CN103091429A - Preparation method and application of solid phase extraction membrane comprising amphipathicity functional group - Google Patents
Preparation method and application of solid phase extraction membrane comprising amphipathicity functional group Download PDFInfo
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- CN103091429A CN103091429A CN2012105934348A CN201210593434A CN103091429A CN 103091429 A CN103091429 A CN 103091429A CN 2012105934348 A CN2012105934348 A CN 2012105934348A CN 201210593434 A CN201210593434 A CN 201210593434A CN 103091429 A CN103091429 A CN 103091429A
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Abstract
The invention relates to a solid phase extraction membrane comprising an amphipathicity functional group and applications of the solid phase extraction membrane in enrichment and extraction of trace phenols in an environment water body. A macromolecular non-woven cloth solid phase extraction membrane material with the amphipathicity functional group is prepared by taking a polypropylene and polyethylene copolymerization melt-blown non-woven cloth material as a base material and uniformly and respectively bonding a lipophilic unsaturated fattyacid alkyl ester monomer and hydrophilic ethoxyethanol unsaturated fattyacid alkyl ester to the surface of the non-woven cloth material. The non-woven cloth prepared by the invention contains a crylic acid alkyl ester lipophilic group and a hydroxyl alkyl ester hydrophilic group, so that in the process of extracting a phenol type polar compound, the non-woven cloth synchronously develops nonpolar intermolecular force and hydrogen-bond interaction and has relatively high extraction performance. The non-woven cloth material is used for preparing a solid-phase disk membrane; and in a water sample enrichment process, the mass transfer speed is high; and a large size of environment water samples can be quickly enriched and extracted.
Description
Technical field
The present invention relates to a kind of Solid-Phase Extraction diaphragm and application that contains amphipathic functional group.Relate in particular to the amphipathic Solid-Phase Extraction diaphragm that Determination of Trace Phenol compounds in environment water is had the extracting and enriching performance.
Background technology
The environmental monitoring and analysis object is more and more trace and even contaminant trace species, although instrument analytical method can reach even ultratrace level of trace at present, yet for complex sample, due to the existence of matrix effect and interfering material, Direct Analysis is still very difficult.The pre-treatments such as the separation of therefore, carrying out before sample analysis, enrichment concentrate are extremely important for the acquisition of final accurate result.The solid phase extraction techniques that 20 century 70 later stages grew up is high for the enrichment factor of sample, rate of extraction is fast, quantity of solvent is few, and easy and Modern Analytical Instrument coupling is now widely used sample-pretreating method.
Phenol and compound thereof are to be present in one of typical organic contaminant in environment water, have potential high toxicity and carcinogenicity, this compounds is at China's integrated wastewater discharge standard (GB8978-1996), water environment quality standard (GB3838-2002), in drinking water sanitary standard (GB5749-2006) by clear emission limit, be a class water pollutant of priority control.In drinking water sanitary standard, take the concentration limit of the volatile phenol of phenol amount representative and compound thereof only as 0.002mg/L.
At present, the assay method stipulated in China's water quality standard of phenol compound is mainly:
(1) 4-AA spectrophotometric method.The method detection limit can reach 0.002mg/L, but at first the method need to distill water sample, then adopts chloroform extraction to measure.The method is consuming time longer, and needs to use poisonous organic solvent.
(2) gas chromatography and liquid phase chromatography.If in water body, phenolic compound concentration is lower, need water sample is measured its content again with resin concentration or after carrying out solid phase extraction concentration.Adopt resin method enrichment water sample need to load the polymeric adsorbent chromatographic column, then use sodium bicarbonate aqueous solution drip washing resin, remove organic acid, then with measuring after the acetonitrile wash-out.Adopt solid phase extraction, can adopt solid phase extraction column or the extraction disc diaphragm of octadecyl silane filler.The filler of 18 alkyl silica gel bonding is a kind of universal sorbing material, has enrichment performance preferably for low pole and nonpolar organic matter, but phenol compound has nonpolar owing to having phenolic hydroxyl group and phenyl so molecule one end has the polarity other end.Adopt octadecyl silane such compound with certain polarity to be extracted often efficient is not high.If fiber material contains lipophilicity and hydrophilic radical simultaneously, bring into play simultaneously the nonpolar suction-operated of fiber material lipophilicity group and the hydrogen bond action of hydrophilic radical, can greatly improve the extraction efficiency of its Pyrogentisinic Acid's compounds.
In sum, often relate to the extracting and enriching of sample for detection of the analytical approach of low concentration in the analysis environments water body and Determination of Trace Phenol compounds, and therefore the defective such as all there are in various degree complicated operation in existing enrichment and extracting process, use poisonous organic solvent, extraction efficiency is low is necessary to develop a kind of extracting and enriching material and method that is suitable for Low Concentration of Benzene phenolic compound in environment water.
