CN1928527B - Functional nano-fiber based method for extracting and enriching pollutants in water - Google Patents
Functional nano-fiber based method for extracting and enriching pollutants in water Download PDFInfo
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- CN1928527B CN1928527B CN2006100415560A CN200610041556A CN1928527B CN 1928527 B CN1928527 B CN 1928527B CN 2006100415560 A CN2006100415560 A CN 2006100415560A CN 200610041556 A CN200610041556 A CN 200610041556A CN 1928527 B CN1928527 B CN 1928527B
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Abstract
The pollutant-in-water enrichment and extraction method based on functional nano fiber comprises: with electronic-spinning technology, adding or not the functional material, or using post-process fiber surface, manufacturing fiber; preparing members with different diameter and thickness to match with proper fitting. This invention can improve interactive force between fiber and target, reduces balance time, and fit to instrumental analysis.
Description
Technical field
The present invention relates to a kind of extracting process, particularly relate to a kind of abstraction technique that is used for the water pollutant enrichment based on functional nano-fiber.The technical field that belongs to the water pollutant extracting and enriching.
Background technology
Because global Pollution by Chemicals is on the rise, various inorganicss, organic lasting contaminative attract much attention gradually to the harm of environmental ecology and human health, the detection of this pollutant have been become a day-to-day work of environment measuring department.
At present the method at the enrichment of pollutant in the water sample mainly contains: liquid-liquid extraction, Solid-Phase Extraction and solid-phase microextraction.Liquid-liquid extraction method generally has the extraction efficiency height, invests characteristics such as less, but liquid-liquid extraction method is only applicable to the improvement of high concentration poisonous organic wastewater, and liquid liquid separation difficulty, extractant easily runs off and causes secondary pollution, the energy consumption height, analysis time is longer, and the recovery is relatively low, and these shortcomings have seriously restricted the use of liquid-liquid extraction method.
Solid-Phase Extraction (SPE) is a kind of effective trace or trace materials isolation of purified means, success avoid liquid-liquid extraction many problems in institute generation.Compare with liquid-liquid extraction, Solid-Phase Extraction is more effective, reaches quantified extract easily, and quick and robotization has also reduced solvent load and working time simultaneously, but generally still needed to evaporate dried solvent, to reach concentrated purpose.The solid-phase microextraction that grows up on the Solid-Phase Extraction basis (SPME) is because of using no or little organic solvent in its extraction process, can not cause secondary pollution and receives much concern.This technology belongs to non-extraction fully, the example enrichment finite capacity, and to time, the temperature of extraction, conditions such as the position of fiber coat are wanted strict control, but these two kinds of methods have limited it and have used widely because of its expensive cost.
Summary of the invention
Technical matters: the objective of the invention is to overcome defective such as complicated operation, cost height, the efficient of prior art is low, thereby adopt functional nano-fiber spe membrane material, utilize the strong adsorptive power of nanostructured surface, with various functional group decorated nanometer fibre structures surface, make it selection adsorbability be arranged, a kind of easy and simple to handle, water pollutant method for extracting and enriching based on functional nano-fiber that efficient is high, with low cost is provided different pollutants.
Technical scheme: the water pollutant method for extracting and enriching based on functional nano-fiber of the present invention comprises the steps:
1) according to the chemical property for the treatment of the enrichment pollutant, by adding functional mass interactional or carrying out surface treatment, utilize electrospinning to prepare the functional nano fiber film material with it, this functional nano fiber film material is installed on the specific extraction equipment;
2) with after the above functional nano fiber film material usefulness appropriate solvent activation processing, be placed in the pending water sample, beating action by stirring rod on the enriching apparatus, pollutant in the absorption ambient water environment, enriching pollutants in the water body has arrived functional nano fiber film material surface, and this film plays the effect of Solid-Phase Extraction;
3) will more than be enriched with pollutant the functional nano fiber film material put into a conical filtering pipe, with acid or alkali or organic solvent, or the mixture of acid, alkali, organic solvent, pollutant is eluted by ambient pressure,
Described interactional functional mass to metal pollutant, is complexing agent; For phenolic comp ' ds pollution, be the material of containing metal element; For ionic compound,,, be the antibody of this molecule for macromolecular substances for containing the compound of gegenion.Described solvent is that water and water are the acid or the alkali of matrix; Or water and alcohol or ketone mixed solvent; Or alcohol, ketone, acid, alkali, ether organic solvent.Fibre diameter in the described functional nano fiber film material is 10-1000nm, and fiber surface is level and smooth or porous.The functional nano fibrous material is organic inorganic or organic and nanofiber that inorganic material mixes, and the functional nano-fiber of above-mentioned a few class nanofiber particular functional group's chemical modification that is carrier, or natural polymkeric substance.In the described functional nano fibrous material, the organic material of functional nano fiber is a kind of in polyoxyethylene, polyvinyl alcohol (PVA), Polyethylene Naphthalate, polyaniline, polyacrylic acid, polyacrylonitrile, polystyrene, polymethylmethacrylate, poly-N-isopropyl acrylamide, polyvinyl acetate and the derivant thereof; The material of inorganic nanofiber is a kind of in silicon dioxide, titania, the carbon; Natural polymkeric substance is a kind of in polysaccharide, polypeptide, cellulose, PLA, casein and the derivant thereof.Described conical filtering pipe volume is 10 μ l-5ml.
