oil, diesel oil, gasoline or kerosene.
The application in processing or the water body purification of oily water of above-mentioned water-oil separating nethike embrane or above-mentioned PLA is also the scope of protection of the invention.
Water-oil separating nethike embrane prepared by the present invention of experiment showed, of the present invention has the feature stable, separative efficiency is high, can large area prepare, and isolated oil can be recycled, and can be repeatedly used and separate nethike embrane itself, does not affect separating effect.After use is discarded, can in natural environment, degrade, can not produce secondary pollution.The biodegradable water-oil separating nethike embrane with super-hydrophobic super-oleophilic matter of the present invention can be used for the water-oil separating of oil-polluted water, contains the water-oil separating of the oil-polluted water such as edible oil, gasoline as can be used for.
Brief description of the drawings
Fig. 1 is the surface topography stereoscan photograph of the amplification of water-oil separating nethike embrane
Fig. 2 is the overall surface topography stereoscan photograph of water-oil separating nethike embrane
Fig. 3 for measuring the shape picture of water droplet (2 microlitre) on the water-oil separating nethike embrane surface of preparation in air
Fig. 4 for measuring the shape picture of oil droplet (2 microlitre) on the water-oil separating nethike embrane surface of preparation in air
Fig. 5 is experimental provision and the experiment effect photo of water-oil separating nethike embrane for separating of oil and water
Detailed description of the invention
The experimental technique using in following embodiment if no special instructions, is conventional method.
Material, reagent etc. used in following embodiment, if no special instructions, all can obtain from commercial channels.
The preparation of embodiment 1, water-oil separating nethike embrane
1, by PLA(PLA, Shenzhen brilliance great achievement Industrial Co., Ltd., molecular weight=69000, PLLA) be dissolved in 1, in 4-dioxane solvent, being mixed with concentration is the PLA solution of 0.1g/mL, get 4mlPLA solution, add again sodium chloride crystal (to add 0.15g, the mass ratio of PLA and sodium chloride is 8: 3), stir into uniform mixed liquor, then by mixed liquor uniform spreading in substrate of glass, it is smooth that in air, standing 3min(makes PLA solution), again the substrate of glass that is covered with mixed liquor is immersed in absolute ethyl alcohol, be separated 30 minutes, form film,
2, by being again immersed in water after the above-mentioned taking-up of the substrate of glass with film, remove pore-foaming agent sodium chloride, after 10 hours, taking-up is put under 40 DEG C of conditions of baking oven and is dried, and obtains water-oil separating nethike embrane.
The feature of embodiment 2, water-oil separating nethike embrane and Function Identification
1, electron-microscope scanning observation aperture
By the above-mentioned 1 water-oil separating nethike embrane electron-microscope scanning obtaining, amplify 9900 times and observe surface topography, result as shown in Figure 1, can find out, there is the compound loose structure of micro-nano, amplify 460 times of observations as shown in Figure 2, find out that this nethike embrane obtains having the macroporous structure of 50nm-300um under the effect of sodium chloride, the aperture in maximum hole can reach 300um, and minimum aperture is only 50nm.
2, the oil absorption of water-oil separating nethike embrane and hydrophobicity research
In air, 2 microlitre water droplets are dropped in to the above-mentioned 1 water-oil separating nethike embrane obtaining, utilize contact angle measurement, result as shown in Figure 3, can be found out, in air, the contact angle of water is approximately to 152.0 °.
In air, 2 microlitre n-hexanes are dropped in to the above-mentioned 1 water-oil separating nethike embrane obtaining, contact angle measurement detects, and result as shown in Figure 4, can be found out, in air, to 0 ° of oily contact angle.
3, water-oil separating nethike embrane separating oil aqueous mixtures
Benzinum-aqueous mixtures is separated by the above-mentioned 1 water-oil separating nethike embrane obtaining (being clipped in the middle of fixture as shown in Figure 5), obtain the You Heshui after separating, can find out, reached good oil-water separation.
Therefore the separable benzinum of this water-oil separating nethike embrane, n-hexane, gasoline, diesel oil, plant wet goods oil water mixture.
Claims (8)
1. a method of preparing water-oil separating nethike embrane, comprises the steps:
1) PLA is dissolved in the organic solvent of PLA described in solubilized, obtains PLA solution;
2) in described PLA solution, add pore-foaming agent to mix, obtain mixed liquor;
3) described mixed liquor is separated, obtains water-oil separating nethike embrane;
Step 1) in, the organic solvent of PLA is at least one in Isosorbide-5-Nitrae-dioxane, carrene, chloroform, carbon tetrachloride and toluene described in described solubilized; The molecular weight of described PLA is 50000-100000;
Step 2) in, described pore-foaming agent is inorganic salts, polyethylene glycol or atoleine;
Step 3) in, described in be separated as described mixed liquor is mixed with the solvent orange 2 A that does not dissolve described PLA, collect solid phase;
Step 2) in, the PLA in described PLA solution and the mass ratio of described pore-foaming agent are 4:1-4:3;
Step 1) in, the final concentration of described PLA in described PLA solution is 0.02-0.2g/mL;
Step 3) in, the time of described mixing is 10-60min;
In described step 3) in, also comprise the steps:, by removing described pore-foaming agent, dry in the solvent B of pore-foaming agent described in described solid phase immersion solubilized, to obtain water-oil separating nethike embrane;
Described in described solubilized, the solvent B of pore-foaming agent is specially water, and described dry temperature is 40 DEG C; The time of described immersion is 4-12 hour;
Described water-oil separating nethike embrane has following 1)-3) middle a kind of, two or three feature:
1) described water-oil separating nethike embrane has micron and nano combined loose structure;
2) at the nethike embrane of water-oil separating described in air, the contact angle of water is greater than to 150 °;
3) be 0 ° at the nethike embrane of water-oil separating described in air to oily contact angle.