Summary of the invention
For the problems referred to above, the object of the invention is to provide a kind of functional organic polymer fiber material with water wettability and lipophilicity group.Another object of the present invention is to provide the purposes of above-mentioned amphipathic fiber material low concentration and Determination of Trace Phenol compounds in the extracting and enriching environment water, to improve the extracting and enriching efficient of this compounds.
The technical solution used in the present invention is as follows:
The present invention is take the macromolecule nonwoven cloth material as base material, in the high-energy electron beam irradiation system, respectively two kinds of opposed polarity monomer unsaturated fat acid alkyl esters and glycol monomethyl unsaturated fat acid alkyl ester evenly are bonded to macromolecule nonwoven cloth material surface, preparation has the macromolecule solid phase fiber material of amphipathic functional group.Of the present inventionly contain amphipathic functional group macromolecule nonwoven fabrics Solid-Phase Extraction material, what comprise macromolecule nonwoven fabrics matrix material and macromolecule nonwoven fabrics matrix bonding contains the functional group strand.Polymer base material is polypropylene and tygon copolymerization meltblown fibers nonwoven cloth material, and fibre diameter is 8～20 μ m.
A kind of lipophilicity monomer of selecting, the unsaturated fat acid alkyl ester is the alkyl acrylate of straight or branched; Another kind of hydrophilic monomer, glycol monomethyl unsaturated fat acid alkyl ester is diethylene glycol monoacrylate or ethylene glycol methacrylate.The present invention adopts in the high-energy electron beam irradiation system, two kinds of monomers and macromolecule nonwoven fabrics matrix material are reacted and is bonded in substrate material surface formation and contains the functional group strand.
The process of macromolecule nonwoven cloth material and two kinds of different monomers reactions, at first preparation contains the reacting solution of two kinds of difference in functionality monomers.This reacting solution contains respectively the alkyl acrylate of straight or branched of 0.1～2.0% mass percent and diethylene glycol monoacrylate or the ethylene glycol methacrylate of 0.1～1.5% mass percent.Reactant liquor all contains the isopropyl alcohol of mass percent 25%, mass percent 0.8% iron ammonium sulfate, mass percent 1.8% sulfuric acid.Then, the macromolecule nonwoven fabrics is immersed in the aqueous solution that contains alkyl acrylate after 24 hours, nonwoven fabrics is taken out is positioned in the tygon sealing bag, after the deoxygenation of nitrogen stripping, be positioned over the intrafascicular irradiation that carries out of high energy electron, irradiation dose is 20～60KGy.After irradiation, taking out nonwoven fabrics infiltrates in the aqueous solution that contains diethylene glycol monoacrylate or ethylene glycol methacrylate after 24 hours again, after the repetition above-mentioned steps is carried out irradiation reaction, adopt the Soxhlet extraction process to remove unreacted monomer and homopolymer nonwoven fabrics, extraction solvent is ethanol, after extracting nonwoven fabrics under 60 ℃ of conditions vacuum drying to constant weight.
It is as follows for the extracting process of environmental water sample low concentration Determination of Trace Phenol compounds that the present invention contains amphipathic functional group macromolecule nonwoven fabrics Solid-Phase Extraction material:
To contain the circle that amphipathic functional group macromolecule nonwoven fabrics is cut into certain area, the single or multiple lift stack is used as the Solid-Phase Extraction diaphragm, can adopt solvent filtration apparatus manually to carry out the extracting and enriching of water sample.Also the stack of diaphragm single or multiple lift can be filled in the robotization solid-phase extraction device and use.
Use has the method that amphipathic Solid-Phase Extraction diaphragm carries out the water sample Solid-Phase Extraction, comprises the following steps:
1. activation: amphipathic Solid-Phase Extraction diaphragm is activated with methyl alcohol drip washing;
2. load sample: under negative pressure, will contain the oxybenzene compound water sample by the extraction diaphragm;
3. washing: under negative pressure, water rinses and drains moisture in diaphragm after diaphragm is removed impurity;
4. wash-out: use methyl alcohol to carry out wash-out to adsorption compound, collect eluent and make chromatograph measure oxybenzene compound content.
Following characteristics and beneficial effect that the present invention has:
1. the combination of practical function monomer and macromolecule nonwoven fabrics in the high energy electron irradiation system, because high energy electron has than macro-energy, can penetrate matrix surface within very short time and make its activation produce free radical, the simultaneous reactions monomer also produces free radical, and the reaction that makes monomer be bonded in the matrix fiber surface occurs fast.Irradiation process only tens seconds to a few minutes just can impel reaction to occur, so should the reaction power consumption lower.