Beneficial effect: compare with existing various abstraction techniques, the advantage of the extracting process of the water pollutant enrichment based on functional nano-fiber provided by the invention is:
1) because the specific surface area of nanofiber is huge, and modified specific functional group, stronger and target molecule interaction force have been arranged.Only use the adsorbent of trace, sorption extraction efficient but can improve greatly;
2) water pollutant since corresponding molecule two chemical potential energy differences between the homophase not, the net flow from a phase transfer to the another one phase can reach a balance in the sufficiently long sampling time.Need not other energy source.
3) in the Membrane Extraction, as long as functional film material is fit in the specific accessory, put into water sample, start stirring and get final product, operating procedure and equipment are simple;
4) functional membrane that will be enriched with pollutant is put into a tapered tube, only needs to use the seldom solvent of volume, pollutant can be eluted by ambient pressure;
5) tapered tube that is used for wash-out does not need filter plate or filter disc, relies on the awl point of taper extracting tube can support the fiber of uniting, and uses the syringe pressurization, and that can carry out sample fast crosses post, washing and wash-out, easy to operation;
6) compare with SPE, the solvent of use is few, can save the process that organic solvent volatilizes substantially, effectively avoids environmental pollution; Compare with existing SPME, loading capacity is big, the extraction equilibrium time short (with benzene is example, to sample little, nanomolar concentration, only needs about 15min), must not control extraction and analysis condition harshly;
7) the present invention has the bioaccumulation efficiency height, and clean-up effect is strong, handles sample time weak point, characteristics such as applied range.
Embodiment
The invention provides a kind of abstraction technique, comprise the steps: based on enriching pollutants in the water sample of functional nano-fiber
1) according to the chemical property for the treatment of the enrichment pollutant, adds functional mass interactional, utilize electrospinning to prepare the functional nano fiber film material, this film is installed on the specific extraction equipment with it.Be example with the polystyrene now, briefly narrate its preparation process:
(PS) is dissolved in N with polystyrene, makes PS solution in dinethylformamide (DMF) and tetrahydrofuran (THF) mixed liquor, carries out electrospinning;
Nanofiber diameter is 10-1000nm, and fiber surface is level and smooth or porous;
2) step 1) is installed in functional nano fiber film material on the extraction equipment and embathes activation processing successively with methyl alcohol or ethanol and water after, be placed in the water sample for the treatment of enrichment, beating action (suitable rotational speed) by stirring rod on the enriching apparatus, through reasonable time, the pollutant in the absorption ambient water environment.Enriching pollutants in the water body has arrived the fiber surface of functional nano fiber film material, finishes the effect of extraction;
3) with step 2) in be enriched with pollutant functional membrane put into a tapered tube, according to the ratio of the every 1mg nanofiber of 5-20 μ l/, the solvent with certain volume elutes pollutant by ambient pressure.
