CN102755764B - Based on oily-water seperating equipment and the method for carbon nano-tube film - Google Patents
Based on oily-water seperating equipment and the method for carbon nano-tube film Download PDFInfo
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- CN102755764B CN102755764B CN201210270301.7A CN201210270301A CN102755764B CN 102755764 B CN102755764 B CN 102755764B CN 201210270301 A CN201210270301 A CN 201210270301A CN 102755764 B CN102755764 B CN 102755764B
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Abstract
The invention discloses a kind of oily-water seperating equipment based on carbon nano-tube film and method.The present invention is using carbon nano-tube film as filter membrane, realizes the separation to oil mixing with water system.The network that described carbon nano-tube film is interweaved by CNT forms, and thickness is in 10-500 nanometer range, and membrane aperture is in 2-1000 nanometer range, and film surface has the character of hydrophobic oleophilic oil, and acid and alkali-resistance better tolerance, in scope inner structure and the stable performance of pH value 1-14.Described oil mixing with water system comprises the system or emulsification profit (water-in-oil type or oil-in-water type) that oil phase and aqueous phase be directly mixed to form.The present invention can be used for low cost, the high-throughout efficient quick separating of the multiple oil water mixture in the fields such as production, life, petrochemical industry, machinery.
Description
Technical field
The present invention relates to a kind of oily water separating equipment and method, particularly relate to a kind of oily-water seperating equipment based on carbon nano-tube film and method, belong to functional material, chemical and field of environment protection.
Background technology
Water-oil separating is a global study hotspot.Due to increasing the weight of of trade effluent problem in recent years, and the generation of the environmental problem such as offshore oil leakage, water-oil separating material obtains people and more and more pays close attention to.Because water-oil separating is an interface characteristics problem, use has special infiltrating material and is prepared into porous membrane structure, according to the difference of its surface nature, thus can reach the separation carrying out oil water mixture.But the product of water-oil separating film is relatively less now, main employing is prepared by polymer or composite, and not only cost is higher, stability of material and reuse efficiency and also all need to be improved further, and the separation be only applicable to specific oil mixing with water system, the scope of application is narrow.
Summary of the invention
The object of the present invention is to provide a kind of oily-water seperating equipment based on carbon nano-tube film and method, it can realize efficient, the quick separating of multiple oil water mixture, and simple to operate, with low cost, thus overcomes deficiency of the prior art.
For achieving the above object, present invention employs following technical scheme:
Carbon nano-tube film is as the application of water-oil separating filter membrane, and described carbon nano-tube film has and to be interweaved the network structure formed by many CNTs.
Based on an oily-water seperating equipment for carbon nano-tube film, it comprises:
Carbon nano-tube film, described carbon nano-tube film has and to be interweaved the network structure formed by many CNTs;
And, for the supporting mechanism of fixing described carbon nano-tube film.
Further, the thickness of described carbon nano-tube film is 10-500nm, and membrane aperture is 2-1000nm.
Described supporting mechanism comprises porous-substrates.
Described porous-substrates be at least selected from wire netting, fabric, macromolecular filter membrane, ceramic membrane any one, but to be not limited thereto.
A kind of oily water separating equipment, it is characterized in that, it comprises oily-water seperating equipment as above.
A kind of oil-water separation method, it is characterized in that, the method is: inputted by oil water mixture in oily-water seperating equipment as above or in oily water separating equipment as above, make oil phase pass through carbon nano-tube film, and make aqueous phase by carbon nano-tube film detention, realize being separated of oil phase and aqueous phase.
Further, the oil water mixture that described oil water mixture is at least selected from oil, aqueous phase is directly mixed to form and oil emulsion aqueous systems, described oil emulsion aqueous systems comprises microemulsion and unstable suspension.
