CN106310710A - Preparation method of magnetic graphene oxide and method for detecting naphthalene content in water by using magnetic graphene oxide solid-phase extraction - Google Patents
Preparation method of magnetic graphene oxide and method for detecting naphthalene content in water by using magnetic graphene oxide solid-phase extraction Download PDFInfo
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- CN106310710A CN106310710A CN201610829109.5A CN201610829109A CN106310710A CN 106310710 A CN106310710 A CN 106310710A CN 201610829109 A CN201610829109 A CN 201610829109A CN 106310710 A CN106310710 A CN 106310710A
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- graphene oxide
- magnetic
- naphthalene
- magnetic oxygenated
- water
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/02—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor with moving adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Abstract
The invention discloses a preparation method of magnetic graphene oxide and a method for detecting naphthalene content in water by using magnetic graphene oxide solid-phase extraction. The preparation method includes: dissolving the graphene oxide in an ethylene glycol solution in a scattered manner for ultrasonic concussion; adding FeCl3.6H2O and NaOAc prior to mechanical stirring; putting mixed liquid into a teflon stainless reactor at the reaction temperature of 190-200DEG C for 5-6 hours of reaction; subjecting obtained samples to filtering and washing with plenty of water and ethyl alcohol prior to drying in an oven to obtain the magnetic graphene oxide. The detection includes the steps of mixing, solid-liquid separation, washing, elution and detection. The magnetic graphene oxide is simple and rapid in preparation technology, high adsorption capability of the graphene oxide on naphthalene can be fully utilized, the magnetic graphene oxide materials can be rapidly separated from sample solutions under the action of external magnetic field, dosage of the organic solutions is reduced, and high efficiency and environment protection are achieved; limit of detection of the naphthalene in water can be effectively improved.
Description
Technical field
The present invention relates to a kind of method preparing magnetic oxygenated Graphene, and utilize magnetic oxygenated Graphene, pass through solid phase
The mode of extraction measures the method for the content of naphthalene in water body.
Background technology
Naphthalene is a kind of condensed-nuclei aromatics, molecular formula C10H8, white and volatile, and have special odor.Produce organic chemical industry
In, it is widely used as preparing the raw material of dyestuff, resin, solvent etc., possesses important value.On its basis, synthesis is derivative
The main naphthols of thing, naphthalene acetic acid, is medicine, the important source material of synthetic rubber etc..The environmental pollution that naphthalene and derivant are brought, with
And human body toxic it is verified that, the relevant diseases such as such as cataract, optic neuritis, cancer can be caused.Therefore, for us
The material of everyday life contact, is necessary for accurately detecting the content of naphthalene and its derivative, and can carry out reclaiming profit to it
With.
Solid phase extraction techniques, as a kind of novel Sample Pretreatment Technique, is widely used at present, solid phase extraction techniques
Typically have the advantage that the high-recovery of 1. objects.2. reduce the usage amount of organic solvent, more environmental protection.3. energy
Enough process small samples.The most simple to operate, it is easy to automatization.At present solid phase extraction techniques with gas phase and liquid phase chromatograph skill
Art is combined, and is widely used in productive life.Current study hotspot focuses primarily upon new solid phase extraction filler and solid phase is micro-
Extraction fiber coating.
Graphene, as a kind of Two-dimensional Carbon nano material being widely studied, has specific surface area big, high adsorption capacity and
The character such as mechanical strength is high.Comparing Graphene, surface of graphene oxide has the oxygen-containing officials such as a large amount of epoxy radicals, phenolic hydroxyl group and carboxyl
Can roll into a ball, therefore can be widely used for being grafted dissimilar compound, thus generate the composite of different functionalities, relevant oxidation stone
Prepared by the design of ink alkene and functional composite material thereof, have become as study hotspot and the core separating analysis field.In recent years,
Graphene oxide has been used as Solid-Phase Extraction, dispersive solid-phase extraction, Magnetic solid phases extraction and solid-phase microextraction, but is studying
Journey finds, owing to graphene oxide is that a kind of density is the lowest, the material that specific surface area is the biggest, cause at same sample solution
The when of separation, it is impossible to use is centrifugal carries out solid-liquid separation, and direct Graphene causes post pressure as solid phase extraction filler simultaneously
Excessive, solid phase extraction column is damaged, and simultaneous oxidation Graphene can occur irreversible reunion, and the absorption of impact analysis thing is conciliate
Inhale.Magnetic oxygenated Graphene can effectively utilize magnetic apparatus and reclaim, and overcomes its defect in Solid-Phase Extraction, protects
Stay the advantage of graphene oxide, there is important practical value.
Summary of the invention
For the technical problem of above-mentioned existence, it is an object of the invention to: propose and a kind of prepare magnetic oxygenated Graphene
Method, and utilize magnetic oxygenated Graphene, by the way of Solid-Phase Extraction, measure the method for the content of naphthalene in water body.