Described interactional functional mass to metal pollutant, is complexing agent; For phenolic comp ' ds pollution, be the material of containing metal element; For ionic compound, for containing the compound of gegenion; For macromolecular substances, be the antibody of this molecule.Described solvent is that water and water are the acid or the alkali of matrix; Or water and alcohol or ketone mixed solvent; Or alcohol, ketone, acid, alkali, ether organic solvent.The functional nano fibrous material is organic inorganic or organic and nanofiber that inorganic material mixes, and the functional nano-fiber of above-mentioned a few class nanofiber particular functional group's chemical modification that is carrier, or natural polymkeric substance.In the described functional nano fibrous material, the organic material of functional nano fiber is a kind of in polyoxyethylene, polyvinyl alcohol (PVA), Polyethylene Naphthalate, polyaniline, polyacrylic acid, polyacrylonitrile, polystyrene, polymethylmethacrylate, poly-N-isopropyl acrylamide, polyvinyl acetate and the derivant thereof; The material of inorganic nanofiber is a kind of in silicon dioxide, titania, the carbon; Natural polymkeric substance is a kind of in polysaccharide, polypeptide, cellulose, PLA, casein and the derivant thereof.Described conical filtering pipe volume is 10 μ l-5ml.
Described step 2) pollutant is in the water sample: alkane, alkene, benzene, substituted benzene, organism such as palycyclic aromatic, aldehyde, ketone, acid, ester; Inorganicss such as metallic ion, mineral acid, alkali, big molecule such as albumen, polysaccharide.
The fiber of nanometer diameter has big specific surface area, stronger and object interaction ability are arranged, adsorption capacity height to object, reaching the effect balance time also significantly reduces, can be efficiently, fast water pollutant is gathered and pre-service, to the collection of the adding up property of the pollutant time of carrying out in the environment, can be with various instrument analytical method quantitative test behind the wash-out; This invention belongs to solvent-free abstraction technique, only uses a small amount of solvent to come wash-out in the processing procedure, improves accuracy, reduces environmental pollution; Than higher, operating procedure and equipment are simple to persistent pollutant enrichment multiple for the method.
Claims (2)
1. the water pollutant method for extracting and enriching based on functional nano-fiber is characterized in that this method comprises the steps:
1) according to the chemical property for the treatment of the enrichment pollutant, by adding functional mass interactional, utilize electrospinning to prepare the functional nano fiber film material with it, this functional nano fiber film material is installed on the specific extraction equipment;
2) above functional nano fiber film material is handled with activating solvent after, be placed in the pending water sample, beating action by stirring rod on the enriching apparatus, pollutant in the absorption ambient water environment, enriching pollutants in the water body has arrived functional nano fiber film material surface, and this film plays the effect of Solid-Phase Extraction;
3) will more than be enriched with pollutant the functional nano fiber film material put into a conical filtering pipe, with acid or alkali or organic solvent, or the mixture of acid, alkali, organic solvent, pollutant is eluted by ambient pressure;
Described interactional functional mass to metal pollutant, is complexing agent; For phenolic comp ' ds pollution, be the material of containing metal element; For ionic compound, for containing the compound of gegenion; For macromolecular substances, be the antibody of this molecule; Fibre diameter in the described functional nano fiber film material is 10-1000nm, and fiber surface is level and smooth or porous; The functional nano fibrous material is organic inorganic or organic and nanofiber that inorganic material mixes, or natural polymkeric substance;
In the described functional nano fibrous material, the organic material of functional nano fiber is a kind of in polyoxyethylene, polyvinyl alcohol (PVA), Polyethylene Naphthalate, polyaniline, polyacrylic acid, polyacrylonitrile, polystyrene, polymethylmethacrylate, poly-N-isopropyl acrylamide, polyvinyl acetate and the derivant thereof; The material of inorganic nanofiber is a kind of in silicon dioxide, titania, the carbon; Natural polymkeric substance is a kind of in polysaccharide, polypeptide, cellulose, PLA, casein and the derivant thereof.
2. the water pollutant method for extracting and enriching based on functional nano-fiber according to claim 1 is characterized in that described conical filtering pipe volume is 10 μ l-5ml.
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| CN103163254A (en) * | 2013-02-04 | 2013-06-19 | 国家海洋局天津海水淡化与综合利用研究所 | Method of trace quantity persistent organic pollutant in enrichment and separation seawater |
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| CN101532921B (en) * | 2008-03-11 | 2011-07-27 | 中国科学院生态环境研究中心 | Passive sampling device with hollow fiber membrane |
| CN101497034B (en) * | 2009-01-05 | 2010-12-08 | 东南大学 | Solid phase extraction method based on nylon nano fiber film and extractor |
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| CN1806880A (en) * | 2005-12-19 | 2006-07-26 | 东南大学 | Solid phase micro-extraction device based on nanometer fiber |
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| CN1552499A (en) * | 2003-05-27 | 2004-12-08 | 中国科学院生态环境研究中心 | Memberane extracting method for trace organic pollutant in water |
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