As one of preferred scheme, for the oil mixture formed by two or more oil phase substance, first aqueous phase system extraction more than one oil phase substance are wherein utilized, form oil water mixture, again described oil water mixture is inputted in oily-water seperating equipment as above or in oily water separating equipment as above, make oil phase by carbon nano-tube film, and make aqueous phase by carbon nano-tube film detention, realize being separated of oil phase and aqueous phase.
The method can be carried out under pressure is the air pressure conditions of-1MPa ~ 1MPa.
Compared with prior art, advantage of the present invention is at least:
(1) raw material adopts commercially available single wall, double-walled or multi-walled carbon nano-tubes, to its process for dispersing without any restriction, as long as target can form the carbon nano-tube film of self-supporting, surface, without any modification and modification, just can utilize the character of carbon nano-tube film itself to carry out water-oil separating.
(2) CNT is relative to the polymer on market; the water-oil separating film of composite, has stable in properties, can resist various acidity or alkaline solution; therefore may be used for the water-oil separating under extreme condition, environmental protection aspect tool is had very important significance.
(3) carbon nano-tube film can be different according to the consumption of CNT simply, control its thickness and aperture.And can obtain aperture is nanometer or sub-micron rank completely, even several nanometer or tens nanometer range adjustable, be not available for general polymer or composite porous film material.The dimensional effect that nano level aperture provides, makes emulsification profit can obtain highly purified separation.
(4) carbon nano-tube film can repeatedly use.In separation of emulsions process, due to breakdown of emulsion and water-oil separating, cause emulsifying agent or separation to meet to deposit at filter membrane surface, the flux that impact is separated, if but wash based on the simple ethanol of diffusion barrier of carbon nano-tube film, just can take out adsorption material, recover evc flux, ensure high separative efficiency.
(5) carbon nano-tube film stable chemical nature, can antiacid alkali resistant, can be used for the separation of the oil water mixture containing a large amount of acid or alkali.
Accompanying drawing explanation
Fig. 1 by the embodiment of the present invention 1 the SEM photo of employing carbon nano-tube film;
Fig. 2 a and 2b is the contact angle photo on the carbon nano-tube film surface that the embodiment of the present invention 1 uses with water droplet and oil droplet (for carrene) respectively;
Fig. 3 is the structural representation of oily-water seperating equipment in the embodiment of the present invention 1, and wherein each assembly and Reference numeral thereof are respectively: carbon nano-tube film 1, open support substrate 2(ceramic membrane).
Detailed description of the invention
Traditional oil-water separation method mainly contains the methods such as extraction, distillation, but this class methods general operation is numerous and diverse, and often causes a large amount of losses of recyclable goods and materials, also easily causes environmental pollution, so people have developed again other multiple water-oil separating technique.What current research was more is uses and has special infiltrating material and be prepared into porous membrane structure, then by the difference of this type of porous film surface character, thus reach the separation carrying out oil water mixture.Existing perforated membrane is made primarily of polymer or composite, its separative efficiency, service life, the scope of application are all very limited, but up to now, industry not yet develops can replace this type of perforated membrane, and the oily water separating equipment that performance is more superior.
Inventor finds to utilize carbon nano-tube film very unexpectedly, especially the separation of oil mixing with water system can be realized by many CNTs that formed, that the there is network structure carbon nano-tube film that is woven, and separative efficiency is high, after being separated, aqueous phase and oil phase all have higher degree.And, inventor also finds, the oily-water seperating equipment formed with carbon nano-tube film all has good tolerance to acid or basic oil water mixed system, and all can produce good separation effect, after repeatedly using, still there is excellent water-oil separating performance.
Based on aforementioned unexpected discovery, inventor spy proposes oily-water seperating equipment of the present invention and method.
This oily-water seperating equipment is primarily of carbon nano-tube film and supporting member composition thereof; Carbon nano-tube film is made up of the interleaving network of CNT, and thickness is in 10-500 nanometer range, and membrane aperture is in 2-1000 nanometer range.