2. method according to claim 1, is characterized in that:
The molecular weight of described PLA is 69000;
Described inorganic salts are sodium chloride;
Described solvent orange 2 A is absolute ethyl alcohol.
3. method according to claim 1, is characterized in that:
The size in described hole is 50nm-300um;
Be 150 °-160 ° at the nethike embrane of water-oil separating described in air to the contact angle of water.
4. the water-oil separating nethike embrane being prepared by method claimed in claim 1;
Described water-oil separating nethike embrane has following 1)-3) middle a kind of, two or three feature:
1) described water-oil separating nethike embrane has micron and nano combined loose structure;
2) at the nethike embrane of water-oil separating described in air, the contact angle of water is greater than to 150 °;
3) be 0 ° at the nethike embrane of water-oil separating described in air to oily contact angle.
5. water-oil separating nethike embrane according to claim 4, is characterized in that:
The size in described hole is 50nm-300um;
Be 150 °-160 ° at the nethike embrane of water-oil separating described in air to the contact angle of water.
6. the application of the water-oil separating nethike embrane described in claim 4 or 5 in separating oil aqueous mixtures.
7. application claimed in claim 6, is characterized in that: described oil is n-hexane, benzinum, vegetable and animals oils, diesel oil, gasoline or kerosene.
8. the application of the water-oil separating nethike embrane described in claim 4 or 5 in processing or the water body purification of oily water.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103157392B (en) * | 2013-03-22 | 2014-12-10 | 清华大学 | Biodegradable oil-water separation net film with super-hydrophobic and super-oleophylic properties and preparation method thereof. |
| CN103263787B (en) * | 2013-05-27 | 2014-12-10 | 中国科学院化学研究所 | Film with oil-water separation tapered needle array having underwater oleophilic property on surface as well as preparation method and use of film |
| CN103316507B (en) * | 2013-06-06 | 2014-12-03 | 华南理工大学 | Super-hydrophilic and underwater-super-oleophobic oil-water separation mesh membrane, and preparation method and application thereof |
| CN105837850B (en) * | 2016-03-11 | 2019-04-19 | 东华理工大学 | A kind of high tenacity and high transparency polylactic acid and preparation method thereof |
| CN107281781B (en) * | 2016-04-11 | 2019-07-09 | 中国科学院宁波材料技术与工程研究所 | Superhydrophilic superoleophobic starch water-oil separationg film, preparation method and application |
| CN110158316B (en) * | 2019-05-29 | 2021-02-26 | 南京大学 | Modified polylactic acid non-woven fabric for oil-water separation and preparation method and application thereof |
| CN113842675B (en) * | 2021-09-26 | 2024-03-15 | 常州大学 | Underwater super oleophobic stainless steel oil-water separation net and preparation method and application thereof |
| CN115746391B (en) * | 2022-12-05 | 2023-09-08 | 江南大学 | Super-hydrophobic polylactic acid film with durable self-cleaning property and preparation method thereof |
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| CN100344341C (en) * | 2005-06-09 | 2007-10-24 | 南京大学 | Super-hydrophobic/super-oleophilic oil-water separating net |
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| EP1093347A2 (en) * | 1998-06-29 | 2001-04-25 | The Procter & Gamble Company | Absorbent article comprising a liquid handling member having high suction and high permeability |
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|---|---|---|---|---|
| CN100344341C (en) * | 2005-06-09 | 2007-10-24 | 南京大学 | Super-hydrophobic/super-oleophilic oil-water separating net |
Non-Patent Citations (2)
| Title |
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| A Morphological Study of Membranes Obtained f rom the Systems Polylactide-Dioxane-Methanol,Polylactide-Dioxane-Water, and Polylactide-N-Methyl Pyrrolidone-Water;P. VAN DE WITTE et al.;《Journal of Polymer Science: Part B Polymer Physics》;19961231;第34卷;第2569页左栏第1段至第2570页右栏第2段 * |
| P. VAN DE WITTE et al..A Morphological Study of Membranes Obtained f rom the Systems Polylactide-Dioxane-Methanol,Polylactide-Dioxane-Water, and Polylactide-N-Methyl Pyrrolidone-Water.《Journal of Polymer Science: Part B Polymer Physics》.1996,第34卷2569-2578. |
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