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Preparation method and application of magnetic metal - organic nanotube material

A technology of organic nanotubes and magnetic metals, applied in the field of environmental inspection, can solve the problems of low recycling rate and poor enrichment effect, achieve high sensitivity, easy desorption, and improve the effect of extraction

Active Publication Date: 2016-06-22
SHANDONG ANALYSIS & TEST CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the magnetic particles reported in the existing literature also have some disadvantages in the detection of pollutants in the environment, such as poor enrichment effect, low reuse rate, etc.

Method used

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  • Preparation method and application of magnetic metal - organic nanotube material
  • Preparation method and application of magnetic metal - organic nanotube material
  • Preparation method and application of magnetic metal - organic nanotube material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Embodiment 1: the preparation of magnetic metal-organic nanotube material, such as figure 1 Shown:

[0053] 1. Solvothermal Synthesis of Fe 3 o 4 nanomaterials:

[0054] 2.7gFeCl 3 ·6H 2 O was dissolved in 50mL of ethylene glycol, and after stirring for half an hour, 5.75g of sodium acetate was added. After stirring for half an hour, it was transferred to an 80mL reaction kettle, and reacted at 473K for 8 hours. After cooling to room temperature, it was washed with ethanol and dried.

[0055] 2. Fe 3 o 4 Surface hydroxylation modification

[0056] 0.25gFe 3 o 4 Add to 50mL sodium dodecylsulfonate solution and stir for 4 hours. Note that 15 minutes of sonication is required for every 1 hour of stirring to ensure uniform dispersion. The samples were then washed and dried.

[0057] 3. Fe 3 o 4 Surface silanization treatment:

[0058] 0.15 g hydroxylated Fe 3 o 4 Disperse in 75 mL of absolute ethanol, add 0.66 mL of 3-aminopropyltrimethoxysilane dropwise an...

Embodiment 2

[0063] Example 2: Condition selection and optimization for improving the enrichment effect of magnetic metal-organic nanotube materials

[0064] The adsorption material prepared in Example 1 carried out magnetic solid-phase extraction:

[0065] Add 10mL of the sample to be tested into the 20mL headspace bottle, and add the prepared magnetic adsorption material into it. Extraction under the action of ultrasound for a period of time to complete the extraction process. After the extraction is completed, the extraction solution is removed under the action of an external magnetic field, and 5 mL of desorption solvent is added for ultrasonic desorption. After the desorption process was completed, the desorption solution was taken out and blown with nitrogen, and 50 μL of the desorption solvent was reconstituted and then directly entered into the instrument for analysis.

[0066] In order to improve the enrichment effect of magnetic solid-phase extraction of this material, the impo...

Embodiment 3

[0067] Example 3: Investigation of the detection limit, linear range and correlation coefficient of the method for detecting polychlorinated biphenyls based on magnetic solid-phase extraction and fast gas chromatography-tandem mass spectrometry

[0068] 1. Chromatography and mass spectrometry conditions:

[0069] Chromatographic column: DB-35MS chromatographic column (30m×0.25mm×0.25μm); column temperature adopts temperature program: initial 150°C and keep for 1min, 10°C / min to 290°C, keep for 4min; carrier gas: 1.0ml / min helium gas; collision gas: 1.5ml / min high-purity N 2 ; EI source is used for mass spectrometry; electron energy: 70ev; detector temperature is 280°C, ion source temperature is 250°C. Multiple reaction monitoring mode was used. See Table 1 for details.

[0070] Table 1 Chromatography-mass spectrometry parameters of seven polychlorinated biphenyls in gas chromatography tandem mass spectrometry MRM mode

[0071]

[0072] Under optimized conditions, the an...

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Abstract

The invention discloses a preparation method and an application of a magnetic metal - organic nanotube material. The preparation method comprises the following steps of (1) preparation of a Fe3O4 (ferroferric oxide) nanometer material; (2) surface hydroxylation of the Fe3O4 nanometer material: adding the Fe3O4 nanometer material prepared in step (1) into sodium dodecyl sulfate, stirring, and performing ultrasonic reaction; (3) surface silanization of Fe3O4; (4) connecting of the silanized Fe3O4 and 4,4'-biphenyldicarboxylic acid; (5) connecting of the surface of Fe3O4 modified by the 4,4'-biphenyldicarboxylic acid and the metal-organic nanotube material. The prepared metal-nanotube material has the advantages that [Co2(bpdc)1.5(Hbpz] DMF CH3CN H2O crystals of a metal - organic nanotube are radially and uniformly distributed at the surface of Fe3O4, and form a sea urchin shape; a one-dimensional weaving structure is formed by stacking different lengths in an overlapping way, so that the absorbing of polychlorinated biphenyl in a sample is favorable.

Description

technical field [0001] The invention relates to a preparation method of a magnetic metal-organic nanotube and its application in detecting polychlorinated biphenyls, belonging to the technical field of environmental inspection. Background technique [0002] Polychlorinated biphenyls are a class of industrial chemicals, which are a class of chlorides formed by replacing the hydrogen atoms on the biphenyl ring with 1-10 chlorines. Due to its characteristics of bioaccumulation, toxicity, and persistence, PCBs became the first batch of persistent organic pollutants included in the controlled list of the "Stockholm Convention on Persistent Organic Pollutants". Polychlorinated biphenyls have good stability, heat resistance and insulation, and can be used as lubricating materials, plasticizers, heat carriers, etc., and are widely used in industrial fields. PCBs can enter the human body through the food chain, causing cumulative poisoning, causing endocrine system disorders, reprod...

Claims

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Application Information

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IPC IPC(8): B01J20/30B01J20/22B01J20/28B01J20/281B01D15/08G01N30/02G01N30/06
CPCB01D15/08B01J20/223B01J20/28007B01J20/28009B01J20/281B01J2220/4806B01J2220/4812B01J2220/52G01N30/02G01N30/06G01N2030/025G01N2030/062
Inventor 赵汝松李秋琳王磊磊王珊珊王晓利王霞
Owner SHANDONG ANALYSIS & TEST CENT
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