Foregoing carbon nanotubes film can be made up of commercially available common single wall and/or double-walled and/or multi-walled carbon nano-tubes, or also can comprise the materials such as other dispersant of commonly seeing.
And, especially it is pointed out that CNT not must in advance chemistry and physical treatment, its film build method is unrestricted.Such as, the preparation method of foregoing carbon nanotubes film can pass through dip coated by carbon nano tube dispersion liquid, spraying coating, spinning, filters or (continuously) vacuum filtration (before proposing see inventor case CN 102110489A etc.), chemical vapour deposition (CVD), Langmuir – Blodgett (LB) embrane method, the techniques such as solution-cast is shaping are formed, and are separated after formation in substrate, form self-supported membrane.Or, according to substrate system porous material, also can with porous material one directly form oily-water seperating equipment.
The form of foregoing supporting member, structure or material can according to the needs of practical application unrestricted choice.Wherein, as one of preferred scheme, foregoing supporting member can adopt porous-substrates, described porous-substrates can be wire netting, fabric, various apertures macromolecular filter membrane, ceramic membrane etc., but be not limited thereto, in the process implementing water-oil separating, carbon nano-tube film can directly be placed on porous-substrates, comprises (emulsification) water-oil separating in pressure-driven or without realizing water-oil separating under pressure-driven.
This oil-water separation method is:
(1) oil water mixture is inputted in aforementioned oil water separator, under normal pressure or secondary stress effect (pressure limit can from-1MPa to 1MPa), oil phase by carbon nano-tube film, aqueous phase then not by, thus reach the object of separation.
(2) oil water mixture inputs in aforementioned oil water separator, without under ambient pressure effect, relies on self gravitation effect, oil phase by carbon nano-tube film, aqueous phase then not by, thus reach the object of separation.
Aforementioned oil water mixture comprises: the oil water mixture that two-phase directly mixes, various emulsification profits etc.Wherein emulsification profit comprises unstable suspension and microemulsion, but is not limited thereto.
In addition, for oil phase/oil mixture, the difference of two kinds of oil phase polarity can be utilized, will wherein one be extracted in aqueous phase, passing through UF membrane.
Below in conjunction with accompanying drawing and some preferred embodiments, technical scheme of the present invention is elaborated.
embodiment 1
(1) get the CNT disperseed in suitable quantity of water solution, suction filtration film forming, after drying, substrate (e.g., hydrophilic filter membrane) is dissolved away.Obtain the carbon nano-tube film (consulting Fig. 1) of self-supporting.Above-mentioned obtained carbon nano-tube film is transferred on ceramic membrane, is placed in separation container.
(2) get isopyknic carrene and water mixing, after concuss, layering disappears, and then pours in separator, under the effect of pressurization, realizes being separated of carrene and water.
embodiment 2
(1) get the CNT disperseed in suitable quantity of water solution, suction filtration film forming, after drying, substrate (e.g., hydrophilic filter membrane) is dissolved away.Obtain the carbon nano-tube film of self-supporting.Above-mentioned obtained carbon nano-tube film is transferred on ceramic membrane, is placed in separation container.
(2) get the carrene of volume ratio 5:1 and water mixing, after concuss, layering disappears, and then pours in separator, under the effect of pressurization, realizes being separated of carrene and water.
embodiment 3
(1) get the CNT disperseed in suitable quantity of water solution, suction filtration film forming, after drying, substrate (e.g., hydrophilic filter membrane) is dissolved away.Obtain the carbon nano-tube film of self-supporting.Above-mentioned obtained carbon nano-tube film is transferred on ceramic membrane, is placed in separation container.
(2) get the carrene of volume ratio 1:5 and water mixing, after concuss, layering disappears, and then pours in separator, under the effect of pressurization, realizes being separated of carrene and water.
embodiment 4
(1) get the CNT disperseed in suitable quantity of water solution, suction filtration film forming, after drying, substrate (e.g., hydrophilic filter membrane) is dissolved away.Obtain the carbon nano-tube film of self-supporting.Above-mentioned obtained carbon nano-tube film is transferred on ceramic membrane, is placed in separation container.