2. carry out reaction kinetic in the high energy electron irradiation system, reaction solution only needs nonwoven fabrics matrix material is infiltrated, and uses the consumptions such as solvent, function monomer, polymerization inhibitor less in reaction, and it is few that end reaction produces waste liquid amount.
3. in the present invention, nonwoven fabrics matrix used is the commercial goods, and material source is extensively cheap, finally obtains cost of products lower.
4. the final nonwoven fabrics that obtains contains alkyl acrylate lipophilic group and hydroxyl Arrcostab hydrophilic radical, makes in nonwoven cloth material extracting phenols compounds process and brings into play simultaneously acting force and hydrogen bond action between non-polar molecule, has higher extraction ability.
5. the nonwoven cloth material of the present invention's acquisition can be prepared into the use of Solid-Phase Extraction disc diaphragm, has very fast mass transfer velocity in this nonwoven cloth material enrichment water sample process, thereby accelerates the processing speed of sample, can realize the fast enriching extraction of large volume environmental water sample.
Embodiment
Embodiment 1
A kind of preparation method of the Solid-Phase Extraction diaphragm that contains amphipathic functional group is as follows: at first preparation contains the reacting solution of two kinds of difference in functionality monomers.Preparation contains 25% isopropyl alcohol, 0.8% iron ammonium sulfate, 1.8% sulfuric acid, the aqueous solution of 0.3% octadecyl acrylate; Preparation contains 25% isopropyl alcohol, 0.8% iron ammonium sulfate, 1.8% sulfuric acid, the diethylene glycol monoacrylate of 0.1% mass percent.Then, polypropylene-polyethylene copolymerization melt spraying non-woven fabrics was immersed in the aqueous solution that contains octadecyl acrylate after 24 hours, nonwoven fabrics is taken out is positioned in the tygon sealing bag, after the deoxygenation of nitrogen stripping, be positioned over the intrafascicular irradiation that carries out of high energy electron, irradiation dose is 20KGy.After irradiation, taking out nonwoven fabrics infiltrates in the aqueous solution that contains diethylene glycol monoacrylate after 24 hours again, after the repetition above-mentioned steps is carried out irradiation reaction, adopt the Soxhlet extraction process to remove unreacted monomer and homopolymer nonwoven fabrics, extraction solvent is ethanol, after extracting nonwoven fabrics under 60 ℃ of conditions vacuum drying to constant weight.
Embodiment 2
A kind of preparation method of the Solid-Phase Extraction diaphragm that contains amphipathic functional group is as follows: at first preparation contains the reacting solution of two kinds of difference in functionality monomers.Preparation contains 25% isopropyl alcohol, 0.8% iron ammonium sulfate, 1.8% sulfuric acid, the aqueous solution of 0.8% octadecyl acrylate; Preparation contains 25% isopropyl alcohol, 0.8% iron ammonium sulfate, 1.8% sulfuric acid, the diethylene glycol monoacrylate of 0.1% mass percent.Then, polypropylene-polyethylene copolymerization melt spraying non-woven fabrics was immersed in the aqueous solution that contains octadecyl acrylate after 24 hours, nonwoven fabrics is taken out is positioned in the tygon sealing bag, after the deoxygenation of nitrogen stripping, be positioned over the intrafascicular irradiation that carries out of high energy electron, irradiation dose is 20KGy.After irradiation, taking out nonwoven fabrics infiltrates in the aqueous solution that contains diethylene glycol monoacrylate after 24 hours again, after the repetition above-mentioned steps is carried out irradiation reaction, adopt the Soxhlet extraction process to remove unreacted monomer and homopolymer nonwoven fabrics, extraction solvent is ethanol, after extracting nonwoven fabrics under 60 ℃ of conditions vacuum drying to constant weight.
Embodiment 3
A kind of preparation method of the Solid-Phase Extraction diaphragm that contains amphipathic functional group is as follows: at first preparation contains the reacting solution of two kinds of difference in functionality monomers.Preparation contains 25% isopropyl alcohol, 0.8% iron ammonium sulfate, 1.8% sulfuric acid, the aqueous solution of 0.3% octadecyl acrylate; Preparation contains 25% isopropyl alcohol, 0.8% iron ammonium sulfate, 1.8% sulfuric acid, the diethylene glycol monoacrylate of 0.1% mass percent.Then, polypropylene-polyethylene copolymerization melt spraying non-woven fabrics was immersed in the aqueous solution that contains octadecyl acrylate after 24 hours, nonwoven fabrics is taken out is positioned in the tygon sealing bag, after the deoxygenation of nitrogen stripping, be positioned over the intrafascicular irradiation that carries out of high energy electron, irradiation dose is 40KGy.After irradiation, taking out nonwoven fabrics infiltrates in the aqueous solution that contains diethylene glycol monoacrylate after 24 hours again, after the repetition above-mentioned steps is carried out irradiation reaction, adopt the Soxhlet extraction process to remove unreacted monomer and homopolymer nonwoven fabrics, extraction solvent is ethanol, after extracting nonwoven fabrics under 60 ℃ of conditions vacuum drying to constant weight.