The technical solution of the present invention is achieved in that the preparation method of a kind of magnetic oxygenated Graphene, including with
Lower step:
1) by graphene oxide dispersing and dissolving in ethylene glycol solution, ultrasonic vibration 2.5-3h;
2) FeCl3 6H2O and NaOAc, mechanical agitation 2.5-30min it are subsequently adding;
3) putting in politef stainless steel cauldron by this mixed liquor, temperature is 190-200 DEG C of reaction 5-6h;
4) gained sample filtering, and with a large amount of water and alcohol flushing, finally 45-50 ° of C oven for drying 4.5-5h.
A kind of utilize the method for naphthalene content in magnetic oxygenated Graphene solid phase extraction detection water body, it is characterised in that: bag
Include following operating procedure:
A) mixing: weigh the magnetic oxygenated Graphene of synthesis, put into containing in the beaker of the aqueous solution of naphthalene, be sufficiently stirred for, concussion
4-6min;
B) solid-liquid separation: the Magnet that magnetic is 1T is put in the outer measuring of beaker, it is achieved magnetic oxygenated Graphene divides with the solid-liquid of aqueous solution
From;
C) clean: get rid of the aqueous solution after extraction, and magnetic oxygenated Graphene water is cleaned three times;
D) eluting: adding eluting solution in magnetic oxygenated Graphene, fully concussion 30-60 s, utilizes Magnet to make the same magnetic of methanol
Property graphene oxide separate;
E) detection: by methanol sample introduction, carries out chromatograph detection naphthalene content.
Preferably, described eluting solution is methanol.
Due to the utilization of technique scheme, the present invention compared with prior art has the advantage that
The magnetic oxygenated Graphene solid phase extraction of producing and utilize of a kind of magnetic oxygenated Graphene of the present invention detects in water body
The method of naphthalene content, prepares the technique simple and fast of magnetic oxygenated Graphene, it is possible to make full use of the graphene oxide height to naphthalene
Absorbability, under the effect of externally-applied magnetic field, makes magnetic oxygenated grapheme material carry out sharp separation with sample solution, can be anti-
Make full use of magnetic oxygenated Graphene again, and reduce the consumption of organic solvent, economic and environment-friendly;Naphthalene in water can be effectively improved
Detection limit.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings technical solution of the present invention is described further:
Accompanying drawing 1 is that the magnetic oxygenated Graphene solid phase extraction of producing and utilize of a kind of magnetic oxygenated Graphene of the present invention detects
In water body the sample of the method for naphthalene content be 0.1ppm naphthalene aqueous solution extraction before and after chromatogram;
Accompanying drawing 2 is that the magnetic oxygenated Graphene solid phase extraction of producing and utilize of a kind of magnetic oxygenated Graphene of the present invention detects
The linearity curve of the method for naphthalene content and scope y=9319000x+139624 in water body.
Detailed description of the invention
The present invention is described below in conjunction with the accompanying drawings.
Of the present invention: the preparation method of a kind of magnetic oxygenated Graphene, comprise the following steps:
1) by 0.4370g graphene oxide dispersing and dissolving in 70ml ethylene glycol solution, ultrasonic vibration 3h;
2) 1.4g FeCl it is subsequently adding3•6H2O and 2.8g NaOAc, mechanical agitation 30min;
3) being put into by this mixed liquor in 100ml politef stainless steel cauldron, temperature is 200 DEG C, reacts 6h;
4) gained sample filtering, and with a large amount of water and alcohol flushing, finally at 45 DEG C, oven for drying 5h.
A kind of utilize the method for naphthalene content in magnetic oxygenated Graphene solid phase extraction detection water body, it is characterised in that: bag
Include following operating procedure:
A) mixing: weighing the magnetic oxygenated Graphene 20mg of synthesis, be equipped with 10ml, concentration is the aqueous solution of the naphthalene of 1ppm
Beaker is this, is sufficiently stirred for, and shakes 5 min;
B) solid-liquid separation: the Magnet that magnetic is 1T is put in the outer measuring of beaker, it is achieved magnetic oxygenated Graphene divides with the solid-liquid of aqueous solution
From;
C) clean: get rid of the aqueous solution after extraction, and magnetic oxygenated Graphene water is cleaned three times;
D) eluting: add methanol in magnetic oxygenated Graphene and make eluting solution, fully concussion 60 s, utilizes Magnet to make methanol same
Magnetic oxygenated Graphene separates;
E) detection: by methanol sample introduction, carries out chromatograph detection naphthalene content;Chromatographic condition is set to: sample size 1ul, wavelength 254nm, stream
Speed 1ml/min, flowing is 100% methanol mutually.
As accompanying drawing 1,2 show detection collection of illustrative plates, based on this Magnetic solid phases abstraction technique, it is possible to be effectively improved the inspection of naphthalene in water
Survey limit, in 0.001-1ppm concentration range in extraordinary linearly, its linear equation linear regression coeffficient (R2) it is 0.9979,
Impart graphene oxide composite material magnetic by simple process, under the effect of externally-applied magnetic field, make magnetic oxygenated grapheme material
Carry out sharp separation with sample solution, then carry out eluting, reach the purpose of extraction detection naphthalene content, the method increase the suction of naphthalene
Attached amount, reduces the loss of adsorbent.