(2) get the isopyknic carbon disulfide of body and water mixing, after concuss, layering disappears, and then pours in separator, under the effect of pressurization, realizes being separated of carbon disulfide and water.
embodiment 5
(1) get the CNT disperseed in suitable quantity of water solution, suction filtration film forming, after drying, substrate (e.g., hydrophilic filter membrane) is dissolved away.Obtain the carbon nano-tube film of self-supporting.Above-mentioned obtained carbon nano-tube film is transferred on ceramic membrane, is placed in separation container.
(2) get the carbon disulfide of volume ratio 10:1 and water mixing, after concuss, layering disappears, and then pours in separator, under the effect of pressurization, realizes being separated of carbon disulfide and water.
embodiment 6
(1) get the CNT disperseed in suitable quantity of water solution, suction filtration film forming, after drying, substrate (e.g., hydrophilic filter membrane) is dissolved away.Obtain the carbon nano-tube film of self-supporting.Above-mentioned obtained carbon nano-tube film is transferred on ceramic membrane, is placed in separation container.
(2) get volume ratio 1:10 carbon disulfide and water mixing, after concuss, layering disappears, and then pours in separator, under the effect of pressurization, realizes being separated of carbon disulfide and water.
embodiment 7
Select carrene/aqueous systems separate benzoic acid and aniline mixed system
(1) benzoic acid is slightly soluble in water, but when pH value=12.6, just can be entirely molten; And when pH=13, benzoic acid is under carrene/aqueous systems, and nearly all in aqueous phase, but aniline is still dissolved in the middle of carrene.
(2) according to the analysis of (1), by aniline, benzoic acid each 0.1g solution 5 ml CH
2cl
2in solution, then add isopyknic NaOH solution (pH=13), vibration, leave standstill for several times, then filter by self-supporting single-wall carbon nanotube membrane obtained above, obtain oil reservoir and water layer respectively.
Carrene/aqueous systems is selected to be separated aniline and toluene mixed system
(3) aniline is water-soluble, but solubility is lower, but during pH=5.3, what aniline can be a large amount of is dissolved in water
(4) aniline (0.05g) is dissolved in toluene (2 ml), joins 5 ml CH
2cl
2in solution, then add isopyknic HCl solution (pH=2), vibration, leave standstill for several times, then filter by self-supporting single-wall carbon nanotube membrane obtained above, obtain oil reservoir and water layer respectively.
embodiment 8
(1) configure the unstable emulsion of Water-In-Oil, choose toluene respectively, cyclohexane, benzinum is oil phase, adds a certain proportion of water, after ultrasonic certain hour, obtains milky water-in-oil emulsion.
(2) above-mentioned self-supporting carbon nano-tube film is selected, above-mentioned obtained water-in-oil emulsion is joined in the middle of separator, under the effect of pressurization, toluene, cyclohexane, benzinums etc. can pass through carbon nano-tube film, and water not by, and leach three kinds of oil phases are what clarify, in this separation process, the breakdown of emulsion of emulsion and water-oil separating are synchronously carried out.
embodiment 9
(1) configure the unstable emulsion of Water-In-Oil, choose the mixed liquor oil phase of toluene and cyclohexane, add a certain proportion of water, after ultrasonic certain hour, obtain milky water-in-oil emulsion.
(2) above-mentioned self-supporting carbon nano-tube film is selected, above-mentioned obtained water-in-oil emulsion is joined in the middle of separator, under the effect of pressurization, oil phase can pass through carbon nano-tube film, and water not by, and the oil phase leached is clarification, in this separation process, the breakdown of emulsion of emulsion and water-oil separating are synchronously carried out.
embodiment 10
(1) configure Water-In-Oil stable emulsion, choosing toluene is oil phase, and sorbester p17, as emulsifying agent, adds a certain proportion of water, after stirring certain hour, obtains milky water-in-oil emulsion.