Embodiment 4
A kind of preparation method of the Solid-Phase Extraction diaphragm that contains amphipathic functional group is as follows: at first preparation contains the reacting solution of two kinds of difference in functionality monomers.Preparation contains 25% isopropyl alcohol, 0.8% iron ammonium sulfate, 1.8% sulfuric acid, the aqueous solution of 1.0% octadecyl acrylate; Preparation contains 25% isopropyl alcohol, 0.8% iron ammonium sulfate, 1.8% sulfuric acid, the diethylene glycol monoacrylate of 0.5% mass percent.Then, polypropylene-polyethylene copolymerization melt spraying non-woven fabrics was immersed in the aqueous solution that contains octadecyl acrylate after 24 hours, nonwoven fabrics is taken out is positioned in the tygon sealing bag, after the deoxygenation of nitrogen stripping, be positioned over the intrafascicular irradiation that carries out of high energy electron, irradiation dose is 20KGy.After irradiation, taking out nonwoven fabrics infiltrates in the aqueous solution that contains diethylene glycol monoacrylate after 24 hours again, after the repetition above-mentioned steps is carried out irradiation reaction, adopt the Soxhlet extraction process to remove unreacted monomer and homopolymer nonwoven fabrics, extraction solvent is ethanol, after extracting nonwoven fabrics under 60 ℃ of conditions vacuum drying to constant weight.Hydroxyl is difference grafting long-chain octadecyl acrylate (SA) and water wettability senecioate-two kinds of monomers of hydroxyl ethyl ester (HEA) on polypropylene (PP) fibrous matrix, and with this fiber as solid phase extraction filler, be used for the Determination of Trace Phenol of Solid-Phase Extraction (SPE) water.
Embodiment 5
A kind of preparation method of the Solid-Phase Extraction diaphragm that contains amphipathic functional group is as follows: at first preparation contains the reacting solution of two kinds of difference in functionality monomers.Preparation contains 25% isopropyl alcohol, 0.8% iron ammonium sulfate, 1.8% sulfuric acid, the aqueous solution of 0.1 octadecyl acrylate; Preparation contains 25% isopropyl alcohol, 0.8% iron ammonium sulfate, 1.8% sulfuric acid, the diethylene glycol monoacrylate of 0.1% mass percent.Then, polypropylene-polyethylene copolymerization melt spraying non-woven fabrics was immersed in the aqueous solution that contains octadecyl acrylate after 24 hours, nonwoven fabrics is taken out is positioned in the tygon sealing bag, after the deoxygenation of nitrogen stripping, be positioned over the intrafascicular irradiation that carries out of high energy electron, irradiation dose is 60KGy.After irradiation, taking out nonwoven fabrics infiltrates in the aqueous solution that contains diethylene glycol monoacrylate after 24 hours again, after the repetition above-mentioned steps is carried out irradiation reaction, adopt the Soxhlet extraction process to remove unreacted monomer and homopolymer nonwoven fabrics, extraction solvent is ethanol, after extracting nonwoven fabrics under 60 ℃ of conditions vacuum drying to constant weight.
Embodiment 6
By the amphipathic nonwoven fabrics that embodiment prepares, be cut into Φ 47mm or Φ 90mm circular, the single or multiple lift stack is used as the Solid-Phase Extraction diaphragm, can adopt solvent filtration apparatus manually to carry out the extracting and enriching of water sample.Also the stack of diaphragm single or multiple lift can be filled in the robotization solid-phase extraction device and use.
Use has the method that amphipathic Solid-Phase Extraction diaphragm carries out the water sample Solid-Phase Extraction, comprises the following steps:
4. activation: amphipathic Solid-Phase Extraction diaphragm is activated with methyl alcohol drip washing;
5. load sample: under negative pressure, will contain the oxybenzene compound water sample by the extraction diaphragm;
6. washing: under negative pressure, water rinses and drains moisture in diaphragm after diaphragm is removed impurity;
7. wash-out: use methyl alcohol to carry out wash-out to adsorption compound, collect eluent and make chromatograph measure oxybenzene compound content.