Above-described embodiment, only for technology design and the feature of the explanation present invention, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and is carried out, and can not limit the scope of the invention with this, all according to the present invention
The equivalence that spirit is made changes or modifies, and all should contain within the scope of the present invention.
Claims (3)
1. the preparation method of a magnetic oxygenated Graphene, it is characterised in that: comprise the following steps:
By graphene oxide dispersing and dissolving in ethylene glycol solution, ultrasonic vibration 2.5-3h;
It is subsequently adding FeCl3•6H2O and NaOAc, mechanical agitation 2.5-30min;
This mixed liquor is put in politef stainless steel cauldron, 190-200 DEG C of reaction 5-6h;
Gained sample filtering, and with a large amount of water and alcohol flushing, finally 45-50 ° of C oven for drying 4.5-5h.
2. one kind utilizes the method for naphthalene content in magnetic oxygenated Graphene solid phase extraction detection water body, it is characterised in that: include
Following operating procedure:
Mixing: weigh the magnetic oxygenated Graphene of synthesis, put into containing in the beaker of the aqueous solution of naphthalene, be sufficiently stirred for, shakes 4-
6min;
Solid-liquid separation: the Magnet that magnetic is 1T is put in the outer measuring of beaker, it is achieved magnetic oxygenated Graphene and the solid-liquid separation of aqueous solution;
Clean: get rid of the aqueous solution after extraction, and magnetic oxygenated Graphene water is cleaned three times;
Eluting: add eluting solution in magnetic oxygenated Graphene, fully the concussion 30-60 second, utilize Magnet to make the same magnetic of methanol
Graphene oxide separates;
Detection: by methanol sample introduction, carries out chromatograph detection naphthalene content.
The most according to claim 2 a kind of utilize the side of naphthalene content in magnetic oxygenated Graphene solid phase extraction detection water body
Method, it is characterised in that: described eluting solution is methanol.
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Cited By (6)
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CN107497398A (en) * | 2017-09-18 | 2017-12-22 | 同济大学 | Utilize the method for variation magnetic field enhancing magnetic adsorbent adsorption capacity |
CN108854976A (en) * | 2018-07-23 | 2018-11-23 | 南华大学 | For the adsorbent of uranium in uranium-containing waste water and the adsorption method of uranium-containing waste water |
CN109336100A (en) * | 2018-09-28 | 2019-02-15 | 潍坊职业学院 | A kind of magnetic graphene with core-shell structure, the application in Detecting Pesticide and application method |
CN109908866A (en) * | 2019-03-28 | 2019-06-21 | 中国科学院兰州化学物理研究所 | The method and its application of two-dimensional magnetic porous carbon composite are prepared by calcining |
CN112697868A (en) * | 2020-12-22 | 2021-04-23 | 江苏荣坔环保科技有限公司 | Method for measuring trivalent antimony and pentavalent antimony by magnetic solid phase extraction-ICP-MS (inductively coupled plasma-mass spectrometry) method |
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Cited By (9)
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---|---|---|---|---|
CN107497398A (en) * | 2017-09-18 | 2017-12-22 | 同济大学 | Utilize the method for variation magnetic field enhancing magnetic adsorbent adsorption capacity |
CN108854976A (en) * | 2018-07-23 | 2018-11-23 | 南华大学 | For the adsorbent of uranium in uranium-containing waste water and the adsorption method of uranium-containing waste water |
CN108854976B (en) * | 2018-07-23 | 2021-06-08 | 南华大学 | Adsorbent for uranium in uranium-containing wastewater and adsorption method of uranium-containing wastewater |
CN109336100A (en) * | 2018-09-28 | 2019-02-15 | 潍坊职业学院 | A kind of magnetic graphene with core-shell structure, the application in Detecting Pesticide and application method |
CN109908866A (en) * | 2019-03-28 | 2019-06-21 | 中国科学院兰州化学物理研究所 | The method and its application of two-dimensional magnetic porous carbon composite are prepared by calcining |
CN109908866B (en) * | 2019-03-28 | 2021-12-31 | 中国科学院兰州化学物理研究所 | Method for preparing two-dimensional magnetic porous carbon composite material through calcination and application thereof |
CN112697868A (en) * | 2020-12-22 | 2021-04-23 | 江苏荣坔环保科技有限公司 | Method for measuring trivalent antimony and pentavalent antimony by magnetic solid phase extraction-ICP-MS (inductively coupled plasma-mass spectrometry) method |
CN115047108A (en) * | 2022-06-16 | 2022-09-13 | 陕西科技大学 | Rapid high-throughput screening method for antibiotic drug residues in mutton |
CN115047108B (en) * | 2022-06-16 | 2024-01-16 | 陕西科技大学 | Rapid high-throughput screening method for antibiotic drug residues in mutton |
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