(2) above-mentioned self-supporting carbon nano-tube film is selected, adding obtained water-in-oil emulsion joins in the middle of separator, under the effect of pressurization, toluene can pass through carbon nano-tube film, and water not by, and the toluene leached is clarification, in this separation process, the breakdown of emulsion of emulsion and water-oil separating are synchronously carried out.
Above-described embodiment is only for illustrating technical conceive of the present invention and feature; its object is to allow the understanding being familiar with technique can understand content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences done according to Spirit Essence of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (4)
1. based on an oily-water seperating equipment for carbon nano-tube film, it is characterized in that, it comprises:
Self-supporting carbon nano-tube film, described carbon nano-tube film has and to be interweaved the network structure formed by many CNTs, and the thickness of described carbon nano-tube film is 10-500nm, and membrane aperture is 2-1000nm;
And for the supporting mechanism of fixing described carbon nano-tube film, described supporting mechanism adopts porous-substrates.
2. the oily-water seperating equipment based on carbon nano-tube film according to claim 1, is characterized in that, described porous-substrates be at least selected from wire netting, fabric, macromolecular filter membrane, ceramic membrane any one.
3. an oily water separating equipment, is characterized in that, it comprises the oily-water seperating equipment according to any one of claim 1-2.
4. an oil-water separation method, it is characterized in that, the method for: by the oily-water seperating equipment of oil water mixture input as claim 1-2 according to any one of or as claimed in claim 3 oily water separating equipment, oil phase is made to pass through carbon nano-tube film, and make aqueous phase by carbon nano-tube film detention, realize being separated of oil phase and aqueous phase.
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| CN103418252A (en) * | 2013-07-20 | 2013-12-04 | 大连理工大学 | Ceramic base carbon nano tube inorganic composite membrane and preparation method thereof |
| CN103470852A (en) * | 2013-09-12 | 2013-12-25 | 东南大学 | Microfluid valve gear based on electrowetting technology |
| CN104548666B (en) * | 2014-12-10 | 2016-04-06 | 东华大学 | Nanofiber foam-based oil hydrosol serialization separation apparatus and preparation method thereof |
| CN104857742B (en) * | 2015-05-28 | 2017-05-31 | 重庆理工大学 | A kind of water-eliminating method of dichloromethane |
| CN105688447B (en) * | 2016-01-21 | 2018-02-06 | 北京理工大学 | A kind of filter screen and its femtosecond laser preparation method of achievable high efficiency water-oil separating |
| CN110038444B (en) * | 2018-01-17 | 2021-09-28 | 中国工程物理研究院材料研究所 | Use and preparation method of novel carbon nanotube separation membrane |
| CN108786273A (en) * | 2018-08-10 | 2018-11-13 | 安徽原野滤材有限公司 | A kind of oil-resistant high-temperature filter cloth for water-oil separating |
| CN110624428B (en) * | 2019-10-21 | 2021-11-19 | 天津工业大学 | Membrane emulsification system |
| CN113819669B (en) * | 2021-09-15 | 2023-05-09 | 浙江大学 | Low-temperature refrigeration device and method based on carbon nano tube gravity oil separation effect |
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| JP2009092949A (en) * | 2007-10-09 | 2009-04-30 | Tokai Kogaku Kk | Optical member and its manufacturing method |
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| CN101450288A (en) * | 2007-11-30 | 2009-06-10 | 清华大学 | Fiber membrane and preparation method thereof |
| CN101607704A (en) * | 2009-07-14 | 2009-12-23 | 清华大学 | A kind of carbon nanotube cotton and preparation method thereof |
| CN102600667A (en) * | 2012-02-13 | 2012-07-25 | 清华大学 | Air filter material based on carbon nano tube and preparation method thereof |
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