Above-described embodiment is only that explanation is of the present invention for example, is not the restriction to embodiments of the present invention.Everyly belong to the row that apparent variation that technical scheme of the present invention amplifies out or change still are in protection scope of the present invention.
Claims (8)
1. preparation method who contains the Solid-Phase Extraction diaphragm of amphipathic functional group: selecting polypropylene and tygon copolymerization meltblown fibers nonwoven fabrics is matrix material, and fibre diameter is 8～20 μ m; The process of macromolecule nonwoven cloth material and two kinds of different monomers reactions, at first preparation contains the reacting solution of two kinds of difference in functionality monomers; This reacting solution contains respectively the alkyl acrylate of straight or branched of 0.1～2.0% mass percent and diethylene glycol monoacrylate or the ethylene glycol methacrylate of 0.1～1.5% mass percent; Reactant liquor all contains 25% isopropyl alcohol, iron ammonium sulfate 0.8%, sulfuric acid 1.8%; Then, the macromolecule nonwoven fabrics is immersed in the aqueous solution that contains alkyl acrylate after 24 hours, nonwoven fabrics is taken out is positioned in the tygon sealing bag, after the deoxygenation of nitrogen stripping, be positioned over the intrafascicular irradiation that carries out of high energy electron, irradiation dose is 20～60KGy; After irradiation, taking out nonwoven fabrics infiltrates in the aqueous solution that contains diethylene glycol monoacrylate or ethylene glycol methacrylate after 24 hours again, after the repetition above-mentioned steps is carried out irradiation reaction, adopt the Soxhlet extraction process to remove unreacted monomer and homopolymer nonwoven fabrics, extraction solvent is ethanol, after extracting nonwoven fabrics under 60 ℃ of conditions vacuum drying to constant weight.
2. according to the described preparation method of claims 1, it is characterized in that, the base material that solid-phase extraction membrane uses is polypropylene and tygon copolymerization meltblown fibers nonwoven fabrics.
3. according to the described preparation method of claims 1, it is characterized in that the functionalization monomer of selecting is alkyl acrylate and diethylene glycol monoacrylate or the ethylene glycol methacrylate of straight or branched.
4. preparation method described according to claims 1, it is characterized in that nonwoven fabrics matrix material is soaked in reacting solution 24 hours, this aqueous solution contains the isopropyl alcohol of 25% mass percent, the iron ammonium sulfate of mass percent 0.8%, the sulfuric acid of 1.8% mass percent.
5. preparation method described according to claims 1 is characterized in that containing respectively in two kinds of aqueous solution of reaction that nonwoven fabrics matrix material soaks the alkyl acrylate of 0.1～2.0% straight or branched and diethylene glycol monoacrylate or the ethylene glycol methacrylate of 0.1～1.5% mass percent.
6. preparation method described according to claims 1, two kinds of function monomers are to complete in the high-energy electron beam irradiation system at nonwoven surface generation bonding reaction.
7. preparation method described according to claims 1, high-power electron beam is 20～60KGy to the irradiation dose of nonwoven cloth material.
8. use amphipathic functional group macromolecule nonwoven fabrics as the method for low concentration or Determination of Trace Phenol compounds in Solid-Phase Extraction diaphragm extracting and enriching environment water, it is characterized in that, nonwoven fabrics is cut into the circle of Φ 47mm or Φ 90mm, the single or multiple lift stack is used as the Solid-Phase Extraction diaphragm, can adopt solvent filtration apparatus manually to carry out the extracting and enriching of water sample; Also the stack of diaphragm single or multiple lift can be filled in the robotization solid-phase extraction device and use.
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| CN106000134A (en) * | 2016-07-08 | 2016-10-12 | 天津工业大学 | Temperature-sensitive filtering membrane with small pore size distribution and preparation method thereof |
| CN111729344A (en) * | 2020-06-15 | 2020-10-02 | 宁波锋成先进能源材料研究院 | Treatment method of amphiphilic nano material and purified amphiphilic nano material |
| CN112447353A (en) * | 2020-11-25 | 2021-03-05 | 滁州恒通磁电科技有限公司 | Anti-corrosion magnetic material and production process thereof |
| WO2022233343A1 (en) * | 2021-07-08 | 2022-11-10 | Focus E-Beam Technology Pte. Ltd. | Method and device for manufacturing hydrophilic substrate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112447353B (en) * | 2020-11-25 | 2024-04-02 | 滁州恒通磁电科技有限公司 | Corrosion-resistant magnetic material and production process thereof |
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Application publication date: 20130508 |